On-line preconcentration and speciation of arsenic by flow injection hydride generation atomic absorption spectrophotometry.

PubMed

Narcise, Cristine Ingrid S; Coo, Lilibeth Dlc; Del Mundo, Florian R

2005-12-15

A flow injection-column preconcentration-hydride generation atomic absorption spectrophotometric (FI-column-HGAAS) method was developed for determining mug/l levels of As(III) and As(V) in water samples, with simultaneous preconcentration and speciation. The speciation scheme involved determining As(V) at neutral pH and As(III+V) at pH 12, with As(III) obtained by difference. The enrichment factor (EF) increased with increase in sample loading volume from 2.5 to 10ml, and for preconcentration using the chloride-form anion exchange column, EFs ranged from 5 to 48 for As(V) and 4 to 24 for As(III+V), with corresponding detection limits of 0.03-0.3 and 0.07-0.3mug/l. Linear concentration range (LCR) also varied with sample loading volume, and for a 5-ml sample was 0.3-5 and 0.2-8mug/l for As(V) and As(III+V), respectively. Sample throughput, which decreased with increase in sample volume, was 8-17 samples/h. For the hydroxide-form column, the EFS for 2.5-10ml samples were 3-23 for As(V) and 2-15 for As(III+V), with corresponding detection limits of 0.07-0.4 and 0.1-0.5mug/l. The LCR for a 5-ml sample was 0.3-10mug/l for As(V) and 0.2-20mug/l for As(III+V). Sample throughput was 10-20 samples/h. The developed method has been effectively applied to tap water and mineral water samples, with recoveries ranging from 90 to 102% for 5-ml samples passed through the two columns.

Concentration of viruses in beef extract by flocculation with ammonium sulfate.

PubMed Central

Shields, P A; Farrah, S R

1986-01-01

Bacteriophages and enteroviruses in water were adsorbed to positively charged filters (Virosorb 1MDS [AMF Cuno, Inc., Meriden, Conn.] or Seitz S [Republic Filters, Milldaler, Conn.]). Adsorbed viruses were eluted by treating the filters with 10% beef extract, pH 9. Organic flocculation of the beef extract at pH 3.5 permitted recovery of more than 40% of the enteroviruses tested but less than 15% of the bacteriophages present. A method was developed that uses salts at pH 7 to flocculate beef extract. Two volumes of saturated ammonium sulfate were added to beef extract, and both enteroviruses and bacteriophages were adsorbed to the flocs that formed. Greater than 70% of the enteroviruses and bacteriophages were recovered by centrifuging the sample and suspending the flocs in a small volume of distilled water. PMID:3006587

pH salivary analysis of subjects suffering from Sjögren's syndrome and laryngopharyngeal reflux.

PubMed

Corvo, Marco Antonio Dos Anjos; Eckley, Claudia Alessandra; Liquidato, Bianca Maria; Castilho, Gustavo Leão; Arruda, Cibelle Nunes de

2012-02-01

Saliva is one of the components for the digestive homeostasis. Recent studies have shown that patients with laryngopharyngeal reflux (LPR) present a drop in salivary pH. Patients with Sjögren's syndrome (SS) are a potential clinical research model for xerostomia and its laryngeal and pharyngeal consequences. The aim was to evaluate the characteristics of saliva of patients with SS and LPR. 19 patients with SS plus LPR, and 12 healthy controls had their saliva studied prospectively for volume and pH. Two salivary samples were obtained from each participant: whole unstimulated saliva(WUS) and whole stimulated saliva(WSS) while chewing parafilm M®. All the participants were females. Mean age was 60 years (study group) and 44 years (control). LPR was diagnosed on all 19 subjects. The mean pH of WUS was 7.53 (SS) and 7.57 (controls), raising to 7.87 and 7.83 respectively after stimulation. The mean salivary volume of patients with SS was 1.27 mL (WUS) and 3.78 mL (WSS), whereas controls had a significantly higher salivary volume both before and after stimuli. A very high prevalence of LPR was found in patients with SS, which is probably caused by a uniform drop in salivary volume and all its contents, rather than a specific deficiency in its components, as shown previously in patients without SS.

Volume of reaction by the Archibald ultracentrifuge method (lobster hemocyanin).

PubMed

Saxena, V P; Kegeles, G; Kikas, R

1976-07-01

Samples of lobster hemocyanin (Homarus americanus) under conditions of reversible reaction between whole (25 S) and half (17 S) molecules have been subjected to accurately known nitrogen pressures in analytical ultracentrifuge cells. A modified pressurization chamber of the type developed by Schumaker and colleagues has been constructed for this purpose. The molecular weight was then determined at the top (liquid-gas) meniscus, by means of the Archibald method. The logarithmic dependence upon pressure of the derived equilibrium constant then gave directly the volume of reaction. Experiments were performed in veronal-citrate buffers at pH 8, where the molar volume of formation of whole (dodecameric) molecules from half molecules appears to be negative, and at pH 8.46 in veronal-citrate buffer in the presence of 0.003 molar free calcium ion, where the molar volume of formation was estimated to be + 390 cm3/mole. In glycine-sodium hydroxide buffer at pH 9.6 containing 0.0047 molar free calcium, the molar volume of formation of whole molecules was estimated to be +120 +/- 70 cm3, corresponding to an estimated difference in partial specific volume between whole molecules and half molecules of only 1.3 (10)-4cm3/gram. The correctness of the sign of this value in glycine buffer has been verified by pressure-jump light-scattering experiments.

Gastric pH and residual volume after 1 and 2 h fasting time for clear fluids in children†.

PubMed

Schmidt, A R; Buehler, P; Seglias, L; Stark, T; Brotschi, B; Renner, T; Sabandal, C; Klaghofer, R; Weiss, M; Schmitz, A

2015-03-01

Current guidelines suggest a fasting time of 2 h for clear fluids, which is often exceeded in clinical practice, leading to discomfort, dehydration and stressful anaesthesia induction to patients, especially in the paediatric population. Shorter fluid fasting might be a strategy to improve patient comfort but has not been investigated yet. This prospective clinical trial compares gastric pH and residual volume after 1 vs 2 h of preoperative clear fluid fasting. Children (1-16 yr, ASA I or II) undergoing elective procedures in general anaesthesia requiring tracheal intubation were randomized into group A with 60 min or B with 120 min preoperative clear fluid fasting. To determine gastric pH and residual volume, the gastric content was sampled in supine, left and right lateral patient position using an oro-gastric tube after intubation. Data are median (interquartile range) for group A or B (P<0.05). In total, 131 children aged 1.01-16.23 yr were included; gastric pH was determined in 120 cases. Patient characteristic data were similar between the two groups, except for gender (46/33 males in group A/B; P=0.02). Despite significantly shorter fasting times for clear fluids in group A compared with group B (76/136 min; P<0.001), no significant difference was observed regarding gastric pH [1.43 (1.30-1.56)/1.44 (1.29-1.68), P=0.66] or residual volume [0.43 (0.21-0.84)/0.46 (0.19-0.78) ml kg(-1), P=0.47]. One hour clear fluid fasting does not alter gastric pH or residual volume significantly compared with 2 h fasting. The study was approved by the local ethics committee (KEK-ZH-Nr. 2011-0034) and registered with ClinicalTrials.gov (NCT01516775). © The Author 2014. Published by Oxford University Press on behalf of the British Journal of Anaesthesia. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Rapid method for measuring rotenone in water at piscicidal concentrations

USGS Publications Warehouse

Dawson, V.K.; Harman, P.D.; Schultz, D.P.; Allen, J.L.

1983-01-01

A high-performance liquid chromatography (HPLC) procedure that is rapid, specific, and sensitive (limit of detection <0.005 mg/liter) was developed for monitoring application and degradation rates of rotenone. For analysis, a water sample is buffered to pH 5 and injected through a Sep Pak(R) C18 disposable cartridge. The cartridge adsorbs and retains the rotenone which then can be eluted quantitatively from the cartridge with a small volume of methanol. This step effectively concentrates the sample and provides sample cleanup. The methanol extract is analyzed directly by HPLC on an MCH 10 reverse-phase column; methanol: water (75:25, volume : volume) is the mobile phase and flow rate is 1.5 ml/minute. The rotenone is detected by ultraviolet spectrophotometry at a wavelength of 295 nm.

Effect of a commercial anion dietary supplement on acid-base balance, urine volume, and urinary ion excretion in male goats fed oat or grass hay diets.

PubMed

Stratton-Phelps, Meri; House, John K

2004-10-01

To determine whether feeding a commercial anionic dietary supplement as a urinary acidifier to male goats may be useful for management of urolithiasis. 8 adult sexually intact male Toggenburg, Saanen, and Nubian goats. Goats were randomly assigned by age-, breed-, and weight-matched pairs to an oat or grass hay diet that was fed for 12 days. On days 13 to 14 (early sample collection time before supplementation), measurements were made of blood and urine sodium, potassium, calcium, magnesium, chloride, phosphorus, and sulfur concentrations; blood and urine pH; urine production; and water consumption. During the next 28 days, the anionic dietary supplement was added to the oat and grass hay diets to achieve a dietary cation-anion difference of 0 mEq/100g of dry matter. Blood and urine samples were analyzed during dietary supplementation on days 12 to 13 (middle sample collection time) and 27 to 28 (late sample collection time). Blood bicarbonate, pH, and urine pH of goats fed grass hay and goats fed oat hay were significantly decreased during the middle and late sample collection times, compared with the early sample collection time. Water consumption and urine production in all goats increased significantly during the late sample collection time, compared with the early sample collection time. The anionic dietary supplement used in our study increases urine volume, alters urine ion concentrations, and is an efficacious urinary acidifier in goats. Goats treated with prolonged anionic dietary supplementation should be monitored for secondary osteoporosis from chronic urinary calcium loss.

Contained radiological analytical chemistry module

DOEpatents

Barney, David M.

1989-01-01

A system which provides analytical determination of a plurality of water chemistry parameters with respect to water samples subject to radiological contamination. The system includes a water sample analyzer disposed within a containment and comprising a sampling section for providing predetermined volumes of samples for analysis; a flow control section for controlling the flow through the system; and a gas analysis section for analyzing samples provided by the sampling system. The sampling section includes a controllable multiple port valve for, in one position, metering out sample of a predetermined volume and for, in a second position, delivering the material sample for analysis. The flow control section includes a regulator valve for reducing the pressure in a portion of the system to provide a low pressure region, and measurement devices located in the low pressure region for measuring sample parameters such as pH and conductivity, at low pressure. The gas analysis section which is of independent utility provides for isolating a small water sample and extracting the dissolved gases therefrom into a small expansion volume wherein the gas pressure and thermoconductivity of the extracted gas are measured.

Contained radiological analytical chemistry module

DOEpatents

Barney, David M.

1990-01-01

A system which provides analytical determination of a plurality of water chemistry parameters with respect to water samples subject to radiological contamination. The system includes a water sample analyzer disposed within a containment and comprising a sampling section for providing predetermined volumes of samples for analysis; a flow control section for controlling the flow through the system; and a gas analysis section for analyzing samples provided by the sampling system. The sampling section includes a controllable multiple port valve for, in one position, metering out sample of a predetermined volume and for, in a second position, delivering the material sample for analysis. The flow control section includes a regulator valve for reducing the pressure in a portion of the system to provide a low pressure region, and measurement devices located in the low pressure region for measuring sample parameters such as pH and conductivity, at low pressure. The gas analysis section which is of independent utility provides for isolating a small water sample and extracting the dissolved gases therefrom into a small expansion volume wherein the gas pressure and thermoconductivity of the extracted gas are measured.

One-step synthesis of magnetic graphene oxide nanocomposite and its application in magnetic solid phase extraction of heavy metal ions from biological samples.

PubMed

Sun, Jieping; Liang, Qionglin; Han, Qiang; Zhang, Xiaoqiong; Ding, Mingyu

2015-01-01

A novel magnetic graphene oxide nanocomposite was synthesized by one-step coprecipitation method and characterized by transmission electron microscopy, X-ray photoelectron spectroscopy and vibrating sample magnetometer. The nanocomposite beard many intriguing properties, including chemical stability, high adsorption capacity, and superparamagnetic. These properties evoked great interest and desire of its exploration in magnetic solid-phase extraction of heavy metal ions from complex samples. Several parameters effecting the analytical performance, such as the sample pH, amounts of adsorbent, sample volumes, elution volumes, and coexisting ions, had been investigated in detail. The adsorbed metal ions were easy eluted by controlling the pH condition and the materials could be reused more than 20 times. Under the optimized conditions, the limits of detection were 0.016, 0.046, 0.395, 0.038, 0.157 μg L(-1) for Co(2+), Ni(2+), Cu(2+), Cd(2+), and Pb(2+), respectively. The intra-day relative standard deviations (n=5) were in the range of 1.8-5.5% at 10 μg L(-1). The proposed method was successfully applied to biological sample analysis and got excellent recoveries in the range of 81-113% even the matrix was complex. Copyright © 2014 Elsevier B.V. All rights reserved.

[Analysis of the dilution deviation in CA19-9 measurement].

PubMed

Hanada, Hiroyuki; Takeoka, Keiko; Nomura, Tomoko; Moriyama, Takanori; Kanakura, Yuzuru

2005-04-01

CA19-9 widely used as a tumor marker of the pancreas and a bile duct. There are a number of reports which describes the measured value discrepancies between RIA and non-RIA kits. RIA results also have shown lack of the linearity over 70 U/ml when the samples are diluted. The pH condition at assay reaction for RIA had been suggested as the major reason, it has been denied by the results from the same pH condition at assay reaction used by COBAS CORE CA19-9 EIA II. On the other hand, the lack of RIA antibody titer is indicated for the discordant results by changing the sample volume to reagent volume ratio in the reaction. Our further investigation also indicates that the specific Lewis blood type, i.e. Le (a-b+), shows the linearity issues by RIA. The discrepancies are not caused by the reaction pH, but the amount of the antibody used in the RIA kit is closely associated. Considering the CA19-9 antibody nature used in RIA kit, which covers broad molecular range, users need to pay more attention to setting up each laboratory's measuring range.

Acid-rain induced changes in streamwater quality during storms on Catoctin Mountain, Maryland

USGS Publications Warehouse

Rice, Karen C.; Bricker, O.P.

1992-01-01

Catoctin Mountain receives some of the most acidic (lowest pH) rain in the United States. In 1990, the U.S. Geological Survey (USGS), in cooperation with the Maryland Department of the Environment (MDE) and the Maryland Department of Natural Resources (DNR), began a study of the effects of acid rain on the quality of streamwater on the part of Catoctin Mountain within Cunningham Falls State Park, Maryland (fig. 1). Samples of precipitation collected on the mountain by the USGS since 1982 have been analyzed for acidity and concentration of chemical constituents. During 1982-91, the volume-weighted average pH of precipitation was 4.2. (Volume weighting corrects for the effect of acids being washed out of the atmosphere at the beginning of rainfall). The pH value is measured on a logarithmic scale, which means that for each whole number change, the acidity changes by a factor of 10. Thus rain with a pH of 4.2 is more than 10 times as acidic as uncontaminated rain, which has a pH of about 5.6. The acidity of rain during several rainstorms on Catoctin Mountain was more than 100 times more acidic than uncontaminated rain.

Micro-apparatus for rapid determinations of protein solubilities

NASA Technical Reports Server (NTRS)

Pusey, Marc L.; Munson, Sibyl

1991-01-01

We have developed a column-based micro-technique for rapid determinations of protein solubilities. While retaining a large crystal surface area, the column dead volume has been reduced to equal to or less than 5 micro liters. The technique was tested with tetragonal lysozyme (pH 4.5, 0.1 M acetate, 3.0 percent NaCl, 5-25 C) and column volumes of about 60, 300, and 900 micro liters. Identical solubility data were obtained, indicating that equilibration was obtained even in the smallest columns. In addition, solubility data for Br- and I- salts of lysozyme (pH 4.5, 0.1 M acetate buffer, 0.5 M salt concentrations) were obtained. It appears that the technique can be further miniaturized. The limit in further reducing the crystalline column volume is determined by the minimum solution sample size needed to determine the protein concentration.

Effects of breathing pattern and inspired air conditions on breath condensate volume, pH, nitrite, and protein concentrations.

PubMed

McCafferty, J B; Bradshaw, T A; Tate, S; Greening, A P; Innes, J A

2004-08-01

The effects of breathing pattern and inspired air conditions on the volume and content of exhaled breath condensate (EBC) were investigated. Total exhaled water (TEW), EBC volume, pH, nitrite and protein concentrations were measured in three groups of 10 healthy subjects breathing into a condenser at different target minute ventilations (Vm), tidal volumes (Vt), and inspired air conditions. The volumes of both TEW and EBC increased significantly with Vm. For Vm 7.5, 15 and 22.5 l/min, mean (SD) EBC was 627 (258) microl, 1019 (313) microl, and 1358 (364) microl, respectively (p<0.001) and TEW was 1879 (378) microl, 2986 (496) microl, and 4679 (700) microl, respectively (p<0.001). TEW was significantly higher than EBC, reflecting a condenser efficiency of 40% at a target Vm of 7.5 l/min which reduced to 29% at Vm 22.5 l/min. Lower Vt gave less TEW than higher Vt (26.6 v 30.7 microl/l, mean difference 4.1 (95% CI 2.6 to 5.6), p<0.001) and a smaller EBC volume (4.3 v 7.6 microl/l, mean difference 3.4 (95% CI 2.3 to 4.5), p<0.001). Cooler and drier inspired air yielded less water vapour and less breath condensate than standard conditions (p<0.05). Changes in the breathing pattern had no effect on EBC protein and nitrite concentrations and pH. These results show that condensate volume can be increased by using high Vt and increased Vm without compromising the dilution of the sample.

Multiple functional ionic liquids based dispersive liquid-liquid microextraction combined with high performance chromatography for the determination of phenolic compounds in water samples.

PubMed

Sun, Jian-Nan; Chen, Juan; Shi, Yan-Ping

2014-07-01

A new mode of ionic liquid based dispersive liquid-liquid microextraction (IL-DLLME) is developed. In this work, [C6MIm][PF6] was chosen as the extraction solvent, and two kinds of hydrophilic ionic liquids, [EMIm][BF4] and [BSO3HMIm][OTf], functioned as the dispersive solvent. So in the whole extraction procedure, no organic solvent was used. With the aid of SO3H group, the acidic compound was extracted from the sample solution without pH adjustment. Two phenolic compounds, namely, 2-naphthol and 4-nitrophenol were chosen as the target analytes. Important parameters affecting the extraction efficiency, such as the type of hydrophilic ionic liquids, the volume ratio of [EMIm][BF4] to [BSO3HMIm][OTf], type and volume of extraction solvent, pH value of sample solution, sonication time, extraction time and centrifugation time were investigated and optimized. Under the optimized extraction conditions, the method exhibited good sensitivity with the limits of detection (LODs) at 5.5 μg L(-1)and 10.0 μg L(-1) for 4-nitrophenol and 2-naphthol, respectively. Good linearity over the concentration ranges of 24-384 μg L(-1) for 4-nitrophenol and 28-336 μg L(-1) for 2-naphthol was obtained with correlation coefficients of 0.9998 and 0.9961, respectively. The proposed method can directly extract acidic compound from environmental sample or even more complex sample matrix without any pH adjustment procedure. Copyright © 2014 Elsevier B.V. All rights reserved.

Solid-phase extraction of copper(II) in water and food samples using silica gel modified with bis(3-aminopropyl)amine and determination by flame atomic absorption spectrometry.

PubMed

Cagirdi, Duygu; Altundag, Hüseyin; Imamoglu, Mustafa; Tuzen, Mustafa

2014-01-01

A simple and selective separation and preconcentration method was developed for the determination of Cu(ll) ions. This method is based on adsorption of Cu(ll) ions from aqueous solution on a bis(3-aminopropyl)amine modified silica gel column and flame atomic absorption spectrometric determination after desorption. Various analytical parameters such as pH, type of eluent solution and its volume, flow rate of sample and eluent, and sample volume were optimized. Effects of some cation, anion, and transition metal ions on the recoveries of Cu(ll) ions were also investigated. Cu(ll) ions were quantitatively recovered at pH 6; 5.0 mL of 2 M HCI was used as the eluent. The preconcentration factor was found to be 150. The LOD was 0.12 microg/L for Cu(ll). The accuracy of the method was confirmed by analysis of Tea Leaves (INCT-TL-1) and Fish Protein (DORM-3) certified reference materials. The optimized method was applied to various water and food samples for the determination of Cu(ll).

External quality-assurance results for the National Atmospheric Deposition Program/National Trends Network, 1997-99

USGS Publications Warehouse

Gordon, John D.; Latysh, Natalie E.; Lindholm, Sandy J.

2003-01-01

Five external quality-assurance programs were operated by the U.S. Geological Survey for the National Atmospheric Deposition Program/ National Trends Network (NADP/NTN) during 1997 through 1999: the intersite-comparison program, the blind-audit program, the field- audit program, the interlaboratory-comparison program, and the collocated-sampler program. The intersite-comparison program assesses the accuracy of pH and specific-conductance determinations made by NADP/NTN site operators. In two 1997 intersite-comparison studies, 83.7 and 85.8 percent of the pH determinations met the NADP/NTN accuracy goals, whereas 97.3 and 92.4 percent of the specific-conductance determinations met the NADP/NTN accuracy goals. The percentage of pH and specific-conductance determinations that met the accuracy goals in 1998 were, for the most part, higher than in 1997. In two 1998 studies, 90.9 and 90.3 percent of the pH determinations met the accuracy goals compared to 94.7 and 96.0 percent of the specific- conductance measurements meeting the accuracy goals. In one 1999 intersite-comparison study, 89.5 percent and 99.4 percent of pH and specific- conductance determinations, respectively, met the NADP/NTN accuracy goals. The blind-audit program evaluates the effects of routine sample handling, processing, and shipping on the analytical bias and precision of weekly precipitation samples. A portion of the blind-audit sample subject to the normal onsite handling and processing of a weekly precipitation sample is referred to as the bucket portion, whereas the portion receiving only minimal handling is referred to as the bottle portion. Positive bias in regard to blind-audit results indicates that the bucket portion has a higher concentration than the bottle portion. The paired t-test for the 1997 through 1999 blind- audit data indicates that routine sample handling, processing, and shipping introduced a positive bias (a=0.05) for calcium and chloride and a negative bias (cz=0.05) for hydrogen ion. During 1997 through 1999, the median paired differences between the bucket and bottle portions ranged from 0.00 milligram per liter for nitrate and ammonium to +0.010 milligram per liter for both chloride and sulfate. The median paired difference between the bucket and bottle portions for hydrogen ion was -1.086 microequivalents per liter, whereas for specific conductance, the median paired difference between the bucket and bottle portions was -0.200 microsiemen per centimeter during 1997 through 1999. Surface-chemistry effects due to variable amounts of precipitation contacting prewashed sample-collection and shipping-container surfaces were studied in the blind-audit program by using three different sample volumes. The sample- collection and shipping containers used for the blind-audit study were obtained from the site operator's supply and could have been used for precipitation samples. Results of a Kruskal-Wallis analysis of variance test of the relation between paired blind-audit sample differences in units of concentration and sample volume were statistically significant for magnesium, chloride, sulfate, and hydrogen ion during 1997 through 1999. Before 1994, at least 5 of the 10 analytes displayed a statistically significant difference between paired blind-audit differences in units of concentration and sample volume, supporting the premise that chemical reactions between the 13-liter bucket shipping container (primarily the butadiene o-ring lid of the shipping container) and the sample, which resulted in an increasing loss of hydrogen ion with increasing volume, have been eliminated by the new l-liter bottle sample- shipping protocol. The field-audit program measures the effects of field exposure, handling, and processing on the chemistry of NADP/NTN precipitation samples. In the field-audit program, the site operator is instructed to process and submit a quality- control sample following a standard 7-day, Tuesday-to-Tuesday sampling period with no

Investigation of dioxin concentrations in the lower Roanoke River basin, North Carolina, February 26-March 7, 2001

USGS Publications Warehouse

Miller, K.F.; Walters, D.A.

2001-01-01

Dioxin is a toxic chemical that, when present in the environment, can cause cancer and birth defects in humans. Dioxin is of particular concern because concentrations of dioxin that were released into the environment many years ago remain a contributing factor to current exposure. Dioxin exposure often occurs in surface-water systems downstream from contaminated sites and is detrimental to aquatic life. For these reasons and because the U.S. Geological Survey has expertise in conducting high-volume dioxin sampling, the U.S. Environmental Protection Agency and the State of North Carolina asked the U.S. Geological Survey to collect water samples in the lower Roanoke River to be analyzed for the presence of dioxin. Water quality of the lower Roanoke River Basin in North Carolina was assessed at eight sites during February 26-March 7, 2001. Water- quality samples were collected for analysis of suspended-sediment and dioxin concentrations; high-volume (750-liter) water samples were collected for dioxin analysis. Discharge measurements were made at or near the high-volume sampling sites. Suspended-sediment sampling and water-quality measurements of specific conductance, pH, water temperature, and dissolved-oxygen concentrations made at each sampling site included multidepth measurements at two cross-section transects and hourly measurements at the point of high-volume sampling. Multidepth measurements were made near the surface, mid-depth, and near the bottom of the water column. These values were averaged for each cross section. During the sampling period, all sites sampled had dioxin concentrations above detection limits (1 part per quintillion) for both suspended and dissolved dioxin. Suspended dioxin ranged from 5.1 to 900 femtograms per liter, and dissolved dioxin values ranged from 0.31 to 41 femtograms per liter. Suspended-sediment concentrations ranged from 1.1 to 14 milligrams per liter. Specific conductance values ranges from 111 to 340 microsiemens per centimeter at 25 degrees Celsius. The range of pH values at the sampling sites was from 6.6 to 7.7. Water temperatures ranged from 8.9 to 13 degrees Celsius. Dissolved-oxygen concentrations ranged from 7.3 to 10.9 milligrams per liter.

Dispersive liquid-liquid microextraction of lead(II) as 5-(4-dimethylaminobenzylidene) rhodanine chelates from food and water samples.

PubMed

Alothman, Zeid A; Al-Shaalan, Nora H; Habila, Mohamed A; Unsal, Yunus E; Tuzen, Mustafa; Soylak, Mustafa

2015-02-01

A dispersive liquid-liquid microextraction procedure for lead(II) as its 5-(4-dimethylaminobenzylidene) rhodanine complex has been established prior to its microsampling flame atomic absorption spectrometric determination. The influences of various analytical parameters including pH, solvent type and volume, dispersive solvent type and volume, 5-(4-dimethylaminobenzylidene) rhodanine amount, salt effect, and centrifugation time and speed were investigated. The effects of certain alkali, alkaline earth, and transition metal ions on the quantitative extraction of lead(II) were also studied. Quantitative recoveries were obtained at pH 6. The enrichment factor was calculated as 125. The detection limit for lead is 1.1 μg/L. The accuracy of the method was tested with the additions recovery test and analysis of the standard reference materials (SPS-WW2 waste water, NIST SRM 1515 apple leaves, and TMDA-51.3 fortified water). Applications of the present procedure were tested by analyzing water and food samples.

Hormone-Dependence of Sarin Lethality in Rats: Sex Differences and Stage of the Estrous Cycle

DTIC Science & Technology

2015-06-12

that causes numerous physiological events including miosis, salivation , respiratory failure, tremors, seizures, and death. Treatment regimens that...into 96-well plates. The reactions were initiated by the addition of 290 μL of 50 mM sodium phosphate buffer ( pH 8.0) containing one of the following...buffer containing 50mMHEPES pH 7.4 in a total volume of 280 μL. Treat- ed samples were loaded into a 96-microtiter plate well, and the reaction was

Ionized calcium analyzer with a built-in pH correction.

PubMed

Fogh-Andersen, N

1981-07-01

We describe a new semi-automated apparatus for simultaneously measuring the concentration of free calcium ion and of hydrogen ion (pH) at 37 degrees C. The sample volume is 110 microL. In addition to the actual values for these concentrations in the sample, the apparatus calculates the concentration of free calcium ion at pH 7.40. Mean values for serum from 51 fasting bedridden patients without calcium metabolic disorders and 64 fasting hospital employees were 1.192 and 1.232 mmol/L, respectively, with SD of 0.042 and 0.040 mmol/L, respectively. The within-series analytical SD was 12 mumol/L and the day-to-day SD of the pH-corrected concentration of free calcium ion was 21 mumol/L, as calculated from measurements made on a serum pool after equilibration with a CO2--air mixture. The mean dependency on pH as determined in 120 consecutive patients' sera equalled the built-in pH correction. The accuracy was evaluated by comparison with other calcium ion-selective electrodes.

Molecular Wiring in Smart Dressings: Opening a New Route to Monitoring Wound pH

PubMed Central

McLister, Anna; Davis, James

2015-01-01

It has been proposed that fluctuations in wound pH can give valuable insights into the healing processes in chronic wounds, but acquiring such data can be a technological challenge especially where there is little sample available. Developments in voltammetric pH sensing have opened up new avenues for the design of probes that can function in ultra-small volumes and can be inherently disposable but, as yet few can meet the demands of wound monitoring. A preliminary investigation of the pH response of a new redox wire prepared from a peptide homopolymer of tryptophan is presented and its potential applicability as a sensing material for use in smart dressings is critically discussed. PMID:27417774

Nitrate and Nitrite Determination in Gunshot Residue Samples by Capillary Electrophoresis in Acidic Run Buffer.

PubMed

Erol, Özge Ö; Erdoğan, Behice Y; Onar, Atiye N

2017-03-01

Simultaneous determination of nitrate and nitrite in gunshot residue has been conducted by capillary electrophoresis using an acidic run buffer (pH 3.5). In previously developed capillary electrophoretic methods, alkaline pH separation buffers were used where nitrite and nitrate possess similar electrophoretic mobility. In this study, the electroosmotic flow has been reversed by using low pH running buffer without any additives. As a result of reversing the electroosmotic flow, very fast analysis has been actualized, well-defined and separated ion peaks emerge in less than 4 min. Besides, the limit of detection was improved by employing large volume sample stacking. Limit of detection values were 6.7 and 4.3 μM for nitrate and nitrite, respectively. In traditional procedure, mechanical agitation is employed for extraction, while in this work the extraction efficiency of ultrasound mixing for 30 min was found sufficient. The proposed method was successfully applied to authentic gunshot residue samples. © 2016 American Academy of Forensic Sciences.

Identification of Pulmonary Hypertension Caused by Left-Sided Heart Disease (World Health Organization Group 2) Based on Cardiac Chamber Volumes Derived From Chest CT Imaging.

PubMed

Aviram, Galit; Rozenbaum, Zach; Ziv-Baran, Tomer; Berliner, Shlomo; Topilsky, Yan; Fleischmann, Dominik; Sung, Yon K; Zamanian, Roham T; Guo, Haiwei Henry

2017-10-01

Evaluations of patients with pulmonary hypertension (PH) commonly include chest CT imaging. We hypothesized that cardiac chamber volumes calculated from the same CT scans can yield additional information to distinguish PH related to left-sided heart disease (World Health Organization group 2) from other PH subtypes. Patients who had PH confirmed by right heart catheterization and contrast-enhanced chest CT studies were enrolled in this retrospective multicenter study. Cardiac chamber volumes were calculated using automated segmentation software and compared between group 2 and non-group 2 patients with PH. This study included 114 patients with PH, 27 (24%) of whom were classified as group 2 based on their pulmonary capillary wedge pressure. Patients with group 2 PH exhibited significantly larger median left atrial (LA) volumes (118 mL vs 63 mL; P < .001), larger median left ventricular (LV) volumes (90 mL vs 76 mL; P = .02), and smaller median right ventricular (RV) volumes (173 mL vs 210 mL; P = .005) than did non-group 2 patients. On multivariate analysis adjusted for age, sex, and mean pulmonary arterial pressure, group 2 PH was significantly associated with larger median LA and LV volumes (P < .001 and P = .008, respectively) and decreased volume ratios of RA/LA, RV/LV, and RV/LA (P = .001, P = .004, and P < .001, respectively). Enlarged LA volumes demonstrated a high discriminatory ability for group 2 PH (area under the curve, 0.92; 95% CI, 0.870-0.968). Volumetric analysis of the cardiac chambers from nongated chest CT scans, particularly with findings of an enlarged left atrium, exhibited high discriminatory ability for identifying patients with PH due to left-sided heart disease. Copyright © 2017. Published by Elsevier Inc.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Slater, Paul B.

Paralleling our recent computationally intensive (quasi-Monte Carlo) work for the case N=4 (e-print quant-ph/0308037), we undertake the task for N=6 of computing to high numerical accuracy, the formulas of Sommers and Zyczkowski (e-print quant-ph/0304041) for the (N{sup 2}-1)-dimensional volume and (N{sup 2}-2)-dimensional hyperarea of the (separable and nonseparable) NxN density matrices, based on the Bures (minimal monotone) metric--and also their analogous formulas (e-print quant-ph/0302197) for the (nonmonotone) flat Hilbert-Schmidt metric. With the same seven 10{sup 9} well-distributed ('low-discrepancy') sample points, we estimate the unknown volumes and hyperareas based on five additional (monotone) metrics of interest, including the Kubo-Mori and Wigner-Yanase.more » Further, we estimate all of these seven volume and seven hyperarea (unknown) quantities when restricted to the separable density matrices. The ratios of separable volumes (hyperareas) to separable plus nonseparable volumes (hyperareas) yield estimates of the separability probabilities of generically rank-6 (rank-5) density matrices. The (rank-6) separability probabilities obtained based on the 35-dimensional volumes appear to be--independently of the metric (each of the seven inducing Haar measure) employed--twice as large as those (rank-5 ones) based on the 34-dimensional hyperareas. (An additional estimate--33.9982--of the ratio of the rank-6 Hilbert-Schmidt separability probability to the rank-4 one is quite clearly close to integral too.) The doubling relationship also appears to hold for the N=4 case for the Hilbert-Schmidt metric, but not the others. We fit simple exact formulas to our estimates of the Hilbert-Schmidt separable volumes and hyperareas in both the N=4 and N=6 cases.« less

Effects of breathing pattern and inspired air conditions on breath condensate volume, pH, nitrite, and protein concentrations

PubMed Central

McCafferty, J; Bradshaw, T; Tate, S; Greening, A; Innes, J

2004-01-01

Background: The effects of breathing pattern and inspired air conditions on the volume and content of exhaled breath condensate (EBC) were investigated. Methods: Total exhaled water (TEW), EBC volume, pH, nitrite and protein concentrations were measured in three groups of 10 healthy subjects breathing into a condenser at different target minute ventilations (Vm), tidal volumes (Vt), and inspired air conditions. Results: The volumes of both TEW and EBC increased significantly with Vm. For Vm 7.5, 15 and 22.5 l/min, mean (SD) EBC was 627 (258) µl, 1019 (313) µl, and 1358 (364) µl, respectively (p<0.001) and TEW was 1879 (378) µl, 2986 (496) µl, and 4679 (700) µl, respectively (p<0.001). TEW was significantly higher than EBC, reflecting a condenser efficiency of 40% at a target Vm of 7.5 l/min which reduced to 29% at Vm 22.5 l/min. Lower Vt gave less TEW than higher Vt (26.6 v 30.7 µl/l, mean difference 4.1 (95% CI 2.6 to 5.6), p<0.001) and a smaller EBC volume (4.3 v 7.6 µl/l, mean difference 3.4 (95% CI 2.3 to 4.5), p<0.001). Cooler and drier inspired air yielded less water vapour and less breath condensate than standard conditions (p<0.05). Changes in the breathing pattern had no effect on EBC protein and nitrite concentrations and pH. Conclusion: These results show that condensate volume can be increased by using high Vt and increased Vm without compromising the dilution of the sample. PMID:15282391

The structural, morphological and thermal properties of grafted pH-sensitive interpenetrating highly porous polymeric composites of sodium alginate/acrylic acid copolymers for controlled delivery of diclofenac potassium.

PubMed

Jalil, Aamir; Khan, Samiullah; Naeem, Fahad; Haider, Malik Suleman; Sarwar, Shoaib; Riaz, Amna; Ranjha, Nazar Muhammad

2017-01-01

In present investigation new formulations of Sodium Alginate/Acrylic acid hydrogels with high porous structure were synthesized by free radical polymerization technique for the controlled drug delivery of analgesic agent to colon. Many structural parameters like molecular weight between crosslinks ( M c ), crosslink density ( M r ), volume interaction parameter ( v 2, s ), Flory Huggins water interaction parameter and diffusion coefficient ( Q ) were calculated. Water uptake studies was conducted in different USP phosphate buffer solutions. All samples showed higher swelling ratio with increasing pH values because of ionization of carboxylic groups at higher pH values. Porosity and gel fraction of all the samples were calculated. New selected samples were loaded with the model drug (diclofenac potassium).The amount of drug loaded and released was determined and it was found that all the samples showed higher release of drug at higher pH values. Release of diclofenac potassium was found to be dependent on the ratio of sodium alginate/acrylic acid, EGDMA and pH of the medium. Experimental data was fitted to various model equations and corresponding parameters were calculated to study the release mechanism. The Structural, Morphological and Thermal Properties of interpenetrating hydrogels were studied by FTIR, XRD, DSC, and SEM.

pH profile of the adsorption of nucleotides onto montmorillonite. I - Selected homoionic clays

NASA Technical Reports Server (NTRS)

Lawless, J. G.; Church, F. M.; Mazzurco, J.; Banin, A.; Huff, R.; Kao, J.; Cook, A.; Lowe, T.; Orenberg, J. B.; Edelson, E.

1985-01-01

The effect of pH and adsorbed ions on the adsorption of purine and pyrimidine nucleotides on montmorillonite clay was studied experimentally. The specific nucleotides examined were: 5 prime-AMP; 3-prime AMP; and 5 prime-CMP. The pH of the clay samples was adjusted to various levels in the 2-12 pH range using microliter volumes of concentrated acid (1N HCl) and base (1NHNaOH). It was found that preferential adsorption among nulceotides was dependent on the pH level and on the characteristics of the substituted metal cation and anion exchange mechanisms. Below pH 4, adsorption was attributed to cation and anion exchange mechanisms. Above pH 4, however, adsorption was attributed to the complexation mechanisms occurring between the metal cations in the clay exchange site and in the biomolecule. The possible role of homoionic clays in the concentration mechanisms of biomonomers in the prebiotic environment is discussed.

Effects of preoperative medications on gastric pH, volume, and flora.

PubMed Central

Laws, H L; Bryant, J W; Palmer, M D; Boudreaux, A M; Donald, J M; Wheeler, A S

1986-01-01

Aspiration of acid gastric juice poses a potential threat during operations. Many anesthesiologists use a variety of agents aimed at decreasing gastric volume and/or acidity. The effect of three agents on gastric volume, pH, and flora, and the effect of cefazolin on gastric flora in morbidly obese patients were studied. Cefazolin did not sterilize the gastric lumen. Almost one-half of patients not treated with an H2 blocker had a pH below 2.5 and a gastric volume of 20 ml or more. Five had both a low pH and significant volume and, thus, the potential for lethal aspiration. Two doses of cimetidine, 300 mgm orally, or of ranitidine, 150 orally, the evening before and the morning of operation decreased gastric volume and raised pH reliably to a level that should be protective from fatal aspiration. However, gastric cultures after these drugs were positive 86% of the time with a larger variety of organisms than in the untreated stomachs. Metoclopramide failed to decrease gastric volume or raise pH. Transoperative cefazolin was used in all patients. Clinical infection was not a problem. PMID:3521506

A Pilot Chemical and Physical Stability Study of Extemporaneously Compounded Levetiracetam Intravenous Solution.

PubMed

Raphael, Chenzira D; Zhao, Fang; Hughes, Susan E; Juba, Katherine M

2015-01-01

Levetiracetam is a commonly used antiepileptic medication for tumor-related epilepsy. However, the 100 mL intravenous (IV) infusion volume can be burdensome to imminently dying hospice patients. A reduced infusion volume would improve patient tolerability. The purpose of this study was to evaluate the stability of 1000 mg/25 mL (40 mg/mL) levetiracetam IV solution in sodium chloride 0.9%. We prepared levetiracetam 40 mg/mL IV solution and added it to polyvinyl chloride (PVC) bags, polyolefin bags, and polypropylene syringes. Triplicate samples of each product were stored at refrigeration (2-8°C) and analyzed on days 0, 1, 4, 7, and 14. Samples were subjected to visual inspection, pH measurement, and stability-indicating high-performance liquid chromatography (HPLC) analysis. Over the 2-week storage period, there was no significant change in visual appearance or pH for any of the stability samples. The HPLC results confirmed that all stability samples retained 94.2-101.3% of initial drug concentration and no degradation products or leachable material from the packaging materials were observed. We conclude that levetiracetam 1000 mg/25 mL IV solution in sodium chloride 0.9% is physically and chemically stable for up to 14 days under refrigeration in polypropylene syringes, PVC bags, and polyolefin bags.

Ultrasound-Assisted Emulsification Microextraction Based on Solidification Floating Organic Drop Trace Amounts of Manganese Prior to Graphite Furnace Atomic Absorption Spectrometry Determination

PubMed Central

Mohadesi, Alireza; Falahnejad, Masoumeh

2012-01-01

In the present study, an ultrasound-assisted emulsification microextraction based on solidification floating organic drop method is described for preconcentration of trace amounts of Mn (II). 2-(5-Bromo-2-pyridylazo)-5 diethylaminophenol was added to a solution of Mn+2 at ph = 10.0. After this, 1-undecanol was added to the solution as an extraction solvent, and solution was stirred. Several factors influencing the microextraction efficiency, such as pH, the amount of chelating agent, nature and volume of extraction solvent, the volume of sample solution, stirring rate, and extraction time were investigated and optimized. Then sample vial was cooled by inserting into an ice bath, and the solidified was transferred into a suitable vial for immediate melting. Finally the sample was injected into a graphite furnace atomic absorption spectrometry. Under the optimum condition the linear dynamic range was 0.50–10.0 ng mL−1 with a correlation coefficient of 0.9926, and the detection limit of 0.3 ng mL−1 was obtained. The enrichment factor was 160. The proposed method was successfully applied for separation and determination of manganese in sea, rain, tap, and river water samples. PMID:22645504

Gradient-free determination of isoelectric points of proteins on chip.

PubMed

Łapińska, Urszula; Saar, Kadi L; Yates, Emma V; Herling, Therese W; Müller, Thomas; Challa, Pavan K; Dobson, Christopher M; Knowles, Tuomas P J

2017-08-30

The isoelectric point (pI) of a protein is a key characteristic that influences its overall electrostatic behaviour. The majority of conventional methods for the determination of the isoelectric point of a molecule rely on the use of spatial gradients in pH, although significant practical challenges are associated with such techniques, notably the difficulty in generating a stable and well controlled pH gradient. Here, we introduce a gradient-free approach, exploiting a microfluidic platform which allows us to perform rapid pH change on chip and probe the electrophoretic mobility of species in a controlled field. In particular, in this approach, the pH of the electrolyte solution is modulated in time rather than in space, as in the case for conventional determinations of the isoelectric point. To demonstrate the general approachability of this platform, we have measured the isoelectric points of representative set of seven proteins, bovine serum albumin, β-lactoglobulin, ribonuclease A, ovalbumin, human transferrin, ubiquitin and myoglobin in microlitre sample volumes. The ability to conduct measurements in free solution thus provides the basis for the rapid determination of isoelectric points of proteins under a wide variety of solution conditions and in small volumes.

Detection of Micrococcus luteus biofilm formation in microfluidic environments by pH measurement using an ion-sensitive field-effect transistor.

PubMed

Matsuura, Koji; Asano, Yuka; Yamada, Akira; Naruse, Keiji

2013-02-18

Biofilm formation in microfluidic channels is difficult to detect because sampling volumes are too small for conventional turbidity measurements. To detect biofilm formation, we used an ion-sensitive field-effect transistor (ISFET) measurement system to measure pH changes in small volumes of bacterial suspension. Cells of Micrococcus luteus (M. luteus) were cultured in polystyrene (PS) microtubes and polymethylmethacrylate (PMMA)-based microfluidic channels laminated with polyvinylidene chloride. In microtubes, concentrations of bacteria and pH in the suspension were analyzed by measuring turbidity and using an ISFET sensor, respectively. In microfluidic channels containing 20 μL of bacterial suspension, we measured pH changes using the ISFET sensor and monitored biofilm formation using a microscope. We detected acidification and alkalinization phases of M. luteus from the ISFET sensor signals in both microtubes and microfluidic channels. In the alkalinization phase, after 2 day culture, dense biofilm formation was observed at the bottom of the microfluidic channels. In this study, we used an ISFET sensor to detect biofilm formation in clinical and industrial microfluidic environments by detecting alkalinization of the culture medium. 

Salting-out assisted liquid-liquid extraction combined with gas chromatography-mass spectrometry for the determination of pyrethroid insecticides in high salinity and biological samples.

PubMed

Niu, Zongliang; Yu, Chunwei; He, Xiaowen; Zhang, Jun; Wen, Yingying

2017-09-05

A salting-out assisted liquid-liquid extraction (SALLE) combined with gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of four pyrethroid insecticides (PYRs) in high salinity and biological samples. Several parameters including sample pH, salting-out solution volume and salting-out solution pH influencing the extraction efficiency were systematically investigated with the aid of orthogonal design. The optimal extraction conditions of SALLE were: 4mL of salting-out solution with pH=4 and the sample pH=3. Under the optimum extraction and determination conditions, good responses for four PYRs were obtained in a range of 5-5000ng/mL, with linear coefficients greater than 0.998. The recoveries of the four PYRs ranged from 74% to 110%, with standard deviations ranging from 1.8% to 9.8%. The limits of detection based on a signal-to-noise ratio of 3 were between 1.5-60.6ng/mL. The method was applied to the determination of PYRs in urine, seawater and wastewater samples with a satisfactory result. The results demonstrated that this SALLE-GC-MS method was successfully applied to determine PYRs in high salinity and biological samples. SALLE avoided the need for the elimination of salinity and protein in the sample matrix, as well as clean-up of the extractant. Most of all, no centrifugation or any special apparatus are required, make this a promising method for rapid sample preparation procedure. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of the titratable acidity and the pH of wine based on potentiometric flow injection analysis.

PubMed

Vahl, Katja; Kahlert, Heike; von Mühlen, Lisandro; Albrecht, Anja; Meyer, Gabriele; Behnert, Jürgen

2013-07-15

A FIA system using a pH-sensitive detector based on a graphite/quinhydrone/silicone composite electrode was applied to determine sequentially the titratable acidity and the pH of wine, as well as the sum of calcium and magnesium ions. For all measurements the same FIA configuration was used employing different carrier solutions. The results for the determination of acidity and pH are in good agreement with those obtained by classical potentiometric titrations and by pH measurements using a conventional glass electrode. The standard deviation was less than 1.5% for both kinds of measurements and the sample volume was 150 μL. The method allows about 40 determinations of titratable acidity per hour and 30 pH measurements per hour. The titration method can be adjusted to the legal requirements in USA and Europe. Copyright © 2013 Elsevier B.V. All rights reserved.

How-to-Do-It: Why Don't Cells Grow Larger? A Lab Exercise.

ERIC Educational Resources Information Center

Stanek, Joseph A., Jr.

1983-01-01

Describes a laboratory investigation designed to analyze surface area to volume ratio related to cell division. Uses agar-gel "cells" with pH indicator added which are then "fed" acid for a measured time. Discusses procedures and materials used, providing a sample data table and important guiding questions. (JM)

The structural, morphological and thermal properties of grafted pH-sensitive interpenetrating highly porous polymeric composites of sodium alginate/acrylic acid copolymers for controlled delivery of diclofenac potassium

PubMed Central

Jalil, Aamir; Khan, Samiullah; Naeem, Fahad; Haider, Malik Suleman; Sarwar, Shoaib; Riaz, Amna; Ranjha, Nazar Muhammad

2017-01-01

Abstract In present investigation new formulations of Sodium Alginate/Acrylic acid hydrogels with high porous structure were synthesized by free radical polymerization technique for the controlled drug delivery of analgesic agent to colon. Many structural parameters like molecular weight between crosslinks (M c), crosslink density (M r), volume interaction parameter (v 2,s), Flory Huggins water interaction parameter and diffusion coefficient (Q) were calculated. Water uptake studies was conducted in different USP phosphate buffer solutions. All samples showed higher swelling ratio with increasing pH values because of ionization of carboxylic groups at higher pH values. Porosity and gel fraction of all the samples were calculated. New selected samples were loaded with the model drug (diclofenac potassium).The amount of drug loaded and released was determined and it was found that all the samples showed higher release of drug at higher pH values. Release of diclofenac potassium was found to be dependent on the ratio of sodium alginate/acrylic acid, EGDMA and pH of the medium. Experimental data was fitted to various model equations and corresponding parameters were calculated to study the release mechanism. The Structural, Morphological and Thermal Properties of interpenetrating hydrogels were studied by FTIR, XRD, DSC, and SEM. PMID:29491802

Structure, microstructure, and size dependent catalytic properties of nanostructured ruthenium dioxide

NASA Astrophysics Data System (ADS)

Nowakowski, Pawel; Dallas, Jean-Pierre; Villain, Sylvie; Kopia, Agnieszka; Gavarri, Jean-Raymond

2008-05-01

Nanostructured powders of ruthenium dioxide RuO 2 were synthesized via a sol gel route involving acidic solutions with pH varying between 0.4 and 4.5. The RuO 2 nanopowders were characterized by X-ray diffraction, scanning and transmission electron microscopy (SEM and TEM). Rietveld refinement of mean crystal structure was performed on RuO 2 nanopowders and crystallized standard RuO 2 sample. Crystallite sizes measured from X-ray diffraction profiles and TEM analysis varied in the range of 4-10 nm, with a minimum of crystallite dimension for pH=1.5. A good agreement between crystallite sizes calculated from Williamson Hall approach of X-ray data and from direct TEM observations was obtained. The tetragonal crystal cell parameter (a) and cell volumes of nanostructured samples were characterized by values greater than the values of standard RuO 2 sample. In addition, the [Ru-O 6] oxygen octahedrons of rutile structure also depended on crystal size. Catalytic conversion of methane by these RuO 2 nanostructured catalysts was studied as a function of pH, catalytic interaction time, air methane composition, and catalysis temperature, by the way of Fourier transform infrared (FTIR) spectroscopy coupled to homemade catalytic cell. The catalytic efficiency defined as FTIR absorption band intensities I(CO 2) was maximum for sample prepared at pH=1.5, and mainly correlated to crystallite dimensions. No significant catalytic effect was observed from sintered RuO 2 samples.

[Relationship between atmospheric particles and rain water chemistry character].

PubMed

Huo, Ming-Qun; Sun, Qian; Xie, Peng; Bai, Yu-Hua; Liu, Zhao-Rong; Li, Ji-Long; Lu, Si-Hua

2009-11-01

Rain and atmospheric particle samples were collected in the rural area of Taian and Shenzhen in 2007, respectively. Rain sampling was carried out during the precipitation process and several samples were got from the beginning of one precipitation to the end. The chemical character changes during precipitation and the changes of concentration of particles before and after rain were studied in this research to understand the contribution of particles on the rain chemical character and the rain-out effect for particles. The volume-weighted mean pH of rainwater in Taian was 5.97 and the total concentration of ions was 1 187.96 microeq x L(-1). The mass concentration of PM10 in Taian was 131.76 microg/m3 and that of PM2.5 was 103.84 microg/m3. The volume-weighted mean pH of rainwater in Shenzhen was 4.72 and the total concentration of ions was 175.89 microeq x L(-1). The mass concentration of PM10 in Shenzhen was 56.66 microg/m3 and that of PM2.5 was 41.52 microg/m3. During precipitation process pH and ion concentration of rain decrease and it is shown the neutralizing effect happens. The difference between rainwater of Taian and Shenzhen is due to cloud water acidity, atmospheric particles character and atmospheric acid-basic gases concentration. The clean-up effect of Na+ and Ca2+ by rain is high and which of NH4+ and NO3- is low. The clean-up effect for mass concentration, ions concentration and element concentration of particles by rain are significant.

Proceedings of the Antenna Applications Symposium (32nd) Held in Monticello, Illinois on 16-18 September 2008. Volume 1

DTIC Science & Technology

2008-12-20

Equation 6 for the sample likelihood function gives a “concentrated likelihood function,” which depends on correlation parameters θh and ph. This...step one and estimates correlation parameters using the new data set including all previous sample points and the new data point x. The algorithm...Unclassified b. ABSTRACT Unclassified c. THIS PAGE Unclassified UU 279 19b. TELEPHONE NUMBER (include area code ) N/A

An assessment of the variability in performance of wet atmospheric deposition samplers

USGS Publications Warehouse

Graham, R.C.; Robertson, J.K.; Obal, John

1987-01-01

The variability in performance of two brands of wet/dry atmospheric deposition samplers were compared for 1 year at a sincle site. A total of nine samplers were used. Samples were collected weekly and analyzed for pH, specific conductance, common chemical constituents, and sample volume. Additionally, data on the duration of each sampler opening were recorded using a microdatalogger. These data disprove the common perception that samplers remain open throughout a precipitation event. The sensitivity of sampler sensors within the range tested did not have a defineable impact on sample collection. The nonnormal distribution within the data set necessitated application of the nonparametric Friedman Test to assess comparability of sample chemical composition and volume between and within sampler brands. Statistically significant differences existed for most comparisons, however the test did not permit quantification of their magnitudes. Differences in analyte concentrations between samplers were small. (USGS)

Analysis of polycyclic aromatic hydrocarbons in water and beverages using membrane-assisted solvent extraction in combination with large volume injection-gas chromatography-mass spectrometric detection.

PubMed

Rodil, Rosario; Schellin, Manuela; Popp, Peter

2007-09-07

Membrane-assisted solvent extraction (MASE) in combination with large volume injection-gas chromatography-mass spectrometry (LVI-GC-MS) was applied for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in aqueous samples. The MASE conditions were optimized for achieving high enrichment of the analytes from aqueous samples, in terms of extraction conditions (shaking speed, extraction temperature and time), extraction solvent and composition (ionic strength, sample pH and presence of organic solvent). Parameters like linearity and reproducibility of the procedure were determined. The extraction efficiency was above 65% for all the analytes and the relative standard deviation (RSD) for five consecutive extractions ranged from 6 to 18%. At optimized conditions detection limits at the ng/L level were achieved. The effectiveness of the method was tested by analyzing real samples, such as river water, apple juice, red wine and milk.

Comparison of daily and weekly precipitation sampling efficiencies using automatic collectors

USGS Publications Warehouse

Schroder, L.J.; Linthurst, R.A.; Ellson, J.E.; Vozzo, S.F.

1985-01-01

Precipitation samples were collected for approximately 90 daily and 50 weekly sampling periods at Finley Farm, near Raleigh, North Carolina from August 1981 through October 1982. Ten wet-deposition samplers (AEROCHEM METRICS MODEL 301) were used; 4 samplers were operated for daily sampling, and 6 samplers were operated for weekly-sampling periods. This design was used to determine if: (1) collection efficiences of precipitation are affected by small distances between the Universal (Belfort) precipitation gage and collector; (2) measurable evaporation loss occurs and (3) pH and specific conductance of precipitation vary significantly within small distances. Average collection efficiencies were 97% for weekly sampling periods compared with the rain gage. Collection efficiencies were examined by seasons and precipitation volume. Neither factor significantly affected collection efficiency. No evaporation loss was found by comparing daily sampling to weekly sampling at the collection site, which was classified as a subtropical climate. Correlation coefficients for pH and specific conductance of daily samples and weekly samples ranged from 0.83 to 0.99.Precipitation samples were collected for approximately 90 daily and 50 weekly sampling periods at Finley farm, near Raleigh, North Carolina from August 1981 through October 1982. Ten wet-deposition samplers were used; 4 samplers were operated for daily sampling, and 6 samplers were operated for weekly-sampling periods. This design was used to determine if: (1) collection efficiencies of precipitation are affected by small distances between the University (Belfort) precipitation gage and collector; (2) measurable evaporation loss occurs and (3) pH and specific conductance of precipitation vary significantly within small distances.

Extraction of Carbon Dioxide from Seawater by an Electrochemical Acidification Cell. Part 1 - Initial Feasibility Studies

DTIC Science & Technology

2010-07-23

approximately 142 ppm (0.0023 M), therefore approximately 23 mL of 0.100 M hydrochloric acid (HCl) acid is required per liter of seawater where Cl- is...deionized water to a total volume of 140 liters, and pH adjusted to 7.6 using hydrochloric acid (HCl); approximately 20 mLs of diluted HCl (5 mL of... hydrochloric acid was required to reduce pH in a 20 mL sample of Key West seawater to 6.0. This required 4.05E-05 moles of hydrogen ions. Based on

Effect of proton pump inhibitors on gastric juice volume, gastric pH and gastric intramucosal pH in critically ill patients : a randomized, double-blind, placebo-controlled study.

PubMed

Gursoy, Olcay; Memiş, Dilek; Sut, Necdet

2008-01-01

This study aimed to determine the effect of administration of a single-dose proton pump inhibitor (PPI) on gastric intramucosal pH (pHi), gastric juice volume and gastric pH in critically ill patients. This prospective, randomized, double-blind, placebo-controlled study included 75 patients who were divided into five groups that received the following treatment: group C (n = 15), saline 100 mL; group O (n = 15), omeprazole 20 mg; group P (n = 15), pantoprazole 40 mg; group E (n = 15), esomeprazole 20 mg; and group R (n = 15), rabeprazole 20 mg. All treatments were administered nasogastrically in 100 mL of physiological saline. Measurements of gastric pHi, gastric juice volume and gastric pH were obtained immediately before and 2, 4 and 6 hours after administration of treatments. In addition, gastric content was aspirated and its volume was recorded. Initial gastric pHi, gastric juice volume and gastric pH values were not statistically significantly different among the groups (p > 0.05). No statistically significant difference in gastric pHi was seen among the groups before or 2, 4 or 6 hours after saline or PPI administration. At hours 2, 4 and 6, gastric pH in the pantoprazole, esomeprazole and rabeprazole groups increased significantly, whereas gastric juice volume decreased significantly, compared with the omeprazole and placebo groups (p < 0.001). No statistically significant differences were seen between the pantoprazole, esomeprazole and rabeprazole groups. This is the first study to show that single-dose pantoprazole, esomeprazole and rabeprazole are associated with greater gastric pH increase and greater gastric juice volume decrease than omeprazole in critically ill patients. Our study also suggests that PPIs do not affect gastric pHi measurements in critically ill patients and can be administered during pH monitoring.

Effect of natural ageing on volume stability of MSW and wood waste incineration residues

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gori, Manuela, E-mail: manuela.gori@dicea.unifi.it; Bergfeldt, Britta; Reichelt, Jürgen

2013-04-15

Highlights: ► Natural weathering on BA from MSW and wood waste incineration was evaluated. ► Type of mineral phases, pH and volume stability were considered. ► Weathering reactions effect in improved stability of the materials. - Abstract: This paper presents the results of a study on the effect of natural weathering on volume stability of bottom ash (BA) from municipal solid waste (MSW) and wood waste incineration. BA samples were taken at different steps of treatment (fresh, 4 weeks and 12 weeks aged) and then characterised for their chemical and mineralogical composition and for volume stability by means of themore » mineralogical test method (M HMVA-StB), which is part of the German quality control system for using aggregates in road construction (TL Gestein-StB 04). Changes of mineralogical composition with the proceeding of the weathering treatment were also monitored by leaching tests. At the end of the 12 weeks of treatment, almost all the considered samples resulted to be usable without restrictions in road construction with reference to the test parameter volume stability.« less

Confocal Raman Microscopy for pH-Gradient Preconcentration and Quantitative Analyte Detection in Optically Trapped Phospholipid Vesicles.

PubMed

Hardcastle, Chris D; Harris, Joel M

2015-08-04

The ability of a vesicle membrane to preserve a pH gradient, while allowing for diffusion of neutral molecules across the phospholipid bilayer, can provide the isolation and preconcentration of ionizable compounds within the vesicle interior. In this work, confocal Raman microscopy is used to observe (in situ) the pH-gradient preconcentration of compounds into individual optically trapped vesicles that provide sub-femtoliter collectors for small-volume samples. The concentration of analyte accumulated in the vesicle interior is determined relative to a perchlorate-ion internal standard, preloaded into the vesicle along with a high-concentration buffer. As a guide to the experiments, a model for the transfer of analyte into the vesicle based on acid-base equilibria is developed to predict the concentration enrichment as a function of source-phase pH and analyte concentration. To test the concept, the accumulation of benzyldimethylamine (BDMA) was measured within individual 1 μm phospholipid vesicles having a stable initial pH that is 7 units lower than the source phase. For low analyte concentrations in the source phase (100 nM), a concentration enrichment into the vesicle interior of (5.2 ± 0.4) × 10(5) was observed, in agreement with the model predictions. Detection of BDMA from a 25 nM source-phase sample was demonstrated, a noteworthy result for an unenhanced Raman scattering measurement. The developed model accurately predicts the falloff of enrichment (and measurement sensitivity) at higher analyte concentrations, where the transfer of greater amounts of BDMA into the vesicle titrates the internal buffer and decreases the pH gradient. The predictable calibration response over 4 orders of magnitude in source-phase concentration makes it suitable for quantitative analysis of ionizable compounds from small-volume samples. The kinetics of analyte accumulation are relatively fast (∼15 min) and are consistent with the rate of transfer of a polar aromatic molecule across a gel-phase phospholipid membrane.

Applications of organo-silica nanocomposites for SPNE of Hg(II)

NASA Astrophysics Data System (ADS)

Kaur, Anupreet

2016-02-01

An analytical method using modified SiO2 nanoparticles as solid-phase extractant has been developed for the preconcentration of trace amounts of Hg(II) in different water samples. Conditions of the analysis such as preconcentration factor, effect of pH, sample volume, shaking time, elution conditions and effects of interfering ions for the recovery of analyte were investigated. The adsorption capacity of nanometer SiO2-APTMS was found to be 181.42 µmol g-1 at optimum pH and the detection limit (3σ) was 0.45 µg L-1. The extractant showed rapid kinetic sorption. The adsorption equilibrium of Hg(II) on nanometer SiO2-APTMS was achieved just in 15 min. Adsorbed Hg(II) was easily eluted with 4 mL of 2.0 M hydrochloric acid. The maximum preconcentration factor was 75. The method was applied for the determination of trace amounts of Hg(II) in various synthetic samples and water samples.

Isolation of organic acids from large volumes of water by adsorption on macroporous resins

USGS Publications Warehouse

Aiken, George R.; Suffet, I.H.; Malaiyandi, Murugan

1987-01-01

Adsorption on synthetic macroporous resins, such as the Amberlite XAD series and Duolite A-7, is routinely used to isolate and concentrate organic acids from forge volumes of water. Samples as large as 24,500 L have been processed on site by using these resins. Two established extraction schemes using XAD-8 and Duolite A-7 resins are described. The choice of the appropriate resin and extraction scheme is dependent on the organic solutes of interest. The factors that affect resin performance, selectivity, and capacity for a particular solute are solution pH, resin surface area and pore size, and resin composition. The logistical problems of sample handling, filtration, and preservation are also discussed.

Comparison between dispersive solid-phase and dispersive liquid-liquid microextraction combined with spectrophotometric determination of malachite green in water samples based on ultrasound-assisted and preconcentration under multi-variable experimental design optimization.

PubMed

Alipanahpour Dil, Ebrahim; Ghaedi, Mehrorang; Asfaram, Arash; Zare, Fahimeh; Mehrabi, Fatemeh; Sadeghfar, Fardin

2017-11-01

The ultrasound-assisted dispersive solid-phase microextraction (USA-DSPME) and the ultrasound-assisted dispersive liquid-liquid microextraction (USA-DLLME) developed for as an ultra preconcentration and/or technique for the determination of malachite green (MG) in water samples. Central composite design based on analysis of variance and desirability function guide finding best operational conditions and represent dependency of response to variables viz. volume of extraction, eluent and disperser solvent, pH, adsorbent mass and ultrasonication time has significant influence on methods efficiency. Optimum conditions was set for USA-DSPME as: 1mg CNTs/Zn:ZnO@Ni 2 P-NCs; 4min sonication time and 130μL eluent at pH 6.0. Meanwhile optimum point for USA-DLLME conditions were fixed at pH 6.0; 4min sonication time and 130, 650μL and 10mL of extraction solvent (CHCl 3 ), disperser solvent (ethanol) and sample volume, respectively. Under the above specified best operational conditions, the enrichment factors for the USA-DSPME and USA-DLLME were 88.89 and 147.30, respectively. The methods has linear response in the range of 20.0 to 4000.0ngmL -1 with the correlation coefficients (r) between 0.9980 to 0.9995, while its reasonable detection limits viz. 1.386 to 2.348ngmL -1 and good relative standard deviations varied from 1.1% to 2.8% (n=10) candidate this method for successful monitoring of analyte from various media. The relative recoveries of the MG dye from water samples at spiking level of 500ngmL -1 were in the range between 94.50% and 98.86%. The proposed methods has been successfully applied to the analysis of the MG dye in water samples, and a satisfactory result was obtained. Copyright © 2017. Published by Elsevier B.V.

Average rainwater pH, concepts of atmospheric acidity, and buffering in open systems

NASA Astrophysics Data System (ADS)

Liljestrand, Howard M.

The system of water equilibrated with a constant partial pressure of CO 2, as a reference point for pH acidity-alkalinity relationships, has nonvolatile acidity and alkalinity components as conservative quantities, but not [H +]. Simple algorithms are presented for the determination of the average pH for combinations of samples both above and below pH 5.6. Averaging the nonconservative quantity [H +] yields erroneously low mean pH values. To extend the open CO 2 system to include other volatile atmospheric acids and bases distributed among the gas, liquid and particulate matter phases, a theoretical framework for atmospheric acidity is presented. Within certain oxidation-reduction limitations, the total atmospheric acidity (but not free acidity) is a conservative quantity. The concept of atmospheric acidity is applied to air-water systems approximating aerosols, fogwater, cloudwater and rainwater. The buffer intensity in hydrometeors is described as a function of net strong acidity, partial pressures of acid and base gases and the water to air ratio. For high liquid to air volume ratios, the equilibrium partial pressures of trace acid and base gases are set by the pH or net acidity controlled by the nonvolatile acid and base concentrations. For low water to air volume ratios as well as stationary state systems such as precipitation scavenging with continuous emissions, the partial pressures of trace gases (NH 3, HCl, HNO 3, SO 2 and CH 3COOH) appear to be of greater or equal importance as carbonate species as buffers in the aqueous phase.

Environmental Limits of Tall Shrubs in Alaska’s Arctic National Parks

PubMed Central

Swanson, David K.

2015-01-01

We sampled shrub canopy volume (height times area) and environmental factors (soil wetness, soil depth of thaw, soil pH, mean July air temperature, and typical date of spring snow loss) on 471 plots across five National Park Service units in northern Alaska. Our goal was to determine the environments where tall shrubs thrive and use this information to predict the location of future shrub expansion. The study area covers over 80,000 km2 and has mostly tundra vegetation. Large canopy volumes were uncommon, with volumes over 0.5 m3/m2 present on just 8% of plots. Shrub canopy volumes were highest where mean July temperatures were above 10.5°C and on weakly acid to neutral soils (pH of 6 to 7) with deep summer thaw (>80 cm) and good drainage. On many sites, flooding helped maintain favorable soil conditions for shrub growth. Canopy volumes were highest where the typical snow loss date was near 20 May; these represent sites that are neither strongly wind-scoured in the winter nor late to melt from deep snowdrifts. Individual species varied widely in the canopy volumes they attained and their response to the environmental factors. Betula sp. shrubs were the most common and quite tolerant of soil acidity, cold July temperatures, and shallow thaw depths, but they did not form high-volume canopies under these conditions. Alnus viridis formed the largest canopies and was tolerant of soil acidity down to about pH 5, but required more summer warmth (over 12°C) than the other species. The Salix species varied widely from S. pulchra, tolerant of wet and moderately acid soils, to S. alaxensis, requiring well-drained soils with near neutral pH. Nearly half of the land area in ARCN has mean July temperatures of 10.5 to 12.5°C, where 2°C of warming would bring temperatures into the range needed for all of the potential tall shrub species to form large canopies. However, limitations in the other environmental factors would probably prevent the formation of large shrub canopies on at least half of the land area with newly favorable temperatures after 2°C of warming. PMID:26379243

Environmental Limits of Tall Shrubs in Alaska's Arctic National Parks.

PubMed

Swanson, David K

2015-01-01

We sampled shrub canopy volume (height times area) and environmental factors (soil wetness, soil depth of thaw, soil pH, mean July air temperature, and typical date of spring snow loss) on 471 plots across five National Park Service units in northern Alaska. Our goal was to determine the environments where tall shrubs thrive and use this information to predict the location of future shrub expansion. The study area covers over 80,000 km2 and has mostly tundra vegetation. Large canopy volumes were uncommon, with volumes over 0.5 m3/m2 present on just 8% of plots. Shrub canopy volumes were highest where mean July temperatures were above 10.5°C and on weakly acid to neutral soils (pH of 6 to 7) with deep summer thaw (>80 cm) and good drainage. On many sites, flooding helped maintain favorable soil conditions for shrub growth. Canopy volumes were highest where the typical snow loss date was near 20 May; these represent sites that are neither strongly wind-scoured in the winter nor late to melt from deep snowdrifts. Individual species varied widely in the canopy volumes they attained and their response to the environmental factors. Betula sp. shrubs were the most common and quite tolerant of soil acidity, cold July temperatures, and shallow thaw depths, but they did not form high-volume canopies under these conditions. Alnus viridis formed the largest canopies and was tolerant of soil acidity down to about pH 5, but required more summer warmth (over 12°C) than the other species. The Salix species varied widely from S. pulchra, tolerant of wet and moderately acid soils, to S. alaxensis, requiring well-drained soils with near neutral pH. Nearly half of the land area in ARCN has mean July temperatures of 10.5 to 12.5°C, where 2°C of warming would bring temperatures into the range needed for all of the potential tall shrub species to form large canopies. However, limitations in the other environmental factors would probably prevent the formation of large shrub canopies on at least half of the land area with newly favorable temperatures after 2°C of warming.

The role of perioperative chewing gum on gastric fluid volume and gastric pH: a meta-analysis.

PubMed

Ouanes, Jean-Pierre P; Bicket, Mark C; Togioka, Brandon; Tomas, Vicente Garcia; Wu, Christopher L; Murphy, Jamie D

2015-03-01

To determine if preoperative gum chewing affects gastric pH and gastric fluid volume. Systematic review and meta-analysis. Data sources included Cochrane, PubMed, and EMBASE databases from inception to June 2012 and reference lists of known relevant articles without language restriction. Randomized controlled trials in which a treatment group that chewed gum was compared to a control group that fasted were included. Relevant data, including main outcomes of gastric fluid volume and gastric pH, were extracted. Four studies involving 287 patients were included. The presence of chewing gum was associated with small but statically significant increases in gastric fluid volume (mean difference = 0.21 mL/kg; 95% confidence interval, 0.02-0.39; P = .03) but not in gastric pH (mean difference = 0.11 mL/kg; 95% confidence interval, -0.14 to 0.36; P = .38). Gastric fluid volume and gastric pH remained unchanged in subgroup analysis by either sugar or sugarless gum type. Chewing gum in the perioperative period causes small but statically significant increases in gastric fluid volume and no change in gastric pH. The increase in gastric fluid most likely is of no clinical significance in terms of aspiration risk for the patient. Elective surgery should not necessarily be canceled or delayed in healthy patients who accidentally chew gum preoperatively. Copyright © 2014 Elsevier Inc. All rights reserved.

The effect of intravenous lactated Ringer's solution versus 0.9% sodium chloride solution on serum osmolality in human volunteers.

PubMed

Williams, E L; Hildebrand, K L; McCormick, S A; Bedel, M J

1999-05-01

Animal studies have shown that large volumes of IV lactated Ringer's solution (LR) decrease serum osmolality, thereby increasing cerebral water. These studies have led to recommendations to limit LR to avoid cerebral edema in neurosurgical patients. Eighteen healthy human volunteers aged 20-48 yr received 50 mL/kg LR over 1 h on one occasion and 0.9% sodium chloride (NS) on another. Venous samples were taken at baseline (T1), at infusion end (T2), and 1 h after T2 (T3). Time until first urination was noted. With LR, serum osmolality decreased by 4+/-3 mOsm/kg from T1 to T2 and increased insignificantly with NS. At T3, osmolality returned almost to baseline in the LR group. Blood pH increased from T1 to T2 with LR by 0.04+/-0.04 and decreased with NS by 0.04+/-0.04. These pH changes persisted at T3. Subjective mental changes occurred only with NS. Abdominal discomfort was more common with NS. Time until first urination was longer with NS (106+/-11 min) than with LR (75+/-10 min) (P < 0.001). In healthy humans, an infusion of large volumes of LR, but not NS, transiently decreased serum osmolality, whereas acidosis associated with NS persisted and urinary output was slower with NS. Large volumes of lactated Ringer's solution administered to healthy humans produced small transient changes in serum osmolality. Large volumes of sodium chloride did not change osmolality but resulted in lower pH.

Gold nanoparticle incorporated inverse opal photonic crystal capillaries for optofluidic surface enhanced Raman spectroscopy.

PubMed

Zhao, Xiangwei; Xue, Jiangyang; Mu, Zhongde; Huang, Yin; Lu, Meng; Gu, Zhongze

2015-10-15

Novel transducers are needed for point of care testing (POCT) devices which aim at facile, sensitive and quick acquisition of health related information. Recent advances in optofluidics offer tremendous opportunities for biological/chemical analysis using extremely small sample volumes. This paper demonstrates nanostructured capillary tubes for surface enhanced Raman spectroscopy (SERS) analysis in a flow-through fashion. The capillary tube integrates the SERS sensor and the nanofluidic structure to synergistically offer sample delivery and analysis functions. Inside the capillary tube, inverse opal photonic crystal (IO PhC) was fabricated using the co-assembly approach to form nanoscale liquid pathways. In the nano-voids of the IO PhC, gold nanoparticles were in situ synthesized and functioned as the SERS hotspots. The advantages of the flow-through SERS sensor are multifold. The capillary effect facilities the sample delivery process, the nanofluidic channels boosts the interaction of analyte and gold nanoparticles, and the PhC structure strengthens the optical field near the SERS hotspots and results in enhanced SERS signals from analytes. As an exemplary demonstration, the sensor was used to measure creatinein spiked in artificial urine samples with detection limit of 0.9 mg/dL. Copyright © 2015 Elsevier B.V. All rights reserved.

Chemical composition of precipitation in a Mexican Maya region

NASA Astrophysics Data System (ADS)

Bravo, H. A.; Saavedra, M. I. R.; Sánchez, P. A.; Torres, R. J.; Granada, L. M. M.

The chemical characteristics of wet precipitation in Puerto Morelos, Quintana Roo State, Mexico, were measured from April 1994 to December 1995. Puerto Morelos is located in the Caribbean Mayan coastal region of the Peninsula of Yucatan, and is normally exposed to winds from the Caribbean region. Wetfall was analyzed for pH, conductivity and Cl -, NO 3-, SO 42-, Na +, NH 4+, K +, Mg 2+ and Ca 2+ ion concentrations. Volume-weighted mean pH for the whole sampling period was 5.35, although values as low as 4.6 were measured in several rain samples. Concentrations of all species correlated negatively with rain volume. Sea-salt aerosols contributed with most of the Na +, Cl -, Mg 2+, K + and SO 42- found in wet precipitation. The mean [SO 42-excess] was 9.7 μEq l -1, which agrees with the background hemispheric values of ≈10 μEq l -1 reported elsewhere. The mean [NO 3-] was 11.4 μEq l -1, almost four times higher than the background hemispheric value of ≈2.5 μEq l -1 reported elsewhere. However, a major component causing the slight acidity character of rain in Puerto Morelos seems to be H 2SO 4.

Preparative Purification of Polyphenols from Aronia melanocarpa (Chokeberry) with Cellular Antioxidant and Antiproliferative Activity.

PubMed

Gao, Ningxuan; Wang, Yuehua; Jiao, Xinyao; Chou, Shurui; Li, Enhui; Li, Bin

2018-01-10

The aim of this study was the purification process of polyphenols from Aronia melanocarpa (chokeberry), and the purification parameters were optimised by adsorption and desorption tests. By comparing adsorption and desorption ability of polyphenols from chokeberry on six kinds of macroporous resin, XAD-7 resin was selected. Experiments prove that the best purification parameters of static adsorption and desorption were sample pH = 4.0 with 4 h of adsorption; and desorption solvent is 95% ethanol (pH = 7.0) with 2 h of desorption. The best dynamic parameters were 9.3 bed volume (BV) of sample loading amount at a feeding flow rate of 2 BV/h, and washing the column with 5.8 BV of water, followed by subsequent elution with an eluent volume of 5.0 mL at an elution flow rate of 2 BV/h. Next the antioxidant and antiproliferative activity of polyphenols from chokeberry, blueberries, haskap berries was studied on HepG2 human liver cancer cells. The results show that polyphenol from chokeberry has a strong antioxidant effect. Taking into account the content of polyphenols in fruit, polyphenols from chokeberry represent a very valuable natural antioxidant source with antiproliferative products.

Does adjuvant radiotherapy suppress liver regeneration after partial hepatectomy?

PubMed

Choi, Jin-Hwa; Kim, Kyubo; Chie, Eui Kyu; Jang, Jin-Young; Kim, Sun Whe; Oh, Do-Youn; Im, Seock-Ah; Kim, Tae-You; Bang, Yung-Jue; Ha, Sung W

2009-05-01

To analyze the influence of the adjuvant radiotherapy (RT) on the liver regeneration and liver function after partial hepatectomy (PH). Thirty-four patients who underwent PH for biliary tract cancer between October 2003 and July 2005 were reviewed. Hemihepatectomy was performed in 14 patients and less extensive surgery in 20. Of the patients, 19 patients had no adjuvant therapy (non-RT group) and 15 underwent adjuvant RT by a three-dimensional conformal technique (RT group). Radiation dose range was 40 to 50 Gy (median, 40 Gy). Liver volume on computed tomography and the results of liver function tests at 1, 4, 12, 24, and 52 weeks after PH were compared between the RT and non-RT groups. The preoperative characteristics were identical for both groups. During the interval between Weeks 4 and 12 when adjuvant RT was delivered in the RT group, the increase in liver volume was significantly smaller in the RT group than non-RT group (22.9 +/- 38.3cm(3) and 81.5 +/- 75.6cm(3), respectively, p = 0.007). However, the final liver volume measured at 1 year after PH did not differ between the two groups (p = 0.878). Liver function tests were comparable for both groups. The resection extent and original liver volume was independent factors for final liver volume measured at 1 year after PH. In this study, adjuvant RT delayed the liver regeneration process after PH, but the volume difference between the two study groups became nonsignificant after 1 year. Adjuvant RT had no additional adverse effect on liver function after PH.

The effects of microfluidization on rheological and textural properties of gluten-free corn breads.

PubMed

Ozturk, Oguz Kaan; Mert, Behic

2018-03-01

This study presents the potential of microfluidization as a value adding process to corn gluten meal (CGM), which is often used as animal feed and is underutilized in food industry. In this study, we aimed to improve water holding ability of corn gluten and to investigate possibility of using this zein-rich byproduct as the main ingredient in gluten-free bread formulations. For this reason, microfluidization as a milling process for CGM, and its effects on rheological and textural properties of gluten-free bread formulations were investigated. In addition, the effects of pH modification and hydrocolloids were analyzed. Microfluidization led to a higher surface area by disintegrating the large CGM molecules, and the structure became compatible to be used in gluten-free bread formulations by overcoming hydrophobic nature. However, structural deformations were detected with pH modifications. The linear viscoelastic region of dough was observed at strains lower than 0.5%. For all formulations, elastic moduli (G') were higher than viscous moduli (G") indicating solid-like behavior. The addition of HPMC and guar resulted in higher moduli values. Microfluidization and pH modifications provided brighter color by revealing lutein and zeaxanthin due to decreased particle size. Texture profile showed that microfluidization and hydrocolloids decreased hardness, increased springiness and cohesiveness, which are desired characteristics for bread. Lastly, the addition of hydrocolloids led to an increase in specific volume by providing gas retention within the structure. HPMC provided 1.23-1.62 times bigger samples than control samples while it was only 1.02-1.12 times bigger for samples with guar according to specific volume analysis. Copyright © 2017 Elsevier Ltd. All rights reserved.

Semiautomated solid-phase extraction followed by derivatisation and gas chromatography–mass spectrometry for determination of perfluoroalkyl acids in water.

PubMed

Jurado-Sánchez, Beatriz; Ballesteros, Evaristo; Gallego, Mercedes

2013-11-29

This paper describes a sensitive approach for the determination of 6 perfluoroalkyl carboxylic acids and perfluorooctane sulfonic acid in water. Samples were preconcentrated using an automatic solid-phase extraction module and then manually derivatised and determined by gas chromatography–mass spectrometry. The analytes were derivatised with a isobutyl chloroformate/isobutanol mixture, using 3% N,N-dicyclohexylcarbodiimide in pyridine as the catalyst. From a systematic comparison of several reversed-phase and anion-exchange sorbent materials for the retention of perfluoroalkyl acids, the high-est retention efficiencies (∼100%) were achieved with LiChrolut EN and Discovery DSC-SAX columns.LiChrolut EN was the sorbent selected due to several advantages (sample pH ∼1; sample flow rate,5.5 mL/min; breakthrough volume, 300 mL) over Discovery DSC-SAX (sample pH ∼6; sample flow rate,3.0 mL/min; breakthrough volume, 45 mL), for the retention of the studied compounds. Detection and quantification limits within the range of 0.1–0.5 ng/L and 0.4–1.7 ng/L, respectively, were obtained for a sorbent column of 70 mg of LiChrolut EN and 250 mL of sample, the relative standard deviation being lower than 7%. The method was applied both to the analysis of water collected at the intake (raw) and atthe exit (treated) of two drinking water treatment plants, as well as to various types of water. Few samples were positive for perfluoroalkyl acids and only one acid (perfluoroheptanoic or perfluorooctanoic) was found in each treatment plant. The highest number and concentration of analytes (perfluoroheptanoic,perfluorooctanoic and perfluorodecanoic acid) were found in one wastewater.

Dispersive liquid-liquid microextraction based on solidification of floating organic drop for preconcentration and determination of trace amounts of copper by flame atomic absorption spectrometry.

PubMed

Karadaş, Cennet; Kara, Derya

2017-04-01

A novel, simple, rapid, sensitive, inexpensive and environmentally friendly dispersive liquid-liquid microextraction method based on the solidification of a floating organic drop (DLLME-SFO) was developed for the determination of copper by flame atomic absorption spectrometry (FAAS). N-o-Vanillidine-2-amino-p-cresol was used as a chelating ligand and 1-undecanol was selected as an extraction solvent. The main parameters affecting the performance of DLLME-SFO, such as sample pH, volume of extraction solvent, extraction time, concentration of the chelating ligand, salt effect, centrifugation time and sample volume were investigated and optimized. The effect of interfering ions on the recovery of copper was also examined. Under the optimum conditions, the detection limit (3σ) was 0.93μgL -1 for Cu using a sample volume of 20mL, yielding a preconcentration factor of 20. The proposed method was successfully applied to the determination of Cu in tap, river and seawater, rice flour and black tea samples as well as certified reference materials. Copyright © 2016. Published by Elsevier Ltd.

Application of ultrasound-assisted emulsification microextraction for simultaneous determination of aminophenol isomers in human urine, hair dye, and water samples using high-performance liquid chromatography.

PubMed

Asghari, Alireza; Fazl-Karimi, Hamidreza; Barfi, Behruz; Rajabi, Maryam; Daneshfar, Ali

2014-08-01

Aminophenol isomers (2-, 3-, and 4-aminophenols) are typically classified as industrial pollutants with genotoxic and mutagenic effects due to their easy penetration through the skin and membranes of human, animals, and plants. In the present study, a simple and efficient ultrasound-assisted emulsification microextraction procedure coupled with high-performance liquid chromatography with ultraviolet detector was developed for preconcentration and determination of these compounds in human fluid and environmental water samples. Effective parameters (such as type and volume of extraction solvent, pH and ionic strength of sample, and ultrasonication and centrifuging time) were investigated and optimized. Under optimum conditions (including sample volume: 5 mL; extraction solvent: chloroform, 80 µL; pH: 6.5; without salt addition; ultrasonication: 3.5 min; and centrifuging time: 3 min, 5000 rpm min(-1)), the enrichment factors and limits of detection were ranged from 42 to 51 and 0.028 to 0.112 µg mL(-1), respectively. Once optimized, analytical performance of the method was studied in terms of linearity (0.085-157 µg mL(-1), r (2) > 0.998), accuracy (recovery = 88.6- 101.7%), and precision (repeatability: intraday precision < 3.98%, and interday precision < 5.12%). Finally, applicability of the method was evaluated by the extraction and determination of these compounds in human urine, hair dye, and real water samples. © The Author(s) 2014.

Microbial population in cloud water at the Puy de Dôme: Implications for the chemistry of clouds

NASA Astrophysics Data System (ADS)

Amato, Pierre; Ménager, Matthieu; Sancelme, Martine; Laj, Paolo; Mailhot, Gilles; Delort, Anne-Marie

Airborne micro-organisms are ubiquitous in the atmosphere where they can remain alive and be transported over long distances, thus colonizing new environments. Despite their great importance in relation to ecological and socio-economical issues (bio-terrorism, health, etc.) very few studies have been carried out in this field. In this study, the structure of the microbial community present in atmospheric water samples from clouds at the Puy de Dôme (alt 1465 m, Massif Central, France) is described and the metabolic potential of some bacteria is investigated. The total microflora has been quantified by epifluorescence microscopy, while the cultivable aerobic micro-organisms were isolated. Bacteria were identified by 16S DNA sequencing and fungi by morphological criteria. The total bacterial count reached about 3×10 4 cells m -3 of cloud volume (1×10 5 cells mL -1 of cloud water), of which less than 1% are cultivable. Most of the isolated micro-organisms, including 12 fungal and 17 bacterial strains, are described here for the first time in atmospheric water. Many bacterial strains seem to be adapted to the extreme conditions found in cloud water (pH, T°, UV radiations, etc.). Comparison of the two samples (March 2003) shows that pH can be a major factor controlling the structure of this community: an acidic pH (Sample 1: pH=4, 9) favours the presence of fungi and spore-forming bacteria, while a more neutral pH (Sample 2: pH=5, 8) favours greater biodiversity. We have also shown, using in situ 1H NMR, that most of the isolated bacteria are able to degrade various organic substrates such as formate, acetate, lactate, methanol and formaldehyde which represent the major organic compounds present in cloud water. In addition, the detection of intermediates indicated preferential metabolic routes for some of the strains.

Fractionation analysis of oxyanion-forming metals and metalloids in leachates of cement-based materials using ion exchange solid phase extraction.

PubMed

Mulugeta, Mesay; Wibetoe, Grethe; Engelsen, Christian J; Lund, Walter

2009-05-15

A simple and versatile solid phase extraction (SPE) method has been developed to determine the anionic species of As, Cr, Mo, Sb, Se and V in leachates of cement mortar and concrete materials in the pH range 3-13. The anionic fractions of these elements were extracted using a strong anion exchanger (SAX) and their concentrations were determined as the difference in element concentration between the sample and the SAX effluent. Inductively coupled plasma mass spectrometry (ICP-MS) was used off-line to analyse solutions before and after passing through the SAX. The extraction method has been developed by optimizing sorbent type, sorbent conditioning and sample percolation rate. Breakthrough volumes and effect of matrix constituents were also studied. It was found that a polymer-based SAX conditioned with a buffer close to the sample pH or in some cases deionised water gave the best retention of the analytes. Optimal conditions were also determined for the quantitative elution of analytes retained on the SAX. Extraction of the cement mortar and concrete leachates showed that most of the elements had similar distribution of anions in both leachate types, and that the distribution was strongly pH dependent. Cr, Mo and V exist in anionic forms in strongly basic leachates (pH>12), and significant fractions of anionic Se were also detected in these solutions. Cr, Mo, Se and V were not determined as anions by the present method in the leachates of pH<12. Anionic As and Sb were found in small fractions in most of the leachates.

Analysis of volatile human urinary metabolome by solid-phase microextraction in combination with gas chromatography-mass spectrometry for biomarker discovery: application in a pilot study to discriminate patients with renal cell carcinoma.

PubMed

Monteiro, Márcia; Carvalho, Márcia; Henrique, Rui; Jerónimo, Carmen; Moreira, Nathalie; de Lourdes Bastos, Maria; de Pinho, Paula Guedes

2014-07-01

A new and simple analytical approach consisting of headspace-solid phase microextraction (HS-SPME) sampling coupled with gas chromatography-ion trap/mass spectrometry (GC-IT/MS) was developed to study the volatile human urinary metabolome. A central composite design (CCD) was used in the optimisation of extraction conditions. Fibre selection and evaluation of pH influence were performed using an univariate mode and the influence of other parameters, such as the time and temperature of extraction, time of incubation and salt addition, that affect the efficiency of the SPME sampling, was carried out using a CCD. With a sample volume of 2 mL, the optimal conditions in terms of total response values and reproducibility were achieved by performing analyses with a divinylbenzene/polydimethylsiloxane (DVB/PDMS) fibre, in an acidic pH (pH 2) with the addition of 0.59 g of NaCl, allowing the sample to equilibrate for 9 min and extracting at 68 °C for 24 min. The applicability of the optimised method was then tested in a pilot non-target analysis of urine samples obtained from patients with renal cell carcinoma (RCC) and healthy individuals. Chemometric unsupervised analyses performed on the volatile pattern acquired for these samples clearly showed the potential of volatile urinary metabolome to discriminate between RCC and control patients. Copyright © 2014 Elsevier Ltd. All rights reserved.

Fog chemistry in the Texas-Louisiana Gulf Coast corridor

NASA Astrophysics Data System (ADS)

Raja, Suresh; Raghunathan, Ravikrishna; Yu, Xiao-Ying; Lee, Taehyoung; Chen, Jing; Kommalapati, Raghava R.; Murugesan, Karthik; Shen, Xinhua; Qingzhong, Yuan; Valsaraj, Kalliat T.; Collett, Jeffrey L.

Fog samples were collected in two population centers of the US Gulf Coast (Houston, Texas and Baton Rouge, Louisiana) using Caltech active strand cloud collectors. A total of 32 fogwater samples were collected in Baton Rouge (November 2004-February 2005) and Houston (February 2006). These samples were analyzed for pH, total and dissolved organic carbon, major inorganic ions, and a variety of organic compounds including organic acids, aromatics, carbonyls, and linear alkanes. Fogs in both environments were of moderate density, with typical fog liquid water contents <100 mg m -3. Fog samples collected in Houston reflect a clear influence of marine and anthropogenic inputs, while Baton Rouge samples also reflect agricultural inputs. The volume-weighted mean fog pH was somewhat more acidic (˜4.3) in Houston than in Baton Rouge (˜5.0). A wide pH range was observed in fog at both locations. Houston fog had higher concentrations of Cl -, NO 3-, Na +, Mg 2+, and Ca 2+. Sulfate to nitrate ratios were high in fogs at both locations, typical of many clouds in the eastern US. Total organic carbon concentrations were much higher in Houston fogs than in Baton Rouge fogs. Efforts to speciate dissolved organic carbon (DOC) reveal large contributions from organic acids and carbonyls, with smaller contributions from other organic compound families including aromatics, alkanes, amides, and alcohols. Approximately 40% of the fog DOC was unspeciated in samples from both study locations.

Study of vesicle size distribution dependence on pH value based on nanopore resistive pulse method

NASA Astrophysics Data System (ADS)

Lin, Yuqing; Rudzevich, Yauheni; Wearne, Adam; Lumpkin, Daniel; Morales, Joselyn; Nemec, Kathleen; Tatulian, Suren; Lupan, Oleg; Chow, Lee

2013-03-01

Vesicles are low-micron to sub-micron spheres formed by a lipid bilayer shell and serve as potential vehicles for drug delivery. The size of vesicle is proposed to be one of the instrumental variables affecting delivery efficiency since the size is correlated to factors like circulation and residence time in blood, the rate for cell endocytosis, and efficiency in cell targeting. In this work, we demonstrate accessible and reliable detection and size distribution measurement employing a glass nanopore device based on the resistive pulse method. This novel method enables us to investigate the size distribution dependence of pH difference across the membrane of vesicles with very small sample volume and rapid speed. This provides useful information for optimizing the efficiency of drug delivery in a pH sensitive environment.

An improved analytical strategy combining microextraction by packed sorbent combined with ultra high pressure liquid chromatography for the determination of fluoxetine, clomipramine and their active metabolites in human urine.

PubMed

Alves, Vera; Gonçalves, João; Conceição, Carlota; Teixeira, Helena M; Câmara, José S

2015-08-21

A powerful and sensitive method, by microextraction packed sorbent (MEPS), and ultra-high performance liquid chromatography (UHPLC) with a photodiode array (PDA) detection, is described for the determination of fluoxetine, clomipramine and their active metabolites in human urine samples. The MEPS variables, such as sample volume, pH, number of extraction cycles (draw-eject), and desorption conditions (solvent and solvent volume of elution) were optimized. The analysis were carried out using small sample volumes (500μL) and in a short time period (5min for the entire sample preparation step). Good linearity was obtained for all antidepressants with the correlation coefficients (R(2)) above 0.9965. The limits of detection (LOD) ranged from 0.068 to 0.087μgmL(-1). The recoveries were from 93% to 98%, with relative standard deviations less than 6%. The inter-day precision, expressed as the relative standard deviation, varied between 3.8% and 8.5% while the intra-day precision between 3.0% and 7.1%. In order to evaluate the proposed method for clinical use, the MEPS/UHPLC-PDA method was applied to analysis of urine samples from depressed patients. Copyright © 2015 Elsevier B.V. All rights reserved.

Ultrasound-assisted dispersive magnetic solid phase extraction based on amino-functionalized Fe3O4 adsorbent for recovery of clomipramine from human plasma and its determination by high performance liquid chromatography: Optimization by experimental design.

PubMed

Hamidi, Fatemeh; Hadjmohammadi, Mohammad Reza; Aghaie, Ali B G

2017-09-15

The applicability of Amino-functionalized Fe 3 O 4 nanoparticles (NPs) as an effective adsorbent was developed for the extraction and determination of clomipramine (CLP) in plasma sample by ultrasound-assisted dispersive magnetic solid phase extraction (UADM-SPE) and high-performance liquid chromatography-ultraviolet (HPLC-UV) detection. Fabrication of the Fe 3 O 4 @SiO 2 -NH 2 magnetic nanoparticles confirmed by Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The effect of different extraction parameters (i.e. pH of the sample solution, the amount of magnetic nanoparticles (MNPs), sample volume, temperature and sonication time) on the extraction recovery of CLP were investigated by response surface methodology through central composite design (CCD). The optimum condition is obtained when the affecting parameters are set to: pH of the sample solution=9, the amount of MNPs=37mg, sample volume=23mL, 25°C temperature and sonication time=1min. Under the optimum condition, extraction recovery was 90.6% with relative standard deviation of 3.5%, and enrichment factor of 117. The linear range for determination of CLP was 0.017-0.70mgL -1 with a determination coefficient (R 2 ) of 0.999. Limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.0167mgL -1 , respectively. The established UADM-SPE-HPLC-UV method was rapid, simple and efficient for determination of CLP in human plasma samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Precise method for the measurement of catalase activity in honey.

PubMed

Huidobro, José F; Sánchez, M Pilar; Muniategui, Soledad; Sancho, M Teresa

2005-01-01

An improved method is reported for the determination of catalase activity in honey. We tested different dialysis membranes, dialysis fluid compositions and amounts, dialysis temperatures, sample amounts, and dialysis times. The best results were obtained by dialysis of 7.50 g sample in a cellulose dialysis sack, using two 3 L portions of 0.015 M sodium phosphate buffer (pH 7.0) as the dialysis fluid at 4 degrees C for 22 h. As in previous methods, catalase activity was determined on the basis of the rate of disappearance of the substrate, H202, with the H202 determined spectrophotometrically at 400 nm in an assay system containing o-dianisidine and peroxidase. Trials indicated that the best solvent for the o-dianisidine was 0.2 M sodium phosphate buffer, pH 6.1; the best starting H202 concentration was 3 mM; the best HCl concentration for stopping the reaction was 6 N; and the best sample volume for catalase measurement was 7.0 mL. Precision values (relative standard deviations for analyses of 10 subsamples of each of 3 samples) were high, ranging from 0.48% for samples with high catalase activity to 1.98% for samples with low catalase activity.

Detection of viruses in drinking water by concentration on magnetic iron oxide.

PubMed

Rao, V C; Waghmare, S V; Lakhe, S B

1981-09-01

Discharge of raw domestic wastes containing human enteric viruses into water courses, consumption of untreated water from canals, streams, and shallow wells in villages, and cross-contamination of water in the distribution system because of intermittent water supply in urban areas continue to cause widespread outbreaks of infectious hepatitis in India. To detect a low number of viruses in 50- to 100-liter samples of water, a method was developed with magnetic iron oxide as the virus adsorbent. Poliovirus-seeded dechlorinated tap water, adjusted to pH 3.0 and 0.0005 M AlCl3, was filtered through a 10-g bed of iron oxide sandwiched between two AP20 prefilter pads held in a 142-mm-diameter, stainless-steel holder. Virus was eluted from iron oxide by recirculating three times a 100-ml volume of 3% beef extract, pH 9.0. The eluate was reconcentrated to 5 ml by adjusting to pH 3, adding 1 g of iron oxide, stirring for 30 min, and eluting the readsorbed virus with 5 ml of beef extract, pH 9.0. Virus recovery varied from 60 to 80%. Using the above method, we took a survey of drinking water at three locations in Nagpur during 1976 and found the presence of virus in 7 of 50 samples. The quantity of virus recovered ranged from 1 to 7 plaque-forming units per 30 to 60 liters. Virus was detected in some samples even with residual chlorine. No coliforms were detected in the virus-positive samples.

Adsorption of tetracycline on soil and sediment: effects of pH and the presence of Cu(II).

PubMed

Zhang, Zheyun; Sun, Ke; Gao, Bo; Zhang, Guixiang; Liu, Xitao; Zhao, Ye

2011-06-15

Tetracycline (TC) is frequently detected in the environment, however, knowledge on the environmental fate and transport of TC is still limited. Batch adsorption experiments of TC by soil and sediment samples were conducted. The distribution of charge and electrostatic potential of individual atoms of various TC species in the aqueous solution were determined using MOPAC version 0.034 W program in ChemBio3D Ultra software. Most of the adsorption isotherms on the soil, river and marine sediments were well fitted with the Freundlich and Polanyi-Manes (PMM) models. The single point organic carbon (OC)-normalized adsorption distribution coefficients (K(OC)) and PMM saturated adsorption capacity (Q(OC)(0)) values of TC were associated with the mesopore volume and clay content to a greater extent, indicating the mesopore volume of the soil and sediments and their clay content possibly influenced the fate and transport of TC in the natural environment. The adsorption of TC on soil and sediments strongly depended on the pH and presence of Cu(II). The presence of Cu(II) facilitated TC adsorption on soil and sediments at low pH (pH<5), possibly due to the metallic complexation and surface-bridging mechanism by Cu(II) adsorption on soil and sediments. The cation exchange interaction, metallic complexation and Coulombic interaction of mechanisms for adsorption of TC to soils and sediments were further supported by quantum chemical calculation of various TC species in different pH. Copyright © 2011 Elsevier B.V. All rights reserved.

Hollow Fiber Supported Liquid Membrane Extraction Combined with HPLC-UV for Simultaneous Preconcentration and Determination of Urinary Hippuric Acid and Mandelic Acid

PubMed Central

Bahrami, Abdulrahman; Ghamari, Farhad; Yamini, Yadollah; Ghorbani Shahna, Farshid; Moghimbeigi, Abbas

2017-01-01

This work describes a new extraction method with hollow-fiber liquid-phase microextraction based on facilitated pH gradient transport for analyzing hippuric acid and mandelic acid in aqueous samples. The factors affecting the metabolites extraction were optimized as follows: the volume of sample solution was 10 mL with pH 2 containing 0.5 mol·L−1 sodium chloride, liquid membrane containing 1-octanol with 20% (w/v) tributyl phosphate as the carrier, the time of extraction was 150 min, and stirring rate was 500 rpm. The organic phase immobilized in the pores of a hollow fiber was back-extracted into 24 µL of a solution containing sodium carbonate with pH 11, which was placed inside the lumen of the fiber. Under optimized conditions, the high enrichment factors of 172 and 195 folds, detection limit of 0.007 and 0.009 µg·mL−1 were obtained. The relative standard deviation (RSD) (%) values for intra- and inter-day precisions were calculated at 2.5%–8.2% and 4.1%–10.7%, respectively. The proposed method was successfully applied to the analysis of these metabolites in real urine samples. The results indicated that hollow-fiber liquid-phase microextraction (HF-LPME) based on facilitated pH gradient transport can be used as a sensitive and effective method for the determination of mandelic acid and hippuric acid in urine specimens. PMID:28208685

Pollutant deposition via dew in urban and rural environment, Cracow, Poland

NASA Astrophysics Data System (ADS)

Muskała, Piotr; Sobik, Mieczysław; Błaś, Marek; Polkowska, Żaneta; Bokwa, Anita

2015-01-01

This study is a comparative analysis of dew in rural and urban environment. Dew samples were collected between May and October, 2009 in two reference stations in southern Poland: Cracow and Gaik-Brzezowa. The investigation included comparison of volume and chemistry of the collected samples. Due to its formation mechanisms, dew is a good indicator of air pollution. Following parameters were analyzed in 159 collected samples: pH, electric conductivity, concentration of formaldehyde and phenols, concentration of NH4+, Ca2 +, K+, Na+, and Mg2 + cations and NO2-, NO3-, SO42 -, Cl-, F-, and PO43 - anions. The frequency of dew was approximately the same, both in urban and rural conditions reaching 43% of the measurement period. Dew intensity, expressed by volume, was on average two times larger in rural environment than in urban conditions. Urban landuse was recognized as the main factor reducing dew intensity in the urban station in comparison to the rural. Furthermore, the intensity of dew depended on synoptic scale air circulation at both measurement sites. As expected, samples collected in Cracow were much more polluted than the ones from Gaik-Brzezowa. The average TIC (Total Ionic Content) parameter was approximately 50% higher at the urban station. The pH in the rural station was more acidic. NO3- anions and Ca2 + cations were predominant in both measurement sites, however the participation of Ca2 + in Cracow was higher. NO3- indicates pollutions emitted by transport and industrial sources. The concentration of the analytes in both stations, as the volume, depended on air circulation direction. For Gaik-Brzezowa the highest TIC was observed mainly within southern circulation, while for Cracow the highest TIC was noted within both northern and southern. In general the rural station represented background pollution for the whole region and the pollution in Cracow was more dependent on local urban sources as transport or industry.

pH-based fiber optic biosensors for use in clinical and biotechnological applications

NASA Astrophysics Data System (ADS)

Mueller, Cord; Hitzmann, Bernd; Schubert, Florian; Scheper, Thomas

1995-05-01

The development of pH-based fiber optic biosensors and their uses in clinical and biotechnological applications are described. Based on a pH-sensitive optode, different biosensors for urea, penicillin, glucose and creatinine were developed. A multichannel modular fluorimeter was used to measure signals from up to three optodes simultaneously. The pH value and the buffer capacity are critical factors for biosensors based on pH probes and influence the biosensor signal. A flow injection analysis (FIA) system is used to eliminate the latter influences. With this integrated system, samples can be analyzed sequentially by the injection of a defined volume of each sample into a continuously flowing buffer stream that transports the samples to the sensors. The complex signal is transformed and analyzed by a computer system. Characteristic features of the FIA peak give information about the buffer capacity in the solution. With the help of intelligent computing (neural networks) it is possible to recognize these features and relate them to the respective buffer capacity to obtain more accurate values. Various applications of these biosensors are discussed. The pH optode is also used to monitor enzymatic reactions in non aqueous solvents. In this case the production of acetic acid can be detected on line.

Gold Nanocluster-DNase 1 Hybrid Materials for DNA Contamination Sensing

DTIC Science & Technology

2014-01-01

or 1 mM) was added to 2 mL of protein solution under vigorous stirring at 37 ̊ C. After 5 minutes 200 µL of NaOH (1 M) was added to raise the pH to...12 for the 1, 5, and 10 mM HAuCl4 samples whereas 400 µL of NaOH (1M) was required. The various protein/gold mixtures were then left to react for...1: AuNCs were carried out in a final volume of 20 µL buffer (100 mM sodium acetate, 6.25 mM magnesium sulfate pH 5.0), containing 2 µg of dsDNA

A comparison of recovery of virus from wastewaters by beef extract-Celite, ferric chloride, and filter concentration procedures.

PubMed

Dahling, D R; Wright, B A

1988-12-01

An improved concentration method using sample volumes as large as 1500 ml has been developed to monitor for viruses in wastewaters. Non-precipitating dry beef extract powder is added to wastewater samples to give a 3% concentration and mixed until dissolved. This is followed by the addition of Celite as a virus adsorbent. By manipulating pH, viruses are eluted from the Celite in small volumes of phosphate buffer. This procedure was further tested without the aid of the Celite additives using a precipitating beef extract powder and substituting FeCl3 as an alternate reagent for the Celite. Comparison testing was also made with the currently recommended cartridge and disc filter procedures. In all cases, the non-precipitating beef extract-Celite method gave higher recovery rates in highly polluted waters.

Electrospun biocompatible Chitosan/MIL-101 (Fe) composite nanofibers for solid-phase extraction of Δ9-tetrahydrocannabinol in whole blood samples using Box-Behnken experimental design.

PubMed

Asiabi, Mina; Mehdinia, Ali; Jabbari, Ali

2017-01-06

The nanofibers of biocompatible Chitosan/MIL-101 (Fe) composite were synthesized by a simple, cheap and accessible electrospining method and applied for mat-based extraction of trace amount of Δ9-tetrahydrocannabinol (THC) from human whole blood sample following its combination by high performance liquid chromatography-ultraviolet detection. The composite nanofibres were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and N 2 adsorption-desorption experiments. The volume of eluting solvent, sorbent amount, pH and% NaCl (w/v) influencing on the responses were investigated using factorial experimental design. The optimum point was achieved by analysis of the results according to design expert (DX) software. The volume of eluting solvent, sorbent amount and pH were significant variables, and 150μL, 7mg and 7.0 were respectively chosen for obtaining the best extraction response. Under the optimum conditions, the method was exhibited a linear range of 0.1-100μgL -1 (R 2 =0.9943) for THC with a detection limit of 0.04μgL -1 . Acceptable values for intra-day (3.2%) and inter-day (4.8%) relative standard deviations were obtained. The high preconcentration factor (970) and satisfactory recoveries (88.2%-92.4%) in whole blood samples were achieved which proved the capability of the method for trace determination of THC in the human whole blood samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Novel synthesis of nanocomposite for the extraction of Sildenafil Citrate (Viagra) from water and urine samples: Process screening and optimization.

PubMed

Asfaram, Arash; Ghaedi, Mehrorang; Purkait, Mihir Kumar

2017-09-01

A sensitive analytical method is investigated to concentrate and determine trace level of Sildenafil Citrate (SLC) present in water and urine samples. The method is based on a sample treatment using dispersive solid-phase micro-extraction (DSPME) with laboratory-made Mn@ CuS/ZnS nanocomposite loaded on activated carbon (Mn@ CuS/ZnS-NCs-AC) as a sorbent for the target analyte. The efficiency was enhanced by ultrasound-assisted (UA) with dispersive nanocomposite solid-phase micro-extraction (UA-DNSPME). Four significant variables affecting SLC recovery like; pH, eluent volume, sonication time and adsorbent mass were selected by the Plackett-Burman design (PBD) experiments. These selected factors were optimized by the central composite design (CCD) to maximize extraction of SLC. The results exhibited that the optimum conditions for maximizing extraction of SLC were 6.0 pH, 300μL eluent (acetonitrile) volume, 10mg of adsorbent and 6min sonication time. Under optimized conditions, virtuous linearity of SLC was ranged from 30 to 4000ngmL -1 with R 2 of 0.99. The limit of detection (LOD) was 2.50ngmL -1 and the recoveries at two spiked levels were ranged from 97.37 to 103.21% with the relative standard deviation (RSD) less than 4.50% (n=15). The enhancement factor (EF) was 81.91. The results show that the combination UAE with DNSPME is a suitable method for the determination of SLC in water and urine samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Optimization of microwave-assisted extraction of analgesic and anti-inflammatory drugs from human plasma and urine using response surface experimental designs.

PubMed

Fernández, Purificación; Fernández, Ana M; Bermejo, Ana M; Lorenzo, Rosa A; Carro, Antonia M

2013-04-01

The performance of microwave-assisted extraction and HPLC with photodiode array detection method for determination of six analgesic and anti-inflammatory drugs from plasma and urine, is described, optimized, and validated. Several parameters affecting the extraction technique were optimized using experimental designs. A four-factor (temperature, phosphate buffer pH 4.0 volume, extraction solvent volume, and time) hybrid experimental design was used for extraction optimization in plasma, and three-factor (temperature, extraction solvent volume, and time) Doehlert design was chosen to extraction optimization in urine. The use of desirability functions revealed the optimal extraction conditions as follows: 67°C, 4 mL phosphate buffer pH 4.0, 12 mL of ethyl acetate and 9 min, for plasma and the same volume of buffer and ethyl acetate, 115°C and 4 min for urine. Limits of detection ranged from 4 to 45 ng/mL in plasma and from 8 to 85 ng/mL in urine. The reproducibility evaluated at two concentration levels was less than 6.5% for both specimens. The recoveries were from 89 to 99% for plasma and from 83 to 99% for urine. The proposed method was successfully applied in plasma and urine samples obtained from analgesic users. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Bulk chlorine uptake by polyamide active layers of thin-film composite membranes upon exposure to free chlorine-kinetics, mechanisms, and modeling.

PubMed

Powell, Joshua; Luh, Jeanne; Coronell, Orlando

2014-01-01

We studied the volume-averaged chlorine (Cl) uptake into the bulk region of the aromatic polyamide active layer of a reverse osmosis membrane upon exposure to free chlorine. Volume-averaged measurements were obtained using Rutherford backscattering spectrometry with samples prepared at a range of free chlorine concentrations, exposure times, and mixing, rinsing, and pH conditions. Our volume-averaged measurements complement previous studies that have quantified Cl uptake at the active layer surface (top ≈ 7 nm) and advance the mechanistic understanding of Cl uptake by aromatic polyamide active layers. Our results show that surface Cl uptake is representative of and underestimates volume-averaged Cl uptake under acidic conditions and alkaline conditions, respectively. Our results also support that (i) under acidic conditions, N-chlorination followed by Orton rearrangement is the dominant Cl uptake mechanism with N-chlorination as the rate-limiting step; (ii) under alkaline conditions, N-chlorination and dechlorination of N-chlorinated amide links by hydroxyl ion are the two dominant processes; and (iii) under neutral pH conditions, the rates of N-chlorination and Orton rearrangement are comparable. We propose a kinetic model that satisfactorily describes Cl uptake under acidic and alkaline conditions, with the largest discrepancies between model and experiment occurring under alkaline conditions at relatively high chlorine exposures.

On-line focusing of flavin derivatives using Dynamic pH junction-sweeping capillary electrophoresis with laser-induced fluorescence detection.

PubMed

Britz-McKibbin, Philip; Otsuka, Koji; Terabe, Shigeru

2002-08-01

Simple yet effective methods to enhance concentration sensitivity is needed for capillary electrophoresis (CE) to become a practical method to analyze trace levels of analytes in real samples. In this report, the development of a novel on-line preconcentration technique combining dynamic pH junction and sweeping modes of focusing is applied to the sensitive and selective analysis of three flavin derivatives: riboflavin, flavin mononucleotide (FMN) and flavin adenine dinucleotide (FAD). Picomolar (pM) detectability of flavins by CE with laser-induced fluorescence (LIF) detection is demonstrated through effective focusing of large sample volumes (up to 22% capillary length) using a dual pH junction-sweeping focusing mode. This results in greater than a 1,200-fold improvement in sensitivity relative to conventional injection methods, giving a limit of detection (S/N = 3) of approximately 4.0 pM for FAD and FMN. Flavin focusing is examined in terms of analyte mobility dependence on buffer pH, borate complexation and SDS interaction. Dynamic pH junction-sweeping extends on-line focusing to both neutral (hydrophobic) and weakly acidic (hydrophilic) species and is considered useful in cases when either conventional sweeping or dynamic pH junction techniques used alone are less effective for certain classes of analytes. Enhanced focusing performance by this hyphenated method was demonstrated by greater than a 4-fold reduction in flavin bandwidth, as compared to either sweeping or dynamic pH junction, reflected by analyte detector bandwidths <0.20 cm. Novel on-line focusing strategies are required to improve sensitivity in CE, which may be applied toward more effective biochemical analysis methods for diverse types of analytes.

The role of H2 receptor antagonist premedication in pregnant day care patients.

PubMed

Stock, J G; Sutherland, A D

1985-09-01

In a randomised study of 132 pregnant outpatients, the effect on gastric volume and pH of oral premedication with a single dose of an H2 antagonist was investigated. Either cimetidine 400 mg (n = 33), or ranitidine 150 mg (n = 33), were given 90 to 120 minutes before scheduled surgery. Mean pH was significantly higher in cimetidine (5.0) and ranitidine (5.2) groups, and mean volume was significantly lower in cimetidine (13.2 ml) and ranitidine (11.1 ml) groups compared with 66 untreated patients (pH 1.6, volume 22.1 ml). A gastric pH less than or equal to 2.5 was found in 97 per cent of unpremedicated patients and 35 per cent of these patients also had a gastric volume greater than or equal to 25 ml. Eighty-three per cent of patients received their premedication within 75-200 minutes of surgery. Patients premedicated within that range had a significantly lower incidence of either a gastric pH less than or equal to 2.5 or a volume greater than or equal to 25 ml (p less than 0.01). Both cimetidine and ranitidine significantly reduced the number of patients with these risk factors. Four patients, however, in the cimetidine group had both a pH less than or equal to 2.5 and a volume greater than or equal to 25 ml. Pharmacological manipulation of the gastric environment does not prevent aspiration and clearly cannot be substituted for careful airway management and vigilance on the part of the anaesthetist. However, premedication of pregnant outpatients with a single, oral dose of an H2 antagonist is a simple, inexpensive, safe and effective way of reducing the risk of a severe aspiration pneumonitis.

Determination of trace metals in drinking water using solid-phase extraction disks and X-ray fluorescence spectrometry.

PubMed

Hou, Xiandeng; Peters, Heather L; Yang, Zheng; Wagner, Karl A; Batchelor, James D; Daniel, Meredith M; Jones, Bradley T

2003-03-01

A convenient method is described for monitoring Cd, Ni, Cu, and Pb at trace levels in drinking water samples. These metals are preconcentrated on a chelating solid-phase extraction disk and then determined by X-ray fluorescence spectrometry. The method tolerates a wide pH range (pH 6-14) and a large amount of alkaline and alkaline earth elements. The preconcentration factor is well over 1600, assuming a 1 L water sample volume. The limits of detection for Cd, Ni, Cu, and Pb are 3.8, 0.6, 0.4, and 0.3 ng/mL, respectively. These are well below the federal maximum contaminant level values, which are 5, 100, 1300, and 15 ng/mL, respectively. The proposed method has many advantages including ease of operation, multielement capability, nondestructiveness, high sensitivity, and relative cost efficiency. The solid-phase extraction step can be conducted in the field and then the disks can be mailed to a laboratory for the analysis, eliminating the cost of transporting large volumes of water samples. Furthermore, the color of the used extraction disk provides an initial estimate of the degree of contamination for some transition metals (for example, Ni and Cu). Thus, the overall cost for analysis of metals in drinking water can be minimized by implementing the method, and small water supply companies with limited budgets will be better able to comply with the Safe Drinking Water Act.

Determination of residual nonsteroidal anti-inflammatory drugs in aqueous sample using magnetic nanoparticles modified with cetyltrimethylammonium bromide by high performance liquid chromatography.

PubMed

Khoeini Sharifabadi, Malihe; Saber-Tehrani, Mohammad; Waqif Husain, Syed; Mehdinia, Ali; Aberoomand-Azar, Parviz

2014-01-01

A simple and sensitive solid-phase extraction method for separation and preconcentration of trace amount of four nonsteroidal anti-inflammatory drugs (naproxen, indomethacin, diclofenac, and ibuprofen) using Fe3O4 magnetic nanoparticles modified with cetyltrimethylammonium bromide has been developed. For this purpose, the surface of MNPs was modified with cetyltrimethylammonium bromide (CTAB) as a cationic surfactant. Effects of different parameters influencing the extraction efficiency of drugs including the pH, amount of salt, shaking time, eluent type, the volume of solvent, amount of adsorbent, sample volume, and the time of desorption were investigated and optimized. Methanol has been used as desorption solvent and the extracts were analysed on a reversed-phase octadecyl silica column using 0.02 M phosphate-buffer (pH = 6.02) acetonitrile (65 : 35 v/v) as the mobile phase and the effluents were measured at 202 nm with ultraviolet detector. The relative standard deviation (RSD%) of the method was investigated at three concentrations (25, 50, and 200 ng/mL) and was in the range of 3.98-9.83% (n = 6) for 50 ng/mL. The calibration curves obtained for studied drugs show reasonable linearity (R (2) > 0.99) and the limit of detection (LODs) ranged between 2 and 7 ng/mL. Finally, the proposed method has been effectively employed in extraction and determination of the drugs in biological and environmental samples.

Selenium adsorption and speciation with Mg-FeCO₃ layered double hydroxides loaded cellulose fibre.

PubMed

Chen, Ming-Li; An, Myog-Il

2012-06-15

A novel adsorbent was developed by coating Mg-FeCO(3) layered double hydroxides (LDHs) on cellulose fibre. The LDHs take up significant amount of selenite and selenate in a wide pH range with similar sorption capacities (pH 3.8-8.0 for selenite and pH 5.8-7.0 for selenate). A mini-column packed with Mg-FeCO(3) LDHs layer coated cellulose fibre particles was incorporated into a sequential injection system for uptake of selenite at pH 6.0. The retained selenite was afterwards collected with 70 μ L of 0.8%(m/v) NaOH as eluent, followed by hydride generation and atomic fluorescence spectrometric detection. Total inorganic selenium was adsorbed at pH 6.0 by the LDHs-cellulose fibre mini-column after selenate was pre-reduced to selenite by 2.0 mol L(-1) HCl at 80°C, and selenium speciation was performed by difference. With a sample volume of 1.0 mL, an enrichment factor of 13.3 was derived with a detection limit of 11 ng L(-1) within a linear range of 0.04-4.0 μg L(-1). A relative standard deviation (RSD) of 3.3% (0.5 μg L(-1), n=11) was achieved. The procedure was validated by analyzing selenium in a certified reference material GBW 10010 (rice), and speciation of inorganic selenium in natural water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Polymer monolithic capillary microextraction combined on-line with inductively coupled plasma MS for the determination of trace rare earth elements in biological samples.

PubMed

Zhang, Lin; Chen, Beibei; He, Man; Hu, Bin

2013-07-01

A rapid and sensitive method based on polymer monolithic capillary microextraction combined on-line with microconcentric nebulization inductively coupled plasma MS has been developed for the determination of trace/ultratrace rare earth elements in biological samples. For this purpose, the iminodiacetic acid modified poly(glycidyl methacrylate-trimethylolpropane trimethacrylate) monolithic capillary was prepared and characterized by SEM and FTIR spectroscopy. Factors affecting the extraction efficiency, such as sample pH, sample flow rate, sample/eluent volume, and coexisting ions were investigated in detail. Under the optimal conditions, the LODs for rare earth elements were in the range of 0.08 (Er) to 0.97 ng/L (Nd) with a sampling frequency of 8.5 h(-1), and the RSDs were between 1.5% (Sm) and 7.4% (Nd) (c = 20 ng/L, n = 7). The proposed method was successfully applied to the analysis of trace/ultratrace rare earth elements in human urine and serum samples, and the recoveries for the spiked samples were in the range of 82-105%. The developed method was simple, rapid, sensitive, and favorable for the analysis of trace/ultratrace rare earth elements in biological samples with limited sample volume. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Small angle neutron scattering (SANS) study of gastric mucin solutions

NASA Astrophysics Data System (ADS)

Hong, Z.; Bansil, R.; Waigh, T.; Turner, B.; Bhaskar, K. R.; Afdhal, N.; Lal, J.

2002-03-01

We report the first results from a SANS study of purified porcine gastric mucin solutions in D2O. The ability of this glycoprotein to protect the stomach epithelium from acid damage, may be due to a pH dependent conformational transition which leads to gelation at low pH Cao et. al. (Biophysical. J. 76, 1250, 1999). SANS measurements were made over the concentration range of 1 -15 mg/ml at pH 7, 4 and 2. The data indicate that at pH 7 the excluded volume exponent is 1.7, characteristic of swollen chains whereas at pH 2 this exponent increases to 2, indicating theta or poor solvent conditions, consistent with the hydrophobic interactions increasing at lower pH. From a Guinier analysis of the 1mg/ml data at low q's (0.003- 0.007 Å-1) we estimate the cross section radius of the effective cylinder to be 23nm and its length as 96nm in an unbuffered sample, i.e. close to pH 7. In the intermediate q-range (0.01 -0.1Å-1) at pH 7 a fit to the Debye chain gives radius of gyration Rg of 16nm. Mucin is best modelled as an elongated micelle with a cylindrical or worm-like chain to represent the protein core and the sugar chains forming the corona. Results of such calculations will be presented.

Automation of high-frequency sampling of environmental waters for reactive species

NASA Astrophysics Data System (ADS)

Kim, H.; Bishop, J. K.; Wood, T.; Fung, I.; Fong, M.

2011-12-01

Trace metals, particularly iron and manganese, play a critical role in some ecosystems as a limiting factor to determine primary productivity, in geochemistry, especially redox chemistry as important electron donors and acceptors, and in aquatic environments as carriers of contaminant transport. Dynamics of trace metals are closely related to various hydrologic events such as rainfall. Storm flow triggers dramatic changes of both dissolved and particulate trace metals concentrations and affects other important environmental parameters linked to trace metal behavior such as dissolved organic carbon (DOC). To improve our understanding of behaviors of trace metals and underlying processes, water chemistry information must be collected for an adequately long period of time at higher frequency than conventional manual sampling (e.g. weekly, biweekly). In this study, we developed an automated sampling system to document the dynamics of trace metals, focusing on Fe and Mn, and DOC for a multiple-year high-frequency geochemistry time series in a small catchment, called Rivendell located at Angelo Coast Range Reserve, California. We are sampling ground and streamwater using the automated sampling system in daily-frequency and the condition of the site is substantially variable from season to season. The ranges of pH of ground and streamwater are pH 5 - 7 and pH 7.8 - 8.3, respectively. DOC is usually sub-ppm, but during rain events, it increases by an order of magnitude. The automated sampling system focuses on two aspects- 1) a modified design of sampler to improve sample integrity for trace metals and DOC and 2) remote controlling system to update sampling volume and timing according to hydrological conditions. To maintain sample integrity, the developed method employed gravity filtering using large volume syringes (140mL) and syringe filters connected to a set of polypropylene bottles and a borosilicate bottle via Teflon tubing. Without filtration, in a few days, the dissolved concentration of Fe and Mn in the ground and streamwater samples stored in low density polyethylene (LDPE) sample bags decreased by 89% and 97%, respectively. In some cases of groundwater, the concentration of Ca decreased by 25%, due to degassing of CO2. However, DOC of the samples in LDPE bags without filtration increased up to 50% in 2 weeks, suggesting contamination from the bag. Performance of the new design was evaluated using the Fe-Mn-spiked Rivendell samples and environmental water samples collected from 1) Rivendell, 2) the Strawberry Creek located at the University of California, Berkeley campus, and 3) the San Francisco Bay. The samples were filtered using the developed method and stored in room temperature in 2 - 3 weeks without further treatment. The method improved the sample integrity significantly; the average recovery rates of Fe, Mn, DOC, and Ca were 92%, 98%, 90%, and 97%, respectively.

Pulmonary hypertension due to left heart disease: diagnostic and prognostic value of CT in chronic systolic heart failure.

PubMed

Colin, Geoffrey C; Gerber, Bernhard L; de Meester de Ravenstein, Christophe; Byl, David; Dietz, Anna; Kamga, Michele; Pasquet, Agnes; Vancraeynest, David; Vanoverschelde, Jean-Louis; D'Hondt, Anne-Marie; Ghaye, Benoit; Pouleur, Anne-Catherine

2018-05-14

To evaluate the ability of chest computed tomography (CT) to predict pulmonary hypertension (PH) and outcome in chronic heart failure with reduced ejection fraction (HFrEF). We reviewed 119 consecutive patients with HFrEF by CT, transthoracic echocardiography (TTE) and right heart catheterization (RHC). CT-derived pulmonary artery (PA) diameter and PA to ascending aorta diameter ratio (PA:A ratio), left atrial, right atrial, right ventricular (RV) and left ventricular volumes were correlated with RHC mean pulmonary arterial pressure (mPAP) . Diagnostic accuracy to predict PH and ability to predict primary composite endpoint of all-cause mortality and HF events were evaluated. RV volume was significantly higher in 81 patients with PH compared to 38 patients without PH (133 ml/m 2 vs. 79 ml/m 2 , p < 0.001) and was moderately correlated with mPAP (r=0.55, p < 0.001). Also, RV volume had higher ability to predict PH (area under the curve: 0.88) than PA diameter (0.79), PA:A ratio (0.76) by CT and tricuspid regurgitation gradient (0.83) and RV basal diameter by TTE (0.84, all p < 0.001). During the follow-up period (median: 3.4 years), 51 patients (43%) had HF events or died. After correction for important clinical, TTE and RHC parameters, RV volume (adjusted hazard ratio [HR]: 1.71, 95% CI 1.31-2.23, p < 0.001) and PA diameter (HR: 1.61, 95% CI 1.18-2.22, p = 0.003) were independent predictors of the primary endpoint. In patients with HFrEF, measurement of RV volume and PA diameter on ungated CT are non-invasive markers of PH and may help to predict the patient outcome. • Right ventricular (RV) volume measured by chest CT has good ability to identify pulmonary hypertension (PH) in patients with chronic heart failure (HF) and reduced ejection fraction (HFrEF). • The accuracy of pulmonary artery (PA) diameter and PA to ascending aorta diameter ratio (PA:A ratio) to predict PH was similar to previous studies, however, with lower cut-offs (28.1 mm and 0.92, respectively). • Chest CT-derived PA diameter and RV volume independently predict all-cause mortality and HF events and improve outcome prediction in patients with advanced HFrEF.

Determination of ochratoxin A in fruit juice by high-performance liquid chromatography after vortex-assisted emulsification microextraction based on solidification of floating organic drop.

PubMed

Asadi, Mohammad

2018-03-01

A rapid, simple, and green vortex-assisted emulsification microextraction method based on solidification of floating organic drop was developed for the extraction and determination of ochratoxin A (OTA) with high-performance liquid chromatography. Some factors influencing the extraction efficiency of OTA such as the type and volume of extraction solvent, sample pH, salt concentration, vortex time, and sample volume were optimized. Under optimized conditions, the calibration curve exhibited linearity in the range of 50.0-500 ng L -1 with a coefficient of determination higher than 0.999. The limit of detection was 15.0 ng L -1 . The inter- and intra-assays relative standard deviations were in a range of 4.7-8.7%. The accuracy of the developed method was investigated through recovery experiments, and it was successfully used for the quantification of OTA in 40 samples of fruit juice.

Xerostomia, salivary characteristics and gland volumes following intensity-modulated radiotherapy for nasopharyngeal carcinoma: a two-year follow up.

PubMed

Sim, Cpc; Soong, Y L; Pang, Epp; Lim, C; Walker, G D; Manton, D J; Reynolds, E C; Wee, Jts

2018-06-01

To evaluate changes in xerostomia status, salivary characteristics and gland volumes 2 years following radiotherapy in nasopharyngeal carcinoma patients. Xerostomia scores, salivary flow rates, pH and buffering capacity were measured at pre-radiotherapy, mid-radiotherapy, 2 weeks, 3 months and 2 years post-radiotherapy. Salivary gland volumes and their correlation with radiation dose were also assessed. Mean radiation dose to oral cavity, parotid and submandibular glands (SMG) was 44.5, 65.0 and 38.6 Gy respectively. Parotid and SMG volumes decreased 33% at 3 months post-radiotherapy; volumes at 2 years post-radiotherapy were 84% and 51% of pre-radiotherapy levels, respectively. Correlations were observed between parotid gland volume per cent reduction and its radiation dose and between resting salivary flow rate reduction and post-radiotherapy/pre-radiotherapy SMG volume ratio. Salivary flow rates and resting saliva pH remained significantly low at 2 years post-radiotherapy (both flow rates, P = 0.001; resting saliva pH, P = 0.005). Similarly, xerostomia scores remained significantly higher compared with pre-radiotherapy levels. Submandibular gland volumetric shrinkage persisted 2 years after radiotherapy. Xerostomia scores remained significantly higher, and salivary flow rates and resting saliva pH remained significantly lower, suggesting that study participants were still at risk for hyposalivation-related oral diseases. © 2018 Australian Dental Association.

Speciation analysis of mercury by dispersive solid-phase extraction coupled with capillary electrophoresis.

PubMed

Li, Jinhua; Liu, Junying; Lu, Wenhui; Gao, Fangfang; Wang, Liyan; Ma, Jiping; Liu, Huitao; Liao, Chunyang; Chen, Lingxin

2018-04-23

A pretreatment method of dispersive solid-phase extraction (DSPE) along with back-extraction followed by CE-UV detector was developed for the determination of mercury species in water samples. Sulfhydryl-functionalized SiO 2 microspheres (SiO 2 -SH) were synthesized and used as DSPE adsorbents for selective extraction and enrichment of three organic mercury species namely ethylmercury (EtHg), methylmercury (MeHg), and phenylmercury (PhHg), along with L-cysteine (L-cys) containing hydrochloric acid as back-extraction solvent. Several main extraction parameters were systematically investigated including sample pH, amount of adsorbent, extraction and back-extraction time, volume of eluent, and concentration of hydrochloric acid. Under optimal conditions, good linearity was achieved with correlation coefficients over 0.9990, in the range of 4-200 μg/L for EtHg, and 2-200 μg/L for MeHg and PhHg. The LODs were obtained of 1.07, 0.34, and 0.24 μg/L for EtHg, MeHg, and PhHg, respectively, as well as the LOQs were 3.57, 1.13, and 0.79 μg/L, respectively, with enrichment factors ranging from 109 to 184. Recoveries were attained with tap and lake water samples in a range of 62.3-107.2%, with relative standard deviations of 3.5-10.1%. The results proved that the method of SiO 2 -SH based DSPE coupled with CE-UV was a simple, rapid, cost-effective, and eco-friendly alternative for the determination of mercury species in water samples. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Characteristics of precipitation pH and conductivity at Mt. Huang].

PubMed

Shi, Chun-e; Deng, Xue-liang; Wu, Bi-wen; Hong, Jie; Zhang, Su; Yang, Yuan-jian

2013-05-01

To understand the general characteristics of pH distribution and pollution in precipitation at Mt. Huang, statistical analyses were conducted for the routine measurements of pH and conductivity (K) at Mt. Huang during 2006-2011. The results showed that: (1) Over the period of study, the annual volume weighted mean (VWM) precipitation pH varied from 4.81 to 5.57, with precipitation acidity strengthening before 2009 and weakening thereafter. The precipitation acidity showed evident seasonal variations, with the VWM pH lowest in winter (4.78), and highest in summer (5.33). The occurrence frequency of acid rain was 46% , accounting for 45% of total rainfalls and with the most frequent pH falling into weak acid to neutral rain. (2) The annual VWM K varied from 16.91 to 27.84 microS x cm(-1), with no evident trend. As for ions pollution, the precipitation was relatively clean at Mt. Huang, with the most frequent K range being below 15 microS x cm(-1), followed by 15-25 microS x cm(-1). From February 2010 to December 2011, precipitation samples were collected on daily basis for ions analysis, as well as pH and K measurement in lab. Detailed comparisons were conducted between the two sets of pH and K, one set from field measurement and the other from lab measurement. The results indicated: (1) The lab measured pH (K) was highly correlated with the field pH (K); however, the lab pH tended to move towards neutral comparing with the corresponding field pH, and the shift range was closely correlated with the field pH and rainfall. The shift range of K from field to lab was highly correlated with the total ion concentration of precipitation. The field K showed evident negative correlation with the field pH with a correlation coefficient of -0.51. (2) When sampling with nylon-polyethylene bags, the statistics showed smaller bias between two sets of pH, with higher correlation coefficient between two sets of K. Furthermore, the lab K also showed evident negative correlation with the lab pH. Comparing with the observations at other alpine sites in central to eastern China, the natural precipitation at Mt. Huang was weaker in acidity and contains lower ion concentration.

A Novel Strategy for Isolation, Molecular and Functional Characterization of Embryonic Mammary Stem Cells Using Molecular Genetics and Microfluidic Sorting

DTIC Science & Technology

2008-06-01

Geoffrey M. Wahl, Ph.D. CONTRACTING ORGANIZATION: The Salk Institute for Biological Studies La Jolla, CA 92037-1099...PERFORMING ORGANIZATION REPORT NUMBER The Salk Institute for Biological Studies La Jolla, CA 92037-1099 9. SPONSORING...validated the use of a micro- volume cell sorter ( Celula , Inc.). This instrument is capable of sorting as few as 150 GFP positive cells from a sample

Synthesis of cross-linked chitosan modified with the glycine moiety for the collection/concentration of bismuth in aquatic samples for ICP-MS determination.

PubMed

Oshita, Koji; Noguchi, Osamu; Oshima, Mitsuko; Motomizu, Shoji

2007-10-01

A chelating resin, cross-linked chitosan modified with the glycine moiety (glycine-type chitosan resin), was developed for the collection and concentration of bismuth in aquatic samples for ICP-MS measurements. The adsorption behavior of bismuth and 55 elements on glycine-type chitosan resin was systematically examined by passing a sample solution containing 56 elements through a mini-column packed with the resin (wet volume; 1 ml). After eluting the elements adsorbed on the resin with nitric acid, the eluates were measured by ICP-MS. The glycine-type chitosan resin could adsorb several cations by a chelating mechanism and several oxoanions by an anion-exchange mechanism. Especially, the resin could adsorb almost 100% Bi(III) over a wide pH region from pH 2 to 6. Bismuth could be strongly adsorbed at pH 3, and eluted quantitatively with 10 ml of 3 M nitric acid. A column pretreatment method with the glycine-type chitosan resin was used prior to removal of high concentrations of matrices in a seawater sample and the preconcentration of trace bismuth in river water samples for ICP-MS measurements. The column pretreatment method was also applied to the determination of bismuth in real samples by ICP-MS. The LOD of bismuth was 0.1 pg ml(-1) by 10-fold column preconcentration for ICP-MS measurements. The analytical results for bismuth in sea and river water samples by ICP-MS were 22.9 +/- 0.5 pg ml(-1) (RSD, 2.2%) and 2.08 +/- 0.05 pg ml(-1) (RSD, 2.4%), respectively.

Preconcentration and solid phase extraction method for the determination of Co, Cu, Ni, Zn and Cd in environmental and biological samples using activated carbon by FAAS.

PubMed

Kiran, K; Suresh Kumar, K; Suvardhan, K; Janardhanam, K; Chiranjeevi, P

2007-08-17

2-{[1-(2-Hydroxynaphthyl) methylidene] amino} benzoic acid (HNMABA) was synthesized for solid phase extraction (SPE) to the determination of Co, Cu, Ni, Zn and Cd in environmental and biological samples by flame atomic absorption spectrophotometry (FAAS). These metals were sorbed as HNMABA complexes on activated carbon (AC) at the pH range of 5.0+/-0.2 and eluted with 6 ml of 1M HNO3 in acetone. The effects of sample volume, eluent volume and recovery have been investigated to enhance the sensitivity and selectivity of proposed method. The effect of interferences on the sorption of metal ions was studied. The concentration of the metal ions detected after preconcentration was in agreement with the added amount. The detection limits for the metals studied were in the range of 0.75-3.82 microg ml(-1). The proposed system produced satisfactory results for the determination of Co, Cu, Ni, Zn and Cd metals in environmental and biological samples.

Rapid analysis of ultraviolet filters using dispersive liquid-liquid microextraction coupled to headspace gas chromatography and mass spectrometry.

PubMed

Pierson, Stephen A; Trujillo-Rodríguez, María J; Anderson, Jared L

2018-05-29

An ionic-liquid-based in situ dispersive liquid-liquid microextraction method coupled to headspace gas chromatography and mass spectrometry was developed for the rapid analysis of ultraviolet filters. The chemical structures of five ionic liquids were specifically designed to incorporate various functional groups for the favorable extraction of the target analytes. Extraction parameters including ionic liquid mass, molar ratio of ionic liquid to metathesis reagent, vortex time, ionic strength, pH, and total sample volume were studied and optimized. The effect of the headspace temperature and volume during the headspace sampling step was also evaluated to increase the sensitivity of the method. The optimized procedure is fast as it only required ∼7-10 min per extraction and allowed for multiple extractions to be performed simultaneously. In addition, the method exhibited high precision, good linearity, and low limits of detection for six ultraviolet filters in aqueous samples. The developed method was applied to both pool and lake water samples attaining acceptable relative recovery values. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Wine pH Prevails over Buffering Capacity of Human Saliva.

PubMed

Obreque-Slier, Elías; Espínola-Espínola, Valeria; López-Solís, Remigio

2016-11-02

Wine is an acidic beverage; its pH (2.9-3.8) is critically important to its organoleptic properties. During degustation, wine interacts with <1 mL of mouth saliva, the pH of which is near 7.0. This is buffered predominantly by the carbonate/bicarbonate pair (pK a = 6.1). Few data are available on whether the buffering capacity of saliva may alter the pH of wine and thus its sensorial properties. In this study both in vitro and in vivo approaches were conducted to measure pH in mixtures of representative red and white wines with human saliva. Continuous additions of microvolumes of either wine to a definite volume (3 mL) of saliva in vitro resulted in a progressive and steep decline in the pH of the wine/saliva mixture. Thus, a few microliters of either wine (<0.27 mL) was sufficient to reduce the pH of saliva by 1 pH unit. Further additions of wine to saliva lowered the pH to that of the corresponding wine. In the in vivo assay, definite volumes (1.5-18 mL) of either wine were mixed for 15 s with the mouth saliva of individual healthy subjects before pH determination in the expectorated wine/saliva mixtures. Compared to saliva, pronounced decreases in pH were observed, thus approaching the pH of wine even with the smallest volume of wine in the assay. Altogether, these results demonstrate that the buffering capacity of wine prevails over that of saliva and that during degustation the pH of the wine/saliva mixture in the mouth is, at least temporarily, that of the corresponding wine.

Mercury(II) and methyl mercury determinations in water and fish samples by using solid phase extraction and cold vapour atomic absorption spectrometry combination.

PubMed

Tuzen, Mustafa; Karaman, Isa; Citak, Demirhan; Soylak, Mustafa

2009-07-01

A method has been developed for mercury(II) and methyl mercury speciation on Staphylococcus aureus loaded Dowex Optipore V-493 micro-column in the presented work, by using cold vapour atomic absorption spectrometry. Selective and sequential elution with 0.1 molL(-1) HCl for methyl mercury and 2 molL(-1) HCl for mercury(II) were performed at the pH range of 2-6. Optimal analytical conditions including pH, amounts of biosorbent, sample volumes were investigated. The detection limits of the analytes were 2.5 ngL(-1) for Hg(II) and 1.7 ngL(-1) for methyl mercury. The capacity of biosorbent for mercury(II) and methyl mercury was 6.5 and 5.4 mgg(-1), respectively. The validation of the presented procedure is performed by the analysis of standard reference material. The speciation procedure established was successfully applied to the speciation of mercury(II) and methyl mercury in natural water and microwave digested fish samples.

Sensitive determination of polycyclic aromatic hydrocarbons in water samples by HPLC coupled with SPE based on graphene functionalized with triethoxysilane.

PubMed

Huang, Ke-Jing; Li, Jing; Liu, Yan-Ming; Wang, Lan

2013-02-01

The graphene functionalized with (3-aminopropyl) triethoxysilane was synthesized by a simple hydrothermal reaction and applied as SPE sorbents to extract trace polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. These sorbents possess high adsorption capacity and extraction efficiency due to strong adsorption ability of carbon materials and large specific surface area of nanoparticles, and only 10 mg of sorbents are required to extract PAHs from 100 mL water samples. Several condition parameters, such as eluent and its volume, adsorbent amount, sample volume, sample pH, and sample flow rate, were optimized to achieve good sensitivity and precision. Under the optimized extraction conditions, the method showed good linearity in the range of 1-100 μg/L, repeatability of the extraction (the RSDs were between 1.8 and 2.9%, n = 6), and satisfactory detection limits of 0.029-0.1 μg/L. The recoveries of PAHs spiked in environmental water samples ranged from 84.6 to 109.5%. All these results demonstrated that this new SPE technique was a viable alternative to conventional enrichment techniques for the extraction and analysis of PAHs in complex samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Detachable strong cation exchange monolith, integrated with capillary zone electrophoresis and coupled with pH gradient elution, produces improved sensitivity and numbers of peptide identifications during bottom-up analysis of complex proteomes.

PubMed

Zhang, Zhenbin; Yan, Xiaojing; Sun, Liangliang; Zhu, Guijie; Dovichi, Norman J

2015-04-21

A detachable sulfonate-silica hybrid strong cation-exchange monolith was synthesized in a fused silica capillary, and used for solid phase extraction with online pH gradient elution during capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) proteomic analysis. Tryptic digests were prepared in 50 mM formic acid and loaded onto the strong cation-exchange monolith. Fractions were eluted using a series of buffers with lower concentration but higher pH values than the 50 mM formic acid background electrolyte. This combination of elution and background electrolytes results in both sample stacking and formation of a dynamic pH junction and allows use of relatively large elution buffer volumes while maintaining reasonable peak efficiency and resolution. A series of five pH bumps were applied to elute E. coli tryptic peptides from the monolith, followed by analysis using CZE coupled to an LTQ-Orbitrap Velos mass spectrometer; 799 protein groups and 3381 peptides were identified from 50 ng of the digest in a 2.5 h analysis, which approaches the identification rate for this organism that was obtained with an Orbitrap Fusion. We attribute the improved numbers of peptide and protein identifications to the efficient fractionation by the online pH gradient elution, which decreased the complexity of the sample in each elution step and improved the signal intensity of low abundance peptides. We also performed a comparative analysis using a nanoACQUITY UltraPerformance LCH system. Similar numbers of protein and peptide identifications were produced by the two methods. Protein identifications showed significant overlap between the two methods, whereas peptide identifications were complementary.

[Determination of four phenolic endocrine disruptors in environmental water samples by high performance liquid chromatography-fluorescence detection using dispersive liquid-liquid microextraction coupled with derivatization].

PubMed

Wang, Xiaoyan; Qi, Weimei; Zhao, Xian'en; Lü, Tao; Wang, Xiya; Zheng, Longfang; Yan, Yehao; You, Jinmao

2014-06-01

To achieve accurate, fast and sensitive detection of phenolic endocrine disruptors in small volume of environmental water samples, a method of dispersive liquid-liquid microextraction (DLLME) coupled with fluorescent derivatization was developed for the determination of bisphenol A, nonylphenol, octylphenol and 4-tert-octylphenol in environmental water samples by high performance liquid chromatography-fluorescence detection (HPLC-FLD). The DLLME and derivatization conditions were investigated, and the optimized DLLME conditions for small volume of environmental water samples (pH 4.0) at room temperature were as follows: 70 microL chloroform as extraction solvent, 400 microL acetonitrile as dispersing solvent, vortex mixing for 3 min, and then high-speed centrifugation for 2 min. Using 2-[2-(7H-dibenzo [a, g] carbazol-7-yl)-ethoxy] ethyl chloroformate (DBCEC-Cl) as precolumn derivatization reagent, the stable derivatives of the four phenolic endocrine disruptors were obtained in pH 10.5 Na2CO3-NaHCO3 buffer/acetonitrile at 50 degrees C for 3 min, and then separated within 10 min by HPLC-FLD. The limits of detection (LODs) were in the range of 0.9-1.6 ng/L, and the limits of quantification (LOQs) were in the range of 3.8-7.1 ng/L. This method had perfect linearity, precision and recovery results, and showed obvious advantages and practicality comparing to the previously reported methods. It is a convenient and validated method for the routine analysis of phenolic endocrine disruptors in waste water of paper mill, lake water, domestic wastewater, tap water, etc.

Gas-water-rock interactions in Frio Formation following CO2 injection: Implications for the storage of greenhouse gases in sedimentary basins

USGS Publications Warehouse

Kharaka, Yousif K.; Cole, David R.; Hovorka, Susan D.; Gunter, W.D.; Knauss, Kevin G.; Freifeild, Barry M.

2006-01-01

To investigate the potential for the geologic storage of CO2 in saline sedimentary aquifers, 1600 t of CO2 were injected at 1500 m depth into a 24-m-thick sandstone section of the Frio Formation, a regional brine and oil reservoir in the U.S. Gulf Coast. Fluid samples obtained from the injection and observation wells before CO2 injection showed a Na-Ca-Cl–type brine with 93,000 mg/L total dissolved solids (TDS) at near saturation with CH4 at reservoir conditions. Following CO2 breakthrough, samples showed sharp drops in pH (6.5–5.7), pronounced increases in alkalinity (100–3000 mg/L as HCO3) and Fe (30–1100 mg/L), and significant shifts in the isotopic compositions of H2O, dissolved inorganic carbon (DIC), and CH4. Geochemical modeling indicates that brine pH would have dropped lower but for the buffering by dissolution of carbonate and iron oxyhydroxides. This rapid dissolution of carbonate and other minerals could ultimately create pathways in the rock seals or well cements for CO2 and brine leakage. Dissolution of minerals, especially iron oxyhydroxides, could mobilize toxic trace metals and, where residual oil or suitable organics are present, the injected CO2 could also mobilize toxic organic compounds. Environmental impacts could be major if large brine volumes with mobilized toxic metals and organics migrated into potable groundwater. The δ18O values for brine and CO2 samples indicate that supercritical CO2 comprises ∼50% of pore-fluid volume ∼6 mo after the end of injection. Postinjection sampling, coupled with geochemical modeling, indicates that the brine gradually will return to its preinjection composition.

Sea water acidification affects osmotic swelling, regulatory volume decrease and discharge in nematocytes of the jellyfish Pelagia noctiluca.

PubMed

Morabito, Rossana; Marino, Angela; Lauf, Peter K; Adragna, Norma C; La Spada, Giuseppa

2013-01-01

Increased acidification/PCO2 of sea water is a threat to the environment and affects the homeostasis of marine animals. In this study, the effect of sea water pH changes on the osmotic phase (OP), regulatory volume decrease (RVD) and discharge of the jellyfish Pelagia noctiluca (Cnidaria, Scyphozoa) nematocytes, collected from the Strait of Messina (Italy), was assessed. Isolated nematocytes, suspended in artificial sea water (ASW) with pH 7.65, 6.5 and 4.5, were exposed to hyposmotic ASW of the same pH values and their osmotic response and RVD measured optically in a special flow through chamber. Nematocyte discharge was analyzed in situ in ASW at all three pH values. At normal pH (7.65), nematocytes subjected to hyposmotic shock first expanded osmotically and then regulated their cell volume within 15 min. Exposure to hyposmotic ASW pH 6.5 and 4.5 compromised the OP and reduced or totally abrogated the ensuing RVD, respectively. Acidic pH also significantly reduced the nematocyte discharge response. Data indicate that the homeostasis and function of Cnidarians may be altered by environmental changes such as sea water acidification, thereby validating their use as novel bioindicators for the quality of the marine environment. © 2014 S. Karger AG, Basel.

Common Loon (Gavia immer) eggshell thickness and egg volume vary with acidity of nest lake in northern Wisconsin

USGS Publications Warehouse

Pollentier, C.D.; Kenow, K.P.; Meyer, M.W.

2007-01-01

Environmental acidification has been associated with factors that may negatively affect reproduction in many waterbirds. Declines in lake pH can lead to reductions in food availability and quality, or result in the altered availability of toxic metals, such as mercury. A recent laboratory study conducted by the U.S. Geological Survey and the Wisconsin Department of Natural Resources indicated that Common Loon (Gavia immer) chicks hatched from eggs collected on acidic lakes in northern Wisconsin may be less responsive to stimuli and exhibit reduced growth compared to chicks from neutral-pH lakes. Here we report on the relation between Common Loon egg characteristics (eggshell thickness and egg volume) and lake pH, as well as eggshell methylmercury content. Eggs (N = 84) and lake pH measurements were obtained from a four county region of northern Wisconsin. Egg-shells were 3-4% thinner on lakes with pH ??? 6.3 than on neutral-pH lakes and this relation was linear across the pH range investigated (P 0.05, n.s.) or lake pH. Results suggest that low lake pH may be associated with thinner eggshells and reduced egg volume in Common Loons. We speculate on the mechanisms that may lead to this phenomeno.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nigro, Valentina, E-mail: nigro@fis.uniroma3.it; Bruni, Fabio; Ricci, Maria Antonietta

The temperature dependence of the local intra-particle structure of colloidal microgel particles, composed of interpenetrated polymer networks, has been investigated by small-angle neutron scattering at different pH and concentrations, in the range (299÷315) K, where a volume phase transition from a swollen to a shrunken state takes place. Data are well described by a theoretical model that takes into account the presence of both interpenetrated polymer networks and cross-linkers. Two different behaviors are found across the volume phase transition. At neutral pH and T ≈ 307 K, a sharp change of the local structure from a water rich open inhomogeneousmore » interpenetrated polymer network to a homogeneous porous solid-like structure after expelling water is observed. Differently, at acidic pH, the local structure changes almost continuously. These findings demonstrate that a fine control of the pH of the system allows to tune the sharpness of the volume-phase transition.« less

[Determination of migration of 25 primary aromatic amines from food contact plastic materials by gas chromatography-mass spectrometry].

PubMed

Li, Ying; Li, Chengfa; Xiao, Daoqing; Liang, Feng; Chen, Zhinan; Schen, Xuhui; Sun, Xiaoying; Li, Yongtao

2013-01-01

A solid phase extraction (SPE) combination with gas chromatography-mass spectrometry (GC-MS) was developed for the determination of the migration of 25 primary aromatic amines (PAAs) from food contact plastic materials and articles. The samples were extracted by deionized water and 30 g/L acetic acid, and the pH value of the solution was adjusted to 8 - 10 with ammonia. The extracts were cleaned up and concentrated on an SPE column, then eluted by equal volume of methyl-tert-butyl ether and ethanol. The analysis of the target compounds was performed by GC-MS. The results indicated that the limits of detection were in the range of 0.4 -2.0 microg/kg for different PAAs. The recoveries and relative standard deviations (n = 7) of 10 microg/kg PAAs ranged from 51.6% -118.4% and 0.5% -9.8%, respectively, except the 2,4-diaminoanisole in the acid simulant. The effects of different experimental conditions such as the pH value and volume ratio of methyl-tert-butyl ether and ethanol were studied. The results showed that the method is accurate and stable, and could meet the requirement of the European Commission Regulation (EU) No 10/2011 for the determination of primary aromatic amines. It can be applied in the analysis of the primary aromatic amines in real food contact plastic material and article samples.

Effect of modified atmosphere packaging on the course of physical and chemical changes in chilled muscle tissue of silver carp (Hypophthalmichthys molitrix, V.).

PubMed

Jezek, F; Buchtová, H

2012-01-01

The effect of two types of modified atmosphere (MA1: 69% N2, 25% CO2, 5% O2, 1% CO; MA2: 70% N2, 30% CO2) on changes in physical and chemical parameters (pH, a(w)--water activity, TVBN - total volatile basic nitrogen, TMA - trimethylamine, FFA - free fatty acids, PV - peroxide value, TBA--thiobarbituric acid) in muscle tissues of the silver carp was monitored in the study. The samples were stored at temperatures +2 +/- 2 degrees C for 18 days. Changes in gas volumes (CO2 and O2) in MAs were also monitored. CO2 levels increased in MA1 but decreased in MA2. At the end of 18 days of storage, a significantly (P < 0.01) lower water activity (a(w)) levels were found in samples packaged under MA1, in contrast to samples packaged under MA2 where water activity values showed considerable fluctuation. Variations in pH values in the two types of MA showed similar trends. Sample pH gradually decreased until day 9 of storage. On day 11, muscle tissue pH increased markedly and then began to decrease again. The overall decrease in pH values was more profound in samples packaged under MA1. TVBN and TMA levels in samples packaged under the two types of MAs remained almost identical until day 9 of the experiment. Later, however, significantly (P < 0.01) higher levels of both parameters were found in muscle tissues packaged under MA1. FFA concentrations in silver carp samples in MA1 were significantly lower (P < 0.01) throughout the experiment. The PV increased significantly in both muscle samples tested. Greater fluctuations in this parameter's values throughout the experiment were observed in samples packaged under MA2. Faster rates of oxidation (P < 0.01) were found in samples packaged under MA1 starting on day 9. Maximum TBA values in MA1 and MA2 were observed on days 14 and 18 of the experiment, respectively. From the course of proteolytic and oxidative changes point of view, the more appropriate combination of gases for silver carp storage seems to be the mixture of 70% N2 and 30% CO2 (MA2), which allows for muscle storage of up to 9 days. We recommend TVBN as a suitable indicator of freshness, and TBA assay as a suitable indicator of the extent of oxidative processes.

Salting-out assisted liquid-liquid extraction with the aid of experimental design for determination of benzimidazole fungicides in high salinity samples by high-performance liquid chromatography.

PubMed

Wen, Yingying; Li, Jinhua; Yang, Fangfang; Zhang, Weiwei; Li, Weiran; Liao, Chunyang; Chen, Lingxin

2013-03-15

A novel method for the simultaneous separation and determination of four benzimidazole fungicides (i.e., carbendazim, fuberidazole, thiophanate-methyl and thiophanate) in high salinity samples was developed by using salting-out assisted liquid-liquid extraction (SALLE) via water-miscible acetonitrile as the extractant coupled with high-performance liquid chromatography. Box-Behnken design and response surface were employed to assist the optimization of SALLE conditions, including volume of salting-out solvent, the pH of sample solution and salting-out solvent as variable factors. The optimal salting-out parameters were obtained as follows: 2 mL of acetonitrile was added to 2 mL of sample solution with pH=4 and then 2 mL salting-out solvent containing 5 mol L(-1) sodium chloride at a pH of 7 was added to the solution for extraction. This procedure afforded a convenient and cost-saving operation with good cleanup ability for the benzimidazole fungicides, such as good linear relationships (R>0.996) between peak area and concentration from 2.5 ng mL(-1) to 500 ng mL(-1), low limits of detection between 0.14 ng mL(-1) and 0.38 ng mL(-1) and the intra-day precisions of retention time below 1.0%. The method recoveries obtained at fortified three concentrations for three seawater samples ranged from 60.4% to 99.1%. The simple, rapid and eco-benign SALLE based method proved potentially applicable for trace benzimidazole fungicides analysis in high salinity samples. Copyright © 2012 Elsevier B.V. All rights reserved.

The effect of pre-anaesthetic fasting time and type of food on gastric content volume and acidity in dogs.

PubMed

Savvas, Ioannis; Rallis, Timoleon; Raptopoulos, Dimitris

2009-11-01

To investigate the effect of pre-anaesthetic fasting time and variety of food on gastric content (GC) volume and pH in dogs. Randomized, cross-over, prospective experimental study. Fifteen mongrel dogs (nine females and six males 1-4 years old, weighing 10-24.5 kg). Each dog received the same seven treatments in random order: dry food 3 hours before anaesthesia (BA) (treatment 3D), canned food (half daily rate) 3 hours BA (treatment 3C), 0% fat cow milk 3 hours BA (treatment 3M), dry food 10 hours BA (treatment 10D), canned food 10 hours BA (treatment 10C), low fat canned food 10 hours BA (treatment 10F) and low protein canned food 10 hours BA (treatment 10P). All animals were pre-medicated with propionyl promazine and anaesthesia was induced with thiopental sodium and maintained with halothane. GC was aspirated using an orogastric catheter and its volume and pH were measured. Treatment 10F had significantly lower GC pH than all the 3-hour treatments. Treatments 10D and 10P had significantly lower pH than treatments 3D and 3C. Treatment 3M had significantly lower pH than the other 3-hour treatments. Treatment 3D had significantly greater gastric volume than treatments 3M, 10C, 10F and 10P. Canned food at half the daily rate administered 3 hours before anaesthesia did not increase significantly the GC volume compared to the other types of food used. The GC pH was also high. This type of food fed 3 hours before induction of anaesthesia may be of benefit in reduction of the incidence of gastro-oesophageal reflux during anaesthesia in dogs.

Adsorption of dyes by ACs prepared from waste tyre reinforcing fibre. Effect of texture, surface chemistry and pH.

PubMed

Acevedo, Beatriz; Rocha, Raquel P; Pereira, Manuel F R; Figueiredo, José L; Barriocanal, Carmen

2015-12-01

This paper compares the importance of the texture and surface chemistry of waste tyre activated carbons in the adsorption of commercial dyes. The adsorption of two commercial dyes, Basic Astrazon Yellow 7GLL and Reactive Rifafix Red 3BN on activated carbons made up of reinforcing fibres from tyre waste and low-rank bituminous coal was studied. The surface chemistry of activated carbons was modified by means of HCl-HNO3 treatment in order to increase the number of functional groups. Moreover, the influence of the pH on the process was also studied, this factor being of great importance due to the amphoteric characteristics of activated carbons. The activated carbons made with reinforcing fibre and coal had the highest SBET, but the reinforcing fibre activated carbon samples had the highest mesopore volume. The texture of the activated carbons was not modified upon acid oxidation treatment, unlike their surface chemistry which underwent considerable modification. The activated carbons made with a mixture of reinforcing fibre and coal experienced the largest degree of oxidation, and so had more acid surface groups. The adsorption of reactive dye was governed by the mesoporous volume, whilst surface chemistry played only a secondary role. However, the surface chemistry of the activated carbons and dispersive interactions played a key role in the adsorption of the basic dye. The adsorption of the reactive dye was more favored in a solution of pH 2, whereas the basic dye was adsorbed more easily in a solution of pH 12. Copyright © 2015 Elsevier Inc. All rights reserved.

Solid-phase extraction and separation procedure for trace aluminum in water samples and its determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS).

PubMed

Ciftci, Harun; Er, Cigdem

2013-03-01

In the present study, a separation/preconcentration procedure for determination of aluminum in water samples has been developed by using a new atomic absorption spectrometer concept with a high-intensity xenon short-arc lamp as continuum radiation source, a high-resolution double-echelle monochromator, and a charge-coupled device array detector. Sample solution pH, sample volume, flow rate of sample solution, volume, and concentration of eluent for solid-phase extraction of Al chelates with 4-[(dicyanomethyl)diazenyl] benzoic acid on polymeric resin (Duolite XAD-761) have been investigated. The adsorbed aluminum on resin was eluted with 5 mL of 2 mol L(-1) HNO(3) and its concentration was determined by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). Under the optimal conditions, limit of detection obtained with HR-CS FAAS and Line Source FAAS (LS-FAAS) were 0.49 μg L(-1) and 3.91 μg L(-1), respectively. The accuracy of the procedure was confirmed by analyzing certified materials (NIST SRM 1643e, Trace elements in water) and spiked real samples. The developed procedure was successfully applied to water samples.

Polyaniline-coated cigarette filters as a solid-phase extraction sorbent for the extraction and enrichment of polycyclic aromatic hydrocarbon in water samples.

PubMed

Bunkoed, Opas; Rueankaew, Thanaschaphorn; Nurerk, Piyaluk; Kanatharana, Proespichaya

2016-06-01

Polyaniline coated cigarette filters were successfully synthesized and used as a solid-phase extraction sorbent for the extraction and preconcentration of polycyclic aromatic hydrocarbons in water samples. The polyaniline helped to enhance the adsorption ability of polycyclic aromatic hydrocarbons on the sorbent through π-π interactions. The high porosity and large surface area of the cigarette filters helped to reduce backpressure and can be operated with high sample flow rate without loss of extraction efficiency. The developed sorbent was characterized by Fourier transform infrared spectroscopy and scanning electron microscopy. The parameters that affected the extraction efficiencies, i.e. polymerization time, type of desorption solvent and its volume, sample flow rate, sample volume, sample pH, ionic strength, and organic modifier were investigated. Under the optimal conditions, the method was linear over the range of 0.5-10 μg/L and a detection limit of 0.5 ng/L. This simple, rapid, and cost-effective method was successfully applied to the preconcentration of polycyclic aromatic hydrocarbons from water samples. The developed method provided a high enrichment factor with good extraction efficiency (85-98%) and a relative standard deviation <10%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An optimized procedure for preconcentration, determination and on-line recovery of palladium using highly selective diphenyldiketone-monothiosemicarbazone modified silica gel.

PubMed

Sharma, R K; Pandey, Amit; Gulati, Shikha; Adholeya, Alok

2012-03-30

A novel, highly selective, efficient and reusable chelating resin, diphenyldiketone-monothiosemicarbazone modified silica gel, was prepared and applied for the on-line separation and preconcentration of Pd(II) ions in catalytic converter and spiked tap water samples. Several parameters like effect of pH, sample volume, flow rate, type of eluent, and influence of various ionic interferences, etc. were evaluated for effective adsorption of palladium at trace levels. The resin was found to be highly selective for Pd(II) ions in the pH range 4-5 with a very high sorption capacity of 0.73 mmol/g and preconcentration factor of 335. The present environment friendly procedure has also been applied for large-scale extraction by employing the use of newly designed reactor in which on-line separation and preconcentration of Pd can be carried out easily and efficiently in short duration of time. Copyright © 2012 Elsevier B.V. All rights reserved.

Separation and Enrichment of Gold in Water, Geological and Environmental Samples by Solid Phase Extraction on Multiwalled Carbon Nanotubes Prior to its Determination by Flame Atomic Absorption Spectrometry.

PubMed

Duran, Ali; Tuzen, Mustafa; Soylak, Mustafa

2015-01-01

This study proposes the application of multi-walled carbon nanotubes as a solid sorbent for the preconcentration of gold prior to its flame atomic absorption spectrometry determination. Extraction was achieved by using a glass column (15.0 cm in length and 1.0 cm in diameter). Quantitative recoveries were obtained in the pH range of 2.5-4.0; the elution step was carried out with 5.0 ml of 1.0 mol/L HNO3 in acetone. In the ligand-free study, variables such as pH, eluent type, sample volume, flow rates, and matrix effect were examined for the optimum recovery of gold ions. The gold ions were able to be pre-concentrated by a factor of 150 and their LOD was determined to be 1.71 μg/L. In order to evaluate the accuracy of the developed method, addition-recovery tests were applied for the tap water, mineral water, and sea water samples. Gold recovery studies were implemented using a wet digestion technique for mine and soil samples taken from various media, and this method was also applied for anodic slime samples taken from the factories located in the Kayseri Industrial Zone of Turkey.

Clinically significant change in stroke volume in pulmonary hypertension.

PubMed

van Wolferen, Serge A; van de Veerdonk, Marielle C; Mauritz, Gert-Jan; Jacobs, Wouter; Marcus, J Tim; Marques, Koen M J; Bronzwaer, Jean G F; Heymans, Martijn W; Boonstra, Anco; Postmus, Pieter E; Westerhof, Nico; Vonk Noordegraaf, Anton

2011-05-01

Stroke volume is probably the best hemodynamic parameter because it reflects therapeutic changes and contains prognostic information in pulmonary hypertension (PH). Stroke volume directly reflects right ventricular function in response to its load, without the correction of compensatory increased heart rate as is the case for cardiac output. For this reason, stroke volume, which can be measured noninvasively, is an important hemodynamic parameter to monitor during treatment. However, the extent of change in stroke volume that constitutes a clinically significant change is unknown. The aim of this study was to determine the minimal important difference (MID) in stroke volume in PH. One hundred eleven patients were evaluated at baseline and after 1 year of follow-up with a 6-min walk test (6MWT) and cardiac MRI. Using the anchor-based method with 6MWT as the anchor, and the distribution-based method, the MID of stroke volume change could be determined. After 1 year of treatment, there was, on average, a significant increase in stroke volume and 6MWT. The change in stroke volume was related to the change in 6MWT. Using the anchor-based method, an MID of 10 mL in stroke volume was calculated. The distribution-based method resulted in an MID of 8 to 12 mL. Both methods showed that a 10-mL change in stroke volume during follow-up should be considered as clinically relevant. This value can be used to interpret changes in stroke volume during clinical follow-up in PH.

Recombinant human hyaluronidase PH20 (rHuPH20) facilitates subcutaneous infusions of large volumes of immunoglobulin in a swine model.

PubMed

Kang, David W; Jadin, Laurence; Nekoroski, Tara; Drake, Fred H; Zepeda, Monica L

2012-08-01

Many patients with primary immunodeficiency disease (PIDD) require lifelong immunoglobulin (Ig) replacement therapy. Home-based subcutaneous (SC) infusion provides advantages to patients with PIDD compared to hospital-based intravenous infusion. One limitation of current practice with SCIg infusion is the need for small-volume infusions at multiple injection sites on a frequent basis. A method was developed for large-volume SC infusion that uses preinfusion of recombinant human hyaluronidase (rHuPH20) to facilitate fluid dispersion. Miniature swine was used as a preclinical model to assess the effects of rHuPH20-facilitated infusions, of a single monthly dose, on fluid dispersion, infusion-related pressure, swelling, induration, and tissue damage. Preinfusion of vehicle (control) or rHuPH20 (75 U/g Ig) was performed simultaneously on contralateral abdominal sites on each animal, followed by infusion of 300 mL 10 % Ig (30 g) at each site. Compared to control infusions, rHuPH20 significantly reduced infusion pressure and induration (p < 0.05) and accelerated postinfusion Ig dispersion. Histological evaluation of infusion site tissue showed moderate to severe swelling for the control. Swelling after rHuPH20-facilitated infusion was mild on day 1 and had completely resolved shortly thereafter. Laser Doppler imaging of control infusion sites revealed local cutaneous hypoperfusion during Ig infusion, which was reduced almost 7-fold (p < 0.05) with the use of rHuPH20. These results demonstrate that rHuPH20-facilitated Ig infusion is associated with improved dispersion of Ig, resulting in reduced tissue pressure, induration, and reduced risk of tissue damage from mechanical trauma or local ischemia, thus enabling SC administration of large volumes of Ig at a single site.

Comparison of the effects of intravenous administration of isotonic and hypertonic sodium bicarbonate solutions on venous acid-base status in dehydrated calves with strong ion acidosis.

PubMed

Coskun, Alparslan; Sen, Ismail; Guzelbektes, Hasan; Ok, Mahmut; Turgut, Kursat; Canikli, Sebnem

2010-05-15

OBJECTIVE-To compare the effects of IV administration of isotonic (1.3%) and hypertonic (8.4%) sodium bicarbonate (NaHCO(3)) solutions on acid-base status in dehydrated calves with strong ion (metabolic) acidosis. DESIGN-Randomized controlled clinical trial. ANIMALS-50 calves with diarrhea and severe dehydration. PROCEDURES-Calves were randomly assigned to receive isotonic NaHCO(3) solution (65 mL/kg [29.5 mL/lb], IV) over 3 hours (n = 30) or hypertonic NaHCO(3) solution (10 mL/kg [4.5 mL/lb], IV) over 20 minutes (20). Blood samples were collected at 0 hours (immediately prior to solution administration) and at 0.5, 1, 2, and 4 hours after administration began. Samples were submitted for blood gas analysis, serum biochemical analysis, and determination of blood Na(+), K(+), and Cl(-) concentrations and percentage change in plasma volume. RESULTS-Calves that received isotonic NaHCO(3) solution had an increase in venous blood pH, HCO(3) concentration, and base excess; a small, transient increase in Po(2); and no change in Pco(2) within 4 hours after administration began. Calves that received hypertonic NaHCO(3) solution had an immediate increase in venous blood pH, HCO(3) concentration, and base excess; a small, transient increase Pco(2); and no change in Po(2) within 0.5 hours after treatment began. Plasma volume increased to a greater extent following administration of isotonic solution than after administration of hypertonic solution. CONCLUSIONS AND CLINICAL RELEVANCE-IV administration of 8.4% NaHCO(3) solution in small volumes provided fast and effective improvement of severe acid-base abnormalities in calves with severe strong ion acidosis but did not improve hydration status as well as administration of a larger volume of isotonic NaHCO(3) solution.

Carbon dioxide sequestration in municipal solid waste incinerator (MSWI) bottom ash.

PubMed

Rendek, Eva; Ducom, Gaëlle; Germain, Patrick

2006-01-16

During bottom ash weathering, carbonation under atmospheric conditions induces physico-chemical evolutions leading to the pacification of the material. Fresh bottom ash samples were subjected to an accelerated carbonation using pure CO2. The aim of this work was to quantify the volume of CO2 that could be sequestrated with a view to reduce greenhouse gas emissions and investigate the possibility of upgrading some specific properties of the material with accelerated carbonation. Carbonation was performed by putting 4mm-sieved samples in a CO2 chamber. The CO2 pressure and the humidity of the samples were varied to optimize the reaction parameters. Unsieved material was also tested. Calcite formation resulting from accelerated carbonation was investigated by thermogravimetry and differential scanning calorimetry (TG/DSC) and metal leaching tests were performed. The volume of sequestrated CO2 was on average 12.5L/kg dry matter (DM) for unsieved material and 24 L/kg DM for 4mm-sieved samples. An ash humidity of 15% appeared to give the best results. The reaction was drastically accelerated at high pressure but it did not increase the volume of sequestrated CO2. Accelerated carbonation, like the natural phenomenon, reduces the dangerous nature of the material. It decreases the pH from 11.8 to 8.2 and causes Pb, Cr and Cd leaching to decrease. This process could reduce incinerator CO2 emissions by 0.5-1%.

Rapid analysis of aflatoxins B1, B2, and ochratoxin A in rice samples using dispersive liquid-liquid microextraction combined with HPLC.

PubMed

Lai, Xian-Wen; Sun, Dai-Li; Ruan, Chun-Qiang; Zhang, He; Liu, Cheng-Lan

2014-01-01

A novel, simple, and rapid method is presented for the analysis of aflatoxin B1, aflatoxin B2, and ochratoxin A in rice samples by dispersive liquid-liquid microextraction combined with LC and fluorescence detection. After extraction of the rice samples with a mixture of acetonitrile/water/acetic acid, mycotoxins were rapidly partitioned into a small volume of organic solvent (chloroform) by dispersive liquid-liquid microextraction. The three mycotoxins were simultaneously determined by LC with fluorescence detection after precolumn derivatization for aflatoxin B1 and B2. Parameters affecting both extraction and dispersive liquid-liquid microextraction procedures, including the extraction solvent, the type and volume of extractant, the volume of dispersive solvent, the addition of salt, the pH and the extraction time, were optimized. The optimized protocol provided an enrichment factor of approximately 1.25 and with detection of limits (0.06-0.5 μg/kg) below the maximum levels imposed by current regulations for aflatoxins and ochratoxin A. The mean recovery of three mycotoxins ranged from 82.9-112%, with a RSD less than 7.9% in all cases. The method was successfully applied to measure mycotoxins in commercial rice samples collected from local supermarkets in China. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effects of moisture content and initial pH in composting process on heavy metal removal characteristics of grass clipping compost used for stormwater filtration.

PubMed

Khan, Eakalak; Khaodhir, Sutha; Ruangrote, Darin

2009-10-01

Heavy metals are common contaminants in stormwater runoff. One of the devices that can be used to effectively and economically remove heavy metals from runoff is a yard waste compost stormwater filter. The primary goal of composting is to reduce waste volume rather than to produce stormwater filter media. Moisture content (MC) and initial pH, the two important parameters in composting, were studied for their effects on yard waste volume reduction and heavy metal adsorption performances of the compost. The main objective of this investigation was to examine whether the conditions that provided high yard waste volume reduction would also result in compost with good heavy metal removal performances. Manila grass was composted at different initial pHs (5-9) and MCs (30-70%) and the composts were used to adsorb cadmium, copper, lead and zinc from water. Results indicated that MC is more critical than initial pH for both volume reduction and production of compost with high metal adsorption performances. The most optimal conditions for the two attributes were not exactly the same but lower MCs of 30-40% and pH 7 or higher tended to satisfy both high volume reduction and effective metal adsorption.

Copper(II)-rubeanic acid coprecipitation system for separation-preconcentration of trace metal ions in environmental samples for their flame atomic absorption spectrometric determinations.

PubMed

Soylak, Mustafa; Erdogan, Nilgun D

2006-09-21

A simple and facile preconcentration procedure based on the coprecipitation of trace heavy metal ions with copper(II)-rubeanic acid complex has been developed. The analytical parameters including pH, amounts of rubeanic acid, sample volume, etc. was investigated for the quantitative recoveries of Pb(II), Fe(III), Cd(II), Au(III), Pd(II) and Ni(II). No interferic effects were observed from the concomitant ions. The detection limits for analyte ions by 3 sigma were in the range of 0.14 microg/l for iron-3.4 microg/l for lead. The proposed coprecipitation method was successfully applied to water samples from Palas Lake-Kayseri, soil and sediment samples from Kayseri and Yozgat-Turkey.

Analysis of plant hormones by microemulsion electrokinetic capillary chromatography coupled with on-line large volume sample stacking.

PubMed

Chen, Zongbao; Lin, Zian; Zhang, Lin; Cai, Yan; Zhang, Lan

2012-04-07

A novel method of microemulsion electrokinetic capillary chromatography (MEEKC) coupled with on-line large volume sample stacking was developed for the analysis of six plant hormones including indole-3-acetic acid, indole-3-butyric acid, indole-3-propionic acid, 1-naphthaleneacetic acid, abscisic acid and salicylic acid. Baseline separation of six plant hormones was achieved within 10 min by using the microemulsion background electrolyte containing a 97.2% (w/w) 10 mM borate buffer at pH 9.2, 1.0% (w/w) ethyl acetate as oil droplets, 0.6% (w/w) sodium dodecyl sulphate as surfactant and 1.2% (w/w) 1-butanol as cosurfactant. In addition, an on-line concentration method based on a large volume sample stacking technique and multiple wavelength detection was adopted for improving the detection sensitivity in order to determine trace level hormones in a real sample. The optimal method provided about 50-100 fold increase in detection sensitivity compared with a single MEEKC method, and the detection limits (S/N = 3) were between 0.005 and 0.02 μg mL(-1). The proposed method was simple, rapid and sensitive and could be applied to the determination of six plant hormones in spiked water samples, tobacco leaves and 1-naphthylacetic acid in leaf fertilizer. The recoveries ranged from 76.0% to 119.1%, and good reproducibilities were obtained with relative standard deviations (RSDs) less than 6.6%.

Electrochemical Detection of Multiple Bioprocess Analytes

NASA Technical Reports Server (NTRS)

Rauh, R. David

2010-01-01

An apparatus that includes highly miniaturized thin-film electrochemical sensor array has been demonstrated as a prototype of instruments for simultaneous detection of multiple substances of interest (analytes) and measurement of acidity or alkalinity in bioprocess streams. Measurements of pH and of concentrations of nutrients and wastes in cell-culture media, made by use of these instruments, are to be used as feedback for optimizing the growth of cells or the production of desired substances by the cultured cells. The apparatus is designed to utilize samples of minimal volume so as to minimize any perturbation of monitored processes. The apparatus can function in a potentiometric mode (for measuring pH), an amperometric mode (detecting analytes via oxidation/reduction reactions), or both. The sensor array is planar and includes multiple thin-film microelectrodes covered with hydrous iridium oxide. The oxide layer on each electrode serves as both a protective and electrochemical transducing layer. In its transducing role, the oxide provides electrical conductivity for amperometric measurement or pH response for potentiometric measurement. The oxide on an electrode can also serve as a matrix for one or more enzymes that render the electrode sensitive to a specific analyte. In addition to transducing electrodes, the array includes electrodes for potential control. The array can be fabricated by techniques familiar to the microelectronics industry. The sensor array is housed in a thin-film liquid-flow cell that has a total volume of about 100 mL. The flow cell is connected to a computer-controlled subsystem that periodically draws samples from the bioprocess stream to be monitored. Before entering the cell, each 100-mL sample is subjected to tangential-flow filtration to remove particles. In the present version of the apparatus, the electrodes are operated under control by a potentiostat and are used to simultaneously measure the pH and the concentration of glucose. It is anticipated that development of procedures for trapping more enzymes into hydrous iridium oxide (and possibly into other electroactive metal oxides) and of means for imparting long-term stability to the transducer layers should make it possible to monitor concentrations of products of many enzyme reactions for example, such key bioprocess analytes as amino acids, vitamins, lactose, and acetate.

Epinigericin toxicity towards Tetrahymena pyriformis GL; changes in cell volume and intracellular pH.

PubMed

Bamdad, M; David, L; Grolière, C A

1995-12-01

A study of the toxicity of epinigericin, an antibiotic ionophor, towards the ciliate Tetrahymena pyriformis showed that this molecule stopped cell division, increased cell volume and led to a more basic intracellular pH. The action of epinigericin was probably linked to its function as an ionophor. The ionic selectivity of this molecule is still not known. The raising of the intracellular pH of ciliates by this antibiotic may be linked to its toxic action and its iontransport mechanism in Tetrahymena.

Physical-chemical characterization of the textile dye Azo Ab52 degradation by corona plasma

NASA Astrophysics Data System (ADS)

Gómez, A.; Torres-Arenas, A. J.; Vergara-Sánchez, J.; Torres, C.; Reyes, P. G.; Martínez, H.; Saldarriaga-Noreña, Hugo

2017-10-01

This work characterizes the degradation of the textile dye azo Acid Black 52 by measuring several physical and chemical parameters. A corona plasma was created at atmospheric pressure and applied on the liquid-air interface of water samples containing the dye. 1.0 mM of ferrous sulfate (FeSO4) was added to 1.0 mM dye solution, for a total volume of 250 mL. For each treatment, a number of parameters were quantified. These were voltage, current, temperature, loss of volume, pH, electrical conductivity, concentration, optical mission spectra, chemical oxygen demand (COD), total organic carbon (TOC), and the removal ratio. Because of the increase in the sample temperature, the volume lost by evaporation was explored. The results show that the efficiency of the dye degradation by plasma is a function of treatment time. Moreover, the reactive concentration of FeSO4 and the exposition time of the plasma were varied at a constant volume, leading to the determination of the concentrations and optimal times. Considering the degradation and removal parameters, at the maximum treated time of 80 min, it found that COD was of 96.36%, TOC of 93.93%, and the removal ratio of 97.47%.

Protein solubilities determined by a rapid technique and modification of that technique to a micro-method

NASA Technical Reports Server (NTRS)

Cacioppo, Elizabeth; Pusey, Marc Lee; Munson, Sibyl

1989-01-01

A simple, rapid method for determination of protein solubilities has been developed which is based upon maximization of the free solution volume to be brought into equilibrium. The tetragonal lysozome solubility diagram has been determined from pH 4.0 to 5.2 (0.1 M sodium acetate), 2-7 percent NaCl, 3-25 C, and portions of the orthorhombic solubility diagram using this technique. Both tetragonal and orthorhombic solubilities were found to increase smoothly with decreasing salt concentration and increasing temperature; no retrograde solubilities were observed. Using column volumes of 75, 300, and 900 microliters, identical tetragonal lysozyme solubility diagrams were obtained. Chymotrypsinogen solubilities have also been determined using this apparatus, being retrograde over the temperature range tested. It is noted that the primary limiting factor in reducing the crystalline volume is the minimum solution sample size needed to accurately quantitate the protein.

Interaction of Jet Fuel Hydrocarbon Components with Red Blood Cells and Hemoglobin

DTIC Science & Technology

2014-06-24

Directorate (RHDJ), Wright-Patterson AFB, OH. The authors would like to thank Maj. Paul Eden, Nicole Schaeublin, Christin Grabinski, Dr. Jeff Gearhart...We would also like to thank LtCol. Norman Fox (Laboratory Flight Commander), Mrs. Nersa Loh (Supervisor, Transfusion Services), and Mr. Dan Fischer ...Approximately 7.8 mg of hemoglobin sample was concentrated into a total volume of 5 mL of Fischer PBS pH 7.5 buffer using an Amicon Centrifugal Filter Unit

An on-line pre-concentration system for determination of cadmium in drinking water using FAAS.

PubMed

dos Santos, Walter N L; Costa, Jorge L O; Araujo, Rennan G O; de Jesus, Djane S; Costa, Antônio C S

2006-10-11

In the present paper, a minicolumn of polyurethane foam loaded with 4-(2-pyridylazo)-resorcinol (PAR) is proposed as pre-concentration system for cadmium determination in drinking water samples by flame atomic absorption spectrometry. The optimization step was performed using two-level full factorial design and Doehlert matrix, involving the variables: sampling flow rate, elution concentration, buffer concentration and pH. Using the established experimental conditions in the optimization step of: pH 8.2, sampling flow rate 8.5 mL min(-1), buffer concentration 0.05 mol L(-1) and elution concentration of 1.0 mol L(-1), this system allows the determination of cadmium with detection limit (LD) (3sigma/S) of 20.0 ng L(-1) and quantification limit (LQ) (10sigma/S) of 64 ng L(-1), precision expressed as relative standard deviation (R.S.D.) of 5.0 and 4.7% for cadmium concentration of 5.0 and 40.0 microg L(-1), respectively, and a pre-concentration factor of 158 for a sample volume of 20.0 mL. The accuracy was confirmed by cadmium determination in the standard reference material, NIST SRM 1643d trace elements in natural water. This procedure was applied for cadmium determination in drinking water samples collected from Salvador City, Bahia, Brazil. For five samples analyzed, the achieved concentrations varied from 0.31 to 0.86 microg L(-1).

Effect of transglutaminase on some properties of cake enriched with various protein sources.

PubMed

Alp, H; Bilgiçli, N

2008-06-01

The effect of transglutaminase (TG) enzyme addition (0% and 0.09%) on batter and cake properties, prepared with different protein sources (nonfat dry milk [NFDM], soy flour, and soymilk) and flour types (type A with 11.4% protein and type B with 8.6% protein), was investigated. Specific gravity and pH of cake batters were determined, and physical and chemical analysis of the cake samples was performed. Soy products improved cake weight, volume, softness, protein, and fat contents. NFDM increased the crust redness and crumb lightness more than the other protein sources. TG enzyme addition affected the volume, softness, crust, and crumb color of the cake samples significantly (P < 0.05). The combination of TG enzyme and flour B with lower protein gave more puffed, symmetrical, and softer cake samples. TG had a potential application with different protein sources in cake production. Especially interactions between TG with soy flour and TG and wheat flour with high protein content were important in cake formulations due to the softening effect on crumb.

Ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometric for selenium speciation in foods and beverages.

PubMed

Tuzen, Mustafa; Pekiner, Ozlem Zeynep

2015-12-01

A rapid and environmentally friendly ultrasound assisted ionic liquid dispersive liquid liquid microextraction (USA-IL-DLLME) was developed for the speciation of inorganic selenium in beverages and total selenium in food samples by using graphite furnace atomic absorption spectrometry. Some analytical parameters including pH, amount of complexing agent, extraction time, volume of ionic liquid, sample volume, etc. were optimized. Matrix effects were also investigated. Enhancement factor (EF) and limit of detection (LOD) for Se(IV) were found to be 150 and 12 ng L(-1), respectively. The relative standard deviation (RSD) was found 4.2%. The accuracy of the method was confirmed with analysis of LGC 6010 Hard drinking water and NIST SRM 1573a Tomato leaves standard reference materials. Optimized method was applied to ice tea, soda and mineral water for the speciation of Se(IV) and Se(VI) and some food samples including beer, cow's milk, red wine, mixed fruit juice, date, apple, orange, grapefruit, egg and honey for the determination of total selenium. Copyright © 2015 Elsevier Ltd. All rights reserved.

Hollow fiber supported ionic liquid membrane microextraction for determination of sulfonamides in environmental water samples by high-performance liquid chromatography.

PubMed

Tao, Yong; Liu, Jing-Fu; Hu, Xia-Lin; Li, Hong-Cheng; Wang, Thanh; Jiang, Gui-Bin

2009-08-28

By using ionic liquid as membrane liquid and tri-n-octylphosphine oxide (TOPO) as additive, hollow fiber supported liquid phase microextraction (HF-LPME) was developed for the determination of five sulfonamides in environmental water samples by high-performance liquid chromatography with ultraviolet detection The extraction solvent and the parameters affecting the extraction enrichment factor such as the type and amount of carrier, pH and volume ratio of donor phase and acceptor phase, extraction time, salt-out effect and matrix effect were optimized. Under the optimal extraction conditions (organic liquid membrane phase: [C(8)MIM][PF(6)] with 14% TOPO (w/v); donor phase: 4mL, pH 4.5 KH(2)PO(4) with 2M Na(2)SO(4); acceptor phase: 25microL, pH 13 NaOH; extraction time: 8 h), low detection limits (0.1-0.4microg/L, RSDor=0.999) were obtained for all the analytes. The presence of humic acid (0-25mg/L dissolved organic carbon) and bovine serum albumin (0-100microg/mL) had no significant effect on the extraction efficiency. Good spike recoveries over the range of 82.2-103.2% were obtained when applying the proposed method on five real environmental water samples. These results indicated that this present method was very sensitive and reliable with good repeatabilities and excellent clean-up in water samples. The proposed method confirmed hollow fiber supported ionic liquid membrane based LPME to be robust to monitoring trace levels of sulfadiazine, sulfamerazine, sulfamethazine, sulfadimethoxine and sulfamethoxazole in aqueous samples.

Enhancing concentration and mass sensitivities for liquid chromatography trace analysis of clopyralid in drinking water.

PubMed

Gu, Binghe; Meldrum, Brian; McCabe, Terry; Phillips, Scott

2012-01-01

A theoretical treatment was developed and validated that relates analyte concentration and mass sensitivities to injection volume, retention factor, particle diameter, column length, column inner diameter and detection wavelength in liquid chromatography, and sample volume and extracted volume in solid-phase extraction (SPE). The principles were applied to improve sensitivity for trace analysis of clopyralid in drinking water. It was demonstrated that a concentration limit of detection of 0.02 ppb (μg/L) for clopyralid could be achieved with the use of simple UV detection and 100 mL of a spiked drinking water sample. This enabled reliable quantitation of clopyralid at the targeted 0.1 ppb level. Using a buffered solution as the elution solvent (potassium acetate buffer, pH 4.5, containing 10% of methanol) in the SPE procedures was found superior to using 100% methanol, as it provided better extraction recovery (70-90%) and precision (5% for a concentration at 0.1 ppb level). In addition, the eluted sample was in a weaker solvent than the mobile phase, permitting the direct injection of the extracted sample, which enabled a faster cycle time of the overall analysis. Excluding the preparation of calibration standards, the analysis of a single sample, including acidification, extraction, elution and LC run, could be completed in 1 h. The method was used successfully for the determination of clopyralid in over 200 clopyralid monoethanolamine-fortified drinking water samples, which were treated with various water treatment resins. Copyright © 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim.

Combination of micelle collapse and field-amplified sample stacking in capillary electrophoresis for determination of trimethoprim and sulfamethoxazole in animal-originated foodstuffs.

PubMed

Liu, Lihong; Wan, Qian; Xu, Xiaoying; Duan, Shunshan; Yang, Chunli

2017-03-15

An on-line preconcentration method combining micelle to solvent stacking (MSS) with field-amplified sample stacking (FASS) was employed for the analysis of trimethoprim (TMP) and sulfamethoxazole (SMZ) by capillary zone electrophoresis (CZE). The optimized experimental conditions were as followings: (1) sample matrix, 10.0mM SDS-5% (v/v) methanol; (2) trapping solution (TS), 35mM H 3 PO 4 -60% acetonitrile (CH 3 CN); (3) running buffer, 30mM Na 2 HPO 4 (pH=7.3); (4) sample solution volume, 168nL; TS volume, 168nL; and (5) 9kV voltage, 214nm UV detection. Under the optimized conditions, the limits of detection (LODs) for SMZ and TMP were 7.7 and 8.5ng/mL, and they were 301 and 329 times better compared to a typical injection, respectively. The contents of TMP and SMZ in animal foodstuffs such as dairy products, eggs and honey were analyzed, too. Recoveries of 80-104% were acquired with relative standard deviations of 0.5-5.4%. Copyright © 2016 Elsevier Ltd. All rights reserved.

Ionic Liquid Dispersive Liquid-Liquid Microextraction Method for the Determination of Irinotecan, an Anticancer Drug, in Water and Urine Samples Using UV-Vis Spectrophotometry.

PubMed

Uysal, Deniz; Karadaş, Cennet; Kara, Derya

2017-05-01

A new, simple, efficient, and environmentally friendly ionic liquid dispersive liquid-liquid microextraction method was developed for the determination of irinotecan, an anticancer drug, in water and urine samples using UV-Vis spectrophotometry. The ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate was used as the extraction solvent, and ethanol was used as the disperser solvent. The main parameters affecting the extraction efficiency, including sample pH, volume of the ionic liquid, choice of the dispersive solvent and its volume, concentration of NaCl, and extraction and centrifugation times, were investigated and optimized. The effect of interfering species on the recovery of irinotecan was also examined. Under optimal conditions, the LOD (3σ) was 48.7 μg/L without any preconcentration. Because the urine sample was diluted 10-fold, the LOD for urine would be 487 μg/L. However, this could be improved 16-fold if preconcentration using a 40 mL aliquot of the sample is used. The proposed method was successfully applied to the determination of irinotecan in tap water, river water, and urine samples spiked with 10.20 mg/L for the water samples and 8.32 mg/L for the urine sample. The average recovery values of irinotecan determined were 99.1% for tap water, 109.4% for river water, and 96.1% for urine.

Muscle damage, hydration, electrolyte balance and vasopressin concentrations in successful and exhausted endurance horses.

PubMed

Muñoz, A; Riber, C; Trigo, P; Castejón, F

2010-01-01

Arginine vasopressin (AVP) is released in response to depletion of the effective circulating blood volume. Endurance horses might develop exhaustion because loss of water and electrolytes in sweat with hypovolaemia and electrolytes abnormalities. Therefore, AVP should act in the control of volemia in these animals. This research evaluates the differences in AVP, hydration, electrolyte status and serum muscle enzymes in successful endurance horses in comparison with those eliminated from the competition because of exhaustion. Eighteen endurance horses, divided into two groups, successful (n = 13) and eliminated at the vet-gates because of exhaustion, dehydration and/or lack of recovery of heart rate (n = 5), were studied during a competition of 76.2 km. Jugular venous blood samples were collected before the event (BF), and at the vet-gates, at 30 km (PH1), 53.6 km (PH2) and at the end (PH3). Endurance exercise in successful horses induced significant increases from BF in Na at PH1, in Mg, CK, LDH at PH2 and microhaematocrit (MHT), total serum proteins (TSP), albumin (ALB), creatinine (CREAT) and lactate (LA) at PH3, together with a decreased in Cl at PH2 and Ca at PH3. Exhausted horses had higher MHT, Na, Ca, TSP, CREAT, LA, and AVP than successful at PH2 and PH3, whereas Cl was lower in exhausted horses. Velocity during the ride was higher in the exhausted group. These results indicate that exhausted endurance horses have laboratorial findings corresponding with a deeper dehydration and increased release of AVP. Therefore, this parameter could be used as a biomarker of early exhaustion and hypovolaemia. Additionally, AVP does not appear to be affected by exercise velocity or covered distance in successful horses.

Pipette-tip solid-phase extraction using polypyrrole as efficient adsorbent for extraction of avermectins and milbemycins in milk.

PubMed

Florez, Diego Hernando Ângulo; Teixeira, Roseane Andrade; da Silva, Ricky Cássio Santos; Pires, Bruna Carneiro; Dutra, Flávia Viana Avelar; Borges, Keyller Bastos

2018-05-01

In this work, we developed a HPLC method for the multidetermination of avermectins (AVM) (abamectin-ABA 1b and ABA 1a, eprinomectin-EPR, and ivermectin-IVM) and milbemycins (moxidectin-MOX) in milk samples using polypyrrole (PPy) as adsorbent material in pipette-tip solid-phase extraction (PT-PPy-SPE). PPy was characterized by scanning electron microscopy, thermogravimetric analysis, Fourier transform infrared spectroscopy, and X-ray diffraction and the data agreed with the literature. The sample preparation included the clean-up of the milk by protein precipitation (PP) with acetonitrile and extraction of the analytes by PT-PPy-SPE. The chromatographic method was developed in reverse phase and isocratic mode with flow rate at 1.2 mL min -1 and ultraviolet detection at 250 nm. The mobile phase composition was acetonitrile:methanol:water (55:25:20, v/v/v). The studied parameters and the optimized conditions for the sample preparation were washing solvent (300 μL water), volume and type of eluent (500 μL methanol), volume and pH of sample (1 mL and pH 10), amount of adsorbent material (50 mg PPy), and without addition of salt (NaCl). The method was linear over the concentration range from 20 to 3000 ng mL -1 with coefficients of correlation (r) ≥ 0.99 for all analytes and recoveries around 100%. The method developed and validated was used for the analyses of real milk samples from cow treated with Ivomec ® (IVM 3.5%), in which were found 21.51 ± 2.94 ng mL -1 of IVM. Finally, the results proved that PT-PPy-SPE coupled to HPLC-UV was economical, simple, and easy-to-perform technique. Graphical abstract Pipette-tip solid phase extraction using polypirrole as adsorbent material for determination of avermectins and milbemycins in milk.

Zincon-modified activated carbon for solid-phase extraction and preconcentration of trace lead and chromium from environmental samples.

PubMed

Li, Zhenhua; Chang, Xijun; Hu, Zheng; Huang, Xinping; Zou, Xiaojun; Wu, Qiong; Nie, Rong

2009-07-15

A new method that utilizes zincon-modified activated carbon (AC-ZCN) as a solid-phase extractant has been developed for simultaneous preconcentration of trace Cr(III) and Pb(II) prior to the measurement by inductively coupled plasma optical emission spectrometry (ICP-OES). The separation/preconcentration conditions of analytes were investigated, including effects of pH, the shaking time, the sample flow rate and volume, the elution condition and the interfering ions. At pH 4, the maximum adsorption capacity of Cr(III) and Pb(II) onto the AC-ZCN were 17.9 and 26.7 mg g(-1), respectively. The adsorbed metal ions were quantitatively eluted by 1 mL of 0.1 mol L(-1) HCl. Common coexisting ions did not interfere with the separation. According to the definition of IUPAC, the detection limits (3 sigma) of this method for Cr(III) and Pb(II) were 0.91 and 0.65 ng mL(-1), respectively. The relative standard deviation under optimum condition is less than 3.5% (n=8). The method has been applied for the determination of Cr(III) and Pb(II) in biological materials and water samples with satisfactory results.

Green Preconcentration of Trace Amounts of Copper from Water and Food Samples onto Novel Organo-Nanoclay Prior to Flame Atomic Absorption Spectrometry.

PubMed

Beyki, Mostafa Hossein; Shemirani, Farzaneh; Khani, Rouhollah

2014-01-01

In this work, the nanoclay was intercalated with acyclovir (9-[(2-hydroxyethoxy) methyl] guanine), the toxicity of which to mammalian cells is very low. We used no organic solvents for preparation of modified clay and desorption of Cu ions from the sorbent. Batch and column methods were used, and sorption of Cu was quantitative (>98%) in the pH range of 7.5 to 10.0. Quantitative desorption occurred with 5.0 mL of 3.0 M HCl, and the amount of Cu(II) was measured by using flame atomic absorption spectrometry. In the initial solution the linear dynamic range and the LOD were 3.0-1000.0 and 0.58 μg/L, respectively. With 500.0 mL of sample, an enrichment factor of 100 was obtained. The RSD was 2.0% (n = 8, concentration = 0.5 mg/L), and the maximum capacity of the sorbent was 45.0 mg/g. The influence of experimental parameters including sample pH, ionic strength, type and volume of the eluent, and interference of some ions on the recoveries of Cu was investigated. The proposed method using a new and easier prepared solid sorbent was applied to the determination of Cu in different real samples with satisfactory results.

Heavy metal contents of play dough, face and finger paint samples sold in turkish markets.

PubMed

Erbas, Zeliha; Karatepe, Aslihan; Soylak, Mustafa

2017-08-01

Lead, cadmium, nickel, manganese, cobalt and copper contents of some play dough, face and finger paint samples were determined by using a new solid phase extraction method which has been developed by using multi-walled carbon nanotube with patent blue (V) sodium salt to selectively separate and preconcentrate these metal ions. Flame atomic absorption spectrometry was used to determine the metal ions. Analytical parameters affecting the complex formation and solid phase extraction performance such as pH, the amount of ligand and volume of sample solution were investigated. The recoveries of the studied metal ions were not affected by the foreign ions. Analytes were recovered quantitatively at pH 5.5 and with a nitric acid of 2molL -1 as eluent. Analysis of a certified reference material was performed to validate the method before applying it to determine the metal ions in the real samples. Detection limits were found to be as Pb(II): 7.71μgL -1 , Cu(II): 1.43μgL -1 , Cd(III): 0.21μgL -1 , Mn(II): 0.47μgL -1 , Ni(II): 3.52μgL -1 and Co(II): 1.96μgL -1 . Copyright © 2017 Elsevier B.V. All rights reserved.

Chemical Composition of Rainwater in Córdoba City, Argentina

NASA Astrophysics Data System (ADS)

López, M. L.; Asar, M. L.; Ceppi, S.; Bürgesser, R. E.; Avila, E.

2013-05-01

Sampling and chemical analysis of rainwater has proved to be a useful technique for studying its chemical composition and provides a greater understanding of local and regional dispersion of pollutants and their potential impacts to ecosystems through deposition processes. Samples of rainwater were collected during 2009-2012, in Córdoba city, Argentina. Two kind of sampling were performed: event-specific and sequential. The objective of the first of these was to determine the chemical concentration of the total rain, while the objective of the second one was to analyze the variability of the chemical concentration during an individual rain event. The total volume of each sample was divided in halves. One half was filtered through 0.45 μm membrane filter. After this, all the samples were reduced by evaporation to a final volume of 10 ml. The non-filtered samples were acidified and digested in accordance to the method 3050B of the Environmental Protection Agency (EPA) for acid digestion of sediments. Multi-elemental standard solutions in different concentrations were prepared by adequate dilutions. Gallium was added as an internal standard in all standard solutions and samples. Exactly 5 μL of these solutions were deposited on acrylic supports. When these droplets were dried, Synchrotron Radiation Total Reflection X-Ray Fluorescence technique was used for determining the chemical elements. Spectra were analyzed with the AXIL package for spectrum analysis. Due to the intrinsic characteristics of the total reflection technique, the background of the measurements is significantly reduced and there are no matrix effects, therefore quantification can be obtained from the linear correlation between fluorescence intensity and the concentration of the element of interest. The elements quantified were S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, and Pb. For all of them a calibration curve was performed in order to quantify their concentrations on the samples. The results show that the average pH in city rainwater was pH=6.5; the elements found in the samples were S, Ca, Cu, Cr, Sr, P, Fe, Mn, Pb, K, Ti, V, Zn and the average concentrations of these elements were below the limits established by World Health Organization for drinking water, and show a high natural variability. The temporal evolution of inorganic ion concentration during rain events was analyzed and the scavenging coefficients were calculated and compared with data from literature. A comparison was made between the rainwater chemical composition and chemical composition in the aerosols scavenging during the rain. This study is the first in Córdoba city to analyze the chemical composition of rainwater and constitute a base for future comparison of variability in pH and elemental composition.

Dissolution of bovine pulp tissue in solutions consisting of varying NaOCl concentrations and combined with EDTA.

PubMed

Irala, Luis Eduardo Duarte; Grazziotin-Soares, Renata; Salles, Alexandre Azevedo; Munari, Aline Zen; Pereira, Joseani Santos

2010-01-01

This in vitro study evaluated (1) the dissolution of bovine pulp tissue in solutions consisting of varying NaOCl concentrations and combined with EDTA; and (2) the pH of these solutions before and after the experiment. The independent variables were the concentration and the volume of the solution. Thirty bovine pulps were divided in equal fragments, resulting in 90 fragments of pulp tissue. Each fragment was immersed in one of the following solutions: 1% NaOCl (4 ml), 2.5% NaOCl (4 ml), 1% NaOCl + 17% EDTA (2 ml : 2 ml), 1% NaOCl + 17% EDTA (1 ml : 3 ml), 2.5% NaOCl + 17% EDTA (2 ml : 2 ml), and 2.5% NaOCl + 17% EDTA (1 ml : 3 ml). The test solutions were dichotomized as either able or not able to dissolve the tissue, the latter being attributed when the dissolution of the pulp tissue was not complete within 48 hours. When the samples were able to dissolve the tissue, the time required for complete tissue dissolution was submitted to statistical analysis. The pH of the solutions was measured before and after the experiment. The pH variable was dichotomized as either changed or unchanged. The results demonstrated that the NaOCl solutions combined with 17% EDTA were not able to dissolve the tissue. The t-test revealed that the 2.5% NaOCl solution presented a lower mean dissolution time than the 1% NaOCl solution (p < 0.001). The pH of the solutions with equal volumes of NaOCl and EDTA decreased in 48 hours.

Fast and "green" method for the analytical monitoring of haloketones in treated water.

PubMed

Serrano, María; Silva, Manuel; Gallego, Mercedes

2014-09-05

Several groups of organic compounds have emerged as being particularly relevant as environmental pollutants, including disinfection by-products (DBPs). Haloketones (HKs), which belong to the unregulated volatile fraction of DBPs, have become a priority because of their occurrence in drinking water at concentrations below 1μg/L. The absence of a comprehensive method for HKs has led to the development of the first method for determining fourteen of these species. In an effort to miniaturise, this study develops a micro liquid-liquid extraction (MLLE) method adapted from EPA Method 551.1. In this method practically, the whole extract (50μL) was injected into a programmed temperature vaporiser-gas chromatography-mass spectrometer in order to improve sensitivity. The method was validated by comparing it to EPA Method 551.1 and showed relevant advantages such as: lower sample pH (1.5), higher aqueous/organic volume ratio (60), lower solvent consumption (200μL) and fast and cost-saving operation. The MLLE method achieved detection limits ranging from 6 to 60ng/L (except for 1,1,3-tribromo-3-chloroacetone, 120ng/L) with satisfactory precision (RSD, ∼6%) and high recoveries (95-99%). An evaluation was carried out of the influence of various dechlorinating agents as well as of the sample pH on the stability of the fourteen HKs in treated water. To ensure the HKs integrity for at least 1 week during storage at 4°C, the samples were acidified at pH ∼1.5, which coincides with the sample pH required for MLLE. The green method was applied to the speciation of fourteen HKs in tap and swimming pool waters, where one and seven chlorinated species, respectively, were found. The concentration of 1.1-dichloroacetone in swimming pool water increased ∼25 times in relation to tap water. Copyright © 2014 Elsevier B.V. All rights reserved.

A motor-driven syringe-type gradient maker for forming immobilized pH gradient gels.

PubMed

Fawcett, J S; Sullivan, J V; Chidakel, B E; Chrambach, A

1988-05-01

A motor driven gradient maker based on the commercial model (Jule Inc., Trumbull, CT) was designed for immobilized pH gradient gels to provide small volumes, rapid stirring and delivery, strict volume and temperature control and air exclusion. The device was constructed and by a convenient procedure yields highly reproducible gradients either in solution or on polyacrylamide gels.

Comparison of the effect of a single dose of erythromycin with pantoprazole on gastric content volume and acidity in elective general surgery patients

PubMed Central

Bhatia, Nidhi; Palta, Sanjeev; Arora, Kanika

2011-01-01

Introduction: Pulmonary aspiration of gastric contents remains one of the most feared complications of anesthesia. A gastric pH of 2.5 or less and a volume of 25 ml (0.4 ml/kg body weight) or more in average adult patients are considered critical factors for the development of pulmonary damage in adults. Materials and Methods: This study compared the efficacy of a single oral dose of erythromycin (a macrolide antibiotic) with oral pantoprazole (a proton pump inhibitor) on pre-operative gastric fluid volume and pH in a prospective, randomized, double-blind controlled fashion in 80 adult patients (of ASA physical status I and II) planned for elective surgery under general anesthesia. Patients were divided into two groups of 40 patients each. The pantoprazole group (Group I) received oral pantoprazole 40 mg and the erythromycin group (Group II) received oral erythromycin 250 mg at least 1 h prior to the induction of anesthesia. After tracheal intubation, gastric fluid was aspirated via a Salem Sump tube and its volume and pH were measured. Results: Although both erythromycin and pantoprazole decreased the gastric fluid volume to a similar extent, the decrease in gastric fluid acidity by pantoprazole was significantly greater than that by erythromycin. The proportion of patients at risk of pulmonary aspiration according to traditional criteria, i.e. pH ≤2.5 and volume ≥25ml, was lower in the pantoprazole group. Conclusion: Administration of pantoprazole was found to be more useful than a sub-therapeutic dose of erythromycin in decreasing both volume and acidity of gastric content. PMID:21772679

The Influences of Stirring and Cow Manure Added on Biogas Production From Vegetable Waste Using Anaerobic Digester

NASA Astrophysics Data System (ADS)

Abdullah, N. O.; Pandebesie, E. S.

2018-03-01

Based on Indonesian Government Regulation number 18, 2008, solid waste management should be conducted from the source to minimize the amount of waste. The process includes the waste from domestic, commercial, and institution. This also includes in 3R program (reduce, reuse, and recycle). Vegetable waste from market is a potential material to produce biogas due to its chemical composition (hemi-cellulose, cellulose, and lignin) which transform the biomass to be the raw material of biogas. Acid substance of vegetable becomes an obstacle in process of producing biogas. There has to be buffer material which can improve the performance of biogas process. Cow manure is a material which can be easily obtained as buffer. This research used 24 biogas reactor in volume 6 L by batch method. Biogas volume is measured by checking the preferment in manometer. Methane measurement is conducted by using Gas Chromatography (GC) Hewlett Packard (HP-series 6890) in day 15 and 30. The research was started by sample characterization, sample test by total solid analysis, volatile solid, lignin, ratio C/N, ammonium, and ash. Analysis of pH, temperature, and biogas volume is conducted every day.

Pyridine-functionalized Fe₃O₄ nanoparticles as a novel sorbent for the preconcentration of lead and cadmium ions in tree leaf as a bioindicator of urban traffic pollution.

PubMed

Sayar, Omid; Zhad, Hamid Reza Lotfi Zadeh; Sadeghi, Omid; Amani, Vahid; Najafi, Ezzatolla; Tavassoli, Najmeh

2012-12-01

We have developed a facile and highly sensitive sorbent for cadmium and lead ions. It is based on Fe₃O₄ nanoparticles functionalized with a derivative of picoline and was characterized by scanning electron microscopy, differential thermographic analysis, and elemental analysis. The material can be applied to the preconcentration of lead and cadmium ions. Factors such as the type, concentration and volume of eluent, the pH of the sample solution, the time for extraction, and the volume of the sample were studied. The effects of a variety of ions on preconcentration and recovery of these ions were also investigated. The ions were determined by FAAS, and the limits of detection are <0.8 and <0.061 μg L⁻¹ for lead and cadmium, respectively. Recoveries and precisions are >98.0 % and <1.3 %, respectively. The method was validated by analyzing several certified leaf reference materials.

Induction of laccases in Trametes versicolor by aqueous wood extracts.

PubMed

Bertrand, Brandt; Martínez-Morales, Fernando; Tinoco, Raunel; Rojas-Trejo, Sonia; Serrano-Carreón, Leobardo; Trejo-Hernández, María R

2014-01-01

The induction of laccase isoforms in Trametes versicolor HEMIM-9 by aqueous extracts (AE) from softwood and hardwood was studied. Samples of sawdust of Pinus sp., Cedrela sp., and Quercus sp. were boiled in water to obtain AE. Different volumes of each AE were added to fungal cultures to determine the amount of AE needed for the induction experiments. Laccase activity was assayed every 24 h for 15 days. The addition of each AE (50 to 150 μl) to the fungal cultures increased laccase production compared to the control (0.42 ± 0.01 U ml(-1)). The highest laccase activities detected were 1.92 ± 0.15 U ml(-1) (pine), 1.87 ± 0.26 U ml(-1) (cedar), and 1.56 ± 0.34 U ml(-1) (oak); laccase productivities were also significantly increased. Larger volumes of any AE inhibited mycelial growth. Electrophoretic analysis revealed two laccase bands (lcc1 and lcc2) for all the treatments. However, when lcc2 was analyzed by isoelectric focusing, inducer-dependent isoform patterns composed of three (pine AE), four (oak AE), and six laccase bands (cedar AE) were observed. Thus, AE from softwood and hardwood had induction effects in T. versicolor HEMIM-9, as indicated by the increase in laccase activity and different isoform patterns. All of the enzymatic extracts were able to decolorize the dye Orange II. Dye decolorization was mainly influenced by pH. The optimum pH for decolorization was pH 5 (85%), followed by pH 7 (50%) and pH 3 (15%). No significant differences in the dye decolorizing capacity were detected between the control and the differentially induced laccase extracts (oak, pine and cedar). This could be due to the catalytic activities of isoforms with pI 5.4 and 5.8, which were detected under all induction conditions.

Solid phase extraction of metal ions in environmental samples on 1-(2-pyridylazo)-2-naphthol impregnated activated carbon cloth.

PubMed

Alothman, Zeid A; Yilmaz, Erkan; Habila, Mohamed; Soylak, Mustafa

2015-02-01

1-(2-Pyridylazo)-2-naphthol impregnated activated carbon cloth (PAN-imp-ACC) was prepared as a solid phase sorbent and, for the first time, was used for the simultaneous separation and preconcentration of trace amounts of lead, cadmium and nickel in water, soil and sewage sludge samples prior to determination by flame atomic absorption spectrometry (FAAS). The parameters governing the efficiency of the method were optimized, including the pH, the eluent type and volume, the sample and eluent flow rates, diverse ions effects and the sample volume. A preconcentration factor of 100 was achieved for all the metal ions, with detection limits of 0.1-2.8 µg L(-1) and relative standard deviations below 6.3%. The adsorption capacity of the PAN-imp-ACC for Pb(II), Cd(II) and Ni(II) ions was found to be 45.0 mg g(-1), 45.0 mg g(-1) and 43.2 mg g(-1), respectively. The method was validated by the analysis of the certified reference materials TMDA-64.2 fortified Lake Ontario water and BCR-146R Sewage Sludge Amended Soil (Industrial Origin). The procedure was applied to determine the analytes content in real samples. Copyright © 2014 Elsevier Inc. All rights reserved.

Investigation of differences between field and laboratory pH measurements of national atmospheric deposition program/national trends network precipitation samples

USGS Publications Warehouse

Latysh, N.; Gordon, J.

2004-01-01

A study was undertaken to investigate differences between laboratory and field pH measurements for precipitation samples collected from 135 weekly precipitation-monitoring sites in the National Trends Network from 12/30/1986 to 12/28/1999. Differences in pH between field and laboratory measurements occurred for 96% of samples collected during this time period. Differences between the two measurements were evaluated for precipitation samples collected before and after January 1994, when modifications to sample-handling protocol and elimination of the contaminating bucket o-ring used in sample shipment occurred. Median hydrogen-ion and pH differences between field and laboratory measurements declined from 3.9 ??eq L-1 or 0.10 pH units before the 1994 protocol change to 1.4 ??eq L-1 or 0.04 pH units after the 1994 protocol change. Hydrogen-ion differences between field and laboratory measurements had a high correlation with the sample pH determined in the field. The largest pH differences between the two measurements occurred for high-pH samples (>5.6), typical of precipitation collected in Western United States; however low- pH samples (<5.0) displayed the highest variability in hydrogen-ion differences between field and laboratory analyses. Properly screened field pH measurements are a useful alternative to laboratory pH values for trend analysis, particularly before 1994 when laboratory pH values were influenced by sample-collection equipment.

Salting-out assisted liquid-liquid extraction combined with capillary HPLC for the determination of sulfonylurea herbicides in environmental water and banana juice samples.

PubMed

Gure, Abera; Lara, Francisco J; Moreno-González, David; Megersa, Negussie; del Olmo-Iruela, Monsalud; García-Campaña, Ana M

2014-09-01

A salting-out assisted liquid-liquid extraction (SALLE) combined with capillary high performance liquid chromatography with diode array detector (capillary HPLC-DAD) was proposed for extraction and determination of residues of nine sulfonylurea herbicides (SUHs) in environmental water and banana juice samples. Various parameters affecting the extraction process such as the type and volume of the organic solvent, sample volume, type and amount of salt, pH of the sample and vortex time were optimized. Under optimum conditions, matrix matched calibration curves were established using river water and banana juice samples. Good linear relationships as well as low limits of detection, LODs (0.4-1.3 and 3-13 µg/L) and quantification, LOQs (1.3-4.3 and 10-43 µg/L) were obtained in water and banana juice samples, respectively. The precision (intra- and inter-day) of the peak areas expressed as relative standard deviations (%, RSD), at two concentration levels were below 10 % in both matrices. Recoveries obtained from spiked environmental waters (river water and groundwater) and banana juice samples, at two concentration levels, ranged from 72 to 115%. The results of the analysis revealed that the proposed SALLE-capillary HPLC method is simple, rapid, cheap and environmentally friendly, being successfully applicable for the determination of SUH residues in waters and banana juices. Copyright © 2014 Elsevier B.V. All rights reserved.

Removal of gallium (III) ions from acidic aqueous solution by supercritical carbon dioxide extraction in the green separation process.

PubMed

Chou, Wei-Lung; Wang, Chih-Ta; Yang, Kai-Chiang; Huang, Yen-Hsiang

2008-12-15

Supercritical carbon dioxide extraction, which is a feasible "green" alternative, was applied in this study as a sample pretreatment step for the removal of gallium (III) ions from acidic aqueous solution. The effect of various process parameters, including various chelating agents, extraction pressure and temperature, dimensionless CO(2) volume, the concentration of the chelating agent, and the pH of the solution, governing the efficiency and throughput of the procedure were systematically investigated. The performance of the various chelating agents from different studies indicated that the extraction efficiency of supercritical CO(2) was in the order: thiopyridine (PySH)>thenoyltrifluoroacetone (TTAH)>acetylacetone (AcAcH). The optimal extraction pressure and temperature for the supercritical CO(2) extraction of gallium (III) with chelating agent PySH were found to be 70 degrees C and 3000psi, respectively. The optimum concentration of the chelating agent was found to be 50ppm. A value of 7.5 was selected as the optimum dimensionless CO(2) volume. The optimum pH of the solution for supercritical CO(2) extraction should fall in the range of 2.0-3.0.

Vacuum packing: a model system for laboratory-scale silage fermentations.

PubMed

Johnson, H E; Merry, R J; Davies, D R; Kell, D B; Theodorou, M K; Griffith, G W

2005-01-01

To determine the utility of vacuum-packed polythene bags as a convenient, flexible and cost-effective alternative to fixed volume glass vessels for lab-scale silage studies. Using perennial ryegrass or red clover forage, similar fermentations (as assessed by pH measurement) occurred in glass tube and vacuum-packed silos over a 35-day period. As vacuum-packing devices allow modification of initial packing density, the effect of four different settings (initial packing densities of 0.397, 0.435, 0.492 and 0.534 g cm(-3)) on the silage fermentation over 16 days was examined. Significant differences in pH decline and lactate accumulation were observed at different vacuum settings. Gas accumulation was apparent within all bags and changes in bag volume with time was observed to vary according to initial packing density. Vacuum-packed silos do provide a realistic model system for lab-scale silage fermentations. Use of vacuum-packed silos holds potential for lab-scale evaluations of silage fermentations, allowing higher throughput of samples, more consistent packing as well as the possibility of investigating the effects of different initial packing densities and use of different wrapping materials.

Evaluation of plasma chemistry and haematological studies on chickens infected with Eimeria tenella and E acervulina.

PubMed

Fukata, T; Komba, Y; Sasai, K; Baba, E; Arakawa, A

1997-07-12

Plasma chemistry and haematological studies were conducted on chickens with coccidiosis. Male White Leghorn chickens, of two weeks old, were inoculated with 5 x 10(4) Eimeria tenella sporulated oocysts or with 1 x 10(6) E acervulina sporulated oocysts. Blood samples were taken four, seven and 11 days after inoculation. A wet chemistry system was applied to measure the plasma activities of aspartate aminotransferase, alanine aminotransferase, alkaline phosphatase, gamma glutamyltransferase, creatine kinase, amylase and lactate dehydrogenase and the concentrations of creatine, total bilirubin, urate, total cholesterol, total protein, albumin, glucose and triglycerides. A dry chemistry system was applied to measure sodium, potassium, chloride and calcium. The number of red blood cells and packed cell volume were determined by a micro cell counter and blood pH was measured with a blood gas analyser. The erythrocyte count, packed cell volume, sodium and chloride levels in the chickens infected with E tenella were significantly (P < 0.05) lower than those of the uninfected controls. The significant decrease in blood pH of the chickens infected with E acervulina suggests malabsorption associated with duodenal lesions induced by the infection.

Magnetic Resonance Characterization of Cardiac Adaptation and Myocardial Fibrosis in Pulmonary Hypertension Secondary to Systemic-To-Pulmonary Shunt.

PubMed

Pereda, Daniel; García-Lunar, Inés; Sierra, Federico; Sánchez-Quintana, Damián; Santiago, Evelyn; Ballesteros, Constanza; Encalada, Juan F; Sánchez-González, Javier; Fuster, Valentín; Ibáñez, Borja; García-Álvarez, Ana

2016-09-01

Pulmonary hypertension (PH) and right ventricular (RV) dysfunction are strong predictors of morbidity and mortality among patients with congenital heart disease. Early detection of RV involvement may be useful in the management of these patients. We aimed to assess progressive cardiac adaptation and quantify myocardial extracellular volume in an experimental porcine model of PH because of aorto-pulmonary shunt using cardiac magnetic resonance (CMR). To characterize serial cardiac adaptation, 12 pigs (aorto-pulmonary shunt [n=6] or sham operation [n=6]) were evaluated monthly with right heart catheterization, CMR, and computed tomography during 4 months, followed by pathology analysis. Extracellular volume by CMR in different myocardial regions was studied in 20 animals (aorto-pulmonary shunt [n=10] or sham operation [n=10]) 3 months after the intervention. All shunted animals developed PH. CMR evidenced progressive RV hypertrophy and dysfunction secondary to increased afterload and left ventricular dilatation secondary to volume overload. Shunt flow by CMR strongly correlated with PH severity, left ventricular end-diastolic pressure, and left ventricular dilatation. T1-mapping sequences demonstrated increased extracellular volume at the RV insertion points, the interventricular septum, and the left ventricular lateral wall, reproducing the pattern of fibrosis found on pathology. Extracellular volume at the RV insertion points strongly correlated with pulmonary hemodynamics and RV dysfunction. Prolonged systemic-to-pulmonary shunting in growing piglets induces PH with biventricular remodeling and myocardial fibrosis that can be detected and monitored using CMR. These results may be useful for the diagnosis and management of congenital heart disease patients with pulmonary overcirculation. © 2016 American Heart Association, Inc.

Miniaturizing and automation of free acidity measurements for uranium (VI)-HNO3 solutions: Development of a new sequential injection analysis for a sustainable radio-analytical chemistry.

PubMed

Néri-Quiroz, José; Canto, Fabrice; Guillerme, Laurent; Couston, Laurent; Magnaldo, Alastair; Dugas, Vincent

2016-10-01

A miniaturized and automated approach for the determination of free acidity in solutions containing uranium (VI) is presented. The measurement technique is based on the concept of sequential injection analysis with on-line spectroscopic detection. The proposed methodology relies on the complexation and alkalimetric titration of nitric acid using a pH 5.6 sodium oxalate solution. The titration process is followed by UV/VIS detection at 650nm thanks to addition of Congo red as universal pH indicator. Mixing sequence as well as method validity was investigated by numerical simulation. This new analytical design allows fast (2.3min), reliable and accurate free acidity determination of low volume samples (10µL) containing uranium/[H(+)] moles ratio of 1:3 with relative standard deviation of <7.0% (n=11). The linearity range of the free nitric acid measurement is excellent up to 2.77molL(-1) with a correlation coefficient (R(2)) of 0.995. The method is specific, presence of actinide ions up to 0.54molL(-1) does not interfere on the determination of free nitric acid. In addition to automation, the developed sequential injection analysis method greatly improves the standard off-line oxalate complexation and alkalimetric titration method by reducing thousand fold the required sample volume, forty times the nuclear waste per analysis as well as the analysis time by eight fold. These analytical parameters are important especially in nuclear-related applications to improve laboratory safety, personnel exposure to radioactive samples and to drastically reduce environmental impacts or analytical radioactive waste. Copyright © 2016 Elsevier B.V. All rights reserved.

The potential influence of CO2, as an agent for euthanasia, on the pharmacokinetics of basic compounds in rodents.

PubMed

Angus, Derek W; Baker, James A; Mason, Rona; Martin, Iain J

2008-02-01

Rodent tissue distribution and pharmacokinetic studies were performed on basic compounds Org A and Org B in support of central nervous system drug discovery programs. A consistent observation from these studies was that drug concentrations in plasma obtained by cardiac puncture after CO(2) euthanasia were markedly higher compared with those from other sampling methods (serial sampling, isoflurane anesthesia, or cervical dislocation). Further investigations demonstrated that CO(2) euthanasia led to a reduction in blood pH in both rats and mice, which was not observed with the other sampling methods. The use of CO(2) euthanasia resulted in a decrease in the brain/plasma ratio of Org B, largely as a result of increased plasma concentrations. The pharmacokinetics of a basic drug, raloxifene, in rat were also influenced by sampling technique. CO(2) euthanasia before sampling, resulted in a 2- to 3-fold increase in the area under the drug concentration-time curve, a decrease in plasma clearance, and a decrease in the steady-state volume of distribution compared with isoflurane anesthesia. It is proposed that a decrease in the pH of blood relative to that of other tissues, as a consequence of CO(2) exposure, results in a redistribution of basic compounds out of the tissues, leading to higher concentrations in plasma.

Optimization of Photooxidative Removal of Phenazopyridine from Water

NASA Astrophysics Data System (ADS)

Saeid, Soudabeh; Behnajady, Mohammad A.; Tolvanen, Pasi; Salmi, Tapio

2018-05-01

The photooxidative removal of analgesic pharmaceutical compound phenazopyridine (PhP) from aqueous solutions by UV/H2O2 system with a re-circulated photoreactor was investigated. Response surface methodology (RSM) was employed to optimize the effect of operational parameters on the photooxidative removal efficiency. The investigated variables were: the initial PhP and H2O2 concentrations, irradiation time, volume of solution and pH. The analysis of variance (ANOVA) of quadratic model demonstrated that the described model was highly significant. The predicted values of the photooxidative removal efficiency were found to be in a fair agreement with experimental values ( R 2 = 0.9832, adjusted R 2 = 0.9716). The model predicted that the optimal reaction conditions for a maximum removal of PhP (>98%) were: initial PhP concentration less than 23 mg L-1, initial concentration of H2O2 higher than 470 mg L-1, solution volume less than 500 mL, pH close to 2 and irradiation time longer than 6 min.

Polypyrrole/multi-walled carbon nanotube composite for the solid phase extraction of lead(II) in water samples.

PubMed

Sahmetlioglu, Ertugrul; Yilmaz, Erkan; Aktas, Ece; Soylak, Mustafa

2014-02-01

A multi-walled carbon nanotubes-polypyrrole conducting polymer nanocomposite has been synthesized, characterized and used for the separation and preconcentration of lead at trace levels in water samples prior to its flame atomic absorption spectrometric detection. The analytical parameters like pH, sample volume, eluent, sample flow rate that were affected the retentions of lead(II) on the new nanocomposite were optimized. Matrix effects were also investigated. Limit of detection and preconcentration factors were 1.1 µg L(-1) and 200, respectively. The adsorption capacity of the nanocomposite was 25.0mg lead(II) per gram composite. The validation of the method was checked by using SPS-WW2 Waste water Level 2 certified reference material. The method was applied to the determination of lead in water samples with satisfactory results. © 2013 Elsevier B.V. All rights reserved.

Ionic liquid-based single-drop microextraction followed by liquid chromatography-ultraviolet spectrophotometry detection to determine typical UV filters in surface water samples.

PubMed

Vidal, Lorena; Chisvert, Alberto; Canals, Antonio; Salvador, Amparo

2010-04-15

A user-friendly and inexpensive ionic liquid-based single-drop microextraction (IL-SDME) procedure has been developed to preconcentrate trace amounts of six typical UV filters extensively used in cosmetic products (i.e., 2-hydroxy-4-methoxybenzophenone, isoamyl 4-methoxycinnamate, 3-(4'-methylbenzylidene)camphor, 2-ethylhexyl 2-cyano-3,3-diphenylacrylate, 2-ethylhexyl 4-dimethylaminobenzoate and 2-ethylhexyl 4-methoxycinnamate) from surface water samples prior to analysis by liquid chromatography-ultraviolet spectrophotometry detection (LC-UV). A two-stage multivariate optimization approach was developed by means of a Plackett-Burman design for screening and selecting the significant variables involved in the SDME procedure, which were later optimized by means of a circumscribed central composite design. The studied variables were drop volume, sample volume, agitation speed, ionic strength, extraction time and ethanol quantity. Owing to particularities, ionic liquid type and pH of the sample were optimized separately. Under optimized experimental conditions (i.e., 10 microL of 1-hexyl-3-methylimidazolium hexafluorophosphate, 20 mL of sample containing 1% (v/v) ethanol and NaCl free adjusted to pH 2, 37 min extraction time and 1300 rpm agitation speed) enrichment factors up to ca. 100-fold were obtained depending on the target analyte. The method gave good levels of repeatability with relative standard deviations varying between 2.8 and 8.8% (n=6). Limits of detection were found in the low microg L(-1) range, varying between 0.06 and 3.0 microg L(-1) depending on the target analyte. Recovery studies from different types of surface water samples collected during the winter period, which were analysed and confirmed free of all target analytes, ranged between 92 and 115%, showing that the matrix had a negligible effect upon extraction. Finally, the proposed method was applied to the analysis of different water samples (taken from two beaches, two swimming pools and a river) collected during the summer period. (c) 2009 Elsevier B.V. All rights reserved.

Water-quality data for selected sites on Reversed, Rush, and Alger Creeks and Gull and Silver Lakes, Mono County, California, April 1994 to March 1995

USGS Publications Warehouse

Wang, Bronwen; Rockwell, G.L.; Blodgett, J.C.

1995-01-01

Water-quality data for selected sites on Reversed, Rush, and Alger Creeks and Gull and Silver Lakes, Mono County, California, were collected from April 1994 to March 1995. Water samples were analyzed for major ions and trace elements, nutrients, methylene blue active substances, and oil and grease. Field measurements were made for discharge, specific conductance, pH, water temperature, barometric pressure, dissolved oxygen, and alkalinity. Additional data collected include vertical water profiles of specific conductance, pH, water temperature, and dissolved oxygen collected at 3.3-foot intervals for Gull and Silver Lakes; chlorophyll-a and -b concentrations and Secchi depth for Gull and Silver Lakes; sediment interstitial- water nutrient concentrations in cores from Gull Lake; and lake surface and volume of Gull and Silver Lakes.

Indicators of induced subacute ruminal acidosis (SARA) in Danish Holstein cows.

PubMed

Danscher, Anne Mette; Li, Shucong; Andersen, Pia H; Khafipour, Ehsan; Kristensen, Niels B; Plaizier, Jan C

2015-07-17

The prevalence of subacute ruminal acidosis (SARA) in dairy cows is high with large impact on economy and welfare. Its current field diagnosis is based on point ruminal pH measurements by oral probe or rumenocentesis. These techniques are invasive and inaccurate, and better markers for the diagnosis of SARA are needed. The goal of this study was to evaluate clinical signs of SARA and to investigate the use of blood, faecal and urinary parameters as indicators of SARA. Six lactating, rumen cannulated, Danish Holstein cows were used in a cross-over study with three periods. The first and second periods included two cows on control diet and two cows on nutritional SARA challenge. The third period only included two cows on SARA challenge. Control diet was a conventional total mixed ration [45.5% dry matter (DM), 17.8% crude protein, 43.8% neutral detergent fibre, and 22.5% acid detergent fibre (DM basis)]. SARA challenge was conducted by substituting control diet with grain pellets (50% wheat/barley) over 3 days to reach 40% grain in the diet. Ruminal pH was measured continuously. Blood samples were collected once daily at 7 h after feeding. Samples of faeces and urine were collected at feeding, and at 7 and 12 h after feeding. Blood samples were analysed for pCO2, pO2, pH, electrolytes, lactate, glucose, packed cell volume (PCV), and total plasma protein concentration. Milk composition, ruminal VFA, and pH of faeces and urine were measured. SARA was associated with decreased (P < 0.05) minimum ruminal, faecal and urinary pH. Daily times and areas of ruminal pH below 5.8, and 5.6 were increased to levels representative for SARA. Significant differences were detected in milk composition and ruminal VFAs. Blood calcium concentration was decreased (P < 0.05), and pCO2 tended to be increased (P = 0.10). Significant differences were not detected in other parameters. SARA challenge was associated with changes in faecal and urinary pH, blood calcium concentration and pCO2. These may be helpful as indicators of SARA. However changes were small, and diurnal variations were present. None of these parameters are able to stand alone as indicators of SARA.

Experimental design for TBT quantification by isotope dilution SPE-GC-ICP-MS under the European water framework directive.

PubMed

Alasonati, Enrica; Fabbri, Barbara; Fettig, Ina; Yardin, Catherine; Del Castillo Busto, Maria Estela; Richter, Janine; Philipp, Rosemarie; Fisicaro, Paola

2015-03-01

In Europe the maximum allowable concentration for tributyltin (TBT) compounds in surface water has been regulated by the water framework directive (WFD) and daughter directive that impose a limit of 0.2 ng L(-1) in whole water (as tributyltin cation). Despite the large number of different methodologies for the quantification of organotin species developed in the last two decades, standardised analytical methods at required concentration level do not exist. TBT quantification at picogram level requires efficient and accurate sample preparation and preconcentration, and maximum care to avoid blank contamination. To meet the WFD requirement, a method for the quantification of TBT in mineral water at environmental quality standard (EQS) level, based on solid phase extraction (SPE), was developed and optimised. The quantification was done using species-specific isotope dilution (SSID) followed by gas chromatography (GC) coupled to inductively coupled plasma mass spectrometry (ICP-MS). The analytical process was optimised using a design of experiment (DOE) based on a factorial fractionary plan. The DOE allowed to evaluate 3 qualitative factors (type of stationary phase and eluent, phase mass and eluent volume, pH and analyte ethylation procedure) for a total of 13 levels studied, and a sample volume in the range of 250-1000 mL. Four different models fitting the results were defined and evaluated with statistic tools: one of them was selected and optimised to find the best procedural conditions. C18 phase was found to be the best stationary phase for SPE experiments. The 4 solvents tested with C18, the pH and ethylation conditions, the mass of the phases, the volume of the eluents and the sample volume can all be optimal, but depending on their respective combination. For that reason, the equation of the model conceived in this work is a useful decisional tool for the planning of experiments, because it can be applied to predict the TBT mass fraction recovery when the experimental conditions are drawn. This work shows that SPE is a convenient technique for TBT pre-concentration at pico-trace levels and a robust approach: in fact (i) number of different experimental conditions led to satisfactory results and (ii) the participation of two institutes to the experimental work did not impact the developed model. Copyright © 2014 Elsevier B.V. All rights reserved.

Effect of the extent of well purging on laboratory parameters of groundwater samples

NASA Astrophysics Data System (ADS)

Reka Mathe, Agnes; Kohler, Artur; Kovacs, Jozsef

2017-04-01

Chemicals reaching groundwater cause water quality deterioration. Reconnaissance and remediation demands high financial and human resources. Groundwater samples are important sources of information. Representativity of these samples is fundamental to decision making. According to relevant literature the way of sampling and the sampling equipment can affect laboratory concentrations measured in samples. Detailed and systematic research on this field is missing from even international literature. Groundwater sampling procedures are regulated worldwide. Regulations describe how to sample a groundwater monitoring well. The most common element in these regulations is well purging prior to sampling. The aim of purging the well is to avoid taking the sample from the stagnant water instead of from formation water. The stagnant water forms inside and around the well because the well casing provides direct contact with the atmosphere, changing the physico-chemical composition of the well water. Sample from the stagnant water is not representative of the formation water. Regulations regarding the extent of the purging are different. Purging is mostly defined as multiply (3-5) well volumes, and/or reaching stabilization of some purged water parameters (pH, specific conductivity, etc.). There are hints for sampling without purging. To define the necessary extent of the purging repeated pumping is conducted, triplicate samples are taken at the beginning of purging, at one, two and three times well volumes and at parameter stabilization. Triplicate samples are the means to account for laboratory errors. The subsurface is not static, the test is repeated 10 times. Up to now three tests were completed.

Investigation of a novel protonic/electronic ceramic composite material as a candidate for hydrogen separation membranes

NASA Astrophysics Data System (ADS)

Fish, Jason S.

A novel ceramic protonic/electronic conductor composite BaCe 0.2Zr0.7Y0.1O3-delta / Sr0.95 Ti0.9Nb0.1O3-delta (BCZY27/STN95: BS27) has been synthesized, and its electrical properties and hydrogen permeability have been investigated. The volume ratio of the STN95 phase was varied from 50 - 70 % to test the effects on conductivity and hydrogen permeability. BCZY27 and STN95 powders were prepared by solid-state reaction, and membrane samples were fabricated through conventional and spark plasma sintering techniques. The phase composition, density, and microstructure were compared between the sintering methodologies. Total conductivities of 0.01 - 0.06 S·cm -1 were obtained in wet (+1 % H2O) dilute H2/(N 2, He, Ar) from 600 - 800 °C for 50 volume % STN95. With increasing STN content (60 and 70 volume %), conductivity generally increased, though remained lower than predicted by standard effective medium models, even at 70 volume % STN95. A new effective medium model was proposed, which accounted for an interfacial resistance term associated with the heterojunctions formed between the BCZY27 and STN95 phases. Better fits for the measured data were achieved with this new method, although some effects remain unexplained. Discrepancies between the model and experiment were attributed to space charge effects, grain boundary resistances, and insulating impurity phase formation during synthesis. Dense BS27 samples were tested for high-temperature hydrogen permeation and a measured flux of 0.006 mumol·cm-2·s -1 was recorded for a 50 volume % STN95 sample at 700 °C, using dry argon as a sweep gas. This value represents a modest improvement on other ceramic composite membranes, but remains short of targets for commercialization. Persistent leaks in the flux experiments generated a shallower hydrogen gradient across the samples, although this p(H2) on the sweep side simultaneously decreased the oxygen partial pressure gradient across the sample and preserved the reduced state of the membrane. The addition of thin palladium layers (100 nm) to another 50 volume % STN95 sample increased the flux five-fold to 0.026 mumol·cm-2·s -1 at 700 °C. Experiments on 60 and 70 volume % STN95 samples revealed no measurable hydrogen flux, which was attributed to the proton-conducting BCZY27 phase being non-percolating for these compositions.

Atmospheric deposition effects on the chemistry of a stream in Northeastern Georgia

USGS Publications Warehouse

Buell, G.R.; Peters, N.E.

1988-01-01

The quantity and quality of precipitation and streamwater were measured from August 1985 through September 1986 in the Brier Creek watershed, a 440-ha drainage in the Southern Blue Ridge Province of northeastern Georgia, to determine stream sensitivity to acidic deposition. Precipitation samples collected at 2 sites had a volume-weighted average pH of 4.40 whereas stream samples collected near the mouth of Brier Creek had a discharge-weighted average pH of 6.70. Computed solute fluxes through the watershed and observed changes in streamwater chemistry during stormflow suggest that cation exchange, mineral weathering, SO42- adsorption by the soil, and groundwater discharge to the stream are probable factors affecting neutralization of precipitation acidity. Net solute fluxes for the watershed indicate that, of the precipitation input, > 99% of the H+, 93% of the NH4+ and NO3-, and 77% of the SO42- were retained. Sources within the watershed yielded base cations, Cl-, and HCO3- and accounted for 84, 47, and 100% of the net transport, respectively. Although streamwater SO42- and NO3- concentrations increased during stormflow, peak concentrations of these anions were much less than average concentrations in the precipitation. This suggests retention of these solutes occurs even when water residence time is short.The quantity and quality of precipitation and streamwater were measured from August 1985 through September 1986 in the Brier Creek watershed, a 440-ha drainage in the Southern Blue Ridge Province of northeastern Georgia, to determine stream sensitivity to acidic deposition. Precipitation samples collected at 2 sites had a volume-weighted average pH of 4.40 whereas stream samples collected near the mouth of Brier Creek had a discharge-weighted average pYH of 6.70. Computed solute fluxes through the watershed and observed changes in streamwater chemistry drying stormflow suggest that cation exchange, mineral weathering, SO42- adsorption by the soil, and groundwater discharge to the stream are probable factors affecting neutralization of precipitation acidity. Although streamwater SO42- and NO3- concentrations increased during stormflow, peak concentrations of these anions were much less than average concentrations in the precipitation. This suggests retention of these solutes occurs even when water residence time is short.

Application of response surface methodology for determination of methyl red in water samples by spectrophotometry method.

PubMed

Khodadoust, Saeid; Ghaedi, Mehrorang

2014-12-10

In this study a rapid and effective method (dispersive liquid-liquid microextraction (DLLME)) was developed for extraction of methyl red (MR) prior to its determination by UV-Vis spectrophotometry. Influence variables on DLLME such as volume of chloroform (as extractant solvent) and methanol (as dispersive solvent), pH and ionic strength and extraction time were investigated. Then significant variables were optimized by using a Box-Behnken design (BBD) and desirability function (DF). The optimized conditions (100μL of chloroform, 1.3mL of ethanol, pH 4 and 4% (w/v) NaCl) resulted in a linear calibration graph in the range of 0.015-10.0mgmL(-1) of MR in initial solution with R(2)=0.995 (n=5). The limits of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.015mgmL(-1), respectively. Finally, the DLLME method was applied for determination of MR in different water samples with relative standard deviation (RSD) less than 5% (n=5). Copyright © 2014 Elsevier B.V. All rights reserved.

Preconcentration of valsartan by dispersive liquid-liquid microextraction based on solidification of floating organic drop and its determination in urine sample: Central composite design.

PubMed

Pebdani, Arezou Amiri; Shabani, Ali Mohammad Haji; Dadfarnia, Shayesteh; Talebianpoor, Mohammad Sharif; Khodadoust, Saeid

2016-05-01

In this work, a fast, easy, and efficient dispersive liquid-liquid microextraction method based on solidification of floating organic drop followed by high-performance liquid chromatography with UV detection was developed for the separation/preconcentration and determination of the drug valsartan. Experimental design was applied for the optimization of the effective variables (such as volume of extracting and dispersing solvents, ionic strength, and pH) on the extraction efficiency of valsartan from urine samples. The optimized values were 250.0 μL ethanol, 65.0 μL 1-dodecanol, 4.0% w/v NaCl, pH 3.8, 1.0 min extraction time, and 4.0 min centrifugation at 4000 rpm min(-1) . The linear response (r(2) = 0.997) was obtained in the range of 0.013-10.0 μg mL(-1) with a limit of detection of 4.0 ng mL(-1) and relative standard deviations of less than 5.0 % (n = 6). © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A mathematical model of the volume, pH, and ion content regulation in reticulocytes. Application to the pathophysiology of sickle cell dehydration.

PubMed Central

Lew, V L; Freeman, C J; Ortiz, O E; Bookchin, R M

1991-01-01

We developed a mathematical model of the reticulocyte, seeking to explain how a cell with similar volume but much higher ionic traffic than the mature red cell (RBC) regulates its volume, pH, and ion content in physiological and abnormal conditions. Analysis of the fluxbalance required by reticulocytes to conserve volume and composition predicted the existence of previously unsuspected Na(+)-dependent Cl- entry mechanisms. Unlike mature RBCs, reticulocytes did not tend to return to their original state after brief perturbations. The model predicted hysteresis and drift in cell pH, volume, and ion contents after transient alterations in membrane permeability or medium composition; irreversible cell dehydration could thus occur by brief K+ permeabilization, transient medium acidification, or the replacement of external Na+ with an impermeant cation. Both the hysteresis and drift after perturbations were shown to depend on the pHi dependence of the K:Cl cotransport, a major reticulocyte transporter. This behavior suggested a novel mechanism for the generation of irreversibly sickled cells directly from reticulocytes, rather than in a stepwise, progressive manner from discocytes. Experimental tests of the model's predictions and the hypothesis are described in the following paper. PMID:1985088

Magnetic solid-phase extraction combined with graphite furnace atomic absorption spectrometry for speciation of Cr(III) and Cr(VI) in environmental waters.

PubMed

Jiang, Hong-mei; Yang, Ting; Wang, Yan-hong; Lian, Hong-zhen; Hu, Xin

2013-11-15

A new approach of magnetic solid phase extraction (MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) has been developed for the speciation of Cr(III) and Cr(VI) using zincon-immobilized silica-coated magnetic Fe3O4 nanoparticles (Zincon-Si-MNPs) as the MSPE absorbent. Cr(III) was quantitatively reserved on the absorbent at pH 9.1 while total Cr was reserved at pH 6.5. The absorbed Cr species were eluted by using 2 mol/L HCl and detected by GFAAS. The concentration of Cr(VI) could be calculated by subtracting Cr(III) from total Cr. All the parameters affecting the separation and extraction efficiency of Cr species such as pH, extraction time, concentration and volume of eluent, sample volume and influence of co-existing ions were systematically examined and the optimized conditions were established accordingly. The detection limit (LOD) of the method was 0.016 and 0.011 ng mL(-1) for Cr(III) and Cr(VI), respectively, with the enrichment factor of 100 and 150. The precisions of this method (Relative standard deviation, RSD, n=7) for Cr(III) and Cr(VI) at 0.1 ng mL(-1) were 6.0% and 6.2%, respectively. In order to validate the proposed method, a certified reference material of environmental water was analyzed, and the result of Cr speciation was in good agreement with the certified value. This MSPE-GFAAS method has been successfully applied for the speciation of Cr(III) and Cr(VI) in lake and tap waters with the recoveries of 88-109% for the spiked samples. Moreover, the MSPE separation mechanism of Cr(III) and Cr(VI) based on their adsorption-desorption on Zincon-Si-MNPs has been explained through various spectroscopic characterization. © 2013 Elsevier B.V. All rights reserved.

Biogas production from pineapple core - A preliminary study

NASA Astrophysics Data System (ADS)

Jehan, O. S.; Sanusi, S. N. A.; Sukor, M. Z.; Noraini, M.; Buddin, M. M. H. S.; Hamid, K. H. K.

2017-09-01

Anaerobic digestion of pineapple waste was investigated by using pineapple core as the sole substrate. Pineapple core was chosen due to its high total sugar content thus, indicating high amount of fermentable sugar. As digestion process requires the involvement of microorganisms, wastewater from the same industry was added in the current study at ratio of 1:1 by weight. Two different sources of wastewater (Point 1 and Point 2) were used in this study to distinguish the performance of microorganism consortia in both samples. The experiment was conducted by using a lab scale batch anaerobic digester made up from 5L container with separate gas collecting system. The biogas produced was collected by using water displacement method. The experiment was conducted for 30 days and the biogas produced was collected and its volume was recorded at 3 days interval. Based on the data available, wastewater from the first point recorded higher volume of biogas with the total accumulated biogas volume is 216.1 mL. Meanwhile, wastewater sample from Point 2 produced a total of 140.5 mL of biogas, by volume. The data shows that the origin and type of microorganism undeniably play significant role in biogas production. In fact, other factors; pH of wastewater and temperature were also known to affect biogas production. The anaerobic digestion is seen as the promising and sustainable alternatives to current disposal method.

Fused silica capillaries with two segments of different internal diameters and inner surface roughnesses prepared by etching with supercritical water and used for volume coupling electrophoresis.

PubMed

Horká, Marie; Karásek, Pavel; Roth, Michal; Šlais, Karel

2017-05-01

In this work, single-piece fused silica capillaries with two different internal diameter segments featuring different inner surface roughness were prepared by new etching technology with supercritical water and used for volume coupling electrophoresis. The concept of separation and online pre-concentration of analytes in high conductivity matrix is based on the online large-volume sample pre-concentration by the combination of transient isotachophoretic stacking and sweeping of charged proteins in micellar electrokinetic chromatography using non-ionogenic surfactant. The modified surface roughness step helped to the significant narrowing of the zones of examined analytes. The sweeping and separating steps were accomplished simultaneously by the use of phosphate buffer (pH 7) containing ethanol, non-ionogenic surfactant Brij 35, and polyethylene glycol (PEG 10000) after sample injection. Sample solution of a large volume (maximum 3.7 μL) dissolved in physiological saline solution was injected into the wider end of capillary with inlet inner diameter from 150, 185 or 218 μm. The calibration plots were linear (R 2 ∼ 0.9993) over a 0.060-1 μg/mL range for the proteins used, albumin and cytochrome c. The peak area RSDs from at least 20 independent measuremens were below 3.2%. This online pre-concentration technique produced a more than 196-fold increase in sensitivity, and it can be applied for detection of, e.g. the presence of albumin in urine (0.060 μg/mL). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid-phase extraction-fluorimetric high performance liquid chromatographic determination of domoic acid in natural seawater mediated by an amorphous titania sorbent.

PubMed

Chan, Ivy O M; Tsang, Vic W H; Chu, K K; Leung, S K; Lam, Michael H W; Lau, T C; Lam, Paul K S; Wu, Rudolf S S

2007-01-30

The feasibility of using sol-gel amorphous titania (TiO2) as a solid-phase sorbent for the pre-concentration of domoic acid (DA), a potent amnesic shellfish poisoning (ASP) toxin, directly from seawater was explored. The sol-gel titania material is able to adsorb DA from seawater, via the formation of ester-linkage between the carboxylic moieties of DA and the Ti-OH groups on the sorbent surface, at low pH and desorb it at high pH. The chemisorption process is not significantly interfered by the seawater matrix. The optimum pH values for the adsorption and desorption of DA were found to be pH 4 and 11, respectively. The optimal sorbent loading for the batch-type solid-phase extraction of DA was 0.67 mg-TiO2 ng-DA(-1) and adsorption equilibrium was achieved in 2 h at room temperature. The desorbed DA in 500 microL of 0.1 M alkaline borate buffer can be directly derviatized by 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) in aqueous media for fluorimetric HPLC quantification. Analyte recovery, repeatability and detection limit of this titania SPE-fluorimetric HPLC determination are 89%, 6.2% and 120 pg-DA mL(-1) (n=7, P<0.05), respectively, for a sample volume of 30 mL. This titania SPE technique should also be applicable to the pre-concentration of other polar carboxylate- and phosphonate-containing biomolecules and pharmaceuticals in complex and interfering environmental sample matrices.

Pharmacokinetics and pharmacodynamics of famotidine and ranitidine in critically ill children.

PubMed

Madani, Shailender; Kauffman, Ralph; Simpson, Pippa; Lehr, Victoria Tutag; Lai, Mary Lieh; Sarniak, Ashok; Tolia, Vasundhara

2014-02-01

To characterize and compare acid suppression (pharmacodynamics) and pharmacokinetics of IV famotidine and ranitidine in critically ill children at risk for stress gastritis. Single-blind, randomized study in PICU patients 6 months to 18 years requiring mechanical ventilation with continuous gastric pH monitoring, randomized to IV famotidine 12 mg/m(2) or ranitidine 60 mg/m(2) when gastric pH < 4.0 >1 hour with serial blood sampling following first dose. Twenty-four children randomized to either famotidine (n = 12) or ranitidine (n = 12). Sixteen out of twenty-four completed both PK and PD study arms (7/12 famotidine; 4.7 ± 3.4 years; 9/12 ranitidine; 6.6 ± 4.7 years; p = 0.38). Time to gastric pH 4.0 and total time pH above 4.0 similar with no difference in pH at 6 and 12 hours (p > 0.2). No difference between drugs in clearance, volume of distribution and half-life (p > 0.05). Ratio of AUC pH to AUC drug concentration 0-12 hours after first dose was significantly greater for famotidine (0.06849 ± 0.01460 SD) than ranitidine (0.02453 ± 0.01448; p < 0.001) demonstrating greater potency of famotidine. pH lowering efficacy of both drugs is similar. Greater potency of famotidine may offer clinical advantage due to lower drug exposure and less frequent dosing to achieve same pH lowering effect. © 2013, The American College of Clinical Pharmacology.

In vitro degradation of ZM21 magnesium alloy in simulated body fluids.

PubMed

Witecka, Agnieszka; Bogucka, Aleksandra; Yamamoto, Akiko; Máthis, Kristián; Krajňák, Tomáš; Jaroszewicz, Jakub; Święszkowski, Wojciech

2016-08-01

In vitro degradation behavior of squeeze cast (CAST) and equal channel angular pressed (ECAP) ZM21 magnesium alloy (2.0wt% Zn-0.98wt% Mn) was studied using immersion tests up to 4w in three different biological environments. Hanks' Balanced Salt Solution (Hanks), Earle's Balanced Salt Solution (Earle) and Eagle minimum essential medium supplemented with 10% (v/v) fetal bovine serum (E-MEM+10% FBS) were used to investigate the effect of carbonate buffer system, organic compounds and material processing on the degradation behavior of the ZM21 alloy samples. Corrosion rate of the samples was evaluated by their Mg(2+) ion release, weight loss and volume loss. In the first 24h, the corrosion rate sequence of the CAST samples was as following: Hanks>E-MEM+10% FBS>Earle. However, in longer immersion periods, the corrosion rate sequence was Earle>E-MEM+10% FBS≥Hanks. Strong buffering effect provided by carbonate buffer system helped to maintain the pH avoiding drastic increase of the corrosion rate of ZM21 in the initial stage of immersion. Organic compounds also contributed to maintain the pH of the fluid. Moreover, they adsorbed on the sample surface and formed an additional barrier on the insoluble salt layer, which was effective to retard the corrosion of CAST samples. In case of ECAP, however, this effect was overcome by the occurrence of strong localized corrosion due to the lower pH of the medium. Corrosion of ECAP samples was much greater than that of CAST, especially in Hanks, due to higher sensitivity of ECAP to localized corrosion and the presence of Cl(-). The present work demonstrates the importance of using an appropriate solution for a reliable estimation of the degradation rate of Mg-base degradable implants in biological environments, and concludes that the most appropriate solution for this purpose is E-MEM+10% FBS, which has the closest chemical composition to human blood plasma. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of heavy metal ions in vegetable samples using a magnetic metal-organic framework nanocomposite sorbent.

PubMed

Hassanpour, Akbar; Hosseinzadeh-Khanmiri, Rahim; Babazadeh, Mirzaagha; Abolhasani, Jafar; Ghorbani-Kalhor, Ebrahim

2015-01-01

This paper describes the synthesis and application of a novel magnetic metal-organic framework (MOF) [(Fe₃O₄-benzoyl isothiocyanate)/Cu₃(benzene-1,3,5-tricarboxylate)₂] to pre-concentrate trace amounts of Cd(II), Pb(II), Zn(II) and Cr(III) ions and their determination by flame atomic absorption spectrometry. A Box-Behnken design was used to find the parameters affecting the pre-concentration procedure through response surface methodology. Three factors including uptake time, amount of the magnetic sorbent and pH of the sample were selected as affecting factors in the sorption step, and four factors including type, volume and concentration of the eluent as well as the elution time were selected in the elution step for the optimisation study. The opted values were 30 mg, 10.1 min, 5.9, EDTA, 4.0 ml, 0.57 mol l(-1) EDTA solution and 13.0 min for the amount of the magnetic sorbent, uptake time, pH of the sample, type, volume, concentration of the eluent, and elution time, respectively. The limits of detection (LODs) were 0.12, 0.7, 0.16, and 0.4 ng ml(-1) for Cd(II), Pb(II), Zn(II) and Cr(III) ions, respectively. The relative standard deviations (RSDs) of the method were less than 7.2% for five separate batch experiments for the determination of 30 μg l(-1) of Cd(II), Pb(II), Zn(II) and Cr(III) ions. The sorption capacity of the [(Fe₃O₄-benzoyl isothiocyanate)/MOF] was 175 mg g(-1) for Cd(II), 168 mg g(-1) for Pb(II), 210 mg g(-1) for Zn(II) and 196 mg g(-1) for Cr(III). It was found that the magnetic MOF nanocomposite demonstrated a higher capacity compared with Fe₃O₄-benzoyl isothiocyanate. Finally, the magnetic MOF nanocomposite was successfully applied to the rapid extraction of trace amounts of the heavy metal ions from vegetable samples.

Strategic Studies Quarterly. Volume 8, Number 1, Spring 2014

DTIC Science & Technology

2014-01-01

Charles E. Costanzo, PhD Christopher M. Hemmer, PhD Kimberly A. Hudson, PhD Nori Katagiri, PhD Zachary J . Zwald, PhD Strategic Studies Quarterly (SSQ...first successful carrier-based takeoff and landing with the Jian-15 ( J -15) in November 2012, certified its first group of aircraft carrier pilots and...September 2013.3 The Liaoning will continue to conduct short deployments and shipboard aviation training until 2015 to 2016, when China’s first J -15

Effect of rapid cooling and acidic pH on cellular homeostasis of Pectinatus frisingensis, a strictly anaerobic beer-spoilage bacterium.

PubMed

Chihib, N E; Tholozan, J L

1999-06-01

Pectinatus frisingensis is a strictly anaerobic mesophilic bacterium involved in bottled beer spoilage. Cellular volume, adenylate energy charge, intracellular pH and intracellular potassium concentration measurements were performed in late exponential-phase cell suspensions placed in different physiological conditions, to evaluate the capability of this bacterium to maintain cellular homeostasis. The intracellular pH was calculated from the intracellular accumulation of a [carboxyl-14C]benzoic acid. Optimum physiological conditions were the presence of a carbon source and pH of 6.2, hostile conditions were a pH 4.5, absence of a carbon source, and rapid cooling treatment. The cell was able to maintain a higher intracellular pH than the external pH under all conditions. Intracellular volume was lower at pH 4.5 than at pH 6.2. A low net potassium efflux rate was routinely measured in starving cells, while glucose addition promoted immediate net potassium uptake from the medium. Cooling treatment resulted in sudden net potassium efflux from the cell, a decrease of the intracellular pH, and low modifications of the adenylate energy charge in metabolizing-glucose cell suspensions. Thus, cold treatment perturbs the P. frisingensis homeostasis but the bacteria were able to restore their homeostasis in the presence of a carbon source, and under warm conditions.

Iron Oxide Silica Derived from Sol-Gel Synthesis

PubMed Central

Darmawan, Adi; Smart, Simon; Julbe, Anne; Diniz da Costa, João Carlos

2011-01-01

In this work we investigate the effect of iron oxide embedded in silica matrices as a function of Fe/Si molar ratio and sol pH. To achieve homogeneous dispersion of iron oxide particles, iron nitrate nonahydrate was dissolved in hydrogen peroxide and was mixed with tetraethyl orthosilicate and ethanol in a sol-gel synthesis method. Increasing the calcination temperature led to a reduction in surface area, although the average pore radius remained almost constant at about 10 Å, independent of the Fe/Si molar ratio or sol pH. Hence, the densification of the matrix was accompanied by similar reduction in pore volume. However, calcination at 700 °C resulted in samples with similar surface area though the iron oxide content increased from 5% to 50% Fe/Si molar ratio. As metal oxide particles have lower surface area than polymeric silica structures, these results strongly suggest that the iron oxides opposed the silica structure collapse. The effect of sol pH was found to be less significant than the Fe/Si molar ratio in the formation of molecular sieve structures derived from iron oxide silica. PMID:28879999

Cloud point extraction and flame atomic absorption spectrometric determination of cadmium and nickel in drinking and wastewater samples.

PubMed

Naeemullah; Kazi, Tasneem G; Shah, Faheem; Afridi, Hassan I; Baig, Jameel Ahmed; Soomro, Abdul Sattar

2013-01-01

A simple method for the preconcentration of cadmium (Cd) and nickel (Ni) in drinking and wastewater samples was developed. Cloud point extraction has been used for the preconcentration of both metals, after formation of complexes with 8-hydroxyquinoline (8-HQ) and extraction with the surfactant octylphenoxypolyethoxyethanol (Triton X-114). Dilution of the surfactant-rich phase with acidified ethanol was performed after phase separation, and the Cd and Ni contents were measured by flame atomic absorption spectrometry. The experimental variables, such as pH, amounts of reagents (8-HQ and Triton X-114), temperature, incubation time, and sample volume, were optimized. After optimization of the complexation and extraction conditions, enhancement factors of 80 and 61, with LOD values of 0.22 and 0.52 microg/L, were obtained for Cd and Ni, respectively. The proposed method was applied satisfactorily for the determination of both elements in drinking and wastewater samples.

Minimizing back exchange in the hydrogen exchange-mass spectrometry experiment.

PubMed

Walters, Benjamin T; Ricciuti, Alec; Mayne, Leland; Englander, S Walter

2012-12-01

The addition of mass spectrometry (MS) analysis to the hydrogen exchange (HX) proteolytic fragmentation experiment extends powerful HX methodology to the study of large biologically important proteins. A persistent problem is the degradation of HX information due to back exchange of deuterium label during the fragmentation-separation process needed to prepare samples for MS measurement. This paper reports a systematic analysis of the factors that influence back exchange (solution pH, ionic strength, desolvation temperature, LC column interaction, flow rates, system volume). The many peptides exhibit a range of back exchange due to intrinsic amino acid HX rate differences. Accordingly, large back exchange leads to large variability in D-recovery from one residue to another as well as one peptide to another that cannot be corrected for by reference to any single peptide-level measurement. The usual effort to limit back exchange by limiting LC time provides little gain. Shortening the LC elution gradient by 3-fold only reduced back exchange by ~2%, while sacrificing S/N and peptide count. An unexpected dependence of back exchange on ionic strength as well as pH suggests a strategy in which solution conditions are changed during sample preparation. Higher salt should be used in the first stage of sample preparation (proteolysis and trapping) and lower salt (<20 mM) and pH in the second stage before electrospray injection. Adjustment of these and other factors together with recent advances in peptide fragment detection yields hundreds of peptide fragments with D-label recovery of 90% ± 5%.

Minimizing Back Exchange in the Hydrogen Exchange-Mass Spectrometry Experiment

NASA Astrophysics Data System (ADS)

Walters, Benjamin T.; Ricciuti, Alec; Mayne, Leland; Englander, S. Walter

2012-12-01

The addition of mass spectrometry (MS) analysis to the hydrogen exchange (HX) proteolytic fragmentation experiment extends powerful HX methodology to the study of large biologically important proteins. A persistent problem is the degradation of HX information due to back exchange of deuterium label during the fragmentation-separation process needed to prepare samples for MS measurement. This paper reports a systematic analysis of the factors that influence back exchange (solution pH, ionic strength, desolvation temperature, LC column interaction, flow rates, system volume). The many peptides exhibit a range of back exchange due to intrinsic amino acid HX rate differences. Accordingly, large back exchange leads to large variability in D-recovery from one residue to another as well as one peptide to another that cannot be corrected for by reference to any single peptide-level measurement. The usual effort to limit back exchange by limiting LC time provides little gain. Shortening the LC elution gradient by 3-fold only reduced back exchange by ~2 %, while sacrificing S/N and peptide count. An unexpected dependence of back exchange on ionic strength as well as pH suggests a strategy in which solution conditions are changed during sample preparation. Higher salt should be used in the first stage of sample preparation (proteolysis and trapping) and lower salt (<20 mM) and pH in the second stage before electrospray injection. Adjustment of these and other factors together with recent advances in peptide fragment detection yields hundreds of peptide fragments with D-label recovery of 90 % ± 5 %.

Switchable polarity solvent for liquid phase microextraction of Cd(II) as pyrrolidinedithiocarbamate chelates from environmental samples.

PubMed

Yilmaz, Erkan; Soylak, Mustafa

2015-07-30

A switchable polarity solvent was synthesized from triethylamine (TEA)/water/CO2 (Dry ice) via proton transfer reaction has been used for the microextraction of cadmium(II) as pyrrolidinedithiocarbamate (APDC) chelate. Cd(II)-APDC chelate was extracted into the switchable polarity solvent drops by adding 2 mL 10 M sodium hydroxide solution. Analytical parameters affecting the complex formation and microextraction efficiency such as pH, amount of ligand, volume of switchable polarity solvent and NaOH, sample volume were optimized. The effects of foreign ions were found tolerably. Under optimum conditions, the detection limit was 0.16 μg L(-1) (3Sb/m, n = 7) and the relative standard deviation was 5.4% (n = 7). The method was validated by the analysis of certified reference materials (TMDA-51.3 fortified water, TMDA-53.3 fortified water and SPS-WW2 waste water, 1573a Tomato Leaves and Oriental Basma Tobacco Leaves (INCT-OBTL-5)) and addition/recovery tests. The method was successfully applied to determination of cadmium contents of water, vegetable, fruit and cigarette samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation and use of maize tassels' activated carbon for the adsorption of phenolic compounds in environmental waste water samples.

PubMed

Olorundare, O F; Msagati, T A M; Krause, R W M; Okonkwo, J O; Mamba, B B

2015-04-01

The determination and remediation of three phenolic compounds bisphenol A (BPA), ortho-nitrophenol (o-NTP), parachlorophenol (PCP) in wastewater is reported. The analysis of these molecules in wastewater was done using gas chromatography (GC) × GC time-of-flight mass spectrometry while activated carbon derived from maize tassel was used as an adsorbent. During the experimental procedures, the effect of various parameters such as initial concentration, pH of sample solution, eluent volume, and sample volume on the removal efficiency with respect to the three phenolic compounds was studied. The results showed that maize tassel produced activated carbon (MTAC) cartridge packed solid-phase extraction (SPE) system was able to remove the phenolic compounds effectively (90.84-98.49%, 80.75-97.11%, and 78.27-97.08% for BPA, o-NTP, and PCP, respectively). The MTAC cartridge packed SPE sorbent performance was compared to commercially produced C18 SPE cartridges and found to be comparable. All the parameters investigated were found to have a notable influence on the adsorption efficiency of the phenolic compounds from wastewaters at different magnitudes.

Pipette-tip solid-phase extraction using poly(1-vinylimidazole-co-trimethylolpropane trimethacrylate) as a new molecularly imprinted polymer in the determination of avermectins and milbemycins in fruit juice and water samples.

PubMed

Teixeira, Roseane Andrade; Flores, Diego Hernando Ângulo; da Silva, Ricky Cássio Santos; Dutra, Flávia Viana Avelar; Borges, Keyller Bastos

2018-10-01

A simple HPLC method was developed for the determination of abamectin (ABA), eprinomectin (EPR), and moxidectin (MOX). Pipette-tip molecularly imprinted polymer solid-phase extraction (PT-MIP-SPE) using poly(1-vinylimidazole-co-trimethylolpropane trimethacrylate) as a selective adsorbent material was studied in detail, including the washing solvent, type and volume of eluent, pH, quantity of adsorbent material and sample volume. The performance criteria for linearity, sensitivity, precision, accuracy, recovery, robustness and stability have been assessed and were within the recommended guidelines. The mean extraction recoveries/relative standard deviation for ABA 1b, EPR, ABA 1a and MOX were 98.77 ± 3.82%, 88.19 ± 2.57%, 110.54 ± 1.52% and 100.42 ± 0.59%, respectively. Finally, the results proved that PT-MIP-SPE coupled to HPLC-UV is an economical, simple and easy-to-perform technique, and presented a high potential for extraction of macrocyclic lactones in mineral water and grape and juice samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

Simultaneous extraction and quantification of albendazole and triclabendazole using vortex-assisted hollow-fiber liquid-phase microextraction combined with high-performance liquid chromatography.

PubMed

Asadi, Mohammad; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh

2016-06-01

A novel, simple, and rapid vortex-assisted hollow-fiber liquid-phase microextraction method was developed for the simultaneous extraction of albendazole and triclabendazole from various matrices before their determination by high-performance liquid chromatography with fluorescence detection. Several factors influencing the microextraction efficiency including sample pH, nature and volume of extraction solvent, ionic strength, vortex time, and sample volume were investigated and optimized. Under the optimal conditions, the limits of detection were 0.08 and 0.12 μg/L for albendazole and triclabendazole, respectively. The calibration curves were linear in the concentration ranges of 0.3-50.0 and 0.4-50.0 μg/L with the coefficients of determination of 0.9999 and 0.9995 for albendazole and triclabendazole, respectively. The interday and intraday relative standard deviations for albendazole and triclabendazole at three concentration levels (1.0, 10.0, and 30.0 μg/L) were in the range of 6.0-11.0 and 5.0-7.9%, respectively. The developed method was successfully applied to determine albendazole and triclabendazole in water, milk, honey, and urine samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preconcentration of Zn2+ and Cu2+ ions from food and vegetable samples using modified activated carbon.

PubMed

Ghaedi, M; Tavallali, H; Montazerozohori, M; Zahedi, E; Amirineko, M; Khodadoust, S; Karimipour, G

2012-11-01

In this work, two N/S-containing chelating agents 2-(4-methoxybenzylideneamino)thiophenol (2-4-MBAT) and 2-(4-chlorobenzylideneamino) benzenethiol (2-4-CBABT) were synthesized as new sorbents and were used for preconcentration of Zn(2+) and Cu(2+) ions in food and vegetable samples. In the proposed procedure, the trace amount of Zn(2+) and Cu(2+) ions from 250 mL of sample solution at pH = 5.0 was preconcentrated by 1 g of activated carbon (AC) loaded with 15 mg of 2-4-MBAT and 2-4-CBABT separately. The breakthrough volumes (maximum sample volume that their metal ions quantitatively can be enriched) for solid-phase extraction (SPE) procedure based on the AC modified with 2-4-MBAT and 2-4-CBABT were 800 and 750 mL, respectively. The sorbed Zn(2+) and Cu(2+) ions were efficiently eluted by 8 mL of 4 mol L(-1) HNO(3) and preconcentration factor of 112.5 and 93.7 and experimental enhancement factor of 30 and 35 ions were obtained for Zn(2+) and Cu(2+), respectively. The application of this enrichment procedure allowed the extraction of trace metal ions with recoveries exceeding of 90%.

Determination of dissolved aluminum in water samples

USGS Publications Warehouse

Afifi, A.A.

1983-01-01

A technique has been modified for determination of a wide range of concentrations of dissolved aluminum (Al) in water and has been tested. In this technique, aluminum is complexed with 8-hydroxyquinoline at pH 8.3 to minimize interferences, then extracted with methyl isobutyl ketone (MIBK). The extract is analyzed colorimetrically at 395 nm. This technique is used to analyze two forms of monomeric Al, nonlabile (organic complexes) and labile (free, Al, Al sulfate, fluoride and hydroxide complexes). A detection limit 2 ug/L is possible with 25-ml samples and 10-ml extracts. The detection limit can be decreased by increasing the volume of the sample and (or) decreasing the volume of the methyl isobutyl ketone extract. The analytical uncertainty of this method is approximately + or - 5 percent. The standard addition technique provides a recovery test for this technique and ensures precision in samples of low Al concentrations. The average percentage recovery of the added Al plus the amount originally present was 99 percent. Data obtained from analyses of filtered standard solutions indicated that Al is adsorbed on various types of filters. However, the relationship between Al concentrations and adsorption remains linear. A test on standard solutions also indicated that Al is not adsorbed on nitric acid-washed polyethylene and polypropylene bottle wells. (USGS)

Ionic liquid-based microwave-assisted dispersive liquid-liquid microextraction and derivatization of sulfonamides in river water, honey, milk, and animal plasma.

PubMed

Xu, Xu; Su, Rui; Zhao, Xin; Liu, Zhuang; Zhang, Yupu; Li, Dan; Li, Xueyuan; Zhang, Hanqi; Wang, Ziming

2011-11-30

The ionic liquid-based microwave-assisted dispersive liquid-liquid microextraction (IL-based MADLLME) and derivatization was applied for the pretreatment of six sulfonamides (SAs) prior to the determination by high-performance liquid chromatography (HPLC). By adding methanol (disperser), fluorescamine solution (derivatization reagent) and ionic liquid (extraction solvent) into sample, extraction, derivatization, and preconcentration were continuously performed. Several experimental parameters, such as the type and volume of extraction solvent, the type and volume of disperser, amount of derivatization reagent, microwave power, microwave irradiation time, pH of sample solution, and ionic strength were investigated and optimized. When the microwave power was 240 W, the analytes could be derivatized and extracted simultaneously within 90 s. The proposed method was applied to the analysis of river water, honey, milk, and pig plasma samples, and the recoveries of analytes obtained were in the range of 95.0-110.8, 95.4-106.3, 95.0-108.3, and 95.7-107.7, respectively. The relative standard deviations varied between 1.5% and 7.3% (n=5). The results showed that the proposed method was a rapid, convenient and feasible method for the determination of SAs in liquid samples. Copyright © 2011 Elsevier B.V. All rights reserved.

Strategic Studies Quarterly. Volume 5, Number 3. Fall 2011

DTIC Science & Technology

2011-01-01

Christopher M. Hemmer, PhD Kimberly A. Hudson, PhD Col Basil S. Norris Jr., USAF, Retired Gary J. Schaub, PhD Strategic Studies Quarterly (SSQ...29). Sloterdijk goes on to describe a direct progression from the wartime use of poi­ son gas to the postwar development of pesticides and of Zyklon

Hydrothermal carbonization (HTC) of wheat straw: influence of feedwater pH prepared by acetic acid and potassium hydroxide.

PubMed

Reza, M Toufiq; Rottler, Erwin; Herklotz, Laureen; Wirth, Benjamin

2015-04-01

In this study, influence of feedwater pH (2-12) was studied for hydrothermal carbonization (HTC) of wheat straw at 200 and 260°C. Acetic acid and KOH were used as acidic and basic medium, respectively. Hydrochars were characterized by elemental and fiber analyses, SEM, surface area, pore volume and size, and ATR-FTIR, while HTC process liquids were analyzed by HPLC and GC. Both hydrochar and HTC process liquid qualities vary with feedwater pH. At acidic pH, cellulose and elemental carbon increase in hydrochar, while hemicellulose and pseudo-lignin decrease. Hydrochars produced at pH 2 feedwater has 2.7 times larger surface area than that produced at pH 12. It also has the largest pore volume (1.1 × 10(-1) ml g(-1)) and pore size (20.2 nm). Organic acids were increasing, while sugars were decreasing in case of basic feedwater, however, phenolic compounds were present only at 260°C and their concentrations were increasing in basic feedwater. Copyright © 2015 Elsevier Ltd. All rights reserved.

A thermal and chemical degradation approach to decipher pristane and phytane precursors in sedimentary organic matter

USGS Publications Warehouse

Koopmans, M.P.; Rijpstra, W.I.C.; Klapwijk, M.M.; De Leeuw, J. W.; Lewan, M.D.; Sinninghe, Damste J.S.

1999-01-01

A thermal and chemical degradation approach was followed to determine the precursors of pristane (Pr) and phytane (Ph) in samples from the Gessoso-solfifera, Ghareb and Green River Formations. Hydrous pyrolysis of these samples yields large amounts of Pr and Ph carbon skeletons, indicating that their precursors are predominantly sequestered in high-molecular-weight fractions. However, chemical degradation of the polar fraction and the kerogen of the unheated samples generally does not release large amounts of Pr and Ph. Additional information on the precursors of Pr and Ph is obtained from flash pyrolysis analyses of kerogens and residues after hydrous pyrolysis and after chemical degradation. Multiple precursors for Pr and Ph are recognised in these three samples. The main increase of the Pr/Ph ratio with increasing maturation temperature, which is associated with strongly increasing amounts of Pr and Ph, is probably due to the higher amount of precursors of Pr compared to Ph, and not to the different timing of generation of Pr and Ph.A thermal and chemical degradation approach was followed to determine the precursors of pristane (Pr) and phytane (Ph) in samples from the Gessoso-solfifera, Ghareb and Green River Formations. Hydrous pyrolysis of these samples yields large amounts of Pr and Ph carbon skeletons, indicating that their precursors are predominantly sequestered in high-molecular-weight fractions. However, chemical degradation of the polar fraction and the kerogen of the unheated samples generally does not release large amounts of Pr and Ph. Additional information on the precursors of Pr and Ph is obtained from flash pyrolysis analyses of kerogens and residues after hydrous pyrolysis and after chemical degradation. Multiple precursors for Pr and Ph are recognised in these three samples. The main increase of the Pr/Ph ratio with increasing maturation temperature, which is associated with strongly increasing amounts of Pr and Ph, is probably due to the higher amount of precursors of Pr compared to Ph, and not to the different timing of generation of Pr and Ph.

Effervescence-assisted dispersive liquid-liquid microextraction using a solid effervescent agent as a novel dispersion technique for the analysis of fungicides in apple juice.

PubMed

Jiang, Wenqing; Chen, Xiaochu; Liu, Fengmao; You, Xiangwei; Xue, Jiaying

2014-11-01

A novel effervescence-assisted dispersive liquid-liquid microextraction method has been developed for the determination of four fungicides in apple juice samples. In this method, a solid effervescent agent is added into samples to assist the dispersion of extraction solvent. The effervescent agent is environmentally friendly and only produces an increase in the ionic strength and a negligible variation in the pH value of the aqueous sample, which does not interfere with the extraction of the analytes. The parameters affecting the extraction efficiency were investigated including the composition of effervescent agent, effervescent agent amount, formulation of effervescent agent, adding mode of effervescent agent, type and volume of extraction solvent, and pH. Under optimized conditions, the method showed a good linearity within the range of 0.05-2 mg/L for pyrimethanil, fludioxonil, and cyprodinil, and 0.1-4 mg/L for kresoxim-methyl, with the correlation coefficients >0.998. The limits of detection for the method ranged between 0.005 and 0.01 mg/L. The recoveries of the target fungicides in apple juice samples were in the range of 72.4-110.8% with the relative standard deviations ranging from 1.2 to 6.8%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Total internal reflection and dynamic light scattering microscopy of gels

NASA Astrophysics Data System (ADS)

Gregor, Brian F.

Two different techniques which apply optical microscopy in novel ways to the study of biological systems and materials were built and applied to several samples. The first is a system for adapting the well-known technique of dynamic light scattering (DLS) to an optical microscope. This can detect and scatter light from very small volumes, as compared to standard DLS which studies light scattering from volumes 1000x larger. The small scattering volume also allows for the observation of nonergodic dynamics in appropriate samples. Porcine gastric mucin (PGM) forms a gel at low pH which lines the epithelial cell layer and acts as a protective barrier against the acidic stomach environment. The dynamics and microscopic viscosity of PGM at different pH levels is studied using polystyrene microspheres as tracer particles. The microscopic viscosity and microrheological properties of the commercial basement membrane Matrigel are also studied with this instrument. Matrigel is frequently used to culture cells and its properties remain poorly determined. Well-characterized and purely synthetic Matrigel substitutes will need to have the correct rheological and morphological characteristics. The second instrument designed and built is a microscope which uses an interferometry technique to achieve an improvement in resolution 2.5x better in one dimension than the Abbe diffraction limit. The technique is based upon the interference of the evanescent field generated on the surface of a prism by a laser in a total internal reflection geometry. The enhanced resolution is demonstrated with fluorescent samples. Additionally. Raman imaging microscopy is demonstrated using the evanescent field in resonant and non-resonant samples, although attempts at applying the enhanced resolution technique to the Raman images were ultimately unsuccessful. Applications of this instrument include high resolution imaging of cell membranes and macroscopic structures in gels and proteins. Finally, a third section incorporating previous research on simulations of complex fluids is included. Two dimensional simulations of oil, water, and surfactant mixtures were computed with a lattice gas method. The simulated systems were randomly mixed and then the temperature was quenched to a predetermined point. Spontaneous micellization is observed for a narrow range of temperature quenches, and the overall growth rate of macroscopic structure is found to follow a Vogel-Fulcher growth law.

Strategic Studies Quarterly. Volume 8, Number 3, Fall 2014

DTIC Science & Technology

2014-01-01

Michael Guillot Measuring Military Power James Jay Carafano Strategy and Force Planning in a Time of Austerity BG Michael J . Meese, USA, Retired...Hudson, PhD Nori Katagiri, PhD Paul J . Springer, PhD Zachary J . Zwald, PhD Strategic Studies Quarterly (SSQ) (ISSN 1936-1815) is published quarterly...19 BG Michael J . Meese, USA, Retired Pensive Sword: Educating Officers in Austere Times ...................... 30 Stephen D. Chiabotti Feature

On the pH of Aqueous Attoliter-Volume Droplets

NASA Astrophysics Data System (ADS)

Ramos, Kieran P.; Velpula, Samson S.; Demille, Trevor B.; Pajela, Ryan; Goldner, Lori S.

Droplets of water dispersed in perfluorinated liquids have widespread use including microfluidics, drug delivery and single-molecule measurements. Perfluorinated liquids are distinctly biocompatible due to their stability, low surface tension, lipophobicity, and hydrophobicity. For this reason, the effect of the perfluorinated surface on droplet contents is usually ignored. However, as the droplet diameter is reduced, we expect that any effect of the water/oil interface on droplet contents will become more obvious. We studied the pH of attoliter-volume aqueous droplets in perfluorinated liquids using pH-sensing fluorescent dyes. Droplets were prepared either by sonication or extrusion from buffer and perfluorinated liquids (FC40 or FC77). A non-ionic surfactant was used to stabilize the droplets. Buffer strength, ionic strength, and pH of the aqueous phase were varied and resulting droplet pH compared to the pH of the buffer from which they were formed. Preliminary data are consistent with a pH in droplets that depends on the concentration of non-ionic surfactant. At low surfactant concentrations, the pH in droplets is distinctly lower than the stock buffer. However, as the concentration of non-ionic surfactant is increased the change in pH decreases. This work was funded by NSF/DBI-1152386.

Regulation of statoconia mineralization in Aplysia californica in vitro

NASA Technical Reports Server (NTRS)

Pedrozo, H. A.; Schwartz, Z.; Dean, D. D.; Wiederhold, M. L.; Boyan, B. D.

1996-01-01

Statoconia are calcium carbonate inclusions in the lumen of the gravity-sensing organ, the statocyst, of Aplysia californica. The aim of the present study was to examine the role of carbonic anhydrase and urease in statoconia mineralization in vitro. The experiments were performed using a previously described culture system (Pedrozo et al., J. Comp. Physiol. (A) 177:415-425). Inhibition of carbonic anhydrase by acetazolamide decreased statoconia production and volume, while inhibition of urease by acetohydroxamic acid reduced total statoconia number, but had no affect on statoconia volume. Inhibition of carbonic anhydrase initially increased and then decreased the statocyst pH, whereas inhibition of urease decreased statocyst pH at all times examined; simultaneous addition of both inhibitors also decreased pH. These effects were dose and time dependent. The results show that carbonic anhydrase and urease are required for statoconia formation and homeostasis, and for regulation of statocyst pH. This suggests that these two enzymes regulate mineralization at least partially through regulation of statocyst pH.

Selective extraction based on poly(MAA-VB-EGMDA) monolith followed by HPLC for determination of hordenine in plasma and urine samples.

PubMed

Chen, Yonggang; Meng, Junhua; Zou, Jili; An, Jing

2015-06-01

Hordenine is an active compound found in several foods, herbs and beer. In this work, a novel sorbent was fabricated for selective solid-phase extraction (SPE) of hordenine in biological samples. The organic polymer sorbent was synthesized in one step in the plastic barrel of a syringe by a pre-polymerization solution consisting of methacrylic acid (MAA), 4-vinylphenylboronic acid (VB) and ethylene glycol dimethacrylate (EGDMA). The conditions for preparation were optimized to generate a poly(MAA-VB-EGMDA) monolith with good permeability. The monolith exhibited good enrichment efficiency towards hordenine. By using tyramine as the internal standard, a poly(MAA-VB-EGMDA)-based SPE-HPLC method was established for analysis of hordenine. Conditions for SPE, including volume of eluting solvent, pH of sample solution, sampling rate and sample volume, were optimized. The proposed SPE-HPLC method presented good linearity (R(2)  = 0.9992) within 10-2000 ng/mL and the detection limits was 3 ng/mL, which is significantly more sensitive than reported methods. The method was also applied in plasma and urine samples; good capability of removing matrices was observed, while hordenine in low content was well extracted and enriched. The recoveries were from 90.6 to 94.7% and from 89.3 to 91.5% for the spiked plasma and urine samples, respectively, with the relative standard deviations <4.7%. Copyright © 2014 John Wiley & Sons, Ltd.

Effects of pH and Magnetic Material on Immunomagnetic Separation of Cryptosporidium Oocysts from Concentrated Water Samples

PubMed Central

Kuhn, Ryan C.; Rock, Channah M.; Oshima, Kevin H.

2002-01-01

In this study, we examined the effect that magnetic materials and pH have on the recoveries of Cryptosporidium oocysts by immunomagnetic separation (IMS). We determined that particles that were concentrated on a magnet during bead separation have no influence on oocyst recovery; however, removal of these particles did influence pH values. The optimal pH of the IMS was determined to be 7.0. The numbers of oocysts recovered from deionized water at pH 7.0 were 26.3% higher than those recovered from samples that were not at optimal pH. The results indicate that the buffers in the IMS kit did not adequately maintain an optimum pH in some water samples. By adjusting the pH of concentrated environmental water samples to 7.0, recoveries of oocysts increased by 26.4% compared to recoveries from samples where the pH was not adjusted. PMID:11916735

Recent advances in enhancing the sensitivity of electrophoresis and electrochromatography in capillaries and microchips (2014-2016).

PubMed

Breadmore, Michael C; Wuethrich, Alain; Li, Feng; Phung, Sui Ching; Kalsoom, Umme; Cabot, Joan M; Tehranirokh, Masoomeh; Shallan, Aliaa I; Abdul Keyon, Aemi S; See, Hong Heng; Dawod, Mohamed; Quirino, Joselito P

2017-01-01

One of the most cited limitations of capillary (and microchip) electrophoresis is the poor sensitivity. This review continues to update this series of biennial reviews, first published in Electrophoresis in 2007, on developments in the field of on-line/in-line concentration methods in capillaries and microchips, covering the period July 2014-June 2016. It includes developments in the field of stacking, covering all methods from field amplified sample stacking and large volume sample stacking, through to isotachophoresis, dynamic pH junction, and sweeping. Attention is also given to on-line or in-line extraction methods that have been used for electrophoresis. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Determination of the distribution of relative molecular mass of organic matter by high pressure size exclusion chromatography with UV and TOC detectors].

PubMed

Zhang, Han; Dong, Bing-Zhi

2012-09-01

An on-line high pressure size exclusion chromatography (HPSEC) with UV and TOC detectors was adapted to examine the distribution of relative molecular mass of natural organic matter (NOM). Through synchronous determination of UV254 and TOC responses in a wide range of relative molecular mass, it was possible to accurately characterize the structure of NOM, especially for some non-aromatic and non-conjugated double bond organics which have low response to UV. It was found that, TOC detector was capable of detecting all kinds of organic matters, including sucrose, sodium alginate and other hydrophilic organic compounds. The sample volume had a positively linear correlation with the TOC response, indicating that the larger volume would produce stronger responses. The effect of ion strength was relatively low, shown by the small decrease of peak area (1.2% ) from none to 0.2 mol x L(-1) NaCl. The pH value of tested samples should be adjusted to neutral or acidic because when the samples were alkaline, the results might be inaccurate. Compared to the sample solvents adopted as ultrapure water, the samples prepared by mobile phase solvents had less interference to salt boundary peak. The on-line HPSEC-UV-TOC can be used accurately to characterize the distribution of relative molecular mass and its four fractions in River Xiang.

Speciation of selenium in environmental samples by solid-phase spectrophotometry using 2,3-dichloro-6-(2,7-dihydroxy-naphthylazo)quinoxaline.

PubMed

Amin, Alaa S

2014-01-01

Solid-phase spectrophotometry was applied to determination of trace amounts of selenium (Se) in water, soil, plant materials, human hair, and a cosmetic preparation (lipstick). Se(IV) was sorbed in a dextran type lipophilic gel as a complex with 2,3-dichloro-6-(2,7-dihydroxy-naphthylazo)quinoxaline (DCDHNAQ), whereas Se(VI) was determined after boiling in HCI for 10 min to convert Se(VI) to Se(IV). Resin phase absorbances at 588 and 800 nm were measured directly, which allowed the determination of Se in the range of 0.2-3.3 microg/L with an RSD of 1.22%. The influences of analytical parameters including pH of the aqueous solution, amounts of DCDHNAQ, and sample volume were investigated. The molar absorptivities were found to be 1.09 x 10(6), 4.60 x 10(6), and 1.23 x 10(7) L/mol cm for 100, 500, and 1000 mL, respectively. The LOD and LOQ of the 500 mL sample method were 110 and 360 ng/L, respectively, when using 50 mg dextran type lipophilic gel. For a 1000 mL sample, the LOD and LOQ were 60 and 200 ng/L, respectively, using 50 mg of the exchanger. Increasing the sample volume enhanced the sensitivity. No considerable interferences were observed from other investigated anions and cations on the Se determination.

Concentration of Enteroviruses, Adenoviruses, and Noroviruses from Drinking Water by Use of Glass Wool Filters▿

PubMed Central

Lambertini, Elisabetta; Spencer, Susan K.; Bertz, Phillip D.; Loge, Frank J.; Kieke, Burney A.; Borchardt, Mark A.

2008-01-01

Available filtration methods to concentrate waterborne viruses are either too costly for studies requiring large numbers of samples, limited to small sample volumes, or not very portable for routine field applications. Sodocalcic glass wool filtration is a cost-effective and easy-to-use method to retain viruses, but its efficiency and reliability are not adequately understood. This study evaluated glass wool filter performance to concentrate the four viruses on the U.S. Environmental Protection Agency contaminant candidate list, i.e., coxsackievirus, echovirus, norovirus, and adenovirus, as well as poliovirus. Total virus numbers recovered were measured by quantitative reverse transcription-PCR (qRT-PCR); infectious polioviruses were quantified by integrated cell culture (ICC)-qRT-PCR. Recovery efficiencies averaged 70% for poliovirus, 14% for coxsackievirus B5, 19% for echovirus 18, 21% for adenovirus 41, and 29% for norovirus. Virus strain and water matrix affected recovery, with significant interaction between the two variables. Optimal recovery was obtained at pH 6.5. No evidence was found that water volume, filtration rate, and number of viruses seeded influenced recovery. The method was successful in detecting indigenous viruses in municipal wells in Wisconsin. Long-term continuous filtration retained viruses sufficiently for their detection for up to 16 days after seeding for qRT-PCR and up to 30 days for ICC-qRT-PCR. Glass wool filtration is suitable for large-volume samples (1,000 liters) collected at high filtration rates (4 liters min−1), and its low cost makes it advantageous for studies requiring large numbers of samples. PMID:18359827

GC-MS Analysis and Gastroprotective Evaluations of Crude Extracts, Isolated Saponins, and Essential Oil from Polygonum hydropiper L.

PubMed Central

Ayaz, Muhammad; Junaid, Muhammad; Ullah, Farhat; Sadiq, Abdul; Shahid, Muhammad; Ahmad, Waqar; Ullah, Ihsan; Ahmad, Ashfaq; Syed, Nawazish-i-Husain

2017-01-01

Peptic ulceration is among the most prevalent gastrointestinal disorders characterized by pepsin and gastric acid mediated mucosal damage, as result of imbalance between defensive and offensive processes. The main objective of the current study was to investigate the antiulcer potentials of Polygonum hydropiper crude methanolic ectract (Ph.Cr) in aspirin induced ulcerogenesis using pylorus ligated rat model. In-vitro urease and Proteus mirabilis inhibitory potentials were evaluated using standard protocols. All fractions were analyzed using GC-MS to identify major components. The aspirin induced ulcerogenesis in pylorus ligated rat model was associated with significant changes in the mean ulcer score [F(5, 30) = 7.141, P = 0.0002], gastric juice volume [F(5, 30) = 8.245, P < 0.0001], gastric juice pH [F(5, 30) = 5.715, P = 0.0008], free acidity [F(5, 30) = 4.544, P = 0.0033], total acidity [F(5, 30) = 2.740, P = 0.0373], and pepsin concentration [F(5, 30) = 2.335, P = 0.0664]. Pre-treatment with Ph.Cr at 100, 200, and 400 mg/kg dose exhibited marked gastroprotective and anti-ulcerogenic effect in the aspirin induced pyloric ligation ulcerogenesis model at 100, 200, and 400 mg/kg as indicated by ulcerative biochemical parameters. In urease inhibition assay, leaves essential oil (Ph.Lo), saponins (Ph.Sp), and chloroform extract (Ph.Chf) exhibited highest activities with IC50 of 90, 98, and 520 μg/ml, respectively. Ph.Sp, Ph.Chf, ethyl acetate (Ph.EtAc), and Ph.Cr showed MICs of 25, 30, 32.25, and 40.50 μg/ml, respectively against P. mirabilis. Several compounds were identified in GC-MS analysis of samples. Significant in-vivo antiulcer, urease inhibitory as well as anti-proteus potentials of P. hydropiper solvent extracts, signify its potential use for the management of peptic ulcers and may provide scientific bases for the traditional uses of the plant. PMID:28824906

GC-MS analysis and gastroprotective evaluations of crude extracts, isolated saponins and essential oil from Polygonum hydropiper L.

NASA Astrophysics Data System (ADS)

Ayaz, Muhammad; Junaid, Muhammad; Ullah, Farhat; Sadiq, Abdul; Shahid, Muhammad; Ahmad, Waqar; Ullah, Ihsan; Ahmad, Ashfaq; Syed, Nawazish-i.-Husain

2017-08-01

Peptic ulceration is among the most prevalent gastrointestinal disorders characterized by pepsin and gastric acid mediated mucosal damage, as result of imbalance between defensive and offensive processes. The main objective of the current study was to investigate the antiulcer potentials of Polygonum hydropiper crude methanolic ectract (Ph.Cr) in aspirin induced ulcerogenesis using pylorus ligated rat model. In-vitro urease and Proteus mirabilis inhibitory potentials were evaluated using standard protocols. All fractions were analyzed using GC-MS to identify major components. The aspirin induced ulcerogenesis in pylorus ligated rat model was associated with significant changes in the mean ulcer score (F5,30 = 7.141, P = 0.0002), gastric juice volume (F5,30 = 8.245, P < 0.0001), gastric juice pH (F5,30 = 5.715, P = 0.0008), free acidity (F5,30 = 4.544, P = 0.0033), total acidity (F5,30 = 2.740, P = 0.0373) and pepsin concentration (F5,30 = 2.335, P = 0.0664). Pre treatment with Ph.Cr at 100, 200 and 400 mg/kg dose exhibited marked gastroprotective and anti-ulcerogenic effect in the aspirin induced pyloric ligation ulcerogenesis model at 100, 200 and 400 mg/kg as indicated by ulcerative biochemical parameters. In urease inhibition assay, leaves essential oil (Ph.Lo), saponins (Ph.Sp) and chloroform extract (Ph.Chf) exhibited highest activities with IC50 of 90, 98 and 520 µg/ml respectively. Ph.Sp, Ph.Chf, ethyl acetate (Ph.EtAc) and Ph.Cr showed MICs of 25, 30, 32.25 and 40.50 µg/ml respectively against Proteus mirabilis. Several compounds were identified in GC-MS analysis of samples. Significant in-vivo antiulcer, urease inhibitory as well as anti-proteus potentials of P. hydropiper solvent extracts, signify its potential use for the management of peptic ulcers and may provide scientific bases for the traditional uses of the plant.

A new solid phase microextraction method using organic ligand in micropipette tip syringe system packed with modified carbon cloth for preconcentration of cadmium in drinking water and blood samples of kidney failure patients.

PubMed

Panhwar, Abdul Haleem; Kazi, Tasneem Gul; Afridi, Hassan Imran; Arain, Salma Aslam; Naeemullah; Brahman, Kapil Dev; Arain, Mariam Shahzadi

2015-03-05

A simple and efficient miniaturized solid phase microextraction (M-SPμE) in a syringe system was developed for preconcentration of cadmium (Cd) in environmental and biological samples, followed by flame atomic absorption technique. The syringe system contains the micropipette tip packed with activated carbon cloth, coated with modified magnetic nanoparticles of iron oxide Triton X114 (ACC-NPs). Scanning electron microscopy and energy dispersive spectroscopy used for characterization of the size, morphology and elemental composition of ACC-NPs. The sample solution treated with a complexing reagent 8-hydroxyqunilone (8-HQ), and drawn into the syringe, filled with ACC-MNPs and dispensed manually for 2-10 drawing/discharging cycles. The analyte retained on ACC-NPs in micropipette tip-syringe system were then eluted with different volume of 1.5molL(-1) HCl by 1-5 drawing/discharging cycles. The syringe system directly couple with FAAS for analysis. The influence of different variables on the extraction efficiency of Cd, including adsorbent dosage, pH, sample volume, eluent volume and drawing/discharging cycles of syringe system were optimized. At optimized extraction conditions, the method showed good linearity in the range of 5-250μgL(-1), with a limit of detection 0.15μgL(-1). Repeatability of the extraction (%RSD) was <5%, n=5. The validity and accuracy of the method was checked by the certified reference materials. The proposed method was successfully applied for the determination of Cd in different drinking water and biological samples of kidney failure patients and healthy controls. Copyright © 2014 Elsevier B.V. All rights reserved.

A new solid phase microextraction method using organic ligand in micropipette tip syringe system packed with modified carbon cloth for preconcentration of cadmium in drinking water and blood samples of kidney failure patients

NASA Astrophysics Data System (ADS)

Panhwar, Abdul Haleem; Kazi, Tasneem Gul; Afridi, Hassan Imran; Arain, Salma Aslam; Naeemullah; Brahman, Kapil Dev; Arain, Mariam Shahzadi

2015-03-01

A simple and efficient miniaturized solid phase microextraction (M-SPμE) in a syringe system was developed for preconcentration of cadmium (Cd) in environmental and biological samples, followed by flame atomic absorption technique. The syringe system contains the micropipette tip packed with activated carbon cloth, coated with modified magnetic nanoparticles of iron oxide Triton X114 (ACC-NPs). Scanning electron microscopy and energy dispersive spectroscopy used for characterization of the size, morphology and elemental composition of ACC-NPs. The sample solution treated with a complexing reagent 8-hydroxyqunilone (8-HQ), and drawn into the syringe, filled with ACC-MNPs and dispensed manually for 2-10 drawing/discharging cycles. The analyte retained on ACC-NPs in micropipette tip-syringe system were then eluted with different volume of 1.5 mol L-1 HCl by 1-5 drawing/discharging cycles. The syringe system directly couple with FAAS for analysis. The influence of different variables on the extraction efficiency of Cd, including adsorbent dosage, pH, sample volume, eluent volume and drawing/discharging cycles of syringe system were optimized. At optimized extraction conditions, the method showed good linearity in the range of 5-250 μg L-1, with a limit of detection 0.15 μg L-1. Repeatability of the extraction (%RSD) was <5%, n = 5. The validity and accuracy of the method was checked by the certified reference materials. The proposed method was successfully applied for the determination of Cd in different drinking water and biological samples of kidney failure patients and healthy controls.

The Water to Solute Permeability Ratio Governs the Osmotic Volume Dynamics in Beetroot Vacuoles.

PubMed

Vitali, Victoria; Sutka, Moira; Amodeo, Gabriela; Chara, Osvaldo; Ozu, Marcelo

2016-01-01

Plant cell vacuoles occupy up to 90% of the cell volume and, beyond their physiological function, are constantly subjected to water and solute exchange. The osmotic flow and vacuole volume dynamics relies on the vacuole membrane -the tonoplast- and its capacity to regulate its permeability to both water and solutes. The osmotic permeability coefficient ( P f ) is the parameter that better characterizes the water transport when submitted to an osmotic gradient. Usually, P f determinations are made in vitro from the initial rate of volume change, when a fast (almost instantaneous) osmolality change occurs. When aquaporins are present, it is accepted that initial volume changes are only due to water movements. However, in living cells osmotic changes are not necessarily abrupt but gradually imposed. Under these conditions, water flux might not be the only relevant driving force shaping the vacuole volume response. In this study, we quantitatively investigated volume dynamics of isolated Beta vulgaris root vacuoles under progressively applied osmotic gradients at different pH, a condition that modifies the tonoplast P f . We followed the vacuole volume changes while simultaneously determining the external osmolality time-courses and analyzing these data with mathematical modeling. Our findings indicate that vacuole volume changes, under progressively applied osmotic gradients, would not depend on the membrane elastic properties, nor on the non-osmotic volume of the vacuole, but on water and solute fluxes across the tonoplast. We found that the volume of the vacuole at the steady state is determined by the ratio of water to solute permeabilites ( P f / P s ), which in turn is ruled by pH. The dependence of the permeability ratio on pH can be interpreted in terms of the degree of aquaporin inhibition and the consequently solute transport modulation. This is relevant in many plant organs such as root, leaves, cotyledons, or stems that perform extensive rhythmic growth movements, which very likely involve considerable cell volume changes within seconds to hours.

The Water to Solute Permeability Ratio Governs the Osmotic Volume Dynamics in Beetroot Vacuoles

PubMed Central

Vitali, Victoria; Sutka, Moira; Amodeo, Gabriela; Chara, Osvaldo; Ozu, Marcelo

2016-01-01

Plant cell vacuoles occupy up to 90% of the cell volume and, beyond their physiological function, are constantly subjected to water and solute exchange. The osmotic flow and vacuole volume dynamics relies on the vacuole membrane -the tonoplast- and its capacity to regulate its permeability to both water and solutes. The osmotic permeability coefficient (Pf) is the parameter that better characterizes the water transport when submitted to an osmotic gradient. Usually, Pf determinations are made in vitro from the initial rate of volume change, when a fast (almost instantaneous) osmolality change occurs. When aquaporins are present, it is accepted that initial volume changes are only due to water movements. However, in living cells osmotic changes are not necessarily abrupt but gradually imposed. Under these conditions, water flux might not be the only relevant driving force shaping the vacuole volume response. In this study, we quantitatively investigated volume dynamics of isolated Beta vulgaris root vacuoles under progressively applied osmotic gradients at different pH, a condition that modifies the tonoplast Pf. We followed the vacuole volume changes while simultaneously determining the external osmolality time-courses and analyzing these data with mathematical modeling. Our findings indicate that vacuole volume changes, under progressively applied osmotic gradients, would not depend on the membrane elastic properties, nor on the non-osmotic volume of the vacuole, but on water and solute fluxes across the tonoplast. We found that the volume of the vacuole at the steady state is determined by the ratio of water to solute permeabilites (Pf/Ps), which in turn is ruled by pH. The dependence of the permeability ratio on pH can be interpreted in terms of the degree of aquaporin inhibition and the consequently solute transport modulation. This is relevant in many plant organs such as root, leaves, cotyledons, or stems that perform extensive rhythmic growth movements, which very likely involve considerable cell volume changes within seconds to hours. PMID:27695468

A comprehensive study of a new versatile microchip device based liquid phase microextraction for stopped-flow and double-flow conditions.

PubMed

Payán, María Ramos; Murillo, Elia Santigosa; Coello, Jordi; López, Miguel Ángel Bello

2018-06-29

A new geometry for a versatile microfluidic-chip device based liquid phase microextraction was developed in order to enhance the preconcentration in microfluidic chips and also to enable double-flow and stopped-flow working modes. The microchip device was combined with a HPLC procedure for the simultaneous determination of two different families as model analytes, which were parabens and non-steroidal anti-inflammatories (NSAIDs): Ethyl 4-hydroxybenzoate (Et-P), Propyl 4-hydroxybenzoate (Pr-P), Butyl 4-hydroxybenzoate (Bu-P), IsoButyl 4-hydroxybenzoate (iBu-P), salycilic acid (SAC), ketoprofen (KET), naproxen (NAX), diclofenac (DIC) and ibuprofen (IBU) in urine samples. The new miniaturized microchip proposed in this work allows not only the possibility of working in double-flow conditions, but also under stagnant conditions (stopped-flow) (SF-μLPME). The sample (pH 1.5) was delivered to the SF-μLPME at 20 μL min -1 while keeping the acceptor phase (pH 11.75) under stagnant conditions during 20 min. The highest enrichment factors (between 16 and 47) were obtained under stopped-flow conditions at 20 μL min -1 (sample flow rate) after 20 min extraction; whereas the extraction efficiencies were within the range of 27-81% for all compounds. The procedure provided very low detection limits between 0.7 and 8.5 μg L -1 with a sample volume consumption of 400 μL. Parabens and NSAIDs have successfully been extracted from urine samples with excellent clean up and recoveries over 90% for all compounds. In parallel, the new device was also tested under double flow conditions, obtaining good but lower enrichment factors (between 9 and 20) and higher extraction efficiencies (between 45 and 95) after 7 min extraction, consuming a volume sample of 140 μL. The versatile device offered very high extraction efficiencies and good enrichment factor for double flow and stopped-flow conditions, respectively. In addition, this new miniaturized SF-μLPME device significantly reduced costs compared to the existing analytical techniques for sample preparation since this microchip require few microliters of sample and reagents and it is reusable. Copyright © 2018 Elsevier B.V. All rights reserved.

Application of the Response Surface Methodology to Optimize the Fermentation Parameters for Enhanced Docosahexaenoic Acid (DHA) Production by Thraustochytrium sp. ATCC 26185.

PubMed

Wu, Kang; Ding, Lijian; Zhu, Peng; Li, Shuang; He, Shan

2018-04-22

The aim of this study was to determine the cumulative effect of fermentation parameters and enhance the production of docosahexaenoic acid (DHA) by Thraustochytrium sp. ATCC 26185 using response surface methodology (RSM). Among the eight variables screened for effects of fermentation parameters on DHA production by Plackett-Burman design (PBD), the initial pH, inoculum volume, and fermentation volume were found to be most significant. The Box-Behnken design was applied to derive a statistical model for optimizing these three fermentation parameters for DHA production. The optimal parameters for maximum DHA production were initial pH: 6.89, inoculum volume: 4.16%, and fermentation volume: 140.47 mL, respectively. The maximum yield of DHA production was 1.68 g/L, which was in agreement with predicted values. An increase in DHA production was achieved by optimizing the initial pH, fermentation, and inoculum volume parameters. This optimization strategy led to a significant increase in the amount of DHA produced, from 1.16 g/L to 1.68 g/L. Thraustochytrium sp. ATCC 26185 is a promising resource for microbial DHA production due to the high-level yield of DHA that it produces, and the capacity for large-scale fermentation of this organism.

TiF(4) and NaF at pH 1.2 but not at pH 3.5 are able to reduce dentin erosion.

PubMed

Wiegand, Annette; Magalhães, Ana Carolina; Sener, Beatrice; Waldheim, Elena; Attin, Thomas

2009-08-01

This study aimed to analyse and compare the protective effect of buffered (pH 3.5) and native (pH 1.2) TiF(4) in comparison to NaF solutions of same pH on dentin erosion. Bovine samples were pretreated with 1.50% TiF(4) or 2.02% NaF (both 0.48M F) solutions, each with a pH of 1.2 and 3.5. The control group received no fluoride pretreatment. Ten samples in each group were eroded with HCl (pH 2.6) for 10x60s. Erosion was analysed by determination of calcium release into the acid. Additionally, the surface and the elemental surface composition were examined by scanning electron microscopy (two samples in each group) and X-ray energy-dispersive spectroscopy in fluoridated but not eroded samples (six samples in each group). Cumulative calcium release (nmol/mm(2)) was statistically analysed by repeated measures ANOVA and one-way ANOVA at t=10min. TiF(4) and NaF at pH 1.2 decreased calcium release significantly, while TiF(4) and NaF at pH 3.5 were not effective. Samples treated with TiF(4) at pH 1.2 showed a significant increase of Ti, while NaF pretreatment increased F concentration significantly. TiF(4) at pH 1.2 led to the formation of globular precipitates occluding dentinal tubules, which could not be observed on samples treated with TiF(4) at pH 3.5. NaF at pH 1.2 but not at pH 3.5 induced the formation of surface precipitates covering dentinal tubules. Dentin erosion can be significantly reduced by TiF(4) and NaF at pH 1.2, but not at pH 3.5.

Determination of a practical pH cutoff level for reliable confirmation of nasogastric tube placement.

PubMed

Gilbertson, Heather Ruth; Rogers, Elizabeth Jessie; Ukoumunne, Obioha Chukwunyere

2011-07-01

Enteral feeding is a common method of nutrition support when oral intake is inadequate. Confirmation of correct nasogastric (NG) tube placement is essential. Risks of morbidity/mortality associated with misplacement in the lung are well documented. Studies indicate that pH ≤ 4 confirms gastric aspirate, but in pediatrics, a pH of gastric aspirate is often >4. The goal of this study was to determine a reliable and practical pH value to confirm NG tube placement, without increasing the risk of not identifying a misplaced NG tube. Pediatric inpatients older than 4 weeks receiving enteral nutrition (nasogastric or gastrostomy) were recruited over 9 months. Aspirate samples were pH tested at NG tube placement and before feedings. If pH >4, NG tube position was confirmed by chest radiograph or further investigations. In addition, intensive care unit (ICU) patients who required endotracheal suctioning were recruited, and endotracheal aspirate samples were pH tested. A total of 4,330 gastric aspirate samples (96% nasogastric) were collected from 645 patients with a median (interquartile range [IQR]) age of 1.0 years (0.3-5.2 years). The mean (standard deviation [SD]) pH of these gastric samples was 3.6 (1.4) (range, 0-9). pH was >4 in 1,339 (30.9%) gastric aspirate samples, and of these, 244 were radiographed, which identified 10 misplaced tubes (1 with pH 5.5). A total of 65 endotracheal aspirate samples were collected from 19 ICU patients with a median (IQR) age of 0.6 years (0.4-5.2 years). The mean (SD) pH of these samples was 8.4 (0.8) (range, 6-9.5). Given that the lowest pH value of endotracheal aspirate sample was 6, and a misplaced NG tube was identified with pH 5.5, it is proposed that a gastric aspirate pH ≤ 5 is a safer, reliable, and practical cutoff in this population.

Trace determination of safranin O dye using ultrasound assisted dispersive solid-phase micro extraction: Artificial neural network-genetic algorithm and response surface methodology.

PubMed

Dil, Ebrahim Alipanahpour; Ghaedi, Mehrorang; Asfaram, Arash; Mehrabi, Fatemeh; Bazrafshan, Ali Akbar; Ghaedi, Abdol Mohammad

2016-11-01

In this study, ultrasound assisted dispersive solid-phase micro extraction combined with spectrophotometry (USA-DSPME-UV) method based on activated carbon modified with Fe2O3 nanoparticles (Fe2O3-NPs-AC) was developed for pre-concentration and determination of safranin O (SO). It is known that the efficiency of USA-DSPME-UV method may be affected by pH, amount of adsorbent, ultrasound time and eluent volume and the extent and magnitude of their contribution on response (in term of main and interaction part) was studied by using central composite design (CCD) and artificial neural network-genetic algorithms (ANN-GA). Accordingly by adjustment of experimental conditions suggested by ANN-GA at pH 6.5, 1.1mg of adsorbent, 10min ultrasound and 150μL of eluent volume led to achievement of best operation performance like low LOD (6.3ngmL(-1)) and LOQ (17.5ngmL(-1)) in the range of 25-3500ngmL(-1). In following stage, the SO content in real water and wastewater samples with recoveries between 93.27-99.41% with RSD lower than 3% was successfully determined. Copyright © 2016 Elsevier B.V. All rights reserved.

Probabilistic evaluation of shallow groundwater resources at a hypothetical carbon sequestration site

DOE PAGES

Dai, Zhenxue; Keating, Elizabeth; Bacon, Diana H.; ...

2014-03-07

Carbon sequestration in geologic reservoirs is an important approach for mitigating greenhouse gases emissions to the atmosphere. This study first develops an integrated Monte Carlo method for simulating CO 2 and brine leakage from carbon sequestration and subsequent geochemical interactions in shallow aquifers. Then, we estimate probability distributions of five risk proxies related to the likelihood and volume of changes in pH, total dissolved solids, and trace concentrations of lead, arsenic, and cadmium for two possible consequence thresholds. The results indicate that shallow groundwater resources may degrade locally around leakage points by reduced pH and increased total dissolved solids (TDS).more » The volumes of pH and TDS plumes are most sensitive to aquifer porosity, permeability, and CO 2 and brine leakage rates. The estimated plume size of pH change is the largest, while that of cadmium is the smallest among the risk proxies. Plume volume distributions of arsenic and lead are similar to those of TDS. The scientific results from this study provide substantial insight for understanding risks of deep fluids leaking into shallow aquifers, determining the area of review, and designing monitoring networks at carbon sequestration sites.« less

The Final Frontier of pH and the Undiscovered Country Beyond

PubMed Central

Bal, Wojciech; Kurowska, Ewa; Maret, Wolfgang

2012-01-01

The comparison of volumes of cells and subcellular structures with the pH values reported for them leads to a conflict with the definition of the pH scale. The pH scale is based on the ionic product of water, K w = [H+]×[OH−].We used K w [in a reversed way] to calculate the number of undissociated H2O molecules required by this equilibrium constant to yield at least one of its daughter ions, H+ or OH− at a given pH. In this way we obtained a formula that relates pH to the minimal volume VpH required to provide a physical meaning to K w, (where N A is Avogadro’s number). For example, at pH 7 (neutral at 25°C) VpH = 16.6 aL. Any deviation from neutral pH results in a larger VpH value. Our results indicate that many subcellular structures, including coated vesicles and lysosomes, are too small to contain free H+ ions at equilibrium, thus the definition of pH based on K w is no longer valid. Larger subcellular structures, such as mitochondria, apparently contain only a few free H+ ions. These results indicate that pH fails to describe intracellular conditions, and that water appears to be dissociated too weakly to provide free H+ ions as a general source for biochemical reactions. Consequences of this finding are discussed. PMID:23049874

Determination Of Ph Including Hemoglobin Correction

DOEpatents

Maynard, John D.; Hendee, Shonn P.; Rohrscheib, Mark R.; Nunez, David; Alam, M. Kathleen; Franke, James E.; Kemeny, Gabor J.

2005-09-13

Methods and apparatuses of determining the pH of a sample. A method can comprise determining an infrared spectrum of the sample, and determining the hemoglobin concentration of the sample. The hemoglobin concentration and the infrared spectrum can then be used to determine the pH of the sample. In some embodiments, the hemoglobin concentration can be used to select an model relating infrared spectra to pH that is applicable at the determined hemoglobin concentration. In other embodiments, a model relating hemoglobin concentration and infrared spectra to pH can be used. An apparatus according to the present invention can comprise an illumination system, adapted to supply radiation to a sample; a collection system, adapted to collect radiation expressed from the sample responsive to the incident radiation; and an analysis system, adapted to relate information about the incident radiation, the expressed radiation, and the hemoglobin concentration of the sample to pH.

Chemical Reaction between Boric Acid and Phosphine Indicates Boric Acid as an Antidote for Aluminium Phosphide Poisoning.

PubMed

Soltani, Motahareh; Shetab-Boushehri, Seyed F; Shetab-Boushehri, Seyed V

2016-08-01

Aluminium phosphide (AlP) is a fumigant pesticide which protects stored grains from insects and rodents. When it comes into contact with moisture, AlP releases phosphine (PH3), a highly toxic gas. No efficient antidote has been found for AlP poisoning so far and most people who are poisoned do not survive. Boric acid is a Lewis acid with an empty p orbital which accepts electrons. This study aimed to investigate the neutralisation of PH3 gas with boric acid. This study was carried out at the Baharlou Hospital, Tehran University of Medical Sciences, Tehran, Iran, between December 2013 and February 2014. The volume of released gas, rate of gas evolution and changes in pH were measured during reactions of AlP tablets with water, acidified water, saturated boric acid solution, acidified saturated boric acid solution, activated charcoal and acidified activated charcoal. Infrared spectroscopy was used to study the resulting probable adduct between PH3 and boric acid. Activated charcoal significantly reduced the volume of released gas (P <0.01). Although boric acid did not significantly reduce the volume of released gas, it significantly reduced the rate of gas evolution (P <0.01). A gaseous adduct was formed in the reaction between pure AlP and boric acid. These findings indicate that boric acid may be an efficient and non-toxic antidote for PH3 poisoning.

Characterizing the variation in pH measurements with apheresis platelets.

PubMed

Moroff, Gary; Seetharaman, Shalini; Kurtz, James; Wagner, Stephen J

2011-11-01

pH measurements of platelet (PLT) components remain a key parameter when assessing how storage and shipping conditions influence the retention of PLT properties. Studies were conducted to characterize variations in pH measured with two pH meters and a blood gas analyzer. Samples were obtained from apheresis PLT units that were stored with or without continuous agitation to measure a range of pH values. pH values were determined with pH meters at room temperature (20-24°C) upon placing of samples in 5-mL sterile polypropylene tubes and with the blood gas analyzer at 37°C upon injection of identical samples, with conversion to 22°C. The calculated coefficient of variation (%CV) of pH measurements using pH meters (n = 10) was 0.43% or less. The %CV values were comparable with different samples having pH values ranging from 6.0 to 7.4. The %CV levels with the blood gas analyzer were comparable to those observed with the pH meters. The difference in the mean pH values for the two pH meters was no greater than 0.10 units, with 9 of 10 samples having differences in values of 0.05 or less; however, greater differences of values (0.1 to 0.2) were observed between pH measured using the blood gas analyzer and pH meters. Our data show good precision and comparability of pH measurements with two pH meters. Differences in pH values were greater on comparison of the blood gas analyzer with the pH meters. © 2011 American Association of Blood Banks.

Construction Materials Used in the Historical Roman Era Bath in Myra

PubMed Central

Oguz, Cem; Turker, Fikret

2014-01-01

The physical, chemical, and mechanical properties of mortars and bricks used in the historical building that was erected at Myra within the boundaries of Antalya Province during the Roman time were investigated. The sample picked points were marked on the air photographs and plans of the buildings and samples were photographed. Then petrographic evaluation was made by stereo microscope on the polished surfaces of construction materials (mortar, brick) taken from such historical buildings in laboratory condition. Also, microstructural analyses (SEM/EDX, XRD), physical analyses (unit volume, water absorption by mass, water absorption by volume, specific mass, compacity, and porosity), chemical analyses (acid loss and sieve analysis, salt analyses, pH, protein, fat, pozzolanic activity, and conductivity analyses), and mechanical experiments (compressive strength, point loading test, and tensile strength at bending) were applied and the obtained results were evaluated. It was observed that good adherence was provided between the binder and the aggregate in mortars. It was also detected that bricks have preserved their originality against environmental, atmospheric, and physicochemical effects and their mechanical properties showed that they were produced by appropriate techniques. PMID:25089290

Construction materials used in the historical Roman era bath in Myra.

PubMed

Oguz, Cem; Turker, Fikret; Kockal, Niyazi Ugur

2014-01-01

The physical, chemical, and mechanical properties of mortars and bricks used in the historical building that was erected at Myra within the boundaries of Antalya Province during the Roman time were investigated. The sample picked points were marked on the air photographs and plans of the buildings and samples were photographed. Then petrographic evaluation was made by stereo microscope on the polished surfaces of construction materials (mortar, brick) taken from such historical buildings in laboratory condition. Also, microstructural analyses (SEM/EDX, XRD), physical analyses (unit volume, water absorption by mass, water absorption by volume, specific mass, compacity, and porosity), chemical analyses (acid loss and sieve analysis, salt analyses, pH, protein, fat, pozzolanic activity, and conductivity analyses), and mechanical experiments (compressive strength, point loading test, and tensile strength at bending) were applied and the obtained results were evaluated. It was observed that good adherence was provided between the binder and the aggregate in mortars. It was also detected that bricks have preserved their originality against environmental, atmospheric, and physicochemical effects and their mechanical properties showed that they were produced by appropriate techniques.

Solid phase microextraction of diclofenac using molecularly imprinted polymer sorbent in hollow fiber combined with fiber optic-linear array spectrophotometry.

PubMed

Pebdani, Arezou Amiri; Shabani, Ali Mohammad Haji; Dadfarnia, Shayessteh; Khodadoust, Saeid

2015-08-05

A simple solid phase microextraction method based on molecularly imprinted polymer sorbent in the hollow fiber (MIP-HF-SPME) combined with fiber optic-linear array spectrophotometer has been applied for the extraction and determination of diclofenac in environmental and biological samples. The effects of different parameters such as pH, times of extraction, type and volume of the organic solvent, stirring rate and donor phase volume on the extraction efficiency of the diclofenac were investigated and optimized. Under the optimal conditions, the calibration graph was linear (r(2)=0.998) in the range of 3.0-85.0 μg L(-1) with a detection limit of 0.7 μg L(-1) for preconcentration of 25.0 mL of the sample and the relative standard deviation (n=6) less than 5%. This method was applied successfully for the extraction and determination of diclofenac in different matrices (water, urine and plasma) and accuracy was examined through the recovery experiments. Copyright © 2015 Elsevier B.V. All rights reserved.

Development of a bar adsorptive micro-extraction-large-volume injection-gas chromatography-mass spectrometric method for pharmaceuticals and personal care products in environmental water matrices.

PubMed

Neng, N R; Nogueira, J M F

2012-01-01

The combination of bar adsorptive micro-extraction using activated carbon (AC) and polystyrene-divinylbenzene copolymer (PS-DVB) sorbent phases, followed by liquid desorption and large-volume injection gas chromatography coupled to mass spectrometry, under selected ion monitoring mode acquisition, was developed for the first time to monitor pharmaceutical and personal care products (PPCPs) in environmental water matrices. Assays performed on 25 mL water samples spiked (100 ng L(-1)) with caffeine, gemfibrozil, triclosan, propranolol, carbamazepine and diazepam, selected as model compounds, yielded recoveries ranging from 74% to 99% under optimised experimental conditions (equilibrium time, 16 h (1,000 rpm); matrix characteristics: pH 5, 5% NaCl for AC phase; LD: methanol/acetonitrile (1:1), 45 min). The analytical performance showed good precision (RSD < 18%), convenient detection limits (5-20 ng L(-1)) and excellent linear dynamic range (20-800 ng L(-1)) with remarkable determination coefficients (r(2) > 0.99), where the PS-DVB sorbent phase showed a much better efficiency. By using the standard addition methodology, the application of the present analytical approach on tap, ground, sea, estuary and wastewater samples allowed very good performance at the trace level. The proposed method proved to be a suitable sorption-based micro-extraction alternative for the analysis of priority pollutants with medium-polar to polar characteristics, showing to be easy to implement, reliable, sensitive and requiring a low sample volume to monitor PPCPs in water matrices.

Drinking 300 mL of clear fluid two hours before surgery has no effect on gastric fluid volume and pH in fasting and non-fasting obese patients.

PubMed

Maltby, J Roger; Pytka, Saul; Watson, Neil C; Cowan, Robert A McTaggart; Fick, Gordon H

2004-02-01

To determine whether, in obese [body mass index (BMI) > 30 kg.m(2)] patients, oral intake of 300 mL clear liquid two hours before elective surgery affects the volume and pH of gastric contents at induction of anesthesia. A single-blind, randomized study of 126 adult patients, age > or = 18 yr, ASA physical status I or II, BMI > 30 kg.m(2) who were scheduled for elective surgery under general anesthesia. Patients were excluded if they had diabetes mellitus, symptoms of gastroesophageal reflux, or had taken medication within 24 hr that affects gastric secretion, gastric fluid pH or gastric emptying. All patients fasted from midnight and were randomly assigned to fasting or fluid group. Two hours before their scheduled time of surgery, all patients drank 10 mL of water containing phenol red 50 mg. Those in the fluid group followed with 300 mL clear liquid of their choice. Immediately following induction of general anesthesia and tracheal intubation, gastric contents were aspirated through a multiorifice Salem sump tube. The fluid volume, pH and phenol red concentration were recorded. Median (range) values in fasting vs fluid groups were: gastric fluid volume 26 (3-107) mL vs 30 (3-187) mL, pH 1.78 (1.31-7.08) vs 1.77 (1.27-7.34) and phenol red retrieval 0.1 (0-30)% vs 0.2 (0-15)%. Differences between groups were not statistically significant. Obese patients without comorbid conditions should follow the same fasting guidelines as non-obese patients and be allowed to drink clear liquid until two hours before elective surgery, inasmuch as obesity per se is not considered a risk factor for pulmonary aspiration.

Application of NaClO-treated multiwalled carbon nanotubes as solid phase extraction sorbents for preconcentration of trace 2,4-dichlorophenoxyacetic acid in aqueous samples.

PubMed

Lu, Ping; Deng, Dayi; Ni, Xiaodan

2012-09-01

Multiwalled carbon nanotubes functionalized by oxidation of original multiwalled carbon nanotubes with NaClO were prepared and their application as solid phase extraction sorbent for 2,4-dichlorophenoxyacetic acid (2,4-D) was investigated systemically, and a new method was developed for the determination of trace 2,4-D in water samples based on extraction and preconcentration of 2,4-D with solid phase extraction columns packed with NaClO-treated multiwalled carbon nanotubes prior to its determination by HPLC. The optimum experimental parameters for preconcentration of 2,4-D, including the column activating conditions, the amount of the sorbent, pH of the sample, elution composition, and elution volume, were investigated. The results indicated 2,4-D could be quantitatively retained by 100 mg NaClO-treated multiwalled carbon nanotubes at pH 5, and then eluted completely with 10 mL 3:1 (v/v) methanol-ammonium acetate solution (0.3 mol/L). The detection limit of this method for 2,4-D was 0.15 μg/L, and the relative standard deviation was 2.3% for fortified tap water samples and 2.5% for fortified riverine water sample at the 10 μg/L level. The method was validated using fortified tap water and riverine water samples with known amount of 2,4-D at the 0.4, 10, and 30 μg/L levels, respectively. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of nutritional status and sampling intensity on recovery after dorsal aorta cannulation in free-swimming Atlantic salmon (Salmo salar L.).

PubMed

Djordjevic, B; Kristensen, T; Øverli, Ø; Rosseland, B O; Kiessling, A

2012-02-01

Recovery from implantation of a cannula in the dorsal aorta (DA) of Atlantic salmon (Salmo salar) was studied in relation to nutritional status and sampling intensity. The incentive for the study was the inconsistency between published reports and our own experience of recovery and longevity of fish exposed to this protocol. In two studies using starved fish, blood (0.3 ml) was sampled 0, 1 and 24 h after DA-cannulation, and thereafter at 48 and 72 h and thereafter once weekly for four weeks. In a third study using fed fish, four consecutive samples (0, 3, 6 and 12 h after a meal) were obtained twice a week over a four-week period. All fish displayed a sharp increase in pCO(2) and haematocrit (Hct) during surgery, followed by a marked raise in cortisol, glucose, sodium and potassium (1 h). pCO(2), pH and Hct approached baseline levels as early as the 1 h post-surgery sample, while this was not the case for cortisol and electrolytes before the 24 h post-surgery sample. Glucose did not display any significant changes post surgery. From then on, all variables displayed minor but non-significant (P > 0.05) changes indicating a steady state close to baseline values for unstressed fish. This pattern was independent of sampling procedure, i.e. repeated single or multiple samples and thus volume of blood removed. Nutritional status (fed vs. starved) did not affect post-surgical recovery pattern. Only K(+) and Hct displayed consistent and significant post-prandial patterns. We found marked differences between baseline level of cannulated fish and uncannulated control fish, in pH, K(+) and Hct indicating that cannulation may be the preferred method to obtain representative resting values in fish.

Poly(1-vinylimidazole) functionalized magnetic ion imprinted polymer for fast and selective extraction of trace gold in geological, environmental and biological samples followed by graphite furnace atomic absorption spectrometry detection

NASA Astrophysics Data System (ADS)

Zhao, Bingshan; He, Man; Chen, Beibei; Xu, Hongrun; Hu, Bin

2018-05-01

In this study, poly(1-vinylimidazole) functionalized gold ion imprinted polymer coated magnetic nanoparticles (MNPs@PVIM-Au-IIP) were prepared and characterized. The adsorption behaviors of the prepared MNPs@PVIM-Au-IIP toward gold ions (Au(III)) were studied, it was found that MNPs@PVIM-Au-IIP has good selectivity, high adsorption capacity (185.4 mg g-1) and fast adsorption kinetic for Au(III). Based on it, a new method of ion imprinted magnetic solid phase extraction (II-MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the analysis of trace Au(III) in real samples with complicated matrix. Factors affecting MSPE including sample pH, desorption reagent, elution concentration and volume, elution time, sample volume and adsorption time were optimized. With high enrichment factor of 100-fold, the detection limit of the proposed method is 7.9 ng L-1 for Au(III) with the relative standard deviation of 7.4% (c = 50 ng L-1, n = 7). In order to validate the accuracy of the proposed method, the Certified Reference Material of GBW07293 geological sample (platinpalladium ore) was analyzed, and the determined value was in good agreement with the certified value. The proposed II-MSPE-GFAAS method is simple, fast, selective, sensitive and has been successfully applied in the determination of trace Au in ore, sediment, environmental water and human urine samples with satisfactory results.

Automated Desalting Apparatus

NASA Technical Reports Server (NTRS)

Spencer, Maegan K.; Liu, De-Ling; Kanik, Isik; Beegle, Luther

2010-01-01

Because salt and metals can mask the signature of a variety of organic molecules (like amino acids) in any given sample, an automated system to purify complex field samples has been created for the analytical techniques of electrospray ionization/ mass spectroscopy (ESI/MS), capillary electrophoresis (CE), and biological assays where unique identification requires at least some processing of complex samples. This development allows for automated sample preparation in the laboratory and analysis of complex samples in the field with multiple types of analytical instruments. Rather than using tedious, exacting protocols for desalting samples by hand, this innovation, called the Automated Sample Processing System (ASPS), takes analytes that have been extracted through high-temperature solvent extraction and introduces them into the desalting column. After 20 minutes, the eluent is produced. This clear liquid can then be directly analyzed by the techniques listed above. The current apparatus including the computer and power supplies is sturdy, has an approximate mass of 10 kg, and a volume of about 20 20 20 cm, and is undergoing further miniaturization. This system currently targets amino acids. For these molecules, a slurry of 1 g cation exchange resin in deionized water is packed into a column of the apparatus. Initial generation of the resin is done by flowing sequentially 2.3 bed volumes of 2N NaOH and 2N HCl (1 mL each) to rinse the resin, followed by .5 mL of deionized water. This makes the pH of the resin near neutral, and eliminates cross sample contamination. Afterward, 2.3 mL of extracted sample is then loaded into the column onto the top of the resin bed. Because the column is packed tightly, the sample can be applied without disturbing the resin bed. This is a vital step needed to ensure that the analytes adhere to the resin. After the sample is drained, oxalic acid (1 mL, pH 1.6-1.8, adjusted with NH4OH) is pumped into the column. Oxalic acid works as a chelating reagent to bring out metal ions, such as calcium and iron, which would otherwise interfere with amino acid analysis. After oxalic acid, 1 mL 0.01 N HCl and 1 mL deionized water is used to sequentially rinse the resin. Finally, the amino acids attached to the resin, and the analytes are eluted using 2.5 M NH4OH (1 mL), and the NH4OH eluent is collected in a vial for analysis.

Effect of Casting Defect on Mechanical Properties of 17-4PH Stainless Steel

NASA Astrophysics Data System (ADS)

Kim, Jong-Yup; Lee, Joon-Hyun; Nahm, Seung-Hoon

Damage and integrity evaluation techniques should be developed steadily in order to ensure the reliability and the economic efficiency of gas turbine engines. Casting defects may exist in most casting components of gas turbine engines, and the defects could give serious effect on mechanical properties and fracture toughness. Therefore, it is very important to understand the effect of casting defects on the above properties in order to predict the safety and life of components. In this study, specimens with internal casting defects, made from 17-4PH stainless steel, were prepared and evaluated and characterized based on the volume fraction of defects. The relation between mechanical properties such as tensile, low cycle fatigue and fracture toughness and volume fraction of defect has been investigated. As a result of the analysis, the mechanical properties of 17-4PH decreased as the defect volume fraction increased with very good linearity. The mechanical properties also showed an inversely proportional relationship to electrical resistivity.

Acidity and Alkalinity in mine drainage: Practical considerations

USGS Publications Warehouse

Cravotta, III, Charles A.; Kirby, Carl S.

2004-01-01

In this paper, we emphasize that the Standard Method hot peroxide treatment procedure for acidity determination (hot acidity) directly measures net acidity or net alkalinity, but that more than one water-quality measure can be useful as a measure of the severity of acid mine drainage. We demonstrate that the hot acidity is related to the pH, alkalinity, and dissolved concentrations of Fe, Mn, and Al in fresh mine drainage. We show that the hot acidity accurately indicates the potential for pH to decrease to acidic values after complete oxidation of Fe and Mn, and it indicates the excess alkalinity or that required for neutralization of the sample. We show that the hot acidity method gives consistent, interpretable results on fresh or aged samples. Regional data for mine-drainage quality in Pennsylvania indicated the pH of fresh samples was predominantly acidic (pH 2.5 to 4) or near neutral (pH 6 to 7); approximately 25 percent of the samples had intermediate pH values. This bimodal frequency distribution of pH was distinctive for fully oxidized samples; oxidized samples had acidic or near-neutral pH, only. Samples that had nearneutral pH after oxidation had negative hot acidity; samples that had acidic pH after oxidation had positive hot acidity. Samples with comparable pH values had variable hot acidities owing to variations in their alkalinities and dissolved Fe, Mn, and Al concentrations. The hot acidity was comparable to net acidity computed on the basis of initial pH and concentrations of Fe, Mn, and Al minus the initial alkalinity. Acidity computed from the pH and dissolved metals concentrations, assuming equivalents of 2 per mole of Fe and Mn and 3 per mole of Al, was comparable to that computed on the basis of aqueous species and FeII/FeIII. Despite changes in the pH, alkalinity, and metals concentrations, the hot acidities were comparable for fresh and aged samples. Thus, meaningful “net” acidity can be determined from a measured hot acidity or by calculation from the pH, alkalinity, and dissolved metals concentrations. Together, these water-quality data can be useful for evaluating the potential for toxicity, corrosion, or encrustation and can be helpful for determining the appropriate remediation. By demonstrating the measurements on fresh and aged samples, we hope to encourage (1) consistent use of the hot peroxide treatment procedure for acidity determination and (2) consistent reporting of negative acidity values.

Groundwater-quality and quality-control data for two monitoring wells near Pavillion, Wyoming, April and May 2012

USGS Publications Warehouse

Wright, Peter R.; McMahon, Peter B.; Mueller, David K.; Clark, Melanie L.

2012-01-01

In June 2010, the U.S. Environmental Protection Agency installed two deep monitoring wells (MW01 and MW02) near Pavillion, Wyoming, to study groundwater quality. During April and May 2012, the U.S Geological Survey, in cooperation with the Wyoming Department of Environmental Quality, collected groundwater-quality data and quality-control data from monitoring well MW01 and, following well redevelopment, quality-control data for monitoring well MW02. Two groundwater-quality samples were collected from well MW01—one sample was collected after purging about 1.5 borehole volumes, and a second sample was collected after purging 3 borehole volumes. Both samples were collected and processed using methods designed to minimize atmospheric contamination or changes to water chemistry. Groundwater-quality samples were analyzed for field water-quality properties (water temperature, pH, specific conductance, dissolved oxygen, oxidation potential); inorganic constituents including naturally occurring radioactive compounds (radon, radium-226 and radium-228); organic constituents; dissolved gasses; stable isotopes of methane, water, and dissolved inorganic carbon; and environmental tracers (carbon-14, chlorofluorocarbons, sulfur hexafluoride, tritium, helium, neon, argon, krypton, xenon, and the ratio of helium-3 to helium-4). Quality-control sample results associated with well MW01 were evaluated to determine the extent to which environmental sample analytical results were affected by bias and to evaluate the variability inherent to sample collection and laboratory analyses. Field documentation, environmental data, and quality-control data for activities that occurred at the two monitoring wells during April and May 2012 are presented.

[Effects of preoperative oral carbohydrate administration on gastric contents].

PubMed

Sato, Chiaki; Shibuya, Hiromi; Nishino, Miho; Maeda, Akihiko; Shimakawa, Noriko; Okada, Toshiki

2012-08-01

Preoperative oral carbohydrate administration for adult patients has been recommended by European Society for Parenteral and Enteral Nutrition and Enhanced Recovery After Surgery. Although preoperative oral carbohydrate may improve patient satisfaction and perioperative glucose metabolism, its effects on the gastric contents remain controversial. We included 232 adult patients without gastrointestinal stenosis or occlusion. Seventy-four patients (group A) were not permitted to eat or drink before operation for eight hours, while 158 patients (group B) took oral carbohydrate (225 ml, 22.3% glucose) two hours before anesthesia induction. After induction, gastric contents were aspirated to examine its volume and pH. Although the mean volume of gastric contents of the patients in group B was significantly lower than that in group A, and gastric pH was also significantly smaller in group B, no patients suffered from aspiration during rapid induction. Fasting interval and gastric volume were inversely related, and almost all the patients with fasting interval above 150 minutes showed gastric contents volume smaller than 25 ml and gastric pH more than 2.5. We conclude that preoperative oral carbohydrate can be given safely, although the fasting interval should be 150 minutes in our diet regimen.

Comparison of arterial and venous blood gases and the effects of analysis delay and air contamination on arterial samples in patients with chronic obstructive pulmonary disease and healthy controls.

PubMed

O'Connor, T M; Barry, P J; Jahangir, A; Finn, C; Buckley, B M; El-Gammal, A

2011-01-01

Arterial blood gases (ABGs) are often sampled incorrectly, leading to a 'mixed' or venous sample. Delays in analysis and air contamination are common. We measured the effects of these errors in patients with chronic obstructive pulmonary disease (COPD) exacerbations and controls. Arterial and venous samples were analyzed from 30 patients with COPD exacerbation and 30 controls. Venous samples were analysed immediately and arterial samples separated into non-air-contaminated and air-contaminated specimens and analysed at 0, 30, 60, 90 and 180 min. Mean venous pH was 7.371 and arterial pH was 7.407 (p < 0.0001). There was a correlation between venous and arterial pH (r = 0.5347, p < 0.0001). The regression equation to predict arterial pH was: arterial pH = 4.2289 + 0.43113 · venous pH. There were no clinically significant differences in arterial PO₂ associated with analysis delay. A statistically significant decline in pH was detected at 30 min in patients with COPD exacerbation (p = 0.0042) and 90 min in controls (p < 0.0001). A clinically significant decline in pH emerged at 73 min in patients with COPD exacerbation and 87 min in controls. Air contamination was associated with a clinically significant increase in PO₂ in all samples, including those that were immediately analyzed. Arterial and venous pH differ significantly. Venous pH cannot accurately replace arterial pH. Temporal delays in ABG analysis result in a significant decline in measured pH. ABGs should be analysed within 30 min. Air contamination leads to an immediate increase in measured PO₂, indicating that air-contaminated ABGs should be discarded. Copyright © 2010 S. Karger AG, Basel.

3-D Surface Visualization of pH Titration "Topos": Equivalence Point Cliffs, Dilution Ramps, and Buffer Plateaus

ERIC Educational Resources Information Center

Smith, Garon C.; Hossain, Md Mainul; MacCarthy, Patrick

2014-01-01

3-D topographic surfaces ("topos") can be generated to visualize how pH behaves during titration and dilution procedures. The surfaces are constructed by plotting computed pH values above a composition grid with volume of base added in one direction and overall system dilution on the other. What emerge are surface features that…

Influence of pH, benzoic acid, glutathione, EDTA, 4-hexylresorcinol, and sodium chloride on the pressure inactivation kinetics of mushroom polyphenol oxidase.

PubMed

Weemaes, C A; Ludikhuyze, L R; Van den Broeck, I; Hendrickx, M E

1999-09-01

Pressure inactivation of mushroom PPO was studied for pH values ranging from 4 to 8, and the effect of some antibrowning agents on the pressure stability of mushroom PPO at pH 6.5 was evaluated. pH reduction below 6.5 resulted in a lowered inactivation threshold pressure and an increase of the absolute value of the activation volume (or a decrease of the z(p) value), the latter two parameters reflecting the pressure dependency of the inactivation rate constant. An increase in pH from 6.5 to 8, on the other hand, did only marginally affect the pressure stability of the enzyme. Mushroom PPO at pH 6.5 was markedly sensitized toward pressure by the presence of 2.5 mM 4-hexylresorcinol and slightly stabilized by the presence of 5 mM EDTA. The presence of 5 mM glutathione, sodium chloride, or benzoic acid caused no significant alteration of the enzyme pressure stability. Only in the presence of 4-hexylresorcinol, significant changes of the activation volume and z(p) value were noticed.

Control of rectal gland secretion by blood acid-base status in the intact dogfish shark (Squalus acanthias).

PubMed

Wood, Chris M; Munger, R Stephen; Thompson, Jill; Shuttleworth, Trevor J

2007-05-14

In order to address the possible role of blood acid-base status in controlling the rectal gland, dogfish were fitted with indwelling arterial catheters for blood sampling and rectal gland catheters for secretion collection. In intact, unanaesthetized animals, isosmotic volume loading with 500 mmol L-1 NaCl at a rate of 15 mL kg-1 h-1 produced a brisk, stable rectal gland secretion flow of about 4 mL kg-1 h-1. Secretion composition (500 mmol L-1 Na+ and Cl-; 5 mmol L-1 K+; <1 mmol L-1 Ca2+, Mg2+, SO(4)2-, or phosphate) was almost identical to that of the infusate with a pH of about 7.2, HCO3- mmol L-1<1 mmol L-1 and a PCO2 (1 Torr) close to PaCO2. Experimental treatments superimposed on the infusion caused the expected disturbances in systemic acid-base status: respiratory acidosis by exposure to high environmental PCO2, metabolic acidosis by infusion of HCl, and metabolic alkalosis by infusion of NaHCO3. Secretion flow decreased markedly with acidosis and increased with alkalosis, in a linear relationship with extracellular pH. Secretion composition did not change, apart from alterations in its acid-base status, and made negligible contribution to overall acid-base balance. An adaptive control of rectal gland secretion by systemic acid-base status is postulated-stimulation by the "alkaline tide" accompanying the volume load of feeding and inhibition by the metabolic acidosis accompanying the volume contraction of exercise.

Net alkalinity and net acidity 2: Practical considerations

USGS Publications Warehouse

Kirby, C.S.; Cravotta, C.A.

2005-01-01

The pH, alkalinity, and acidity of mine drainage and associated waters can be misinterpreted because of the chemical instability of samples and possible misunderstandings of standard analytical method results. Synthetic and field samples of mine drainage having various initial pH values and concentrations of dissolved metals and alkalinity were titrated by several methods, and the results were compared to alkalinity and acidity calculated based on dissolved solutes. The pH, alkalinity, and acidity were compared between fresh, unoxidized and aged, oxidized samples. Data for Pennsylvania coal mine drainage indicates that the pH of fresh samples was predominantly acidic (pH 2.5-4) or near neutral (pH 6-7); ??? 25% of the samples had pH values between 5 and 6. Following oxidation, no samples had pH values between 5 and 6. The Standard Method Alkalinity titration is constrained to yield values >0. Most calculated and measured alkalinities for samples with positive alkalinities were in close agreement. However, for low-pH samples, the calculated alkalinity can be negative due to negative contributions by dissolved metals that may oxidize and hydrolyze. The Standard Method hot peroxide treatment titration for acidity determination (Hot Acidity) accurately indicates the potential for pH to decrease to acidic values after complete degassing of CO2 and oxidation of Fe and Mn, and it indicates either the excess alkalinity or that required for neutralization of the sample. The Hot Acidity directly measures net acidity (= -net alkalinity). Samples that had near-neutral pH after oxidation had negative Hot Acidity; samples that had pH < 6.3 after oxidation had positive Hot Acidity. Samples with similar pH values before oxidation had dissimilar Hot Acidities due to variations in their alkalinities and dissolved Fe, Mn, and Al concentrations. Hot Acidity was approximately equal to net acidity calculated based on initial pH and dissolved concentrations of Fe, Mn, and Al minus the initial alkalinity. Acidity calculated from the pH and dissolved metals concentrations, assuming equivalents of 2 per mole of Fe and Mn and 3 per mole of Al, was equivalent to that calculated based on complete aqueous speciation of FeII/FeIII. Despite changes in the pH, alkalinity, and metals concentrations, the Hot Acidities were comparable for fresh and most aged samples. A meaningful "net" acidity can be determined from a measured Hot Acidity or by calculation from the pH, alkalinity, and dissolved metals concentrations. The use of net alkalinity = (Alkalinitymeasured - Hot Aciditymeasured) to design mine drainage treatment can lead to systems with insufficient Alkalinity to neutralize metal and H+ acidity and is not recommended. The use of net alkalinity = -Hot Acidity titration is recommended for the planning of mine drainage treatment. The use of net alkalinity = (Alkalinitymeasured - Aciditycalculated) is recommended with some cautions. ?? 2005 Elsevier Ltd. All rights reserved.

Carbonate system at Iheya North in Okinawa Trough~IODP drilling and post drilling environment~

NASA Astrophysics Data System (ADS)

Noguchi, T.; Hatta, M.; Sunamura, M.; Fukuba, T.; Suzue, T.; Kimoto, H.; Okamura, K.

2012-12-01

The Iheya North hydrothermal field in middle Okinawa Trough is covered with thick hemipelagic and volcanic sediment. Geochemical characteristics of Okinawa Trough is to provide abundant of CO2, CH4, NH4, H2, and H2S which originated from magmatic gases, sedimentary organic matters. On this hydrothermal field, a scientific drilling by Integrated Ocean Drilling Program (IODP) Expedition 331 was conducted to investigate metabolically diverse subseafloor microbial ecosystem and their physical and chemical settings. To clarify the spatial distribution of physical condition beneath seafloor around the hydrothermal filed, we focus on the carbonate species analysis to reconstruct in-situ pH, which regulate the diversities of microbial community and mineral composition. We developed the small sample volume dissolved total inorganic carbon (DIC) analyzer and conducted the onboard analysis for the interstitial water during IODP Exp.331. Total alkalinity, boron, phosphate, and ammonium also analyzed for thermodynamic calculation. In this presentation, we represent the spatial distribution of pH beneath the Iheya North hydrothermal field. In addition, we developed a 128 bottles multiple water sampler (ANEMONE) for post drilling environmental monitoring. ANEMONE sampler was deployed on the manned submersible Shinkai 6500 with other chemical sensors (CTD, turbidity, pH, ORP, and H2S), and collected the hydrothermal plume samples every 5 minutes during YK12-05 cruise by R/V Yokosuka (Japan Agency for Marine-Earth Science and Technology, JAMSTEC). DIC concentration of plume samples collected by ANEMONE sampler were analyzed just after submersible retrieve, and nutrients, manganese, density, and total cell counts determination were conducted onshore analysis. Based on these results, we describe the spatial distribution of DIC and carbonate system on Iheya North hydrothermal field (interstitial water, hydrothermal fluid, and hydrothermal plume).

Dipstick Spot urine pH does not accurately represent 24 hour urine PH measured by an electrode.

PubMed

Omar, Mohamed; Sarkissian, Carl; Jianbo, Li; Calle, Juan; Monga, Manoj

2016-01-01

To determine whether spot urine pH measured by dipstick is an accurate representation of 24 hours urine pH measured by an electrode. We retrospectively reviewed urine pH results of patients who presented to the urology stone clinic. For each patient we recorded the most recente pH result measured by dipstick from a spot urine sample that preceded the result of a 24-hour urine pH measured by the use of a pH electrode. Patients were excluded if there was a change in medications or dietary recommendations or if the two samples were more than 4 months apart. A difference of more than 0.5 pH was considered na inaccurate result. A total 600 patients were retrospectively reviewed for the pH results. The mean difference in pH between spot urine value and the 24 hours collection values was 0.52±0.45 pH. Higher pH was associated with lower accuracy (p<0.001). The accuracy of spot urine samples to predict 24-hour pH values of <5.5 was 68.9%, 68.2% for 5.5 to 6.5 and 35% for >6.5. Samples taken more than 75 days apart had only 49% the accuracy of more recent samples (p<0.002). The overall accuracy is lower than 80% (p<0.001). Influence of diurnal variation was not significant (p=0.588). Spot urine pH by dipstick is not an accurate method for evaluation of the patients with urolithiasis. Patients with alkaline urine are more prone to error with reliance on spot urine pH.

Synthesis, characterization, and application of novel Zn(II)-ionic imprinted polymer for preconcentration of Zn(II) ions from aqueous solution

NASA Astrophysics Data System (ADS)

Wirawan, T.; Supriyanto, G.; Soegianto, A.

2018-04-01

Preparation of a new Zn2+ ion-imprinted polymer (Zn-IIP) is presented in this report. The Zn-IIP are prepared by precipitation polymerization using 8-hydroxyquinoline (8HQ) as a ligand, methacrylic acid (MAA) as functional monomer, and ethylene glycol dimethacrylate (EGDMA) as a cross-linker has been prepared. The benzoyl peroxide and ethanol/acetonitrile (2:1) mixture were used as initiator and porogen, respectively. Precipitation polymerization was carried out by heating in a water bath at 60°C for 8 hours. After polymerization, cavities in the polymer particles corresponding to the Zn2+ ions were created by leaching the polymer with 2 mol L-1 HNO3. The polymer was washed with aquabidest and dried in an oven at the temperature of 60°C for 24 hours. The Zn-IIP was characterized by Fourier Transform Infrared Spectrophotometry (FT-IR) and Scanning Electron Microscopy (SEM). The synthesized Zn-IIP was used as a new adsorbent for solid phase extraction (SPE) of Zn(II) prior to Flame Atomic Absorption Spectrometry (FAAS) determination. The experimental parameters for SPE, such as pH of the sample, loading rate, and elution volume, have been optimized. The effect of pH of the sample on the extraction of analyte was studied in batch mode. The effects of loading rate and elution volume on the extraction of analyte were studied in dynamic mode by loading of the sample through IIP-SPE cartridge containing 100 mg of the synthesized Zn-IIP. The imprinted polymer (Zn-IIP) have bands at 3433.06 cm-1 (O-H), 1508.23 cm-1 (C=N aromatics), 1284.5 cm-1 (C-N aromatics), 1056.9 cm-1 (C-O phenol), 1724.24 cm-1 (C=O), and 1639.38 cm-1 (conjugated C=O with C=C). The Scanning Electron Microscopy (SEM) images of IIP and IIP show that the IIP is seen to have more cavities than NIP. The optimum pH for quantitative Zn(II) retention was 5.5, and the elution was completed with 2 mL of 1.0 mol L-1 nitric acid. The optimum loading rate was 0.5 mL min-1. The recovery of Zn(II) from solution samples after its SPE extraction on IIP with 50-fold theoretical preconcentration was 94.60-104.50%. The LOD and LOQ with 50-fold theoretical preconcentration obtained were 0.0073 mg L-1 and 0.0244 mg L-1, respectively.

Solid-phase extraction of heavy metal ions on bucky tubes disc in natural water and herbal plant samples.

PubMed

Soylak, Mustafa; Unsal, Yunus Emre

2011-10-01

A preconcentration-separation procedure has been established based on solid-phase extraction of Fe(III) and Pb(II) on bucky tubes (BTs) disc. Fe(III) and Pb(II) ions were quantitatively recovered at pH 6. The influences of the analytical parameters like sample volume, flow rates on the recoveries of analytes on BT disc were investigated. The effects of co-existing ions on the recoveries were also studied. The detection limits for iron and lead were found 1.6 and 4.9 μg L⁻¹, respectively. The validation of the presented method was checked by the analysis of TMDA-51.3 fortified water certified reference material. The presented procedure was successfully applied to the separation-preconcentration and determination of iron and lead content of some natural water and herbal plant samples from Kayseri, Turkey.

Novel polymeric monolith materials with a β-cyclodextrin-graphene composite for the highly selective extraction of methyl jasmonate.

PubMed

Yu, Xinhong; Ling, Xu; Zou, Li; Chen, Zilin

2017-04-01

A novel polymeric monolith column with a  β-cyclodextrin-graphene composite was prepared for extraction of methyl jasmonate. A simple, sensitive, and effective polymeric monolith microextraction with high-performance liquid chromatography method has been presented for the determination. To carry out the best microextraction efficiency, several parameters such as sample flow rate, sample volume, and sample pH value were systematically optimized. In addition, the method validation showed a wide linear range of 5-2000 ng/mL, with a good linearity and low limits of detection for methyl jasmonate. The proposed method was successfully applied for the determination of methyl jasmonate in wintersweet flowers with recoveries of 90.67%. The result was confirmed by high-performance liquid chromatography with mass spectrometry. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Observations of radiation fog chemistry in the Eastern United States

NASA Astrophysics Data System (ADS)

Straub, D.; Hutchings, J.; Herckes, P.

2010-07-01

The chemical composition of radiation fog in the Mid-Atlantic region of the United States has been the focus of an ongoing field campaign based in Selinsgrove, PA. This field study was established to provide a long term record that can be used to identify the effects of meteorology and air mass source regions on fog composition and to shed light on the role that fog can play in the production of secondary inorganic and organic aerosol mass. In the United States, studies that focus on radiation fog have been relatively rare. For the most part, they have been limited geographically to the Central Valley of California, though individual studies have also been conducted in the Central United States and along the Texas-Louisiana Gulf Coast. Sample collection for the current study began during the fall of 2007. Through 2009, samples from 25 radiation fog events have been obtained. A Caltech Heated Rod Cloudwater Collector (CHRCC) having a Dp50 of approximately 8 microns was used to collect one fog sample per event. Samples were typically collected between 2:00 AM and 7:00 AM under conditions of light winds, clear skies, and recent rainfall. Sample volumes ranged from 2.9 ml to 150 ml. Following collection, samples were analyzed for pH and then one of the following: major inorganic ions, dissolved total organic carbon, N-nitrosodimethylamine (NDMA), metals, or organic speciation. Through 2009, sample pH varied between 4.28 and 6.86 and averaged 5.03 based on H+ concentration. Ammonium and sulfate were found to be the most abundant ionic species in the fog samples. Sufficient ammonium was detected in nearly every sample to fully neutralize nitrate and sulfate. The concentrations of sulfate, nitrate, and ammonium observed in this study were lower than values reported in the literature for most other cloud and fog studies conducted in the US. Due to significant ammonium input, pH in the current study was higher than most other studies. Concentrations of total organic carbon averaged 7.22 mgC/L, which is lower than other radiation fogs studies but similar to that for many cloud studies. NDMA concentrations in two analyzed samples were considered high, but not outside the range that could be expected through equilibrium with potential gas phase concentrations.

The final frontier of pH and the undiscovered country beyond.

PubMed

Bal, Wojciech; Kurowska, Ewa; Maret, Wolfgang

2012-01-01

The comparison of volumes of cells and subcellular structures with the pH values reported for them leads to a conflict with the definition of the pH scale. The pH scale is based on the ionic product of water, K(w) = [H(+)]×[OH(-)].We used K(w) [in a reversed way] to calculate the number of undissociated H(2)O molecules required by this equilibrium constant to yield at least one of its daughter ions, H(+) or OH(-) at a given pH. In this way we obtained a formula that relates pH to the minimal volume V(pH) required to provide a physical meaning to K(w), V(pH)=10(pH-pK(w/2) x 10(pK(w/2)/N(A) (where N(A) is Avogadro's number). For example, at pH 7 (neutral at 25°C) V(pH) =16.6 aL. Any deviation from neutral pH results in a larger V(pH) value. Our results indicate that many subcellular structures, including coated vesicles and lysosomes, are too small to contain free H(+) ions at equilibrium, thus the definition of pH based on K(w) is no longer valid. Larger subcellular structures, such as mitochondria, apparently contain only a few free H(+) ions. These results indicate that pH fails to describe intracellular conditions, and that water appears to be dissociated too weakly to provide free H(+) ions as a general source for biochemical reactions. Consequences of this finding are discussed.

Uncertainty Estimation for the Determination of Ni, Pb and Al in Natural Water Samples by SPE-ICP-OES

NASA Astrophysics Data System (ADS)

Ghorbani, A.; Farahani, M. Mahmoodi; Rabbani, M.; Aflaki, F.; Waqifhosain, Syed

2008-01-01

In this paper we propose uncertainty estimation for the analytical results we obtained from determination of Ni, Pb and Al by solidphase extraction and inductively coupled plasma optical emission spectrometry (SPE-ICP-OES). The procedure is based on the retention of analytes in the form of 8-hydroxyquinoline (8-HQ) complexes on a mini column of XAD-4 resin and subsequent elution with nitric acid. The influence of various analytical parameters including the amount of solid phase, pH, elution factors (concentration and volume of eluting solution), volume of sample solution, and amount of ligand on the extraction efficiency of analytes was investigated. To estimate the uncertainty of analytical result obtained, we propose assessing trueness by employing spiked sample. Two types of bias are calculated in the assessment of trueness: a proportional bias and a constant bias. We applied Nested design for calculating proportional bias and Youden method to calculate the constant bias. The results we obtained for proportional bias are calculated from spiked samples. In this case, the concentration found is plotted against the concentration added and the slop of standard addition curve is an estimate of the method recovery. Estimated method of average recovery in Karaj river water is: (1.004±0.0085) for Ni, (0.999±0.010) for Pb and (0.987±0.008) for Al.

Preconcentration of Sn (II) using the methylene blue on the activated carbon and its determination by spectrophotometry method.

PubMed

Khodadoust, Saeid; Cham Kouri, Narges

2014-04-05

A simple and accurate spectrophotometric method for determination of trace amounts of Sn (II) ion in soil sample was developed by using the methylene blue (MB) in the presence of activated carbon (AC) as the adsorbent Solid Phase Extraction (SPE) of Sn (II) and then determined by UV-Vis. The Beer's law is obeyed over the concentration range of 1-80ngmL(-1) of Sn (II) with the detection limits of 0.34ngmL(-1). The influence of type and volume of eluent, concentration of MB, pH, and amount of AC on sensitivity of spectrophotometric method were optimized. The method has been successfully applied for Sn (II) ion determination in soil sample. Copyright © 2013 Elsevier B.V. All rights reserved.

Solid-phase extraction of some heavy metal ions on a double-walled carbon nanotube disk and determination by flame atomic absorption spectrometry.

PubMed

Karatepe, Aslihan; Soylak, Mustafa; Elçi, Latif

2011-01-01

A new preconcentration method was developed for the determination of trace amounts of Cu(II), Fe(III), Pb(II), Ni(II), and Cd(II) on a double-walled carbon nanotube disk. 4-(2-Thiazolylazo) resorcinol was used as a complexing reagent. The effects of parameters, including pH of the solutions, amounts of complexing reagent, eluent type, sample volume, flow rates of solutions, and matrix ions were examined for quantitative recoveries of the studied analyte ions. The retained metal ions were eluted by 2 M HNO3. The LOD values for the analytes were in the range of 0.7-4.4 microg/mL. Natural water samples and standard reference materials were analyzed by the presented method.

Annual Progress Report FY-91. Volume 1 and 2.

DTIC Science & Technology

1992-03-12

Pulmonary Med Tech 11 0644 GS Berger, TA Allergy Microbiologist 12 0403 GS Billups, L Flow Cytom Chemist 12 1320 GS Vacant Pulmonary Kyle Metabolic Unit...Reactions 11 (11/89) 3349 Salata, Kalman PhD. Mitogen-Inducible T Suppressor Cell 12 Assay by Flow Cytometry (12/89) 3350 Salata, Kalman PhD. Flow ...3/90) 3354 Salata, Kalman PhD. Two Way Mixed Lymphocyte Culture: 17 Analysis by Two Color Flow Cytometry (4/90) 3355 Salata, Kalman PhD. Effect of

The colour degradation of anthocyanin-rich extract from butterfly pea (Clitoria ternatea L.) petal in various solvents at pH 7.

PubMed

Marpaung, Abdullah Muzi; Andarwulan, Nuri; Hariyadi, Purwiyatno; Nur Faridah, Didah

2017-10-01

A spectroscopic study was conducted to evaluate the colour degradation mechanism of anthocyanin-rich extract from butterfly pea petal. The extract was diluted in four different solvent systems, which were buffer solution pH 7 (AQ7) and the mixture of organic solvent with buffer solution pH 7 (4:1 v/v). The organic cosolvent involved were methanol (ME7), ethanol (ET7) and acetone (AC7). The samples were stored in containers with 0% and 50% headspace, and their colour intensity, total anthocyanin and hypsochromic shift were evaluated periodically. The rank of colour and anthocyanin degradation from the biggest was AQ7 > ME7 > ET7 > AC7. The longest hypsochromic shift was AQ7 > ME7 > ET7, while in AC7 the shift was absent. There was evidence that the volume of package headspace provoked colour stability. The colour degradation in AC7 was proposed to occur through hydrophobic interaction unfolding, and in AQ7 was through the deacylation, while in ME7 and ET7 was due to both mechanisms.

Dispersive liquid-liquid microextraction based on the solidification of floating organic drop followed by ICP-MS for the simultaneous determination of heavy metals in wastewaters

NASA Astrophysics Data System (ADS)

Li, Yong; Peng, Guilong; He, Qiang; Zhu, Hui; Al-Hamadani, Sulala M. Z. F.

2015-04-01

In the present work, a dispersive liquid-liquid microextraction based on the solidification of floating organic drop (DLLME-SFO) combined with inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of Pb, Co, Cu, Ni, Zn. The influences of analytical parameters, including pH, extraction solvent volume, disperser solvent volume, concentration of chelating agent on the quantitative recoveries of Pb, Co, Cu, Ni, Zn were investigated. The effect of the interfering ions on the analytes recovery was also investigated. Under the optimized conditions, the limits of detection were 0.97-2.18 ng L-1. The relative standard deviations (RSDs) were 2.62-4.51% (n = 7, C = 20 ng L-1). The proposed method was successfully applied for the analysis of ultra trace metals in wastewater samples.

Pleurotus eryngii immobilized Amberlite XAD-16 as a solid-phase biosorbent for preconcentrations of Cd2+ and Co2+ and their determination by ICP-OES.

PubMed

Özdemir, Sadin; Okumuş, Veysi; Kılınç, Ersin; Bilgetekin, Havin; Dündar, Abdurrahman; Ziyadanogˇulları, Berrin

2012-09-15

This article reports a method that is used for the preconcentration and determination of Cd(2+) and Co(2+) in vegetables, using Pleurotus eryngii immobilized Amberlite XAD-16 as a solid-phase biosorbent. The concentrations of metals were determined by inductively coupled plasma-optical spectrometry (ICP-OES). Critical parameters, such as the pH of the solution, flow rate, the amount of biosorbent, type and volume of eluent, and the sample volume, that affect the solid-phase extraction (SPE) procedure were optimized. The optimum extraction conditions were determined as being a pH of 6.0 for Cd(2+) and of 5.0 for Co(2+); a sample flow rate of 2.0 mL min(-1); 200.0mg of biosorbent; and 5.0 mL of 1.0 mol L(-1) HCl as eluent. The capacities of the biosorbent for metal uptake were found to be 11.3 and 9.8 mg g(-1) for Cd(2+) and Co(2+) ions, respectively. Limit of quantitations (LOQs) were found to be 0.67 and 0.82 ng mL(-1), respectively, for Cd(2+) and Co(2+). The linear working curves were observed to be in the linear range from 1.0 to 50.0 ng mL(-1), and possessed high correlation coefficients. The use of the SPE method showed 50.7- and 35.7-fold improvements in the sensitivities of ICP-OES. The developed method was successfully applied to NCS ZC-73014 (a certified reference tea sample). Relative standard deviations (RSD) were lower than 5.0%. The Cd(2+) and Co(2+) concentrations in the different parts (leave, root, stem, and fruit) of purslane, onion, rocket, okra, and aubergine were determined after microwave digestion and solid-phase extraction by P. eryngii immobilized on Amberlite XAD-16. Copyright © 2012 Elsevier B.V. All rights reserved.

An Optimized Method for the Measurement of Acetaldehyde by High-Performance Liquid Chromatography

PubMed Central

Guan, Xiangying; Rubin, Emanuel; Anni, Helen

2011-01-01

Background Acetaldehyde is produced during ethanol metabolism predominantly in the liver by alcohol dehydrogenase, and rapidly eliminated by oxidation to acetate via aldehyde dehydrogenase. Assessment of circulating acetaldehyde levels in biological matrices is performed by headspace gas chromatography and reverse phase high-performance liquid chromatography (RP-HPLC). Methods We have developed an optimized method for the measurement of acetaldehyde by RP-HPLC in hepatoma cell culture medium, blood and plasma. After sample deproteinization, acetaldehyde was derivatized with 2,4-dinitrophenylhydrazine (DNPH). The reaction was optimized for pH, amount of derivatization reagent,, time and temperature. Extraction methods of the acetaldehyde-hydrazone (AcH-DPN) stable derivative and product stability studies were carried out. Acetaldehyde was identified by its retention time in comparison to AcH-DPN standard, using a new chromatography gradient program, and quantitated based on external reference standards and standard addition calibration curves in the presence and absence of ethanol. Results Derivatization of acetaldehyde was performed at pH 4.0 with a 80-fold molar excess of DNPH. The reaction was completed in 40 min at ambient temperature, and the product was stable for 2 days. A clear separation of AcH-DNP from DNPH was obtained with a new 11-min chromatography program. Acetaldehyde detection was linear up to 80 μM. The recovery of acetaldehyde was >88% in culture media, and >78% in plasma. We quantitatively determined the ethanol-derived acetaldehyde in hepatoma cells, rat blood and plasma with a detection limit around 3 μM. The accuracy of the method was <9% for intraday and <15% for interday measurements, in small volume (70 μl) plasma sampling. Conclusions An optimized method for the quantitative determination of acetaldehyde in biological systems was developed using derivatization with DNPH, followed by a short RP-HPLC separation of AcH-DNP. The method has an extended linear range, is reproducible and applicable to small volume sampling of culture media and biological fluids. PMID:21895715

Rapid ultrasound-assisted magnetic microextraction of gallic acid from urine, plasma and water samples by HKUST-1-MOF-Fe3O4-GA-MIP-NPs: UV-vis detection and optimization study.

PubMed

Asfaram, Arash; Ghaedi, Mehrorang; Dashtian, Kheibar

2017-01-01

Magnetite (Fe 3 O 4 nanoparticles (NPs)) HKUST-1 metal organic framework (MOF) composite as a support was used for surface imprinting of gallic acid imprinted polymer (HKUST-1-MOF-Fe 3 O 4 -GA-MIP) using vinyltrimethoxysilane (VTMOS) as the cross-linker. Subsequently, HKUST-1-MOF-Fe 3 O 4 -NPs-GA-MIP characterized by FT-IR, XRD and FE-SEM analysis and applied for fast and selective and sensitive ultrasound assisted dispersive magnetic solid phase microextraction of gallic acid (GA) by UV-Vis (UA-DMSPME-UV-Vis) detection method. Plackett-Burman design (PBD) and central composite design (CCD) according to desirability function (DF) indicate the significant variables among the extraction factors vortex (mixing) time (min), sonication time (min), temperature (°C), eluent volume (L), pH and HKUST-1-MOF-Fe 3 O 4 -NPs-GA-MIP mass (mg) and their contribution on the response. Optimum conditions and values correspond to pH, HKUST-1-MOF-Fe 3 O 4 -NPs-GA-MIP mass, sonication time and the eluent volume were set as follow 3.0, 1.6mg, 4.0min and 180μL, respectively. The average recovery (ER%) of GA was 98.13% with desirability of 0.997, while the present method has best operational performance like wide linear range 8-6000ngmL -1 with a Limit of detection (LOD) of 1.377ngmL -1 , limit of quantification (LOQ) 4.591ngmL -1 and precision (<3.50% RSD). The recovery of GA in urine, human plasma and water samples within the range of 92.3-100.6% that strongly support high applicability of present method for real samples analysis, which candidate this method as promise for further application. Copyright © 2016. Published by Elsevier B.V.

An optimized method for the measurement of acetaldehyde by high-performance liquid chromatography.

PubMed

Guan, Xiangying; Rubin, Emanuel; Anni, Helen

2012-03-01

Acetaldehyde is produced during ethanol metabolism predominantly in the liver by alcohol dehydrogenase and rapidly eliminated by oxidation to acetate via aldehyde dehydrogenase. Assessment of circulating acetaldehyde levels in biological matrices is performed by headspace gas chromatography and reverse phase high-performance liquid chromatography (RP-HPLC). We have developed an optimized method for the measurement of acetaldehyde by RP-HPLC in hepatoma cell culture medium, blood, and plasma. After sample deproteinization, acetaldehyde was derivatized with 2,4-dinitrophenylhydrazine (DNPH). The reaction was optimized for pH, amount of derivatization reagent, time, and temperature. Extraction methods of the acetaldehyde-hydrazone (AcH-DNP) stable derivative and product stability studies were carried out. Acetaldehyde was identified by its retention time in comparison with AcH-DNP standard, using a new chromatography gradient program, and quantitated based on external reference standards and standard addition calibration curves in the presence and absence of ethanol. Derivatization of acetaldehyde was performed at pH 4.0 with an 80-fold molar excess of DNPH. The reaction was completed in 40 minutes at ambient temperature, and the product was stable for 2 days. A clear separation of AcH-DNP from DNPH was obtained with a new 11-minute chromatography program. Acetaldehyde detection was linear up to 80 μM. The recovery of acetaldehyde was >88% in culture media and >78% in plasma. We quantitatively determined the ethanol-derived acetaldehyde in hepatoma cells, rat blood and plasma with a detection limit around 3 μM. The accuracy of the method was <9% for intraday and <15% for interday measurements, in small volume (70 μl) plasma sampling. An optimized method for the quantitative determination of acetaldehyde in biological systems was developed using derivatization with DNPH, followed by a short RP-HPLC separation of AcH-DNP. The method has an extended linear range, is reproducible and applicable to small-volume sampling of culture media and biological fluids. Copyright © 2011 by the Research Society on Alcoholism.

Ultratrace determination of arsenic in water samples by electrothermal atomic absorption spectrometry after pre-concentration with Mg-Al-Fe ternary layered double hydroxide nano-sorbent.

PubMed

Abdolmohammad-Zadeh, Hossein; Jouyban, Abolghasem; Amini, Roghayeh

2013-11-15

A selective solid phase extraction method, based on nano-structured Mg-Al-Fe(NO3(-)) ternary layered double hydroxide as a sorbent, is developed for the pre-concentration of ultra-trace levels of arsenic (As) prior to determination by electrothermal atomic absorption spectrometry. It is found that both As(III) and As(V) could be quantitatively retained on the sorbent within a wide pH range of 4-12. Accordingly, the presented method is applied to determination of total inorganic As in aqueous solutions. Maximum analytical signal of As is achieved when the pyrolysis and atomization temperatures are close to 900 °C and 2300 °C, respectively. Several variables affecting the extraction efficiency including pH, sample flow rate, amount of nano-sorbent, elution conditions and sample volume are optimized. Under the optimized conditions, the limit of detection (3Sb/m) and the relative standard deviation are 4.6 pg mL(-1) and 3.9%, respectively. The calibration graph is linear in the range of 15.0-650 pg mL(-1) with a correlation coefficient of 0.9979, sorption capacity and pre-concentration factor are 8.68 mg g(-1) and 300, respectively. The developed method is validated by the analysis of a standard reference material (SRM 1643e) and is successfully applied to the determination of ultra-trace amounts of As in different water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Preparation of an aminopropyl imidazole-modified silica gel as a sorbent for solid-phase extraction of carboxylic acid compounds and polycyclic aromatic hydrocarbons.

PubMed

Wang, Na; Guo, Yong; Wang, Licheng; Liang, Xiaojing; Liu, Shujuan; Jiang, Shengxiang

2014-05-21

In this paper, a kind of aminopropyl imidazole-modified silica sorbent was synthesized and used as a solid-phase extraction (SPE) sorbent for the determination of carboxylic acid compounds and polycyclic aromatic hydrocarbons (PAHs). The resultant aminopropyl imidazole-modified silica sorbent was characterized by Fourier transform infrared spectroscopy (FT-IR) and elemental analysis (EA) to ensure the successful binding of aminopropyl imidazole on the surface of silica gel. Then the aminopropyl imidazole-modified silica sorbent served as a SPE sorbent for the enrichment of carboxylic acid compounds and PAHs. The new sorbent exhibited high extraction efficiency towards the tested compounds and the results show that such a sorbent can offer multiple intermolecular interactions: electrostatic, π-π, and hydrophobic interactions. Several parameters affecting the extraction recovery, such as the pH of sample solution, the pH of eluent, the solubility of eluent, the volume of eluent, and sample loading, were also investigated. Under the optimized conditions, the proposed method was applied to the analysis of four carboxylic acid compounds and four PAHs in environmental water samples. Good linearities were obtained for all the tested compounds with R(2) larger than 0.9903. The limits of detection were found to be in the range of 0.0065-0.5 μg L(-1). The recovery values of spiked river water samples were from 63.2% to 112.3% with relative standard deviations (RSDs) less than 10.1% (n = 4).

Speciation analysis of Mn(II)/Mn(VII) using Fe3O4@ionic liquids-β-cyclodextrin polymer magnetic solid phase extraction coupled with ICP-OES.

PubMed

Chen, Songqing; Qin, Xingxiu; Gu, Weixi; Zhu, Xiashi

2016-12-01

Ionic liquids-β-cyclodextrin polymer (ILs-β-CDCP) was attached on Fe 3 O 4 nanoparticles to prepare magnetic solid phase extraction agent (Fe 3 O 4 @ILs-β-CDCP). The properties and morphology of Fe 3 O 4 @ILs-β-CDCP were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction(XRD), size distribution and magnetic analysis. A new method of magnetic solid phase extraction (MSPE) coupled to ICP-OES for the speciation of Mn(II)/Mn(VII) in water samples was established. The results showed that Mn(VII) and total manganese [Mn(II)+Mn(VII)] were quantitatively extracted after adjusting aqueous sample solution to pH 6.0 and 10.0, respectively. Mn(II) was calculated by subtraction of Mn(VII) from total manganese. Fe 3 O 4 @ILs-β-CDCP showed a higher adsorption capacity toward Mn(II) and Mn(VII). Several factors, such as the pH value, extraction temperature and sample volume, were optimized to achieve the best extraction efficiency. Moreover, the adsorption ability of Fe 3 O 4 @ILs-β-CDCP would not be significantly lower after reusing of 10 times. The accuracy of the developed method was confirmed by analyzing certified reference materials (GSB 07-1189-2000), and by spiking spring water, city water and lake water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Chemical Reaction between Boric Acid and Phosphine Indicates Boric Acid as an Antidote for Aluminium Phosphide Poisoning

PubMed Central

Soltani, Motahareh; Shetab-Boushehri, Seyed F.; Shetab-Boushehri, Seyed V.

2016-01-01

Objectives: Aluminium phosphide (AlP) is a fumigant pesticide which protects stored grains from insects and rodents. When it comes into contact with moisture, AlP releases phosphine (PH3), a highly toxic gas. No efficient antidote has been found for AlP poisoning so far and most people who are poisoned do not survive. Boric acid is a Lewis acid with an empty p orbital which accepts electrons. This study aimed to investigate the neutralisation of PH3 gas with boric acid. Methods: This study was carried out at the Baharlou Hospital, Tehran University of Medical Sciences, Tehran, Iran, between December 2013 and February 2014. The volume of released gas, rate of gas evolution and changes in pH were measured during reactions of AlP tablets with water, acidified water, saturated boric acid solution, acidified saturated boric acid solution, activated charcoal and acidified activated charcoal. Infrared spectroscopy was used to study the resulting probable adduct between PH3 and boric acid. Results: Activated charcoal significantly reduced the volume of released gas (P <0.01). Although boric acid did not significantly reduce the volume of released gas, it significantly reduced the rate of gas evolution (P <0.01). A gaseous adduct was formed in the reaction between pure AlP and boric acid. Conclusion: These findings indicate that boric acid may be an efficient and non-toxic antidote for PH3 poisoning. PMID:27606109

A dispersive liquid--liquid microextraction methodology for copper (II) in environmental samples prior to determination using microsample injection flame atomic absorption spectrometry.

PubMed

Alothman, Zeid A; Habila, Mohamed; Yilmaz, Erkan; Soylak, Mustafa

2013-01-01

A simple, environmentally friendly, and efficient dispersive liquid-liquid microextraction method combined with microsample injection flame atomic absorption spectrometry was developed for the separation and preconcentration of Cu(II). 2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol (5-Br-PADAP) was used to form a hydrophobic complex of Cu(II) ions in the aqueous phase before extraction. To extract the Cu(II)-5-Br-PADAP complex from the aqueous phase to the organic phase, 2.0 mL of acetone as a disperser solvent and 200 microL of chloroform as an extraction solvent were used. The influences of important analytical parameters, such as the pH, types and volumes of the extraction and disperser solvents, amount of chelating agent, sample volume, and matrix effects, on the microextraction procedure were evaluated and optimized. Using the optimal conditions, the LOD, LOQ, preconcentration factor, and RSD were determined to be 1.4 microg/L, 4.7 microg/L, 120, and 6.5%, respectively. The accuracy of the proposed method was investigated using standard addition/recovery tests. The analysis of certified reference materials produced satisfactory analytical results. The developed method was applied for the determination of Cu in real samples.

Monitoring of trace amounts of heavy metals in different food and water samples by flame atomic absorption spectrophotometer after preconcentration by amine-functionalized graphene nanosheet.

PubMed

Behbahani, Mohammad; Tapeh, Nasim Akbari Ghareh; Mahyari, Mojtaba; Pourali, Ali Reza; Amin, Bahareh Golrokh; Shaabani, Ahmad

2014-11-01

We are introducing graphene oxide modified with amine groups as a new solid phase for extraction of heavy metal ions including cadmium(II), copper(II), nickel(II), zinc(II), and lead(II). Effects of pH value, flow rates, type, concentration, and volume of the eluent, breakthrough volume, and the effect of potentially interfering ions were studied. Under optimized conditions, the extraction efficiency is >97 %, the limit of detections are 0.03, 0.05, 0.2, 0.1, and 1 μg L(-1) for the ions of cadmium, copper, nickel, zinc, and lead, respectively, and the adsorption capacities for these ions are 178, 142, 110, 125, and 210 mg g(-1). The amino-functionalized graphene oxide was characterized by thermogravimetric analysis, transmission electron microscopy, scanning electron microscopy, and Fourier transform infrared spectrometry. The proposed method was successfully applied in the analysis of environmental water and food samples. Good spiked recoveries over the range of 95.8-100.0 % were obtained. This work not only proposes a useful method for sample preconcentration but also reveals the great potential of modified graphene as an excellent sorbent material in analytical processes.

Vortex-assisted surfactant-enhanced emulsification microextraction based on solidification of floating organic drop combined with high performance liquid chromatography for determination of naproxen and nabumetone.

PubMed

Asadi, Mohammad; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh; Abbasi, Bijan

2015-12-18

A novel, rapid, simple and green vortex-assisted surfactant-enhanced emulsification microextraction method based on solidification of floating organic drop was developed for simultaneous separation/preconcentration and determination of ultra trace amounts of naproxen and nabumetone with high performance liquid chromatography-fluorescence detection. Some parameters influencing the extraction efficiency of analytes such as type and volume of extractant, type and concentration of surfactant, sample pH, KCl concentration, sample volume, and vortex time were investigated and optimized. Under optimal conditions, the calibration graph exhibited linearity in the range of 3.0-300.0ngL(-1) for naproxen and 7.0-300.0ngL(-1) for nabumetone with a good coefficient of determination (R(2)>0.999). The limits of detection were 0.9 and 2.1ngL(-1). The relative standard deviations for inter- and intra-day assays were in the range of 5.8-10.1% and 3.8-6.1%, respectively. The method was applied to the determination of naproxen and nabumetone in urine, water, wastewater and milk samples and the accuracy was evaluated through recovery experiments. Copyright © 2015 Elsevier B.V. All rights reserved.

Suitability of dispersive liquid-liquid microextraction for the in situ silylation of chlorophenols in water samples before gas chromatography with mass spectrometry.

PubMed

Saraji, Mohammad; Ghambari, Hoda

2015-10-01

Trace analysis of chlorophenols in water was performed by simultaneous silylation and dispersive liquid-liquid microextraction followed by gas chromatography with mass spectrometry. Dispersive liquid-liquid microextraction was carried out using an organic solvent lighter than water (n-hexane). The effect of different silylating reagents on the method efficiency was investigated. The influence of derivatization reagent volume, presence of catalyst and derivatization/extraction time on the yield of the derivatization reaction was studied. Different parameters affecting extraction efficiency such as kind and volume of extraction and disperser solvents, pH of the sample and addition of salt were also investigated and optimized. Under the optimum conditions, the calibration graphs were linear in the range of 0.05-100 ng/mL and the limit of detection was 0.01 ng/mL. The enrichment factors were 242, 351, and 363 for 4-chlorophenol, 2,4-dichlorophenol, and 2,4,6-trichlorophenol, respectively. The values of intra- and inter-day relative standard deviations were in the range of 3.0-6.4 and 6.1-9.9%, respectively. The applicability of the method was investigated by analyzing water and wastewater samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Young's Modulus, Fracture Stress, and Fracture Strain of Gellan Hydrogels Filled with Whey Protein Microparticles.

PubMed

Lam, Cherry Wing Yu; Ikeda, Shinya

2017-05-01

Texture modifying abilities of whey protein microparticles are expected to be dependent on pH during heat-induced aggregation of whey protein in the microparticulation process. Therefore, whey protein microparticles were prepared at either pH 5.5 or 6.8 and their effects on small and large deformation properties of gellan gels containing whey protein microparticles as fillers were investigated. The majority of whey protein microparticles had diameters around 2 μm. Atomic force microscopy images showed that whey protein microparticles prepared at pH 6.8 partially collapsed and flatted by air-drying, while those prepared at pH 5.5 did not. The Young's modulus of filled gels adjusted to pH 5.5 decreased by the addition of whey protein microparticles, while those of filled gels adjusted to pH 6.8 increased with increasing volume fraction of filler particles. These results suggest that filler particles were weakly bonded to gel matrices at pH 5.5 but strongly at pH 6.8. Whey protein microparticles prepared at pH 5.5 showed more enhanced increases in the Young's modulus than those prepared at pH 6.8 at volume fractions between 0.2 and 0.4, indicating that microparticles prepared at pH 5.5 were mechanically stronger. The fracture stress of filled gels showed trends somewhat similar to those of the Young's modulus, while their fracture strains decreased by the addition of whey protein microparticles in all examined conditions, indicating that the primary effect of these filler particles was to enhance the brittleness of filled gels. © 2017 Institute of Food Technologists®.

Feasibility of conducting wetfall chemistry investigations around the Bowen Power Plant

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, N.C.J.; Patrinos, A.A.N.

1979-10-01

The feasibility of expanding the Meteorological Effects of Thermal Energy Releases - Oak Ridge National Laboratory (METER-ORNL) research at Bower Power Plant, a coal-fired power plant in northwest Georgia, to include wetfall chemistry is evaluated using results of similar studies around other power plants, several atmospheric washout models, analysis of spatial variability in precipitation, and field logistical considerations. An optimal wetfall chemistry network design is proposed, incorporating the inner portion of the existing rain-gauge network and augmented by additional sites to ensure adequate coverage of probable target areas. The predicted sulfate production rate differs by about four orders of magnitudemore » among the models reviewed with a pH of 3. No model can claim superiority over any other model without substantive data verification. The spatial uniformity in rain amount is evaluated using four storms that occurred at the METER-ORNL network. Values of spatial variability ranged from 8 to 31% and decreased as the mean rainfall increased. The field study of wetfall chemistry will require a minimum of 5 persons to operate the approximately 50 collectors covering an area of 740 km/sup 2/. Preliminary wetfall-only samples collected on an event basis showed lower pH and higher electrical conductivity of precipitation collected about 5 km downwind of the power plant relative to samples collected upwind. Wetfall samples collected on a weekly basis using automatic samplers, however, showed variable results, with no consistent pattern. This suggests the need for event sampling to minimize variable rain volume and multiple-source effects often associated with weekly samples.« less

Dispersive liquid-liquid microextraction based on solidification of floating organic droplet followed by high-performance liquid chromatography with ultraviolet detection and liquid chromatography-tandem mass spectrometry for the determination of triclosan and 2,4-dichlorophenol in water samples.

PubMed

Zheng, Cao; Zhao, Jing; Bao, Peng; Gao, Jin; He, Jin

2011-06-24

A novel, simple and efficient dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) technique coupled with high-performance liquid chromatography with ultraviolet detection (HPLC-UV) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of triclosan and its degradation product 2,4-dichlorophenol in real water samples. The extraction solvent used in this work is of low density, low volatility, low toxicity and proper melting point around room temperature. The extractant droplets can be collected easily by solidifying it at a lower temperature. Parameters that affect the extraction efficiency, including type and volume of extraction solvent and dispersive solvent, salt effect, pH and extraction time, were investigated and optimized in a 5 mL sample system by HPLC-UV. Under the optimum conditions (extraction solvent: 12 μL of 1-dodecanol; dispersive solvent: 300 of μL acetonitrile; sample pH: 6.0; extraction time: 1 min), the limits of detection (LODs) of the pretreatment method combined with LC-MS/MS were in the range of 0.002-0.02 μg L(-1) which are lower than or comparable with other reported approaches applied to the determination of the same compounds. Wide linearities, good precisions and satisfactory relative recoveries were also obtained. The proposed technique was successfully applied to determine triclosan and 2,4-dichlorophenol in real water samples. Copyright © 2011 Elsevier B.V. All rights reserved.

A microfluidic chip with a staircase pH gradient generator, a packed column and a fraction collector for chromatofocusing of proteins.

PubMed

Rho, Hoon Suk; Hanke, Alexander Thomas; Ottens, Marcel; Gardeniers, Han J G E

2018-04-01

A microfluidic device for pH gradient chromatofocusing is presented, which performs creation of a micro-column, pH gradient generation, and fraction collection in a single device. Using a sieve micro-valve, anion exchange particles were packed into a microchannel in order to realize a solid-phase absorption column. To fractionate proteins according to their isoelectric points, elution buffer solutions with a stepwise pH gradient were prepared in 16 parallel mixing reactors and flowed through the micro-column, wherein a protein mixture was previously loaded. The volume of the column is only 20 nL, hence it allows extremely low sample consumption and fast analysis compared with a conventional system. We demonstrated separation of two proteins, albumin-fluorescein isothiocyanate conjugate (FITC-BSA) and R-Phycoerythrin (R-PE), by using a microcolumn of commercial charged polymeric particles (Source 15Q). The microfluidic device can be used as a rapid diagnostic tool to analyse crude mixtures of proteins or nucleic acids and determine adsorption/desorption characteristics of various biochemical products, which can be helpful for scientific fundamental understanding as well as instrumental in various industrial applications, especially in early stage screening and process development. © 2018 The Authors Electrophoresis Published by WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The suppression of enhanced bitterness intensity of macrolide dry syrup mixed with an acidic powder.

PubMed

Ishizaka, Toshihiko; Okada, Sachie; Takemoto, Eri; Tokuyama, Emi; Tsuji, Eriko; Mukai, Junji; Uchida, Takahiro

2007-10-01

The aim of the present study was to identify a medicine which strongly enhanced the bitterness of clarithromycin dry syrup (CAMD) when administered concomitantly and to develop a method to suppress this enhanced bitterness. The bitterness enhancement was evaluated not only by gustatory sensation tests but also using pH and taste sensor measurements of the mixed sample. A remarkable bitterness enhancement was found when CAMD was mixed with the acidic powder L-carbocysteine. The acidic pH (pH 3.40) of the suspension made from these two preparations, seemed to be due to enhanced release of clarithromycin caused by the dissolution of the alkaline polymer film-coating. Several methods for preventing this bitterness enhancement were investigated. Neither increasing the volume of water taken with the mixture, nor changing the ratio of CAMD:L-carbocysteine in the mixture, were effective in reducing the bitterness intensity of the CAMD/L-carbocysteine mixture. The best way to achieve taste masking was to first administer CAMD mixed with chocolate jelly, which has a neutral pH, followed by the L-carbocysteine suspension. Similar results were obtained for the bitterness suppression of azithromycin fine granules with L-carbocysteine. The chocolate jelly will be useful for taste masking of bitter macrolide drug formulations, when they need to be administered together with acidic drug formulations.

The Impact of Alkaliphilic Biofilm Formation on the Release and Retention of Carbon Isotopes from Nuclear Reactor Graphite.

PubMed

Rout, S P; Payne, L; Walker, S; Scott, T; Heard, P; Eccles, H; Bond, G; Shah, P; Bills, P; Jackson, B R; Boxall, S A; Laws, A P; Charles, C; Williams, S J; Humphreys, P N

2018-03-13

14 C is an important consideration within safety assessments for proposed geological disposal facilities for radioactive wastes, since it is capable of re-entering the biosphere through the generation of 14 C bearing gases. The irradiation of graphite moderators in the UK gas-cooled nuclear power stations has led to the generation of a significant volume of 14 C-containing intermediate level wastes. Some of this 14 C is present as a carbonaceous deposit on channel wall surfaces. Within this study, the potential of biofilm growth upon irradiated and 13 C doped graphite at alkaline pH was investigated. Complex biofilms were established on both active and simulant samples. High throughput sequencing showed the biofilms to be dominated by Alcaligenes sp at pH 9.5 and Dietzia sp at pH 11.0. Surface characterisation revealed that the biofilms were limited to growth upon the graphite surface with no penetration of the deeper porosity. Biofilm formation resulted in the generation of a low porosity surface layer without the removal or modification of the surface deposits or the release of the associated 14 C/ 13 C. Our results indicated that biofilm formation upon irradiated graphite is likely to occur at the pH values studied, without any additional release of the associated 14 C.

Phenol removal onto novel activated carbons made from lignocellulosic precursors: influence of surface properties.

PubMed

Nabais, J M Valente; Gomes, J A; Suhas; Carrott, P J M; Laginhas, C; Roman, S

2009-08-15

The adsorption of phenol from dilute aqueous solutions onto new activated carbons (AC) was studied. The novel activated carbon was produced from lignocellulosic (LC) precursors of rapeseed and kenaf. Samples oxidised with nitric acid in liquid phase were also studied. The results have shown the significant potential of rapeseed and kenaf for the activated carbon production. The activated carbons produced by carbon dioxide activation were mainly microporous with BET apparent surface area up to 1350 m(2)g(-1) and pore volume 0.5 cm(3)g(-1). The effects of concentration (0.1-2 mM) and pH (3-13) were studied. The phenol adsorption isotherms at 25 degrees C followed the Freundlich model with maximum adsorption capacities of approximately 80 and 50 mg g(-1) for the pristine and oxidised activated carbons, respectively. The influence of pH on the adsorption has two trends for pH below and above 10. It was possible to conclude that when phenol is predominantly in the molecular form the most probable mechanism is based on the pi-pi dispersion interaction between the phenol aromatic ring and the delocalised pi electrons present in the activated carbon aromatic structure. When phenolate is the major component the electrostatic repulsion that occurs at high pH values is the most important aspect of the adsorption mechanism.

Removal of sulfa drugs by sewage treatment in aqueous solution systems: activated carbon treatment and ozone oxidation.

PubMed

Ogata, Fumihiko; Tominaga, Hisato; Kangawa, Moe; Inoue, Kenji; Kawasaki, Naohito

2012-01-01

This study investigates the activated carbon (AC) treatment and ozone oxidation of the sulfa drugs--sulfamethoxazole (SMX), sulfamonomethoxine (SMM), sulfadimidine (SDD), and sulfadimethoxine (SDM)--in aqueous solution systems. Three AC samples were prepared from Shirasagi (AC1 and AC2) and coal (AC3), and the surface functional groups, solution pH, specific surface areas, pore volumes, and morphologies of the three samples were evaluated. The specific surface areas were in the following order: AC1 (1391 m²/g) > AC2 (1053 m²/g) > AC3 (807 m²/g). The pore volume and mean pore diameter of AC3 were greater than those of AC1 and AC2. The concentration of sulfa drugs adsorbed onto the AC samples reached equilibrium within 150 h. Experimental data of the adsorption rate were fitted to a pseudo-second-order model. The amount of sulfa drugs adsorbed onto the AC samples was in the order of SDM < SMM < SDD < SMX; the mechanism of adsorption of the sulfa drugs onto the AC samples depended on the hydrophobicity of the AC surface. The adsorption isotherm data were fitted to Freundlich and Langmuir models. Ozone was generated from oxygen gas using an A-27 ozone generator, and the complete degradation of the sulfa drugs by ozone treatment at 60 mL/min was achieved within 50 min. Ozone treatment caused the structure of the sulfa drugs to decompose via ozone oxidation.

Solid phase extraction of trace amounts of Ag, Cd, Cu, and Zn in environmental samples using magnetic nanoparticles coated by 3-(trimethoxysilyl)-1-propantiol and modified with 2-amino-5-mercapto-1,3,4-thiadiazole and their determination by ICP-OES.

PubMed

Mashhadizadeh, Mohammad Hossein; Karami, Zahra

2011-06-15

A fast, sensitive, and simple method using magnetic nanoparticles (MNPs) coated by 3-(trimethoxysilyl)-1-propantiol and modified with 2-amino-5-mercapto-1,3,4-thiadiazole, as an adsorbent has been successfully developed for extraction, preconcentration, and determination of trace amounts of Ag, Cd, Cu, and Zn from environmental samples. The prepared nanoparticles were characterized by Fourier transform infrared spectroscopy (FT-IR) and scanning electron microscopy (SEM). These magnetic nanoparticles can be easily dispersed in aqueous samples and retrieved by the application of external magnetic field via a piece of permanent magnet. The main factors affecting the extraction efficiency such as pH value, sample volume, eluent concentration and volume, ultrasonication time, and coexisting ions have been investigated and established. Under the optimal conditions, high concentration factors (194, 190, 170, and 182) were achieved for Ag, Cd, Cu, and Zn with relative standard deviations of 5.31%, 4.03%, 3.62%, and 4.20%, respectively. The limits of detection for Ag, Cd, Cu, and Zn were as low as 0.12, 0.12, 0.13 and 0.11 ng mL(-1). The prepared sorbent was applied for preconcentration of trace amounts of Ag, Cd, Cu, and Zn in the various water samples with satisfactory results. Copyright © 2011 Elsevier B.V. All rights reserved.

Synthesis, characterization and application of ion imprinted polymeric nanobeads for highly selective preconcentration and spectrophotometric determination of Ni2 + ion in water samples

NASA Astrophysics Data System (ADS)

Rajabi, Hamid Reza; Razmpour, Saham

2016-01-01

Here, the researchers report on the synthesis of ion imprinted polymeric (IIP) nanoparticles using a thermal polymerization strategy, and their usage for the separation of Ni2 + ion from water samples. The prepared Ni-IIP was characterized by colorimetry, FT-IR spectroscopy, and scanning electron microscopy. It was found that the particle size of the prepared particle to be 50-70 nm in diameter with the highly selective binding capability for Ni2 + ion, with reasonable adsorption and desorption process. After preconcentration, bound ions can be eluted with an aqueous solution of hydrochloric acid, after their complexation with dimethylglyoxime, these ions can be quantified by UV-Vis absorption spectrophotometry. The effect of various parameters on the extraction efficiency including pH of sample solution, adsorption and leaching times, initial sample volume, concentration and volume of eluent were investigated. In selectivity study, it was found that imprinting causes increased affinity of the prepared IIP toward Ni2 + ion over other ions such as Na+, K+, Ag+, Co2 +, Cu2 +, Cd2 +, Hg2 +, Pb2 +, Zn2 +, Mn2 +, Mg2 +, Cr3 +, and Fe3 +. The prepared IIP can be used and regenerated for at least eight times without any significant decrease in binding affinities. The prepared IIP is considered to be promising and selective sorbent for solid-phase extraction and preconcentration of Ni2 + ion from different water samples.

In-Syringe Micro Solid-Phase Extraction Method for the Separation and Preconcentration of Parabens in Environmental Water Samples.

PubMed

Mashile, Geaneth Pertunia; Mpupa, Anele; Nomngongo, Philiswa Nosizo

2018-06-14

In this study, a simple, rapid and effective in-syringe micro-solid phase extraction (MSPE) method was developed for the separation and preconcetration of parabens (methyl, ethyl, propyl and butyl paraben) in environmental water samples. The parabens were determined and quantified using high performance liquid chromatography and a photo diode array detector (HPLC-PDA). Chitosan-coated activated carbon (CAC) was used as the sorbent in the in-syringe MSPE device. A response surface methodology based on central composite design was used for the optimization of factors (eluent solvent type, eluent volume, number of elution cycles, sample volume, sample pH) affecting the extraction efficiency of the preconcentration procedure. The adsorbent used displayed excellent absorption performance and the adsorption capacity ranged from 227⁻256 mg g −1 . Under the optimal conditions the dynamic linear ranges for the parabens were between 0.04 and 380 µg L −1 . The limits of detection and quantification ranged from 6⁻15 ng L −1 and 20⁻50 ng L −1 , respectively. The intraday (repeatability) and interday (reproducibility) precisions expressed as relative standard deviations (%RSD) were below 5%. Furthermore, the in-syringe MSPE/HPLC procedure was validated using spiked wastewater and tap water samples and the recoveries ranged between from 96.7 to 107%. In conclusion, CAC based in-syringe MSPE method demonstrated great potential for preconcentration of parabens in complex environmental water.

Application of 1-(2-pyridylazo)-2-naphthol-modified nanoporous silica as a technique in simultaneous trace monitoring and removal of toxic heavy metals in food and water samples.

PubMed

Abolhasani, Jafar; Behbahani, Mohammad

2015-01-01

Solid-phase extraction is one the most useful and efficient techniques for sample preparation, purification, cleanup, preconcentration, and determination of heavy metals at trace levels. In this paper, functionalized MCM-48 nanoporous silica with 1-(2-pyridylazo)-2-naphthol was applied for trace determination of copper, lead, cadmium, and nickel in water and seafood samples. The experimental conditions such as pH, sample and eluent flow rate, type, concentration and volume of the eluent, breakthrough volume, and effect of coexisting ions were optimized for efficient solid-phase extraction of trace heavy metals in different water and seafood samples. The content of solutions containing the mentioned heavy metals was determined by flame atomic absorption spectrometry (FAAS), and the limits of detection were 0.3, 0.4, 0.6, and 0.9 ng mL(-1) for cadmium, copper, nickel, and lead, respectively. Recoveries and precisions were >98.0 and <4%, respectively. The adsorption capacity of the modified nanoporous silica was 178 mg g(-1) for cadmium, 110 mg g(-1) for copper, 98 mg g(-1) for nickel, and 210 mg g(-1) for lead, respectively. The functionalized MCM-48 nanoporous silica with 1-(2-pyridylazo)-2-naphthol was characterized by thermogravimetry analysis (TGA), differential thermal analysis (DTA), transmission electron microscopy (TEM), Fourier transform infrared spectrometry (FT-IR), X-ray diffraction (XRD), elemental analysis (CHN), and N2 adsorption surface area measurement.

Chemically modified activated carbon with 1-acylthiosemicarbazide for selective solid-phase extraction and preconcentration of trace Cu(II), Hg(II) and Pb(II) from water samples.

PubMed

Gao, Ru; Hu, Zheng; Chang, Xijun; He, Qun; Zhang, Lijun; Tu, Zhifeng; Shi, Jianping

2009-12-15

A new sorbent 1-acylthiosemicarbazide-modified activated carbon (AC-ATSC) was prepared as a solid-phase extractant and applied for removing of trace Cu(II), Hg(II) and Pb(II) prior to their determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The separation/preconcentration conditions of analytes were investigated, including effects of pH, the shaking time, the sample flow rate and volume, the elution condition and the interfering ions. At pH 3, the maximum static adsorption capacity of Cu(II), Hg(II) and Pb(II) onto the AC-ATSC were 78.20, 67.80 and 48.56 mg g(-1), respectively. The adsorbed metal ions were quantitatively eluted by 3.0 mL of 2% CS(NH2)2 and 2.0 mol L(-1) HCl solution. Common coexisting ions did not interfere with the separation. According to the definition of IUPAC, the detection limits (3sigma) of this method for Cu(II), Hg(II) and Pb(II) were 0.20, 0.12 and 0.45 ng mL(-1), respectively. The relative standard deviation under optimum conditions is less than 4.0% (n=8). The prepared sorbent was applied for the preconcentration of trace Cu(II), Hg(II) and Pb(II) in certified and water samples with satisfactory results.

Simultaneous extraction and HPLC determination of 3-indole butyric acid and 3-indole acetic acid in pea plant by using ionic liquid-modified silica as sorbent.

PubMed

Sheikhian, Leila; Bina, Sedigheh

2016-01-15

In this study, ionic liquid-modified silica was used as sorbent for simultaneous extraction and preconcentration of 3-indole butyric acid and 3-indole acetic acid in pea plants. The effect of some parameters such as pH and ionic strength of sample solution, amount of sorbent, flow rate of aqueous sample solution and eluent solution, concentration of eluent solution, and temperature were studied for each hormone solution. Percent extraction of 3-indole butyric acid and 3-indole acetic acid was strongly affected by pH of aqueous sample solution. Ionic strength of aqueous phase and temperature showed no serious effects on extraction efficiency of studied plant hormones. Obtained breakthrough volume was 200mL for each of studied hormones. Preconcentration factor for spectroscopic and chromatographic determination of studied hormones was 100 and 4.0×10(3) respectively. Each solid sorbent phase was reusable for almost 10 times of extraction/stripping procedure. Relative standard deviations of extraction/stripping processes of 3-indole butyric acid and 3-indole acetic acid were 2.79% and 3.66% respectively. The calculated limit of detections for IBA and IAA were 9.1×10(-2)mgL(-1) and 1.6×10(-1)mgL(-1) respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

AFM study of adsorption of protein A on a poly(dimethylsiloxane) surface

NASA Astrophysics Data System (ADS)

Yu, Ling; Lu, Zhisong; Gan, Ye; Liu, Yingshuai; Li, Chang Ming

2009-07-01

In this paper, the morphology and kinetics of adsorption of protein A on a PDMS surface is studied by AFM. The results of effects of pH, protein concentration and contact time of the adsorption reveal that the morphology of adsorbed protein A is significantly affected by pH and adsorbed surface concentration, in which the pH away from the isoelectric point (IEP) of protein A could produce electrical repulsion to change the protein conformation, while the high adsorbed surface protein volume results in molecular networks. Protein A can form an adsorbed protein film on PDMS with a maximum volume of 2.45 × 10-3 µm3. This work enhances our fundamental understanding of protein A adsorption on PDMS, a frequently used substrate component in miniaturized immunoassay devices.

Large volume preconcentration and determination of nanomolar concentrations of iron in seawater using a renewable cellulose 8-hydroquinoline sorbent microcolumn and universal approach of post-column eluate utilization in a Lab-on-Valve system.

PubMed

Horstkotte, Burkhard; Chocholouš, Petr; Solich, Petr

2016-04-01

We report on a Lab-On-Valve (LOV) configuration for analyte preconcentration from milliliter sample volumes using confluent mixing in the holding coil for in-line addition of loading buffer. The system was applied to the spectrophotometric determination of iron(II) in acidified seawater using 1,10-phenanthroline as color reagent. A cellulose-based chelating sorbent containing 8-hydroxyquinoline was used for the first time in LOV and excellent retention behavior and loading capacity were found. The flow system employs a syringe pump for handling all solutions (sorbent suspension, loading buffer, water, eluent, and color reagent) and a peristaltic pump for sample propulsion and includes a fit-for-purpose 14 cm long detection glass flow cell and a bubble trap for in-line carrier degasification. Advantage was taken of the LOV flow-through port to keep the eluted analytes for re-aspiration for subsequent chromogenic reaction. In effect, a universal analyzer configuration and preconcentration procedure was developed, which is combinable with other analytes, sorbents, and reagents. Among the studied parameters were the compositions, pH, volumes, and flow rates of loading buffer, eluent, and color reagent, as well as the microcolumn size, repeatability, and system stability. Reproducibility of 4.1% RSD over the entire working range, a LOD of down to 5 nmol L(-1), sampling frequency of 12h(-1), and linearity up to 1 µmol L(-1) for 3.3 mL of sample were obtained and applicability to real samples was demonstrated. It was proven that both Fe(III) and Fe(II) were retained and yielded similar recovery and sensitivity values. The method was applied to coastal seawater samples and spiking experiments yielded recovery values close to 100%. Copyright © 2015 Elsevier B.V. All rights reserved.

Differences in composition of honey samples and their impact on the antimicrobial activities against drug multiresistant bacteria and pathogenic fungi.

PubMed

AL-Waili, Noori; Al Ghamdi, Ahmad; Ansari, Mohammad Javed; Al-Attal, Yehya; Al-Mubarak, Aarif; Salom, Khelod

2013-05-01

Antibiotic multiresistant microbes represent a challenging problem. Because honey has a potent antibacterial property, the antimicrobial effects of different honey samples against multiresistant pathogens and their compositions were investigated. Five honey samples were used: Talah, Dhahian, Sumra-1, Sidr, and Sumra-2. Samples were analyzed to determine chemical composition such as fructose, glucose, sucrose, pH, total flavonoids, total phenolics, hydrogen peroxide concentration, minerals and trace elements. Antimicrobial activities of the samples against 17 (16 were multiresistant) human pathogenic bacteria and three types of fungi were studied. Specimens of the isolates were cultured into 10 mL of 10-100% (volume/volume) honey diluted in broth. Microbial growth was assessed on a solid plate media after 24 h and 72 h incubation. The composition of honey samples varied considerably. Sumra 1 and 2 contained the highest level of flavonoids and phenolics and the lowest level of hydrogen peroxide, whereas Dhahian honey contained the highest level of hydrogen peroxide. Sixteen pathogens were antibiotic multiresistant. A single dose of each honey sample inhibited all the pathogens tested after 24 h and 72 h incubation. The most sensitive pathogens were Aspergillus nidulans, Salmonella typhimurum and Staphylococcus epidermidis (S. epidermidis). Although there was no statistically significant difference in the effectiveness of honey samples, the most effective honey against bacteria was Talah and against fungi were Dhahian and Sumra-2. Various honey samples collected from different geographical areas and plant origins showed almost similar antimicrobial activities against multiresistant pathogens despite considerable variation in their composition. Honey may represent an alternative candidate to be tested as part of management of drug multiresistant pathogens. Copyright © 2013 IMSS. Published by Elsevier Inc. All rights reserved.

Improved Segmented-Flow Tracer-Monitored Titration for Automated Measurement of Total Alkalinity in Seawater

NASA Astrophysics Data System (ADS)

Spaulding, R. S.; Hales, B.; Beck, J. C.; Degrandpre, M. D.

2008-12-01

The four measurable inorganic carbon parameters commonly measured as part of oceanic carbon cycle studies are total dissolved inorganic carbon (DIC), total alkalinity (AT), hydrogen ion concentration (pH) and partial pressure of CO2 (pCO2). AT determination is critical for anthropogenic CO2 inventory calculations and for quantifying CaCO3 saturation. Additionally, measurement of AT in combination with one other carbonate parameter can be used to describe the inorganic carbon equilibria. Current methods for measuring AT require calibrated volumetric flasks and burettes, gravimetry, or precise flow measurements. These methods also require analysis times of ˜15 min and sample volumes of ˜200 mL, and sample introduction is not automated, resulting in labor-intensive measurements and low temporal resolution. The Tracer Monitored Titration (TMT) system was previously developed at the University of Montana for AT measurements. The TMT is not dependent on accurate gravimetric, volumetric or flow rate measurements because it relies on a pH-sensitive indicator (tracer) to track the amount of titrant added to the sample. Sample and a titrant-indicator mixture are mechanically stirred in an optical flow cell and pH is calculated using the indicator equilibrium constant and the spectrophotometrically determined concentrations of the acid and base forms of the indicator. AT is then determined using these data in a non-linear least squares regression of the AT mass and proton balances. The precision and accuracy of the TMT are 2 and 4 micromol per kg in 16 min using 110-mL of sample. The TMT is dependent on complete mixing of titrant with the sample and accurate absorbance measurements. We have developed the segmented-flow TMT (SF- TMT) to improve on these aspects and decrease sample analysis time. The TMT uses segmented flow instead of active mixing and a white LED instead of a tungsten-halogen light source. Air is added to the liquid flow stream, producing segments of liquid separated by air bubbles. Because liquid is not transferred between flow segments, there is rapid flushing which reduces sample volume to <10 mL. Additionally, the slower movement of liquid at the tube walls compared to that at the tube center creates circulation within each liquid segment, mixing the sample and eliminating the need for mechanical stirring. The white LED has higher output at the wavelengths of interest, thus improving the precision of absorbance measurements. These improvements result in a faster, simpler method for measuring AT.

Methodological implications in pH standardization of exhaled breath condensate.

PubMed

Hoffmeyer, F; Berresheim, H; Beine, A; Sucker, K; Brüning, T; Bünger, J

2015-05-14

The variable amount of dissolved carbon dioxide is one of the main confounding factors of exhaled breath condensate (EBC) pH measurements. There have been many attempts at identifying the optimal approach to displace CO2 as a way to gain reproducible and valid pH values in EBC samples. The aim of the present study was to assess the correlation of pH and pCO2 in untreated, neat EBC samples and, after deaeration, to reevaluate the standardization of CO2 as a means to obtain valid pH values. A further aim was to evaluate the impact of deaeration on the acid-base balance in EBC samples. EBC was collected from seven female and 31 male subjects. The pH and pCO2 values immediately determined in untreated, neat EBC samples were strongly correlated (rp = -0.723, p <  0.0001). This correlation was not observed after deaeration with argon (rs = 0.264, p = 0.109). Based on a regression function for the pH/pCO2 relationship, the calculated pH at a pCO2 of 5.33 kPa was 6.07 (IQR 5.99, 6.20). No significant difference was observed between the pH measured in neat EBC samples and those calculated after deaeration with regression function and measured neat pCO2. Our data suggest that pCO2 is the most important confounder of pH measurement in EBC samples and, when adjusting for pCO2, the acid-base balance of EBC samples is not significantly influenced by the process of deaeration. Furthermore, measurement with a blood-gas analyzer and standardization of pH for pCO2 allows sensitive assaying of EBC samples. Therefore, this method provides a basis for detection of even small changes in airway pH due to inhalative exposure or respiratory disease.

Measurement of trace levels of antibiotics in river water using on-line enrichment and triple-quadrupole LC-MS/MS.

PubMed

Dinh, Quoc Tuc; Alliot, Fabrice; Moreau-Guigon, Elodie; Eurin, Joëlle; Chevreuil, Marc; Labadie, Pierre

2011-09-15

This study presents the development of an automated on-line solid phase extraction (SPE)-liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of 23 antibiotics in environmental water samples. After optimisation of LC-MS/MS conditions, SPE parameters such as sorbent type, sample pH or sample volume were optimised. Antibiotic recoveries ranged from 64% to 98% and compared favourably with those achieved using off-line SPE. Limits of detection were in the range 0.5-13.7 ng L(-1). This on-line SPE-LC-MS/MS procedure was applied to the analysis of water samples taken in three rivers within the Seine River basin, near Paris (France). The obtained results revealed the occurrence of 12 antibiotics, including tylosin, erythromycin, tetracycline, amoxicillin, trimethoprim, sulfamethoxazole, oxolinic acid, flumequine, norfloxacin, ciprofloxacin, ofloxacin, and vancomycin (2-1435 ng L(-1)). Copyright © 2011 Elsevier B.V. All rights reserved.

Solid-phase extraction of iridium from soil and water samples by using activated carbon cloth prior to its spectrophotometric determination.

PubMed

Ozkantar, Nebiye; Yilmaz, Erkan; Soylak, Mustafa; Tuzen, Mustafa

2015-08-01

A solid-phase extraction method for separation and preconcentration of Ir(IV) ion by using activated carbon cloth (ACC) has been presented. Ir(IV) as their 1-(2-pyridylazo) 2-naphtol (PAN) chelate was adsorbed on ACC at pH 2.0 and was eluted from ACC with acidic dimethylformamide (DMF). The Ir(IV) concentration was determined at 536 nm as Ir(IV)-PAN complex by using UV-vis spectrophotometer. The analytical parameters including pH, sample and eluent flow rates, amount of PAN, eluent type, concentration, and sample volume were optimized. The effects of foreign ions on the recoveries of iridium were also investigated. The preconcentration factor was calculated as 60. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were found as 0.039 and 0.129 μg L(-1), respectively. The method was applied to soil and water samples for iridium determination.

Value of Impedance Cardiography during 6‐Minute Walk Test in Pulmonary Hypertension

PubMed Central

Alkukhun, Laith; Arelli, Vineesha; Ramos, José; Newman, Jennie; McCarthy, Kevin; Pichurko, Bohdan; Minai, Omar A.; Dweik, Raed A.

2013-01-01

Abstract Background Methods that predict prognosis and response to therapy in pulmonary hypertension (PH) are lacking. We tested whether the noninvasive estimation of hemodynamic parameters during 6‐minute walk test (6MWT) in PH patients provides information that can improve the value of the test. Methods We estimated hemodynamic parameters during the 6MWT using a portable, signal‐morphology‐based, impedance cardiograph (PhysioFlow Enduro) with real‐time wireless monitoring via a bluetooth USB adapter. Results We recruited 48 subjects in the study (30 with PH and 18 healthy controls). PH patients had significantly lower maximum stroke volume (SV) and CI and slower cardiac output (CO) acceleration and decelerations slopes during the test when compared with healthy controls. In PH patients, CI change was associated with total distance walked (R = 0.62; P < 0.001) and percentage of predicted (R = 0.4, P = 0.03), HR recovery at 1 minute (0.57, P < 0.001), 2 minutes (0.65, P < 0.001), and 3 minutes (0.66, P < 0.001). Interestingly, in PH patients CO change during the test was predominantly related to an increase in SV instead of HR. Conclusions Estimation of hemodynamic parameters such as cardiac index during 6‐minute walk test is feasible and may provide useful information in patients with PH. Clin Trans Sci 2013; Volume #: 1–7 PMID:24330692

Effect of Exposed Surface Area, Volume and Environmental pH on the Calcium Ion Release of Three Commercially Available Tricalcium Silicate Based Dental Cements.

PubMed

Rajasekharan, Sivaprakash; Vercruysse, Chris; Martens, Luc; Verbeeck, Ronald

2018-01-13

Tricalcium silicate cements (TSC) are used in dental traumatology and endodontics for their bioactivity which is mostly attributed to formation of calcium hydroxide during TSC hydration and its subsequent release of calcium and hydroxide ions. The aim of this study was to determine the effect of volume (Vol), exposed surface area (ESA) and pH of surrounding medium on calcium ion release. Three commercially available hydraulic alkaline dental cements were mixed and condensed into cylindrical tubes of varying length and diameter ( n = 6/group). For the effect of ESA and Vol, tubes were immersed in 10 mL of deionized water. To analyze the effect of environmental pH, the tubes were randomly immersed in 10 mL of buffer solutions with varying pH (10.4, 7.4 or 4.4). The solutions were collected and renewed at various time intervals. pH and/or calcium ion release was measured using a pH glass electrode and atomic absorption spectrophotometer respectively. The change of pH, short-term calcium ion release and rate at which calcium ion release reaches maximum were dependent on ESA ( p < 0.05) while maximum calcium ion release was dependent on Vol of TSC ( p < 0.05). Maximum calcium ion release was significantly higher in acidic solution followed by neutral and alkaline solution ( p < 0.05).

Effect of Exposed Surface Area, Volume and Environmental pH on the Calcium Ion Release of Three Commercially Available Tricalcium Silicate Based Dental Cements

PubMed Central

Rajasekharan, Sivaprakash; Vercruysse, Chris; Martens, Luc; Verbeeck, Ronald

2018-01-01

Tricalcium silicate cements (TSC) are used in dental traumatology and endodontics for their bioactivity which is mostly attributed to formation of calcium hydroxide during TSC hydration and its subsequent release of calcium and hydroxide ions. The aim of this study was to determine the effect of volume (Vol), exposed surface area (ESA) and pH of surrounding medium on calcium ion release. Three commercially available hydraulic alkaline dental cements were mixed and condensed into cylindrical tubes of varying length and diameter (n = 6/group). For the effect of ESA and Vol, tubes were immersed in 10 mL of deionized water. To analyze the effect of environmental pH, the tubes were randomly immersed in 10 mL of buffer solutions with varying pH (10.4, 7.4 or 4.4). The solutions were collected and renewed at various time intervals. pH and/or calcium ion release was measured using a pH glass electrode and atomic absorption spectrophotometer respectively. The change of pH, short-term calcium ion release and rate at which calcium ion release reaches maximum were dependent on ESA (p < 0.05) while maximum calcium ion release was dependent on Vol of TSC (p < 0.05). Maximum calcium ion release was significantly higher in acidic solution followed by neutral and alkaline solution (p < 0.05). PMID:29342837

Uneven biofilm and current distribution in three-dimensional macroporous anodes of bio-electrochemical systems composed of graphite electrode arrays.

PubMed

Li, Jun; Hu, Linbin; Zhang, Liang; Ye, Ding-Ding; Zhu, Xun; Liao, Qiang

2017-03-01

A 3-D macroporous anode was constructed using different numbers of graphite rod arrays in fixed-volume bio-electrochemical systems (BESs), and the current and biofilm distribution were investigated by dividing the 3-D anode into several subunits. In the fixed-volume chamber, current production was not significantly improved after the electrode number increased to 36. In the case of 100 electrodes, a significant uneven current distribution was found in the macroporous anode. This was attributed to a differential pH distribution, which resulted from proton accumulation inside the macroporous anode. The pH distribution influenced the biofilm development and led to an uneven biofilm distribution. With respect to current generation, the uneven distribution of both the pH and biofilm contributed to the uneven current distribution. The center had a low pH, which led to less biofilm and a lower contribution to the total current, limiting the performance of the BESs. Copyright © 2016 Elsevier Ltd. All rights reserved.

Physicochemical characteristics of Fe3O4 magnetic nanocomposites based on Poly(N-isopropylacrylamide) for anti-cancer drug delivery.

PubMed

Davaran, Soodabeh; Alimirzalu, Samira; Nejati-Koshki, Kazem; Nasrabadi, Hamid Tayef; Akbarzadeh, Abolfazl; Khandaghi, Amir Ahmad; Abbasian, Mojtaba; Alimohammadi, Somayeh

2014-01-01

Hydrogels are a class of polymers that can absorb water or biological fluids and swell to several times their dry volume, dependent on changes in the external environment. In recent years, hydrogels and hydrogel nanocomposites have found a variety of biomedical applications, including drug delivery and cancer treatment. The incorporation of nanoparticulates into a hydrogel matrix can result in unique material characteristics such as enhanced mechanical properties, swelling response, and capability of remote controlled actuation. In this work, synthesis of hydrogel nanocomposites containing magnetic nanoparticles are studied. At first, magnetic nanoparticles (Fe3O4) with an average size 10 nm were prepared. At second approach, thermo and pH-sensitive poly (N-isopropylacrylamide -co-methacrylic acid-co-vinyl pyrrolidone) (NIPAAm-MAA- VP) were prepared. Swelling behavior of co-polymer was studied in buffer solutions with different pH values (pH=5.8, pH=7.4) at 37 °C. Magnetic iron oxide nanoparticles (Fe3O4) and doxorubicin were incorporated into copolymer and drug loading was studied. The release of drug, carried out at different pH and temperatures. Finally, chemical composition, magnetic properties and morphology of doxorubicin-loaded magnetic hydrogel nanocomposites were analyzed by FT- IR, vibrating sample magnetometry (VSM), scanning electron microscopy (SEM). The results indicated that drug loading efficiency was increased by increasing the drug ratio to polymer. Doxorubicin was released more at 40 °C and in acidic pH compared to that 37 °C and basic pH. This study suggested that the poly (NIPAAm-MAA-VP) magnetic hydrogel nanocomposite could be an effective carrier for targeting drug delivery systems of anti-cancer drugs due to its temperature sensitive properties.

Left atrium function by 2D speckle tracking in aortic valve disease.

PubMed

Salas-Pacheco, Jose L; Ávila-Vanzzini, Nydia; Eugenia, Ruiz-Esparza M; Arias-Godínez, Jose A

2016-12-01

A paucity of data exists about left atrium (LA) function in aortic valve stenosis (AS) or regurgitation (AR). Two-dimensional speckle tracking echocardiography allows the noninvasive study of LA functional disturbances in aortic valve disease and their impact in the development of pulmonary hypertension (PH). Consecutive patients with moderate or severe AS or AR were included. Left ventricle (LV) and LA speckle tracking strain quantification was performed. We included 42 patients with AS and 30 with AR. Differences were not found in LA volumes and strain in AS or AR. The LA volumetric derangements parallel the decrease in LA longitudinal strain. Maximum LA volume, minimum LA volume, and indexed LA volume were higher in severe valvular disease (SVD) than in moderate [23 cc (P=.018, IC 95% : 4-41), 16 cc (P=.035, IC 95% : 2-31), and 14 cc (P=.022, IC 95% : 2-25), respectively], occurred in the same way with LA strain in the conduit (6.3%, P=.034, IC 95% : 1-12) and reservoir (7.1%, P=.04, IC 95% : 2-14) phases. In multivariable model, strain of reservoir phase was the variable mainly associated with PH; each decrease in one unit of strain of reservoir phase increased 6% the PH probability (OR: 1.06, P=.01). This study demonstrates that in patients with AS and AR, the LA has a similar behavior and that exist a close correlation between LA volumetric and functional parameters. The variable mainly associated with PH was LA strain of reservoir phase. © 2016, Wiley Periodicals, Inc.

Miniaturized and direct spectrophotometric multi-sample analysis of trace metals in natural waters.

PubMed

Albendín, Gemma; López-López, José A; Pinto, Juan J

2016-03-15

Trends in the analysis of trace metals in natural waters are mainly based on the development of sample treatment methods to isolate and pre-concentrate the metal from the matrix in a simpler extract for further instrumental analysis. However, direct analysis is often possible using more accessible techniques such as spectrophotometry. In this case a proper ligand is required to form a complex that absorbs radiation in the ultraviolet-visible (UV-Vis) spectrum. In this sense, the hydrazone derivative, di-2-pyridylketone benzoylhydrazone (dPKBH), forms complexes with copper (Cu) and vanadium (V) that absorb light at 370 and 395 nm, respectively. Although spectrophotometric methods are considered as time- and reagent-consuming, this work focused on its miniaturization by reducing the volume of sample as well as time and cost of analysis. In both methods, a micro-amount of sample is placed into a microplate reader with a capacity for 96 samples, which can be analyzed in times ranging from 5 to 10 min. The proposed methods have been optimized using a Box-Behnken design of experiments. For Cu determination, concentration of phosphate buffer solution at pH 8.33, masking agents (ammonium fluoride and sodium citrate), and dPKBH were optimized. For V analysis, sample (pH 4.5) was obtained using acetic acid/sodium acetate buffer, and masking agents were ammonium fluoride and 1,2-cyclohexanediaminetetraacetic acid. Under optimal conditions, both methods were applied to the analysis of certified reference materials TMDA-62 (lake water), LGC-6016 (estuarine water), and LGC-6019 (river water). In all cases, results proved the accuracy of the method. Copyright © 2015 Elsevier Inc. All rights reserved.

Measurements of fog composition at a rural site

NASA Astrophysics Data System (ADS)

Straub, Derek J.; Hutchings, James W.; Herckes, Pierre

2012-02-01

Studies that focus on fog chemistry in the United States have been limited to relatively few locations. Apart from measurements along the East and West coasts and extensive analysis of radiation fog in the Central Valley of California, fog composition has been characterized in only a handful of other locations. To complement and expand the existing fog chemistry data that are currently available, a new field campaign was established at a rural location in Central Pennsylvania to produce a unique, long term record of fog composition. From 2007 to 2010, 41 fog events were sampled with an automated Caltech Heated Rod Cloudwater Collector (CHRCC). The collected samples were analyzed primarily for pH and major inorganic ions. Dissolved organic carbon (DOC) and trace metals were analyzed in selected samples and N-nitrosodimethylamine (NDMA) was quantified in two samples. Sample composition varied widely during the study period. Sulfate concentrations ranged from 15 to 955 (median = 123) μN and pH varied between 3.08 and 7.41 (median = 5.77). In terms of volume weighted averages, ammonium was the most abundant ionic species followed by sulfate, calcium, and nitrate. For the subset of samples in which DOC was analyzed, concentrations ranged from 2.2 to 22.6 mgC l -1. Comparisons with regional precipitation chemistry measurements reveal the influence of local agricultural and soil sources on fog composition. The sum of sulfate, nitrate, and ammonium measured in the present study is considerably lower than the majority of radiation, precipitation, and coastal fogs collected in the United States although the ammonium/(nitrate + sulfate) ratio is similar to those found in the Central Valley of California.

Stability of extemporaneously prepared glycopyrrolate oral suspensions.

PubMed

Cober, Mary Petrea; Johnson, Cary E; Sudekum, David; Penprase, Kimberly

2011-05-01

The stability of extemporaneously prepared glycopyrrolate 0.5-mg/mL suspensions was evaluated. An oral suspension of glycopyrrolate 0.5 mg/mL was prepared by thoroughly grinding 30 1-mg tablets of glycopyrrolate in a glass mortar. Thirty milliliters of Ora-Plus and 30 mL of either Ora-Sweet or Ora-Sweet SF were mixed and added to the powder to make a final volume of 60 mL. Three identical samples of the formulation were prepared and placed in 2-oz amber plastic bottles with child-resistant caps and stored at room temperature (23-25 °C). A 1-mL sample was withdrawn from each of the three bottles with a micropipette immediately after preparation and 7, 15, 30, 60, and 90 days afterward. After further dilution to an expected concentration of 50 μg/mL with sample diluent, the samples were assayed in duplicate by stability-indicating high-performance liquid chromatography. The samples were visually examined for any color change and evaluated for pH on each day of analysis. Taste evaluations were performed at the beginning and end of the study. Stability was defined as the retention of at least 90% of the initial concentration. At least 95% of the initial glycopyrrolate remained throughout the 90-day study period in both preparations. There were no detectable changes in color, odor, taste, and pH, and no visible microbial growth was observed in any sample. Extemporaneously compounded suspensions of glycopyrrolate 0.5 mg/mL in a 1:1 mixture of Ora-Plus/Ora-Sweet or Ora-Plus/Ora-Sweet SF were stable for at least 90 days when stored in amber plastic bottles at room temperature.

Modifying the Cold Gelation Properties of Quinoa Protein Isolate: Influence of Heat-Denaturation pH in the Alkaline Range.

PubMed

Mäkinen, Outi E; Zannini, Emanuele; Arendt, Elke K

2015-09-01

Heat-denaturation of quinoa protein isolate (QPI) at alkali pH and its influence on the physicochemical and cold gelation properties was investigated. Heating QPI at pH 8.5 led to increased surface hydrophobicity and decreases in free and bound sulfhydryl group contents. Heating at pH 10.5 caused a lesser degree of changes in sulfhydryl groups and surface hydrophobicity, and the resulting solutions showed drastically increased solubility. SDS PAGE revealed the presence of large aggregates only in the sample heated at pH 8.5, suggesting that any aggregates present in the sample heated at pH 10.5 were non-covalently bound and disintegrated in the presence of SDS. Reducing conditions partially dissolved the aggregates in the pH 8.5 heated sample indicating the occurrence of disulphide bonding, but caused no major alterations in the separation pattern of the pH 10.5 heated sample. Denaturation pH influenced the cold gelation properties greatly. Solutions heated at pH 8.5 formed a coarse coagulum with maximum G' of 5 Pa. Heat-denaturation at 10.5 enabled the proteins to form a finer and regularly structured gel with a maximum G' of 1140 Pa. Particle size analysis showed that the pH 10.5 heated sample contained a higher level of very small particles (0.1-2 μm), and these readily aggregated into large particles (30-200 μm) when pH was lowered to 5.5. Differences in the nature of aggregates formed during heating may explain the large variation in gelation properties.

Influence of pH on the physical and electromagnetic properties of Mg–Mn ferrite synthesized by a solution combustion method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lwin, Nilar, E-mail: nilarlwin111@gmail.com; School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia, Engineering Campus, 14300 Nibong Tebal, Penang; Othman, Radzali, E-mail: radzali@utem.edu.my

The synthesis of nano-crystalline Mg–Mn ferrites by a solution combustion method using citric acid and ammonia was investigated by varying the pH of the precursor solution, which played an important role in controlling the morphology of the synthesized powders. The phase formation, microstructure and electromagnetic properties were studied using X-ray diffraction, scanning electron microscopy, impedance analyzer and vibrating sample magnetometer. Single phase pure spinel Mg–Mn ferrite powders were obtained for all the samples at different pH (< 1, 3, 5, 7, 9). The results showed that an increase of pH improves the crystallinity of the Mg–Mn ferrite nanoparticles. The averagemore » grain size of sintered samples was found to decrease from 2 μm to 0.5 μm with increasing pH values from pH < 1 to pH 9, respectively. The dielectric constant of the samples with different pH is in the range of 7–12 from frequencies of 1 MHz to 1 GHz. The highest saturation magnetization (30.04 emu/g) was obtained for the sample with pH < 1. - Highlights: • Mg–Mn ferrites were synthesized by a solution combustion method with different pH. • Auto-combustion process resulted in the formation of single phase spinel ferrite. • An increase of pH improves the crystallinity of the Mg–Mn ferrite nanoparticles. • pH variation has influence on phase formation and morphology of the ferrite.« less

Effect of water-column pH on sediment-phosphorus release rates in Upper Klamath Lake, Oregon, 2001

USGS Publications Warehouse

Fisher, Lawrence H.; Wood, Tamara M.

2004-01-01

Sediment-phosphorus release rates as a function of pH were determined in laboratory experiments for sediment and water samples collected from Shoalwater Bay in Upper Klamath Lake, Oregon, in 2001. Aerial release rates for a stable sediment/water interface that is representative of the sediment surface area to water column volume ratio (1:3) observed in the lake and volumetric release rates for resuspended sediment events were determined at three different pH values (8.1, 9.2, 10.2). Ambient water column pH (8.1) was maintained by sparging study columns with atmospheric air. Elevation of the water column pH to 9.2 was achieved through the removal of dissolved carbon dioxide by sparging with carbon dioxide-reduced air, partially simulating water chemistry changes that occur during algal photosynthesis. Further elevation of the pH to 10.2 was achieved by the addition of sodium hydroxide, which doubled average alkalinities in the study columns from about 1 to 2 milliequivalents per liter. Upper Klamath Lake sediments collected from the lake bottom and then placed in contact with lake water, either at a stable sediment/water interface or by resuspension, exhibited an initial capacity to take up soluble reactive phosphorus (SRP) from the water column rather than release phosphorus to the water column. At a higher pH this initial uptake of phosphorus is slowed, but not stopped. This initial phase was followed by a reversal in which the sediments began to release SRP back into the water column. The release rate of phosphorus 30 to 40 days after suspension of sediments in the columns was 0.5 mg/L/day (micrograms per liter per day) at pH 8, and 0.9 mg/L/day at pH 10, indicating that the higher pH increased the rate of phosphorus release by a factor of about two. The highest determined rate of release was approximately 10% (percent) of the rate required to explain the annual internal loading to Upper Klamath Lake from the sediments as calculated from a lake-wide mass balance and observed in total phosphorus data collected at individual locations.

Evaluation of Dried Urine Spot Method to Screen Cotinine among Tobacco Dependents: An Exploratory Study.

PubMed

Jain, Raka; Quraishi, Rizwana; Verma, Arpita

2017-01-01

Assessment of cotinine, a metabolite of nicotine in body fluids, is an important approach for validating the self-report among tobacco users. Adaptation of assays on dried urine spots (DUSs) has advantages of ease of collection, transportation, minimal invasiveness, and requirement of small volume. The aim of the present study was to develop an efficient method for testing cotinine in DUSs and evaluating its clinical applicability. This involved optimization of conditions for detection, recovery, and stability of cotinine from dried urine, spotted on filter paper. Enzyme-linked immunosorbent assay was used for screening, whereas confirmation was done by gas chromatography. For clinical applicability, urine samples of tobacco users were tested. Water was found to be a suitable extracting solvent as compared to carbonate-bicarbonate buffer (pH 9.2) and saline. Screening was achieved by two punches taken from a 20 μl (diameter 1.3 cm) spotted urine samples, and confirmation was achieved by five complete circles each of 20 μl sample volume. The recovery was found to be 97% in water. Limit of detection for the method was found to be 100 ng/ml. No signs of significant degradation were found under all storage conditions. All the urine samples of tobacco users were found to be positive by a conventional method as well as DUSs, and the method proved to be efficient. DUS samples are a useful alternative for biological monitoring of recent nicotine use, especially in developing countries where sample logistics could be an important concern.

Covalent triazine framework-1 as adsorbent for inline solid phase extraction-high performance liquid chromatographic analysis of trace nitroimidazoles in porcine liver and environmental waters.

PubMed

Zhong, Cheng; Chen, Beibei; He, Man; Hu, Bin

2017-02-03

In this study, covalent triazine framework-1 (CTF-1) was adopted as solid phase extraction (SPE) sorbents, and a method of SPE inline coupled with high performance liquid chromatography-ultraviolet (HPLC-UV) detection was developed for trace analysis of three nitroimidazolaes (including metronidazole, ronidazole and dimetridazole) in porcine liver and environmental water samples. CTF-1 has rich π-electron and N containing triazine, thus can form π-π interaction and intermolecular hydrogen bond with three target polar nitroimidazoles, resulting in high extraction efficiency (87%-98%). Besides, CTF-1 has large specific area, which benefits rapid mass transfer and low column pressure, leading to fast adsorption/desorption dynamics. Several parameters affecting inline SPE including pH, sample flow rate, sample volume, desorption reagents, elution flow rate, elution volume, and ionic strength were investigated. Under the optimal experimental conditions, the limits of detection (S/N=3) were found to be in the range of 0.11-0.13μg/L. The enrichment factors (EFs) ranged from 52 to 59 fold (theoretical EF was 60-fold). The relative standard deviations were in the range of 4.3-9.4% (n=7, c=1μg/L), and the linear range was 0.5-500μg/L for three target analytes. The sample throughput is 7/h. The proposed method was successfully applied to the analysis of nitroimidazoles in porcine liver and environmental water samples with good recoveries for the spiked samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Iodine retention during evaporative volume reduction

DOEpatents

Godbee, H.W.; Cathers, G.I.; Blanco, R.E.

1975-11-18

An improved method for retaining radioactive iodine in aqueous waste solutions during volume reduction is disclosed. The method applies to evaporative volume reduction processes whereby the decontaminated (evaporated) water can be returned safely to the environment. The method generally comprises isotopically diluting the waste solution with a nonradioactive iodide and maintaining the solution at a high pH during evaporation.

Synthesis and characterization of smart N-isopropylacrylamide-based magnetic nanocomposites containing doxorubicin anti-cancer drug.

PubMed

Motaali, Soheila; Pashaeiasl, Maryam; Akbarzadeh, Abolfazl; Davaran, Soodabeh

2017-05-01

In the present study, magnetic and thermo/pH-sensitive (multiresponsive) nanocomposites based on N-isopropylacrylamide (NIPAAM) were synthesized and characterized. Nanocomposites were synthesized by free radical emulsion polymerization of NIPAAM as thermosensitive monomer and N,N-dimethyl-aminoethyl methacrylate (DMAEMA) as pH-sensitive monomer in the presence of methylene-bis-acrylamide as cross-linking agent. Doxorubicin, an anti-cancer drug, was loaded into these nanocomposites via equilibrium swelling method. Thermo/pH-sensitive cross-linked poly (NIPAAM-DMAEMA)-Fe 3 O 4 nanocomposites were characterized by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), and vibrating sample magnetometer (VSM). The volume of the loaded drug and drug release amount was determined by UV measurements. The results showed that this thermo/pH-sensitive magnetic nanocomposite has a high drug-loading efficiency. Doxorubicin was released at 40 °C and pH 5.8 more than the 37 °C and pH 7.4.

SERS detection of Biomolecules at Physiological pH via aggregation of Gold Nanorods mediated by Optical Forces and Plasmonic Heating

NASA Astrophysics Data System (ADS)

Fazio, Barbara; D'Andrea, Cristiano; Foti, Antonino; Messina, Elena; Irrera, Alessia; Donato, Maria Grazia; Villari, Valentina; Micali, Norberto; Maragò, Onofrio M.; Gucciardi, Pietro G.

2016-06-01

Strategies for in-liquid molecular detection via Surface Enhanced Raman Scattering (SERS) are currently based on chemically-driven aggregation or optical trapping of metal nanoparticles in presence of the target molecules. Such strategies allow the formation of SERS-active clusters that efficiently embed the molecule at the “hot spots” of the nanoparticles and enhance its Raman scattering by orders of magnitude. Here we report on a novel scheme that exploits the radiation pressure to locally push gold nanorods and induce their aggregation in buffered solutions of biomolecules, achieving biomolecular SERS detection at almost neutral pH. The sensor is applied to detect non-resonant amino acids and proteins, namely Phenylalanine (Phe), Bovine Serum Albumin (BSA) and Lysozyme (Lys), reaching detection limits in the μg/mL range. Being a chemical free and contactless technique, our methodology is easy to implement, fast to operate, needs small sample volumes and has potential for integration in microfluidic circuits for biomarkers detection.

Aspects of the "Design Space" in high pressure liquid chromatography method development.

PubMed

Molnár, I; Rieger, H-J; Monks, K E

2010-05-07

The present paper describes a multifactorial optimization of 4 critical HPLC method parameters, i.e. gradient time (t(G)), temperature (T), pH and ternary composition (B(1):B(2)) based on 36 experiments. The effect of these experimental variables on critical resolution and selectivity was carried out in such a way as to systematically vary all four factors simultaneously. The basic element is a gradient time-temperature (t(G)-T) plane, which is repeated at three different pH's of the eluent A and at three different ternary compositions of eluent B between methanol and acetonitrile. The so-defined volume enables the investigation of the critical resolution for a part of the Design Space of a given sample. Further improvement of the analysis time, with conservation of the previously optimized selectivity, was possible by reducing the gradient time and increasing the flow rate. Multidimensional robust regions were successfully defined and graphically depicted. Copyright (c) 2010 Elsevier B.V. All rights reserved.

SERS detection of Biomolecules at Physiological pH via aggregation of Gold Nanorods mediated by Optical Forces and Plasmonic Heating

PubMed Central

Fazio, Barbara; D’Andrea, Cristiano; Foti, Antonino; Messina, Elena; Irrera, Alessia; Donato, Maria Grazia; Villari, Valentina; Micali, Norberto; Maragò, Onofrio M.; Gucciardi, Pietro G.

2016-01-01

Strategies for in-liquid molecular detection via Surface Enhanced Raman Scattering (SERS) are currently based on chemically-driven aggregation or optical trapping of metal nanoparticles in presence of the target molecules. Such strategies allow the formation of SERS-active clusters that efficiently embed the molecule at the “hot spots” of the nanoparticles and enhance its Raman scattering by orders of magnitude. Here we report on a novel scheme that exploits the radiation pressure to locally push gold nanorods and induce their aggregation in buffered solutions of biomolecules, achieving biomolecular SERS detection at almost neutral pH. The sensor is applied to detect non-resonant amino acids and proteins, namely Phenylalanine (Phe), Bovine Serum Albumin (BSA) and Lysozyme (Lys), reaching detection limits in the μg/mL range. Being a chemical free and contactless technique, our methodology is easy to implement, fast to operate, needs small sample volumes and has potential for integration in microfluidic circuits for biomarkers detection. PMID:27246267

Capillary zone electrophoresis-tandem mass spectrometry detects low concentration host cell impurities in monoclonal antibodies

PubMed Central

Zhu, Guijie; Sun, Liangliang; Heidbrink-Thompson, Jennifer; Kuntumalla, Srilatha; Lin, Hung-yu; Larkin, Christopher J.; McGivney, James B.; Dovichi, Norman J.

2016-01-01

We have evaluated capillary zone electrophoresis-electrospray ionization-tandem mass spectrometry (CZE-ESI-MS/MS) for detection of trace amounts of host cell protein impurities in recombinant therapeutics. Compared to previously published procedures, we have optimized the buffer pH used in the formation of a pH junction to increase injection volume. We also prepared a five-point calibration curve by spiking twelve standard proteins into a solution of a human monoclonal antibody. A custom CZE-MS/MS system was used to analyze the tryptic digest of this mixture without depletion of the antibody. CZE generated a ~70 min separation window (~90 min total analysis duration) and ~300 peak capacity. We also analyzed the sample using ultra-performance liquid chromatography (UPLC)-MS/MS. CZE-MS/MS generated ~five times higher base peak intensity and more peptide identifications for low-level spiked proteins. Both methods detected all proteins spiked at the ~100 ppm level with respect to the antibody. PMID:26530276

Irreversibility of 2,4-Dichlorophenoxyacetic Acid Sorption onto a Volcanic Ash Soil

NASA Astrophysics Data System (ADS)

Mon, E.; Kawamoto, K.; Komatsu, T.; Moldrup, P.

2008-12-01

Pesticide sorption and desorption in soils are key processes governing fate and transport of pesticides in the soil environment. The irreversibility (or hysteresis) in the processes of pesticide sorption and desorption needs to be known to accurately predict behavior of pesticides in soil systems. 2,4-dichlorophenoxyacetic acid (2,4-D) is a widely used pesticide in agriculture fields. However, only few studies of 2,4-D adsorption onto Andosols (volcanic ash soils) have been published, and the knowledge of 2,4-D desorption onto Andosols is very limited. In this study, a volcanic ash soil sampled from a pasture site in Nishi-Tokyo, Japan was used as a sorbent in order to investigate the irreversibility of 2,4-D sorption. For comparison, a pure clay mineral (kaolinite) obtained from Clay Science Society of Japan (CSSJ) was also used. 2,4-D solutions with three concentrations (0.011, 0.022 and 0.045 mmol/L) were prepared in artificial rain water (ARW= 0.085mM NaCl + 0.015mM CaCl2) to simulate field conditions. To prepare the sample solutions, the solid mass/liquid volume ratio of 1:10 was used for both sorbents (volcanic ash soil and kaolinite). The experiments were conducted in triplicate using a batch method under different pH conditions to examine the effect of pH. Desorption was measured during a equilibration procedure: After removal of 7 mL of supernatant in the sorption step, 7 mL of ARW excluding 2,4-D was added to the sample solution after which, it was equilibrated and centrifuged. The procedure was performed sequentially three or four times to obtain a desorption isotherm. Sorption and desorption generally followed Freundlich isotherms. The results showed markedly effects of pH on 2,4-D sorption and desorption in both the soil and kaolinite, with the percentage of sorption increasing with decreasing pH whereas the percentage of desorption decreased. There was a larger adsorption-desorption hysteresis in the volcanic ash soil as compared to kaolinite. Moreover, the largest hysteresis was found under the lowest pH condition indicating that the hysteretic effect likely depended on the variation of pH. In summary, the volcanic ash soil exhibited higher sorption coefficients and hysteresis than kaolinite, likely due to soil properties such as high organic matter content and the presence of different clay minerals.

Geochemical interactions between constituents in acidic groundwater and alluvium in an aquifer near Globe, Arizona

USGS Publications Warehouse

Stollenwerk, Kenneth G.

1994-01-01

Acidic water from a copper-mining area has contaminated an alluvial aquifer and stream near Globe, Arizona. The most contaminated groundwater has a pH of 3.3, and contains about 100 mmol/1 SO4, 50 mmol/1 Fe, 11 mmol/1 Al and 3 mmol/1 Cu. Reactions between alluvium and acidic groundwater were first evaluated in laboratory column experiments. A geochemical model was developed and used in the equilibrium speciation program, MINTEQA2, to simulate breakthrough curves for different constituents from the column. The geochemical model was then used to simulate the measured changes in concentration of aqueous constituents along a flow path in the aquifer.The pH was predominantly controlled by reaction with carbonate minerals. Where carbonates had been dissolved, adsorption of H+ by iron oxides was used to simulate pH. Acidic groundwater contained little or no dissolved oxygen, and most aqueous Fe was present as Fe(II). In the anoxic core of the plume, Fe(II) was oxidized by MnO2 to Fe(III), which then precipitated as Fe(OH)3. Attenuation of aqueous Cu, Co, Mn, Ni and Zn was a function of pH and could be quantitatively modeled with the diffuse-layer, surface complexation model in MINTEQA2. Aluminum precipitated as amorphous Al(OH)3 at pH < 4.7 and as AlOHSO4 at pH < 4.7. Aqueous Ca and SO4were close to equilibrium with gypsum.After the alluvium in the column had reached equilibrium with acidic groundwater, uncontaminated groundwater was eluted through the column to evaluate the effect of reactants on groundwater remediation. The concentration of Fe, Mn, Cu, Co, Ni and Zn rapidly decreased to the detection limits within a few pore volumes. All of the gypsum that had precipitated initially redissolved, resulting in elevated Ca and SO4concentrations for about 5 pore volumes. Aluminum and pH exhibited the most potential for continued adverse effects on groundwater quality. As H+ desorbed from Fe(OH)3, pH remained below 4.5 for more than 20 pore volumes, resulting in dissolution of AlOHSO4 and elevated aqueous Al.

Dispersive liquid-liquid microextraction of quinolones in porcine blood: Optimization of extraction procedure and CE separation using experimental design.

PubMed

Vera-Candioti, Luciana; Teglia, Carla M; Cámara, María S

2016-10-01

A dispersive liquid-liquid microextraction procedure was developed to extract nine fluoroquinolones in porcine blood, six of which were quantified using a univariate calibration method. Extraction parameters including type and volume of extraction and dispersive solvent and pH, were optimized using a full factorial and a central composite designs. The optimum extraction parameters were a mixture of 250 μL dichloromethane (extract solvent) and 1250 μL ACN (dispersive solvent) in 500 μL of porcine blood reached to pH 6.80. After shaking and centrifugation, the upper phase was transferred in a glass tube and evaporated under N 2 steam. The residue was resuspended into 50 μL of water-ACN (70:30, v/v) and determined by CE method with DAD, under optimum separation conditions. Consequently, a tenfold enrichment factor can potentially be reached with the pretreatment, taking into account the relationship between initial sample volume and final extract volume. Optimum separation conditions were as follows: BGE solution containing equal amounts of sodium borate (Na 2 B 4 O 7 ) and di-sodium hydrogen phosphate (Na 2 HPO 4 ) with a final concentration of 23 mmol/L containing 0.2% of poly (diallyldimethylammonium chloride) and adjusted to pH 7.80. Separation was performed applying a negative potential of 25 kV, the cartridge was maintained at 25.0°C and the electropherograms were recorded at 275 nm during 4 min. The hydrodynamic injection was performed in the cathode by applying a pressure of 50 mbar for 10 s. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The effect of acidity of electrolyte on the porosity and the nanostructure morphology of electrolytic manganese dioxide

NASA Astrophysics Data System (ADS)

Adelkhani, H.

2012-06-01

The effects of acidity of electrolyte (pH) on the hysteresis behavior, the specific surface area, and nanostructure morphology of electrolytic manganese dioxides (EMDs) have been studied by using the Barrett-Joyner-Halenda (BJH) analysis, X-ray diffraction (XRD) and scanning electron microscopy (SEM) images analysis. EMD samples are electrodeposited at a variable pH (6 to 1) and many fixed pH (2, 3, 4, 5, and 6). Results indicate that pH play key roles in the characteristics of EMD. The samples obtained at low pH (2 and 3) show multi-branched morphology and represent a H4 hysteresis loop. At pH 4 and 5, a uniform and dense structure of MnO2 is obtained without hysteresis behavior. The sample electrodeposited at pH 6 shows a regular reticulate, that its adsorption-desorption isotherm show hysteresis behavior. By electrodeposition at a variable pH, the sample shows a cauliflower-like and multi-branched form. From the viewpoint of classification of isotherm, pH strongly affects on Type of isotherm. The results show that γ-MnO2 is as main-product of electrodeposition and α-MnO2 and β-MnO2 were obtained as side-product at low and high pH, respectively.

Application of solvent floatation to separation and determination of triazine herbicides in honey by high-performance liquid chromatography.

PubMed

Wang, Kun; Jiang, Jia; Lv, Xinping; Zang, Shuang; Tian, Sizhu; Zhang, Hanqi; Yu, Aimin; Zhang, Ziwei; Yu, Yong

2018-03-01

Based on the foaming property of the honey, a rapid, simple, and effective method solvent floatation (SF) was developed and firstly applied to the extraction and separation of triazine herbicides in honey. The analytes were determined by high-performance liquid chromatography. Some parameters affecting the extraction efficiencies, such as the type and volume of extraction solvent, type of salt, amount of (NH 4 ) 2 SO 4 , pH value of sample solution, gas flow rate, and floatation time, were investigated and optimized. The limits of detection for analytes are in the range of 0.16-0.56 μg kg -1 . The recoveries and relative standard deviations for determining triazines in five real honey samples are in the range of 78.2-112.9 and 0.2-9.2%, respectively.

Mapping Soil pH Buffering Capacity of Selected Fields

NASA Technical Reports Server (NTRS)

Weaver, A. R.; Kissel, D. E.; Chen, F.; West, L. T.; Adkins, W.; Rickman, D.; Luvall, J. C.

2003-01-01

Soil pH buffering capacity, since it varies spatially within crop production fields, may be used to define sampling zones to assess lime requirement, or for modeling changes in soil pH when acid forming fertilizers or manures are added to a field. Our objective was to develop a procedure to map this soil property. One hundred thirty six soil samples (0 to 15 cm depth) from three Georgia Coastal Plain fields were titrated with calcium hydroxide to characterize differences in pH buffering capacity of the soils. Since the relationship between soil pH and added calcium hydroxide was approximately linear for all samples up to pH 6.5, the slope values of these linear relationships for all soils were regressed on the organic C and clay contents of the 136 soil samples using multiple linear regression. The equation that fit the data best was b (slope of pH vs. lime added) = 0.00029 - 0.00003 * % clay + 0.00135 * % O/C, r(exp 2) = 0.68. This equation was applied within geographic information system (GIS) software to create maps of soil pH buffering capacity for the three fields. When the mapped values of the pH buffering capacity were compared with measured values for a total of 18 locations in the three fields, there was good general agreement. A regression of directly measured pH buffering capacities on mapped pH buffering capacities at the field locations for these samples gave an r(exp 2) of 0.88 with a slope of 1.04 for a group of soils that varied approximately tenfold in their pH buffering capacities.

MULTIELEMENT SOLID PHASE PRECONCENTRATION USING A CHELATING RESIN OF STYRENE DIVINYLBENZENE COPOLYMER AND APPLICATION TO ANALYSIS OF SEAWATER AND FISH OTOLITHS BY INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY (ICP�MS)

PubMed Central

Zereen, Fahmida; Yilmaz, Vedat; Arslan, Zikri

2013-01-01

A new chelating resin has been synthesized by immobilizing 4–(2–thiazolylazo) resorcinol (TAR) onto styrene divinlybenzene copolymer and examined for on-line solid phase extraction/preconcentration of Cd, Co, Cu, Ni, Pb and Zn in seawater and fish otoliths for determination by inductively plasma mass spectrometry (ICP-MS). A volume of 5.0 mL sample solution was loaded onto the mini column of TAR immobilized resin at 2.0 mL min−1 via a sequential injection system. The optimum pH for multielement preconcentration was around pH 5.5. Recoveries were better than 96% in artificial seawater. Elution was achieved with 1.0 mL of 0.75 mol L−1 HNO3. The resin possesses large sorption capacity ranging from 82.0 µmol g−1 for Pb to 319 µmol g−1 for Cu. The detection limits (3s) varied between 0.0016 µg L−1 (Cd) and to 0.015 µg L−1 (Zn) for preconcentration of 5.0 mL blank solutions (pH 5.5). Relative standard deviation (RSD)for three replicate runs was between 0.3% (Cd) and 6% (Zn) at 1.0 µg L−1 level. The procedure was validated by analysis of Nearshore Seawater certified reference material (CASS–4), and then successfully applied to the determination of the trace elements in fish otoliths (CRM 22) and in coastal seawater and estuarine water samples. PMID:24976635

Measurement of urinary calcium using AT89C51RD2 microcontroller.

PubMed

Neelamegam, P; Jamaludeen, A; Rajendran, A; Raghunathan, R

2009-04-01

A simple and inexpensive absorption technique for determination of calcium ion in urine samples is developed, comprising a light emitting diode (650 nm) as the light source and photodiode as the detector with AT89C51RD2 microcontroller. The design of the system and details of interface, calibration, and procedure of operation are explained in this paper. Software is developed to monitor sample processing and to display the results in liquid crystal display screen. With 15 microl sample volume, a linear output is obtained in the range of 2.5-7.5 mM calcium with a detection limit of 0.06 mM. Interferences from other cations such as monovalent ion and divalent ion are investigated in the expected range, which are normally present in clinical samples, and absorption changes over the pH range of 3-12 are also determined. This system has been demonstrated successfully for the successive assay of calcium in urine samples, with the results comparing well to those achieved and in good agreement with values obtained with the current clinical spectrophotometric method at 95% of confidence level.

Light-induced pH change and its application to solid phase extraction of trace heavy metals by high-magnetization Fe3O4@SiO2@TiO2 nanoparticles followed by inductively coupled plasma mass spectrometry detection.

PubMed

Zhang, Nan; Peng, Hanyong; Hu, Bin

2012-05-30

We report here the preparation of high-magnetization Fe(3)O(4)@SiO(2)@TiO(2) nanoparticles for solid phase extraction of trace amounts of Cd(II), Cr(III), Mn(II) and Cu(II) from environmental waters. The prepared nanoparticles were characterized by scanning electron micrograph (SEM) and transmission electron microscopy (TEM). The high-magnetization nanoparticles carrying the target metals could be easily and fast separated from the aqueous solution simply by applying an external magnetic field while no filtration or centrifugation was necessary. A light-induced hydroxide ion emitter, molecular malachite green carbinol base (MGCB) was applied to adjust pH value of solution for quantitative adsorption instead of the conventional used buffer. In the presence of UV light, MGCB gives out OH(-) ions, and this leads to an increase in the pH value without the aid of buffer solution. Using high-magnetization Fe(3)O(4)@SiO(2)@TiO(2) nanoparticles as the extraction material and the light-induced MGCB for pH adjustment, we developed an efficient and convenient two-step method for separation/preconcentration trace amounts of Cd(II), Cr(III), Mn(II) and Cu(II) in environmental water samples followed by inductively coupled plasma mass spectrometry (ICP-MS) detection. The parameters affecting the extraction such as MGCB concentration, exposal time, sample volume, eluent condition, and interfering ions have been investigated in detail. Under the optimized conditions, the limits of detection for Cd(II), Cr(III), Mn(II) and Cu(II) were 4.0, 2.6, 1.6 and 2.3 ng L(-1), respectively, and the relative standard deviations (RSDs, c=1 μg L(-1), n=7) were 3.6%, 4.5%, 4.0 and 4.1%, respectively. The proposed method has been validated using certified reference materials, and it has been successfully applied in the determination of trace Cd(II), Cr(III), Mn(II) and Cu(II) in environmental water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

The precision of wet atmospheric deposition data from national atmospheric deposition program/national trends network sites determined with collocated samplers

USGS Publications Warehouse

Nilles, M.A.; Gordon, J.D.; Schroder, L.J.

1994-01-01

A collocated, wet-deposition sampler program has been operated since October 1988 by the U.S. Geological Survey to estimate the overall sampling precision of wet atmospheric deposition data collected at selected sites in the National Atmospheric Deposition Program and National Trends Network (NADP/NTN). A duplicate set of wet-deposition sampling instruments was installed adjacent to existing sampling instruments at four different NADP/NTN sites for each year of the study. Wet-deposition samples from collocated sites were collected and analysed using standard NADP/NTN procedures. Laboratory analyses included determinations of pH, specific conductance, and concentrations of major cations and anions. The estimates of precision included all variability in the data-collection system, from the point of sample collection through storage in the NADP/NTN database. Sampling precision was determined from the absolute value of differences in the analytical results for the paired samples in terms of median relative and absolute difference. The median relative difference for Mg2+, Na+, K+ and NH4+ concentration and deposition was quite variable between sites and exceeded 10% at most sites. Relative error for analytes whose concentrations typically approached laboratory method detection limits were greater than for analytes that did not typically approach detection limits. The median relative difference for SO42- and NO3- concentration, specific conductance, and sample volume at all sites was less than 7%. Precision for H+ concentration and deposition ranged from less than 10% at sites with typically high levels of H+ concentration to greater than 30% at sites with low H+ concentration. Median difference for analyte concentration and deposition was typically 1.5-2-times greater for samples collected during the winter than during other seasons at two northern sites. Likewise, the median relative difference in sample volume for winter samples was more than double the annual median relative difference at the two northern sites. Bias accounted for less than 25% of the collocated variability in analyte concentration and deposition from weekly collocated precipitation samples at most sites.A collocated, wet-deposition sampler program has been operated since OCtober 1988 by the U.S Geological Survey to estimate the overall sampling precision of wet atmospheric deposition data collected at selected sites in the National Atmospheric Deposition Program and National Trends Network (NADP/NTN). A duplicate set of wet-deposition sampling instruments was installed adjacent to existing sampling instruments four different NADP/NTN sites for each year of the study. Wet-deposition samples from collocated sites were collected and analysed using standard NADP/NTN procedures. Laboratory analyses included determinations of pH, specific conductance, and concentrations of major cations and anions. The estimates of precision included all variability in the data-collection system, from the point of sample collection through storage in the NADP/NTN database.

Combination of dispersive liquid-liquid microextraction with flame atomic absorption spectrometry using microsample introduction for determination of lead in water samples.

PubMed

Naseri, Mohammad Taghi; Hemmatkhah, Payam; Hosseini, Mohammad Reza Milani; Assadi, Yaghoub

2008-03-03

The dispersive liquid-liquid microextraction (DLLME) was combined with the flame atomic absorption spectrometry (FAAS) for determination of lead in the water samples. Diethyldithiophosphoric acid (DDTP), carbon tetrachloride and methanol were used as chelating agent, extraction solvent and disperser solvent, respectively. A new FAAS sample introduction system was employed for the microvolume nebulization of the non-flammable chlorinated organic extracts. Injection of 20 microL volumes of the organic extract into an air-acetylene flame provided very sensitive spike-like and reproducible signals. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters include extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH and amount of the chelating agent. Under the optimized conditions, the enrichment factor of 450 was obtained from a sample volume of 25.0 mL. The enhancement factor, calculated as the ratio of the slopes of the calibration graphs with and without preconcentration, which was about 1000. The calibration graph was linear in the range of 1-70 microgL(-1) with a detection limit of 0.5 microgL(-1). The relative standard deviation (R.S.D.) for seven replicate measurements of 5.0 and 50 microgL(-1) of lead were 3.8 and 2.0%, respectively. The relative recoveries of lead in tap, well, river and seawater samples at the spiking level of 20 microgL(-1) ranged from 93.8 to 106.2%. The characteristics of the proposed method were compared with those of the liquid-liquid extraction (LLE), cloud point extraction (CPE), on-line and off-line solid-phase extraction (SPE) as well as co-precipitation, based on bibliographic data. Operation simplicity, rapidity, low cost, high enrichment factor, good repeatability, and low consumption of the extraction solvent at a microliter level are the main advantages of the proposed method.

A dispersive liquid-liquid microextraction based on solidification of floating organic droplet followed by injector port silylation coupled with gas chromatography-tandem mass spectrometry for the determination of nine bisphenols in bottled carbonated beverages.

PubMed

Mandrah, Kapil; Satyanarayana, G N V; Roy, Somendu Kumar

2017-12-15

In the present study, a method has been efficiently developed for the first time to determine nine bisphenol analogues [bisphenol A (BPA), bisphenol C (BPC), bisphenol AF (BPAF), bisphenol E (BPE), bisphenol F (BPF), bisphenol G (BPG), bisphenol M (BPM), bisphenol S (BPS), and bisphenol Z (BPZ)] together in bottled carbonated beverages (collected from the local market of Lucknow, India) using dispersive liquid-liquid microextraction process. This is based on solidification of floating organic droplet (DLLME-SFO) followed by injector port silylation coupled with gas chromatography-tandem mass spectrometry. The process investigated parameters of DLLME-SFO (including the type of extraction and disperser solvents with their volumes, effect of pH, ionic strength, and the sample volume), factors influencing to injection port derivatization like, collision energy, injector port temperature, derivatizing reagent with sample injection volume, and type of organic solvent. BPA, BPF, BPZ, and BPS were detected in each sample; whereas, other bisphenols were also detected in some carbonated beverage samples. After optimizing the required conditions, good linearity of analytes was achieved in the range of 0.097-100ngmL -1 with coefficients of determination (R 2 )≥0.995. Intra-day and inter day precision of the method was good, with relative standard deviation (% RSD)≤10.95%. The limits of detection (LOD) and limits of quantification (LOQ) values of all bisphenols were ranged from 0.021 to 0.104ngmL -1 and 0.070 to 0.343ngmL -1 , respectively. The recovery of extraction was good (73.15-95.08%) in carbonated beverage samples and good enrichment factors (96.36-117.33) were found. Thus, the developed method of microextraction was highly precise, fast, and reproducible to determine the level of contaminants in bottled carbonated beverages. Copyright © 2017 Elsevier B.V. All rights reserved.

Regional postprandial differences in pH within the stomach and gastroesophageal junction.

PubMed

Simonian, Hrair P; Vo, Lien; Doma, Siva; Fisher, Robert S; Parkman, Henry P

2005-12-01

Our objective was to determine regional differences in intragastric pH after different types of meals. Ten normal subjects underwent 27-hr esophagogastric pH monitoring using a four-probe pH catheter. Meals were a spicy lunch, a high-fat dinner, and a typical bland breakfast. The fatty dinner had the highest postprandial buffering effect, elevating proximal and mid/distal gastric pH to 4.9 +/- 0.4 and 4.0 +/- 0.4, respectively, significantly (P < 0.05) higher compared to 4.2 +/- 0.3 and 3.0 +/- 0.4 for the spicy lunch and 3.0 +/- 0.3 and 2.5 +/- 0.8 for the breakfast. The buffering effect of the high-volume fatty meal to pH > 4 was also longer (150 min) compared to that of the spicy lunch (45 min) and the bland breakfast, which did not increase gastric pH to > 4 at any time. Proximal gastric acid pockets were seen between 15 and 90 min postprandially. These were located 3.4 +/- 0.8 cm below the proximal LES border, extending for a length of 2.3 +/- 0.8 cm, with a drop in mean pH from 4.7 +/- 0.4 to 1.5 +/- 0.9. Acid pockets were seen equally after the spicy lunch and fatty dinner but less frequently after the bland breakfast. We conclude that a high-volume fatty meal has the highest buffering effect on gastric pH compared to a spicy lunch or a bland breakfast. Buffering effects of meals are significantly higher in the proximal than in the mid/distal stomach. Despite the intragastric buffering effect of meals, focal areas of acidity were observed in the region of the cardia-gastroesophageal junction during the postprandial period.

Development of a new multi-residue laser diode thermal desorption atmospheric pressure chemical ionization tandem mass spectrometry method for the detection and quantification of pesticides and pharmaceuticals in wastewater samples.

PubMed

Boisvert, Michel; Fayad, Paul B; Sauvé, Sébastien

2012-11-19

A new solid phase extraction (SPE) method coupled to a high throughput sample analysis technique was developed for the simultaneous determination of nine selected emerging contaminants in wastewater (atrazine, desethylatrazine, 17β-estradiol, ethynylestradiol, norethindrone, caffeine, carbamazepine, diclofenac and sulfamethoxazole). We specifically included pharmaceutical compounds from multiple therapeutic classes, as well as pesticides. Sample pre-concentration and clean-up was performed using a mixed-mode SPE cartridge (Strata ABW) having both cation and anion exchange properties, followed by analysis by laser diode thermal desorption atmospheric pressure chemical ionization coupled to tandem mass spectrometry (LDTD-APCI-MS/MS). The LDTD interface is a new high-throughput sample introduction method, which reduces total analysis time to less than 15s per sample as compared to minutes with traditional liquid-chromatography coupled to tandem mass spectrometry (LC-MS/MS). Several SPE parameters were evaluated in order to optimize recovery efficiencies when extracting analytes from wastewater, such as the nature of the stationary phase, the loading flow rate, the extraction pH, the volume and composition of the washing solution and the initial sample volume. The method was successfully applied to real wastewater samples from the primary sedimentation tank of a municipal wastewater treatment plant. Recoveries of target compounds from wastewater ranged from 78% to 106%, the limit of detection ranged from 30 to 122ng L(-1) while the limit of quantification ranged from 90 to 370ng L(-1). Calibration curves in the wastewater matrix showed good linearity (R(2)≥0.991) for all target analytes and the intraday and interday coefficient of variation was below 15%, reflecting a good precision. Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis, bioactivity and zeta potential investigations of chlorine and fluorine substituted hydroxyapatite.

PubMed

Fahami, Abbas; Beall, Gary W; Betancourt, Tania

2016-02-01

Chlorine and fluorine substituted hydroxyapatites (HA-Cl-F) with different degrees of ion replacement were successfully prepared by the one step mechanochemical activation method. X-ray diffraction (XRD) and FT-IR spectra indicated that substitution of these anions in milled powders resulted in the formation of pure hydroxyapatite phase except for the small observed change in the lattice parameters and unit cell volumes of the resultant hydroxyapatite. Microscopic observations showed that the milled product had a cluster-like structure made up of polygonal and spherical particles with an average particle size of approximately ranged from 20±5 to 70±5nm. The zeta potential of milled samples was performed at three different pH (5, 7.4, and 9). The obtained zeta potential values were negative for all three pH values. Negative zeta potential was described to favor osseointegration, apatite nucleation, and bone regeneration. The bioactivity of samples was investigated on sintered pellets soaked in simulated body fluid (SBF) solution and apatite crystals formed on the surface of the pellets after being incubated for 14days. Zeta potential analysis and bioactivity experiment suggested that HA-Cl-F will lead to the formation of new apatite particles and therefore be a potential implant material. Copyright © 2015 Elsevier B.V. All rights reserved.

Parsley! Mechanism as antiurolithiasis remedy.

PubMed

Al-Yousofy, Fayed; Gumaih, Hussein; Ibrahim, Hassan; Alasbahy, Afrah

2017-01-01

Parsley is a medicinal plant used widely in urolithiasis. The present study aimed to evaluate the antiurolithiatic effect of parsley and its mechanism. 24 rats divided into four groups: group A (negative control), group B (positive control), group C (cystone ® group) and group D (parsley group). Group B were treated with EG and Ammonium chloride (AC). Group C were treated as B plus cystone ® and group D was treated as B plus parsley. The period of experiment was 15 days. Urine samples were analysis on days 0 and 15 days. Kidneys of rats from all groups were removed, and histopathologically examined. The kidnies of parsley treated group appeared mostly to be calculi-free (less CaOx) even better than the cystone treated group. CaOx crystals was significantly lower both in histological sections and in urine samples in parsley treated group. We further investigated the mechanism of parsley by adding another 6 rats. The latter treated by parsley only after adaptation period. We found significant increase in urine volume and pH in parsley treated rats compared to negative control. We concluded that parsley acts as antiurolithiatic drug through decreasing urinary calcium excretion, increasing urinary pH, dieresis, decreasing urinary protein excretion and its nephroprtective activity. We recommended to use it in pharmaceutical forms as it is safe and effective as antiurolithiasis remedy.

Brain aging: Evaluation of pH using phosphorus magnetic resonance spectroscopy.

PubMed

Cichocka, Monika; Kozub, Justyna; Urbanik, Andrzej

2018-02-02

Very important aspects of aging include age-related changes occurring in the brain. The aim of the present study was to identify the standard pH value in the entire brain volume using phosphorus magnetic resonance spectroscopy in healthy individuals of both sexes in different age groups, and then to determine whether there are differences in these values. A total of 65 individuals aged 20-32 years (mean age 24.5 ± 2.1 years, 31 women and 34 men) and 31 individuals aged 60-81 years (mean age 64.9 ± 5.5 years, 17 women and 14 men) were studied. The phosphorus magnetic resonance spectroscopy examination was carried out using a 1.5-T magnetic resonance system. The signal was acquired from the volume of interest that covered the whole brain. A vast majority of the examined individuals had slightly alkaline brain pH regardless of age. In the ≥20 years group, pH was 7.09 ± 0.11, and in the ≥60 years group, the average pH was 7.03 ± 0.05. This comparison of the pH identified in all the tested individuals shows a negative correlation of pH with age. The present findings might provide a valuable basis for further research into "healthy aging" as well as pathology in older adults. Geriatr Gerontol Int 2018; ••: ••-••. © 2018 Japan Geriatrics Society.

Influence of the kind of peat and the depth of sampling on the biochemical properties of Tagan peatland

NASA Astrophysics Data System (ADS)

Wojciech Szajdak, Lech; Inisheva, Lydia I.

2010-05-01

The upper layer of a peat bog in which organic matter decomposes aerobically much more rapidly than in the underlying, anaerobic catotelm. As litter accumulates at the surface the size of the catotelm increases, because the thickness of the acrotelm is limited to depth at which aerobic respiration can occur. Although the rate of decomposition per unit volume of material is much greater in the acrotelm than in the catotelm, a point is reached at which the difference in volume between the two layers is such that the total rate of decomposition in the catotelm is equal to that in the acrotelm. This limits the thickness to which the bog can grow. Should there be a climate change (e.g. an increase in precipitation) growth can resume. Bogs therefore preserve a record of climatic conditions. Soils samples were taken from four places marked as No 1, 2, 3 and 4 each from two depth 0-25 and 50-75 cm of the peatland Tagan. Peatlands Tagan is located near Tomsk, West Siberia, Russia. Place No 1 in both layers represents grasses peat with the degree of the decomposition ranged from 25 to 35% (pH 6.31-7.95). Point 2 is characterized by wooden and wooden grasses peat with 35% degree of the decomposition (pH 5.16-9.31. There is buckbean peat in the points 3 and 4 (pH 6.4-6.49). However, 1.5 m depth of sapropel is located in point 4. The activity of the following enzymes: xanthine oxidase, phenolic oxidase, peroxidase, urease, nitrate reductase were measured and two forms of organic carbon (total organic carbon and dissolved organic carbon) and two form of iron Fe(II) and Fe(III) were determined in these samples. These enzymes participate in several biochemical pathways in soil connected with redox potential. The concentrations of indole-3-acetic acid, very famous fitohormone were also measured. It was observed in all places of sampling significant increase of the total organic carbon with an increase of the depth. However, the quantity of dissolved organic carbon closely decreased with an increase of the depth, suggesting lower microbiological activity of this level. The increase of the ratios Fe(II)/Fe(III) for place 1 and 2 and 4 and both depth 0-25 were similar (0.56; 0.59 and 0.65) indicating similar redox properties of these levels. Higher contents of F(III) were determined in upper layer than in lower layer of all samples. It indicate higher oxidizing properties upper layer than lower one The activity of nitrate reductase, peroxidase, phenolic axidase and xanthine oxidase agree with the content of two forms of iron in samples from all depth. In all samples was observed the decrease of the activity of urease with an increase of the depth. It suggest higher rate of the degradation process of urea created from the decomposition of peptides in peat. In sample No 1 the concentrations of indole-3-acetic acid very famous phytohormone were similar in both determined levels. However for sample No 2, 3 and 4 the significant decrease of the concentrations of indole-3-acetic acid with and increase of the depth of sampling was observed. Acknowledgements: This work was supported by a grant No. N N305 3204 36 founded by Polish Ministry of Education and by RFFR (No.No. 09-05-00235, 09-05-00395), Minister of Education and Science (No. 02.740.11.0325).

Comprehensive evaluation of formulation factors for ocular penetration of fluoroquinolones in rabbits using cassette dosing technique.

PubMed

Sharma, Charu; Biswas, Nihar R; Ojha, Shreesh; Velpandian, Thirumurthy

2016-01-01

Corneal permeability of drugs is an important factor used to assess the efficacy of topical preparations. Transcorneal penetration of drugs from aqueous formulation is governed by various physiological, physiochemical, and formulation factors. In the present study, we investigated the effect of formulation factors like concentration, pH, and volume of instillation across the cornea using cassette dosing technique for ophthalmic fluoroquinolones (FQs). Sterile cocktail formulations were prepared using four congeneric ophthalmic FQs (ofloxacin, sparfloxacin, pefloxacin mesylate, and gatifloxacin) at concentrations of 0.025%, 0.5%, and 0.1%. Each formulation was adjusted to different pH ranges (4.5, 7.0, and 8.0) and assessed for transcorneal penetration in vivo in rabbit's cornea (n=4 eyes) at three different volumes (12.5, 25, and 50 μL). Aqueous humor was aspirated through paracentesis after applying local anesthesia at 0, 5, 15, 30, 60, 120, and 240 minutes postdosing. The biosamples collected from a total of 27 groups were analyzed using liquid chromatography-tandem mass spectroscopy to determine transcorneal permeability of all four FQs individually. Increase in concentration showed an increase in penetration up to 0.05%; thereafter, the effect of concentration was found to be dependent on volume of instillation as we observed a decrease in transcorneal penetration. The highest transcorneal penetration of all FQs was observed at pH 7.0 at concentration 0.05% followed by 0.025% at pH 4.5. Lastly, increasing the volume of instillation from 12.5 to 50 μL showed a significant fall in transcorneal penetration. The study concludes that formulation factors showed discernible effect on transcorneal permeation; therefore, due emphasis should be given on drug development and design of ophthalmic formulation.

Preparation and characterization of magnetic carboxylated nanodiamonds for vortex-assisted magnetic solid-phase extraction of ziram in food and water samples.

PubMed

Yılmaz, Erkan; Soylak, Mustafa

2016-09-01

A simple and rapid vortex-assisted magnetic solid phase extraction (VA-MSPE) method for the separation and preconcentration of ziram (zinc dimethyldithiocarbamate), subsequent detection of the zinc in complex structure of ziram by flame atomic absorption spectrometry (AAS) has been developed. The ziram content was calculated by using stoichiometric relationship between the zinc and ziram. Magnetic carboxylated nanodiamonds (MCNDs) as solid-phase extraction adsorbent was prepared and characterized by Fourier transform infrared (FT-IR) spectra, X-ray diffraction (XRD) spectrometry and scanning electron microscopy (SEM). These magnetic carboxylated nanodiamonds carrying the ziram could be easily separated from the aqueous solution by applying an external magnetic field; no filtration or centrifugation was necessary. Some important factors influencing the extraction efficiency of ziram such as pH of sample solution, amount of adsorbent, type and volume of eluent, extraction and desorption time and sample volume were studied and optimized. The total extraction and detection time was lower than 10min The preconcentration factor (PF), the precision (RSD, n=7), the limit of detection (LOD) and limit of quantification (LOQ) were 160, 7.0%, 5.3µgL(-1) and 17.5µgL(-1), respectively. The interference of various ions has been examined and the method has been applied for the determination of ziram in various waters, foodstuffs samples and synthetic mixtures. Copyright © 2016 Elsevier B.V. All rights reserved.

Concentration of seeded simian rotavirus SA-11 from potable waters by using talc-celite layers and hydroextraction.

PubMed

Ramia, S; Sattar, S A

1980-03-01

There is mounting evidence for the waterborne transmission of diarrhea caused by rotaviruses. As a result, proper techniques are required for their recovery from samples of incriminated water. The combined efficiency of the talc-Celite technique and polyethylene glycol 6000 hydroextraction was, therefore, tested for this purpose, using Simian rotavirus SA-11 and MA-104 cells. Conditioning of the dechlorinated tap water samples was carried out by pH adjustment to 6.0 and the addition of Earle balanced salt solution to a final concentration of 1:100. Passage of a 1-liter volume of such a conditioned sample through a layer containing a mixture of talc (300 mg) and Celite 503 (100 mg) led to the adsorption of nearly 93% of the added SA-11 plaque-forming units. For the recovery of the layer-adsorbed virus, 3% beef extract and 1x tryptose phosphate broth were found to be superior to a variety of other eluents tested. When we tested 100-liter sample volumes, layers containing 1.2 g of talc and 0.4 g of Celite were employed. Virus elution was carried out with 100 ml of tryptose phosphate broth. The eluate was concentrated 10-fold by overnight (4 degrees C) hydroextraction with polyethylene glycol. With a total input virus of 7.0 x 10(5) and 1.4 x 10(2) plaque-forming units, the recoveries were about 71 and 59%, respectively.

The influence of normal and high ultimate muscle pH on the microbiology and colour stability of previously frozen black wildebeest (Connochaetes gnou) meat.

PubMed

Shange, Nompumelelo; Makasi, Thandeka N; Gouws, Pieter A; Hoffman, Louwrens C

2018-01-01

Changes in pH, colour and microbiological counts were investigated in previously frozen Biceps femoris (BF) muscles from black wildebeest. Samples were stored under vacuum at refrigerated conditions (4.2±0.8°C) for 12days. Seven BF muscles had a high pH (DFD) (pH≥6) and five had a normal pH (pH<6). Overtime the pH of DFD did not significantly change whilst that of normal pH meat decreased. Browning under anaerobic storage conditions was seen, more for normal meat than DFD meat. Initial total viable counts, lactic acid bacteria and coliform counts from samples with normal pH, were significantly higher than counts from the DFD samples. However, overtime DFD meat showed a faster increase for all microorganisms tested compared to normal pH meat. Overall, this study revealed that DFD meat can have a shorter shelf-life than normal pH meat stored at 4.2±0.8°C. Copyright © 2017 Elsevier Ltd. All rights reserved.

The choice of ultrasound assisted extraction coupled with spectrophotometric for rapid determination of gallic acid in water samples: Central composite design for optimization of process variables.

PubMed

Pooralhossini, Jaleh; Ghaedi, Mehrorang; Zanjanchi, Mohammad Ali; Asfaram, Arash

2017-01-01

A sensitive procedure namely ultrasound-assisted (UA) coupled dispersive nano solid-phase microextraction spectrophotometry (DNSPME-UV-Vis) was designed for preconcentration and subsequent determination of gallic acid (GA) from water samples, while the detailed of composition and morphology and also purity and structure of this new sorbent was identified by techniques like field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) and Energy-dispersive X-ray spectroscopy (EDX) techniques. Among conventional parameters viz. pH, amount of sorbent, sonication time and volume of elution solvent based on Response Surface Methodology (RSM) and central composite design according to statistics based contour the best operational conditions was set at pH of 2.0; 1.5mg sorbent, 4.0min sonication and 150μL ethanol. Under these pre-qualified conditions the method has linear response over wide concentration range of 15-6000ngmL -1 with a correlation coefficient of 0.9996. The good figure of merits like acceptable LOD (S/N=3) and LOQ (S/N=10) with numerical value of 2.923 and 9.744ngmL -1 , respectively and relative recovery between 95.54 and 100.02% show the applicability and efficiency of this method for real samples analysis with RSDs below 6.0%. Finally the method with good performance were used for monitoring under study analyte in various real samples like tap, river and mineral waters. Copyright © 2016 Elsevier B.V. All rights reserved.

Sampling and storage of blood for pH and blood gas analysis.

PubMed

Haskins, S C

1977-02-15

Techniques used in sampling and storage of a blood sample for pH and gas measurements can have an important effect on the measured values. Observation of these techniques and principles will minimize in vitro alteration of the pH and blood gas values. To consider that a significant change has occurred in a pH or blood gas measurement from previous values, the change must exceed 0.015 for pH, 3 mm Hg for PCO2, 5 mm Hg for PO2, and 2 mEq/L for [HCO-3] or base excess/deficit. In vitro dilution of the blood sample with anticoagulant should be avoided because it will alter the measured PCO2 and base excess/deficit values. Arterial samples should be collected for meaningful pH and blood gas values. Central venous and free-flowing capillary blood can be used for screening procedures in normal patients but are subject to considerable error. A blood sample can be stored for up to 30 minutes at room temperature without significant change in acid-base values but only up to 12 minutes before significant changes occur in PO2. A blood sample can be stored for up to 3.5 hours in an ice-water bath without significant change in pH and for 6 hours without significant change in PCO2 or PO2. Variations of body temperatures from normal will cause a measurable change in pH and blood gas values when the blood is exposed to the normal water bath temperatures of the analyzer.

Pediatric Cystic Fibrosis Sputum Can Be Chemically Dynamic, Anoxic, and Extremely Reduced Due to Hydrogen Sulfide Formation

PubMed Central

Cowley, Elise S.; Kopf, Sebastian H.; LaRiviere, Alejandro

2015-01-01

ABSTRACT Severe and persistent bacterial lung infections characterize cystic fibrosis (CF). While several studies have documented the microbial diversity within CF lung mucus, we know much less about the inorganic chemistry that constrains microbial metabolic processes and their distribution. We hypothesized that sputum is chemically heterogeneous both within and between patients. To test this, we measured microprofiles of oxygen and sulfide concentrations as well as pH and oxidation-reduction potentials in 48 sputum samples from 22 pediatric patients with CF. Inorganic ions were measured in 20 samples from 12 patients. In all cases, oxygen was depleted within the first few millimeters below the sputum-air interface. Apart from this steep oxycline, anoxia dominated the sputum environment. Different sputum samples exhibited a broad range of redox conditions, with either oxidizing (16 mV to 355 mV) or reducing (−300 to −107 mV) potentials. The majority of reduced samples contained hydrogen sulfide and had a low pH (2.9 to 6.5). Sulfide concentrations increased at a rate of 0.30 µM H2S/min. Nitrous oxide was detected in only one sample that also contained sulfide. Microenvironmental variability was observed both within a single patient over time and between patients. Modeling oxygen dynamics within CF mucus plugs indicates that anoxic zones vary as a function of bacterial load and mucus thickness and can occupy a significant portion of the mucus volume. Thus, aerobic respiration accounts only partially for pathogen survival in CF sputum, motivating research to identify mechanisms of survival under conditions that span fluctuating redox states, including sulfidic environments. PMID:26220964

Stability of an extemporaneously prepared tadalafil suspension.

PubMed

Pettit, Rebecca S; Johnson, Cary E; Caruthers, Regine L

2012-04-01

The stability of an extemporaneously prepared tadalafil oral suspension was studied. An oral suspension of tadalafil 5 mg/mL was prepared by thoroughly grinding 15 20-mg tadalafil tablets in a glass mortar. Thirty milliliters of Ora-Plus and 30 mL of Ora-Sweet were mixed and added to the powder to make a final volume of 60 mL. Three identical samples of the formulation were prepared and placed in 2-oz amber plastic bottles with child-resistant caps and stored at room temperature (23-25 °C). A 1-mL sample was withdrawn from each of the three bottles with a micropipette immediately after preparation and at 7, 14, 28, 57, and 91 days. After double dilution (1:10 and 0.1:5 v/v) to an expected concentration of 10 μg/mL with methanol and mobile phase, respectively, the samples were assayed in duplicate using stability-indicating high-performance liquid chromatography. The samples were visually examined for any color change and evaluated for pH changes on each day of analysis. Taste evaluation was performed at the beginning and end of the study. Stability was defined as the retention of at least 90% of the initial concentration. At least 99% of the initial tadalafil concentration remained throughout the 91-day study period. There were no detectable changes in color, odor, taste, and pH, and no visible microbial growth was observed in any sample. An extemporaneously prepared suspension of tadalafil 5 mg/mL in a 1:1 mixture of Ora-Plus and Ora-Sweet was stable for at least 91 days when stored in amber plastic bottles at room temperature.

Stability of extemporaneously prepared rifaximin oral suspensions.

PubMed

Cober, Mary Petrea; Johnson, Cary E; Lee, Jordan; Currie, Kenne

2010-02-15

The stability of extemporaneously prepared rifaximin oral suspensions was studied. An oral suspension of rifaximin 20 mg/mL was prepared by thoroughly grinding six 200-mg tablets of rifaximin in a glass mortar. Thirty milliliters of Ora-Plus and 30 mL of either Ora-Sweet or Ora-Sweet SF were mixed and added to the powder to make a final volume of 60 mL. Three identical samples of each formulation were prepared and placed in 2-oz amber plastic bottles with child-resistant caps and were stored at room temperature (23-25 degrees C). A 1-mL sample was withdrawn from each of the six bottles with a micropipette immediately after preparation and at 7, 15, 30, and 60 days. After further dilution to an expected concentration of 20 microg/mL with mobile phase, the samples were assayed in duplicate using stability-indicating high-performance liquid chromatography. The samples were visually examined for any color change and pH was tested on each day of analysis. Stability was determined by evaluating the percentage of the initial concentration remaining at each time point and defined as retention of at least 90% of the initial concentration of rifaximin. At least 99% of the initial rifaximin remained throughout the 60-day study period in both preparations. There were no detectable changes in color, odor, taste, or pH and no visible microbial growth in any sample. Extemporaneously prepared suspensions of rifaximin 20 mg/mL in 1:1 mixtures of Ora-Plus with either Ora-Sweet or Ora-Sweet SF were stable for at least 60 days when stored in 2-oz amber plastic bottles at room temperature.

β-CD/ATP composite materials for use in dispersive solid-phase extraction to measure (fluoro)quinolone antibiotics in honey samples.

PubMed

Cui, Xiangqian; Zhang, Panjie; Yang, Xiaoling; Yang, Miyi; Zhou, Wenfeng; Zhang, Sanbin; Gao, Haixiang; Lu, Runhua

2015-06-09

A novel sorbent (β-CD/ATP composite) for dispersive solid-phase extraction (d-SPE) prepared by bonding β-cyclodextrin to modified attapulgite via silane coupling was used to determine the concentrations of four (fluoro)quinolones (Qs) in honey samples. The subsequent quantification of the Qs (ciprofloxacin, norfloxacin, ofloxacin, and gatifloxacin) was accomplished using high-performance liquid chromatography (HPLC) with ultraviolet detection after the d-SPE procedure. Parameters that may influence the extraction efficiency, such as type and volume of the eluent, type and amount of the sorbent, times of the vortex and sonication process, and pH of the sample, were investigated using batch and column procedures. The optimal experimental conditions (5 mL sample at pH 3, 4 mg of β-CD/ATP composite as the sorbent, 200 μL of 40% ammonia in methanol as the eluent, with vortex time 60s and sonication time 6 min, and no addition of salt) were obtained from this statistical evaluation. The limits of detection (LODs) were determined to the range from 0.30 to 3.95 μg L(-1). Good recoveries (83.6-88.6%) were obtained under the optimum conditions, and the relative standard deviations (RSDs), which are used to indicate reproducibility, were less than 7.4%. The method was validated with three real honey samples, and the results demonstrated that β-CD/ATP composite possessed a high adsorption capacity for Qs. Although the LODs were slightly higher than expected, this study confirmed the possibility of using cyclodextrin grafted palygorskite in analytical applications. Copyright © 2015 Elsevier B.V. All rights reserved.

Annual Progress Report FY-92. Volume 1

DTIC Science & Technology

1993-01-21

Billups, L Flow Cytom Resh Psychologist 12 0180 CS Hamm, C DCI 7 DESCRIPTION GRADE MOS BRANCH NAME ACTIVITY Kyle Metabolic Unit Nursing Service Supv...3349 Salata, Kalman PhD. Mitogen-Inducible T Suppressor Cell 13 Assay by Flow Cytometry (12/89) 3350 Salata, Kalman PhD. Flow Cytometric Analysis of...17 Immunotherapy (3/90) 3354 Salata, Kalman PhD. Two Way Mixed Lymphocyte Culture: 18 Analysis by Two Color Flow Cytometry (4/90) 3355 Salata, Kalman

Aroma profile design of wine spirits: Multi-objective optimization using response surface methodology.

PubMed

Matias-Guiu, Pau; Rodríguez-Bencomo, Juan José; Pérez-Correa, José R; López, Francisco

2018-04-15

Developing new distillation strategies can help the spirits industry to improve quality, safety and process efficiency. Batch stills equipped with a packed column and an internal partial condenser are an innovative experimental system, allowing a fast and flexible management of the rectification. In this study, the impact of four factors (heart-cut volume, head-cut volume, pH and cooling flow rate of the internal partial condenser during the head-cut fraction) on 18 major volatile compounds of Muscat spirits was optimized using response surface methodology and desirability function approaches. Results have shown that high rectification at the beginning of the heart-cut enhances the overall positive aroma compounds of the product, reducing off-flavor compounds. In contrast, optimum levels of heart-cut volume, head-cut volume and pH factors varied depending on the process goal. Finally, three optimal operational conditions (head off-flavors reduction, flowery terpenic enhancement and fruity ester enhancement) were evaluated by chemical and sensory analysis. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effect of pH on fecal recovery of energy derived from volatile fatty acids.

PubMed

Kien, C L; Liechty, E A

1987-01-01

We assessed the effect of pH on volatilization of short-chain fatty acids during lyophilization. Acetic, propionic, valeric, and butyric acids were added to a fecal homogenate in amounts sufficient to raise the energy density by 18-27%. Fecal homogenate samples were either acidified (pH 2.8-3.2), alkalinized (pH 7.9-8.7), or left unchanged (4.0-4.8) prior to lyophilization and subsequent bomb calorimetry. Alkalinizing the fecal samples prevented the 20% loss of energy derived from each of these volatile fatty acids observed in samples either acidified or without pH adjustment. These data suggest that in energy balance studies involving subjects with active colonic fermentation, fecal samples should be alkalinized prior to lyophilization and bomb calorimetry.

Theory and practice in the electrometric determination of pH in precipitation

NASA Astrophysics Data System (ADS)

Brennan, Carla Jo; Peden, Mark E.

Basic theory and laboratory investigations have been applied to the electrometric determination of pH in precipitation samples in an effort to improve the reliability of the results obtained from these low ionic strength samples. The theoretical problems inherent in the measurement of pH in rain have been examined using natural precipitation samples with varying ionic strengths and pH values. The importance of electrode design and construction has been stressed. The proper choice of electrode can minimize or eliminate problems arising from residual liquid junction potentials, streaming potentials and temperature differences. Reliable pH measurements can be made in precipitation samples using commercially available calibration buffers providing low ionic strength quality control solutions are routinely used to verify electrode and meter performance.

Zero valent Fe-reduced graphene oxide quantum dots as a novel magnetic dispersive solid phase microextraction sorbent for extraction of organophosphorus pesticides in real water and fruit juice samples prior to analysis by gas chromatography-mass spectrometry.

PubMed

Akbarzade, Samaneh; Chamsaz, Mahmoud; Rounaghi, Gholam Hossein; Ghorbani, Mahdi

2018-01-01

A selective and sensitive magnetic dispersive solid-phase microextraction (MDSPME) coupled with gas chromatography-mass spectrometry was developed for extraction and determination of organophosphorus pesticides (Sevin, Fenitrothion, Malathion, Parathion, and Diazinon) in fruit juice and real water samples. Zero valent Fe-reduced graphene oxide quantum dots (rGOQDs@ Fe) as a new and effective sorbent were prepared and applied for extraction of organophosphorus pesticides using MDSPME method. In order to study the performance of this new sorbent, the ability of rGOQDs@ Fe was compared with graphene oxide and magnetic graphene oxide nanocomposite by recovery experiments of the organophosphorus pesticides. Several affecting parameters in the microextraction procedure, including pH of donor phase, donor phase volume, stirring rate, extraction time, and desorption conditions such as the type and volume of solvents and desorption time were thoroughly investigated and optimized. Under the optimal conditions, the method showed a wide linear dynamic range with R-square between 0.9959 and 0.9991. The limit of detections, the intraday and interday relative standard deviations (n = 5) were less than 0.07 ngmL -1 , 4.7, and 8.6%, respectively. The method was successfully applied for extraction and determination of organophosphorus pesticides in real water samples (well, river and tap water) and fruit juice samples (apple and grape juice). The obtained relative recoveries were in the range of 82.9%-113.2% with RSD percentages of less than 5.8% for all the real samples.

Surfactant-enhanced spectrofluorimetric determination of total aflatoxins from wheat samples after magnetic solid-phase extraction using modified Fe3O4 nanoparticles

NASA Astrophysics Data System (ADS)

Manafi, Mohammad Hanif; Allahyari, Mehdi; Pourghazi, Kamyar; Amoli-Diva, Mitra; Taherimaslak, Zohreh

2015-07-01

The extraction and preconcentration of total aflatoxins (including aflatoxin B1, B2, G1, and G2) using magnetic nanoparticles based solid phase extraction (MSPE) followed by surfactant-enhanced spectrofluorimetric detection was proposed. Ethylene glycol bis-mercaptoacetate modified silica coated Fe3O4 nanoparticles as an efficient antibody-free adsorbent was successfully applied to extract aflatoxins from wheat samples. High surface area and strong magnetization properties of magnetic nanoparticles were utilized to achieve high enrichment factor (97), and satisfactory recoveries (92-105%) using only 100 mg of the adsorbent. Furthermore, the fast separation time (less than 10 min) avoids many time-consuming cartridge loading or column-passing procedures accompany with the conventional SPE. In determination step, signal enhancement was performed by formation of Triton X-100 micelles around the analytes in 15% (v/v) acetonitrile-water which dramatically increase the sensitivity of the method. Main factors affecting the extraction efficiency and signal enhancement of the analytes including pH of sample solution, desorption conditions, extraction time, sample volume, adsorbent amount, surfactant concentration and volume and time of micelle formation were evaluated and optimized. Under the optimum conditions, wide linear range of 0.1-50 ng mL-1 with low detection limit of 0.03 ng mL-1 were obtained. The developed method was successfully applied to the extraction and preconcentration of aflatoxins in three commercially available wheat samples and the results were compared with the official AOAC method.

VALIDATION FOR THE PERMANGANATE DIGESTION OF REILLEX HPQ ANION RESIN

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kyser, E.

2009-09-23

The flowsheet for the digestion of Reillex{trademark} HPQ was validated both under the traditional alkaline conditions and under strongly acidic conditions. Due to difficulty in performing a pH adjustment in the large tank where this flowsheet must be performed, the recommended digestion conditions were changed from pH 8-10 to 8 M HNO{sub 3}. Thus, no pH adjustment of the solution is required prior to performing the permanganate addition and digestion and the need to sample the digestion tank to confirm appropriate pH range for digestion may be avoided. Neutralization of the acidic digestion solution will be performed after completion ofmore » the resin digestion cycle. The amount of permanganate required for this type of resin (Reillex{trademark} HPQ) was increased from 1 kg/L resin to 4 kg/L resin to reduce the amount of residual resin solids to a minimal amount (<5%). The length of digestion time at 70 C remains unchanged at 15 hours. These parameters are not optimized but are expected to be adequate for the conditions. The flowsheet generates a significant amount of fine manganese dioxide (MnO{sub 2}) solids (1.71 kg/L resin) and involves the generation of a significant liquid volume due to the low solubility of permanganate. However, since only two batches of resin (40 L each) are expected to be digested, the total waste generated is limited.« less

Treatment of meats with ionising radiations. VIII.—pH, water-binding capacity and proteolysis of irradiated raw beef and pork during storage, and the ATP-ase activity of irradiated rabbit muscle

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lawrie, R. A.; Sharp, J. G.; Bendall, J. R.

1961-11-01

The immediate effects of 5-Mrad ionizing radiation on beef and pork longissimus dorsi muscles were an increase in pH, a decrease in water-holding capacity, in increment in gel-volume for a given pH rise, and in soluble protein, and increased resistance to low- and high-speed homogenization. The indications of cross-binding induced by irradiation were supported by studies of isolated myofibrils from rabbit psoas muscle. Irradiation markedly reduced the syneresis (18 deg , mu = 0.04) and the swelling (0 deg , mu = 0.25) induced by ATP and, to a lesser extent, over-all fibrillar ATP-ase activity (the initial fast phase beingmore » depressed more than the slower second phase of the reaction). On storage (at -20 deg +37 deg pH and water-binding capacity increased generally with increase of temperature. Changes in pH occurred earlier with pork and to a greater extent than with beef. In sterile beef longissimus dorsi (irradiated or unirradiated) there was a decrease in soluble protein during storage for 60-90 days at 37- (indicating denaturation) and lncreases in TCA-soluble nitrogen and tyrosine (indicating proteolysis, which was more marked in unirradiated samples). The absence of soluble hydroxyproline and the presence of clearly marked cross- striations indicated that the autolysis must have involved sarcoplasmic and not fibrillar or connective tissue protein.« less

Automated multisyringe stir bar sorptive extraction using robust montmorillonite/epoxy-coated stir bars.

PubMed

Ghani, Milad; Saraji, Mohammad; Maya, Fernando; Cerdà, Víctor

2016-05-06

Herein we present a simple, rapid and low cost strategy for the preparation of robust stir bar coatings based on the combination of montmorillonite with epoxy resin. The composite stir bar was implemented in a novel automated multisyringe stir bar sorptive extraction system (MS-SBSE), and applied to the extraction of four chlorophenols (4-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol) as model compounds, followed by high performance liquid chromatography-diode array detection. The different experimental parameters of the MS-SBSE, such as sample volume, selection of the desorption solvent, desorption volume, desorption time, sample solution pH, salt effect and extraction time were studied. Under the optimum conditions, the detection limits were between 0.02 and 0.34μgL(-1). Relative standard deviations (RSD) of the method for the analytes at 10μgL(-1) concentration level ranged from 3.5% to 4.1% (as intra-day RSD) and from 3.9% to 4.3% (as inter-day RSD at 50μgL(-1) concentration level). Batch-to-batch reproducibility for three different stir bars was 4.6-5.1%. The enrichment factors were between 30 and 49. In order to investigate the capability of the developed technique for real sample analysis, well water, wastewater and leachates from a solid waste treatment plant were satisfactorily analyzed. Copyright © 2016 Elsevier B.V. All rights reserved.

Sensitive determination of three aconitum alkaloids and their metabolites in human plasma by matrix solid-phase dispersion with vortex-assisted dispersive liquid-liquid microextraction and HPLC with diode array detection.

PubMed

Wang, Xiaozhong; Li, Xuwen; Li, Lanjie; Li, Min; Liu, Ying; Wu, Qian; Li, Peng; Jin, Yongri

2016-05-01

A simple and sensitive method for determination of three aconitum alkaloids and their metabolites in human plasma was developed using matrix solid-phase dispersion combined with vortex-assisted dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection. The plasma sample was directly purified by matrix solid-phase dispersion and the eluate obtained was concentrated and further clarified by vortex-assisted dispersive liquid-liquid microextraction. Some important parameters affecting the extraction efficiency, such as type and amount of dispersing sorbent, type and volume of elution solvent, type and volume of extraction solvent, salt concentration as well as sample solution pH, were investigated in detail. Under optimal conditions, the proposed method has good repeatability and reproducibility with intraday and interday relative standard deviations lower than 5.44 and 5.75%, respectively. The recoveries of the aconitum alkaloids ranged from 73.81 to 101.82%, and the detection limits were achieved within the range of 1.6-2.1 ng/mL. The proposed method offered the advantages of good applicability, sensitivity, simplicity, and feasibility, which makes it suitable for the determination of trace amounts of aconitum alkaloids in human plasma samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous determination of copper, cobalt, and mercury ions in water samples by solid-phase extraction using carbon nanotube sponges as adsorbent after chelating with sodium diethyldithiocarbamate prior to high performance liquid chromatography.

PubMed

Wang, Lei; Zhou, Jia-Bin; Wang, Xia; Wang, Zhen-Hua; Zhao, Ru-Song

2016-06-01

Recently, a sponge-like material called carbon nanotube sponges (CNT sponges) has drawn considerable attention because it can remove large-area oil, nanoparticles, and organic dyes from water. In this paper, the feasibility of CNT sponges as a novel solid-phase extraction (SPE) adsorbent for the enrichment and determination of heavy metal ions (Co(2+), Cu(2+), and Hg(2+)) was investigated for the first time. Sodium diethyldithiocarbamate (DDTC) was used as the chelating agent and high performance liquid chromatography (HPLC) for the final analysis. Important factors which may influence extraction efficiency of SPE were optimized, such as the kind and volume of eluent, volume of DDTC, sample pH, flow rate, etc. Under the optimized conditions, wide range of linearity (0.5-400 μg L(-1)), low limits of detection (0.089~0.690 μg L(-1); 0.018~0.138 μg), and good repeatability (1.27~3.60 %, n = 5) were obtained. The developed method was applied for the analysis of the three metal ions in real water samples, and satisfactory results were achieved. All of these findings demonstrated that CNT sponges will be a good choice for the enrichment and determination of target ions at trace levels in the future.

A simple, sensitive and rapid isocratic reversed-phase high-performance liquid chromatography method for determination and stability study of curcumin in pharmaceutical samples

PubMed Central

Amanolahi, Farjad; Mohammadi, Ali; Kazemi Oskuee, Reza; Nassirli, Hooriyeh; Malaekeh-Nikouei, Bizhan

2017-01-01

Objective: This study was designed to develop and validate a new reversed-phase high-performance liquid chromatography (RP-HPLC) method based on Q2 (R1) International Conference on Harmonization (ICH) guideline for determination of curcumin in pharmaceutical samples. Materials and Methods: The HPLC instrument method was optimized with isocratic elution with acetonitrile: ammonium acetate (45:55, v/v, pH 3.5), C18 column (150 mm×4.6 mm×5 µm particle size) and a flow rate of 1 ml/min in ambient condition and total retention time of 17 min. The volume of injection was set at 20 µl and detection was recorded at 425 nm. The robustness of the method was examined by changing the mobile phase composition, mobile phase pH, and flow rate. Results: The method was validated with respect to precision, accuracy and linearity in a concentration range of 2-100 µg/ml. The limit of detection (LOD) and limit of quantification (LOQ) were 0.25 and 0.5 µg/ml, respectively. The percentage of recovery was 98.9 to 100.5 with relative standard deviation (RSD) < 0.638%. Conclusion: The method was found to be simple, sensitive and rapid for determination of curcumin in pharmaceutical samples and had enough sensitivity to detect degradation product of curcumin produced under photolysis and hydrolysis stress condition. PMID:29062806

Application of mercapto-silica polymerized high internal phase emulsions for the solid-phase extraction and preconcentration of trace lead(II).

PubMed

Su, Rihui; Ruan, Guihua; Chen, Zhengyi; Du, Fuyou; Li, Jianping

2015-12-01

A new class of solid-phase extraction column prepared with grafted mercapto-silica polymerized high internal phase emulsion particles was used for the preconcentration of trace lead. First, mercapto-silica polymerized high internal phase emulsion particles were synthesized by using high internal phase emulsion polymerization and carefully assembled in a polyethylene syringe column. The influences of various parameters including adsorption pH value, adsorption and desorption solvents, flow rate of the adsorption and desorption procedure were optimized, respectively, and the suitable uploading sample volumes, adsorption capacity, and reusability of solid phase extraction column were also investigated. Under the optimum conditions, Pb(2+) could be preconcentrated quantitatively over a wide pH range (2.0-5.0). In the presence of foreign ions, such as Na(+) , K(+) , Ca(2+) , Zn(2+) , Mg(2+) , Cu(2+) , Fe(2+) , Cd(2+) , Cl(-) and NO3 (-) , Pb(2+) could be recovered successfully. The prepared solid-phase extraction column performed with high stability and desirable durability, which allowed more than 100 replicate extractions without measurable changes of performance. The feasibility of the developed method was further validated by the extraction of Pb(2+) in rice samples. At three spiked levels of 40.0, 200 and 800 μg/kg, the average recoveries for Pb(2+) in rice samples ranged from 87.3 to 105.2%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Extraction and purification technologies of total flavonoids from Aconitum tanguticum].

PubMed

Li, Yan-Rong; Yan, Li-Xin; Feng, Wei-Hong; Li, Chun; Wang, Zhi-Min

2014-04-01

To optimize the extraction and purification technologies of total flavonoids from Aconitum tanguticum whole plant. With the content of total flavonoids as index, the optimum extraction conditions for the concentration, volume of alcohol, extracting time and times were selected by orthogonal optimized; Comparing the adsorption quantity (mg/g) and resolution (%), four kinds of macroporous adsorption resins including D101, AB-8, X-5 and XAD-16 were investigated for the enrichment ability of total flavonoids from Aconitum tanguticum; Concentration and pH value of sample, sampling amount, elution solvent and loading and elution velocity for the optimum adsorption resin were determined. The content of total flavonoids in Aconitum tanguticum was about 4.39%; The optimum extraction technique was 70% alcohol reflux extraction for three times,each time for one hour, the ratio of material and liquid was 1:10 (w/v); The optimum purification technology was: using XAD-16 macroporous resin, the initial concentration of total flavonoids of Aconitum tanguticum was 8 mg/mL, the sampling amount was 112 mg/g dry resin, the pH value was 5, the loading velocity was 3 mL/min, the elution solvent was 70% ethanol and the elution velocity was 5 mL/min. Under the optimum conditions, the average content of total flavonoids was raised from 4.39% to 46.19%. The optimum extraction and purification technologies for total flavonoids of Aconitum tanguticum were suitable for industrial production for its simplicity and responsibility.

Multiwalled carbon nanotubes as a sorbent material for the solid phase extraction of lead from urine and subsequent determination by electrothermal atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Peña Crecente, Rosa M.; Lovera, Carlha Gutiérrez; García, Julia Barciela; Méndez, Jennifer Álvarez; Martín, Sagrario García; Latorre, Carlos Herrero

2014-11-01

The determination of lead in urine is a way of monitoring the chemical exposure to this metal. In the present paper, a new method for the Pb determination by electrothermal atomic absorption spectrometry (ETAAS) in urine at low levels has been developed. Lead was separated from the undesirable urine matrix by means of a solid phase extraction (SPE) procedure. Oxidized multiwalled carbon nanotubes have been used as a sorbent material. Lead from urine was retained at pH 4.0 and was quantitatively eluted using a 0.7 M nitric acid solution and was subsequently measured by ETAAS. The effects of parameters that influence the adsorption-elution process (such as pH, eluent volume and concentration, sampling and elution flow rates) and the atomic spectrometry conditions have been studied by means of different factorial design strategies. Under the optimized conditions, the detection and quantification limits obtained were 0.08 and 0.26 μg Pb L- 1, respectively. The results demonstrate the absence of a urine matrix effect and this is the consequence of the SPE process carried out. Therefore, the developed method is useful for the analysis of Pb at low levels in real samples without the influence of other urine components. The proposed method was applied to the determination of lead in urine samples of unexposed healthy people and satisfactory results were obtained (in the range 3.64-22.9 μg Pb L- 1).

Crosslinked polymeric ionic liquids as solid-phase microextraction sorbent coatings for high performance liquid chromatography.

PubMed

Yu, Honglian; Merib, Josias; Anderson, Jared L

2016-03-18

Neat crosslinked polymeric ionic liquid (PIL) sorbent coatings for solid-phase microextraction (SPME) compatible with high-performance liquid chromatography (HPLC) are reported for the first time. Six structurally different PILs were crosslinked to nitinol supports and applied for the determination of select pharmaceutical drugs, phenolics, and insecticides. Sampling conditions including sample solution pH, extraction time, desorption solvent, desorption time, and desorption solvent volume were optimized using design of experiment (DOE). The developed PIL sorbent coatings were stable when performing extractions under acidic pH and remained intact in various organic desorption solvents (i.e., methanol, acetonitrile, acetone). The PIL-based sorbent coating polymerized from the IL monomer 1-vinyl-3-(10-hydroxydecyl) imidazolium chloride [VC10OHIM][Cl] and IL crosslinker 1,12-di(3-vinylbenzylimidazolium) dodecane dichloride [(VBIM)2C12] 2[Cl] exhibited superior extraction performance compared to the other studied PILs. The extraction efficiency of pharmaceutical drugs and phenolics increased when the film thickness of the PIL-based sorbent coating was increased while many insecticides were largely unaffected. Satisfactory analytical performance was obtained with limits of detection (LODs) ranging from 0.2 to 2 μg L(-1) for the target analytes. The accuracy of the analytical method was examined by studying the relative recovery of analytes in real water samples, including tap water and lake water, with recoveries varying from 50.2% to 115.9% and from 48.8% to 116.6%, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Scaling impact and shock-compression response for porous materials: Application to planetary formation

NASA Astrophysics Data System (ADS)

Jeanloz, R.

2016-12-01

A thermodynamic model based on the Mie-Grüneisen equation of state does a good job of describing the response of porous materials to impact, so can provide insights into the accretion and cohesion of planetesimals too small to be significantly held together by gravity (e.g., tens of km or less in average diameter). The model identifies an offset in Hugoniot pressure (ΔPH) due to porosity that is found to be in agreement with experimental shock-compression measurements for samples having a wide range of initial porosities. Assuming the Grüneisen parameter (γ) is proportional to volume (γ/V = constant), the relative offset in Hugoniot pressure as a function of initial porosity (φ = 1 - V0/V0por) and compression (η = 1 - V/V0) is ΔPH/PH = γ0 φ/[2(1 - φ) - γ0 (φ + η(1 - φ))] where subscripts 0 and por represent zero-pressure (non-porous) conditions and a porous sample, respectively. This additional thermal pressure at a given volume is due to the extra internal energy and corresponding temperature increase associated with collapsing pores (Fig. 1: near-identical curves for φ = 0.001 and 0.01). This result can be interpreted as indicating that upon collapse individual pores create hot spots with temperatures of order 103-104K above the background, suggesting that impact into an initially porous target can result in cohesion due to partial melting and vaporization. Moreover, the waste heat associated with pore closure far exceeds the dissipation in shock loading of non-porous material, reflecting the ability of a porous target to absorb and dissipate impact energy. The Mie-Grüneisen model along with analysis of waste heat thus provides a scaling for planetesimal impact that might explain how rock and regolith accrete into a gravitationally bound planet. Fig. 1. Porosity-induced anomaly in Hugoniot temperature per unit of porosity, shown as a function of compression for samples with initial porosity φ = 0.001 (green), 0.01 (blue) and 0.1 (gold) assuming values: γ0 = 1.5, thermal expansion coefficient α0 ≈ 10-5 K-1 and a linear shock velocity-particle velocity (US-up) slope s = 1.25. Melting at temperatures of about 103-104 K, and electron excitation at temperatures of 104 K and higher can reduce these calculated values by factors of about 2-3.

RuO2 pH Sensor with Super-Glue-Inspired Reference Electrode

PubMed Central

Wajrak, Magdalena; Alameh, Kamal

2017-01-01

A pH-sensitive RuO2 electrode coated in a commercial cyanoacrylate adhesive typically exhibits very low pH sensitivity, and could be paired with a RuO2 working electrode as a differential type pH sensor. However, such sensors display poor performance in real sample matrices. A pH sensor employing a RuO2 pH-sensitive working electrode and a SiO2-PVB junction-modified RuO2 reference electrode is developed as an alternative high-performance solution. This sensor exhibits a performance similar to that of a commercial glass pH sensor in some common sample matrices, particularly, an excellent pH sensitivity of 55.7 mV/pH, a hysteresis as low as 2.7 mV, and a drift below 2.2 mV/h. The developed sensor structure opens the way towards the development of a simple, cost effective, and robust pH sensor for pH analysis in various sample matrices. PMID:28878182

RuO₂ pH Sensor with Super-Glue-Inspired Reference Electrode.

PubMed

Lonsdale, Wade; Wajrak, Magdalena; Alameh, Kamal

2017-09-06

A pH-sensitive RuO₂ electrode coated in a commercial cyanoacrylate adhesive typically exhibits very low pH sensitivity, and could be paired with a RuO₂ working electrode as a differential type pH sensor. However, such sensors display poor performance in real sample matrices. A pH sensor employing a RuO₂ pH-sensitive working electrode and a SiO₂-PVB junction-modified RuO₂ reference electrode is developed as an alternative high-performance solution. This sensor exhibits a performance similar to that of a commercial glass pH sensor in some common sample matrices, particularly, an excellent pH sensitivity of 55.7 mV/pH, a hysteresis as low as 2.7 mV, and a drift below 2.2 mV/h. The developed sensor structure opens the way towards the development of a simple, cost effective, and robust pH sensor for pH analysis in various sample matrices.

The Limitations of an Exclusively Colloidal View of Protein Solution Hydrodynamics and Rheology

PubMed Central

Sarangapani, Prasad S.; Hudson, Steven D.; Migler, Kalman B.; Pathak, Jai A.

2013-01-01

Proteins are complex macromolecules with dynamic conformations. They are charged like colloids, but unlike colloids, charge is heterogeneously distributed on their surfaces. Here we overturn entrenched doctrine that uncritically treats bovine serum albumin (BSA) as a colloidal hard sphere by elucidating the complex pH and surface hydration-dependence of solution viscosity. We measure the infinite shear viscosity of buffered BSA solutions in a parameter space chosen to tune competing long-range repulsions and short-range attractions (2 mg/mL ≤ [BSA] ≤ 500 mg/mL and 3.0 ≤ pH ≤ 7.4). We account for surface hydration through partial specific volume to define volume fraction and determine that the pH-dependent BSA intrinsic viscosity never equals the classical hard sphere result (2.5). We attempt to fit our data to the colloidal rheology models of Russel, Saville, and Schowalter (RSS) and Krieger-Dougherty (KD), which are each routinely and successfully applied to uniformly charged suspensions and to hard-sphere suspensions, respectively. We discover that the RSS model accurately describes our data at pH 3.0, 4.0, and 5.0, but fails at pH 6.0 and 7.4, due to steeply rising solution viscosity at high concentration. When we implement the KD model with the maximum packing volume fraction as the sole floating parameter while holding the intrinsic viscosity constant, we conclude that the model only succeeds at pH 6.0 and 7.4. These findings lead us to define a minimal framework for models of crowded protein solution viscosity wherein critical protein-specific attributes (namely, conformation, surface hydration, and surface charge distribution) are addressed. PMID:24268154

Seasonal variations in urinary risk factors among patients with nephrolithiasis

NASA Technical Reports Server (NTRS)

Hill, K.; Poindexter, J.; Pak, C. Y.

1991-01-01

Twenty-four hour urine specimens from 5,677 stone-forming patients throughout the United States were analyzed for seasonal variations in urinary risk factors for nephrolithiasis. Determinations were performed for urine volume, pH, calcium, oxalate, phosphorus, sodium, magnesium, citrate, sulfate, uric acid, and the relative supersaturation (RS) of calcium oxalate, brushite, monosodium urate, and uric acid. Criteria for significant seasonal variation included a significant difference in monthly means of risk factors, seasonal grouping of the data by the Student-Newman-Keuls multiple range test, consistent year-to-year trends and a physiologically significant range. Minimum urine volume of 1.54 +/- 0.70 SD L/day occurred in October while a maximum urine volume of 1.76 +/- 0.78 SD L/day was observed during February. Minimum urine pH of 5.94 +/- 0.64 SD was observed during July and August while a maximum pH of 6.18 +/- 0.61 SD was observed during February. Daily urinary excretion of sodium was lowest during August, 158 +/- 74 SD mEq/day and highest during February 177 +/- 70 SD mEq/day. The RS of brushite and uric acid were found to display significant pH-dependent seasonal variation with a maximum RS of uric acid 2.26 +/- 1.98 SD in June and a low of 1.48 +/- 1.30 SD in February. Maximum RS of brushite 2.75 +/- 2.58 was observed during February. Minimum RS of brushite 1.93 +/- 1.70 SD was observed in June. Phosphorus excretion displayed seasonal variation about a spring-fall axis with a maximum value 1042 +/- 373 SD mg/day in April and a minimum value of 895 +/- 289 SD mg/day. Urine volume, sodium, and pH were significantly lower during the summer (June, July, August) than in the winter (December, January, February). The RS of uric acid was higher, but that of brushite and monosodium urate was lower in the summer than in the winter. The seasonal changes observed in urine volume, pH, sodium, and the RS of brushite and uric acid are consistent with summertime sweating and increased physical activity. Seasonal variations in phosphorus excretion are probably dietary in origin. The summertime was characterized by an increased propensity for the crystallization of uric acid but not of calcium oxalate or calcium phosphate.

A geochemical module for "AMDTreat" to compute caustic quantity, effluent quantity, and sludge volume

USGS Publications Warehouse

Cravotta, Charles A.; Parkhurst, David L.; Means, Brent P; McKenzie, Bob; Morris, Harry; Arthur, Bill

2010-01-01

Treatment with caustic chemicals typically is used to increase pH and decrease concentrations of dissolved aluminum, iron, and/or manganese in largevolume, metal-laden discharges from active coal mines. Generally, aluminum and iron can be removed effectively at near-neutral pH (6 to 8), whereas active manganese removal requires treatment to alkaline pH (~10). The treatment cost depends on the specific chemical used (NaOH, CaO, Ca(OH)2, Na2CO3, or NH3) and increases with the quantities of chemical added and sludge produced. The pH and metals concentrations do not change linearly with the amount of chemical added. Consequently, the amount of caustic chemical needed to achieve a target pH and the corresponding effluent composition and sludge volume can not be accurately determined without empirical titration data or the application of geochemical models to simulate the titration of the discharge water with caustic chemical(s). The AMDTreat computer program (http://amd.osmre.gov/ ) is widely used to compute costs for treatment of coal-mine drainage. Although AMDTreat can use results of empirical titration with industrial grade caustic chemicals to compute chemical costs for treatment of net-acidic or net-alkaline mine drainage, such data are rarely available. To improve the capability of AMDTreat to estimate (1) the quantity and cost of caustic chemicals to attain a target pH, (2) the concentrations of dissolved metals in treated effluent, and (3) the volume of sludge produced by the treatment, a titration simulation is being developed using the geochemical program PHREEQC (wwwbrr.cr.usgs.gov/projects/GWC_coupled/phreeqc/) that will be coupled as a module to AMDTreat. The simulated titration results can be compared with or used in place of empirical titration data to estimate chemical quantities and costs. This paper describes the development, evaluation, and potential utilization of the PHREEQC titration module for AMDTreat.

Hydrogen ion dynamics in human red blood cells

PubMed Central

Swietach, Pawel; Tiffert, Teresa; Mauritz, Jakob M A; Seear, Rachel; Esposito, Alessandro; Kaminski, Clemens F; Lew, Virgilio L; Vaughan-Jones, Richard D

2010-01-01

Our understanding of pH regulation within red blood cells (RBCs) has been inferred mainly from indirect experiments rather than from in situ measurements of intracellular pH (pHi). The present work shows that carboxy-SNARF-1, a pH fluorophore, when used with confocal imaging or flow cytometry, reliably reports pHi in individual, human RBCs, provided intracellular fluorescence is calibrated using a ‘null-point’ procedure. Mean pHi was 7.25 in CO2/HCO3−-buffered medium and 7.15 in Hepes-buffered medium, and varied linearly with extracellular pH (slope of 0.77). Intrinsic (non-CO2/HCO3−-dependent) buffering power, estimated in the intact cell (85 mmol (l cell)−1 (pH unit)−1 at resting pHi), was somewhat higher than previous estimates from cell lysates (50–70 mmol (l cell)−1 (pH unit)−1). Acute displacement of pHi (superfusion of weak acids/bases) triggered rapid pHi recovery. This was mediated via membrane Cl−/HCO3− exchange (the AE1 gene product), irrespective of whether recovery was from an intracellular acid or base load, and with no evident contribution from other transporters such as Na+/H+ exchange. H+-equivalent flux through AE1 was a linear function of [H+]i and reversed at resting pHi, indicating that its activity is not allosterically regulated by pHi, in contrast to other AE isoforms. By simultaneously monitoring pHi and markers of cell volume, a functional link between membrane ion transport, volume and pHi was demonstrated. RBC pHi is therefore tightly regulated via AE1 activity, but modulated during changes of cell volume. A comparable volume–pHi link may also be important in other cell types expressing anion exchangers. Direct measurement of pHi should be useful in future investigations of RBC physiology and pathology. PMID:20962000

Adsorption by and artificial release of zinc and lead from porous concrete for recycling of adsorbed zinc and lead and of porous concrete to reduce urban non-point heavy metal runoff.

PubMed

Harada, Shigeki; Yanbe, Miyu

2018-04-01

This report describes the use of porous concrete at the bottom of a sewage trap to prevent runoff of non-point heavy metals into receiving waters, and, secondarily, to reduce total runoff volume during heavy rains in urbanized areas while simultaneously increasing the recharge volume of heavy-metal-free water into underground aquifers. This idea has the advantage of preventing clogging, which is fundamentally very important when using pervious materials. During actual field experiments, two important parameters were identified: maximum adsorption weight of lead and zinc by the volume of porous concrete, and heavy metal recovery rate by artificial acidification after adsorption. To understand the effect of ambient heavy metal concentration, a simple mixing system was used to adjust the concentrations of lead and zinc solutions. The concrete blocks used had been prepared for a previous study by Harada & Komuro (2010). The results showed that maximum adsorption depended on the ambient concentration, expressed as the linear isothermal theory, and that recovery depended on the final pH value (0.5 or 0.0). The dependence on pH is very important for recycling the porous concrete. A pH of 0.5 is important for recycling both heavy metals, especially zinc, (8.0-22.1% of lead and 42-74% of zinc) and porous concrete because porous concrete has not been heavily damaged by acid. However, at a pH of 0.0, the heavy metals could be recovered: 30-60% of the lead and 75-125% of the zinc. At a higher pH, such as 2.0, no release of heavy metals occurred, indicating the safety to the environment of using porous concrete, because the lowest recorded pH of rainfall in Japan is. 4.0. Copyright © 2018 Elsevier Ltd. All rights reserved.

Use of marker ion and cationic surfactant plastic membrane electrode for potentiometric titration of cationic polyelectrolytes.

PubMed

Masadome, Takashi; Imato, Toshihiko

2003-07-04

A plasticized poly (vinyl chloride) (PVC) membrane electrode sensitive to stearyltrimethylammonium (STA) ion is applied to the determination of cationic polyelectrolytes such as poly (diallyldimethylammonium chloride) (Cat-floc) by potentiometric titration, using a potassium poly (vinyl sulfate) (PVSK) solution as a titrant. The end-point of the titration is detected as the potential change of the plasticized PVC membrane electrode caused by decrease in the concentration of STA ion added to the sample solution as a marker ion due to the ion association reaction between the STA ion and PVSK. The effects of the concentration of STA ion, coexisting electrolytes in the sample solution and pH of the sample on the degree of the potential change at the end-point were examined. A linear relationship between the concentration of cationic polyelectrolyte and the end-point volume of the titrant exists in the concentration range from 2x10(-5) to 4x10(-4) N for Cat-floc, glycol chitosan, and methylglycol chitosan.

Solidified Floating Organic Drop Microextraction for the Detection of Trace Amount of Lead in Various Samples by Electrothermal Atomic Absorption Spectrometry.

PubMed

Aydın Urucu, Oya; Dönmez, Şeyda; Kök Yetimoğlu, Ece

2017-01-01

A novel method was developed for determination of trace amounts of lead in water and food samples. Solidified floating organic drop microextraction was used to preconcentrate the lead ion. After the analyte was complexed with 1-(2-pyridylazo)-2-naphthol, undecanol and acetonitrile were added as extraction and dispersive solvent, respectively. Variables such as pH, volumes of extraction and dispersive solvents, and concentration of chelating agent were optimized. Under the optimum conditions, the detection limit of Pb (II) was determined as 0.042  µ g L -1 with an enrichment factor of 300. The relative standard deviation is <10%. Accuracy of the developed procedure was evaluated by the analysis of certified reference material of human hair (NCS DC 73347) and wastewater (SPS-WW2) with satisfactory results. The developed procedure was then successfully applied to biscuit and water samples for detection of Pb (II) ions.

Development and validation of a magnetic solid-phase extraction with high-performance liquid chromatography method for the simultaneous determination of amphetamine and methadone in urine.

PubMed

Taghvimi, Arezou; Hamishehkar, Hamed; Ebrahimi, Mahmoud

2016-06-01

The simultaneous determination of amphetamine and methadone was carried out by magnetic graphene oxide nanoparticles, a magnetic solid-phase extraction adsorbent, as a new sample treatment technique. The main factors (the amounts of sample volume, amount of adsorbent, type and amount of extraction organic solvent, time of extraction and desorption, pH, the ionic strength of extraction medium, and agitation rate) influencing the extraction efficiency were investigated and optimized. Under the optimized conditions, good linearity was observed in the range of 100-1500 ng/mL for amphetamine and 100-1000 ng/mL for methadone. The method was evaluated for determination of AM and methadone in positive urine samples, satisfactory results were obtained, therefore magnetic solid-phase extraction can be applied as a novel method for the determination of drugs of abuse in forensic laboratories. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Novel magnetic hollow zein nanoparticles for preconcentration of chlorpyrifos from water and soil samples prior to analysis via high-performance liquid chromatography (HPLC).

PubMed

Rahimi Moghadam, Mojtaba; Zargar, Behrooz; Rastegarzadeh, Saadat

2018-04-30

Herein, magnetically hollow zein nanoparticles were synthesized and used as a magnetic sorbent for the preconcentration of chlorpyrifos and its analysis by high-performance liquid chromatography (HPLC). Morphology of the sorbent was characterized by transmission electron microscopy (TEM). In this study, the effects of important parameters such as pH of the solution, adsorption and desorption time, type and volume of desorption solvent, and salt addition were investigated. Under optimized experimental conditions, the linear range was from 50 to 2000 μg mL-1, and an LOD of 25 μg L-1 was calculated. The relative standard deviations (RSD) varied from 3.8 to 5.1% (n = 5). The enrichment factors for 50 and 100 μg L-1 samples were calculated as 187 and 210, respectively. The developed method was successfully applied in soil and water samples and showed good extraction recoveries.

Polyhydroxybutyrate-b-polyethyleneglycol block copolymer for the solid phase extraction of lead and copper in water, baby foods, tea and coffee samples.

PubMed

Wadhwa, Sham Kumar; Tuzen, Mustafa; Kazi, Tasneem Gul; Soylak, Mustafa; Hazer, Baki

2014-01-01

A new adsorbent, polyhydroxybutyrate-b-polyethyleneglycol, was used for the separation and preconcentration of copper(II) and lead(II) ions prior to their flame atomic absorption spectrometric detections. The influences of parameters such as pH, amount of adsorbent, flow rates and sample volumes were investigated. The polymer does not interact with alkaline, alkaline-earth metals and transition metals. The enrichment factor was 50. The detection limits were 0.32 μg L(-1) and 1.82 μg L(-1) for copper and lead, respectively. The recovery values were found >95%. The relative standard deviations were found to be less than 6%. The validation of the procedure was performed by analysing certified reference materials; NIST SRM 1515 Apple leaves, IAEA-336 Lichen and GBW-07605 Tea. The method was successfully applied for the analysis of analytes in water and food samples. Copyright © 2013 Elsevier Ltd. All rights reserved.

Development of a rapid and sensitive method combining a cellulose ester microfilter and a real-time quantitative PCR assay to detect Campylobacter jejuni and Campylobacter coli in 20 liters of drinking water or low-turbidity waters.

PubMed

Tissier, Adeline; Denis, Martine; Hartemann, Philippe; Gassilloud, Benoît

2012-02-01

Investigations of Campylobacter jejuni and Campylobacter coli in samples of drinking water suspected of being at the origin of an outbreak very often lead to negative results. One of the reasons for this failure is the small volume of water typically used for detecting these pathogens (10 to 1,000 ml). The efficiencies of three microfilters and different elution procedures were determined using real-time quantitative PCR to propose a procedure allowing detection of Campylobacter in 20 liters of drinking water or low-turbidity water samples. The results showed that more than 80% of the bacteria inoculated in 1 liter of drinking water were retained on each microfilter. An elution with a solution containing 3% beef extract, 0.05 M glycine at pH 9, combined with direct extraction of the bacterial genomes retained on the cellulose ester microfilter, allowed recovery of 87.3% (±22% [standard deviation]) of Campylobacter per 1 liter of tap water. Recoveries obtained from 20-liter volumes of tap water spiked with a C. coli strain were 69.5% (±10.3%) and 78.5% (±15.1%) for 91 CFU and 36 CFU, respectively. Finally, tests performed on eight samples of 20 liters of groundwater collected from an alluvial well used for the production of drinking water revealed the presence of C. jejuni and C. coli genomes, whereas no bacteria were detected with the normative culture method in volumes ranging from 10 to 1,000 ml. In the absence of available epidemiological data and information on bacterial viability, these last results indicate only that the water resource is not protected from contamination by Campylobacter.

Development of a Rapid and Sensitive Method Combining a Cellulose Ester Microfilter and a Real-Time Quantitative PCR Assay To Detect Campylobacter jejuni and Campylobacter coli in 20 Liters of Drinking Water or Low-Turbidity Waters

PubMed Central

Tissier, Adeline; Denis, Martine; Hartemann, Philippe

2012-01-01

Investigations of Campylobacter jejuni and Campylobacter coli in samples of drinking water suspected of being at the origin of an outbreak very often lead to negative results. One of the reasons for this failure is the small volume of water typically used for detecting these pathogens (10 to 1,000 ml). The efficiencies of three microfilters and different elution procedures were determined using real-time quantitative PCR to propose a procedure allowing detection of Campylobacter in 20 liters of drinking water or low-turbidity water samples. The results showed that more than 80% of the bacteria inoculated in 1 liter of drinking water were retained on each microfilter. An elution with a solution containing 3% beef extract, 0.05 M glycine at pH 9, combined with direct extraction of the bacterial genomes retained on the cellulose ester microfilter, allowed recovery of 87.3% (±22% [standard deviation]) of Campylobacter per 1 liter of tap water. Recoveries obtained from 20-liter volumes of tap water spiked with a C. coli strain were 69.5% (±10.3%) and 78.5% (±15.1%) for 91 CFU and 36 CFU, respectively. Finally, tests performed on eight samples of 20 liters of groundwater collected from an alluvial well used for the production of drinking water revealed the presence of C. jejuni and C. coli genomes, whereas no bacteria were detected with the normative culture method in volumes ranging from 10 to 1,000 ml. In the absence of available epidemiological data and information on bacterial viability, these last results indicate only that the water resource is not protected from contamination by Campylobacter. PMID:22138985

Analysis of drugs of abuse in human plasma using microextraction by packed sorbents and ultra-high-performance liquid chromatography.

PubMed

Fernández, P; González, M; Regenjo, M; Ares, A M; Fernández, A M; Lorenzo, R A; Carro, A M

2017-02-17

A miniaturized and simple method based on digitally programmed microextraction by packed sorbent (eVol ® -MEPS) coupled to ultra-performance liquid chromatography (UPLC) has been developed for quantitative determination of three synthetic cathinones and seven conventional drugs of abuse and metabolites. The influence of several extraction parameters, such as washing and elution solvents were tested. In addition important variables affecting MEPS performance, namely sample volume, sorbent drying time, washing solvent volume, elution volume, number of extraction cycles, sorbent phase and pH, were evaluated using an asymmetrical screening design. The optimal experimental conditions involved 300μL of plasma, loading 10×100μL of sample through a C8/SCX sorbent in a MEPS syringe placed in the semi-automatic eVol ® system, washing using 150μL H 2 O:MeOH (90:10, v/v), drying for 0.5min and elution using 200μL dichloromethane:2-propanol:ammonium hydroxide (78:20:2, v/v/v). The drugs separation was achieved using an ACQUITY BEH Shield RP18 column (2.1mm×100mm×1.7μm) in 3min. Under optimized conditions the proposed method was validated in terms of selectivity, linearity, limits of detection (LOD) and quantitation (LOQ), precision and matrix effect, using standard addition calibration. The combination of MEPS and UPLC provides a method for the primary screening of the analytes in 18min with excellent recoveries at three concentration levels, ranging between 80 and 104% (relative standard deviation <11%). The developed methodology has been successfully applied to plasma samples from polydrug abusers. Copyright © 2017 Elsevier B.V. All rights reserved.

[Pharmacological and mechanical support of the myocardium in perioperative period in cardio-surgical patients with chronic heart failure].

PubMed

Babaev, M A; Eremenko, A A; Ziuliaeva, T P; Fedulova, S V; Molochnikov, I O; Fominykh, M V; Poliakova, P V; Dzemeshkevich, S L

2014-01-01

The article deals with a retrospective study devoted to the combined methods of myocardial support in cardiosurgical patients with chronic heart failure (III-IY FC according to NYHA) and low myocardial reserves capacity (LVEF 28.3 +/- 9.4%). This methods include pharmacologic (Levosimendan) and mechanical support (IABP). During the work we have analyzed data of 116 patients and measured pressure in the pulmonary artery (mmHg), end-systolic volume (ESV ml), end-diastolic volume (ED, ml), stroke volume output (SVO, ml), left ventricular ejection fraction (LVEF, %). We evaluated the level of valvular insufficiency and pulmonary hypertension (PH) and BNP concentration (pg/ml). The following indications for the usage of pharmacological and/or mechanical myocardial support were identified: I) Preventive usage of pharmacological and/or mechanical myocardial support is recommended for patients with CHF III-IY FC (NYHA) and low left ventricular EF(< or = 35%), significant valvular insufficiency, PH, PICS (postinfarction cardiosclerosis); 2) The certain method of the support can be chosen with the help of Levosimendan infusion testing; 3) In case one of the above mentioned indications (point 1) or in case of mild reaction to levosimendan infusion in patients with the lesions of more than 2 coronary arteries (including the trunk of the left coronary artery) the usage of combined support is recommended; 4) In case of < or = 6 scores according to EUROSCORE scale, lesions of 2 or more coronary arteries, tricuspid insufficiency (TriI), PH, and high pressure in pulmonary artery (higher than the 2nd degree), high end-diastolic volume, end-systolic volume of LV the isolated usage of levosimendan is recommended; 5) In case of significant ischemic heart disease, PICS, lesions of more than 2 coronary arteries, (including the trunk of the left coronary artery) but without significant decrease of pressure in the pulmonary artery, end-diastolic volume, end-systolic volume and TriI the isolated usage of IABP is recommended.

Intrapartum fetal scalp lactate sampling for fetal assessment in the presence of a non-reassuring fetal heart rate trace.

PubMed

East, Christine E; Leader, Leo R; Sheehan, Penelope; Henshall, Naomi E; Colditz, Paul B; Lau, Rosalind

2015-05-01

Fetal scalp blood sampling for lactate estimation may be considered following identification of an abnormal or non-reassuring fetal heart rate pattern. The smaller volume of blood required for this test, compared with the more traditional pH estimation, may improve sampling rates. The appropriate use of this practice mandates systematic review of its safety and clinical effectiveness prior to widespread introduction. To evaluate the effectiveness and risks of fetal scalp lactate sampling in the assessment of fetal well-being during labour, compared with no testing or alternative testing. We searched the Cochrane Pregnancy and Childbirth Group's Trials Register (31 January 2015). All published and unpublished randomised and quasi-randomised trials that compared fetal scalp lactate testing with no testing or alternative testing to evaluate fetal status in the presence of a non-reassuring cardiotocograph during labour. We used the standard methodological procedures of the Cochrane Pregnancy and Childbirth Group. Two review authors independently assessed the studies. The search identified two completed randomised controlled trials (RCTs) and two ongoing trials. The two published RCTs considered outcomes for 3348 mother-baby pairs allocated to either lactate or pH estimation of fetal blood samples when clinically indicated in labour. Overall, the published RCTs were of low or unclear risk of bias. There was a high risk of performance bias, because it would not have been feasible to blind clinicians or participants.No statistically significant between-group differences were found for neonatal encephalopathy (risk ratio (RR) 1.00, 95% confidence interval (CI) 0.32 to 3.09, one study, 2992 infants) or death. No studies reported neonatal seizures. We had planned to report death with other morbidities, for example, neonatal encephalopathy; however, the data were not available in a format suitable for this, therefore death due to congenital abnormality was considered alone. The three reported neonatal deaths occurred in babies with diaphragmatic hernias (n = 2) or congenital cardiac fibrosis (n = 1). All three babies had been randomised to the pH group and were not acidaemic at birth.There were no statistically significant differences for any of the pre-specified secondary fetal/neonatal/infant outcomes for which data were available. This included low Apgar score at five minutes (RR 1.13, 95% CI 0.76 to 1.68, two studies, 3319 infants) and admission to neonatal intensive care units (RR 1.02, 95% CI 0.83 to 1.25, one study, 2992 infants), or metabolic acidaemia (RR 0.91, 95% CI 0.60 to 1.36, one study, 2675 infants) considered within the studies, either overall or where data were available for those where fetal blood sampling had occurred within 60 minutes of delivery.Similar proportions of fetuses underwent additional tests to further evaluate well-being during labour, including scalp pH if in the lactate group or scalp lactate if in the pH group (RR 0.22, 95% CI 0.04 to 1.30, two studies, 3333 infants;Tau² 1.00, I² = 58%). Fetal blood sampling attempts for lactate and pH estimation were successful in 98.7% and 79.4% of procedures respectively in the one study that reported this outcome.There were no significant between-group differences in mode of birth or operative birth for non-reassuring fetal status, either for all women, or within the group where the fetal blood sample had been taken within 60 minutes of delivery (for example, caesarean section for all enrolled, RR 1.09, 95% CI 0.97 to 1.22, two studies, 3319 women; operative delivery for non-reassuring fetal status for all enrolled RR 1.02, 95% CI 0.93 to 1.11, one study, 2992 women).Neither study reported on adverse effects of fetal scalp lacerations or maternal anxiety. When further testing to assess fetal well-being in labour is indicated, fetal scalp blood lactate estimation is more likely to be successfully undertaken than pH estimation. Further studies may consider subgroup analysis by gestational age, the stage of labour and sampling within a prolonged second stage of labour. Additionally, we await the findings from the ongoing studies that compare allocation to no fetal blood sample with sampling for lactate and address longer-term neonatal outcomes, maternal satisfaction with intrapartum fetal monitoring and an economic analysis.

Novel Palm Fatty Acid Functionalized Magnetite Nanoparticles for Magnetic Solid-Phase Extraction of Trace Polycyclic Aromatic Hydrocarbons from Environmental Samples.

PubMed

Rozi, Siti Khalijah Mahmad; Nodeh, Hamid Rashidi; Kamboh, Muhammad Afzal; Manan, Ninie Suhana Abdul; Mohamad, Sharifah

2017-07-01

A novel adsorbent, palm fatty acid coated magnetic Fe 3 O 4 nanoparticles (MNP-FA) was successfully synthesized with immobilization of the palm fatty acid onto the surface of MNPs. The successful synthesis of MNP-FA was further confirmed by X-Ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR) and Energy dispersive X-Ray spectroscopy (EDX) analyses and water contact angle (WCA) measurement. This newly synthesized MNP-FA was applied as magnetic solid phase extraction (MSPE) adsorbent for the enrichment of polycyclic aromatic hydrocarbons (PAHs), namely fluoranthene (FLT), pyrene (Pyr), chrysene (Cry) and benzo(a)pyrene (BaP) from environmental samples prior to High Performance Liquid Chromatography- Diode Array Detector (HPLC-DAD) analysis. The MSPE method was optimized by several parameters such as amount of sorbent, desorption solvent, volume of desorption solvent, extraction time, desorption time, pH and sample volume. Under the optimized conditions, MSPE method provided a low detection limit (LOD) for FLT, Pyr, Cry and BaP in the range of 0.01-0.05 ng mL -1 . The PAHs recoveries of the spiked leachate samples ranged from 98.5% to 113.8% with the RSDs (n = 5) ranging from 3.5% to 12.2%, while for the spiked sludge samples, the recoveries ranged from 81.1% to 119.3% with the RSDs (n = 5) ranging from 3.1% to 13.6%. The recyclability study revealed that MNP-FA has excellent reusability up to five times. Chromatrographic analysis demonstrated the suitability of MNP-FA as MSPE adsorbent for the efficient extraction of PAHs from environmental samples.

Solid phase microextraction Arrow for the sampling of volatile amines in wastewater and atmosphere.

PubMed

Helin, Aku; Rönkkö, Tuukka; Parshintsev, Jevgeni; Hartonen, Kari; Schilling, Beat; Läubli, Thomas; Riekkola, Marja-Liisa

2015-12-24

A new method is introduced for the sampling of volatile low molecular weight alkylamines in ambient air and wastewater by utilizing a novel SPME Arrow system, which contains a larger volume of sorbent compared to a standard SPME fiber. Parameters affecting the extraction, such as coating material, need for preconcentration, sample volume, pH, stirring rate, salt addition, extraction time and temperature were carefully optimized. In addition, analysis conditions, including desorption temperature and time as well as gas chromatographic parameters, were optimized. Compared to conventional SPME fiber, the SPME Arrow had better robustness and sensitivity. Average intermediate reproducibility of the method expressed as relative standard deviation was 12% for dimethylamine and 14% for trimethylamine, and their limit of quantification 10μg/L and 0.13μg/L respectively. Working range was from limits of quantification to 500μg/L for dimethylamine and to 130μg/L for trimethylamine. Several alkylamines were qualitatively analyzed in real samples, while target compounds dimethyl- and trimethylamines were quantified. The concentrations in influent and effluent wastewater samples were almost the same (∼80μg/L for dimethylamine, 120μg/L for trimethylamine) meaning that amines pass the water purification process unchanged or they are produced at the same rate as they are removed. For the air samples, preconcentration with phosphoric acid coated denuder was required and the concentration of trimethylamine was found to be around 1ng/m(3). The developed method was compared with optimized method based on conventional SPME and advantages and disadvantages of both approaches are discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

Chromium speciation in environmental samples using a solid phase spectrophotometric method

NASA Astrophysics Data System (ADS)

Amin, Alaa S.; Kassem, Mohammed A.

2012-10-01

A solid phase extraction technique is proposed for preconcentration and speciation of chromium in natural waters using spectrophotometric analysis. The procedure is based on sorption of chromium(III) as 4-(2-benzothiazolylazo)2,2'-biphenyldiol complex on dextran-type anion-exchange gel (Sephadex DEAE A-25). After reduction of Cr(VI) by 0.5 ml of 96% concentrated H2SO4 and ethanol, the system was applied to the total chromium. The concentration of Cr(VI) was calculated as the difference between the total Cr and the Cr(III) content. The influences of some analytical parameters such as: pH of the aqueous solution, amounts of 4-(2-benzothiazolylazo)2,2'-biphenyldiol (BTABD), and sample volumes were investigated. The absorbance of the gel, at 628 and 750 nm, packed in a 1.0 mm cell, is measured directly. The molar absorptivities were found to be 2.11 × 107 and 3.90 × 107 L mol-1 cm-1 for 500 and 1000 ml, respectively. Calibration is linear over the range 0.05-1.45 μg L-1 with RSD of <1.85% (n = 8.0). Using 35 mg exchanger, the detection and quantification limits were 13 and 44 ng L-1 for 500 ml sample, whereas for 1000 ml sample were 8.0 and 27 ng L-1, respectively. Increasing the sample volume can enhance the sensitivity. No considerable interferences have been observed from other investigated anions and cations on the chromium speciation. The proposed method was applied to the speciation of chromium in natural waters and total chromium preconcentration in microwave digested tobacco, coffee, tea, and soil samples. The results were simultaneously compared with those obtained using an ET AAS method, whereby the validity of the method has been tested.

Quality of wet deposition in the Grand Calumet River watershed, northwestern Indiana, June 30, 1992-August 31, 1993

USGS Publications Warehouse

Willoughby, T.C.

1995-01-01

Northwestern Indiana is one of the most heavily industrialized and largest steel-producing areas in the United States. High temperature processes, such as fossil-fuel combustion and steel production, release contaminants to the atmosphere that may result in wet deposition being a major contributor to major ion and trace-metal loadings in north- western Indiana and Lake Michigan. A wet-deposition collection site was established at the Gary (Indiana) Regional Airport in June 1992 to monitor the chemical quality of wet deposition. Weekly samples were collected at this site from June 30, 1992, through August 31, 1993, and were analyzed for pH, specific conductance, and selected major ions and trace metals. Forty-eight samples collected during the study were of sufficient volumes for some of the determinations to be performed. Median constituent concentrations were determined for samples collected during warm weather and cold weather (November 1 through March 31). Median concentrations were substituted for missing values from samples with insufficient volumes for analysis of all the constituents of interest. Constituent concentrations were converted to weekly loadings. Two values were calculated to provide a range for the weekly loading for samples with measured concentrations of constituents less than the method reporting limit. The minimum weekly loading was computed by substituting zero for the constituent concentration; the maximum weekly loading was computed by substituting the method reporting limit for the concentration. If all of the sample concentrations measured were greater than the method reporting limit, an annual loading value was computed. The annual loadings could be used to assist in estimating the contribution of wet deposition to the total annual constituent loadings in the Grand Calumet River in northwestern Indiana.

Ultrasonic-energy enhance the ionic liquid-based dual microextraction to preconcentrate the lead in ground and stored rain water samples as compared to conventional shaking method.

PubMed

Nizamani, Sooraj; Kazi, Tasneem G; Afridi, Hassan I

2018-01-01

An efficient preconcentration technique based on ultrasonic-assisted ionic liquid-based dual microextraction (UA-ILDµE) method has been developed to preconcentrate the lead (Pb +2 ) in ground and stored rain water. In the current proposed method, Pb +2 was complexed with a chelating agent (dithizone), whereas an ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate) was used for extraction purpose. The ultrasonic irradiation and electrical shaking system were applied to enhance the dispersion and extraction of Pb +2 complex in aqueous samples. For second phase, dual microextraction (DµE phase), the enriched Pb +2 complex in ionic liquid, extracted back into the acidic aqueous solution and finally determined by flame atomic absorption spectrometry. Some major analytical parameters that influenced the extraction efficiency of developed method, such as pH, concentration of ligand, volume of ionic liquid and samples, time of shaking in thermostatic electrical shaker and ultrasonic bath, effect of back extracting HNO 3 volume, matrix effect, centrifugation time and rate were optimized. At the sample volume of 25mL, the calculated preconcentration factor was 62.2. The limit of detection of proposed procedure for Pb +2 ions was found to be 0.54μgL -1 . The validation of developed method was performed by the analysis of certified sample of water SRM 1643e and standard addition method in a real water sample. The extraction recovery of Pb +2 was enhanced≥2% with shaking time of 80s in ultrasonic bath as compared to used thermostatic electrical shaker, where for optimum recovery up to 10min was required. The developed procedure was successfully used for the enrichment of Pb +2 in ground and stored rain water (surface water) samples of an endemic region of Pakistan. The resulted data indicated that the ground water samples were highly contaminated with Pb +2 , while some of the surface water samples were also have higher values of Pb +2 than permissible limit of WHO. The concentration of Pb +2 in surface and ground water samples was found in the range of 17.5-24.5 and 25.6-99.1μgL - 1 respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Time dependence of the pH of rain

Treesearch

John A. Kadlecek; Volkar A. Mohnen

1976-01-01

Standard procedures for determining the pH of rain samples usually involve substantial delays from the time of rainfall to the time of analysis. This assumes that no change in pH occurs during the storage period. We have found that this is not always true. We have determined that individual rain water samples possess a time dependent pH which can be correlated with the...

Modeling a CO2 mineralization experiment of fractured peridotite from the Semail ophiolite/ Oman

NASA Astrophysics Data System (ADS)

Muller, Nadja; Zhang, Guoxiang; van Noort, Reinier; Spiers, Chris; Ten Grotenhuis, Saskia; Hoedeman, Gerco

2010-05-01

Most geologic CO2 sequestration technologies focus on sedimentary rocks, where the carbon dioxide is stored in a fluid phase. A possible alternative is to trap it as a mineral in the subsurface (in-situ) in basaltic or even (ultra)mafic rocks. Carbon dioxide in aqueous solution reacts with Mg-, Ca-, and Fe-bearing silicate minerals, precipitates as (MgCa,Fe)CO3 (carbonate), and can thus be permanently sequestered. The cation donors are silicate minerals such as olivine and pyroxene which are abundant in (ultra)mafic rocks, such as peridotite. Investigations are underway to evaluate the sequestration potential of the Semail Ophiolite in Oman, utilizing the large volumes of partially serpentinized peridotite that are present. Key factors are the rate of mineralization due to dissolution of the peridotite and precipitation of carbonate, the extent of the natural and hydraulic fracture network and the accessibility of the rock to reactive fluids. To quantify the influence of dissolution rates on the overall CO2 mineralization process, small, fractured peridotite samples were exposed to supercritical CO2 and water in laboratory experiments. The samples are cored from a large rock sample in the dimension of small cylinders with 1 cm in height and diameter, with a mass of ~2g. Several experimental conditions were tested with different equipment, from large volume autoclave to small volume cold seal vessel. The 650 ml autoclave contained 400-500g of water and a sample under 10 MPa of partial CO2 pressure up to 150. The small capsules in the cold seal vessel held 1-1.5g of water and the sample under CO2 partial pressure from 15MPa to 70 MPa and temperature from 60 to 200°C. The samples remained for two weeks in the reaction vessels. In addition, bench acid bath experiments in 150 ml vials were performed open to the atmosphere at 50-80°C and pH of ~3. The main observation was that the peridotite dissolved two orders of magnitude slower in the high pressure and temperature cell of the cold seal vessel than comparative experiments in large volume autoclaves and bench acid bath vials under lower and atmospheric pressure conditions. We attributed this observation to the limited water availability in the cold seal vessel, limiting the aqueous reaction of bi-carbonate formation and magnesite precipitation. To test this hypothesis, one of the cold seal vessel experiments at 20 MPa and 100°C was simulated with a reactive transport model, using TOUGHREACT. To simulate the actual experimental conditions, the model used a grid on mm and 100's of μm scale and a fractured peridotite medium with serpentine filling the fractures. The simulation produced dissolution comparable to the experiment and showed an effective shut down of the bi-carbonation reaction within one day after the start of the experiment. If the conditions of limited water supply seen in our experiments are applicable in a field setting, we could expect dissolution may be limited by the buffering of the pH and shut down of the bi-carbonate formation. Under field conditions water and CO2 will only flow in hydraulic induced fractures and the natural fracture network that is filled with serpentine and some carbonate. The simulation result and potential implication for the field application will require further experimental investigation in the lab or field in the future.

Evaluation of pH of Bathing Soaps and Shampoos for Skin and Hair Care.

PubMed

Tarun, Jose; Susan, Jose; Suria, Jacob; Susan, Veronica John; Criton, Sebastian

2014-09-01

Normal healthy skin has potential of hydrogen (pH) range of 5.4-5.9 and a normal bacterial flora. Use of soap with high pH causes an increase in skin pH, which in turn causes an increase in dehydrative effect, irritability and alteration in bacterial flora. The majority of soaps and shampoos available in the market do not disclose their pH. The aim of this study was to assess the pH of different brands of bathing soaps and shampoos available in the market. The samples of soaps and shampoos were collected from shops in the locality. The samples of different brands are coded before the analysis of the pH. Solution of each sample was made and pH was measured using pH meter. Majority of the soaps have a pH within the range of 9-10. Majority of the shampoos have a pH within the range of 6-7. The soaps and shampoos commonly used by the population at large have a pH outside the range of normal skin and hair pH values. Therefore, it is hoped that before recommending soap to patient especially those who have sensitive and acne prone skin, due consideration is given to the pH factor and also that manufacturers will give a thought to pH of soaps and shampoos manufactured by them, so that their products will be more skin and hair friendly.

Determination of rhodamine B in soft drink, waste water and lipstick samples after solid phase extraction.

PubMed

Soylak, Mustafa; Unsal, Yunus Emre; Yilmaz, Erkan; Tuzen, Mustafa

2011-08-01

A new solid phase extraction method is described for sensitive and selective determination of trace levels of rhodamine B in soft drink, food and industrial waste water samples. The method is based on the adsorption of rhodamine B on the Sepabeads SP 70 resin and its elution with 5 mL of acetonitrile in a mini chromatographic column. Rhodamine B was determined by using UV visible spectrophotometry at 556 nm. The effects of different parameters such as pH, amount of rhodamine B, flow rates of sample and eluent solutions, resin amount, and sample volume were investigated. The influences of some alkali, alkali earth and transition metals on the recoveries of rhodamine B were investigated. The preconcentration factor was found 40. The detection limit based on three times the standard deviation of the reagent blank for rhodamine B was 3.14 μg L⁻¹. The relative standard deviations of the procedure were found as 5% in 1×10⁻⁵ mol L⁻¹ rhodamine B. The presented procedure was successfully applied to real samples including soft drink, food and industrial waste water and lipstick samples. Copyright © 2011 Elsevier Ltd. All rights reserved.

Excess glycogen does not resolve high ultimate pH of oxidative muscle.

PubMed

England, Eric M; Matarneh, Sulaiman K; Oliver, Emily M; Apaoblaza, Ariel; Scheffler, Tracy L; Shi, Hao; Gerrard, David E

2016-04-01

Skeletal muscle glycogen content can impact the extent of postmortem pH decline. Compared to glycolytic muscles, oxidative muscles contain lower glycogen levels antemortem which may contribute to the higher ultimate pH. In an effort to explore further the participation of glycogen in postmortem metabolism, we postulated that increasing the availability of glycogen would drive additional pH decline in oxidative muscles to equivalent pH values similar to the ultimate pH of glycolytic muscles. Glycolysis and pH declines were compared in porcine longissimus lumborum (glycolytic) and masseter (oxidative) muscles using an in vitro system in the presence of excess glycogen. The ultimate pH of the system containing longissimus lumborum reached a value similar to that observed in intact muscle. The pH decline of the system containing masseter samples stopped prematurely resulting in a higher ultimate pH which was similar to that of intact masseter muscle. To investigate further, we titrated powdered longissimus lumborum and masseter samples in the reaction buffer. As the percentage of glycolytic sample increased, the ultimate pH decreased. These data show that oxidative muscle produces meat with a high ultimate pH regardless of glycogen content and suggest that inherent muscle factors associated with glycolytic muscle control the extent of pH decline in pig muscles. Copyright © 2015 Elsevier Ltd. All rights reserved.

Randomised prospective study compares efficacy of five different stomach tubes for rumen fluid sampling in dairy cows.

PubMed

Steiner, S; Neidl, A; Linhart, N; Tichy, A; Gasteiner, J; Gallob, K; Baumgartner, W; Wittek, T

2015-01-10

The objective of the study was to compare the performance of five types of stomach tubes for rumen fluid sampling. Rumen fluid was sampled in rumen fistulated cows assigned to a 5×5 Latin square study design. The pH values of samples taken by stomach tubes and via fistulas were measured; the results were compared with indwelling sensor measurements. The practicability of the stomach tubes for regular use was tested in the field. Rumen fluid samples were obtained rapidly. Volumes for transfaunation could be obtained. The pH-values of samples taken with the four out of the five tubes (Dirksen, Geishauser, tube 4 and a simple water hose used with a gag) did not show significant differences to samples taken via rumen fistulas. Mean differences ranged between -0.02 and +0.09. Samples taken with tube 4 and the water hose showed also no significant differences to pH-sensor measurements. This study demonstrates that stomach tubes are suitable for rumen fluid sampling. Tube 4 seems to be the best probe for work in the field. It was well tolerated by the animals, saliva contamination is negligible. We, therefore, conclude that the evaluation of rumen acid base status in the field is possible. British Veterinary Association.

Dispersive liquid-phase microextraction with solidification of floating organic droplet coupled with high-performance liquid chromatography for the determination of Sudan dyes in foodstuffs and water samples.

PubMed

Chen, Bo; Huang, Yuming

2014-06-25

Dispersive liquid-phase microextraction with solidification of floating organic drop (SFO-DLPME) is one of the most interesting sample preparation techniques developed in recent years. In this paper, a new, rapid, and efficient SFO-DLPME coupled with high-performance liquid chromatography (HPLC) was established for the extraction and sensitive detection of banned Sudan dyes, namely, Sudan I, Sudan II, Sudan III, and Sudan IV, in foodstuff and water samples. Various factors, such as the type and volume of extractants and dispersants, pH and volume of sample solution, extraction time and temperature, ion strength, and humic acid concentration, were investigated and optimized to achieve optimal extraction of Sudan dyes in one single step. After optimization of extraction conditions using 1-dodecanol as an extractant and ethanol as a dispersant, the developed procedure was applied for extraction of the target Sudan dyes from 2 g of food samples and 10 mL of the spiked water samples. Under the optimized conditions, all Sudan dyes could be easily extracted by the proposed SFO-DLPME method. Limits of detection of the four Sudan dyes obtained were 0.10-0.20 ng g(-1) and 0.03 μg L(-1) when 2 g of foodstuff samples and 10 mL of water samples were adopted, respectively. The inter- and intraday reproducibilities were below 4.8% for analysis of Sudan dyes in foodstuffs. The method was satisfactorily used for the detection of Sudan dyes, and the recoveries of the target for the spiked foodstuff and water samples ranged from 92.6 to 106.6% and from 91.1 to 108.6%, respectively. These results indicated that the proposed method is simple, rapid, sensitive, and suitable for the pre-concentration and detection of the target dyes in foodstuff samples.

Integrin αvβ3 as a Promising Target to Image Neoangiogenesis Using In-House Generator-Produced Positron Emitter (68)Ga-Labeled DOTA-Arginine-Glycine-Aspartic Acid (RGD) Ligand.

PubMed

Vatsa, Rakhee; Bhusari, Priya; Kumar, Sunil; Chakraborty, Sudipta; Dash, Ashutosh; Singh, Gurpreet; Dhawan, Devinder Kumar; Shukla, Jaya; Mittal, Bhagwant Rai

2015-06-01

For the growth and spread of a tumor beyond 2 mm, angiogenesis plays a crucial role, and association of various integrins with angiogenesis is evidential. The aim of the study was radiolabeling of DOTA-chelated RGD (arginine-glycine-aspartic acid) peptide with (68)Ga for PET imaging in locally advanced breast carcinoma. DOTA-RGD was incubated with (68)GaCl3, eluted in 0.05 m HCl. Elution volume, peptide amount, and reaction pH were studied. Radio-ITLC, gas chromatography, endotoxin, and sterility testing were performed. Serial (n=3) and whole-body (n=2) PET/CT imaging was done on patients post i.v. injection of 111-185 MBq of (68)Ga-DOTA-RGD. Maximum radiolabeling yield was achieved with 3 mL elution volume of 15-20 μg peptide at pH 3.5-4.0 with 10 minutes of incubation at 95°C. Product samples were sterile having 99.5% radiochemical purity with residual ethanol content and endotoxins in injectable limits. Intense radiotracer uptake was noticed in the tumor with SUVmax 15.3 at 45 minutes in serial images. Physiological radiotracer uptake was seen in the liver, spleen, ventricles, and thyroid with excretion through the kidneys. The authors concluded that (68)Ga-DOTA-RGD has the potential for imaging α,vβ3 integrin-expressing tumors.

Reperfusion-Associated Hemorrhagic Transformation in SHR Rats

PubMed Central

Henning, Erica C.; Latour, Lawrence L.; Hallenbeck, John M.; Warach, Steven

2016-01-01

Background and Purpose Symptomatic hemorrhagic transformation (HT) is the most important complicating factor after treatment with intravenous tissue plasminogen activator. In this study, we used multimodal magnetic resonance imaging to investigate the incidence and severity of reperfusion-based HT in spontaneously hypertensive rats after ischemia/reperfusion. Methods Twenty male spontaneously hypertensive rats were subjected to 30 minutes of middle cerebral artery occlusion via the suture model. Diffusion-weighted, T2-weighted, and gradient-echo imaging were performed on days 1, 2, 3, 4, and 7 for longitudinal evaluation of lesion evolution, vasogenic edema, and HT, respectively. Findings on gradient-echo images were classified according to the severity of hemorrhage: no HT; punctate or small petechial hemorrhage (HI-1); confluent petechial hemorrhage (HI-2); hematoma with absent/mild space-occupying effect (PH-1, ≤30% lesion volume); and hematoma with significant space-occupying effect and potential perihematomal edema (PH-2, >30% lesion volume). Histopathologic evaluation of HT was performed after final imaging for comparison with magnetic resonance imaging results. Results Final hemorrhage scores based on severity were as follows: HI-1 23.1%, HI-2 30.8%, PH-1 30.8%, and PH-2 15.4%. Similar to clinical observations, only PH-2 was associated with neurologic deterioration and associated weight loss. Conclusions This model has a high incidence of parenchymal hematomas (46.2%) and therefore is appropriate for the evaluation of novel therapeutics targeting blood-brain barrier integrity and the reduction of symptomatic HT events (PH-2), as well as those potentially “at risk” for neurologic deterioration (PH-1). PMID:18757286

Comparison of two thin-film microextractions for the analysis of estrogens in aqueous tea extract and environmental water samples by high performance liquid chromatography-ultraviolet detection.

PubMed

Cai, Pei-Shan; Li, Dan; Chen, Jing; Xiong, Chao-Mei; Ruan, Jin-Lan

2015-04-15

Two thin-film microextractions (TFME), octadecylsilane (ODS)-polyacrylonitrile (PAN)-TFME and polar enhanced phase (PEP)-PAN-TFME have been proposed for the analysis of bisphenol-A, diethylstilbestrol and 17β-estradiol in aqueous tea extract and environmental water samples followed by high performance liquid chromatography-ultraviolet detection. Both thin-films were prepared by spraying. The influencing factors including pH, extraction time, desorption solvent, desorption volume, desorption time, ion strength and reusability were investigated. Under the optimal conditions, the two TFME methods are similar in terms of the analytical performance evaluated by standard addition method. The limits of detection for three estrogens in environmental water and aqueous tea extract matrix ranged from 1.3 to 1.6 and 2.8 to 7.1 ng mL(-1) by the two TFME methods, respectively. Both approaches were applied for the analysis of analytes in real aqueous tea extract and environmental water samples, presenting satisfactory recoveries ranged from 87.3% to 109.4% for the spiked samples. Copyright © 2014 Elsevier Ltd. All rights reserved.

An innovative method for analysis of Pb (II) in rice, milk and water samples based on TiO2 reinforced caprylic acid hollow fiber solid/liquid phase microextraction.

PubMed

Bahar, Shahriyar; Es'haghi, Zarrin; Nezhadali, Azizollah; Banaei, Alireza; Bohlooli, Shahab

2017-04-15

In the present study, nano-sized titanium oxides were applied for preconcentration and determination of Pb(II) in aqueous samples using hollow fiber based solid-liquid phase microextraction (HF-SLPME) combined with flame atomic absorption spectrometry (FAAS). In this work, the nanoparticles dispersed in caprylic acid as an extraction solvent was placed into a polypropylene porous hollow fiber segment supported by capillary forces and sonification. This membrane was in direct contact with solutions containing Pb (II). The effect of experimental conditions on the extraction, such as pH, stirring rate, sample volume, and extraction time were optimized. Under the optimal conditions, the performance of the proposed method was investigated for the determination of Pb (II) in food and water samples. The method was linear in the range of 0.6-3000μgmL -1 . The relative standard deviations and relative recovery of Pb (II) was 4.9% and 99.3%, respectively (n=5). Copyright © 2016 Elsevier Ltd. All rights reserved.

Column preconcentration and electrothermal atomic absorption spectrometric determination of rhodium in some food and standard samples.

PubMed

Taher, Mohammad Ali; Pourmohammad, Fatemeh; Fazelirad, Hamid

2015-12-01

In the present work, an electrothermal atomic absorption spectrometric method has been developed for the determination of ultra-trace amounts of rhodium after adsorption of its 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol/tetraphenylborate ion associated complex at the surface of alumina. Several factors affecting the extraction efficiency such as the pH, type of eluent, sample and eluent flow rates, sorption capacity of alumina and sample volume were investigated and optimized. The relative standard deviation for eight measurements of 0.1 ng/mL of rhodium was ±6.3%. In this method, the detection limit was 0.003 ng/mL in the original solution. The sorption capacity of alumina and the linear range for Rh(III) were evaluated as 0.8 mg/g and 0.015-0.45 ng/mL in the original solution, respectively. The proposed method was successfully applied for the extraction and determination of rhodium content in some food and standard samples with high recovery values. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Micellar electrokinetic chromatographic determination of triazine herbicides in water samples.

PubMed

Li, Zhi; Zhang, Shuaihua; Yin, Xiaofang; Wang, Chun; Wang, Zhi

2014-09-01

Dispersive liquid-liquid microextraction combined with online sweeping preconcentration in micellar electrokinetic chromatography was developed for the simultaneous determination of five triazine herbicides (atrazine, simazine, propazine, prometon and simetryn) in water samples. Several experimental parameters affecting the extraction efficiencies such as the type and volume of both the extraction and dispersive solvents, the addition of salt to sample solution, the extraction time and the pH of the sample solution were investigated. Under optimum conditions, the linearity of the method was good in the range from 0.33 to 20 ng mL(-1) for simazine, propazine, atrazine and simetryn, and from 0.17 to 20 ng mL(-1) for prometon, respectively. The sensitivity enrichment factors were in the range from 1750 to 2100, depending on the compound. The limit of detection (S/N = 3) ranged from 0.05 to 0.10 ng mL(-1). The developed method was successfully applied to the analysis of the five triazines in river, ground and well waters. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Application of Chitosan-Zinc Oxide Nanoparticles for Lead Extraction From Water Samples by Combining Ant Colony Optimization with Artificial Neural Network

NASA Astrophysics Data System (ADS)

Khajeh, M.; Pourkarami, A.; Arefnejad, E.; Bohlooli, M.; Khatibi, A.; Ghaffari-Moghaddam, M.; Zareian-Jahromi, S.

2017-09-01

Chitosan-zinc oxide nanoparticles (CZPs) were developed for solid-phase extraction. Combined artificial neural network-ant colony optimization (ANN-ACO) was used for the simultaneous preconcentration and determination of lead (Pb2+) ions in water samples prior to graphite furnace atomic absorption spectrometry (GF AAS). The solution pH, mass of adsorbent CZPs, amount of 1-(2-pyridylazo)-2-naphthol (PAN), which was used as a complexing agent, eluent volume, eluent concentration, and flow rates of sample and eluent were used as input parameters of the ANN model, and the percentage of extracted Pb2+ ions was used as the output variable of the model. A multilayer perception network with a back-propagation learning algorithm was used to fit the experimental data. The optimum conditions were obtained based on the ACO. Under the optimized conditions, the limit of detection for Pb2+ ions was found to be 0.078 μg/L. This procedure was also successfully used to determine the amounts of Pb2+ ions in various natural water samples.

Flame Atomic Absorption Spectrometric Determination of Gold After Solid-Phase Extraction of Its 2-Aminobenzothiazole Complex on Diaion SP-207.

PubMed

Unsal, Yunus Emre; Tuzen, Mustafa; Soylak, Mustafa

2016-01-01

An SPE of Au (III) on a 2-aminobenzothiazole-coated Diaion SP 207-column system has been developed. The parameters, including pH of solution, amount of 2-aminobenzothiazole, eluent type, sample volume, and flow rates, were examined. The effects of alkali, alkali earth, and some metals were also studied. The recovery values at optimal conditions and detection limits for Au (III) were found as >95% and 3.8 μg L(-1), respectively. The factor of preconcentration was 250. The RSD value was <5%. The capacity of adsorption for the resin was 10.4 mg g(-1). The accuracy of the method was evaluated by the use of CDN-GS-3D gold-certified reference material. The proposed procedure for the determination of gold was applied to water, mine, soil, and anodic slime samples.

Characterization of doped hydrogenated nanocrystalline silicon films prepared by plasma enhanced chemical vapour deposition

NASA Astrophysics Data System (ADS)

Wang, Jin-Liang; Wu, Er-Xing

2007-03-01

The B- and P-doped hydrogenated nanocrystalline silicon films (nc-Si:H) are prepared by plasma-enhanced chemical vapour deposition (PECVD). The microstructures of doped nc-Si:H films are carefully and systematically characterized by using high resolution electron microscopy (HREM), Raman scattering, x-ray diffraction (XRD), Auger electron spectroscopy (AES), and resonant nucleus reaction (RNR). The results show that as the doping concentration of PH3 increases, the average grain size (d) tends to decrease and the crystalline volume percentage (Xc) increases simultaneously. For the B-doped samples, as the doping concentration of B2H6 increases, no obvious change in the value of d is observed, but the value of Xc is found to decrease. This is especially apparent in the case of heavy B2H6 doped samples, where the films change from nanocrystalline to amorphous.

Mud volcanoes of trinidad as astrobiological analogs for martian environments.

PubMed

Hosein, Riad; Haque, Shirin; Beckles, Denise M

2014-10-13

Eleven onshore mud volcanoes in the southern region of Trinidad have been studied as analog habitats for possible microbial life on Mars. The profiles of the 11 mud volcanoes are presented in terms of their physical, chemical, mineralogical, and soil properties. The mud volcanoes sampled all emitted methane gas consistently at 3% volume. The average pH for the mud volcanic soil was 7.98. The average Cation Exchange Capacity (CEC) was found to be 2.16 kg/mol, and the average Percentage Water Content was 34.5%. Samples from three of the volcanoes, (i) Digity; (ii) Piparo and (iii) Devil's Woodyard were used to culture bacterial colonies under anaerobic conditions indicating possible presence of methanogenic microorganisms. The Trinidad mud volcanoes can serve as analogs for the Martian environment due to similar geological features found extensively on Mars in Acidalia Planitia and the Arabia Terra region.

Mud Volcanoes of Trinidad as Astrobiological Analogs for Martian Environments

PubMed Central

Hosein, Riad; Haque, Shirin; Beckles, Denise M.

2014-01-01

Eleven onshore mud volcanoes in the southern region of Trinidad have been studied as analog habitats for possible microbial life on Mars. The profiles of the 11 mud volcanoes are presented in terms of their physical, chemical, mineralogical, and soil properties. The mud volcanoes sampled all emitted methane gas consistently at 3% volume. The average pH for the mud volcanic soil was 7.98. The average Cation Exchange Capacity (CEC) was found to be 2.16 kg/mol, and the average Percentage Water Content was 34.5%. Samples from three of the volcanoes, (i) Digity; (ii) Piparo and (iii) Devil’s Woodyard were used to culture bacterial colonies under anaerobic conditions indicating possible presence of methanogenic microorganisms. The Trinidad mud volcanoes can serve as analogs for the Martian environment due to similar geological features found extensively on Mars in Acidalia Planitia and the Arabia Terra region. PMID:25370529

A survey of water activity and pH values in fresh pasta packed under modified atmosphere manufactured in Argentina and Uruguay.

PubMed

Schebor, C; Chirife, J

2000-07-01

The water activity (a(w)) and pH values of commercially available filled fresh pasta and gnocchi packed under modified atmosphere and manufactured in Argentina and Uruguay were examined. The retail survey included 58 samples (several brands) of filled pasta and 11 samples of gnocchi. Fillings consisted of different combinations of cheese (various types), beef, ricotta, ham, chicken, and spinach. The survey revealed that the a(w) values of the 58 samples of filled pasta ranged from 0.916 to 0.973, and their pH values ranged from 5.2 to 7.0. The a(w) of gnocchi was consistently higher and ranged from 0.936 to 0.983, with pH values from 4.8 to 6.4. Some samples of filled pasta and most gnocchi samples were found to have a(w) and pH values that would support growth of spores of Clostridium botulinum, if present, under conditions of temperature abuse (i.e., 30 degrees C).

Study of Vis/NIR spectroscopy measurement on acidity of yogurt

NASA Astrophysics Data System (ADS)

He, Yong; Feng, Shuijuan; Wu, Di; Li, Xiaoli

2006-09-01

A fast measurement of pH of yogurt using Vis/NIR-spectroscopy techniques was established in order to measuring the acidity of yogurt rapidly. 27 samples selected separately from five different brands of yogurt were measured by Vis/NIR-spectroscopy. The pH of yogurt on positions scanned by spectrum was measured by a pH meter. The mathematical model between pH and Vis/NIR spectral measurements was established and developed based on partial least squares (PLS) by using Unscramble V9.2. Then 25 unknown samples from 5 different brands were predicted based on the mathematical model. The result shows that The correlation coefficient of pH based on PLS model is more than 0.890, and standard error of calibration (SEC) is 0.037, standard error of prediction (SEP) is 0.043. Through predicting the pH of 25 samples of yogurt from 5 different brands, the correlation coefficient between predictive value and measured value of those samples is more than 0918. The results show the good to excellent prediction performances. The Vis/NIR spectroscopy technique had a significant greater accuracy for determining the value of pH. It was concluded that the VisINIRS measurement technique can be used to measure pH of yogurt fast and accurately, and a new method for the measurement of pH of yogurt was established.

Control of the microstructure and surface chemistry of graphene aerogels via pH and time manipulation by a hydrothermal method.

PubMed

García-Bordejé, E; Víctor-Román, S; Sanahuja-Parejo, O; Benito, A M; Maser, W K

2018-02-15

Three-dimensional graphene aerogels of controlled pore size have emerged as an important platform for several applications such as energy storage or oil-water separation. The aerogels of reduced graphene oxide are mouldable and light weight, with a porosity up to 99.9%, consisting mainly of macropores. Graphene aerogel preparation by self-assembly in the liquid phase is a promising strategy due to its tunability and sustainability. For graphene aerogels prepared by a hydrothermal method, it is known that the pH value has an impact on their properties but it is unclear how pH affects the auto-assembly process leading to the final properties. We have monitored the time evolution of the chemical and morphological properties of aerogels as a function of the initial pH value. In the hydrothermal treatment process, the hydrogel is precipitated earlier and with lower oxygen content for basic pH values (∼13 wt% O) than for acidic pH values (∼20 wt% O). Moreover, ∼7 wt% of nitrogen is incorporated on the graphene nanosheets at basic pH generated by NH 3 addition. To our knowledge, there is no precedent showing that the pH value affects the microstructure of graphene nanosheets, which become more twisted and bent for the more intensive deoxygenation occurring at basic pH. The bent nanosheets attained at pH = 11 reduce the stacking by the basal planes and they connect via the borders, hence leading eventually to higher pore volumes. In contrast, the flatter graphene nanosheets attained under acidic pH entail more stacking and higher oxygen content after a long hydrothermal treatment. The gravimetric absorption capacity of non-polar solvents scales directly with the pore volume. The aerogels have proved to be highly selective, recyclable and robust for the absorption of nonpolar solvents in water. The control of the porous structure and surface chemistry by manipulation of pH and time will also pave the way for other applications such as supercapacitors or batteries.

The effect of pH and chloride concentration on the stability and antimicrobial activity of chlorine-based sanitizers.

PubMed

Waters, Brian W; Hung, Yen-Con

2014-04-01

Chlorinated water and electrolyzed oxidizing (EO) water solutions were made to compare the free chlorine stability and microbicidal efficacy of chlorine-containing solutions with different properties. Reduction of Escherichia coli O157:H7 was greatest in fresh samples (approximately 9.0 log CFU/mL reduction). Chlorine loss in "aged" samples (samples left in open bottles) was greatest (approximately 40 mg/L free chlorine loss in 24 h) in low pH (approximately 2.5) and high chloride (Cl(-) ) concentrations (greater than 150 mg/L). Reduction of E. coli O157:H7 was also negatively impacted (<1.0 log CFU/mL reduction) in aged samples with a low pH and high Cl(-) . Higher pH values (approximately 6.0) did not appear to have a significant effect on free chlorine loss or numbers of surviving microbial cells when fresh and aged samples were compared. This study found chloride levels in the chlorinated and EO water solutions had a reduced effect on both free chlorine stability and its microbicidal efficacy in the low pH solutions. Greater concentrations of chloride in pH 2.5 samples resulted in decreased free chlorine stability and lower microbicidal efficacy. © 2014 Institute of Food Technologists®

Optical properties of fly ash. Volume 1, Final report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Self, S.A.

1994-12-01

Research performed under this contract was divided into four tasks under the following headings: Task 1, Characterization of fly ash; Task 2, Measurements of the optical constants of slags; Task 3, Calculations of the radiant properties of fly ash dispersions; and Task 4, Measurements of the radiant properties of fly ash dispersions. Tasks 1 and 4 constituted the Ph.D. research topic of Sarbajit Ghosal, while Tasks 2 and 3 constituted the Ph.D. research topic of Jon Ebert. Together their doctoral dissertations give a complete account of the work performed. This final report, issued in two volumes consists of an executivemore » summary of the whole program followed by the dissertation of Ghosal. Volume 1 contains the dissertation of Ghosal which covers the characterization of fly ash and the measurements of the radiant properties of fly ash dispersions. A list of publications and conference presentations resulting from the work is also included.« less

Optical sensing properties of Au nanoparticle/hydrogel composite microbeads using droplet microfluidics

NASA Astrophysics Data System (ADS)

Li, Huilin; Men, Dandan; Sun, Yiqiang; Zhang, Tao; Hang, Lifeng; Liu, Dilong; Li, Cuncheng; Cai, Weiping; Li, Yue

2017-10-01

Uniform Au nanoparticle (NP)/poly (acrylamide-co-acrylic acid) [P(AAm-co-AA)] hydrogel microbeads were successfully prepared using droplet microfluidics technology. The microbeads exhibited a good stimuli-responsive behavior to pH value. Particularly in the pH value ranging from pH 2-pH 9, the composite microbead sizes gradually increased along with the increase of pH value. The homogeneous Au NPs, which were encapsulated in the P(AAm-co-AA) hydrogel microbeads, could transform the volume changes of hydrogel into optical signals by a tested single microbead with a microspectrometre system. The glucose was translated into gluconic acid by glucose oxidase. Thus, the Au NP/P(AAm-co-AA) hydrogel microbeads were used for detecting glucose based on pH effects on the composite microbeads. For this, the single Au NP/P(AAm-co-AA) hydrogel microbead could act as a good pH- or glucose-visualizing sensor.

Pore-scale supercritical CO 2 dissolution and mass transfer under drainage conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chang, Chun; Zhou, Quanlin; Oostrom, Mart

Abstract: Recently, both core- and pore-scale imbibition experiments have shown non-equilibrium dissolution of supercritical CO 2 (scCO 2) and a prolonged depletion of residual scCO 2. In this study, pore-scale scCO 2 dissolution and mass transfer under drainage conditions were investigated using a two-dimensional heterogeneous micromodel and a novel fluorescent water dye with a sensitive pH range between 3.7 and 6.5. Drainage experiments were conducted at 9 MPa and 40 °C by injecting scCO 2 into the sandstone-analogue pore network initially saturated by water without dissolved CO 2 (dsCO 2). During the experiments, time-lapse images of dye intensity, reflecting watermore » pH, were obtained. These images show non-uniform pH in individual pores and pore clusters, with average pH levels gradually decreasing with time. Further analysis on selected pores and pore clusters shows that (1) rate-limited mass transfer prevails with slowly decreasing pH over time when the scCO 2-water interface area is low with respect to the volume of water-filled pores and pore clusters, (2) fast scCO 2 dissolution and phase equilibrium occurs when scCO 2 bubbles invade into water-filled pores, significantly enhancing the area-to-volume ratio, and (3) a transition from rate-limited to diffusion-limited mass transfer occurs in a single pore when a medium area-to-volume ratio is prevalent. The analysis also shows that two fundamental processes – scCO 2 dissolution at phase interfaces and diffusion of dsCO 2 at the pore scale (10-100 µm) observed after scCO 2 bubble invasion into water-filled pores without pore throat constraints – are relatively fast. The overall slow dissolution of scCO 2 in the millimeter-scale micromodel can be attributed to the small area-to-volume ratios that represent pore-throat configurations and characteristics of phase interfaces. This finding is applicable for the behavior of dissolution at pore, core, and field scales when water-filled pores and pore clusters of varying size are surrounded by scCO 2 at narrow pore throats.« less

Yogurt made from milk heated at different pH values.

PubMed

Ozcan, Tulay; Horne, David S; Lucey, John A

2015-10-01

Milk for yogurt manufacture is subjected to high heat treatment to denature whey proteins. Low milk pH values (≤ 6.5) at heating result in most denatured whey proteins becoming associated with casein micelles, whereas high milk pH values (≥ 7.0) at heating result in the formation of mostly soluble (nonmicellar) denatured whey protein complexes. There are conflicting reports on the relative importance of soluble and casein-bound whey protein aggregates on the properties of acid gels. Prior studies investigating the effect of pH of milk at heating used model gels in which milk was acidified by glucono-δ-lactone; in this study, we prepared yogurt gels using commercial starter cultures. Model acid gels can have very different texture and physical properties from those made by fermentation with starter cultures. In this study, we investigated the effects of different pH values of milk at heating on the rheological, light backscatter, and microstructural properties of yogurt gels. Reconstituted skim milk was adjusted to pH values 6.2, 6.7, and 7.2 and heated at 85°C for 30 min. A portion of the heated milk samples was readjusted back to pH 6.7 after heating. Milks were inoculated with 3% (wt/wt) yogurt starter culture and incubated at 40°C until pH 4.6. Gel formation was monitored using dynamic oscillatory rheology, and parameters measured included the storage modulus (G') and loss tangent (LT) values. Light-backscattering properties, such as the backscatter ratio (R) and the first derivative of light backscatter ratio (R'), were also monitored during fermentation. Fluorescence microscopy was used to observe gel microstructure. The G' values at pH 4.6 were highest in gels made from milk heated at pH 6.7 and lowest in milk heated at pH 6.2, with or without pH adjustment after heating. The G' values at pH 4.6 were lower in samples after adjustment back to pH 6.7 after heating. No maximum in the LT parameter was observed during gelation for yogurts made from milk heated at pH 6.2; a maximum in LT was observed at pH ~4.8 for samples heated at pH 6.7 or 7.2, with or without pH adjustment after heating. Higher R-values were observed with an increase in pH of heating, with or without pH adjustment after heating. The sample heated at pH 6.2 had only one major peak in its R' profile during acidification, whereas samples heated at pH 6.7 and 7.2 had 2 large peaks. The lack of a maximum in LT parameter and the presence of a single peak in the R' profile for the samples heated at pH 6.2 were likely due to the partial solubilization of insoluble calcium phosphate when milk was acidified to this lower pH value. No clear differences were observed in the microstructures of gels between the different treatments. This study indicates that heating milk at the natural pH (~6.7) created an optimum balance of casein-bound and soluble denatured whey proteins, which resulted in yogurt with the highest gel stiffness. Copyright © 2015 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Mechanisms of iodine release from iodoapatite in aqueous solution

NASA Astrophysics Data System (ADS)

Zhang, Z.; Wang, J.

2017-12-01

Immobilization of iodine-129 with waste forms in geological setting is challenging due to its extremely long half-life and high volatility in the environment. To evaluate the long-term performance of waste form, it is imperative to determine the release mechanism of iodine hosted in the waste form materials. This study investigated the iodine released from apatite structured waste form Pb9.85 (VO4)6 I1.7 to understand how diffusion and dissolution control the durability of apatite waste form. A standard semi-dynamic leach test was adopted in this study. Samples were exposed in fresh leachant periodically and the leachant was replaced after each interval. Each experiment was carried out in cap-sealed Teflon vessels under constant temperature (e.g. 90 °C). ICP-MS analysis on the reacted leachates shows that Pb and V were released constantly and congruently with the stoichiometric ratio of Pb/V. However, iodine release is incongruent and time dependent. The iodine release rate starts significantly higher than the corresponding stoichiometric value and gradually decreases, approaching the stoichiometric value. Therefore, a dual-mode mechanism is proposed to account for the iodine release from apatite, which is dominated by short-term diffusion and long-term dissolution processes. Additional tests show that the element release rates depend on a number of test parameters, including sample surface to solution volume ratio (m-1), interval (day), temperature (°C), and solution pH. This study provides a quantitative characterization of iodine release mechanism. The activation energy of iodine leaching 21±1.6 kJ/mol was obtained by varying the test temperature. At the test conditions of to neutral pH and 90 °C, the long-term iodine release rate 3.3 mg/(m2 • day) is projected by normalizing sample surface area to solution volume ratio (S/V) to 1.0 m-1 and interval to 1 day. These findings demonstrate i) the feasibility of our approach to quantify the release mechanism and ii) the performance of iodine apatite as a favorable waste form candidate for I-129 disposal.

Quality of semen: a 6-year single experience study on 5680 patients.

PubMed

Cozzolino, Mauro; Coccia, Maria E; Picone, Rita

2018-02-08

The aim of our study was to evaluate the quality of semen of a large sample from general healthy population living in Italy, in order to identify possible variables that could influence several parameters of spermiogram. We conducted a cross-sectional study from February 2010 to March 2015, collecting semen samples from the general population. Semen analysis was performed according to the WHO guidelines. The collected data were inserted in a database and processed using the software Stata 12. The Mann - Whitney test was used to assess the relationship of dichotomus variables with the parameters of the spermiogram; Kruskal-Wallis test for variables with more than two categories. We used also Robust regression and Spearman correlation to analyze the relationship between age and the parameters. We collected 5680 samples of semen. The mean age of our patients was 41.4 years old. Mann-Whitney test showed that the citizenship (codified as "Italian/Foreign") influences some parameters: pH, vitality, number of spermatozoa, sperm concentration, with worse results for the Italian group. Kruskal-Wallis test showed that the single nationality influences pH, volume, Sperm motility A-B-C-D, vitality, morphology, number of spermatozoa, sperm concentration. Robust regression showed a relationship between age and several parameters: volume (p=0.04, R squared= 0.0007 β: - 0.06); sperm motility A (p<0.01; R squared 0.0051 β: 0.02); sperm motility B (p<0.01; R squared 0.02 β: -0.35); sperm motility C (p<0.01; R squared 0.01 β: 0.12); sperm motility D (p<0.01; R squared 0.006 β: 0.2); vitality (p<0.01; R squared 0.01 β: -0.32); sperm concentration (p=0.01; R squared 0.001 β: 0.19). Our patients had spermiogram's results quite better than the standard guidelines. Our study showed that the country of origin could be a factor influencing several parameters of the spermiogram in healthy population and through Robust regression confirmed a strict correlation between age and these parameters.

Effect of Salivary pH on Color Stability of Different Flowable Composites - A Prospective In-vitro Study.

PubMed

Batra, Renu; Kataria, Pratik; Kapoor, Sonali

2016-10-01

Scientifically and clinically there has been lot of development in the field of aesthetic dentistry. However, there is limited or restricted information regarding the color stability of flowable composite materials. The aim of this study was to evaluate the spectrophotometric color stability of three different flowable composite materials with respect to three different pH of saliva. The study included 90 different samples. Thirty samples in each composite group; (Group A: G-aenial universal flo; Group B: Z 350 XT flowable; Group C: Esthet x flow). All samples from each group were immersed in distilled water for 24 hours. Total color difference (ΔE) was recorded for each sample. After this 10 samples from each group were respectively immersed in 6.5, 7 and 7.5 pH of artificial saliva. All samples were kept in dark room for seven days and then ΔE for each sample was recorded and was compared to previous recorded ΔE for the same sample. Maximum color change was seen irrespective of material in 6.5 pH of saliva. G-aenial universal flo showed least change irrespective of pH of saliva. Thus, the present study reveals that acidic pH level affects the coloration of composite resins by affecting the surface integrity and as reported in previous studies, various coloring agents in beverages and other dietary components assists the process due to absorption of these coloring substances into the resin matrix.

The impacts of anthropogenic emissions on the precipitation chemistry at an elevated site in North-eastern China

NASA Astrophysics Data System (ADS)

Wang, Yan; Wai, Ka Ming; Gao, Jian; Liu, Xiaohuan; Wang, Tao; Wang, Wenxing

Ninety precipitation samples were collected from 2004 to 2006 at the summit of the Mt. Tai in order to detect the impacts of regional sources of pollution on precipitation chemistry in the highly polluted North China Plains. The annual volume-weighted pH of the precipitation was found to be 4.7, in contrast to the less-acidic nature (pH>5.6) of precipitation in northern China reported in many past studies. Non-sea-salt (nss)-SO 42- (131.5 μeq L -1), NH 4+ (82.2 μeq L -1) and Ca 2+ (61.4 μeq L -1) were the most abundant species in precipitation. The wide range of the Cl -/Na + ratios (0.2-5.4) in precipitation implied the co-existence of Cl - enrichment and depletion. The nss-SO 42-, NO 3-, NH 4+, Ca 2+ and K + concentrations peaked in spring, but with the lowest acidity. The very strong correlations of Ca 2+ with nss-SO 42- and NO 3- suggested a significant uptake of nss-SO 42- and NO 3- on dust aerosol during spring. Samples with the lowest pH value (4.5) are associated with the stagnant air conditions. The nss-SO 42- and NH 4+ concentrations at Mt. Tai were the highest compared with those at the EANET, NADP and EMEP sites of similar elevations. With relatively high rainfall amount measured at our site, the high wet deposition of the major acidic/alkaline species exerted large loadings to the ecosystem. The associated impacts on agriculture, soil and aquatic systems should be investigated.

Effect of heavy metals on pH buffering capacity and solubility of Ca, Mg, K, and P in non-spiked and heavy metal-spiked soils.

PubMed

Najafi, Sarvenaz; Jalali, Mohsen

2016-06-01

In many parts of the world, soil acidification and heavy metal contamination has become a serious concern due to the adverse effects on chemical properties of soil and crop yield. The aim of this study was to investigate the effect of pH (in the range of 1 to 3 units above and below the native pH of soils) on calcium (Ca), magnesium (Mg), potassium (K), and phosphorus (P) solubility in non-spiked and heavy metal-spiked soil samples. Spiked samples were prepared by cadmium (Cd), copper (Cu), nickel (Ni), and zinc (Zn) as chloride salts and incubating soils for 40 days. The pH buffering capacity (pHBC) of each sample was determined by plotting the amount of H(+) or OH(-) added (mmol kg(-1)) versus the related pH value. The pHBC of soils ranged from 47.1 to 1302.5 mmol kg(-1) for non-spiked samples and from 45.0 to 1187.4 mmol kg(-1) for spiked soil samples. The pHBC values were higher in soil 2 (non-spiked and spiked) which had higher calcium carbonate content. The results indicated the presence of heavy metals in soils generally decreased the solution pH and pHBC values in spiked samples. In general, solubility of Ca, Mg, and K decreased with increasing equilibrium pH of non-spiked and spiked soil samples. In the case of P, increasing the pH to about 7, decreased the solubility in all soils but further increase of pH from 7, enhanced P solubility. The solubility trends and values for Ca, Mg, and K did not differed significantly in non-spiked and spiked samples. But in the case of P, a reduction in solubility was observed in heavy metal-spiked soils. The information obtained in this study can be useful to make better estimation of the effects of soil pollutants on anion and cation solubility from agricultural and environmental viewpoints.

Nevada National Security Site 2014 Data Report: Groundwater Monitoring Program Area 5 Radioactive Waste Management Site

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hudson, David

2015-02-01

This report is a compilation of the groundwater sampling results from the Area 5 Radioactive Waste Management Site (RWMS) at the Nevada National Security Site, Nye County, Nevada. Groundwater samples from the aquifer immediately below the Area 5 RWMS have been collected and analyzed and static water levels have been measured in this aquifer since 1993. This report updates these data to include the 2014 results. Analysis results for leachate contaminants collected from the mixed-waste cell at the Area 5 RWMS (Cell 18) are also included. During 2014, groundwater samples were collected and static water levels were measured at threemore » wells surrounding the Area 5 RWMS. Groundwater samples were collected at wells UE5PW-1, UE5PW-2, and UE5PW-3 on March 11 and August 12, 2014, and static water levels were measured at each of these wells on March 10, June 2, August 11, and October 14, 2014. Groundwater samples were analyzed for the following indicators of contamination: pH, specific conductance, total organic carbon, total organic halides, and tritium. General water chemistry (cations and anions) was also measured. Results from samples collected in 2014 are within the limits established by agreement with the Nevada Division of Environmental Protection for each analyte. The data from the shallow aquifer indicate that there has been no measurable impact to the uppermost aquifer from the Area 5 RWMS, and there were no significant changes in measured groundwater parameters compared to previous years. Leachate from above the primary liner of Cell 18 drains into a sump and is collected in a tank at the ground surface. Cell 18 began receiving waste in January 2011. Samples were collected from the tank when the leachate volume approached the 3,000-gallon tank capacity. Leachate samples have been collected 16 times since January 2011. During 2014, samples were collected on February 25, March 5, May 20, August 12, September 16, November 11, and December 16. Each leachate sample was analyzed for toxicity characteristic contaminants and polychlorinated biphenyls (PCB). Beginning with the sample from July 31, 2013, pH and specific conductance were also measured. Leachate analysis results show no evidence of contamination. Results for toxicity characteristic contaminants are all below regulatory levels and analysis quantification limits. No quantifiable PCB levels were detected in any sample. Results for pH and specific conductance are also within expected ranges. After analysis, leachate was pumped from the collection tank and used in Cell 18 for dust control. The report contains an updated cumulative chronology for the Area 5 RWMS Groundwater Monitoring Program and a brief description of the site hydrogeology.« less

An investigation of the stability of free and glucuronidated 11-nor-delta9-tetrahydrocannabinol-9-carboxylic acid in authentic urine samples.

PubMed

Skopp, Gisela; Pötsch, Lucia

2004-01-01

Preanalytical stability of a drug and its major metabolites is an important consideration in pharmacokinetic studies or whenever the analyte pattern is used to estimate drug habits. Firstly, the stability of free and glucuronidated 11-nor-delta9-tetrahydrocannabinol-9-carboxylic acid (THCCOOH, THCCOOglu) in authentic urine samples was investigated. Random urine samples of cannabis users (n = 38) were stored at -20, 4, and 20 degrees C up to 15 days and up to 5 days at 40 degrees C, and alterations of the analyte pattern during storage were followed by liquid chromatography-tandem mass spectrometry. Secondly, the influence of pH (range 5.0-8.0) on the stability of the analytes was studied using spiked urine to elucidate the results obtained from authentic samples. In authentic urine samples, the initial pH ranged from 5.1 to 8.8. The glucuronide was found to be highly labile at a storage temperature of 4 degrees C and above. Initially, 18 urine samples tested positive for THCCOOH. After 2 days storage at 20 degrees C, THCCOOH was detectable in a further 4 samples, and 7 more samples tested positive for THCCOOH (5-81 ng/mL) after 15 days. Depending on time and temperature, the glucuronide concentration decreased, resulting in an increase of THCCOOH concentration. However, a loss in mean total THCCOOH concentration was found, which was significantly higher in deteriorated samples than in samples without signs of deterioration after 15 days of storage at 20 degrees C. In the drug-free urine sample separately spiked with THCCOOglu or THCCOOH, the investigations on the stability of the target analytes at various pH values revealed that THCCOOH was stable at pH 5.0. At higher pH values, its concentration slightly decreased with time, and about 69% of the initial THCCOOH concentration was still present at pH 8.0 on day 5. THCCOOglu concentrations rapidly decreased with increasing pH value. For example, only 72% of the initial THCCOOglu concentration could be detected at pH 5.0 on day 1. Degradation of the glucuronide resulted in formation of THCCOOH, which was observed even at pH 5.0. In light of the present findings, advanced forensic interpretations based on the presence of THCCOOH or the pattern of THCCOOH and THCCOOglu in stored urine samples seems questionable.

Measurement of pH in whole blood by near-infrared spectroscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Alam, M. Kathleen; Maynard, John D.; Robinson, M. Ries

1999-03-01

Whole blood pH has been determined {ital in vitro} by using near-infrared spectroscopy over the wavelength range of 1500 to 1785 nm with multivariate calibration modeling of the spectral data obtained from two different sample sets. In the first sample set, the pH of whole blood was varied without controlling cell size and oxygen saturation (O{sub 2} Sat) variation. The result was that the red blood cell (RBC) size and O{sub 2} Sat correlated with pH. Although the partial least-squares (PLS) multivariate calibration of these data produced a good pH prediction cross-validation standard error of prediction (CVSEP)=0.046, R{sup 2}=0.982, themore » spectral data were dominated by scattering changes due to changing RBC size that correlated with the pH changes. A second experiment was carried out where the RBC size and O{sub 2} Sat were varied orthogonally to the pH variation. A PLS calibration of the spectral data obtained from these samples produced a pH prediction with an R{sup 2} of 0.954 and a cross-validated standard error of prediction of 0.064 pH units. The robustness of the PLS calibration models was tested by predicting the data obtained from the other sets. The predicted pH values obtained from both data sets yielded R{sup 2} values greater than 0.9 once the data were corrected for differences in hemoglobin concentration. For example, with the use of the calibration produced from the second sample set, the pH values from the first sample set were predicted with an R{sup 2} of 0.92 after the predictions were corrected for bias and slope. It is shown that spectral information specific to pH-induced chemical changes in the hemoglobin molecule is contained within the PLS loading vectors developed for both the first and second data sets. It is this pH specific information that allows the spectra dominated by pH-correlated scattering changes to provide robust pH predictive ability in the uncorrelated data, and visa versa. {copyright} {ital 1999} {ital Society for Applied Spectroscopy}« less

Nutrient infiltrate concentrations from three permeable pavement types.

PubMed

Brown, Robert A; Borst, Michael

2015-12-01

While permeable pavement is increasingly being used to control stormwater runoff, field-based, side-by-side investigations on the effects different pavement types have on nutrient concentrations present in stormwater runoff are limited. In 2009, the U.S. EPA constructed a 0.4-ha parking lot in Edison, New Jersey, that incorporated permeable interlocking concrete pavement (PICP), pervious concrete (PC), and porous asphalt (PA). Each permeable pavement type has four, 54.9-m(2), lined sections that direct all infiltrate into 5.7-m(3) tanks enabling complete volume collection and sampling. This paper highlights the results from a 12-month period when samples were collected from 13 rainfall/runoff events and analyzed for nitrogen species, orthophosphate, and organic carbon. Differences in infiltrate concentrations among the three permeable pavement types were assessed and compared with concentrations in rainwater samples and impervious asphalt runoff samples, which were collected as controls. Contrary to expectations based on the literature, the PA infiltrate had significantly larger total nitrogen (TN) concentrations than runoff and infiltrate from the other two permeable pavement types, indicating that nitrogen leached from materials in the PA strata. There was no significant difference in TN concentration between runoff and infiltrate from either PICP or PC, but TN in runoff was significantly larger than in the rainwater, suggesting meaningful inter-event dry deposition. Similar to other permeable pavement studies, nitrate was the dominant nitrogen species in the infiltrate. The PA infiltrate had significantly larger nitrite and ammonia concentrations than PICP and PC, and this was presumably linked to unexpectedly high pH in the PA infiltrate that greatly exceeded the optimal pH range for nitrifying bacteria. Contrary to the nitrogen results, the PA infiltrate had significantly smaller orthophosphate concentrations than in rainwater, runoff, and infiltrate from PICP and PC, and this was attributed to the high pH in PA infiltrate possibly causing rapid precipitation of orthophosphate with metal cations. Orthophosphate was exported from the PICP and PC, as evidenced by the significantly larger infiltrate concentrations compared with influent sources of rainwater and runoff. Copyright © 2015 Elsevier Ltd. All rights reserved.

Effects of Habitat Type and Drying on Ascogregarina barretti (Eugregarinida: Lecudinidae) Infection in Aedes triseritatus (Diptera: Culicidae)

PubMed Central

VAN RHEIN, STEPHEN L.; FLANARY, BARRY E.; JULIANO, STEVEN A.

2008-01-01

The intensity and prevalence of parasitism by Ascogregarina barretti (Vavra) in Aedes triseriatus (Say) did not differ between tires and tree holes in field samples taken in September 1996. There was significant variation in the intensity of parasitism among containers that was not significantly correlated with the pH, conductivity, or temperature of the container water. In an experiment manipulating habitat drying, treatments had a significant effect on A. barretti infection of Ae. triseriatus, only during midsummer in one of two years. Containers maintained at maximal volume had the lowest prevalence of parasitism, and containers that dried out had the greatest prevalence. In this experiment, there was also a season-dependent difference in the intensity and prevalence of infection between tree holes and tires. The first larvae to reach the fourth instar in tires in the early summer had lower intensity and prevalence of infection than did larvae in tree holes during the same period. The seasonal difference in intensity of parasitism between tires and tree holes was not related to differences in pH, conductivity, and temperature. PMID:11126556

IPE 7

NASA Technical Reports Server (NTRS)

1983-01-01

A description is given of the collection and treatment of samples of Prochloron cells. The cells of Prochloron were obtained and prepared in the following way. Colonies of the symbiotic host, the giant didemnid ascidian Lissoclinum patella, were collected at low-tide level on reef-flat sand between Kamori Island and Koror, Palau, Western Caroline Islands. The animal colonies were taken, immersed in sea water, to an 8,000-litre holding tank and kept with constantly running sea water at 30 deg. Individual colonies were picked clean of contaminants, rinsed in sea water buffered with 40 nM or 100 mM Tris buffer at pH 8.4, and squeezed by hand to express the algal cells from the cloacal atria. The algae were received in about an equal volume of the same buffered sea water; this neutralized the acids liberated by the bruised ascidians and thereby maintained the Ph high enough to keep the algal cells green. The Prochloron cells were washed twice with buffered sea water and concentrated by centrifugation at about 50 g for 90 seconds. Microscopic examination revealed that contamination by animal host cells or bacteria was negligible (much less than 1%).

Compatibility of 5-fluorouracil and total parenteral nutrition solutions.

PubMed

Hardin, T C; Clibon, U; Page, C P; Cruz, A B

1982-01-01

The physicochemical stability and availability of 0.1% 5-fluorouracil solutions in D5W and a typical total parenteral nutrition solution (hypertonic dextrose and crystalline amino acids) were studied in both glass and Viaflex delivery systems. Serial samples collected over a 48-hour period were assayed for 5-fluorouracil concentration using a high performance liquid chromatographic technique. Changes in the pH as well as precipitate formation were also investigated. There was no reduction in the amount of 5-fluorouracil at 48 hours in either the glass or plastic system, regardless of whether the drug was added to D5W or to the total parenteral nutrition solution. No pH changes or precipitates were observed. These findings indicate that 5-fluorouracil is compatible with and available from total parenteral solutions of hypertonic dextrose and amino acid in both plastic and glass containers. Use of such a system would allow for (1) a reduction in vascular access in patients receiving both treatments and (2) continued administration of nutritional support without the requirement for additional fluid volume.

Characterization and evaluation of acid rain in East Central Florida from 1978 to 1987: Ten year summary report

NASA Technical Reports Server (NTRS)

Madsen, Brooks C.; Dreschel, Thomas W.; Hinkle, C. Ross

1989-01-01

Rainfall was collected on the University of Central Florida (UCF) campus near Orlando since July 1977 and at the Kennedy Space Center (KSC), Florida since August 1977. Since November 1983, the KSC site has been affiliated with the National Atmospheric Deposition Network. Annual volume weighted pH was slightly above the 10 year mean of 4.58 during four of the past five years. Nitrate concentrations have risen somewhat during recent years while excess sulfate concentrations have remained below the 10 year mean during four of the past years. These observations hold for both the UCF and KSC data. The distribution of individual sample pH was nearly identical at UCF and KSC. Stepwise regression suggests that sulfate, nitrate, ammonium ion, and calcium play major roles in the description of rainwater acidity. Annual acid deposition and annual rainfall have varied from 30 to 50 meq/m2-yr and 100 to 180 cm/yr, respectively. Sea salt comprises about 25 percent (UCF) and greater than 50 percent (KSC) of total ionic composition.

Water-quality parameters and benthic algal communities at selected streams in Minnesota, August 2000 - Study design, methods and data

USGS Publications Warehouse

Lee, K.E.

2002-01-01

This report describes the study design, sampling methods, and summarizes the physical, chemical, and benthic algal data for a component of the multiagency study that was designed to document diurnal water-quality measurements (specific conductance, pH, water temperature, and dissolved oxygen), benthic algal community composition and chlorophyll-a content, and primary productivity at 12 stream sites on 6 streams in Minnesota during August 2000. Specific conductance, pH, water temperature, dissolved oxygen concentrations and percent dissolved oxygen saturation measurements were made with submersible data recorders at 30 minute intervals for a period of 3-6 days during August 2000. Benthic algae collected from wood and rock substrate were identified and enumerated. Biovolume (volume of algal cells per unit area), density (number of cells per unit area), and chlorophyll-a content from benthic algae were determined. These data can be used as part of the multiagency study to develop an understanding of the relations among nutrient concentrations, algal abundance, algal community composition, and primary production and respiration processes in rivers of differing ecoregions in Minnesota.

The effect of heavy metal concentration and soil pH on the abundance of selected microbial groups within ArcelorMittal Poland steelworks in Cracow.

PubMed

Lenart, Anna; Wolny-Koładka, Katarzyna

2013-01-01

The present study aimed to identify the effect of heavy metal concentration and soil pH on the abundance of the selected soil microorganisms within ArcelorMittal Poland steelworks, Cracow. The analysis included 20 soil samples, where the concentration of Fe, Zn, Cd, Pb, Ni, Cu, Mn, Cr and soil pH were evaluated together with the number of mesophilic bacteria, fungi, Actinomycetes and Azotobacter spp. In the majority of samples soil pH was alkaline. The limits of heavy metals exceeded in eight samples and in one sample, the concentration of Zn exceeded 31-fold. Chromium was the element which most significantly limited the number of bacteria and Actinomycetes.

Device For Controlling Crystallization Of Protein

NASA Technical Reports Server (NTRS)

Noever, David A.

1993-01-01

Variable sandwich spacer enables optimization of evaporative driving force that governs crystallization of protein from solution. Mechanically more rigid than hanging-drop and sitting-drop devices. Large oscillations and dislodgment of drop of solution in response to vibrations suppressed by glass plates. Other advantages include: suitable for automated delivery, stable handling, and programmable evaporation of protein solution; controlled configuration enables simple and accurate determination of volume of solution without disrupting crystallization; pH and concentration of precipitant controlled dynamically because pH and concentration coupled to rate of evaporation, controllable via adjustment of gap between plates; and enables variation of ratio between surface area and volume of protein solution. Alternative version, plates oriented vertically instead of horizontally.

Preparation and characterization of magnetic allylamine modified graphene oxide-poly(vinyl acetate-co-divinylbenzene) nanocomposite for vortex assisted magnetic solid phase extraction of some metal ions.

PubMed

Khan, Mansoor; Yilmaz, Erkan; Sevinc, Basak; Sahmetlioglu, Ertugrul; Shah, Jasmin; Jan, Muhammad Rasul; Soylak, Mustafa

2016-01-01

Magnetic allylamine modified graphene oxide-poly(vinyl acetate-co-divinylbenzene) (MGO-DVB-VA) was synthesized and used for magnetic solid phase extraction of Pb(II), Cd(II), Cu(II), Ni(II) and Co(II) prior to their determination by flame atomic absorption spectroscopy. The adsorbent surface functional group was characterized by using FT-IR and Raman spectroscopy. XRD pattern was used to determine the layers of GO. Surface morphology and elemental composition of the adsorbent were evaluated by using SEM and EDX analysis. Various parameters, effecting adsorption efficiency like initial solution pH, adsorbent dose, type and volume of eluent, volume of sample and diverse ions effects were optimized. The preconcentration factor (PF) is 40 for all the metals and the limits of detection for Pb, Cd, Cu, Ni and Co are in the range of 0.37-2.39 µg L(-1) and relative standard deviation below 3.1%. The method was validated by using the method for certified reference materials (Tobacco Leaves (INCT-OBTL-5), Tomato Leaves (1573a), Certified Water (SPS-ww2) and Certified Water (TMDA 64-2)). The method was successfully applied for natural water and food samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of Cu Environments in the Cyanobacterium Anabaena flos-aquae by X-Ray Absorption Spectroscopy

PubMed Central

Kretschmer, X. C.; Meitzner, G.; Gardea-Torresdey, J. L.; Webb, R.

2004-01-01

Whole cells and peptidoglycan isolated from cell walls of the cyanobacterium Anabaena flos-aquae were lyophilized and used at pH 2 and pH 5 in Cu(II) binding studies. X-ray absorption spectra measured at the Cu K-edge were used to determine the oxidation states and chemical environments of Cu species in the whole-cell and peptidoglycan samples. In the whole-cell samples, most of the Cu retained at both pH values was coordinated by phosphate ligands. The whole-cell fractions contained significant concentrations of Cu(I) as well as Cu(II). An X-ray absorption near-edge spectrum analysis suggested that Cu(I) was coordinated by amine and thiol ligands. An analysis of the peptidoglycan fractions found that more Cu was adsorbed by the peptidoglycan fraction prepared at pH 5, due to increased chelation by amine and carboxyl ligands. The peptidoglycan fractions, also referred to as the cell wall fractions, contained little or no Cu(I). The Cu loading level was 30 times higher in the cell wall sample prepared at pH 5 than in the sample prepared at pH 2. Amine and bidentate carboxyl ligands had similar relative levels of importance in cell wall peptidoglycan samples prepared at both pH values, but phosphate coordination was insignificant. PMID:14766554

Response surface methodology based on central composite design as a chemometric tool for optimization of dispersive-solidification liquid-liquid microextraction for speciation of inorganic arsenic in environmental water samples.

PubMed

Asadollahzadeh, Mehdi; Tavakoli, Hamed; Torab-Mostaedi, Meisam; Hosseini, Ghaffar; Hemmati, Alireza

2014-06-01

Dispersive-solidification liquid-liquid microextraction (DSLLME) coupled with electrothermal atomic absorption spectrometry (ETAAS) was developed for preconcentration and determination of inorganic arsenic (III, V) in water samples. At pH=1, As(III) formed complex with ammonium pyrrolidine dithiocarbamate (APDC) and extracted into the fine droplets of 1-dodecanol (extraction solvent) which were dispersed with ethanol (disperser solvent) into the water sample solution. After extraction, the organic phase was separated by centrifugation, and was solidified by transferring into an ice bath. The solidified solvent was transferred to a conical vial and melted quickly at room temperature. As(III) was determined in the melted organic phase while As(V) remained in the aqueous layer. Total inorganic As was determined after the reduction of the pentavalent forms of arsenic with sodium thiosulphate and potassium iodide. As(V) was calculated by difference between the concentration of total inorganic As and As(III). The variable of interest in the DSLLME method, such as the volume of extraction solvent and disperser solvent, pH, concentration of APDC (chelating agent), extraction time and salt effect, was optimized with the aid of chemometric approaches. First, in screening experiments, fractional factorial design (FFD) was used for selecting the variables which significantly affected the extraction procedure. Afterwards, the significant variables were optimized using response surface methodology (RSM) based on central composite design (CCD). In the optimum conditions, the proposed method has been successfully applied to the determination of inorganic arsenic in different environmental water samples and certified reference material (NIST RSM 1643e). Copyright © 2014 Elsevier B.V. All rights reserved.

Determination of melamine in soil samples using surfactant-enhanced hollow fiber liquid phase microextraction followed by HPLC–UV using experimental design

PubMed Central

Sarafraz Yazdi, Ali; Raouf Yazdinezhad, Samaneh; Heidari, Tahereh

2014-01-01

Surfactant-enhanced hollow fiber liquid phase (SE-HF-LPME) microextraction was applied for the extraction of melamine in conjunction with high performance liquid chromatography with UV detection (HPLC–UV). Sodium dodecyl sulfate (SDS) was added firstly to the sample solution at pH 1.9 to form hydrophobic ion-pair with protonated melamine. Then the protonated melamine–dodecyl sulfate ion-pair (Mel–DS) was extracted from aqueous phase into organic phase immobilized in the pores and lumen of the hollow fiber. After extraction, the analyte-enriched 1-octanol was withdrawn into the syringe and injected into the HPLC. Preliminary, one variable at a time method was applied to select the type of extraction solvent. Then, in screening step, the other variables that may affect the extraction efficiency of the analyte were studied using a fractional factorial design. In the next step, a central composite design was applied for optimization of the significant factors having positive effects on extraction efficiency. The optimum operational conditions included: sample volume, 5 mL; surfactant concentration, 1.5 mM; pH 1.9; stirring rate, 1500 rpm and extraction time, 60 min. Using the optimum conditions, the method was analytically evaluated. The detection limit, relative standard deviation and linear range were 0.005 μg mL−1, 4.0% (3 μg mL−1, n = 5) and 0.01–8 μg mL−1, respectively. The performance of the procedure in extraction of melamine from the soil samples was good according to its relative recoveries in different spiking levels (95–109%). PMID:26644934

Development and validation of an HPLC-DAD method for simultaneous determination of cocaine, benzoic acid, benzoylecgonine and the main adulterants found in products based on cocaine.

PubMed

Floriani, Gisele; Gasparetto, João Cleverson; Pontarolo, Roberto; Gonçalves, Alan Guilherme

2014-02-01

Here, an HPLC-DAD method was developed and validated for simultaneous determination of cocaine, two cocaine degradation products (benzoylecgonine and benzoic acid), and the main adulterants found in products based on cocaine (caffeine, lidocaine, phenacetin, benzocaine and diltiazem). The new method was developed and validated using an XBridge C18 4.6mm×250mm, 5μm particle size column maintained at 60°C. The mobile phase consisted of a gradient of acetonitrile and ammonium formate 0.05M - pH 3.1, eluted at 1.0mL/min. The volume of injection was 10μL and the DAD detector was set at 274nm. Method validation assays demonstrated suitable sensitivity, selectivity, linearity, precision and accuracy. For selectivity assay, a MS detection system could be directly adapted to the method without the need of any change in the chromatographic conditions. The robustness study indicated that the flow rate, temperature and pH of the mobile phase are critical parameters and should not be changed considering the conditions herein determined. The new method was then successfully applied for determining cocaine, benzoylecgonine, benzoic acid, caffeine, lidocaine, phenacetin, benzocaine and diltiazem in 115 samples, seized in Brazil (2007-2012), which consisted of cocaine paste, cocaine base and salt cocaine samples. This study revealed cocaine contents that ranged from undetectable to 97.2%, with 97 samples presenting at least one of the degradation products or adulterants here evaluated. All of the studied degradation products and adulterants were observed among the seized samples, justifying the application of the method, which can be used as a screening and quantification tool in forensic analysis. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

Zeolite/iron oxide composite as sorbent for magnetic solid-phase extraction of benzene, toluene, ethylbenzene and xylenes from water samples prior to gas chromatography⬜mass spectrometry.

PubMed

Fernández, Elena; Vidal, Lorena; Canals, Antonio

2016-08-05

This study reports a new composite based on ZSM-5 zeolite decorated with iron oxide magnetic nanoparticles as a valuable sorbent for magnetic solid-phase extraction (MSPE). A proposal is made to determine benzene, toluene, ethylbenzene and xylenes (BTEX) as model analytes in water samples using gas chromatography-mass spectrometry. A two-step multivariate optimization strategy, using Plackett⬜Burman and circumscribed central composite designs, was employed to optimize experimental parameters affecting MSPE. The method was evaluated under optimized extraction conditions (i.e., amount of sorbent, 138mg; extraction time, 11min; sample pH, pH of water (i.e., 5.5⬜6.5); eluent solvent volume, 0.5mL; and elution time, 5min), obtaining a linear response from 1 to 100μgL(↙1) for benzene; from 10 to 100μgL(↙1) for toluene, ethylbenzene and o-xylene; and from 10 to 75μgL(↙1) for m,p-xylene. The repeatability of the proposed method was evaluated at a 40μgL(↙1) spiking level and coefficients of variation ranged between 8 and 11% (n=5). Limits of detection were found to be 0.3μgL(↙1) for benzene and 3μgL(↙1) for the other analytes. These values satisfy the current normative of the Environmental Protection Agency and European Union for BTEX content in waters for human consumption. Finally, drinking water, wastewater and river water were selected as real water samples to assess the applicability of the method. Relative recoveries varied between 85% and 114% showing negligible matrix effects. Copyright © 2016 Elsevier B.V. All rights reserved.

The pH of chemistry assays plays an important role in monoclonal immunoglobulin interferences.

PubMed

Alberti, Michael O; Drake, Thomas A; Song, Lu

2015-12-01

Immunoglobulin paraproteins can interfere with multiple chemistry assays. We want to investigate the mechanisms of immunoglobulin interference. Serum samples containing paraproteins from the index patient and eight additional patients were used to investigate the interference with the creatinine and total protein assays on the Beckman Coulter AU5400/2700 analyzer, and to determine the effects of pH and ionic strength on the precipitation of different immunoglobulins in these patient samples. The paraprotein interference with the creatinine and total protein assays was caused by the precipitation of IgM paraprotein in the index patient's samples under alkaline assay conditions. At extremely high pH (12-13) and extremely low pH (1-2) and low ionic strength, paraprotein formed large aggregates in samples from the index patient but not from other patients. The pH and ionic strength are the key factors that contribute to protein aggregation and precipitation which interfere with the creatinine and total protein measurements on AU5400/2700. The different amino acid sequence of each monoclonal paraprotein will determine the pH and ionic strength at which the paraprotein will precipitate.

Preliminary Studies on Oleochemical Wastewater Treatment using Submerged Bed Biofilm Reactor (SBBR)

NASA Astrophysics Data System (ADS)

Ismail, Z.; Mahmood, N. A. N.; Ghafar, U. S. A.; Umor, N. A.; Muhammad, S. A. F.

2017-06-01

Wastewater discharge from the industry into water sources is one of the main reason for water pollution. The oleochemicals industry effluent produces high content of chemical oxygen demand (COD) with value between 6000-20,000 ppm. Effective treatment is required before wastewater effluent is discharged to environment. The aim of the study is to develop submerged bed biofilm reactor (SBBR) with packing materials in the cosmoball® carrier. Water quality such as chemical oxygen demands (COD), turbidity and pH were analysed. The result shows that the initial COD of 6000 ppm was reduced below 200 ppm. The optimum conditions for SBBR were obtained when green sponges used as packing material in cosmoball® effluent flowrate set at 100 mL/min; 1:1 ratio of cosmoball® volume to reactor volume and 1:1 ratio of active sludge (mixed culture) volume to reactor volume. Turbidity and pH were recorded with 9.0 NTU and 7.0 respectively, which indicated that SBBR is feasible as an alternative for conventional biological treatment in oleochemical industry.

USAF/SCEEE Summer Faculty Research Program (1982). Research Reports. Volume 2.

DTIC Science & Technology

1982-10-01

Engineering (802) 658-3330 Assigned: RADC/Griffiss Dr. Milton J. Alexander Degree: D.B.A., Management , 1968 Professor Specialty: Management ...Information Auburn University Systems, Operational Management Department Research Auburn, AL 36830 Assigned: LMC (205) 826-4730 Dr. Gary L. Allen Degree: Ph.D...Ph.D., Industrial Professor Engineering, 1951 Oklahoma State University Specialty: Project Management , Industrial Engineering & Management Dept

Precipitation of a monoclonal antibody by soluble tungsten.

PubMed

Bee, Jared S; Nelson, Stephanie A; Freund, Erwin; Carpenter, John F; Randolph, Theodore W

2009-09-01

Tungsten microparticles may be introduced into some pre-filled syringes during the creation of the needle hole. In turn, these microcontaminants may interact with protein therapeutics to produce visible particles. We found that soluble tungsten polyanions formed in acidic buffer below pH 6.0 can precipitate a monoclonal antibody within seconds. Soluble tungsten in pH 5.0 buffer at about 3 ppm was enough to cause precipitation of a mAb formulated at 0.02 mg/mL. The secondary structure of the protein was near-native in the collected precipitate. Our observations are consistent with the coagulation of a monoclonal antibody by tungsten polyanions. Tungsten-induced precipitation should only be a concern for proteins formulated below about pH 6.0 since tungsten polyanions are not formed at higher pHs. We speculate that the heterogenous nature of particle contamination within the poorly mixed syringe tip volume could mean that a specification for tungsten contamination based on the entire syringe volume is not appropriate. The potential potency of tungsten metal contamination is highlighted by the small number of particles that would be required to generate soluble tungsten levels needed to coagulate this antibody at pH 5.0.

Precipitation of a Monoclonal Antibody by Soluble Tungsten

PubMed Central

Bee, Jared S.; Nelson, Stephanie A.; Freund, Erwin; Carpenter, John F.; Randolph, Theodore W.

2009-01-01

Tungsten microparticles may be introduced into some pre-filled syringes during the creation of the needle hole. In turn, these microcontaminants may interact with protein therapeutics to produce visible particles. We found that soluble tungsten polyanions formed in acidic buffer below pH 6.0 can precipitate a monoclonal antibody within seconds. Soluble tungsten in pH 5.0 buffer at about 3 ppm was enough to cause precipitation of a mAb formulated at 0.02 mg/mL. The secondary structure of the protein was near-native in the collected precipitate. Our observations are consistent with the coagulation of a monoclonal antibody by tungsten polyanions. Tungsten-induced precipitation should only be a concern for proteins formulated below about pH 6.0 since tungsten polyanions are not formed at higher pHs. We speculate that the heterogenous nature of particle contamination within the poorly mixed syringe tip volume could mean that a specification for tungsten contamination based on the entire syringe volume is not appropriate. The potential potency of tungsten metal contamination is highlighted by the small number of particles that would be required to generate soluble tungsten levels needed to coagulate this antibody at pH 5.0. PMID:19230018

Protein separation through preliminary experiments concerning pH and salt concentration by tube radial distribution chromatography based on phase separation multiphase flow using a polytetrafluoroethylene capillary tube.

PubMed

Kan, Hyo; Tsukagoshi, Kazuhiko

2017-07-01

Protein mixtures were separated using tube radial distribution chromatography (TRDC) in a polytetrafluoroethylene (PTFE) capillary (internal diameter=100µm) separation tube. Separation by TRDC is based on the annular flow in phase separation multiphase flow and features an open-tube capillary without the use of specific packing agents or application of high voltages. Preliminary experiments were conducted to examine the effects of pH and salt concentration on the phase diagram of the ternary mixed solvent solution of water-acetonitrile-ethyl acetate (8:2:1 volume ratio) and on the TRDC system using the ternary mixed solvent solution. A model protein mixture containing peroxidase, lysozyme, and bovine serum albumin was analyzed via TRDC with the ternary mixed solvent solution at various pH values, i.e., buffer-acetonitrile-ethyl acetate (8:2:1 volume ratio). Protein was separated on the chromatograms by the TRDC system, where the elution order was determined by the relation between the isoelectric points of protein and the pH values of the solvent solution. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of new portable miniaturize solid phase microextraction of silver-APDC complex using micropipette tip in-syringe system couple with electrothermal atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Naeemullah; Kazi, Tasneem Gul; Afridi, Hassan Imran; Shah, Faheem; Arain, Sadaf Sadia; Arain, Salma Aslam; Panhwar, Abdul Haleem; Arain, Mariam Shahzadi; Samoon, Muhammad Kashif

2016-02-01

An innovative and simple miniaturized solid phase microextraction (M-SPME) method, was developed for preconcentration and determination of silver(I) in the fresh and waste water samples. For M-SPME, a micropipette tip packed with activated carbon cloth (ACC) as sorbent, in a syringe system. The size, morphology and elemental composition of ACC before and after adsorption of analyte have been characterized by scanning electron microscopy and energy dispersive spectroscopy. The sample solution treated with a complexing reagent, ammonium pyrrolidine dithiocarbamate (APDC), was drawn into the syringe filled with ACC and dispensed manually for 2 to 10 aspirating/dispensing cycle. Then the Ag- complex sorbed on the ACC in micropipette was quantitatively eluted by drawing and dispensing of different concentrations of acids for 2 to 5 aspirating/dispensing cycles. The extracted Ag ions with modifier were injected directly into the electrothermal atomic absorption spectrometry for analysis. The influence of different variables on the extraction efficiency, including the concentration of ligand, pH, sample volume, eluent type, concentration and volume was investigated. Validity and accuracy of the developed method was checked by the standard addition method. Reliability of the proposed methodology was checked by the relative standard deviation (%RSD), which was found to be < 5%. Under the optimized experimental variables, the limits of detection (LOD) and enhancement factors (EF), were obtained to be 0.86 ng L- 1 and 120, respectively. The proposed method was successfully applied for the determination of trace levels of silver ions in fresh and waste water samples.

Development of a Plastic Embedding Method for Large-Volume and Fluorescent-Protein-Expressing Tissues

PubMed Central

Yang, Zhongqin; Hu, Bihe; Zhang, Yuhui; Luo, Qingming; Gong, Hui

2013-01-01

Fluorescent proteins serve as important biomarkers for visualizing both subcellular organelles in living cells and structural and functional details in large-volume tissues or organs. However, current techniques for plastic embedding are limited in their ability to preserve fluorescence while remaining suitable for micro-optical sectioning tomography of large-volume samples. In this study, we quantitatively evaluated the fluorescence preservation and penetration time of several commonly used resins in a Thy1-eYFP-H transgenic whole mouse brain, including glycol methacrylate (GMA), LR White, hydroxypropyl methacrylate (HPMA) and Unicryl. We found that HMPA embedding doubled the eYFP fluorescence intensity but required long durations of incubation for whole brain penetration. GMA, Unicryl and LR White each penetrated the brain rapidly but also led to variable quenching of eYFP fluorescence. Among the fast-penetrating resins, GMA preserved fluorescence better than LR White and Unicryl. We found that we could optimize the GMA formulation by reducing the polymerization temperature, removing 4-methoxyphenol and adjusting the pH of the resin solution to be alkaline. By optimizing the GMA formulation, we increased percentage of eYFP fluorescence preservation in GMA-embedded brains nearly two-fold. These results suggest that modified GMA is suitable for embedding large-volume tissues such as whole mouse brain and provide a novel approach for visualizing brain-wide networks. PMID:23577174

Development of a γ-alumina- nanoparticle-functionalized porous polymer monolith for the enrichment of Sudan dyes in red wine samples.

PubMed

Li, Wanjun; Zhou, Xiao; Ye, Juanjuan; Jia, Qiong

2013-10-01

Monolithic materials were synthesized in capillaries by in situ polymerization with N-isopropylacrylamide, glycidyl methacrylate, and ethylene dimethacrylate as the monomers, and methanol and PEG as the porogens. With γ-alumina nanoparticles attached to the surface of the porous monolithic column via epoxide groups, a novel polymer monolith microextraction (PMME) material was prepared with a good mechanical stability and a high extraction capacity. SEM and X-ray photoelectron spectroscopy were employed to characterize the modified monolithic column, demonstrating that γ-alumina nanoparticles were effectively functionalized onto the monolithic column. In addition, a new method was developed for the analysis of Sudan I-IV dyes using PMME coupled with HPLC. In order to obtain the optimum extraction efficiency, the PMME conditions including desorption solvent type, sample pH, sample volume, sample flow rate, and eluent flow rate were investigated. Under the optimum conditions, we obtained acceptable linearities, low LODs, and good intra- and interday RDSs. When applied to the determination of Sudan I-IV dyes in red wine samples, satisfactory recoveries were obtained in the range of 84.0-115.9%. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis, characterization and application of a new chelating resin for solid phase extraction, preconcentration and determination of trace metals in some dairy samples by flame atomic absorption spectrometry.

PubMed

Daşbaşı, Teslima; Saçmacı, Şerife; Çankaya, Nevin; Soykan, Cengiz

2016-11-15

In this study, a simple and rapid solid phase extraction/preconcentration procedure was developed for determination of Cd(II), Co(II), Cr(III), Cu(II), Fe(III), Mn(II), Pb(II), and Zn(II) trace metals by flame atomic absorption spectrometry (FAAS). A new chelating resin, poly(N-cyclohexylacrylamide-co-divinylbenzene-co-2-acrylamido-2-methyl-1-propanesulfonic acid) (NCA-co-DVB-co-AMPS) (hereafter CDAP) was synthesized and characterized. The influences of the analytical parameters such as pH of the sample solution, type and concentration of eluent, flow rates of the sample and eluent, volume of the sample and eluent, amount of chelating resin, and interference of ions were examined. The limit of detection (LOD) of analytes were found (3s) to be in the range of 0.65-1.90μgL(-1). Preconcentration factor (PF) of 200 and the relative standard deviation (RSD) of ⩽2% were achieved (n=11). The developed method was applied for determination of analytes in some dairy samples and certified reference materials. Copyright © 2016 Elsevier Ltd. All rights reserved.

Flow injection analysis-flame atomic absorption spectrometry system for indirect determination of sulfite after on-line reduction of solid-phase manganese (IV) dioxide reactor.

PubMed

Zare-Dorabei, Rouholah; Boroun, Shokoufeh; Noroozifar, Meissam

2018-02-01

A new and simple flow injection method followed by atomic absorption spectrometry was developed for indirect determination of sulfite. The proposed method is based on the oxidation of sulfite to sulphate ion using solid-phase manganese dioxide (30% W/W suspended on silica gel beads) reactor. MnO 2 will be reduced to Mn(II) by sample injection in to the column under acidic carrier stream of HNO 3 (pH 2) with flow rate of 3.5mLmin -1 at room temperature. Absorption measurement of Mn(II) which is proportional to the concentration of sulfite in the sample was carried out by atomic absorption spectrometry. The calibration curve was linear up to 25mgL -1 with a detection limit (DL) of 0.08mgL -1 for 400µL injection sample volume. The presented method is efficient toward sulfite determination in sugar and water samples with a relative standard deviation (RSD) less than 1.2% and a sampling rate of about 60h -1 . Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of Iodate in Food, Environmental, and Biological Samples after Solid-Phase Extraction with Ni-Al-Zr Ternary Layered Double Hydroxide as a Nanosorbent

PubMed Central

Abdolmohammad-Zadeh, Hossein; Tavarid, Keyvan; Talleb, Zeynab

2012-01-01

Nanostructured nickel-aluminum-zirconium ternary layered double hydroxide was successfully applied as a solid-phase extraction sorbent for the separation and pre-concentration of trace levels of iodate in food, environmental and biological samples. An indirect method was used for monitoring of the extracted iodate ions. The method is based on the reaction of the iodate with iodide in acidic solution to produce iodine, which can be spectrophotometrically monitored at 352 nm. The absorbance is directly proportional to the concentration of iodate in the sample. The effect of several parameters such as pH, sample flow rate, amount of nanosorbent, elution conditions, sample volume, and coexisting ions on the recovery was investigated. In the optimum experimental conditions, the limit of detection (3s) and enrichment factor were 0.12 μg mL−1 and 20, respectively. The calibration graph using the preconcentration system was linear in the range of 0.2–2.8 μg mL−1 with a correlation coefficient of 0.998. In order to validate the presented method, a certified reference material, NIST SRM 1549, was also analyzed. PMID:22619590

Effect of experimental technique on the determination of strontium distribution coefficients of a surficial sediment from the Idaho National Engineering Laboratory, Idaho

USGS Publications Warehouse

Hemming, C.H.; Bunde, R.L.; Liszewski, M.J.; Rosentreter, J.J.; Welhan, J.

1997-01-01

The effect of experimental technique on strontium distribution coefficients (K(d)'s) was determined as part of an investigation of strontium geochemical transport properties of surficial sediment from the Idaho National Engineering Laboratory, Idaho. The investigation was conducted by the U.S. Geological Survey and Idaho State University, in cooperation with the U.S. Department of Energy. Batch experiments were conducted to quantify the effect of different experimental techniques on experimentally derived strontium K(d)'s at a fixed pH of 8.0. Combinations of three variables were investigated: method of sample agitation (rotating-mixer and shaker table), ratio of the mass-of-sediment to the volume-of-reaction-solution (1:2 and 1:20), and method of sediment preparation (crushed and non-crushed). Strontium K(d)'s ranged from 11 to 23 mlg-1 among all three experimental variables examined. Strontium K(d)'s were bimodally grouped around 12 and 21 mlg-1. Among the three experimental variables examined, the mass-to-volume ratio appeared to be the only one that could account for this bimodal distribution. The bimodal distribution of the derived strontium K(d)'s may occur because the two different mass-to-volume ratios represent different natural systems. The high mass-to-volume ratio of 1:2 models a natural system, such as an aquifer, in which there is an abundance of favorable sorption sites relative to the amount of strontium in solution. The low mass-to-volume ratio of 1:20 models a natural system, such as a stream, in which the relative amount of strontium in solution exceeds the favorable surface sorption site concentration. Except for low mass-to-volume ratios of non-crushed sediment using a rotating mixer, the method of agitation and sediment preparation appears to have little influence on derived strontium K(d)'s.The effect of experimental technique on strontium distribution coefficients (Kd's) was determined as part of an investigation of strontium geochemical transport properties of surficial sediment from the Idaho National Engineering Laboratory, Idaho. The investigation was conducted by the U.S. Geological Survey and Idaho State University, in cooperation with the U.S. Department of Energy. Batch experiments were conducted to quantify the effect of different experimental techniques on experimentally derived strontium Kd's at a fixed pH of 8.0. Combinations of three variables were investigated: method of sample agitation (rotating-mixer and shaker table), ratio of the mass-of-sediment to the volume-of-reaction-solution (1:2 and 1:20), and method of sediment preparation (crushed and non-crushed). Strontium Kd's ranged from 11 to 23 mlg-1 among all three experimental variables examined. Strontium Kd's were bimodally grouped around 12 and 21 mlg-1. Among the three experimental variables examined, the mass-to-volume ratio appeared to be the only one that could account for this bimodal distribution. The bimodal distribution of the derived strontium Kd's may occur because the two different mass-to-volume ratios represent different natural systems. The high mass-to-volume ratio of 1:2 models a natural system, such as an aquifer, in which there is an abundance of favorable sorption sites relative to the amount of strontium in solution. The low mass-to-volume ratio of 1:20 models a natural system, such as a stream, in which the relative amount of strontium in solution exceeds the favorable surface sorption site concentration. Except for low mass-to-volume ratios of non-crushed sediment using a rotating mixer, the method of agitation and sediment preparation appears to have little influence on derived strontium Kd's.

Room temperature ionic liquid-based dispersive liquid phase microextraction for the separation/preconcentration of trace Cd(2+) as 1-(2-pyridylazo)-2-naphthol (PAN) complex from environmental and biological samples and determined by FAAS.

PubMed

Khan, Sumaira; Soylak, Mustafa; Kazi, Tasneem Gul

2013-12-01

The current work develops a new green methodology for the separation/preconcentration of cadmium ions (Cd(2+)) using room temperature ionic liquid-dispersive liquid phase microextraction (RTIL-DLME) prior to analysis by flame atomic absorption spectrometry with microsample introduction system. Room temperature ionic liquids (RTIL) are considered "Green Solvents" for their thermally stable and non-volatile properties, here 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6] was used as an extractant. The preconcentration of Cd(2+) in different waters and acid digested scalp hair samples were complexed with 1-(2-pyridylazo)-2-naphthol and extracted into the fine drops of RTILs. Some significant factors influencing the extraction efficiency of Cd(2+) and its subsequent determination, including pH, amount of ligand, volume of RTIL, dispersant solvent, sample volume, temperature, and incubation time were investigated in detail. The limit of detection and the enhancement factor under the optimal conditions were 0.05 μg/L and 50, respectively. The relative standard deviation of 100 μg/L Cd(2+) was 4.3 %. The validity of the proposed method was checked by determining Cd(2+) in certified reference material (TM-25.3 fortified water). The sufficient recovery (>98 %) of Cd(2+) with the certified value. The mean concentrations of Cd in lake water 13.2, waste water 15.7 and hair sample 16.8 μg/L, respectively and the developed method was applied satisfactorily to the preconcentration and determination of Cd(2+) in real samples.

Rapid analysis of chlorinated anilines in environmental water samples using ultrasound assisted emulsification microextraction with solidification of floating organic droplet followed by HPLC-UV detection.

PubMed

Ramkumar, Abilasha; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon

2012-08-15

The present study demonstrates a simple, rapid and efficient method for the determination of chlorinated anilines (CAs) in environmental water samples using ultrasonication assisted emulsification microextraction technique based on solidification of floating organic droplet (USAEME-SFO) coupled with high performance liquid chromatography-ultraviolet (HPLC-UV) detection. In this extraction method, 1-dodecanol was used as extraction solvent which is of lower density than water, low toxicity, low volatility, and low melting point (24 °C). After the USAEME, extraction solvent could be collected easily by keeping the extraction tube in ice bath for 2 min and the solidified organic droplet was scooped out using a spatula and transferred to another glass vial and allowed to thaw. Then, 10 μL of extraction solvent was diluted with mobile phase (1:1) and taken for HPLC-UV analysis. Parameters influencing the extraction efficiency, such as the kind and volume of extraction solvent, volume of sample, ultrasonication time, pH and salt concentration were thoroughly examined and optimized. Under the optimal conditions, the method showed good linearity in the concentration range of 0.05-500 ng mL(-1) with correlation coefficients ranging from 0.9948 to 0.9957 for the three target CAs. The limit of detection based on signal to noise ratio of 3 ranged from 0.01 to 0.1 ng mL(-1). The relative standard deviations (RSDs) varied from 2.1 to 6.1% (n=3) and the enrichment factors ranged from 44 to 124. The proposed method has also been successfully applied to analyze real water samples and the relative recoveries of environmental water samples ranged from 81.1 to 116.9%. Copyright © 2012 Elsevier B.V. All rights reserved.

Synthesis and characterization of low-cost activated carbon prepared from Malawian baobab fruit shells by H3PO4 activation for removal of Cu(II) ions: equilibrium and kinetics studies

NASA Astrophysics Data System (ADS)

Vunain, Ephraim; Kenneth, Davie; Biswick, Timothy

2017-12-01

In this study, low-cost activated carbon (AC) prepared from baobab fruit shells by chemical activation using phosphoric acid was evaluated for the removal of Cu(II) ions from aqueous solution. The prepared activated carbon samples were characterized using N2-adsorption-desorption isotherms, SEM, FTIR, EDX and XRD analysis. The sample activated at 700 °C was chosen as our optimized sample because its physicochemical properties and BET results were similar to those of a commercial sample. The N2-adsorption-desorption results of the optimized sample revealed a BET surface area of 1089 m2/g, micropore volume of 0.3764 cm3/g, total pore volume of 0.4330 cm3/g and pore size of 1.45 nm. Operational parameters such as pH, initial copper concentration, contact time, adsorbent dosage and temperature were studied in a batch mode. Equilibrium data were obtained by testing the adsorption data using three different isotherm models: Langmuir, Freundlich and Dubinin-Radushkevish (D-R) models. It was found that the adsorption of copper correlated well with the Langmuir isotherm model with a maximum monolayer adsorption capacity of 3.0833 mg/g. The kinetics of the adsorption process was tested through pseudo-first-order and pseudo-second-order models. The pseudo-second-order kinetic model provided the best correlation for the experimental data studied. The adsorption followed chemisorption process. The study provided an effective use of baobab fruit shells as a valuable source of adsorbents for the removal of copper ions from aqueous solution. This study could add economic value to baobab fruit shells in Malawi, reduce disposal problems, and offer an economic source of AC to the AC users.

Simultaneous Determination of Procainamide and N-acetylprocainamide in Rat Plasma by Ultra-High-Pressure Liquid Chromatography Coupled with a Diode Array Detector and Its Application to a Pharmacokinetic Study in Rats.

PubMed

Balla, Anusha; Cho, Kwan Hyung; Kim, Yu Chul; Maeng, Han-Joo

2018-03-30

A simple, sensitive, and reliable reversed-phase, Ultra-High-Pressure Liquid Chromatography (UHPLC) coupled with a Diode Array Detector (DAD) method for the simultaneous determination of Procainamide (PA) and its major metabolite, N -acetylprocainamide (NAPA), in rat plasma was developed and validated. A simple deproteinization method with methanol was applied to the rat plasma samples, which were analyzed using UHPLC equipped with DAD at 280 nm, and a Synergi™ 4 µm polar, reversed-phase column using 1% acetic acid (pH 5.5) and methanol (76:24, v / v ) as eluent in isocratic mode at a flow rate 0.2 mL/min. The method showed good linearity ( r ² > 0.998) over the concentration range of 20-100,000 and 20-10,000 ng/mL for PA and NAPA, respectively. Intra- and inter-day accuracies ranged from 97.7 to 110.9%, and precision was <10.5% for PA and 99.7 to 109.2 and <10.5%, respectively, for NAPA. The lower limit of quantification was 20 ng/mL for both compounds. This is the first report of the UHPLC-DAD bioanalytical method for simultaneous measurement of PA and NAPA. The most obvious advantage of this method over previously reported HPLC methods is that it requires small sample and injection volumes, with a straightforward, one-step sample preparation. It overcomes the limitations of previous methods, which use large sample volume and complex sample preparation. The devised method was successfully applied to the quantification of PA and NAPA after an intravenous bolus administration of 10 mg/kg procainamide hydrochloride to rats.

Utilization of carrageenan, citric acid and cinnamon oil as an edible coating of chicken fillets to prolong its shelf life under refrigeration conditions.

PubMed

Khare, Anshul Kumar; Abraham, Robinson J J; Appa Rao, V; Babu, R Narendra

2016-02-01

The present study was conducted to determine efficacy of edible coating of carrageenan and cinnamon oil to enhance the shelf life of chicken meat stored under refrigeration conditions. Chicken breast was coated with carrageenan and cinnamon oil by three methods of application viz., spraying brushing and dipping. The coated meat was evaluated for drip loss, pH, thiobarbituric acid number (TBA), tyrosine value (TV), extract release volume (ERV), Warner-Bratzler shear force value (WBSFV), instrumental color, microbiological, and sensory qualities as per standard procedures. There was a significant difference observed for physicochemical parameters (pH, TBA, TV, ERV, drip loss and WBSFV) and microbiological analysis between storage periods in all the samples and between the control and treatments throughout the storage period but samples did not differed significantly for hunter color scores. However, there was no significant difference among three methods of application throughout the storage period though dipping had a lower rate of increase. A progressive decline in mean sensory scores was recorded along with the increase in storage time. The carrageenan and cinnamon edible coating was found to be a good alternative to enhance the shelf life of chicken meat under refrigeration conditions. It was also observed from study that dipping method of the application had comparatively higher shelf life than other methods of application.

Two-step liquid phase microextraction combined with capillary electrophoresis: a new approach to simultaneous determination of basic and zwitterionic compounds.

PubMed

Nojavan, Saeed; Moharami, Arezoo; Fakhari, Ali Reza

2012-08-01

In this work, two-step hollow fiber-based liquid-phase microextraction procedure was evaluated for extraction of the zwitterionic cetirizine (CTZ) and basic hydroxyzine (HZ) in human plasma. In the first step of extraction, the pH of sample was adjusted at 5.0 in order to promote liquid-phase microextraction of the zwitterionic CTZ. In the second step, the pH of sample was increased up to 11.0 for extraction of basic HZ. In this procedure, the extraction times for the first and the second steps were 30 and 20 min, respectively. Owing to the high ratio between the volumes of donor phase and acceptor phase, CTZ and HZ were enriched by factors of 280 and 355, respectively. The linearity of the analytical method was investigated for both compounds in the range of 10-500 ng mL(-1) (R(2) > 0.999). Limit of quantification (S/N = 10) for CTZ and HZ was 10 ng mL(-1) , while the limit of detection was 3 ng mL(-1) for both compounds at a signal to noise ratio of 3:1. Intraday and interday relative standard deviations (RSDs, n = 6) were in the range of 6.5-16.2%. This procedure enabled CTZ and HZ to be analyzed simultaneously by capillary electrophoresis. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analysis of Three Compounds in Flos Farfarae by Capillary Electrophoresis with Large-Volume Sample Stacking

PubMed Central

Hao, Zeng-Yan; Li, Lu; Huang, Ya-yun

2017-01-01

The aim of this study was to develop a method combining an online concentration and high-efficiency capillary electrophoresis separation to analyze and detect three compounds (rutin, hyperoside, and chlorogenic acid) in Flos Farfarae. In order to get good resolution and enrichment, several parameters such as the choice of running buffer, pH and concentration of the running buffer, organic modifier, temperature, and separation voltage were all investigated. The optimized conditions were obtained as follows: the buffer of 40 mM NaH2P04-40 mM Borax-30% v/v methanol (pH 9.0); the sample hydrodynamic injection of up to 4 s at 0.5 psi; 20 kV applied voltage. The diode-array detector was used, and the detection wavelength was 364 nm. Based on peak area, higher levels of selective and sensitive improvements in analysis were observed and about 14-, 26-, and 5-fold enrichment of rutin, hyperoside, and chlorogenic acid were achieved, respectively. This method was successfully applied to determine the three compounds in Flos Farfarae. The linear curve of peak response versus concentration was from 20 to 400 µg/ml, 16.5 to 330 µg/mL, and 25 to 500 µg/mL, respectively. The regression coefficients were 0.9998, 0.9999, and 0.9991, respectively. PMID:29056967

Eggshell membrane-based biotemplating of mixed hemimicelle/admicelle as a solid-phase extraction adsorbent for carcinogenic polycyclic aromatic hydrocarbons.

PubMed

Wang, Weidong; Chen, Bo; Huang, Yuming

2014-08-13

A new solid-phase extraction (SPE) format was demonstrated, based on eggshell membrane (ESM) templating of the mixed hemimicelle/admicelle of linear alkylbenzenesulfonates (LAS) as an adsorbent for the enrichment of carcinogenic polycyclic aromatic hydrocarbons (PAHs) in environmental aqueous samples. The LAS mixed hemimicelle/admicelle formation and SPE of the target PAHs were conducted simultaneously by adding the organic target and LAS through a column filled with 500 mg of ESM. The effect of various factors, including LAS concentration, solution pH, ionic strength, and humic acid concentration on the recoveries of PAHs were investigated and optimized. The results showed that LAS concentration and solution pH had obvious effect on extraction of PAHs, and the recoveries of PAHs compounds decreased in the presence of salt and humic acid. Under the optimized analytical conditions, the present method could respond down to 0.1-8.6 ng/L PAHs with a linear calibration ranging from 0.02 to 10 μg/L, showing a good PAHs enrichment ability with high sensitivity. The developed method was used satisfactorily for the detection of PAHs in environmental water samples. The mixed hemimicelle/admicelle adsorbent exhibited high extraction efficiency to PAHs and good selectivity with respect to natural organic matter and was advantageous over commercial C₁₈ adsorbent, for example, high extraction yield, high breakthrough volume, and easy regeneration.

Chemical characterization of rain water in a seasonally dry tropical region (Varanasi), India.

PubMed

Pandey, Jitendra; Singh, Ashima

2012-05-01

Rain water samples, covering 44 rain events of 2008 and 52 rain events of 2009, were collected at urban and suburban locations of Varanasi and analyzed for pH, conductivity and for metal and nutrient ions. The pH of rainwater varied between 6.3 and 7.9, with over 70% of samples having alkaline range. Volume weighed mean concentration of ions indicated Ca2+ (11.62- 41.60 microeq l(-1)) to be the most dominant species followed by SO4(2-) (4.7-25.2 microeq I(-1)), Na+ (1.60-10.25 microeq l(-1)), Mg2+ (0.22-7.21 microeq I(-1)), (NO3(-) (0.73-4.02 microeq l(-1)), K+(0.50-3.70 microeq l(-1)) and PO4(3-) (0.02-0.97 microeq l(-1)) respectively. Among the heavy metals, Cr (12.60 to 44.60 microg l(-1)), Zn (4.25 to 34.55 microg l(-1)) and Mn (10.62 to 28.40 microg l(-1)) were found to be the dominant component of rain water. The varimax rotation of PCA results extracted four major factors namely urban-industrial emission, crustal aerosols, wind transport and biomass burning accounting for 80% of the total variance. The study has relevance in establishing cause-effect relationships for terrestrial as well as for aquatic ecosystems.

Evaluation and source attribution of freshwater contributions to Kinvarra Bay, Ireland, using (222)Rn, EC and stable isotopes as natural indicators.

PubMed

Schubert, Michael; Knoeller, Kay; Rocha, Carlos; Einsiedl, Florian

2015-03-01

Freshwater discharge into the coastal sea is of general interest for two reasons: (i) It acts as vehicle for the transport of contaminants or nutrients into the ocean, and (ii) it indicates the loss of significant volumes of freshwater that might be needed for irrigation or drinking water supply. Due to the large-scale and long-term nature of the related hydrological processes, locating and quantitatively assessing freshwater discharge into the sea require naturally occurring tracers that allow fast, inexpensive and straightforward detection. In several studies, the standard water parameters electrical conductivity (EC) and pH have proven their suitability in this regard. However, while distribution patterns of EC and pH in the coastal sea indicate freshwater discharge in general, a separation between discharging surface water and submarine groundwater discharge (SGD) is not possible with these alone. The naturally occurring radionuclide radon-222 has been shown to be useful in the quantification of SGD and its distinction from surface runoff. This study aimed to evaluate and compare the informative value of the three parameters-EC, pH and radon concentration-in detecting and quantifying SGD by carrying out a case study in a bay located in western Ireland. The results reveal that radon activity is the most sensitive parameter for detecting SGD. However, only the combined evaluation of radon, EC and pH allows a quantitative allocation of groundwater and surface water contributions to the overall freshwater discharge into the sea. This conclusion is independently supported by stable isotope data measured on selected samples.

Functionalized nanoparticles based solid-phase membrane micro-tip extraction and high-performance liquid chromatography analyses of vitamin B complex in human plasma.

PubMed

Ali, Imran; Kulsum, Umma; Al-Othman, Zeid A; Alwarthan, Abdulrahman; Saleem, Kishwar

2016-07-01

Iron nanoparticles were prepared by a green method following functionalization using 1-butyl-3-methylimidazolium bromide. 1-Butyl-3-methylimidazole iron nanoparticles were characterized using FTIR spectroscopy, energy dispersive X-ray fluorescence, X-ray diffraction, scanning electron microscopy and transmission electron microscopy. The nanoparticles were used in solid-phase membrane micro-tip extraction to separate vitamin B complex from plasma before high-performance liquid chromatography. The optimum conditions obtained were sorbent (15 mg), agitation time (30 min), pH (9.0), desorbing solvent [water (5 mL) + methanol (5 mL) + sodium hydroxide (0.1 N) + acetic acid (d = 1.05 kg/L, pH 5.5), desorbing volume (10 mL) and desorption time (30 min). The percentage recoveries of all the eight vitamin B complex were from 60 to 83%. A high-performance liquid chromatography method was developed using a PhE column (250 × 4.6 mm, 5.0 μm) and water/acetonitrile (95:5, v/v; pH 4.0 with 0.1% formic acid) mobile phase. The flow rate was 1.0 mL/min with detection at 270 and 210 nm. The values of the capacity, separation and resolution factor were 0.57-39.47, 1.12-6.00 and 1.84-26.26, respectively. The developed sample preparation and chromatographic methods were fast, selective, inexpensive, economic and reproducible. The developed method can be applied for analyzing these drugs in biological and environmental matrices. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microplate-reader method for the rapid analysis of copper in natural waters with chemiluminescence detection.

PubMed

Durand, Axel; Chase, Zanna; Remenyi, Tomas; Quéroué, Fabien

2012-01-01

We have developed a method for the determination of copper in natural waters at nanomolar levels. The use of a microplate-reader minimizes sample processing time (~25 s per sample), reagent consumption (~120 μL per sample), and sample volume (~700 μL). Copper is detected by chemiluminescence. This technique is based on the formation of a complex between copper and 1,10-phenanthroline and the subsequent emission of light during the oxidation of the complex by hydrogen peroxide. Samples are acidified to pH 1.7 and then introduced directly into a 24-well plate. Reagents are added during data acquisition via two reagent injectors. When trace metal clean protocols are employed, the reproducibility is generally less than 7% on blanks and the detection limit is 0.7 nM for seawater and 0.4 nM for freshwater. More than 100 samples per hour can be analyzed with this technique, which is simple, robust, and amenable to at-sea analysis. Seawater samples from Storm Bay in Tasmania illustrate the utility of the method for environmental science. Indeed other trace metals for which optical detection methods exist (e.g., chemiluminescence, fluorescence, and absorbance) could be adapted to the microplate-reader.

Monomer volume fraction profiles in pH responsive planar polyelectrolyte brushes

DOE PAGES

Mahalik, Jyoti P.; Yang, Yubo; Deodhar, Chaitra V.; ...

2016-03-06

Spatial dependencies of monomer volume fraction profiles of pH responsive polyelectrolyte brushes were investigated using field theories and neutron reflectivity experiments. In particular, planar polyelectrolyte brushes in good solvent were studied and direct comparisons between predictions of the theories and experimental measurements are presented. The comparisons between the theories and the experimental data reveal that solvent entropy and ion-pairs resulting from adsorption of counterions from the added salt play key roles in affecting the monomer distribution and must be taken into account in modeling polyelectrolyte brushes. Furthermore, the utility of this physics-based approach based on these theories for the predictionmore » and interpretation of neutron reflectivity profiles in the context of pH responsive planar polyelectrolyte brushes such as polybasic poly(2-(dimethylamino)ethyl methacrylate) (PDMAEMA) and polyacidic poly(methacrylic acid) (PMAA) brushes is demonstrated. The approach provides a quantitative way of estimating molecular weights of the polymers polymerized using surface-initiated atom transfer radical polymerization.« less

Right Atrial Deformation in Predicting Outcomes in Pediatric Pulmonary Hypertension.

PubMed

Jone, Pei-Ni; Schäfer, Michal; Li, Ling; Craft, Mary; Ivy, D Dunbar; Kutty, Shelby

2017-12-01

Elevated right atrial (RA) pressure is a risk factor for mortality, and RA size is prognostic of adverse outcomes in pulmonary hypertension (PH). There is limited data on phasic RA function (reservoir, conduit, and pump) in pediatric PH. We sought to evaluate (1) the RA function in pediatric PH patients compared with controls, (2) compare the RA deformation indices with Doppler indices of diastolic dysfunction, functional capacity, biomarkers, invasive hemodynamics, and right ventricular functional indices, and (3) evaluate the potential of RA deformation indices to predict clinical outcomes. Sixty-six PH patients (mean age 7.9±4.7 years) were compared with 36 controls (7.7±4.4 years). RA and right ventricular deformation indices were obtained using 2-dimensional speckle tracking (2DCPA; TomTec, Germany). RA strain, strain rates, emptying fraction, and right ventricular longitudinal strain were measured. RA function was impaired in PH patients versus controls ( P <0.001). There were significant associations between RA function with invasive hemodynamics ( P <0.01). RA reservoir, pump function, the rate of RA filling, and atrial minimum volume predicted adverse clinical outcomes (hazard ratio [HR], 0.15; confidence interval [CI], 0.03-0.73; P <0.01; HR, 0.05; CI, 0.003-0.43; P <0.004; HR, 0.04; CI, 0.006-0.56; P <0.01; and HR, 8.6; CI, 1.6-37.2; P <0.01, respectively). RA deformation properties are significantly altered in pediatric PH patients. Progressive worsening of RA reservoir and conduit functions is related to changes in right ventricular diastolic dysfunction. RA reservoir function, pump function, the rate of atrial filling, and atrial minimum volume emerged as outcome predictors in pediatric PH. © 2017 American Heart Association, Inc.

A thermodynamic study of electroneutral K-Cl cotransport in pH- and volume-clamped low K sheep erythrocytes with normal and low internal magnesium.

PubMed

Lauf, P K; Adragna, N C

1996-10-01

Swelling-induced human erythrocyte K-Cl cotransport is membrane potential independent and capable of uphill transport. However, a complete thermodynamic analysis of basal and stimulated K-Cl cotransport, at constant cell volume, is missing. This study was performed in low K sheep red blood cells before and after reducing cellular free Mg into the nanomolar range with the divalent cation ionophore A23187 and a chelator, an intervention known to stimulate K-Cl cotransport. The anion exchange inhibitor 4,4'diisothiocyanato-2,2'disulfonic stilbene was used to clamp intracellular pH and Cl or NO3 concentrations. Cell volume was maintained constant as external and internal pH differed by more than two units. K-Cl cotransport was calculated from the K effluxes and Rb (as K congener) influxes measured in Cl and NO3, at constant internal K and external anions, and variable concentrations of extracellular Rb and internal anions, respectively. The external Rb concentration at which net K-Cl cotransport is zero was defined as flux reversal point which changed with internal pH and hence Cl. Plots of the ratio of external Rb concentrations corresponding to the flux reversal points and the internal K concentration versus the ratio of the internal and external Cl concentrations (i.e., the Donnan ratio of the transported ions) yielded slopes near unity for both control and low internal Mg cells. Thus, basal as well as low internal Mg-stimulated net K-Cl cotransport depends on the electrochemical potential gradient of KCl.

A thermodynamic study of electroneutral K-Cl cotransport in pH- and volume-clamped low K sheep erythrocytes with normal and low internal magnesium

PubMed Central

1996-01-01

Swelling-induced human erythrocyte K-Cl cotransport is membrane potential independent and capable of uphill transport. However, a complete thermodynamic analysis of basal and stimulated K-Cl cotransport, at constant cell volume, is missing. This study was performed in low K sheep red blood cells before and after reducing cellular free Mg into the nanomolar range with the divalent cation ionophore A23187 and a chelator, an intervention known to stimulate K- Cl cotransport. The anion exchange inhibitor 4,4'diisothiocyanato- 2,2'disulfonic stilbene was used to clamp intracellular pH and Cl or NO3 concentrations. Cell volume was maintained constant as external and internal pH differed by more than two units. K-Cl cotransport was calculated from the K effluxes and Rb (as K congener) influxes measured in Cl and NO3, at constant internal K and external anions, and variable concentrations of extracellular Rb and internal anions, respectively. The external Rb concentration at which net K-Cl cotransport is zero was defined as flux reversal point which changed with internal pH and hence Cl. Plots of the ratio of external Rb concentrations corresponding to the flux reversal points and the internal K concentration versus the ratio of the internal and external Cl concentrations (i.e., the Donnan ratio of the transported ions) yielded slopes near unity for both control and low internal Mg cells. Thus, basal as well as low internal Mg-stimulated net K-Cl cotransport depends on the electrochemical potential gradient of KCl. PMID:8894982

Magnetic sulfur-doped porous carbon for preconcentration of trace mercury in environmental water prior to ICP-MS detection.

PubMed

Peng, Chuyu; He, Man; Chen, Beibei; Huang, Lijin; Hu, Bin

2017-11-20

A novel magnetic sulfur-doped porous carbon (MSPC) was fabricated via a simple one-step carbonization of a mixture of sucrose, basic magnesium sulfate whiskers and Fe 3 O 4 @SiO 2 nanoparticles. Due to the high S content, the prepared MSPC possessed high adsorption capacity for Hg 2+ (343 mg g -1 ) with good selectivity. Based on this, a method coupling magnetic solid phase extraction (MSPE) with inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of trace Hg 2+ in environmental water samples. Various parameters such as pH, desorption solvent and its concentration, desorption volume and time, sample volume, and adsorption time that affect the determination have been optimized. Under the optimal conditions, a high enrichment factor of 100-fold was obtained, the limit of detection (LOD) was found to be 0.52 pg mL -1 with a relative standard deviation (c = 10 pg mL -1 , n = 7) of 7.1%, and a good linearity was obtained within the concentration range of 2-5000 pg mL -1 for Hg 2+ . Besides, the proposed method has very fast adsorption/desorption kinetics, target Hg 2+ could be rapidly adsorbed on the prepared MSPC in 2 min and desorbed from the MSPC in 2 min with the assistance of a permanent magnet. Therefore, the proposed method of MSPE-ICP-MS exhibits good application potential in the determination of trace Hg 2+ in environmental water samples.

Simultaneous extraction and determination of albendazole and triclabendazole by a novel syringe to syringe dispersive liquid phase microextraction-solidified floating organic drop combined with high performance liquid chromatography.

PubMed

Asadi, Mohammad; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad

2016-08-17

A syringe to syringe dispersive liquid phase microextraction-solidified floating organic drop was introduced and used for the simultaneous extraction of trace amounts of albendazole and triclabendazole from different matrices. The extracted analytes were determined by high performance liquid chromatography along with fluorescence detection. The analytical parameters affecting the microextraction efficiency including the nature and volume of the extraction solvent, sample volume, sample pH, ionic strength and the cycles of extraction were optimized. The calibration curves were linear in the range of 0.1-30.0 μg L(-1) and 0.2-30.0 μg L(-1) with determination coefficients of 0.9999 and 0.9998 for albendazole and triclabendazole respectively. The detection limits defined as three folds of the signal to noise ratio were found to be 0.02 μg L(-1) for albendazole and 0.06 μg L(-1) for triclabendazole. The inter-day and intra-day precision (RSD%) for both analytes at three concentration levels (0.5, 2.0 and 10.0 μg L(-1)) were in the range of 6.3-10.1% and 5.0-7.5% respectively. The developed method was successfully applied to determine albendazole and triclabendazole in water, cow milk, honey, and urine samples. Copyright © 2016. Published by Elsevier B.V.

Depth matters: Soil pH and dilution effects in the northern Great Plains

USDA-ARS?s Scientific Manuscript database

In the northern Great Plans (NGP), surface sampling depths of 0-15.2 cm or 0-20.3 cm are suggested for testing soil characteristics such as pH. However, acidification is often most pronounced near-surface (e.g., <10 cm). Thus, sampling deeper can potentially dilute (increase) pH measurements and the...

Antibacterial and dissolution ability of sodium hypochlorite in different pHs on multi-species biofilms.

PubMed

del Carpio-Perochena, Aldo; Bramante, Clovis Monteiro; de Andrade, Flaviana Bombarda; Maliza, Amanda G Alves; Cavenago, Bruno Cavalini; Marciano, Marina A; Amoroso-Silva, Pablo; Duarte, Marco Hungaro

2015-11-01

The aim of this study was to investigate whether variation in pH of sodium hypochlorite (NaOCl) increased its antibacterial and dissolution ability on polymicrobial biofilms formed in situ. Fifty-six dentin blocks (eight/group) were intraorally infected for 48 h and incubated in BHI for 48 h to standardize the biofilm growth. The specimens were irrigated with 1 and 2.5% NaOCl with pH levels of 5, 7, and 12 for 20 min. The control group was irrigated with distilled water. The cell viability and the bacterial volume were measured at the pre- and post-irrigation procedures. Five random areas of each sample were chosen and analyzed with confocal laser scanning microscopy (CLSM). Statistical analysis was performed using the non-parametric Kruskal-Wallis and Dunn's tests (p < 0.05). All the experimental solutions were able to decrease the biomass (p < 0.05) except for the 1% NaOCl-pH 5 group. The antibacterial ability of the NaOCl was dependent on the concentration and acidification of the solution. The acidification of NaOCl improves its antibacterial ability, but the dissolution effect of the irrigant is decreased. Bacteria and their products are the main factors in development of apical periodontitis. The pH reduction in the NaOCl could enhance the reduction or elimination of the root canal bacterial colonies in comparison with the unaltered solution.

Optimized ultrasound-assisted emulsification microextraction for simultaneous trace multielement determination of heavy metals in real water samples by ICP-OES.

PubMed

Sereshti, Hassan; Heravi, Yeganeh Entezari; Samadi, Soheila

2012-08-15

Ultrasonic-assisted emulsification microextraction (USAEME) combined with inductively coupled plasma-optical emission spectrometry (ICP-OES) was used for preconcentration and determination of aluminum, bismuth, cadmium, cobalt, copper, iron, gallium, indium, nickel, lead, thallium and zinc in real water samples. Ammonium pyrrolidine dithiocarbamate (APDC) and carbon tetrachloride (CCl(4)) were used as the chelating agent and extraction solvent, respectively. The effective parameters (factors) of the extraction process such as volume of extraction solvent, pH, sonication time, and concentration of chelating agent were optimized by a small central composite design (CCD). The optimum conditions were found to be 98 μL for extraction solvent, 1476 mg L(-1) for chelating agent, 3.8 for pH and 9 min for sonication time. Under the optimal conditions, the limits of detection (LODs) for Al, Bi, Cd, Co, Cu, Fe, Ga, In, Ni, Pb, Tl and Zn were 0.13, 0.48, 0.19, 0.28, 0.29, 0.27, 0.27, 0.38, 0.44, 0.47, 0.52 and 0.17 μg L(-1), respectively. The linear dynamic range (LDR) was 1-1000 μ gL(-1) with determination coefficients of 0.991-0.998. Relative standard deviations (RSDs, C=200 μg L(-1), n=6) were between 1.87%-5.65%. The proposed method was successfully applied to the extraction and determination of heavy metals in real water samples and the satisfactory relative recoveries (90.3%-105.5%) were obtained. Copyright © 2012 Elsevier B.V. All rights reserved.

Ion-pair vortex assisted liquid-liquid microextraction with back extraction coupled with high performance liquid chromatography-UV for the determination of metformin in plasma.

PubMed

Alshishani, Anas; Makahleh, Ahmad; Yap, Hui Fang; Gubartallah, Elbaleeq Adam; Salhimi, Salizawati Muhamad; Saad, Bahruddin

2016-12-01

A new sample preparation method, ion-pair vortex assisted liquid-liquid microextraction (VALLME-BE), for the determination of a highly polar anti-diabetic drug (metformin) in plasma sample was developed. The VALLME-BE was performed by diluting the plasma in borate buffer and extracted to 150µL 1-octanol containing 0.2M di-(2-ethylhexyl)phosphoric acid as intermediate phase. The drug was next back-extracted into 20µL of 0.075M HCl solution. The effects of pH, ion-pair concentration, type of organic solvent, volume of extraction phases, ionic strength, vortexing and centrifugation times on the extraction efficiency were investigated. The optimum conditions were at pH 9.3, 60s vortexing and 2min centrifugation. The microextract, contained metformin and buformin (internal standard), was directly injected into a HPLC unit using C1 column (250mm×4.6mm×10µm) and detected at 235nm. The method was validated and calibration curve was linear with r 2 >0.99 over the range of 20-2000µgL -1 . The limits of detection and quantitation were 1.4 and 4.1µgL -1 , respectively. The accuracy was within 94.8-108% of the nominal concentration. The relative standard deviation for inter- and intra-day precision was less than 10.8%. The method was conveniently applied for the determination of metformin in plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Combined solid-phase extraction and gas chromatography-mass spectrometry used for determination of chloropropanols in water.

PubMed

González, Paula; Racamonde, Inés; Carro, Antonia M; Lorenzo, Rosa A

2011-10-01

A sensitive and rapid derivatization method for the simultaneous determination of 1,3-dichloro-2-propanol (1,3-DCP) and 3-chloropropane-1,2-diol (3-MCPD) in water samples has been developed. The aim was to research the optimal conditions of the derivatization process for two selected reagents. A central composite design was used to determine the influence of derivatization time, derivatization temperature and reagent volume. A global desirability function was applied for multi-response optimization. The analysis was performed by gas chromatography-mass spectrometry. During the optimization of the extraction procedure, four different types of solid-phase extraction (SPE) columns were tested. It was demonstrated that the Oasis HLB cartridge produced the best recoveries of the target analytes. The pH value and the salinity were investigated using a Doehlert design. The best results for the SPE of both analytes were obtained with 1.5 g of NaCl and pH 6. The proposed method provides high sensitivity, good linearity (R(2)≥0.999) and repeatability (relative standard deviations % between 2.9 and 3.4%). Limits of detection and quantification were in the range of 1.4-11.2 ng/mL and 4.8-34.5 ng/mL, respectively. Recoveries obtained for water samples were ca. 100% for 1,3-DCP and 3-MCPD. The method has been successfully applied to the analysis of different samples including commercially bottled water, an influent and effluent sewage. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Association of digital cushion thickness with sole temperature measured with the use of infrared thermography.

PubMed

Oikonomou, G; Trojacanec, P; Ganda, E K; Bicalho, M L S; Bicalho, R C

2014-07-01

The main objective of this study was to investigate the association between digital cushion thickness and sole temperature measured by infrared thermography. Data were collected from 216 lactating Holstein cows at 4 to 10d in milk (DIM). Cows were locomotion scored and sole temperature was measured after claw trimming (a minimum delay of 3 min was allowed for the hoof to cool) using an infrared thermography camera. Temperature was measured at the typical ulcer site of the lateral digit of the left hind foot. Immediately after the thermographic image was obtained, the thickness of the digital cushion was measured by ultrasonography. Rumen fluid samples were collected with a stomach tube and sample pH was measured immediately after collection. Additionally, a blood sample was obtained and used for measurements of serum concentrations of β-hydroxybutyrate (BHBA), nonesterified fatty acids (NEFA), and haptoglobin. To evaluate the associations of digital cushion thickness with sole temperature, a linear regression model was built using the GLIMMIX procedure in SAS software (SAS Institute Inc., Cary, NC). Sole temperature was the response variable, and digital cushion thickness quartiles, locomotion score group, rumen fluid pH, rumen fluid sample volume, environmental temperature, age in days, and serum levels of NEFA, BHBA, and haptoglobin were fitted in the model. Only significant variables were retained in the final model. Simple linear regression scatter plots were used to illustrate associations between sole temperature (measured by infrared thermography at the typical ulcer site) and environmental temperature and between NEFA and BHBA serum levels and haptoglobin. One-way ANOVA was used to compare rumen fluid pH for different locomotion score groups and for different digital cushion quartiles. Results from the multivariable linear regression model showed that sole temperature increased as locomotion scores increased and decreased as digital cushion thickness increased. These results were adjusted for environmental temperature, which was significantly associated with sole temperature. Serum levels of NEFA, BHBA, and haptoglobin were not associated with sole temperature. However, significant correlations existed between serum levels of NEFA and haptoglobin and between serum levels of BHBA and haptoglobin. Rumen fluid pH was not associated with either locomotion score or digital cushion thickness. In conclusion, we show here that digital cushion thickness was associated with sole temperature in cows at 4 to 10 DIM. Copyright © 2014 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Use of a control test to aid pH assessment of chemical eye injuries.

PubMed

Connor, A J; Severn, P

2009-11-01

Chemical burns of the eye represent 7.0%-9.9% of all ocular trauma. Initial management of ocular chemical injuries is irrigation of the eye and conjunctival sac until neutralisation of the tear surface pH is achieved.We present a case of alkali injury in which the raised tear film pH seemed to be unresponsive to irrigation treatment. Suspicion was raised about the accuracy of the litmus paper used to test the tear film pH. The error was confirmed by use of a control litmus pH test of the examining doctor's eyes. Errors in litmus paper pH measurement can occur because of difficulty in matching the paper with scale colours and drying of the paper, which produces a darker colour. A small tear film sample can also create difficulty in colour matching, whereas too large a sample can wash away pigment from the litmus paper. Samples measured too quickly after irrigation can result in a falsely neutral pH measurement. Use of faulty or inappropriate materials can also result in errors. We advocate the use of control litmus pH test in all patients. This would highlight errors in pH measurements and aid in the detection of the end point of irrigation.

Evaluation of metal ion absorptive characteristics of three types of plastic sample bags used for pecipitation sampling

USGS Publications Warehouse

Good, A.B.; Schroder, L.J.

1984-01-01

Simulated precipitation samples containing 16 metal ions were prepared at 4 pH values. Absorptive characteristics of polypropylene, polyethylene, and polyester/polyolefin sacks were evaluated at pH 3.5, 4.0, 4.5, and 5.0. Simulated precipitation was in contact with the sacks for 17 days, and subsamples were removed for chemical analysis at 3, 7, 10, 14, and 17 days after initial contact. All three types of plastic sacks absorbed Fe throughout the entire pH range. Polypropylene and polyethylene absorbed Pb throughout the entire pH range; polyester/polyolefin sacks absorbed Pb at pH 4.0 or greater. All plastic sacks also absorbed Cu, Mo, and V at pH 4.5 and 5.0. Leaching the plastic sacks with 0.7 percent HNO3 did not result in 100 percent of Cu, Fe, Pb, and V. These sacks would be suitable collection vessels for Ba, Be, Ca, Cd, Co, Li, Mg, Mn, Na Sr and Zn in precipitation through the pH range of 3.5 to 5.0.

Comparison of pH and refractometry index with calcium concentrations in preparturient mammary gland secretions of mares.

PubMed

Korosue, Kenji; Murase, Harutaka; Sato, Fumio; Ishimaru, Mutsuki; Kotoyori, Yasumitsu; Tsujimura, Koji; Nambo, Yasuo

2013-01-15

To test the usefulness of measuring pH and refractometry index, compared with measuring calcium carbonate concentration, of preparturient mammary gland secretions for predicting parturition in mares. Evaluation study. 27 pregnant Thoroughbred mares. Preparturient mammary gland secretion samples were obtained once or twice daily 10 days prior to foaling until parturition. The samples were analyzed for calcium carbonate concentration with a water hardness kit (151 samples), pH with pH test paper (222 samples), and refractometry index with a Brix refractometer (214 samples). The sensitivity, specificity, and positive and negative predictive values for each test were calculated for evaluation of predicting parturition. The PPV within 72 hours and the NPV within 24 hours for calcium carbonate concentration determination (standard value set to 400 μg/g) were 93.8% and 98.3%, respectively. The PPV within 72 hours and the NPV within 24 hours for the pH test (standard value set at 6.4) were 97.9% and 99.4%, respectively. The PPV within 72 hours and the NPV within 24 hours for the Brix test (standard value set to 20%) were 73.2% and 96.5%, respectively. Results suggested that the pH test with the standard value set at a pH of 6.4 would be useful in the management of preparturient mares by predicting when mares are not ready to foal. This was accomplished with equal effectiveness of measuring calcium carbonate concentration with a water hardness kit.

Positive affect, negative affect, and physiological hyperarousal among referred and nonreferred youths.

PubMed

Laurent, Jeff; Joiner, Thomas E; Catanzaro, Salvatore J

2011-12-01

The Positive and Negative Affect Scale for Children (PANAS-C) and the Physiological Hyperarousal Scale for Children (PH-C) seem ideal measures for school mental health screenings, because they are theory based, psychometrically sound, and brief. This study provides descriptive information and preliminary cutoff scores in an effort to increase the practical utility of the measures. Scores on the PANAS-C Positive Affect (PA) and Negative Affect (NA) scales and the PH-C were compared for a general sample of schoolchildren (n = 226), a group of students referred for special education services (n = 83), and youths on an inpatient psychiatric unit (n = 37). Expected patterns of scores emerged for the general school and referred school samples, although only scores on the PH-C were statistically significantly different. Differences in scores between the general school and inpatient samples were significant for all 3 scales. Differences in scores between the referred school and inpatient samples were significant for the NA scale and the PH-C but not for the PA scale. In addition, we used traditional self-report measures to form groups of normal, anxious, depressed, and mixed anxious and depressed youths. Again, predicted general patterns of PA, NA and PH scores were supported, although statistical differences were not always evident. In particular, scores on the PH-C for the anxious and depressed groups were inconsistent with predictions. Possible reasons related to sample and scale issues are discussed. Finally, preliminary cutoff scores were proposed for the PANAS-C scales and the PH-C.

Visualization of Buffer Capacity with 3-D "Topo" Surfaces: Buffer Ridges, Equivalence Point Canyons and Dilution Ramps

ERIC Educational Resources Information Center

Smith, Garon C.; Hossain, Md Mainul

2016-01-01

BufCap TOPOS is free software that generates 3-D topographical surfaces ("topos") for acid-base equilibrium studies. It portrays pH and buffer capacity behavior during titration and dilution procedures. Topo surfaces are created by plotting computed pH and buffer capacity values above a composition grid with volume of NaOH as the x axis…

Low temperature synthesis of polyaniline-crystalline TiO2-halloysite composite nanotubes with enhanced visible light photocatalytic activity.

PubMed

Li, Cuiping; Wang, Jie; Guo, Hong; Ding, Shujiang

2015-11-15

A series of one-dimensional polyaniline-crystalline TiO2-halloysite composite nanotubes with different mass ratio of polyaniline to TiO2 are facilely prepared by employing the low-temperature synthesis of crystalline TiO2 on halloysite nanotubes. The halloysite nanotubes can adsorb TiO2/polyaniline precursors and induce TiO2 nanocrystals/polyaniline to grow on the support in situ simultaneously. By simply adjusting the acidity of reaction system, PANI-crystalline TiO2-HA composite nanotubes composed of anatase, a mixed phase TiO2 and different PANI redox state are obtained. The XRD and UV-vis results show that the surface polyaniline sensitization has no effect on the crystalline structure of halloysite and TiO2 and the light response of TiO2 is extended to visible-light regions. Photocatalysis test results reveal the photocatalytic activity will be affected by the pH value and the volume ratio of ANI to TTIP. The highest photocatalytic activity is achieved with the composite photocatalysts prepared at pH 0.5 and 1% volume ratio of ANI and TTIP owing to the sensitizing effect of polyaniline and the charge transfer from the photoexcited PANI sensitizer to TiO2. Moreover, the PANI-TiO2-HA composite nanotubes synthesized by one-step at pH 0.5 with 1% volume ratio of ANI to TTIP exhibit higher visible light photocatalytic activity than those synthesized by the two-step. Heterogeneous PANI-TiO2-HA composite nanotubes prepared at pH 0.5 exhibit a higher degradation activity than that prepared at pH 1.5. The redoped experiment proves that the PANI redox state plays the main contribution to the enhanced visible light catalytic degradation efficiency of PANI-TiO2-HA prepared at pH 0.5. Furthermore, the heterogeneous PANI-crystalline TiO2-HA nanotubes have good photocatalytic stability and can be reused four times with only gradual loss of activity under visible light irradiation. Copyright © 2015 Elsevier Inc. All rights reserved.

Effect of induced ruminal acidosis on blood variables in heifers

PubMed Central

2013-01-01

Background Ruminal acidosis is responsible for the onset of different pathologies in dairy and feedlot cattle, but there are major difficulties in the diagnosis. This study modelled the data obtained from various blood variables to identify those that could indicate the severity of ruminal acidosis. Six heifers were fed three experimental rations throughout three periods. The diets were characterised by different starch levels: high starch (HS), medium starch (MS) and low starch, as the control diet (CT). Ruminal pH values were continuously measured using wireless sensors and compared with pH measurements obtained by rumenocentesis. Blood samples were analysed for complete blood count, biochemical profile, venous blood gas, blood lipopolysaccharide (LPS) and LPS-binding proteins (LBP). Results The regression coefficient comparing the ruminal pH values, obtained using the two methods, was 0.56 (P = 0.040). Feeding the CT, MS and HS led to differences in the time spent below the 5.8, 5.5 and 5.0 pH thresholds and in several variables, including dry matter intake (7.7 vs. 6.9 vs. 5.1 kg/d; P = 0.002), ruminal nadir pH (5.69 vs. 5.47 vs. 5.44; P = 0.042), mean ruminal pH (6.50 vs. 6.34 vs. 6.31; P = 0.012), haemoglobin level (11.1 vs. 10.9 vs. 11.4 g/dL; P = 0.010), platelet count (506 vs. 481 vs. 601; P = 0.008), HCO3- (31.8 vs. 31.3 vs. 30.6 mmol/L; P = 0.071) and LBP (5.9 vs. 9.5 vs. 10.5 μg/mL; P < 0.001). A canonical discriminant analysis (CDA) was used to classify the animals into four ruminal pH classes (normal, risk of acidosis, subacute ruminal acidosis and acute ruminal acidosis) using haemoglobin, mean platelet volume, β-hydroxybutyrate, glucose and reduced haemoglobin. Conclusions Although additional studies are necessary to confirm the reliability of these discriminant functions, the use of plasma variables in a multifactorial model appeared to be useful for the evaluation of ruminal acidosis severity. PMID:23647881

Effect of induced ruminal acidosis on blood variables in heifers.

PubMed

Marchesini, Giorgio; De Nardi, Roberta; Gianesella, Matteo; Stefani, Anna-Lisa; Morgante, Massimo; Barberio, Antonio; Andrighetto, Igino; Segato, Severino

2013-05-06

Ruminal acidosis is responsible for the onset of different pathologies in dairy and feedlot cattle, but there are major difficulties in the diagnosis. This study modelled the data obtained from various blood variables to identify those that could indicate the severity of ruminal acidosis. Six heifers were fed three experimental rations throughout three periods. The diets were characterised by different starch levels: high starch (HS), medium starch (MS) and low starch, as the control diet (CT). Ruminal pH values were continuously measured using wireless sensors and compared with pH measurements obtained by rumenocentesis. Blood samples were analysed for complete blood count, biochemical profile, venous blood gas, blood lipopolysaccharide (LPS) and LPS-binding proteins (LBP). The regression coefficient comparing the ruminal pH values, obtained using the two methods, was 0.56 (P = 0.040). Feeding the CT, MS and HS led to differences in the time spent below the 5.8, 5.5 and 5.0 pH thresholds and in several variables, including dry matter intake (7.7 vs. 6.9 vs. 5.1 kg/d; P = 0.002), ruminal nadir pH (5.69 vs. 5.47 vs. 5.44; P = 0.042), mean ruminal pH (6.50 vs. 6.34 vs. 6.31; P = 0.012), haemoglobin level (11.1 vs. 10.9 vs. 11.4 g/dL; P = 0.010), platelet count (506 vs. 481 vs. 601; P = 0.008), HCO3(-) (31.8 vs. 31.3 vs. 30.6 mmol/L; P = 0.071) and LBP (5.9 vs. 9.5 vs. 10.5 μg/mL; P < 0.001). A canonical discriminant analysis (CDA) was used to classify the animals into four ruminal pH classes (normal, risk of acidosis, subacute ruminal acidosis and acute ruminal acidosis) using haemoglobin, mean platelet volume, β-hydroxybutyrate, glucose and reduced haemoglobin. Although additional studies are necessary to confirm the reliability of these discriminant functions, the use of plasma variables in a multifactorial model appeared to be useful for the evaluation of ruminal acidosis severity.

Dispersive liquid-liquid microextraction for the determination of vitamins D and K in foods by liquid chromatography with diode-array and atmospheric pressure chemical ionization-mass spectrometry detection.

PubMed

Viñas, Pilar; Bravo-Bravo, María; López-García, Ignacio; Hernández-Córdoba, Manuel

2013-10-15

A simple and rapid method was developed using reversed-phase liquid chromatography (LC) with both diode array (DAD) and atmospheric pressure chemical ionization mass spectrometric (APCI-MS) detection, for the simultaneous analysis of the vitamins ergocalciferol (D2), cholecalciferol (D3), phylloquinone (K1), menaquinone-4 (K2) and a synthetic form of vitamin K, menadione (K3). The Taguchi experimental method, an orthogonal array design (OAD), was used to optimize an efficient and clean preconcentration step based on dispersive liquid-liquid microextraction (DLLME). A factorial design was applied with six factors and three levels for each factor, namely, carbon tetrachloride volume, methanol volume, aqueous sample volume, pH of sample, sodium chloride concentration and time of the centrifugation step. The DLLME optimized procedure consisted of rapidly injecting 3 mL of acetonitrile (disperser solvent) containing 150 µL carbon tetrachloride (extraction solvent) into the aqueous sample, thereby forming a cloudy solution. Phase separation was performed by centrifugation, and the sedimented phase was evaporated with nitrogen, reconstituted with 50 µL of acetonitrile, and injected. The LC analyses were carried out using a mobile phase composed of acetonitrile, 2-propanol and water, under gradient elution. Quantification was carried out by the standard additions method. The APCI-MS spectra, in combination with UV spectra, permitted the correct identification of compounds in the food samples. The method was validated according to international guidelines and using a certified reference material. The validated method was applied for the analysis of vitamins D and K in infant foods and several green vegetables. There was little variability in the forms of vitamin K present in vegetables, with the most abundant vitamer in all the samples being phylloquinone, while menadione could not be detected. Conversely, cholecalciferol, which is present in food of animal origin, was the main form in infant foods, while ergocalciferol was not detected. Copyright © 2013 Elsevier B.V. All rights reserved.

Liquid-liquid microextraction of synthetic pigments in beverages using a hydrophobic deep eutectic solvent.

PubMed

Zhu, Shuqiang; Zhou, Jia; Jia, Hongfang; Zhang, Haixia

2018-03-15

A method was developed for the determination of eight synthetic pigments in beverage samples by liquid-liquid microextraction followed by high performance liquid chromatography. Using hydrophobic deep eutectic solvent (DES) as the microextraction solvent, several key parameters were optimized, including the type and volume of the hydrophobic DES, pH value, vortex time and salt content. Detection limits were in the range 0.016-1.12 ng/mL, recoveries were in the range 74.5-102.5% and relative standard deviations were <5.4%. The method is simple, green and practical, and could be applied to the extraction and determination of synthetic pigments in beverages. Copyright © 2017 Elsevier Ltd. All rights reserved.

The ROSCOE Manual. Volume 2-1. Sample Case.

DTIC Science & Technology

1980-03-01

X X — !*• » X X r*- ro H •1 ^ X IN UJ ** "O r Jul%9 c a 2 O J M X UJ .. 3 U — CO PH 4 X 3C t- L3 u • • 1C U. U3 H tD UJ UJ a...3 •-ooaooao-n »-030300030331 »-oooooooooox» »-00 3303000am i-a a 3 x •- ua 1-0 tO •- L3 2 •-• -3 ^ IU Q JaJ J...O C3 nuuv) tD CO CD 2 IftJ UJ •- I J J J M Iß Ifl li. WCJUCO o o (BfDIDZiiituHlO • • Z CO x 3 OCM

Production of pullulan by a thermotolerant aureobasidium pullulans strain in non-stirred fed batch fermentation process.

PubMed

Singh, Ranjan; Gaur, Rajeeva; Tiwari, Soni; Gaur, Manogya Kumar

2012-07-01

Total 95 isolates of Aureobasidium pullulans were isolated from different flowers and leaves samples, out of which 11 thermotolerant strains produced pullulan. One thermotolerant non-melanin pullulan producing strain, designated as RG-5, produced highest pullulan (37.1±1.0 g/l) at 42(o)C, pH 5.5 in 48h of incubation with 3% sucrose and 0.5% ammonium sulphate in a non-stirred fed batch fermentor of 6 liters capacity. The two liters of initial volume of fermentation medium was further fed with the 2 liters in two successive batches at 5 h interval into the fermentor. The sterile air was supplied only for 10h at the rate of 0.5 vvm.

Using membrane composition to fine-tune the pKa of an optical liposome pH sensor.

PubMed

Clear, Kasey J; Virga, Katelyn; Gray, Lawrence; Smith, Bradley D

2016-04-14

Liposomes containing membrane-anchored pH-sensitive optical probes are valuable sensors for monitoring pH in various biomedical samples. The dynamic range of the sensor is maximized when the probe p K a is close to the expected sample pH. While some biomedical samples are close to neutral pH there are several circumstances where the pH is 1 or 2 units lower. Thus, there is a need to fine-tune the probe p K a in a predictable way. This investigation examined two lipid-conjugated optical probes, each with appended deep-red cyanine dyes containing indoline nitrogen atoms that are protonated in acid. The presence of anionic phospholipids in the liposomes stabilized the protonated probes and increased the probe p K a values by < 1 unit. The results show that rational modification of the membrane composition is a general non-covalent way to fine-tune the p K a of an optical liposome sensor for optimal pH sensing performance.

Long period grating-based fiber-optic PH sensor for ocean monitoring

NASA Astrophysics Data System (ADS)

Wang, Ke; Klimov, Denis; Kolber, Zbigniew

2007-09-01

A fiber-optic PH sensor is developed based-on the long period grating (LPG). The LPG is fabricated by using CO II laser with a point-by-point technique. Then the grating portion is coated with PH sensitive hydrogel. The hydrogel, made of PVA/PAA, swells its volume in response to the PH change in the surrounding environment and results in a change in the refractive index. As a result, the LPG can response to the refractive index change in the coating by shifting its wavelength. Therefore, change in refractive index can be measured by tracking the wavelength shift using an optical spectrum analyzer (OSA). In this research, the LPG is dip-coated by the hydrogel. A chemostat is designed to simulate the marine environment. The PH in the chemostat is varied by controlling the CO II concentration in the sea water. A PH resolution 0.046/nm using the OSA has been obtained. This sensor is designed to monitor the sea water PH change in a long term basis.

Considerations on prevention of phlebitis and venous pain from intravenous prostaglandin E(1) administration by adjusting solution pH: in vitro manipulations affecting pH.

PubMed

Kohno, Emiko; Nishikata, Mayumi; Okamura, Noboru; Matsuyama, Kenji

2008-01-01

Prostaglandin E(1) (PGE(1); Alprostadil Alfadex) is a potent vasodilator and inhibitor of platelet aggregation used to treat patients with peripheral vascular disease. The main adverse effects of intravenous PGE(1) administration, phlebitis and venous pain, arise from the unphysiologically low pH of infusion solutions. When PGE(1) infusion solutions with a pH value greater then 6 are used, phlebitis and venous pain are considered to be avoidable. Beginning with a PGE(1) infusion solution with pH greater than 6, we add the amount of 7% sodium bicarbonate needed to bring the solution to pH 7.4 if phlebitis or venous pain develops. In the present study we established a convenient nomogram showing the relationship between the titratable acidity of various infusion solutions and the volume of 7% sodium bicarbonate required to attain pH 7.4 for preventing the phlebitis and venous pain associated with PGE(1) infusion.

In-vitro investigations of a pH- and ionic-strength-responsive polyelectrolytic hydrogel using a piezoresistive microsensor

PubMed Central

Schulz, Volker; Guenther, Margarita; Gerlach, Gerald; Magda, Jules J.; Tathireddy, Prashant; Rieth, Loren; Solzbacher, Florian

2010-01-01

Environmental responsive or smart hydrogels show a volume phase transition due to changes of external stimuli such as pH or ionic strength of an ambient solution. Thus, they are able to convert reversibly chemical energy into mechanical energy and therefore they are suitable as sensitive material for integration in biochemical microsensors and MEMS devices. In this work, micro-fabricated silicon pressure sensor chips with integrated piezoresistors were used as transducers for the conversion of mechanical work into an appropriate electrical output signal due to the deflection of a thin silicon bending plate. Within this work two different sensor designs have been studied. The biocompatible poly(hydroxypropyl methacrylate-N,N-dimethylaminoethyl methacrylate-tetra-ethyleneglycol dimethacrylate) (HPMA-DMA-TEGDMA) was used as an environmental sensitive element in piezoresistive biochemical sensors. This polyelectrolytic hydrogel shows a very sharp volume phase transition at pH values below about 7.4 which is in the range of the physiological pH. The sensor's characteristic response was measured in-vitro for changes in pH of PBS buffer solution at fixed ionic strength. The experimental data was applied to the Hill equation and the sensor sensitivity as a function of pH was calculated out of it. The time-dependent sensor response was measured for small changes in pH, whereas different time constants have been observed. The same sensor principal was used for sensing of ionic strength. The time-dependent electrical sensor signal of both sensors was measured for variations in ionic strength at fixed pH value using PBS buffer solution. Both sensor types showed an asymmetric swelling behavior between the swelling and the deswelling cycle as well as different time constants, which was attributed to the different nature of mechanical hydrogel-confinement inside the sensor. PMID:21152365

The acid-base impact of free water removal from, and addition to, plasma.

PubMed

Haskins, Steve C; Hopper, Kate; Rezende, Marlis L

2006-03-01

Water, compared with plasma at a pH of 7.4, is a weak acid. The addition of free water to a patient should have an acidifying effect (dilutional acidosis) and the removal of it, an alkalinizing effect (concentrational alkalosis). The specific effects of free water loss or gain in a relatively complex fluid such as plasma has, to the authors' knowledge, not been reported. This information would be useful in the interpretation of the effect of changes in free water in patients. Plasma samples from goats were either evaporated in a tonometer to 80% of baseline volume or hydrated by the addition of distilled water to 120% of baseline volume. The pH and partial pressure of carbon dioxide, sodium, potassium, ionized calcium, chloride, lactate, phosphorous, albumin, and total protein concentrations were measured. Actual base excess (ABE), standard bicarbonate, anion gap, strong ion difference, strong ion gap, unmeasured anions, and the effects of sodium, chloride, phosphate, and albumin changes on ABE were calculated. Most parameters changed 20% in proportion to the magnitude of dehydration or hydration. Bicarbonate concentration, however, increased only 11% in the evaporation trial and decreased only -2% in the dehydration trial. The evaporation trial was associated with a mild, but significant, metabolic alkalotic effect (ABE increased 3.2 mM/L), whereas the hydration trial was associated with a slight, insignificant metabolic acidotic effect (ABE decreased only 0.6 mM/L). The calculated free water ABE effect (change in sodium concentration) was offset by opposite changes in calculated chloride, lactate, phosphate, and albumin ABE effects.

Sampling depth confounds soil acidification outcomes

USDA-ARS?s Scientific Manuscript database

In the northern Great Plains (NGP) of North America, surface sampling depths of 0-15 or 0-20 cm are suggested for testing soil characteristics such as pH. However, acidification is often most pronounced near the soil surface. Thus, sampling deeper can potentially dilute (increase) pH measurements an...

Optical properties of fly ash. Volume 2, Final report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Self, S.A.

1994-12-01

Research performed under this contract was divided into four tasks under the following headings: Task 1, Characterization of fly ash; Task 2, Measurements of the optical constants of slags; Task 3, Calculations of the radiant properties of fly ash dispersions; and Task 4, Measurements of the radiant properties of fly ash dispersions. Tasks 1 and 4 constituted the Ph.D. research topic of Sarbajit Ghosal, while Tasks 2 and 3 constituted the Ph.D. research topic of Jon Ebert. Together their doctoral dissertations give a complete account of the work performed. This final report, issued in two volumes consists of an executivemore » summary of the whole program followed by the dissertation of Ghosal and Ebert. Volume 2 contains the dissertation of Ebert which covers the measurements of the optical constants of slags, and calculations of the radiant properties of fly ash dispersions. A list of publications and conference presentations resulting from the work is also included.« less

The Effects of Flocculation on the Propagation of Ultrasound in Dilute Kaolin Slurries.

PubMed

Austin; Challis

1998-10-01

A broadband ultrasonic spectrometer has been used to measure ultrasonic attenuation and phase velocity dispersion as functions of frequency in kaolin suspensions over a range of solid volume fractions from phi = 0.01 to phi = 0.08 and over a pH range from 3 to 9. The Harker and Temple theory was used to simulate ultrasound propagation in the suspension, using measured slope viscosity, particle size, and size distribution. Simulated results for ultrasonic attenuation and phase velocity agree well with measured values. Both sets of results agree well and show that for volume fractions above phi approximately 0.05 attenuation and velocity dispersion increase for increasing floc size, whereas for volume fractions below phi approximately 0.05 attenuation and velocity dispersion both decrease. It is proposed that the mechanism for this change in behavior around phi approximately 0.05 involves changes in floc density and floc size distribution with phi and pH. Copyright 1998 Academic Press.

Effect of pH on Cleavage of Glycogen by Vaginal Enzymes

PubMed Central

Spear, Greg T.; McKenna, Mary; Landay, Alan L.; Makinde, Hadijat; Hamaker, Bruce; French, Audrey L.; Lee, Byung-Hoo

2015-01-01

Glycogen expressed by the lower genital tract epithelium is believed to support Lactobacillus growth in vivo, although most genital isolates of Lactobacillus are not able to use glycogen as an energy source in vitro. We recently reported that α-amylase is present in the genital fluid of women and that it breaks down glycogen into small carbohydrates that support growth of lactobacilli. Since the pH of the lower genital tract can be very low, we determined how low pH affects glycogen processing by α-amylase. α-amylase in saliva degraded glycogen similarly at pH 6 and 7, but activity was reduced by 52% at pH 4. The glycogen degrading activity in nine genital samples from seven women showed a similar profile with an average reduction of more than 50% at pH 4. However, two samples collected from one woman at different times had a strikingly different pH profile with increased glycogen degradation at pH 4, 5 and 6 compared to pH 7. This second pH profile did not correlate with levels of human α-acid glucosidase or human intestinal maltase glucoamylase. High-performance anion-exchange chromatography showed that mostly maltose was produced from glycogen by samples with the second pH profile in contrast to genital α-amylase that yielded maltose, maltotriose and maltotetraose. These studies show that at low pH, α-amylase activity is reduced to low but detectable levels, which we speculate helps maintain Lactobacillus growth at a limited but sustained rate. Additionally, some women have a genital enzyme distinct from α-amylase with higher activity at low pH. Further studies are needed to determine the identity and distribution of this second enzyme, and whether its presence influences the makeup of genital microbiota. PMID:26171967

Ionic liquid-anionic surfactant based aqueous two-phase extraction for determination of antibiotics in honey by high-performance liquid chromatography.

PubMed

Yang, Xiao; Zhang, Shaohua; Yu, Wei; Liu, Zhongling; Lei, Lei; Li, Na; Zhang, Hanqi; Yu, Yong

2014-06-01

An ionic liquid-anionic surfactant based aqueous two-phase extraction was developed and applied for the extraction of tetracycline, oxytetracycline and chloramphenicol in honey. The honey sample was mixed with Na2EDTA aqueous solution. The sodium dodecyl sulfate, ionic liquid 1-octyl-3-methylimidazolium bromide and sodium chloride were added in the mixture. After the resulting mixture was ultrasonically shaken and centrifuged, the aqueous two phase system was formed and analytes were extracted into the upper phase. The parameters affecting the extraction efficiency, such as the volume of ionic liquid, the category and amount of salts, sample pH value, extraction time and temperature were investigated. The limits of detection of tetracycline, oxytetracycline and chloramphenicol were 5.8, 8.2 and 4.2 μg kg(-1), respectively. When the present method was applied to the analysis of real honey samples, the recoveries of analytes ranged from 85.5 to 110.9% and relative standard deviations were lower than 6.9%. Copyright © 2014 Elsevier B.V. All rights reserved.

Speciation of Mn(II), Mn(VII) and total manganese in water and food samples by coprecipitation-atomic absorption spectrometry combination.

PubMed

Citak, Demirhan; Tuzen, Mustafa; Soylak, Mustafa

2010-01-15

A speciation procedure based on the coprecipitation of manganese(II) with zirconium(IV) hydroxide has been developed for the investigation of levels of manganese species. The determination of manganese levels was performed by flame atomic absorption spectrometry (FAAS). Total manganese was determined after the reduction of Mn(VII) to Mn(II) by ascorbic acid. The analytical parameters including pH, amount of zirconium(IV), sample volume, etc., were investigated for the quantitative recoveries of manganese(II). The effects of matrix ions were also examined. The recoveries for manganese(II) were in the range of 95-98%. Preconcentration factor was calculated as 50. The detection limit for the analyte ions based on 3 sigma (n=21) was 0.75 microg L(-1) for Mn(II). The relative standard deviation was found to be lower than 7%. The validation of the presented procedure was performed by analysis of certified reference material having different matrices, NIST SRM 1515 (Apple Leaves) and NIST SRM 1568a (Rice Flour). The procedure was successfully applied to natural waters and food samples.