[Determination of Fe, Ti and V in vanadium and titanium magnetite by ICP-OES and microwave-assisted digestion].

PubMed

Zhu, Xia-ping; Yin, Ji-xian; Chen, Wei-dong; Hu, Zi-Wen; Liang, Qing-xun; Chen, Tie-yao

2010-08-01

The method of determination of iron, titanium and vanadium in indissolvable vanadium and titanium magnetite has been established by inductively coupled plasma atomic emission spectroscopy through adding the complexant A and using microwave-assisted digestion. The optimal conditions are confirmed by orthogonal experiment: 0.1 g vanadium and titanium magnetite, 0.04 g complexant A, 12 mL concentrated HC1, 10 min digestion time, and 385 W microwave power. The newly-established method has been applied to digest vanadium and titanium magnetite of Panzhihua Iron and Steel Institute (GBW07226). The iron, titanium and vanadium were detected by ICP-OES, and both comparative error (Er%) and comparative standard deviation (RSD%) met the demand of analytical chemistry, and the complexant A can significantly accelerate the dissolution of vanadium and titanium magnetite through the complexation with the dissolved metal ions, and making the surface of sample and hydrochloric acid medium to update constantly. The determination of the main and trace elements of digestion solution at the same time was achieved by ICP-OES. The method has the advantages of less use of reagents, economy, rapidness, and being friendly to environment, and it meets the requirement for rapid and volume determination. So the method has the value of practical application for the entry-exit inspection and quarantine department of the state and other relevant inspection units.

Studying the effect of microwave heating on the digestion process and identification of proteins.

PubMed

Devi, Shobha; Wu, Bo-Hung; Chu, Pei-Yu; Liu, Yue-Pei; Wu, Hsin-Lin; Ho, Yen-Peng

2017-02-01

The impact of microwave irradiation on the in-solution digestion processes and the detection limit of proteins are systematically studied. Kinetic processes of many peptides produced through the trypsin digestion of various proteins under microwave heating at 50°C were investigated with MALDI-MS. This study also examines the detection limits and digestion completeness of individual proteins under microwave heating at 50°C and at different time intervals (1, 5 and 30 min) using LC-MS. We conclude that if the peptides without missed cleavage dictate the detection limit, conventional digestion will lead to a better detection limit. The detection limit may not differ between the microwave and conventional heating if the peptides with missed cleavage sites and strong intensity are formed at the very early stage (i.e., less than 1 min) and are not further digested throughout the entire digestion process. The digestion of Escherichia coli lysate was compared under conventional and short time (microwave) conditions. The number of proteins identified under conventional heating exceeded that obtained from microwave heating over heating periods less than 5 min. The overall results show that the microwave-assisted digestion is not complete. Although the sequence coverage might be better, the detection limit might be worse than that under conventional heating. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparison of Dilution, Filtration, and Microwave Digestion Sample Pretreatments in Elemental Profiling of Wine by ICP-MS.

PubMed

Godshaw, Joshua; Hopfer, Helene; Nelson, Jenny; Ebeler, Susan E

2017-09-25

Wine elemental composition varies by cultivar, geographic origin, viticultural and enological practices, and is often used for authenticity validation. Elemental analysis of wine by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is challenging due to the potential for non-spectral interferences and plasma instability arising from organic matrix components. Sample preparation mitigates these interferences, however, conflicting recommendations of best practices in ICP-MS analysis of wine have been reported. This study compared direct dilution, microwave-assisted acid digestion, and two filtration sample pretreatments, acidification prior to filtration and filtration followed by acidification, in elemental profiling of one white and three red table wines by ICP-MS. Of 43 monitored isotopes, 37 varied by sample preparation method, with significantly higher results of 17 isotopes in the microwave-digested samples. Both filtration treatments resulted in lower results for 11 isotopes compared to the other methods. Finally, isotope dilution determination of copper based on natural abundances and the 63 Cu: 65 Cu instrument response ratio agreed with external calibration and confirmed a significant sample preparation effect. Overall, microwave digestion did not compare favorably, and direct dilution was found to provide the best compromise between ease of use and result accuracy and precision, although all preparation strategies were able to differentiate the wines.

Comparative study on conventional, ultrasonication and microwave assisted extraction of γ-oryzanol from rice bran.

PubMed

Kumar, Pramod; Yadav, Devbrat; Kumar, Pradyuman; Panesar, Paramjeet Singh; Bunkar, Durga Shankar; Mishra, Diwaker; Chopra, H K

2016-04-01

In present study, conventional, ultrasonic and microwave assisted extraction methods were compared with the aim of optimizing best fitting solvent and method, solvent concentration and digestion time for high yield of γ-oryzanol from rice bran. Petroleum ether, hexane and methanol were used to prepare extracts. Extraction yield were evaluated for giving high crude oil yield, total phenolic content (TPC) and γ-oryzanol content. Gas chromatography-mass spectrophotometry was used for the determination of γ-oryzanol concentration. The highest concentration of γ-oryzanol was detected in methanolic extracts of microwave treatment (85.0 ppm) followed by ultrasonication (82.0 ppm) and conventional extraction method (73.5 ppm). Concentration of γ-oryzanol present in the extracts was found to be directly proportional to the total phenolic content. A combination of 80 % methanolic concentration and 55 minutes digestion time of microwave treatment yielded the best extraction method for TPC and thus γ-oryzanol (105 ppm).

Micro-quantity tissue digestion for metal measurements by use of a microwave acid-digestion bomb.

PubMed

Nicholson, J R; Savory, M G; Savory, J; Wills, M R

1989-03-01

We describe a simple and convenient method for processing small amounts of tissue samples for trace-metal measurements by atomic absorption spectrometry, by use of a modified Parr microwave digestion bomb. Digestion proceeds rapidly (less than or equal to 90 s) in a sealed Teflon-lined vessel that eliminates contamination or loss from volatilization. Small quantities of tissue (5-100 mg dry weight) are digested in high-purity nitric acid, yielding concentrations of analyte that can be measured directly without further sample manipulation. We analyzed National Institute of Standards and Technology bovine liver Standard Reference Material to verify the accuracy of the technique. We assessed the applicability of the technique to analysis for aluminum in bone by comparison with a dry ashing procedure.

Comparison of dry, wet and microwave digestion methods for the multi element determination in some dried fruit samples by ICP-OES.

PubMed

Altundag, Huseyin; Tuzen, Mustafa

2011-11-01

The aim of this study was used to investigate the level of trace metals (Ba, Pb, Cd, Mn, Cr, Co, Ni, Cu, Mn, Zn, Sr and Fe) in some dried fruits (Prunus domestica L., Ficus carica L., Morus alba L., Vitis vinifera L., Prunus armeniaca L., and Malus domestica) samples from Turkey. Trace elements were determined by ICP-OES after dry, wet and microwave digestion methods in dried fruit samples. Validation of the proposed method was carried out by using a NIST-SRM 1515-Apple Leaves certified reference material. Element concentrations in dried fruit samples were 0.33-1.77 (Ba), 0.12-0.54 (Cd), 0.25-1.03 (Co), 0.45-2.30 (Cr), 0.43-2.74 (Cu), 0.56-4.87 (Mn), 0.61-2.54 (Ni), 0.40-2.14 (Pb), 2.16-6.54 (Zn), 0.83-12.02 (Al), 11.82-40.80 (Fe) and 0.16-6.34 (Sr) μg/g. The analytical parameters show that the microwave oven digestion procedure provided best results as compared to the wet and dry digestion procedures. The results were compared with the literature values. Copyright © 2011 Elsevier Ltd. All rights reserved.

Single-step microwave-assisted hot water extraction of hemicelluloses from selected lignocellulosic materials - A biorefinery approach.

PubMed

Mihiretu, Gezahegn T; Brodin, Malin; Chimphango, Annie F; Øyaas, Karin; Hoff, Bård H; Görgens, Johann F

2017-10-01

The viability of single-step microwave-induced pressurized hot water conditions for co-production of xylan-based biopolymers and bioethanol from aspenwood sawdust and sugarcane trash was investigated. Extraction of hemicelluloses was conducted using microwave-assisted pressurized hot water system. The effects of temperature and time on extraction yield and enzymatic digestibility of resulting solids were determined. Temperatures between 170-200°C for aspenwood and 165-195°C for sugarcane trash; retention times between 8-22min for both feedstocks, were selected for optimization purpose. Maximum xylan extraction yields of 66 and 50%, and highest cellulose digestibilities of 78 and 74%, were attained for aspenwood and sugarcane trash respectively. Monomeric xylose yields for both feedstocks were below 7%, showing that the xylan extracts were predominantly in non-monomeric form. Thus, single-step microwave-assisted hot water method is viable biorefinery approach to extract xylan from lignocelluloses while rendering the solid residues sufficiently digestible for ethanol production. Copyright © 2017 Elsevier Ltd. All rights reserved.

[Simultaneous Determination of Sn and S in Methyltin Mercaptide by Microwave-Assisted Acid Digestion and ICP-OES].

PubMed

Chen, Qian; Wu, Xi; Hou, Xian-deng; Xu, Kai-lai

2015-09-01

Methyltin mercaptide is widely used as one of the best heat stabilizer in the polyvinylchloride (PVC) thermal processing due to its excellent stability, good transparency, high compatibility and weather resistance. The content of sulfur and tin significantly affects its quality and performance, so it is of great significance to develop an analytical method for the simultaneous determination of sulfur and tin. Inductively coupled plasma atomic emission spectrometry (ICP-OES) has been a powerful analytical tool for a myriad of complex samples owing to its advantages of the low detection limits, rapid and precise determinations over wide dynamic ranges, freedom from chemical inter-element interferences, the high sample throughput and above all, simultaneous multi-elements analysis. Microwave technique as a well-developed method for sample preparation can dramatically reduce the digestion time and the loss of volatile elements compared with the traditional open digestion. Hereby, a microwave-assisted acid digestion (MW-AAD) procedure followed by inductively coupled plasma optical emission spectroscopy (ICP-OES) analysis was developed for the simultaneous determination of Sn and S in methyltin mercaptide. This method has the advantages of simplicity, rapidness, good accuracy, green and less use of samples. Parameters affecting the MW-AAD such as the digestion solution and digestion time were optimized by using a chemical analyzed reference sample (DX-181) to attain tin and sulfur quantitative recoveries. HNO3-HCl-HClO4 (v/v/v=9:3:1) and 10 min were the optimum digestion solution and digestion time, respectively. Under optimum conditions, the standard addition method and the standard calibration curve method were both been used to detect Sn and S in DX-181. There was no significant difference between two methods and the relative deviations to the chemical analysis values were both less than 2%. Additionally, the accuracy of the MW-AAD method was examined by analyzing three methyltin mercaptide samples (DX-181, DX-990, DX-960). The results were satisfactory with the relative deviations (<3%) and the recoveries of standard addition (99%~102%).

Improvement of AOAC Official Method 984.27 for the determination of nine nutritional elements in food products by Inductively coupled plasma-atomic emission spectroscopy after microwave digestion: single-laboratory validation and ring trial.

PubMed

Poitevin, Eric; Nicolas, Marine; Graveleau, Laetitia; Richoz, Janique; Andrey, Daniel; Monard, Florence

2009-01-01

A single-laboratory validation (SLV) and a ring trial (RT) were undertaken to determine nine nutritional elements in food products by inductively coupled plasma-atomic emission spectroscopy in order to improve and update AOAC Official Method 984.27. The improvements involved optimized microwave digestion, selected analytical lines, internal standardization, and ion buffering. Simultaneous determination of nine elements (calcium, copper, iron, potassium, magnesium, manganese, sodium, phosphorus, and zinc) was made in food products. Sample digestion was performed through wet digestion of food samples by microwave technology with either closed or open vessel systems. Validation was performed to characterize the method for selectivity, sensitivity, linearity, accuracy, precision, recovery, ruggedness, and uncertainty. The robustness and efficiency of this method was proved through a successful internal RT using experienced food industry laboratories. Performance characteristics are reported for 13 certified and in-house reference materials, populating the AOAC triangle food sectors, which fulfilled AOAC criteria and recommendations for accuracy (trueness, recovery, and z-scores) and precision (repeatability and reproducibility RSD and HorRat values) regarding SLV and RT. This multielemental method is cost-efficient, time-saving, accurate, and fit-for-purpose according to ISO 17025 Norm and AOAC acceptability criteria, and is proposed as an improved version of AOAC Official Method 984.27 for fortified food products, including infant formula.

[Determination of metals in waste bag filter of steel works by microwave digestion-flame atomic absorption spectrometry].

PubMed

Ning, Xun-An; Zhou, Yun; Liu, Jing-Yong; Wang, Jiang-Hui; Li, Lei; Ma, Xiao-Guo

2011-09-01

A method of microwave digestion technique-flame atomic absorption spectrometry was proposed to determine the total contents of Cu, Zn, Pb, Cd, Cr and Ni in five different kinds of waste bag filters from a steel plant. The digestion effects of the six acid systems on the heavy metals digestion were studied for the first time. The relative standard deviation (RSD) of the method was between 1.02% and 9.35%, and the recovery rates obtained by standard addition method ranged from 87.7% to 105.6%. The results indicated that the proposed method exhibited the advantages of simplicity, speediness, accuracy and repeatability, and it was suitable for determining the metal elements of the waste bag filter. The results also showed that different digestion systems should be used according to different waste bag filters. The waste bag filter samples from different production processes had different metal elements content. The Pb and Zn were the highest in the waste bag filters, while the Cu, Ni, Cd and Cr were relatively lower. These determination results provided the scientific data for further treatment and disposal of the waste bag filter.

Enhancement in mesophilic aerobic digestion of waste activated sludge by chemically assisted thermal pretreatment method.

PubMed

Tyagi, Vinay Kumar; Lo, Shang-Lien

2012-09-01

The effects of hybrid microwave (MW)-alkali pretreatment methods on the efficiency of mesophilic aerobic digestion were studied. The MW-alkali pretreatment (95°C-pH 12) was observed to enhance the sludge solubilization synergistically from 0.5% (raw) to 52.5% (MW-NaOH) and 48.7% (MW-KOH), which are 20% greater than the additive value of MW only and alkali only (16%(MW)+28.4%(NaOH)=44.4% and 16%(MW)+25.5(KOH)=41.5). The higher VSS solubilization was observed for hybrid MW-NaOH (53.9%) and MW-KOH (47.4%) methods. The batch mesophilic (35°C) aerobic digestion system led to 81.1% TCOD degradation and 72.4% VSS degradation at 20 days of retention time, with 35% higher TCOD and VSS reduction in comparison with the control system. The filterability of microwave-alkali pretreated sludge was improved remarkably after aerobic digestion. Moreover, the proposed method is capable of effectively sanitize the sewage sludge and produce Class A biosolids. Copyright © 2012 Elsevier Ltd. All rights reserved.

Determination of calcium, copper, iron, magnesium, manganese, potassium, phosphorus, sodium, and zinc in fortified food products by microwave digestion and inductively coupled plasma-optical emission spectrometry: single-laboratory validation and ring trial.

PubMed

Poitevin, Eric

2012-01-01

A single-laboratory validation (SLV) and a ring trial (RT) were undertaken to determine nine nutritional elements in food products by inductively coupled plasma-optical emission spectrometry in order to modernize AOAC Official Method 984.27. The improvements involved extension of the scope to all food matrixes (including infant formula), optimized microwave digestion, selected analytical lines, internal standardization, and ion buffering. Simultaneous determination of nine elements (calcium, copper, iron, potassium, magnesium, manganese, sodium, phosphorus, and zinc) was made in food products. Sample digestion was performed through wet digestion of food samples by microwave technology with either closed- or open-vessel systems. Validation was performed to characterize the method for selectivity, sensitivity, linearity, accuracy, precision, recovery, ruggedness, and uncertainty. The robustness and efficiency of this method was proven through a successful RT using experienced independent food industry laboratories. Performance characteristics are reported for 13 certified and in-house reference materials, populating the AOAC triangle food sectors, which fulfilled AOAC criteria and recommendations for accuracy (trueness, recovery, and z-scores) and precision (repeatability and reproducibility RSD, and HorRat values) regarding SLVs and RTs. This multielemental method is cost-efficient, time-saving, accurate, and fit-for-purpose according to ISO 17025 Norm and AOAC acceptability criteria, and is proposed as an extended updated version of AOAC Official Method 984.27 for fortified food products, including infant formula.

[Determination of 27 elements in Maca nationality's medicine by microwave digestion ICP-MS].

PubMed

Yu, Gui-fang; Zhong, Hai-jie; Hu, Jun-hua; Wang, Jing; Huang, Wen-zhe; Wang, Zhen-zhong; Xiao, Wei

2015-12-01

An analysis method has been established to test 27 elements (Li, Be, B, Mg, Al, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Sr, Mo, Cd, Sn, Sb, Ba, La, Hg, Pb, Bi) in Maca nationality's medicine with microwave digestion-ICP-MS. Sample solutions were analyzed by ICP-MS after microwave digestion, and the contents of elements were calculated according to their calibration curves, and internal standard method was adopted to reduce matrix effect and other interference effects. The experimental results showed that the linear relations of all the elements were very good; the correlation coefficient (r) was 0.9994-1.0000 (Hg was 0.9982) ; the limits of detection were 0.003-2.662 microg x L(-1); the relative standard deviations for all elements of reproducibility were lower than 5% (except the individual elements); the recovery rate were 78.5%-123.7% with RSD lower than 5% ( except the individual elements). The analytical results of standard material showed acceptable agreement with the certified values. This method was applicable to determinate the contents of multi-elements in Maca which had a high sensitivity, good specificity and good repeatability, and provide basis for the quality control of Maca.

Antioxidant activity measurement and potential antioxidant peptides exploration from hydrolysates of novel continuous microwave-assisted enzymolysis of the Scomberomorus niphonius protein.

PubMed

Huang, Yipeng; Ruan, Guihua; Qin, Zhijun; Li, Haiyun; Zheng, Yanjie

2017-05-15

A novel continuous microwave-assisted enzymatic digestion (cMAED) method is proposed for the digestion of protein from Scomberomorus niphonius to obtain potential antioxidant peptides. In this study, bromelain was found to have a high capacity for the digestion of the Scomberomorus niphonius protein. The following cMAED conditions were investigated: protease species, microwave power, temperature, bromelain content, acidity of the substrate solution, and incubation time. At 400W, 40°C, 1500U·g -1 bromelain, 20% substrate concentration, pH 6.0 and 5min incubation, the degree of hydrolysis and total antioxidant activity of the hydrolysates were 15.86% and 131.49μg·mL -1 , respectively. The peptide analyses showed that eight of the potential antioxidant peptide sequences, which ranged from 502.32 to 1080.55Da with 4-10 amino acid residues, had features typical of well-known antioxidant proteins. Thus, the new cMAED method can be useful to obtain potential antioxidant peptides from protein sources, such as Scomberomorus niphonius. Copyright © 2016 Elsevier Ltd. All rights reserved.

[Study on microwave digestion of gypsum for the determination of multielement by ICP-OES and ICP-MS].

PubMed

Wang, Hui; Song, Qiang; Yang, Rui-ming; Yao, Qiang; Chen, Chang-he

2010-09-01

Three acids (HNO3, HNO3/HF and HNO3 /HF+ H3BO3) were used to decompose gypsum with microwave digestion system. The contents of 10 mineral elements (Al, Ca, Mg, Fe, K, Na, S, Ti, Si and Sr) in gypsum were determined by inductively coupled plasma-optical emission spectrometry (ICP-OES) while 6 heavy metals (V, Cr, Mn, Zn, Se and Ce) were determined by inductively coupled plasma-mass spectrometry (ICP-MS). GBW03109a, GBW03110 and FGD-2 were used as gypsum standard reference materials. The results showed that two-step microwave digestion with HNO3/HF at 210 degrees C and then adding H3BO3 for the removal of HF and fluorides completely decomposed the gypsums, while this method achieved good recoveries for all elements in the three gypsum standard reference materials. The recovery was from 88% to 112% and the RSD of tests was below 3%. The method was applied to the elemental analysis for flue gas desulfurization gypsums from three coal-fired power plants.

Coupled high performance liquid chromatography-microwave digestion-hydride generation-atomic absorption spectrometry for inorganic and organic arsenic speciation in fish tissue.

PubMed

Villa-Lojo, M C; Alonso-Rodríguez, E; López-Mahía, P; Muniategui-Lorenzo, S; Prada-Rodríguez, D

2002-06-10

A high performance liquid chromatography-microwave digestion-hydride generation-atomic absorption spectrometry (HPLC-MW-HG-AAS) coupled method is described for As(III), As(V), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), arsenobetaine (AsB) and arsenocholine (AsC) determination. A Hamilton PRP-X100 anion-exchange column is used for carrying out the arsenic species separation. As mobile phase 17 mM phosphate buffer (pH 6.0) is used for As(III), As(V), MMA and DMA separation, and ultrapure water (pH 6.0) for AsB and AsC separation. Prior to injection into the HPLC system AsB and AsC are isolated from the other arsenic species using a Waters Accell Plus QMA cartridge. A microwave digestion with K(2)S(2)O(8) as oxidizing agent is used for enhancing the efficiency of conversion of AsB and AsC into arsenate. Detection limits achieved were between 0.3 and 1.1 ng for all species. The method was applied to arsenic speciation in fish samples.

Comparison of Digestion Methods for the Determination of Trace Elements and Heavy Metals in Human Hair and Nails

PubMed Central

Ishak, Ismarulyusda; Rosli, Farah Dayana; Mohamed, Jamaludin; Mohd Ismail, Muhammad Faiz

2015-01-01

Background Microwave is the most reliable sample digestion method. However, it requires expensive microwave digester automation and has relatively low productivity. In this study, three non-automated digestion methods, i.e. wet acid digestion using nitric acid (HNO3) and hydrogen peroxide (H2O2), wet acid digestion using HNO3, and dry washing, are compared in order to determine the best approach. Methods Certified reference material IAEA-086 (International Atomic Energy Agency, Austria) and hair and nail samples from 20 female students of Universiti Kebangsaan Malaysia, aged 19 to 30 years, were collected and analysed using the three digestion methods. Results For hair samples, analysis of variance of repeated measures showed significant differences in the level of all elements (P < 0.001) between the three methods. For nail samples, only the copper (Cu) level showed no significant difference (P = 0.100) between methods. Wet acid digestion using HNO3 and H2O2 showed the best within- and between-run relative standard deviation (RSD) values, with within-run RSD for all elements, except for selenium (Se), < 5%. The between-run precision ranges from 6.14% to 17.96% for hair and from 3.53% to 11.52% for nail samples. Wet acid digestion using HNO3 and H2O2 showed both good accuracy and precision for manganese (Mn) and magnesium (Mg), with percentage recoveries of 110% and 96.9%, respectively. All elements show higher method detection limit (MDL) values than the previous study: 0.05 μg/g Mg for wet acid digestion using HNO3, 0.02 μg/g Se for wet acid digestion using HNO3 and H2O2, and 0.2 μg/g Mg for dry ash method. Conclusion Wet acid digestion using HNO3 and H2O2 proved to be the best method in terms of precision, accuracy, recovery, and MDL. However, only Mn and Mg showed adequate precision, accuracy, and percentage of recovery. PMID:28223880

[Study on microwave digestion of coal for the determination of multi-element by ICP-OES and ICP-MS].

PubMed

Wang, Hui; Song, Qiang; Yao, Qiang; Chen, Chang-He; Yu, Fei-Lu

2012-06-01

Effects of temperature and four acids (HNO3, HNO3/H2O2, HNO3/HF and HNO3/HF+H3BO3) on the coal decomposition by microwave digestion and the multi-element analysis were studied. SARM20 was used as a coal standard reference material. The contents of 10 mineral elements (Al, Ca, Fe, Mg, K, Na, S, Si, Sr and Ti) in the coal SARM20 were determined by inductively coupled plasma-optical emission spectrometry (ICP-OES). And the contents of 20 heavy metals (Li, Be, Sc, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, As, Se, Zr, Sn, Cs, Ba, Ce, Eu and Pb) were determined by inductively coupled plasma-mass spectrometry (ICP-MS). The results showed that the coal was completely decomposed by microwave digestion with HNO3/HF+ H3BO3 at 210 degrees C. Good recoveries for all elements in the coal SARM20 were obtained by this two-step microwave digestion method. The recoveries of the 10 mineral elements were from 87.5% to 98.8%, and the recoveries of the 20 heavy metals were from 85% to 112.5%. All RSDs of tests were below 3%.

Comparison of four USEPA digestion methods for trace metal analysis using certified and Florida soils

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

Chen, M.; Ma, L.Q.

1998-11-01

It is critical to compare existing sample digestion methods for evaluating soil contamination and remediation. USEPA Methods 3050, 3051, 3051a, and 3052 were used to digest standard reference materials and representative Florida surface soils. Fifteen trace metals (Ag, As, Ba, Be, Cd, Cr, Cu, Hg, Mn, Mo, Ni, Pb, Sb, Se, and Za), and six macro elements (Al, Ca, Fe, K, Mg, and P) were analyzed. Precise analysis was achieved for all elements except for Cd, Mo, Se, and Sb in NIST SRMs 2704 and 2709 by USEPA Methods 3050 and 3051, and for all elements except for As, Mo,more » Sb, and Se in NIST SRM 2711 by USEPA Method 3052. No significant differences were observed for the three NIST SRMs between the microwave-assisted USEPA Methods 3051 and 3051A and the conventional USEPA Method 3050 Methods 3051 and 3051a and the conventional USEPA Method 3050 except for Hg, Sb, and Se. USEPA Method 3051a provided comparable values for NIST SRMs certified using USEPA Method 3050. However, for method correlation coefficients and elemental recoveries in 40 Florida surface soils, USEPA Method 3051a was an overall better alternative for Method 3050 than was Method 3051. Among the four digestion methods, the microwave-assisted USEPA Method 3052 achieved satisfactory recoveries for all elements except As and Mg using NIST SRM 2711. This total-total digestion method provided greater recoveries for 12 elements Ag, Be, Cr, Fe, K, Mn, Mo, Ni, Pb, Sb, Se, and Zn, but lower recoveries for Mg in Florida soils than did the total-recoverable digestion methods.« less

Effects of dehulling, steam-cooking and microwave-irradiation on digestive value of white lupin (Lupinus albus) seed meal for rainbow trout (Oncorhynchus mykiss) and Atlantic salmon (Salmo salar).

PubMed

Saez, Patricio; Borquez, Aliro; Dantagnan, Patricio; Hernández, Adrián

2015-01-01

A digestibility trial was conducted to assess the effect of dehulling, steam-cooking and microwave-irradiation on the apparent digestibility of nutrients in white lupin (Lupinus albus) seed meal when fed to rainbow trout (Oncorhynchus mykiss) and Atlantic salmon (Salmo salar). Six ingredients, whole lupin seed meal (LSM), dehulled LSM, dehulled LSM steam-cooked for 15 or 45 min (SC15 and SC45, respectively) and LSM microwave-irradiated at 375 or 750 W (MW375 and MW750, respectively), were evaluated for digestibility of dry matter, crude protein (CP), lipids, nitrogen-free extractives (NFE) and gross energy (GE). The diet-substitution approach was used (70% reference diet + 30% test ingredient). Faeces from each tank were collected using a settlement column. Dehulled LSM showed higher levels of proximate components (except for NFE and crude fibre), GE and phosphorus in comparison to whole LSM. Furthermore, SC15, SC45, MW375 and MW750 showed slight variations of chemical composition in comparison to dehulled LSM. Results from the digestibility trial indicated that dehulled LSM, SC15, SC45 and MW375 are suitable processing methods for the improvement of nutrients' apparent digestibility coefficient (ADC) in whole LSM. MW750 showed a lower ADC of nutrients (except for CP and lipids for rainbow trout) in comparison with MW350 for rainbow trout and Atlantic salmon, suggesting a heat damage of the ingredient when microwave-irradiation exceeded 350 W.

Enhancement of anaerobic digestion efficiency of wastewater sludge and olive waste: Synergistic effect of co-digestion and ultrasonic/microwave sludge pre-treatment.

PubMed

Alagöz, B Aylin; Yenigün, Orhan; Erdinçler, Ayşen

2015-12-01

This study investigates the effect of ultrasonic and microwave pre-treatment on biogas production from the anaerobic co-digestion of olive pomace and wastewater sludges. It was found that co-digestion of wastewater sludge with olive pomace yielded around 0.21 L CH4/g VS added, whereas the maximum methane yields from the mono-digestion of olive pomace and un-pretreated wastewater sludges were 0.18 and 0.16L CH4/g VS added. In the same way, compared to mono-digestion of these substrates, co-digestion increased methane production by 17-31%. The microwave and ultrasonic pre-treatments applied to sludge samples prior to co-digestion process led to further increase in the methane production by 52% and 24%, respectively, compared to co-digestion with un-pretreated wastewater sludge. The highest biogas and methane yields were obtained from the co-digestion of 30 min microwave pre-treated wastewater sludges and olive pomace to be 0.46 L/g VS added and 0.32 L CH4/g VS added, respectively. Copyright © 2015 Elsevier Ltd. All rights reserved.

Mechanised flow system for on-line microwave digestion of food samples with off-line catalytic spectrophotometric determination of cobalt at ng l-1 levels.

PubMed

Pereira-Filho, E R; Arruda, M A

1999-12-01

A mechanised system for on-line slurry food sample digestion was developed and an off-line cobalt determination was performed. The stabilised slurry sample was introduced into an air carrier stream until reaching the digestion coils located inside a household microwave oven. Software written in Visual Basic 3.0 was developed to permit the transport of the slurry samples and the programming of the microwave oven and also the control of the mineralization valve. The proposed system was optimized for determination of cobalt in certified samples such as mussels, bovine liver and fish and also uncertified fish samples. The digestion parameters were established as 3 mol l-1 HNO3 for mussels, 3 mol l-1 HNO3 plus 0.16% v/v H2O2 for bovine liver and 12 mol l-1 HNO3 for fish employing maximum power for 5 min of microwave actuation. In the subsequent spectrophotometric method for the catalytic determination of cobalt, the Tiron and hydrogen peroxide concentrations were 1.8 x 10(-3) and 3.0 x 10(-4) mol l-1, respectively, and the sample residence time was 300 s as determined by an optimisation process. The proposed method features a linear range from 10 to 200 ng l-1 Co (r > 0.996) with detection and quantification limits of 1.7 and 5.5 ng l-1 Co, respectively. The precision, expressed as RSD, was 2.4% (n = 12) for repeatability and 5.2% (n = 10) for reproducibility and the accuracy of the proposed method was assessed by using certified samples and an alternative technique (ETAAS).

Enhancing anaerobic digestibility and phosphorus recovery of dairy manure through microwave-based thermochemical pretreatment.

PubMed

Jin, Ying; Hu, Zhenhu; Wen, Zhiyou

2009-08-01

Anaerobic digestion and struvite precipitation are two effective ways of treating dairy manure for recovering biogas and phosphorus. Anaerobic digestion of dairy manure is commonly limited by slow fiber degradation, while struvite precipitation is limited by the availability of orthophosphate. The aim of this work is to study the possibility of using microwave-based thermochemical pretreatment to simultaneously enhance manure anaerobic digestibility (through fiber degradation) and struvite precipitation (through phosphorus solubilization). Microwave heating combined with different chemicals (NaOH, CaO, H(2)SO(4), or HCl) enhanced solubilization of manure and degradation of glucan/xylan in dairy manure. However, sulfuric acid-based pretreatment resulted in a low anaerobic digestibility, probably due to the sulfur inhibition and Maillard side reaction. The pretreatments released 20-40% soluble phosphorus and 9-14% ammonium. However, CaO-based pretreatment resulted in lower orthophosphate releases and struvite precipitation efficiency as calcium interferes with phosphate to form calcium phosphate. Collectively, microwave heating combined with NaOH or HCl led to a high anaerobic digestibility and phosphorus recovery. Using these two chemicals, the performance of microwave- and conventional-heating in thermochemical pretreatment was further compared. The microwave heating resulted in a better performance in terms of COD solubilization, glucan/xylan reduction, phosphorus solubilization and anaerobic digestibility. Lastly, temperature and heating time used in microwave treatment were optimized. The optimal values of temperature and heating time were 147 degrees C and 25.3 min for methane production, and 135 degrees C and 26 min for orthophosphate release, respectively.

[Evaluation of three methods for forensic diatom test].

PubMed

Wang, Yuzhong; Zhao, Jian; Li, Peng; Hu, Sunlin; Wang, Huipin; Wang, Huijun; Liu, Chao

2015-03-01

To compare the efficacy of three methods for forensic diatom test, namely strong acid digestion-centrifuge enrichment-light microscopy (SD-CE-LM), microwave digestion-membrane filtration-automated scanning electron microscopy (MD-ME-SEM), and microwave digestion-membrane filtration-light microscopy (MD-MF-LM). Sixty samples were randomly divided into 3 groups for diatom test using three methods, and the sample preparation time, degree of digestion and recovery rate of diatoms were compared. The sample preparation time was the shortest with MD-MF-LM and the longest with SD-CE-LM (P<0.05). MD-ME-SEM and MD-MF-LM allowed more thorough tissue digestion than SD-CE-LM. MD-ME-SEM resulted in the highest total recovery rate of diatom, followed by MD-MF-LM and then by SD-CE-LM (P<0.05); the recover rate of different diatom species was the highest with MD-ME-SEM, followed by MD-MF-LM and SD-CE-LM (P<0.05). SD-CE-LM has a low recovery rate of diatoms especially for those with lengths shorter than 40 µm or densities less than 1/5. With a high recovery rate and accuracy in diatom test, MD-ME-SEM is suitable for diagnosis of suspected drowning cases. MD-MF-LM is highly efficient, sensitive and convenient for forensic diatom test.

Ultrasound assisted biogas production from co-digestion of wastewater sludges and agricultural wastes: Comparison with microwave pre-treatment.

PubMed

Aylin Alagöz, B; Yenigün, Orhan; Erdinçler, Ayşen

2018-01-01

This study investigates the effect of ultrasonication and microwave sludge disintegration/pre-treatment techniques on the anaerobic co-digestion efficiency of wastewater sludges with olive and grape pomaces. The effects of both co-digestion and sludge pre-treatment techniques were evaluated in terms of the organic removal efficiency and the biogas production. The "co-digestion" of wastewater sludge with both types of pomaces was revealed to be a much more efficient way for the biogas production compared to the single (mono) sludge digestion. The ultrasonication and microwave pre-treatments applied to the sludge samples caused to a further increase in biogas and methane yields. Based on applied specific energies, ultrasonication pre-treatment was found much more effective than microwave irradiation. The specific energy applied in microwave pre-treatment (87,000kj/kgTS) was almost 9 times higher than that of used in ultrasonication (10,000kj/kgTS), resulting only 10-15% increases in biogas/methane yield. Co-digestion of winery and olive industry residues with pre-treated wastewater sludges appears to be a suitable technique for waste management and energy production. Copyright © 2017 Elsevier B.V. All rights reserved.

Performance evaluation of a high-pressure microwave-assisted flow digestion system for juice and milk sample preparation.

PubMed

Marques, Thiago L; Wiltsche, Helmar; Nóbrega, Joaquim A; Winkler, Monika; Knapp, Günter

2017-07-01

Acid digestion is usually required for metal determination in food samples. However, this step is usually performed in batch mode which is time consuming, labor intensive, and may lead to sample contamination. Flow digestion can overcome these limitations. In this work, the performance of a high-pressure microwave-assisted flow digestion system with a large volume reactor was evaluated for liquid samples high in sugar and fat (fruit juice and milk). The digestions were carried out in a coiled perfluoroalkoxy (PFA) tube reactor (13.5 mL) installed inside an autoclave pressurized with 40 bar nitrogen. The system was operated at 500 W microwave power and 5.0 mL min -1 carrier flow rate. Digestion conditions were optimized with phenylalanine, as this substance is known to be difficult to digest completely. The combinations of HCl or H 2 O 2 with HNO 3 increased the digestion efficiency of phenylalanine, and the residual carbon content (RCC) was around 50% when 6.0% V/V HCl or H 2 O 2 was used in combination with 32% V/V HNO 3 . Juice samples were digested with 3.7 mol L -1 HNO 3 and 0.3 mol L -1 HCl, and the RCC was 16 and 29% for apple and mango juices, respectively. Concentrated HNO 3 (10.5 mol L -1 ) was successfully applied for digesting milk samples, and the RCCs were 23 and 25% for partially skimmed and whole milk, respectively. Accuracy and precision of the flow digestion procedure were compared with reference digestions using batch mode closed vessel microwave-assisted digestion and no statistically significant differences were encountered at the 95% confidence level. Graphical abstract Application of a high-pressure microwave-assisted flow digestion system for fruit juice and milk sample preparation.

Comparison of the DNA extraction methods for polymerase chain reaction amplification from formalin-fixed and paraffin-embedded tissues.

PubMed

Sato, Y; Sugie, R; Tsuchiya, B; Kameya, T; Natori, M; Mukai, K

2001-12-01

To obtain an adequate quality and quantity of DNA from formalin-fixed and paraffin-embedded tissue, six different DNA extraction methods were compared. Four methods used deparaffinization by xylene followed by proteinase K digestion and phenol-chloroform extraction. The temperature of the different steps was changed to obtain higher yields and improved quality of extracted DNA. The remaining two methods used microwave heating for deparaffinization. The best DNA extraction method consisted of deparaffinization by microwave irradiation, protein digestion with proteinase K at 48 degrees C overnight, and no further purification steps. By this method, the highest DNA yield was obtained and the amplification of a 989-base pair beta-globin gene fragment was achieved. Furthermore, DNA extracted by means of this procedure from five gastric carcinomas was successfully used for single strand conformation polymorphism and direct sequencing assays of the beta-catenin gene. Because the microwave-based DNA extraction method presented here is simple, has a lower contamination risk, and results in a higher yield of DNA compared with the ordinary organic chemical reagent-based extraction method, it is considered applicable to various clinical and basic fields.

Methods of ammonia removal in anaerobic digestion: a review.

PubMed

Krakat, Niclas; Demirel, Burak; Anjum, Reshma; Dietz, Donna

2017-10-01

The anaerobic digestion of substrates with high ammonia content has always been a bottleneck in the methanisation process of biomasses. Since microbial communities in anaerobic digesters are sensitive to free ammonia at certain conditions, the digestion of nitrogen-rich substrates such as livestock wastes may result in inhibition/toxicity eventually leading to process failures, unless appropriate engineering precautions are taken. There are many different options reported in literature to remove ammonia from anaerobic digesters to achieve a safe and stable process so that along with high methane yields, a good quality of effluents can also be obtained. Conventional techniques to remove ammonia include physical/chemical methods, immobilization and adaptation of microorganisms, while novel methods include ultrasonication, microwave, hollow fiber membranes and microbial fuel cell applications. This paper discusses conventional and novel methods of ammonia removal from anaerobic digesters using nitrogen-rich substrates, with particular focus on recent literature available about this topic.

[Determination of aluminium in flour foods with photometric method].

PubMed

Ma, Lan; Zhao, Xin; Zhou, Shuang; Yang, Dajin

2012-05-01

To establish a determination method for aluminium in flour foods with photometric method. After samples being treated with microwave digestion and wet digestion, aluminium in staple flour foods was determined by photometric method. There was a good linearity of the result in the range of 0.25 - 5.0 microg/ml aluminium, r = 0.9998; limit of detection (LOD) : 2.3 ng/ml; limit of quantitation (LOQ) : 7 ng/ml. This method of determining aluminium in flour foods is simple, rapid and reliable.

Method validation for simultaneous determination of chromium, molybdenum and selenium in infant formulas by ICP-OES and ICP-MS.

PubMed

Khan, Naeem; Jeong, In Seon; Hwang, In Min; Kim, Jae Sung; Choi, Sung Hwa; Nho, Eun Yeong; Choi, Ji Yeon; Kwak, Byung-Man; Ahn, Jang-Hyuk; Yoon, Taehyung; Kim, Kyong Su

2013-12-15

This study aimed to validate the analytical method for simultaneous determination of chromium (Cr), molybdenum (Mo), and selenium (Se) in infant formulas available in South Korea. Various digestion methods of dry-ashing, wet-digestion and microwave were evaluated for samples preparation and both inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) were compared for analysis. The analytical techniques were validated by detection limits, precision, accuracy and recovery experiments. Results showed that wet-digestion and microwave methods were giving satisfactory results for sample preparation, while ICP-MS was found more sensitive and effective technique than ICP-OES. The recovery (%) of Se, Mo and Cr by ICP-OES were 40.9, 109.4 and 0, compared to 99.1, 98.7 and 98.4, respectively by ICP-MS. The contents of Cr, Mo and Se in infant formulas by ICP-MS were found in good nutritional values in accordance to nutrient standards for infant formulas CODEX values. Copyright © 2013 Elsevier Ltd. All rights reserved.

Accurate determination of sulfur in gasoline and related fuel samples using isotope dilution ICP-MS with direct sample injection and microwave-assisted digestion.

PubMed

Heilmann, Jens; Boulyga, Sergei F; Heumann, Klaus G

2004-09-01

Inductively coupled plasma isotope-dilution mass spectrometry (ICP-IDMS) with direct injection of isotope-diluted samples into the plasma, using a direct injection high-efficiency nebulizer (DIHEN), was applied for accurate sulfur determinations in sulfur-free premium gasoline, gas oil, diesel fuel, and heating oil. For direct injection a micro-emulsion consisting of the corresponding organic sample and an aqueous 34S-enriched spike solution with additions of tetrahydronaphthalene and Triton X-100, was prepared. The ICP-MS parameters were optimized with respect to high sulfur ion intensities, low mass-bias values, and high precision of 32S/34S ratio measurements. For validation of the DIHEN-ICP-IDMS method two certified gas oil reference materials (BCR 107 and BCR 672) were analyzed. For comparison a wet-chemical ICP-IDMS method was applied with microwave-assisted digestion using decomposition of samples in a closed quartz vessel inserted into a normal microwave system. The results from both ICP-IDMS methods agree well with the certified values of the reference materials and also with each other for analyses of other samples. However, the standard deviation of DIHEN-ICP-IDMS was about a factor of two higher (5-6% RSD at concentration levels above 100 mircog g(-1)) compared with those of wet-chemical ICP-IDMS, mainly due to inhomogeneities of the micro-emulsion, which causes additional plasma instabilities. Detection limits of 4 and 18 microg g(-1) were obtained for ICP-IDMS in connection with microwave-assisted digestion and DIHEN-ICP-IDMS, respectively, with a sulfur background of the used Milli-Q water as the main limiting factor for both methods.

Conductive heating and microwave hydrolysis under identical heating profiles for advanced anaerobic digestion of municipal sludge.

PubMed

Mehdizadeh, Seyedeh Neda; Eskicioglu, Cigdem; Bobowski, Jake; Johnson, Thomas

2013-09-15

Microwave (2.45 GHz, 1200 W) and conventional heating (custom pressure vessel) pretreatments were applied to dewatered municipal waste sludge (18% total solids) using identical heating profiles that span a wide range of temperatures (80-160 °C). Fourteen lab-scale semi-continuous digesters were set up to optimize the energy (methane) output and sludge retention time (SRT) requirements of untreated (control) and thermally pretreated anaerobic digesters operated under mesophilic and thermophilic temperatures. Both pretreatment methods indicated that in the pretreatment range of 80-160 °C, temperature was a statistically significant factor (p-value < 0.05) for increasing solubilization of chemical oxygen demand and biopolymers (proteins, sugars, humic acids) of the waste sludge. However, the type of pretreatment method, i.e. microwave versus conventional heating, had no statistically significant effect (p-value >0.05) on sludge solubilization. With the exception of the control digesters at a 5-d SRT, all control and pretreated digesters achieved steady state at all three SRTs, corresponding to volumetric organic loading rates of 1.74-6.96 g chemical oxygen demand/L/d. At an SRT of 5 d, both mesophilic and thermophilic controls stopped producing biogas after 20 d of operation with total volatile fatty acids concentrations exceeding 1818 mg/L at pH <5.64 for mesophilic and 2853 mg/L at pH <7.02 for thermophilic controls, while the pretreated digesters continued producing biogas. Furthermore, relative (to control) organic removal efficiencies dramatically increased as SRT was shortened from 20 to 10 and then 5 d, indicating that the control digesters were challenged as the organic loading rate was increased. Energy analysis showed that, at an elevated temperature of 160 °C, the amount of methane recovered was not enough to compensate for the energy input. Among the digesters with positive net energy productions, control and pretreated digesters at 80 °C were more favorable at an SRT of 10 d. Copyright © 2013 Elsevier Ltd. All rights reserved.

In vitro starch digestibility and expected glycemic index of pound cakes baked in two-cycle microwave-toaster and conventional oven.

PubMed

García-zaragoza, Francisco J; Sánchez-Pardo, María E; Ortiz-Moreno, Alicia; Bello-Pérez, Luis A

2010-11-01

Bread baking technology has an important effect on starch digestibility measured as its predicted glycemic index tested in vitro. The aim of this work was to evaluate the changes in predicted glycemic index of pound cake baked in a two-cycle microwave toaster and a conventional oven. The glycemic index was calculated from hydrolysis index values by the Granfeldt method. Non-significant differences (P > 0.05) were found in hydrolysis index (60.67 ± 3.96 for the product baked in microwave oven and 65.94 ± 4.09 for the product baked in conventional oven) and predicted glycemic index content (60.5 for product baked in microwave oven and 65 for the product baked in conventional oven) in freshly-baked samples. Results clearly demonstrate that the baking pound cake conventional process could be replicated using a two-cycle multifunction microwave oven, reducing the traditional baking time. Further research is required in order to achieve pound cake crumb uniformity.

Microwave acid digestion and preconcentration neutron activation analysis of biological and diet samples for iodine.

PubMed

Rao, R R; Chatt, A

1991-07-01

A simple preconcentration neutron activation analysis (PNAA) method has been developed for the determination of low levels of iodine in biological and nutritional materials. The method involves dissolution of the samples by microwave digestion in the presence of acids in closed Teflon bombs and preconcentration of total iodine, after reduction to iodide with hydrazine sulfate, by coprecipitation with bismuth sulfide. The effects of different factors such as acidity, time for complete precipitation, and concentrations of bismuth, sulfide, and diverse ions on the quantitative recovery of iodide have been studied. The absolute detection limit of the PNAA method is 5 ng of iodine. Precision of measurement, expressed in terms of relative standard deviation, is about 5% at 100 ppb and 10% at 20 ppb levels of iodine. The PNAA method has been applied to several biological reference materials and total diet samples.

Three Birds with One Fe3O4 Nanoparticle: Integration of Microwave Digestion, Solid Phase Extraction, and Magnetic Separation for Sensitive Determination of Arsenic and Antimony in Fish.

PubMed

Jia, Yun; Yu, Huimin; Wu, Li; Hou, Xiandeng; Yang, Lu; Zheng, Chengbin

2015-06-16

An environmentally friendly and fast sample treatment approach that integrates accelerated microwave digestion (MWD), solid phase extraction, and magnetic separation into a single step was developed for the determination of arsenic and antimony in fish samples by using Fe3O4 magnetic nanoparticles (MNPs). Compared to conventional microwave digestion, the consumption of HNO3 was reduced significantly to 12.5%, and the digestion time and temperature were substantially decreased to 6 min and 80 °C, respectively. This is largely attributed to Fe3O4 magnetic nanoparticles being a highly effective catalyst for rapid generation of oxidative radicals from H2O2, as well as an excellent absorber of microwave irradiation. Moreover, potential interferences from sample matrices were eliminated because the As and Sb species adsorbed on the nanoparticles were efficiently separated from the digests with a hand-held magnet prior to analysis. Limits of detection for arsenic and antimony were in the range of 0.01-0.06 μg g(-1) and 0.03-0.08 μg g(-1) by using hydride generation atomic fluorescence spectrometry, respectively, and further improved to 0.002-0.005 μg g(-1) and 0.005-0.01 μg g(-1) when inductively coupled plasma mass spectrometry was used as a detector. The precision of replicate measurements (n = 9) was better than 6% by analyzing 0.1 g test sample spiked with 1 μg g(-1) arsenic and antimony. The proposed method was validated by analysis of two certified reference materials (DORM-3 and DORM-4) with good recoveries (90%-106%).

Effect of Microwave Irradiation on the Physicochemical and Digestive Properties of Lotus Seed Starch.

PubMed

Zeng, Shaoxiao; Chen, Bingyan; Zeng, Hongliang; Guo, Zebin; Lu, Xu; Zhang, Yi; Zheng, Baodong

2016-03-30

The objective of this study is to investigate the effect of microwave irradiation on the physicochemical and digestive properties of lotus seed starch. The physicochemical properties of lotus seed starch were characterized by light microscopy, (1)H NMR, FT-IR spectroscopy, and HPSEC-MALLS-RI. The starch-water interaction and crystalline region increased due to the changed water distribution of starch granules and the increase of the double-helix structure. The swelling power, amylose leaching, molecular properties, and radius of gyration reduced with the increasing microwave power, which further affected the sensitivity of lotus seed starch to enzymatic degradation. Furthermore, the resistant starch and slowly digestible starch increased with the increasing microwave irradiation, which further resulted in their decreasing hydrolysis index and glycemic index. The digestive properties of lotus seed starch were mainly influenced by the reduced branching degree of amylopectin and the strong amylose-amylose interaction.

[Determination of metal elements in PM2. 5 by ICP-OES with microwave digestion].

PubMed

Zhang, Liu-Yi; Fu, Chuan; Yang, Fu-Mo; Yang, Ji-Dong; Huang, Yi-Min; Zhang, Qiang; Wu, Bing-Yu

2014-11-01

In the present work, a method was developed for determining lead, zinc, copper, cadmium, znd chromium in PM2. 5 by inductively coupled plasma-optical emission spectrometry (ICP-OES) analysis with microwave digestion and glass fibre filter collection of samples. The microwave digestion systems were investigated and the experimental conditions were optimized. The results show that (1) HNO3-H2O02 digestion system is more stable and complete than HNO3-HCl and HNO3-H2 SO4 digestion systems; (2) The most sensitive emission wave length of lead, zinc, copper, cadmium, and chromium are 220.353, 213.857, 327.393, 228.802, and 267.716 nm, respectively; (3) The highest signal-to-noise ratios were observed under the conditions: RF power of 1 300 W, peristaltic pump flow rate of 1.5 mL x min(-1), cooling gas flow rate of 15 L x min(-1), and carrier gas flow rate of 0.8 L x min(-1). In addition, the detection limit for these elements ranged between 2.02 x 10(-3) and 8.20 x 10(-3(μg x mL(-1), the relative standard deviations (RSD, n = 6) for the samples were in the range of 1.86%-2.82%, and the recovery for the elements determined was from 91.6% to 103.7%. The proposed method was used for determination of the above five elements in atmospheric fine particulate matter at Wanzhou Monitoring Site of Chongqing Institute of Green and Intelligent Technology. The results revealed that the atmospheric fine particulate matter at this monitoring site was not polluted by cadmium and chromium, lead was at the level of potential contamination, while zinc and copper were at the level of slight pollution.

Microwave digestion preparation and ICP determination of boron in human plasma

NASA Technical Reports Server (NTRS)

Ferrando, A. A.; Green, N. R.; Barnes, K. W.; Woodward, B.

1993-01-01

A microwave digestion procedure, followed by Inductively Coupled Argon Plasma Spectroscopy, is described for the determination of boron (B) in human plasma. The National Institute of Standards and Technology (NIST) currently does not certify the concentration of B in any substance. The NIST citrus leaves 1572 (CL) Standard Reference Material (SRM) and wheat flour 1567a (WF) were chosen to determine the efficacy of digestion. CL and WF values compare favorably to those obtained from an open-vessel, wet digestion followed by ICP, and by neutron activation and mass spectrometric measurements. Plasma samples were oxidized by doubled-distilled ultrapure HNO3 in 120 mL PFA Teflon vessels. An MDS-81D microwave digestion procedure allows for rapid and relatively precise determination of B in human plasma, while limiting handling hazards and sources of contamination.

Multivariate optimization of a procedure employing microwave-assisted digestion for the determination of nickel and vanadium in crude oil by ICP OES.

PubMed

Dos Anjos, Shirlei L; Alves, Jeferson C; Rocha Soares, Sarah A; Araujo, Rennan G O; de Oliveira, Olivia M C; Queiroz, Antonio F S; Ferreira, Sergio L C

2018-02-01

This work presents the optimization of a sample preparation procedure using microwave-assisted digestion for the determination of nickel and vanadium in crude oil employing inductively coupled plasma optical emission spectrometry (ICP OES). The optimization step was performed utilizing a two-level full factorial design involving the following factors: concentrated nitric acid and hydrogen peroxide volumes, and microwave-assisted digestion temperature. Nickel and vanadium concentrations were used as responses. Additionally, a multiple response based on the normalization of the concentrations by the highest values was built to establish a compromise condition between the two analytes. A Doehlert matrix optimized the instrumental conditions of the ICP OE spectrometer. In this design, the plasma robustness was used as chemometric response. The experiments were performed using a digested oil sample solution doped with magnesium(II) ions, as well as a standard magnesium solution. The optimized method allows for the determination of nickel and vanadium with quantification limits of 0.79 and 0.20μgg -1 , respectively, for a digested sample mass of 0.1g. The precision (expressed as relative standard deviations) was determined using five replicates of two oil samples and the results obtained were 1.63% and 3.67% for nickel and 0.42% and 4.64% for vanadium. Bismuth and yttrium were also tested as internal standards, and the results demonstrate that yttrium allows for a better precision for the method. The accuracy was confirmed by the analysis of the certified reference material trace element in fuel oil (CRM NIST 1634c). The proposed method was applied for the determination of nickel and vanadium in five crude oil samples from Brazilian Basins. The metal concentrations found varied from 7.30 to 33.21μgg -1 for nickel and from 0.63 to 19.42μgg -1 for vanadium. Copyright © 2017. Published by Elsevier B.V.

Validation of a Sulfuric Acid Digestion Method for Inductively Coupled Plasma Mass Spectrometry Quantification of TiO2 Nanoparticles.

PubMed

Watkins, Preston S; Castellon, Benjamin T; Tseng, Chiyen; Wright, Moncie V; Matson, Cole W; Cobb, George P

2018-04-13

A consistent analytical method incorporating sulfuric acid (H 2 SO 4 ) digestion and ICP-MS quantification has been developed for TiO 2 quantification in biotic and abiotic environmentally relevant matrices. Sample digestion in H 2 SO 4 at 110°C provided consistent results without using hydrofluoric acid or microwave digestion. Analysis of seven replicate samples for four matrices on each of 3 days produced Ti recoveries of 97% ± 2.5%, 91 % ± 4.0%, 94% ± 1.8%, and 73 % ± 2.6% (mean ± standard deviation) from water, fish tissue, periphyton, and sediment, respectively. The method demonstrated consistent performance in analysis of water collected over a 1 month.

Optimization and microbial community analysis of anaerobic co-digestion of food waste and sewage sludge based on microwave pretreatment.

PubMed

Zhang, Junya; Lv, Chen; Tong, Juan; Liu, Jianwei; Liu, Jibao; Yu, Dawei; Wang, Yawei; Chen, Meixue; Wei, Yuansong

2016-01-01

The effects of microwave pretreatment (MW) on co-digestion of food waste (FW) and sewage sludge (SS) have never been investigated. In this study, a series of mesophilic biochemical methane potential (BMP) tests were conducted to determine the optimized ratio of FW and SS based on MW, and the evolution of bacterial and archaeal community was investigated through high-throughput sequencing method. Results showed that the optimized ratio was 3:2 for co-digestion of FW and SS based on MW, and the methane production was 316.24 and 338.44mLCH4/gVSadded for MW-FW and MW-SS, respectively. The MW-SS was superior for methane production compared to MW-FW, in which accumulation of propionic acid led to the inhibition of methanogenesis. Proteiniborus and Parabacteroides were responsible for proteins and polysaccharides degradation for all, respectively, while Bacteroides only dominated in co-digestion. Methanosphaera dominated in MW-FW at the active methane production phase, while it was Methanosarcina in MW-SS and mono-SS. Copyright © 2015 Elsevier Ltd. All rights reserved.

A novel and eco-friendly analytical method for phosphorus and sulfur determination in animal feed.

PubMed

Novo, Diogo L R; Pereira, Rodrigo M; Costa, Vanize C; Hartwig, Carla A; Mesko, Marcia F

2018-04-25

An eco-friendly method for indirect determining phosphorus and sulfur in animal feed by ion chromatography was proposed. Using this method, it was possible to digest 500 mg of animal feed in a microwave system under oxygen pressure (20 bar) using only a diluted acid solution (2 mol L -1 HNO 3 ). The accuracy of the proposed method was evaluated by recovery tests, by analysis of reference material (RM) and by comparison of the results with those obtained using conventional microwave-assisted digestion. Moreover, P results were compared with those obtained from the method recommended by AOAC International for animal feed (Method nr. 965.17) and no significant differences were found between the results. Recoveries for P and S were between 94 and 97%, and agreements with the reference values of RM were better than 94%. Phosphorus and S concentrations in animal feeds ranged from 10,026 to 28,357 mg kg -1 and 2259 to 4601 mg kg -1 , respectively. Copyright © 2017 Elsevier Ltd. All rights reserved.

Determination of total lead in lipstick: development and validation of a microwave-assisted digestion, inductively coupled plasma-mass spectrometric method.

PubMed

Hepp, Nancy M; Mindak, William R; Cheng, John

2009-01-01

Recent reports describing the presence of lead (Pb) in lipsticks have suggested that, under ordinary use, the potential amount of Pb exposure is harmful. To permit independent assessment of the Pb contamination, a method for determining total Pb in lipstick using microwave-assisted digestion and analysis employing inductively coupled plasma-mass spectrometry (ICP-MS) was developed and validated. Since lipsticks may contain fats, oils, pigments, dyes, and minerals, several reference materials (RM) were analyzed, including coal, wear metals in oil, organic Pb in oil, milk powder, and estuarine sediment. With the exception of the RM with mineral content (estuarine sediment), complete recovery of Pb from the RMs was obtained by simple nitric acid (HNO(3)) digestion. Complete recovery of Pb from estuarine sediment was achieved only when hydrofluoric acid (HF) was added to the digestion mix, followed by treatment with excess boric acid (H(3)BO(3)) to neutralize the HF and to dissolve insoluble fluorides. Commercial lipsticks were tested for total Pb by the validated method. The detection limit was estimated to be 0.04 microg Pb/g. The average value obtained for the lipsticks was 1.07 microg/g. Undigested material was present in some lipstick digests when only HNO(3) was used, and generally lower Pb values were obtained. All of the Pb levels found by the U.S. Food and Drug Administration (FDA) were within the range the agency would expect to find in lipsticks formulated with permitted color additives and other ingredients prepared under good manufacturing practice (GMP) conditions. This method will be useful for the FDA and industry in helping to ensure the safety of cosmetic products.

Microwave Thermal Hydrolysis Of Sewage Sludge As A Pretreatment Stage For Anaerobic Digestion

NASA Astrophysics Data System (ADS)

Qiao, W.; Wang, W.; Xun, R.

2008-02-01

This article focuses on the effects of microwave thermal hydrolysis on sewage sludge anaerobic digestion. Volatile suspended solid (VSS) and COD solubilization of treated sludge were investigated. It was found that the microwave hydrolysis provided a rapid and efficient process to release organics from sludge. The increase of organic dissolution ratio was not obvious when holding time was over 5 min. The effect of the VSS solubilization was mainly dependent on temperature. The highest value of VSS dissolving ratio, 36.4%, was obtained at 170 °C for 30 min. COD dissolving ratio was about 25% at 170 °C. BMP test of excess sludge and mixture of primary and excess sludge proved the increase of methane production. Total biogas production of microwave treated mixture sludge increased by 12.9% to 20.2% over control after 30 days digestion. For excess sludge, biogas production was 11.1% to 25.9% higher than untreated sludge.

A simple design for microwave assisted digestion vessel with low reagent consumption suitable for food and environmental samples

NASA Astrophysics Data System (ADS)

Gholami, Mehrdad; Behkami, Shima; Zain, Sharifuddin Md.; Bakirdere, Sezgin

2016-11-01

The objective of this work is to prepare a cost-effective, low reagent consumption and high performance polytetrafluoroethylene (PTFE) vessel that is capable to work in domestic microwave for digesting food and environmental samples. The designed vessel has a relatively thicker wall compared to that of commercial vessels. In this design, eight vessels are placed in an acrylonitrile butadiene styrene (ABS) holder to keep them safe and stable. This vessel needs only 2.0 mL of HNO3 and 1.0 mL H2O2 to digest 100 mg of biological sample. The performance of this design is then evaluated with an ICP-MS instrument in the analysis of the several NIST standard reference material of milk 1849a, rice flour 1568b, spinach leave 1570a and Peach Leaves 1547 in a domestic microwave oven with inverter technology. Outstanding agreement to (SRM) values are observed by using the suggested power to time microwave program, which simulates the reflux action occurring in this closed vessel. Taking into account the high cost of commercial microwave vessels and the volume of chemicals needed for various experiments (8-10 mL), this simple vessel is cost effective and suitable for digesting food and environmental samples.

Partial microwave-assisted wet digestion of animal tissue using a baby-bottle sterilizer for analyte determination by inductively coupled plasma optical emission spectrometry

NASA Astrophysics Data System (ADS)

Matos, Wladiana O.; Menezes, Eveline A.; Gonzalez, Mário H.; Costa, Letícia M.; Trevizan, Lilian C.; Nogueira, Ana Rita A.

2009-06-01

A procedure for partial digestion of bovine tissue is proposed using polytetrafluoroethylene (PTFE) micro-vessels inside a baby-bottle sterilizer under microwave radiation for multi-element determination by inductively coupled plasma optical emission spectrometry (ICP OES). Samples were directly weighed in laboratory-made polytetrafluoroethylene vessels. Nitric acid and hydrogen peroxide were added to the uncovered vessels, which were positioned inside the baby-bottle sterilizer, containing 500 mL of water. The hydrogen peroxide volume was fixed at 100 µL. The system was placed in a domestic microwave oven and partial digestion was carried out for the determination of Ca, Cu, Fe, Mg, Mn and Zn by inductively coupled plasma optical emission spectrometry. The single-vessel approach was used in the entire procedure, to minimize contamination in trace analysis. Better recoveries and lower residual carbon content (RCC) levels were obtained under the conditions established through a 2 4-1 fractional factorial design: 650 W microwave power, 7 min digestion time, 50 µL nitric acid and 50 mg sample mass. The digestion efficiency was ascertained according to the residual carbon content determined by inductively coupled plasma optical emission spectrometry. The accuracy of the proposed procedure was checked against two certified reference materials.

ICP-AES determination of minor- and major elements in apples after microwave assisted digestion.

PubMed

Juranović Cindrić, Iva; Krizman, Ivona; Zeiner, Michaela; Kampić, Štefica; Medunić, Gordana; Stingeder, Gerhard

2012-12-15

The aim of this paper was to determine the content of minor and major elements in apples by inductively coupled plasma atomic emission spectrometry (ICP-AES). Prior to ICP-AES measurement, dried apples were digested in a microwave assisted digestion system. The differences in the measured element concentrations after application of open and closed microwave system as sample preparation procedures are discussed. In whole apples, flesh and peel Ag, Al, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, Sr and Zn were analysed after optimisation and validating the analytical method using ICP-AES. The accuracy of the method determined by spiking experiments was very good (recoveries 88-115%) and the limits of detection of elements of interest were from 0.01 up to 14.7 μg g(-1). The reference ranges determined in all apple samples are 39-47 mg g(-1) for K, 9-14 mg g(-1) for Na, 3-7 mg g(-1) for Mg, 3-7 μg g(-1) for Zn, 0.7-2.8 μg g(-1) for Sr. The range of Mn in peel 4-6 μg g(-1) is higher compared to whole apple from 0.7 to 1.7 μg g(-1). Cd is found only in peel, in the concentration range of 0.4-1.1 μg g(-1). Copyright © 2012 Elsevier Ltd. All rights reserved.

The Successful Diagnosis and Typing of Systemic Amyloidosis Using A Microwave-Assisted Filter-Aided Fast Sample Preparation Method and LC/MS/MS Analysis

PubMed Central

Zou, Lili; Shen, Kaini; Zhong, Dingrong; Zhou, Daobin; Sun, Wei; Li, Jian

2015-01-01

Laser microdissection followed by mass spectrometry has been successfully used for amyloid typing. However, sample contamination can interfere with proteomic analysis, and overnight digestion limits the analytical throughput. Moreover, current quantitative analysis methods are based on the spectrum count, which ignores differences in protein length and may lead to misdiagnoses. Here, we developed a microwave-assisted filter-aided sample preparation (maFASP) method that can efficiently remove contaminants with a 10-kDa cutoff ultrafiltration unit and can accelerate the digestion process with the assistance of a microwave. Additionally, two parameters (P- and D-scores) based on the exponentially modified protein abundance index were developed to define the existence of amyloid deposits and those causative proteins with the greatest abundance. Using our protocol, twenty cases of systemic amyloidosis that were well-typed according to clinical diagnostic standards (training group) and another twenty-four cases without subtype diagnoses (validation group) were analyzed. Using this approach, sample preparation could be completed within four hours. We successfully subtyped 100% of the cases in the training group, and the diagnostic success rate in the validation group was 91.7%. This maFASP-aided proteomic protocol represents an efficient approach for amyloid diagnosis and subtyping, particularly for serum-contaminated samples. PMID:25984759

Plasma-based determination of inorganic contaminants in waste of electric and electronic equipment after microwave-induced combustion

NASA Astrophysics Data System (ADS)

Mello, Paola A.; Diehl, Lisarb O.; Oliveira, Jussiane S. S.; Muller, Edson I.; Mesko, Marcia F.; Flores, Erico M. M.

2015-03-01

A systematic study was performed for the determination of inorganic contaminants in polymeric waste from electrical and electronic equipment (EEE) for achieving an efficient digestion to minimize interferences in determination using plasma-based techniques. The determination of As, Br, Cd, Co, Cr, Cu, Ni, Pb, Sb, and Zn by inductively coupled plasma mass spectrometry (ICP-MS) and also by inductively coupled plasma optical emission spectrometry (ICP OES) was carried out after digestion using microwave-induced combustion (MIC). Arsenic and Hg were determined by flow-injection chemical vapor generation inductively coupled plasma mass spectrometry (FI-CVG-ICP-MS). Dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS) with ammonia was also used for Cr determination. The suitability of MIC for digestion of sample masses up to 400 mg was demonstrated using microcrystalline cellulose as aid for combustion of polymers from waste of EEEs that usually contain flame retardants that impair the combustion. The composition and concentration of acid solutions (HNO3 or HNO3 plus HCl) were evaluated for metals and metalloids and NH4OH solutions were investigated for Br absorption. Accuracy was evaluated by comparison of results with those obtained using high pressure microwave-assisted wet digestion (HP-MAWD) and also by the analysis of certified reference material (CRM) of polymer (EC680k-low-density polyethylene). Bromine determination was only feasible using digestion by MIC once losses were observed when HP-MAWD was used. Lower limits of detection were obtained for all analytes using MIC (from 0.005 μg g- 1 for Co by ICP-MS up to 3.120 μg g-1 for Sb by ICP OES) in comparison to HP-MAWD due to the higher sample mass that can be digested (400 mg) and the use of diluted absorbing solutions. The combination of HNO3 and HCl for digestion showed to be crucial for quantitative recovery of some elements, as Cr and Sb. In addition, suitable agreement of Cr to CRM value was only obtained by mixing NH4Cl to samples before combustion. No statistical difference (95% confidence level) was observed between the results obtained for As, Cd, Co, Cr, Cu, Hg, Ni, Pb, Sb, and Zn by MIC and HP-MAWD methods. Agreement with certified values was better than 96% using MIC for all inorganic contaminants. Particularly for Br, MIC was the method of choice for digestion due to the possibility of using diluted alkaline solutions for analyte absorption. Based on the obtained results, MIC can be considered as a suitable method for digestion of polymers from waste of EEEs for further plasma based determination of inorganic contaminants.

A novel methodology for rapid digestion of rare earth element ores and determination by microwave plasma-atomic emission spectrometry and dynamic reaction cell-inductively coupled plasma-mass spectrometry.

PubMed

Helmeczi, Erick; Wang, Yong; Brindle, Ian D

2016-11-01

Short-wavelength infrared radiation has been successfully applied to accelerate the acid digestion of refractory rare-earth ore samples. Determinations were achieved with microwave plasma-atomic emission spectrometry (MP-AES) and dynamic reaction cell - inductively coupled plasma-mass spectrometry (DRC-ICP-MS). The digestion method developed was able to tackle high iron-oxide and silicate matrices using only phosphoric acid in a time frame of only 8min, and did not require perchloric or hydrofluoric acid. Additionally, excellent recoveries and reproducibilities of the rare earth elements, as well as uranium and thorium, were achieved. Digestions of the certified reference materials OREAS-465 and REE-1, with radically different mineralogies, delivered results that mirror those obtained by fusion processes. For the rare-earth CRM OKA-2, whose REE data are provisional, experimental data for the rare-earth elements were generally higher than the provisional values, often exceeding z-values of +2. Determined values for Th and U in this reference material, for which certified values are available, were in excellent agreement. Copyright © 2016 Elsevier B.V. All rights reserved.

Changes on antioxidant activity of microwave-treated protein hydrolysates after simulated gastrointestinal digestion: Purification and identification.

PubMed

Ketnawa, Sunantha; Wickramathilaka, Malithi; Liceaga, Andrea M

2018-07-15

Two samples of trout frame protein hydrolysates were prepared by Microwave Pretreatment followed by Conventional Enzymatic hydrolysis (MPCE) and Non-Pretreated followed by Microwave-assisted Enzymatic hydrolysis (NPME), respectively, were subjected to simulated gastrointestinal digestion. Changes on degree of hydrolysis, antioxidant activity, molecular weight, and amino acid composition between undigested and after gastrointestinal digestion of peptides were investigated. Comparing to undigested peptides, a breakdown of MPCE and NPME into smaller molecules was observed. Degree of hydrolysis, ABTS + radical scavenging activity and reducing power increased (P < 0.05) for both samples after gastrointestinal digestion. A purified peptide from GI-MPCE had two possible sequences, NGRLGYSEGVM or GNRLGYSWDD (1182.65 Da). Whereas GI-NPME had two peptides IRGPEEHMHR or RVAPEEHMHR (1261.77 Da) and SAGVPRHK or SARPRHK (962.63 Da). These results indicate that digested hydrolysates can be a rich source of antioxidants. Isolated peptides extracted from trout frame by-products could be new food ingredients used as natural antioxidants. Copyright © 2018 Elsevier Ltd. All rights reserved.

Comparison of Conventional and Microwave Treatment on Soymilk for Inactivation of Trypsin Inhibitors and In Vitro Protein Digestibility

PubMed Central

Vagadia, Brinda Harish; Raghavan, Vijaya

2018-01-01

Soymilk is lower in calories compared to cow’s milk, since it is derived from a plant source (no cholesterol) and is an excellent source of protein. Despite the beneficial factors, soymilk is considered as one of the most controversial foods in the world. It contains serine protease inhibitors which lower its nutritional value and digestibility. Processing techniques for the elimination of trypsin inhibitors and lipoxygenase, which have shorter processing time and lower production costs are required for the large-scale manufacturing of soymilk. In this study, the suitable conditions of time and temperature are optimized during microwave processing to obtain soymilk with maximum digestibility with inactivation of trypsin inhibitors, in comparison to the conventional thermal treatment. The microwave processing conditions at a frequency of 2.45 GHz and temperatures of 70 °C, 85 °C and 100 °C for 2, 5 and 8 min were investigated and were compared to conventional thermal treatments at the same temperature for 10, 20 and 30 min. Response surface methodology is used to design and optimize the experimental conditions. Thermal processing was able to increase digestibility by 7% (microwave) and 11% (conventional) compared to control, while trypsin inhibitor activity reduced to 1% in microwave processing and 3% in conventional thermal treatment when compared to 10% in raw soybean. PMID:29316679

Microstructural characteristics and gastro-small intestinal digestion in vitro of potato starch: Effects of refrigerated storage and reheating in microwave.

PubMed

Colussi, Rosana; Singh, Jaspreet; Kaur, Lovedeep; Zavareze, Elessandra da Rosa; Dias, Alvaro Renato Guerra; Stewart, Robert B; Singh, Harjinder

2017-07-01

The objective of our study was to evaluate paste clarity, retrogradation (syneresis %), thermal characteristics and kinetics of glucose release during in vitro gastro-small intestinal digestion of freshly cooked and refrigerated potato starch. Freshly cooked starch pastes had a paste clarity of 71%, which decreased to 35.4% whereas syneresis (%) increased after 7days of refrigerated storage. The X-ray and thermal characteristics of native, retrograded and microwave reheated starch samples differed significantly from each other. For the freshly cooked starch pastes, ∼88% starch hydrolysis was observed at the end (150min) of digestion under simulated gastro-small intestinal conditions that decreased to ∼70% for the 7day stored pastes. The hydrolysis (%) of refrigerated pastes increased to 86% and 92% after one and two cycles of microwave reheating, respectively. These results contribute to the understanding of starch retrogradation in relation to starch digestion. Copyright © 2017 Elsevier Ltd. All rights reserved.

Experimental continuous sludge microwave system to enhance dehydration ability and hydrogen production from anaerobic digestion of sludge.

PubMed

Zhou, Cuihong; Huang, Xintong; Zeng, Meng

2018-05-01

Dehydrating large amounts of sludge produced by sewage treatment plants is difficult. Microwave pretreatment can effectively and significantly improve the dewaterability and hydrogen production of sludge subjected to anaerobic digestion. The aim of this study was to investigate the effects of different microwave conditions on hydrogen production from anaerobic digestion and dewaterability of sludge. Based on an analysis of the electric field distribution, a spiral reactor was designed and a continuous microwave system was built to conduct intermittent and continuous experiments under different conditions. Settling Volume, Capillary Suction Time, particle size, and moisture content of the sludge were measured. The results show that sludge pretreatment in continuous experiments has equally remarkable dehydration performance as in intermittent experiments; the minimum moisture content was 77.29% in the intermittent experiment under a microwave power of 300W and an exposure time of 60sec, and that in the continuous experiment was 77.56% under a microwave power of 400W and an exposure time of 60sec. The peak measured by Differential Scanning Calorimeter appeared earliest under a microwave power of 600W and an exposure time of 180sec. The heat flux at the peak was 4.343W/g, which is relatively small. This indicates that microwave pretreatment induced desirable effects. The maximum yield of hydrogen production was 7.967% under the conditions of microwave power of 500W, exposure time of 120sec, and water bath at 55°C. This research provides a theoretical and experimental basis for the development of a continuous microwave sludge-conditioning system. Copyright © 2017. Published by Elsevier B.V.

Maxwell-Wagner Effect Applied to Microwave-Induced Self-Ignition: A Novel Approach for Carbon-Based Materials.

PubMed

Bizzi, Cezar A; Cruz, Sandra M; Schmidt, Lucas; Burrow, Robert A; Barin, Juliano S; Paniz, Jose N G; Flores, Erico M M

2018-04-03

A new method for analytical applications based on the Maxwell-Wagner effect is proposed. Considering the interaction of carbonaceous materials with an electromagnetic field in the microwave frequency range, a very fast heating is observed due to interfacial polarization that results in localized microplasma formation. Such effect was evaluated in this work using a monomode microwave system, and temperature was recorded using an infrared camera. For analytical applications, a closed reactor under oxygen pressure was evaluated. The combination of high temperature and oxidant atmosphere resulted in a very effective self-ignition reaction of sample, allowing its use as sample preparation procedure for further elemental analysis. After optimization, a high sample mass (up to 600 mg of coal and graphite) was efficiently digested using only 4 mol L -1 HNO 3 as absorbing solution. Several elements (Ba, Ca, Fe, K, Li, Mg, Na, and Zn) were determined by inductively coupled plasma optical emission spectrometry (ICP-OES). Accuracy was evaluated by using a certified reference material (NIST 1632b). Blanks were negligible, and only a diluted solution was required for analytes absorption preventing residue generation and making the proposed method in agreement with green chemistry recommendations. The feasibility of the proposed method for hard-to-digest materials, the minimization of reagent consumption, and the possibility of multi elemental analysis with lower blanks and better limits of detection can be considered as the main advantages of this method.

Evaluation of the effects of low energetic microwave irradiation on anaerobic digestion.

PubMed

Bastiaens, Bert; Van den Broeck, Rob; Appels, Lise; Dewil, Raf

2017-11-01

The present study investigates the effects of microwave irradiation on the performance of anaerobic digestion processes. A first set of experiments is performed to distinguish the upper limit of the applied energy levels. Secondly, the effects of these treatments on the performance of the digestion process are evaluated in 3 experimental setups: (i) monitoring the acetic acid degradation, (ii) performing a biological methane potential (BMP) assay and (iii) conducting a specific methanogenic activity (SMA) test. The solubilisation experiment reveals a limited degree of disintegration of anaerobic biomass up to a microwave treatment of 10000 kJ/kg TS. Above this threshold value the soluble COD level started to rise, with up to 350% at 30000 kJ/kg TS regardless of the microwave output power. Because solubilisation of the biomass increases the easily degradable content, this would lead to false observations regarding increased activity. Therefore, solubilisation is minimized by limiting the microwave treatment to a maximum of 6000 kJ/kg TS during the second part of the experiments. Monitoring the degradation of acetic acid after a low intensity microwave treatment, reveals that microwave irradiation shortens the lag phase, e.g., from 21 to 3 h after a microwave treatment of 1000 kJ/kg TS at 100 W. However most treatments also result in a decrease of the maximum degradation and of the degradation rate of acetic acid. BMP assays are performed to evaluate the activity and performance of the entire anaerobic community. Every treatment results in a decreased biogas production potential and decreased biogas production rate. Moreover, each treatment induced an increase of the lag phase. The SMA experiments show no influence of the microwave irradiation in terms of biogas or methane production. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effect of microwave hydrolysis on transformation of steroidal hormones during anaerobic digestion of municipal sludge cake.

PubMed

Hamid, Hanna; Eskicioglu, Cigdem

2013-09-15

Fate and removal of 16 steroidal (estrogenic, androgenic and progestogenic) hormones were studied during advanced anaerobic digestion of sludge cake using microwave (MW) pretreatment. Effect of pretreatment temperature (80, 120, 160 °C), operating temperature (mesophilic at 35 ± 2 °C, thermophilic at 55 ± 2 °C) and sludge retention time (SRT: 20, 10, 5 days) were studied employing eight lab-scale semi-continuously fed digesters. To determine the potential effect of MW hydrolysis, hormones were quantified in total (sorbed + soluble) and supernatant (soluble) phases of the digester influent and effluent streams. Seven of 16 hormones were above the method reporting limit (RL) in one or more of the samples. Hormone concentrations in total phase of un-pretreated (control) and pretreated digester feeds ranged in <157-2491 ng/L and <157-749 ng/L, respectively. The three studied factors were found to be statistically significant (95% confidence level) in removal of one or more hormones from soluble and/or total phase. MW hydrolysis of the influent resulted in both release (from sludge matrix) and attenuation of hormones in the soluble phase. Accumulation of estrone (E1) as well as progesterone (Pr) and androstenedione (Ad) in most of the digesters indicated possible microbial transformations among the hormones. Compared to controls, all pretreated digesters had lower total hormone concentrations in their influent streams. At 20 days SRT, highest total removal (E1+E2+Ad +Pr) was observed for the thermophilic control digester (56%), followed by pretreated mesophilic digesters at 120 °C and 160 °C with around 48% efficiency. In terms of conventional performance parameters, relative (to control) improvements of MW pretreated digesters at a 5-d SRT ranged in 98-163% and 57-121%, for volatile solids removal and methane production, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

Method for Extraction and Multielement Analysis of Hypogymnia Physodes Samples from the Athabasca Oil Sands Region

EPA Science Inventory

A microwave-assisted digestion technique followed by ICPMS (inductively coupled plasma-mass spectrometry) analysis was used to measure concentrations of 43 elements in Hypogymnia physodes samples collected in the Athabasca Oil Sands Region (AOSR) of northern Alberta, Canad...

Microwave Digestion and Furnace Atomic Absorption Method for the Quantification of Nano-scale TiO2 in Aqueous Samples

EPA Science Inventory

Many nanomaterials posses physical, and potentially biological, activity that is unique relative to their macro-scaled or soluble forms. One such property is surface plasmon resonance; a phenomenon that can generate or facilitate photoreactivity. Optimization of these properties ...

[Study on the determination of 14 inorganic elements in coffee by inductively coupled plasma mass spectrometry].

PubMed

Nie, Xi-Du; Fu, Liang

2013-07-01

Samples of coffee were digested by microwave digestion, and inorganic elements amounts of Na, Mg, P, Ca, Cr, Mn, Fe, Co, Cu, Zn, As, Se, Mo and Pb in sample solutions were determined by inductively coupled plasma mass spectrometry (ICP-MS). HNO3 + H2O2 was used to achieve the complete decomposition of the organic matrix in a closed-vessel microwave oven. The working parameters of the instrument were optimized. The results showed that the relative standard deviation (RSD) was less than 3.84% for all the elements, and the recovery was found to be 92.00% -106.52% by adding standard recovery experiment. This method was simple, sensitive and precise and can perform simultaneous multi-elements determination of coffee, which could satisfy the sample examination request and provide scientific rationale for determining inorganic elements of coffee.

Determination of arsenic, cadmium, cobalt, chromium, lead, molybdenum, nickel, and selenium in fertilizers by microwave digestion and inductively coupled plasma-optical emission spectrometry detection: collaborative study.

PubMed

Kane, Peter F; Hall, William L

2006-01-01

There is increasing regulatory interest in the non-nutritive metals content of fertilizer materials, but at present there is no consensus analytical method for acid digestion and instrument detection of those elements in fertilizer matrixes. This lack of method standardization has resulted in unacceptable variability of results between fertilizer laboratories performing metals analysis. A method has been developed using microwave digestion with nitric acid at 200 degrees C, followed by inductively coupled plasma-optical emission spectrometry instrument detection, for the elements arsenic, cadmium, cobalt, chromium, molybdenum, nickel, lead, and selenium. The method has been collaboratively studied, and statistical results are here reported. Fourteen collaborators were sent 62 sample materials in a blind duplicate design. Materials represented a broad cross section of fertilizer types, including phosphate ore, manufactured phosphate products, N-P-K blends, organic fertilizers, and micro-nutrient materials. As much as possible within the limit of the number of samples, materials were selected from different regions of the United States and the world. Limit of detection (LOD) was determined using synthetic fertilizers consisting of reagent grade chemicals with near zero levels of the non-nutritive elements, analyzed blindly. Samples with high iron content caused the most variability between laboratories. Most samples reasonably above LOD gave HorRat values within the range 0.5 to 2.0, indicating acceptable method performance according to AOAC guidelines for analyses in the mg/kg range. The method is recommended for AOAC Official First Action status.

Effect of alkaline microwaving pretreatment on anaerobic digestion and biogas production of swine manure.

PubMed

Yu, Tao; Deng, Yihuan; Liu, Hongyu; Yang, Chunping; Wu, Bingwen; Zeng, Guangming; Lu, Li; Nishimura, Fumitake

2017-05-10

Microwave assisted with alkaline (MW-A) condition was applied in the pretreatment of swine manure, and the effect of the pretreatment on anaerobic treatment and biogas production was evaluated in this study. The two main microwaving (MW) parameters, microwaving power and reaction time, were optimized for the pretreatment. Response surface methodology (RSM) was used to investigate the effect of alkaline microwaving process for manure pretreatment at various values of pH and energy input. Results showed that the manure disintegration degree was maximized of 63.91% at energy input of 54 J/g and pH of 12.0, and variance analysis indicated that pH value played a more important role in the pretreatment than in energy input. Anaerobic digestion results demonstrated that MW-A pretreatment not only significantly increased cumulative biogas production, but also shortened the duration for a stable biogas production rate. Therefore, the alkaline microwaving pretreatment could become an alternative process for effective treatment of swine manure.

Simultaneous Determination of 10 Ultratrace Elements in Infant Formula, Adult Nutritionals, and Milk Products by ICP/MS After Pressure Digestion: Single-Laboratory Validation.

PubMed

Dubascoux, Stephane; Nicolas, Marine; Rime, Celine Fragniere; Payot, Janique Richoz; Poitevin, Eric

2015-01-01

A single-laboratory validation (SLV) is presented for the simultaneous determination of 10 ultratrace elements (UTEs) including aluminum (Al), arsenic (As), cadmium (Cd), cobalt (Co), chromium (Cr), mercury (Hg), molybdenum (Mo), lead (Pb), selenium (Se), and tin (Sn) in infant formulas, adult nutritionals, and milk based products by inductively coupled plasma (ICP)/MS after acidic pressure digestion. This robust and routine multielemental method is based on several official methods with modifications of sample preparation using either microwave digestion or high pressure ashing and of analytical conditions using ICP/MS with collision cell technology. This SLV fulfills AOAC method performance criteria in terms of linearity, specificity, sensitivity, precision, and accuracy and fully answers most international regulation limits for trace contaminants and/or recommended nutrient levels established for 10 UTEs in targeted matrixes.

Determination of calcium, magnesium, sodium, and potassium in foodstuffs by using a microsampling flame atomic absorption spectrometric method after closed-vessel microwave digestion: method validation.

PubMed

Chekri, Rachida; Noël, Laurent; Vastel, Christelle; Millour, Sandrine; Kadar, Ali; Guérin, Thierry

2010-01-01

This paper describes a validation process in compliance with the NFIEN ISO/IEC 17025 standard for the determination of the macrominerals calcium, magnesium, sodium, and potassium in foodstuffs by microsampling with flame atomic absorption spectrometry after closed-vessel microwave digestion. The French Standards Commission (Agence Francaise de Normalisation) standards NF V03-110, NF EN V03-115, and XP T-90-210 were used to evaluate this method. The method was validated in the context of an analysis of the 1322 food samples of the second French Total Diet Study (TDS). Several performance criteria (linearity, LOQ, specificity, trueness, precision under repeatability conditions, and intermediate precision reproducibility) were evaluated. Furthermore, the method was monitored by several internal quality controls. The LOQ values obtained (25, 5, 8.3, and 8.3 mg/kg for Ca, Mg, Na, and K, respectively) were in compliance with the needs of the TDS. The method provided accurate results as demonstrated by a repeatability CV (CVr) of < 7% and a reproducibility CV (CVR) of < 12% for all the elements. Therefore, the results indicated that this method could be used in the laboratory for the routine determination of these four elements in foodstuffs with acceptable analytical performance.

Effects of digestion, chemical separation, and deposition on Po-210 quantitative analysis

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

Seiner, Brienne N.; Morley, Shannon M.; Beacham, Tere A.

Polonium-210 is a radioactive isotope often used to study sedimentation processes, food chains, aerosol behavior, and atmospheric circulations related to environmental sciences. Materials for the analysis of Po-210 range from tobacco leaves or cotton fibers, to soils and sediments. The purpose of this work was to determine polonium losses from a variety of sample types (soil, cotton fiber, and air filter) due to digestion technique, chemical separation, and deposition method for alpha energy analysis. Results demonstrated that yields from a perchloric acid wet-ash were similar to that from a microwave digestion. Both were greater than the dry-ash procedure. The poloniummore » yield from the perchloric acid wet ash was 87 ± 5%, the microwave digestion had a yield of 100 ± 7%, and the dry ash had a yield of 38 ± 5%. The chemical separation of polonium by an anion exchange resin was used only on the soil samples due to the complex nature of this sample. The yield of Po-209 tracer after chemical separation and deposition for alpha analysis was 83 ± 7% for the soil samples. Spontaneous deposition yields for the cotton and air filters were 87 ± 4% and 92 ± 6%, respectively. Based on the overall process yields for each sample type the amount of Po-210 was quantified using alpha energy analysis. The soil contained 0.18 ± 0.08 Bq/g, the cotton swipe contained 0.7 mBq/g, and the air filter contained 0.04 ± 0.02 mBq/g. High and robust yields of polonium are possible using a suitable digestion, separation, and deposition method.« less

Simultaneous determination of suspended particulate trace metals (Co, Ni, Cu, Zn, Cd and Pb) in seawater with small volume filtration assisted by microwave digestion and flow injection inductively coupled plasma mass spectrometer.

PubMed

Nakatsuka, Seiji; Okamura, Kei; Norisuye, Kazuhiro; Sohrin, Yoshiki

2007-06-26

A new technique for the determination of suspended particulate trace metals (P-metals >0.2 microm), such as Co, Ni, Cu, Zn, Cd and Pb, in open ocean seawater has been developed by using microwave digestion coupled with flow injection inductively coupled plasma mass spectrometry (FI-ICP-MS). Suspended particulate matter (SPM) was collected from 500 mL of seawater on a Nuclepore filter (0.2 microm) using a closed filtration system. Both the SPM and filter were completely dissolved by microwave digestion. Reagents for the digestion were evaporated using a clean evaporation system, and the metals were redissolved in 0.8 M HNO3. The solution was diluted with buffer solution to give pH 5.0 and the metals were determined by FI-ICP-MS using a chelating adsorbent of 8-hydroxyquinoline immobilized on fluorinated metal alkoxide glass (MAF-8HQ). The procedure blanks with a filter were found to be 0.048+/-0.008, 10.3+/-0.3, 0.27+/-0.05, 3.3+/-1.8, 0.02+/-0.03 and 0.85+/-0.09 ng L(-1) for Co, Ni, Cu, Zn, Cd and Pb, respectively (n=14). Detection limits defined as 3 times the standard deviation of the blanks were 0.023, 0.90, 0.14, 5.3, 0.078 and 0.28 ng L(-1) for Co, Ni, Cu, Zn, Cd and Pb, respectively. Accuracy was evaluated using certified reference materials of chlorella (NES CRM No. 3) and marine sediment (HISS-1). The method was applied to the determination of vertical distributions for P-Co, Ni, Cu, Zn, Cd and Pb in the Western North Pacific.

Rheological properties of sewage sludge during enhanced anaerobic digestion with microwave-H2O2 pretreatment.

PubMed

Liu, Jibao; Yu, Dawei; Zhang, Jian; Yang, Min; Wang, Yawei; Wei, Yuansong; Tong, Juan

2016-07-01

The rheological behavior of sludge is of serious concern in anaerobic digestion. This study investigated the rheological properties of sewage sludge during enhanced anaerobic digestion with microwave-H2O2 pretreatment (MW-H2O2). The results showed that MW-H2O2 pretreatment resulted in the improvement of sludge flowability and weakening of its viscoelastic properties. Further positive effects on the rheological properties of digested sludge during anaerobic digestion were observed. The flowability was improved with a low level of apparent viscosity. The decrease of the consistency index and increase of the flow behavior index indicated that the strength of the inner structures and non-Newtonian flow characteristics of digested sludge weakened. Both the storage modulus (G') and loss modulus (G″) decreased, indicating that the viscoelastic behavior became weak. These effects were possibly attributed to the changes of the digested sludge micro-structures, such as extracellular polymeric substances (EPS). This study concluded that anaerobic digestion for treating sewage sludge combined with pretreatment is a more favorable option than single anaerobic digestion from the perspective of rheology. Copyright © 2016 Elsevier Ltd. All rights reserved.

Survival of Anisakis simplex in microwave-processed arrowtooth flounder (Atheresthes stomias).

PubMed

Adams, A M; Miller, K S; Wekell, M M; Dong, F M

1999-04-01

The purpose of this study was to define the relationship between survival and temperature of nematodes of the species Anisakis simplex in microwave-processed arrowtooth flounder (Atheresthes stomias). Ten fillets (each 126 to 467 g, 0.5 to 1.75 cm thick), with an average of five larvae of Anisakis simplex per fillet, were processed to target temperatures on high (100%) power using a commercial 700-W microwave oven. Fillets were neither covered nor rotated and had a temperature probe inserted to two-thirds depth into the thickest portion. After the fillet was digested using a 1% pepsin solution, the viability of nematodes was determined by viewing them under a dissecting microscope. Survival rates were 31% at 140 degrees F (60 degrees C), 11% at 150 degrees F (65 degrees C), 2% at 160 degrees F (71 degrees C), 3% at 165 degrees F (74 degrees C), and 0% at 170 degrees F (77 degrees C). Microwave processing of standardized fillet "sandwiches," 14 cm long, 4.5 cm wide, and approximately 1.75 cm high, each of which was preinoculated with 10 live nematodes, resulted in no survival at either 160 degrees F or 170 degrees F. Using ultraviolet light to detect both viable and nonviable nematodes in fillet sandwiches as an alternative method to pepsin digestion resulted in survival rates of 1% at 140 degrees F (60 degrees C), 3% at 145 degrees F (63 degrees C), and 0% at 150 degrees F (65 degrees C). Smaller fillet sandwiches, which most likely had fewer cold spots during microwave processing, required 150 degrees F (65 degrees C), whereas larger whole fillets required 170 degrees F (77 degrees C) to kill larvae of Anisakis simplex. The parasites were most likely inactivated by a thermal mechanism of microwave treatment. Damage to the nematodes was often evident from ruptured cuticles that were no longer resistant to digestive enzymes. The high hydrostatic pressure and low chloride content of the pseudocoelomic fluid probably contributed greatly to the damage incurred by the larvae.

Analysis of four toxic metals in a single rice seed by matrix solid phase dispersion -inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

He, Xiufen; Chen, Lixia; Chen, Xin; Yu, Huamei; Peng, Lixu; Han, Bingjun

2016-12-01

Toxic metals in rice pose great risks to human health. Metal bioaccumulation in rice grains is a criterion of breeding. Rice breeding requires a sensitive method to determine metal content in single rice grains to assist the variety selection. In the present study, four toxic metals of arsenic (As), cadmium (Cd), chromium (Cr) and lead (Pb) in a single rice grain were determined by a simple and rapid method. The developed method is based on matrix solid phase dispersion using multi-wall carbon nanotubes (MWCNTs) as dispersing agent and analyzed by inductively coupled plasma mass spectrometry. The experimental parameters were systematically investigated. The limits of detection (LOD) were 5.0, 0.6, 10 and 2.1 ng g-1 for As, Cd, Cr, and Pb, respectively, with relative standard deviations (n = 6) of <7.7%, demonstrating the good sensitivity and precision of the method. The results of 30 real world rice samples analyzed by this method agreed well with those obtained by the standard microwave digestion. The amount of sample required was reduced approximately 100 fold in comparison with the microwave digestion. The method has a high application potential for other sample matrices and elements with high sensitivity and sample throughput.

Analysis of four toxic metals in a single rice seed by matrix solid phase dispersion -inductively coupled plasma mass spectrometry.

PubMed

He, Xiufen; Chen, Lixia; Chen, Xin; Yu, Huamei; Peng, Lixu; Han, Bingjun

2016-12-06

Toxic metals in rice pose great risks to human health. Metal bioaccumulation in rice grains is a criterion of breeding. Rice breeding requires a sensitive method to determine metal content in single rice grains to assist the variety selection. In the present study, four toxic metals of arsenic (As), cadmium (Cd), chromium (Cr) and lead (Pb) in a single rice grain were determined by a simple and rapid method. The developed method is based on matrix solid phase dispersion using multi-wall carbon nanotubes (MWCNTs) as dispersing agent and analyzed by inductively coupled plasma mass spectrometry. The experimental parameters were systematically investigated. The limits of detection (LOD) were 5.0, 0.6, 10 and 2.1 ng g -1 for As, Cd, Cr, and Pb, respectively, with relative standard deviations (n = 6) of <7.7%, demonstrating the good sensitivity and precision of the method. The results of 30 real world rice samples analyzed by this method agreed well with those obtained by the standard microwave digestion. The amount of sample required was reduced approximately 100 fold in comparison with the microwave digestion. The method has a high application potential for other sample matrices and elements with high sensitivity and sample throughput.

Microwave-assisted Extraction of Rare Earth Elements from Petroleum Refining Catalysts and Ambient Fine Aerosols Prior to Inductively Coupled Plasma - Mass Spectrometry

NASA Technical Reports Server (NTRS)

Mittlefehldt, David W.; Kulkarni, Pranav; Chellam, Shankar

2006-01-01

In the absence of a certified reference material, a robust microwave-assisted acid digestion procedure followed by inductively coupled plasma - mass spectrometry (ICP-MS) was developed to quantify rare earth elements (REEs) in fluidized-bed catalytic cracking (FCC) catalysts and atmospheric fine particulate matter (PM2.5). High temperature (200 C), high pressure (200 psig), acid digestion (HNO3, HF, and H3BO3) with 20 minute dwell time effectively solubilized REEs from six fresh catalysts, a spent catalyst, and PM2.5. This method was also employed to measure 27 non-REEs including Na, Mg, Al, Si, K, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Zr, Mo, Cd, Cs, Ba, Pb, and U. Complete extraction of several REEs (Y, La, Ce, Pr, Nd, Tb, Dy, and Er) required HF indicating that they were closely associated with the aluminosilicate structure of the zeolite FCC catalysts. Internal standardization using 115In quantitatively corrected non-spectral interferences in the catalyst digestate matrix. Inter-laboratory comparison using ICP-optical emission spectroscopy (ICP-OES) and instrumental neutron activation analysis (INAA) demonstrated the applicability of the newly developed analytical method for accurate analysis of REEs in FCC catalysts. The method developed for FCC catalysts was also successfully implemented to measure trace to ultra-trace concentrations of La, Ce, Pr, Nd, Sm, Gd, Eu, and Dy in ambient PM2.5 in an industrial area of Houston, TX.

[Comparative study on five pretreatment methods for ICP-OES determination of mineral elements in Rosa rugosa].

PubMed

Zhao, Ning; Yang, Bin; Duan, Yu-Cen; Lei, Ran

2011-08-01

Abstract Five different pretreatment methods, including dry ashing and microwave digestion with four acid systems (HNO3 + H2O2, HNO3 + H2O2 + HF, HNO3 + HClO4 and HNO3 + HClO4 + HF), were employed for digestion of the samples of Rosa rugosa. Nine major and trace elements were determined using ICP-OES method. The addition standard recovery rates indicate that, with the system of HNO3 + HClO4, better results can be obtained for most of the determined elements. With this method, except for Fe, the recovery rates are in the range of 95.4%-104.6%. For Fe, higher recovery rate (99%) was obtained with HNO3 + H2O2 + HF system.

Microwave-assisted wet digestion with H2O2 at high temperature and pressure using single reaction chamber for elemental determination in milk powder by ICP-OES and ICP-MS.

PubMed

Muller, Edson I; Souza, Juliana P; Muller, Cristiano C; Muller, Aline L H; Mello, Paola A; Bizzi, Cezar A

2016-08-15

In this work a green digestion method which only used H2O2 as an oxidant and high temperature and pressure in the single reaction chamber system (SRC-UltraWave™) was applied for subsequent elemental determination by inductively coupled plasma-based techniques. Milk powder was chosen to demonstrate the feasibility and advantages of the proposed method. Samples masses up to 500mg were efficiently digested, and the determination of Ca, Fe, K, Mg and Na was performed by inductively coupled plasma optical emission spectrometry (ICP-OES), while trace elements (B, Ba, Cd, Cu, Mn, Mo, Pb, Sr and Zn) were determined by inductively coupled plasma mass spectrometry (ICP-MS). Residual carbon (RC) lower than 918mgL(-1) of C was obtained for digests which contributed to minimizing interferences in determination by ICP-OES and ICP-MS. Accuracy was evaluated using certified reference materials NIST 1549 (non-fat milk powder certified reference material) and NIST 8435 (whole milk powder reference material). The results obtained by the proposed method were in agreement with the certified reference values (t-test, 95% confidence level). In addition, no significant difference was observed between results obtained by the proposed method and conventional wet digestion using concentrated HNO3. As digestion was performed without using any kind of acid, the characteristics of final digests were in agreement with green chemistry principles when compared to digests obtained using conventional wet digestion method with concentrated HNO3. Additionally, H2O2 digests were more suitable for subsequent analysis by ICP-based techniques due to of water being the main product of organic matrix oxidation. The proposed method was suitable for quality control of major components and trace elements present in milk powder in consonance with green sample preparation. Copyright © 2016 Elsevier B.V. All rights reserved.

[Determination of trace metals in atmospheric dry deposition with a heavy matrix of PUF by inductively coupled plasma mass spectroscopy after microwave digestion].

PubMed

Pan, Yue-peng; Wang, Yue-si; Yang, Yong-jie; Wu, Dan; Xin, Jin-yuan; Fan, Wen-yan

2010-03-01

Interest in atmospheric dry deposition results mostly from concerns about the effects of the deposited trace elements entering waterbody, soil and vegetation as well as their subsequent health effects. A microwave assisted digestion method followed by inductively coupled plasma mass spectrometric (MAD-ICP/MS) analysis was developed to determine the concentrations of a large number of trace metals in atmospheric dry deposition samples with a heavy matrix of polyurethane foam (PUF). A combination of HNO3-H2O2-HF was used for digestion. The experimental protocol for the microwave assisted digestion was established using two different SRMs (GBW 07401, Soil and GBW 08401, Coal fly ash). Subsequently, blanks and limits of detection for total trace metal concentrations were determined for PUF filter which was used for dry deposition sampling. Finally, the optimized digestion method was applied to real world atmospheric dry deposition samples collected at 10 sites in Jingjinji area in winter from Dec. 2007 to Feb. 2008. The results showed that the area-averaged total mass fluxes ranged between 85 and 912 mg x (m2 x d)(-1), and fluxes of most elements were highest at Baoding and lowest at Xinglong. In addition, the elemental fluxes in urban areas of Beijing, Tianjin and Tangshan were measured to be higher than that in suburb and rural sites. The average fluxes of crust elements (A1, Fe, Mn, K, Na, Ca and Mg) were one to three orders of magnitude higher than anthropogenic elements (Cu, Pb, Cr, Ni, V, Zn and Ba), varying from 151 to 16034 microg x (m2 x d)(-1) versus 14 to 243 microg x (m2 x d)(-1). Zinc was the most abundant heavy metal and calcium the highest of the crust elements while the elements Mo, Co, Cd, As and Be deposited less or even could not be detected. The anthropogenic and crustal contributions were estimated by employing enrichment factors (EF) calculated relative to the average crustal composition. The EF values of all elements except Pb and Zn were below 10, suggesting that local soil and/or dust generally dominate in the dry deposition flux.

Inorganic elemental compositions of commercial multivitamin/mineral dietary supplements: application of collision/reaction cell inductively coupled-mass spectroscopy

USDA-ARS?s Scientific Manuscript database

Microwave digestion followed by analysis using ICP-MS has been shown to be a simple, fast reliable method for the multi-element determination in multivitamin/mineral dietary supplements (MVM). A study of 35 popular MVM dietary supplements revealed that composition and levels varied among products, a...

Determination of silica coating efficiency on metal particles using multiple digestion methods.

PubMed

Wang, Jun; Topham, Nathan; Wu, Chang-Yu

2011-10-15

Nano-sized metal particles, including both elemental and oxidized metals, have received significant interest due to their biotoxicity and presence in a wide range of industrial systems. A novel silica technology has been recently explored to minimize the biotoxicity of metal particles by encapsulating them with an amorphous silica shell. In this study, a method to determine silica coating efficiency on metal particles was developed. Metal particles with silica coating were generated using gas metal arc welding (GMAW) process with a silica precursor tetramethylsilane (TMS) added to the shielding gas. Microwave digestion and Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) were employed to solubilize the metal content in the particles and analyze the concentration, respectively. Three acid mixtures were tested to acquire the appropriate digestion method targeting at metals and silica coating. Metal recovery efficiencies of different digestion methods were compared through analysis of spiked samples. HNO(3)/HF mixture was found to be a more aggressive digestion method for metal particles with silica coating. Aqua regia was able to effectively dissolve metal particles not trapped in the silica shell. Silica coating efficiencies were thus calculated based on the measured concentrations following digestion by HNO(3)/HF mixture and aqua regia. The results showed 14-39% of welding fume particles were encapsulated in silica coating under various conditions. This newly developed method could also be used to examine the silica coverage on particles of silica shell/metal core structure in other nanotechnology areas. Copyright © 2011 Elsevier B.V. All rights reserved.

Evolution of efficient methods to sample lead sources, such as house dust and hand dust, in the homes of children

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

Que Hee, S.S.; Peace, B.; Clark, C.S.

Efficient sampling methods to recover lead-containing house dust and hand dust have been evolved so that sufficient lead is collected for analysis and to ensure that correlational analyses linking these two parameters to blood lead are not dependent on the efficiency of sampling. Precise collection of loose house dust from a 1-unit area (484 cmS) with a Tygon or stainless steel sampling tube connected to a portable sampling pump (1.2 to 2.5 liters/min) required repetitive sampling (three times). The Tygon tube sampling technique for loose house dust <177 m in diameter was around 72% efficient with respect to dust weightmore » and lead collection. A representative house dust contained 81% of its total weight in this fraction. A single handwipe for applied loose hand dust was not acceptably efficient or precise, and at least three wipes were necessary to achieve recoveries of >80% of the lead applied. House dusts of different particle sizes <246 m adhered equally well to hands. Analysis of lead-containing material usually required at least three digestions/decantations using hot plate or microwave techniques to allow at least 90% of the lead to be recovered. It was recommended that other investigators validate their handwiping, house dust sampling, and digestion techniques to facilitate comparison of results across studies. The final methodology for the Cincinnati longitudinal study was three sampling passes for surface dust using a stainless steel sampling tube; three microwave digestion/decantations for analysis of dust and paint; and three wipes with handwipes with one digestion/decantation for the analysis of six handwipes together.« less

Evaluation of digestion methods for analysis of trace metals in mammalian tissues and NIST 1577c.

PubMed

Binder, Grace A; Metcalf, Rainer; Atlas, Zachary; Daniel, Kenyon G

2018-02-15

Digestion techniques for ICP analysis have been poorly studied for biological samples. This report describes an optimized method for analysis of trace metals that can be used across a variety of sample types. Digestion methods were tested and optimized with the analysis of trace metals in cancerous as compared to normal tissue as the end goal. Anthropological, forensic, oncological and environmental research groups can employ this method reasonably cheaply and safely whilst still being able to compare between laboratories. We examined combined HNO 3 and H 2 O 2 digestion at 170 °C for human, porcine and bovine samples whether they are frozen, fresh or lyophilized powder. Little discrepancy is found between microwave digestion and PFA Teflon pressure vessels. The elements of interest (Cu, Zn, Fe and Ni) yielded consistently higher and more accurate values on standard reference material than samples heated to 75 °C or samples that utilized HNO 3 alone. Use of H 2 SO 4 does not improve homogeneity of the sample and lowers precision during ICP analysis. High temperature digestions (>165 °C) using a combination of HNO 3 and H 2 O 2 as outlined are proposed as a standard technique for all mammalian tissues, specifically, human tissues and yield greater than 300% higher values than samples digested at 75 °C regardless of the acid or acid combinations used. The proposed standardized technique is designed to accurately quantify potential discrepancies in metal loads between cancerous and healthy tissues and applies to numerous tissue studies requiring quick, effective and safe digestions. Copyright © 2017 Elsevier Inc. All rights reserved.

[Determination of trace elements in waste beer yeasts by ICP-MS with microwave digestion].

PubMed

Cheng, Xian-zhong; Jin, Can; Zhang, Kai-cheng

2008-10-01

The waste beer yeast has rich nutritional compositions and is widely used in food, medical and forage industries. The security of the yeast plays an important role in everyone's daily life. But the yeast contanining microamount of lead, cadmium, chromium, arsenic and other harmful metals is endangering human health. A new method was developed for the direct determination of eight elements, namely copper, lead, zinc, iron, manganese, cadmium, chromium and arsenic in waste beer yeast by inductively coupled plasma-mass spectrometry (ICP-MS) with microwave digestion. The parameters of plasma system, mass system, vacuum system and spectrometer system were optimized. The spectral interferences were eliminated by selecting alternation analytical isotopes of 65Cu, 208Pb, 66Zn, 57Fe, 55Mn, 114Cd, 52Cr and 5As, and the internal standards of Rh was selected to compensate the drift of analytical signals. The samples were digested with concentrated nitric acid-hydrogen peroxide (2:1) mixed solution more rapidly and more effectively. The effects of the type of mixed acid , the volume of digesting solution, heating time, and heating power were investigated in detail. In the closed system, the complete digestion was performed using 4 mL HNO3 and 2mL H2O2 for 2.0 min at 0.5 MPa, 3 min at 1.0 MPa and 5 min at 1.5 MPa. The detection limits of these eight elements were 0.013-0.122 microg x L(-1). The relative standard deviation (RSD) was 0.94%-3.26% (n=9), and the addition standard recovery was 98.4%-102.6% for all elements. The proposed method has been applied to the determination of trace elements of Cu, Pb, Zn, Fe, Mn, Cd, Cr and As in waste beer yeast samples with satisfactory results. The determination results indicated that the content of trace elements of Cu, Pb, Cd and As in waste beer yeast samples are significantly low.

237Np analytical method using 239Np tracers and application to a contaminated nuclear disposal facility

DOE PAGES

Snow, Mathew S.; Morrison, Samuel S.; Clark, Sue B.; ...

2017-03-21

In this study, environmental 237Np analyses are challenged by low 237Np concentrations and lack of an available yield tracer; we report a rapid, inexpensive 237Np analytical approach employing the short lived 239Np (t1/2 = 2.3 days) as a chemical yield tracer followed by 237Np quantification using inductively coupled plasma-mass spectrometry. 239Np tracer is obtained via separation from a 243Am stock solution and standardized using gamma spectrometry immediately prior to sample processing. Rapid digestions using a commercial, 900 W "Walmart" microwave and Parr microwave vessels result in 99.8 ± 0.1% digestion yields, while chromatographic separations enable Np/U separation factors on themore » order of 10 6 and total Np yields of 95 ± 4% (2σ). Application of this method to legacy soil samples surrounding a radioactive disposal facility (the Subsurface Disposal Area at Idaho National Laboratory) reveal the presence of low level 237Np contamination within 600 m of this site, with maximum 237Np concentrations on the order of 10 3 times greater than nuclear weapons testing fallout levels.« less

237 Np analytical method using 239 Np tracers and application to a contaminated nuclear disposal facility

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

Snow, Mathew S.; Morrison, Samuel S.; Clark, Sue B.

2017-06-01

Environmental 237Np analyses are challenged by low 237Np concentrations and lack of an available yield tracer; we report a rapid, inexpensive 237Np analytical approach employing the short lived 239Np (t1/2 = 2.3 days) as a chemical yield tracer followed by 237Np quantification using inductively coupled plasma-mass spectrometry. 239Np tracer is obtained via separation from a 243Am stock solution and standardized using gamma spectrometry immediately prior to sample processing. Rapid digestions using a commercial, 900 watt “Walmart” microwave and Parr microwave vessels result in 99.8 ± 0.1% digestion yields, while chromatographic separations enable Np/U separation factors on the order of 106more » and total Np yields of 95 ± 4% (2σ). Application of this method to legacy soil samples surrounding a radioactive disposal facility (the Subsurface Disposal Area at Idaho National Laboratory) reveal the presence of low level 237Np contamination within 600 meters of this site, with maximum 237Np concentrations on the order of 103 times greater than nuclear weapons testing fallout levels.« less

237Np analytical method using 239Np tracers and application to a contaminated nuclear disposal facility.

PubMed

Snow, Mathew S; Morrison, Samuel S; Clark, Sue B; Olson, John E; Watrous, Matthew G

2017-06-01

Environmental 237 Np analyses are challenged by low 237 Np concentrations and lack of an available yield tracer; we report a rapid, inexpensive 237 Np analytical approach employing the short lived 239 Np (t 1/2  = 2.3 days) as a chemical yield tracer followed by 237 Np quantification using inductively coupled plasma-mass spectrometry. 239 Np tracer is obtained via separation from a 243 Am stock solution and standardized using gamma spectrometry immediately prior to sample processing. Rapid digestions using a commercial, 900 W "Walmart" microwave and Parr microwave vessels result in 99.8 ± 0.1% digestion yields, while chromatographic separations enable Np/U separation factors on the order of 10 6 and total Np yields of 95 ± 4% (2σ). Application of this method to legacy soil samples surrounding a radioactive disposal facility (the Subsurface Disposal Area at Idaho National Laboratory) reveal the presence of low level 237 Np contamination within 600 m of this site, with maximum 237 Np concentrations on the order of 10 3 times greater than nuclear weapons testing fallout levels. Copyright © 2017 Elsevier Ltd. All rights reserved.

New type of dry substances content meter using microwaves for application in biogas plants.

PubMed

Nacke, Thomas; Brückner, Kathleen; Göller, Arndt; Kaufhold, Sebastian; Nakos, Xenia; Noack, Stephan; Stöber, Heinrich; Beckmann, Dieter

2005-11-01

Dry substances (DS) are an important index for monitoring and controlling anaerobic co-digestion in biogas plants. We have developed and tested an online meter that measures suspended solids by means of the reflection coefficient of an exiting microwave signal, which is dependent on the dielectric properties of the suspensions. Intelligent models based on partial least squares regression (PLSR) and artificial neural network (ANN) for calibration allow exact and reproducible measurements under different circumstances. This measuring method is appropriate for contactless and online measurements of dry substance contents in biogas plants in a large range from 2-14%.

Influence of Continuous Flow Microwave Pre-Treatment on Anaerobic Digestion of Secondary Thickened Sludge for Sustainable Energy Recovery in Sewage Treatment Plant

NASA Astrophysics Data System (ADS)

Hephzibah, D.; Kumaran, P.; Saifuddin, N. M.

2016-03-01

This work elucidates the effects of pre-treatment of secondary thickened sludge (STS) for enhancement of biogas production that has great potential to generate energy for the utilization of the sewage treatment plant (STP) itself. Microwave pre-treatment has been adopted for this study. Experiment works have been designed and conducted to examine the effectiveness of continuous flow microwave pre-treatment on the solubility of STS, digestibility of STS and biogas production at a power level of 80 W for 5, 10 and 15 minutes. A few characteristics of the sewage sludge were monitored daily to identify the effect of pre-treatment on the sludge. The soluble chemical oxygen demand (SCOD)/total chemical oxygen demand (TCOD) ratio increased by 0.1, 1.0 and 1.8%, while the volatile fatty acids (VFA) concentration of the pre-treated sludge improved by 4.4, 5.1, 5.9% at the irradiation time of 5, 10 and 15 minutes, respectively at a microwave power level of 80 W. Besides that, the digestate also indicates that the pre-treated sludge undergoes efficient VS removal and TCOD removal after anaerobic digestion compared to the untreated sludge. Moreover, the biogas quantity increased by an average of 19.2, 24.1 and 32.2% in 5, 10 and 15 minutes irradiation time respectively compared to the untreated sludge. The additional quantity of biogas generated has shown a great potential for sustainable energy generation that can be utilized internally by the STP.

[Determination of 24 minerals in human milk by inductively coupled plasma mass spectrometry with microwave digestion].

PubMed

Sun, Zhongqing; Yue, Bing; Yang, Zhenyu; Li, Xiaowei; Wu, Yongning; Yin, Shian

2013-05-01

To determine the levels of 24 minerals in human milk by inductively coupled plasma mass spectrometry with microwave digestion. The samples were digested by microwave. The contents of minerals were determined by inductively coupled plasma mass spectrometry. The standard reference minerals of 1849a and 1568a from National Institute of Science and Technology were used for quality control. The accuracy and reproduability for this method were evaluated with mix standards and 1849a and 1568a standard reference materials. The ranges of the levels of sodium, magnesium, phosphorus, potassium, calcium, aluminum, chromium, arsenic, selenium, iron, zinc, manganese, copper, molybdenum, vanadium, cobalt, nickel, gallium, cadmium, silver, strontium, cesium, barium, lead in human milk was 34.97-415.83 mg/kg, 19.00-39.52 mg/kg, 102.13-274.53 mg/kg, 351.19-713.99 mg/kg, 180.08-349.64 mg/kg, 0.06-0.44 mg/kg, 0.9-7.37 microg/kg, 0.92-2.72 microg/kg, 0.20-21.15 microg/kg, 0.10-0.70 mg/kg, 0.56-3.25 mg/kg, 3.00-16.12 micro.g/kg, 62.16-591.69 microg/kg, 0.02-6.91 microg/kg, 5.99-13.70 microg/kg, 0.07-2.11 microg/kg, 0.77-209.26 microg/kg, 0.005-0.28 microg/kg, 0.02-0.23 microg/kg, 0.02-0.71 microg/kg, 36.89-132.26 microg/kg, 0.01-4.72 microg/kg, 0.83-28.16 microg/kg, 2.5-5.3 microg/kg, respectively. The levels of minerals in human milk in present study were consisted with other similar studies. The experiment examined the levels of minerals in human milk satisfactorily. The method has high accuracy and good reproducibility, which could be used for understanding the levels of minerals in human milk.

Digestibility of (Poly)phenols and Antioxidant Activity in Raw and Cooked Cactus Cladodes ( Opuntia ficus-indica).

PubMed

De Santiago, Elsy; Pereira-Caro, Gema; Moreno-Rojas, José Manuel; Cid, Concepción; De Peña, María-Paz

2018-05-29

This study aims to investigate whether heat treatment applied to cactus cladodes influences the bioaccessibility of their (poly)phenolic compounds after simulated gastric and intestinal digestion. A total of 45 (poly)phenols were identified and quantified in raw and cooked cactus cladodes by ultra high performance liquid chromatography photodiode array detector high resolution mass spectrometry. Both flavonoids (60-68% total), mainly isorhamnetin derivatives, and phenolic acids (32-40%) with eucomic acids as the predominant ones significantly ( p < 0.05) increased with microwaving and griddling processes. After in vitro gastrointestinal digestion, 55-64% of the total (poly)phenols of cooked cactus cladodes remained bioaccessible versus 44% in raw samples. Furthermore, digestive conditions and enzymes degraded or retained more flavonoids (37-63% bioaccessibility) than phenolic acids (56-87% bioaccessibility). Microwaved cactus cladodes contributed the highest amount of (poy)phenols (143.54 mg/g dm) after gastrointestinal process, followed by griddled samples (133.98 mg/g dm), showing the highest antioxidant capacity. Additionally, gastrointestinal digestion induced isomerizations among the three stereoisomeric forms of piscidic and eucomic acids.

Polymorph-dependent titanium dioxide nanoparticle dissolution in acidic and alkali digestions

EPA Science Inventory

Multiple polymorphs (anatase, brookite and rutile) of titanium dioxide nanoparticles (TiO2-NPs) with variable structures were quantified in environmental matrices via microwave-based hydrofluoric (HF) and nitric (HNO3) mixed acid digestion and muffle furnace (MF)-based potassium ...

Profitable ultrasonic assisted microwave disintegration of sludge biomass: Modelling of biomethanation and energy parameter analysis.

PubMed

Kavitha, S; Rajesh Banu, J; Kumar, Gopalakrishnan; Kaliappan, S; Yeom, Ick Tae

2018-04-01

In this study, microwave irradiation has been employed to disintegrate the sludge biomass profitably by deagglomerating the sludge using a mechanical device, ultrasonicator. The outcomes of the study revealed that a specific energy input of 3.5 kJ/kg TS was found to be optimum for deagglomeration with limited cell lysis. A higher suspended solids (SS) reduction and biomass lysis efficiency of about 22.5% and 33.2% was achieved through ultrasonic assisted microwave disintegration (UMWD) when compared to microwave disintegration - MWD (15% and 20.9%). The results of biochemical methane potential (BMP) test were used to estimate biodegradability of samples. Among the samples subjected to BMP, UMWD showed better amenability towards anaerobic digestion with higher methane production potential of 0.3 L/g COD representing enhanced liquefaction potential of disaggregated sludge biomass. Economic analysis of the proposed method of sludge biomass pretreatment showed a net profit of 2.67 USD/Ton respectively. Copyright © 2018 Elsevier Ltd. All rights reserved.

Study on the Volatility of Cesium in Dry Ashing Pretreatment and Dissolution of Ash by Microwave Digestion System - 13331

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

Choi, Kwang-Soon; Lee, Chang Heon; Ahn, Hong-Joo

2013-07-01

Based on the regulation of the activity concentration of Cs-137, Co-58, Co-60, Fe-55, Ni-59, Ni-63, Sr-90, Nb-94, and Tc-99, and the total alpha from the radioactive waste acceptance criteria, the measurement of the activity concentration of these nuclides in low and intermediate levels of radioactive waste such as in paper, cotton, vinyl and plastic samples was investigated. A dry ashing method was applied to obtain a concentration effect of the samples. Owing to the temperature dependence of the volatility for cesium, the temperature of 300 to 650 deg. C was examined. It was found that 450 deg. C is themore » optimum dry ashing temperature. After dry ashing, the produced ash was dissolved with HNO{sub 3}, HCl, and HF by a high-performance microwave digestion system. The ash sample, for the most part, was completely dissolved with 10 mL of HNO{sub 3}, 4 mL of HCl, and 0.25 mL of HF by a high-performance microwave digestion system using a nova high temperature rotor at 250 deg. C for 90 min until reaching 0.2 g. To confirm the reliability of cesium loss after the performance of the dry ashing procedure, a cesium standard solution for AAS and a Cs-137 standard solution for gamma spectrometry were added to a paper towel or a planchet of stainless steel, respectively. Cesium was measured by AAS, ICP-MS, and gamma spectrometry. The volatility of cesium did not occur until 450 deg. C ashing. (authors)« less

Improvement of anaerobic digestion of sewage sludge through microwave pre-treatment.

PubMed

Serrano, A; Siles, J A; Martín, M A; Chica, A F; Estévez-Pastor, F S; Toro-Baptista, E

2016-07-15

Sewage sludge generated in the activated sludge process is a polluting waste that must be treated adequately to avoid important environmental impacts. Traditional management methods, such as landfill disposal or incineration, are being ruled out due to the high content in heavy metal, pathogens, micropolluting compounds of the sewage sludge and the lack of use of resources. Anaerobic digestion could be an interesting treatment, but must be improved since the biomethanisation of sewage sludge entails low biodegradability and low methane production. A microwave pre-treatment at pilot scale is proposed to increase the organic matter solubilisation of sewage sludge and enhance the biomethanisation yield. The operational variables of microwave pre-treatment (power and specific energy applied) were optimised by analysing the physicochemical characteristics of sewage sludge (both total and soluble fraction) under different pre-treatment conditions. According to the variation in the sCOD and TN concentration, the optimal operation variables of the pre-treatment were fixed at 20,000 J/g TS and 700 W. A subsequent anaerobic digestion test was carried out with raw and pre-treated sewage sludge under different conditions (20,000 J/g TS and 700 W; 20,000 J/g TS and 400 W; and 30,000 J/g TS and 400 W). Although stability was maintained throughout the process, the enhancement in the total methane yield was not high (up to 17%). Nevertheless, very promising improvements were determined for the kinetics of the process, where the rG and the OLR increased by 43% and 39%, respectively, after carrying out a pre-treatment at 20,000 J/g TS and 700 W. Copyright © 2016 Elsevier Ltd. All rights reserved.

Comparison of digestion methods for determination of trace and minor metals in plant samples.

PubMed

Lavilla, I; Filgueiras, A V; Bendicho, C

1999-12-01

In this paper, three dissolution methods using pressure digestion vessels (low-, medium-, and high-pressure vessels) for the determination of metals in plant samples are described. The Plackett-Burman saturated factorial design was used to identify the significant factors influencing wet ashing and to select optimized dissolution conditions. The three methods were statistically compared (on-way ANOVA) on the same sample; no significant differences were obtained. In all cases the relative standard deviation values were <3%. The digestion method based on the use of low-pressure vessels and a microwave oven was validated against CRM GBW07605 tea leaves. This method was applied to the determination of Cu, Zn, Mn, Fe, Mg, and Ca in 22 different medicinal, aromatic, and seasoning plants by flame-atomic absorption spectrometry. The concentration intervals of metal in the plants analyzed were the following: Cu, 4 (Allium sativum)-35 (Thea sinensis) microg g(-1); Zn, 7 (Piper nigrum)-90 (Betula alba) microg g(-1); Mn, 9 (Allium sativum)-939 (Caryophylus aromaticus) microg g(-1); Fe, 33 (Allium sativum)-2486 (Anethum graveolens) microg g(-1); Mg, 495 (Allium sativum)-7458 (Ocimum basilicum) microg g(-1); Ca, 386 (Allium sativum)-21500 (Ocimum basilicum) microg g(-1).

Epitope enhancement for immunohistochemical demonstration of tartrate-resistant acid phosphatase.

PubMed

Janckila, A J; Lear, S C; Martin, A W; Yam, L T

1996-03-01

We have developed a monoclonal antibody (9C5) for immunohistochemical localization of tartrate-resistant acid phosphatase (TRAcP). This antibody reacts with a denatured epitope of TRAcP and requires enhancement methods to promote antigenicity in paraffin-embedded tissues. We used this antibody to systematically examine proteolytic digestion and heat denaturation conditions for epitope enhancement in both paraffin sections and fixed smears. The goal was to increase the sensitivity of the immunohistochemical stain for TRAcP. Optimal conditions for proteolytic digestion were established. Denaturation in a conventional boiling water bath was compared to microwave irradiation in several commonly used solutions. Immunohistochemistry was compared directly to TRAcP cytochemistry in fixed smears from hairy cell leukemia specimens to gauge the level of sensitivity of our improved method. Attempts were made to "retrieve" the 9C5 epitope from overfixed tissues and aged smears. Maximal immunoreactivity of TRAcP was achieved by microwave irradiation in a citrate or Tris buffer of pH 6.0-8.0 without the need for a subsequent protease digestion step. With this method of epitope enhancement, immunohistochemistry with antibody 9C5 was as sensitive as direct cytochemical staining of TRAcP activity. However, once a tissue specimen had been overfixed or a smear stored for a year or more, the 9C5 epitope was no longer retrievable. The key element in epitope enhancement for 9C5 immunohistochemistry is heat denaturation of the target epitope. Immunohistochemistry of TRAcP in paraffin sections would be a great asset to the study of specialized forms of the monocyte/macrophage lineage and to the process of macrophage activation. It would also provide another means for more precise evaluation of residual disease in bone marrow of patients treated for hairy cell leukemia.

Determination of minor and trace elements in aromatic spices by micro-wave assisted digestion and inductively coupled plasma-mass spectrometry.

PubMed

Khan, Naeem; Choi, Ji Yeon; Nho, Eun Yeong; Jamila, Nargis; Habte, Girum; Hong, Joon Ho; Hwang, In Min; Kim, Kyong Su

2014-09-01

This study aimed at analyzing the concentrations of 23 minor and trace elements in aromatic spices by inductively coupled plasma-mass spectrometry (ICP-MS), after wet digestion by microwave system. The analytical method was validated by linearity, detection limits, precision, accuracy and recovery experiments, obtaining satisfactory values in all cases. Results indicated the presence of variable amounts of both minor and trace elements in the selected aromatic spices. Manganese was high in cinnamon (879.8 μg/g) followed by cardamom (758.1 μg/g) and clove (649.9 μg/g), strontium and zinc were high in ajwain (489.9 μg/g and 84.95 μg/g, respectively), while copper was high in mango powder (77.68 μg/g). On the whole some of the minor and essential trace elements were found to have good nutritional contribution in accordance to RDA. The levels of toxic trace elements, including As, Cd, and Pb were very low and did not found to pose any threat to consumers. Copyright © 2014 Elsevier Ltd. All rights reserved.

Biochemical methane potential tests of different autoclaved and microwaved lignocellulosic organic fractions of municipal solid waste.

PubMed

Pecorini, Isabella; Baldi, Francesco; Carnevale, Ennio Antonio; Corti, Andrea

2016-10-01

The aim of this research was to enhance the anaerobic biodegradability and methane production of two synthetic Organic Fractions of Municipal Solid Waste with different lignocellulosic contents by assessing microwave and autoclave pre-treatments. Biochemical Methane Potential assays were performed for 21days. Changes in the soluble fractions of the organic matter (measured by soluble chemical oxygen demand, carbohydrates and proteins), the first order hydrolysis constant kh and the cumulated methane production at 21days were used to evaluate the efficiency of microwaving and autoclaving pretreatments on substrates solubilization and anaerobic digestion. Microwave treatment led to a methane production increase of 8.5% for both the tested organic fractions while autoclave treatment had an increase ranging from 1.0% to 4.4%. Results showed an increase of the soluble fraction after pre-treatments for both the synthetic organic fractions. Soluble chemical oxygen demand observed significant increases for pretreated substrates (up to 219.8%). In this regard, the mediocre results of methane's production led to the conclusion that autoclaving and microwaving resulted in the hydrolysis of a significant fraction of non-biodegradable organic substances recalcitrant to anaerobic digestion. Copyright © 2016 Elsevier Ltd. All rights reserved.

Solid State Technology Branch of NASA Lewis Research Center: Fifth Annual Digest

NASA Technical Reports Server (NTRS)

1993-01-01

The digest is a collection of papers written by the members of the Solid State Technology Branch of NASA Lewis Research Center from June 1992-June 1993. The papers cover a range of topics relating to superconductivity, monolithic microwave integrated circuits (MMIC's), coplanar waveguide, and material characterization.

Lead and cadmium in human placentas and maternal and neonatal blood (in a heavily polluted area) measured by graphite furnace atomic absorption spectrometry.

PubMed Central

Baranowska, I

1995-01-01

OBJECTIVE--To measure the concentrations of the trace elements lead and cadmium in human placenta and in maternal and neonatal (cord) blood. To assess the influence of the strongly polluted environment on the content of metals in tissues and on the permeability of placenta to cadmium and lead. Various methods of mineralisation were tested before analysis. METHODS--Graphite furnace atomic absorption spectrometry was used for the determination of lead and cadmium. The samples for analysis were prepared by mineralisation under pressure in a Teflon bomb (HNO3, 110 degrees C), by wet ashing under normal pressure (HNO3 + H2O2 for 12 hours), and by microwave digestion in concentrated nitric acid. RESULTS--In analysed samples the following mean concentrations of cadmium and lead were found: in venous blood Pb = 72.50 ng/ml, Cd = 4.90 ng/ml; in placenta Pb = 0.50 microgram/g, Cd = 0.11 microgram/g; in cord blood Pb = 38.31 ng/ml, Cd = 1.13 ng/ml. CONCLUSION--High concentrations of lead and cadmium were found in placentas and in maternal blood whereas in neonatal blood there was an increased concentration of lead and only traces of cadmium. It is concluded that the placenta is a better barrier for cadmium than for lead. Among the examined methods of mineralisation, microwave digestion was the best. PMID:7795737

[Determination of trace heavy metal elements in cortex Phellodendron chinense by ICP-MS after microwave-assisted digestion].

PubMed

Kou, Xing-Ming; Xu, Min; Gu, Yong-Zuo

2007-06-01

An inductively coupled plasma mass spectrometry (ICP-MS) for determination of the contents of 8 trace heavy metal elements in cortex Phellodendron chinense after microwave-assisted digestion of the sample has been developed. The accuracy of the method was evaluated by the analysis of corresponding trace heavy metal elements in standard reference materials (GBW 07604 and GBW 07605). By applying the proposed method, the contents of 8 trace heavy metal elements in cortex Phellodendron chinense cultivated in different areas (in Bazhong, Yibin and Yingjing, respectively) of Sichuan and different growth period (6, 8 and 10 years of samples from Yingjing) were determined. The relative standard deviation (RSD) is in the range of 3.2%-17.8% and the recoveries of standard addition are in the range of 70%-120%. The results of the study indicate that the proposed method has the advantages of simplicity, speediness and sensitivity. It is suitable for the determination of the contents of 8 trace heavy metal elements in cortex Phellodendron chinense. The results also show that the concentrations of 4 harmful trace heavy metal elements As, Cd, Hg and Pb in cortex Phellodendron chinense are all lower than the limits of Chinese Pharmacopoeia and Green Trade Standard for Importing and Exporting Medicinal Plant and Preparation. Therefore, the cortex Phellodendron chinense is fit for use as medicine and export.

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

Not Available

This volume contains the interim change notice for sample preparation methods. Covered are: acid digestion for metals analysis, fusion of Hanford tank waste solids, water leach of sludges/soils/other solids, extraction procedure toxicity (simulate leach in landfill), sample preparation for gamma spectroscopy, acid digestion for radiochemical analysis, leach preparation of solids for free cyanide analysis, aqueous leach of solids for anion analysis, microwave digestion of glasses and slurries for ICP/MS, toxicity characteristic leaching extraction for inorganics, leach/dissolution of activated metal for radiochemical analysis, extraction of single-shell tank (SST) samples for semi-VOC analysis, preparation and cleanup of hydrocarbon- containing samples for VOCmore » and semi-VOC analysis, receiving of waste tank samples in onsite transfer cask, receipt and inspection of SST samples, receipt and extrusion of core samples at 325A shielded facility, cleaning and shipping of waste tank samplers, homogenization of solutions/slurries/sludges, and test sample preparation for bioassay quality control program.« less

Effects of microwave and alkali induced pretreatment on sludge solubilization and subsequent aerobic digestion.

PubMed

Chang, Chia-Jung; Tyagi, Vinay Kumar; Lo, Shang-Lien

2011-09-01

Individual and combined effects of microwave (MW) and alkali pretreatments on sludge disintegration and subsequent aerobic digestion of waste activated sludge (WAS) were studied. Pretreatments with MW (600W-85°C-2 min), conventional heating (520 W-80°C-12 min) and alkali (1.5 g NaOH/L - pH 12-30 min) achieved 8.5%, 7% and 18% COD solubilization, respectively. However, combined MW-alkali pretreatment synergistically enhanced sludge solubilization and achieved 46% COD solubilization, 20% greater than the additive value of MW alone and alkali alone (8.5+18%=26.5%). Moreover, the results of the batch aerobic digestion study on MW-alkali pretreated sludge showed 93% and 63% reductions in SCOD and VSS concentrations, respectively, at 16 days of SRT. The VSS reduction was 20% higher than that of WAS without pretreatment. Copyright © 2011 Elsevier Ltd. All rights reserved.

Bioaccessibility of cadmium in fresh and cooked Agaricus blazei Murill assessed by in vitro biomimetic digestion system.

PubMed

Sun, Liping; Liu, Gaoxiang; Yang, Meizhizi; Zhuang, Yongliang

2012-05-01

Bioaccessibility of cadmium (Cd) in fresh and cooked Agaricus blazei Murill (AbM) was studied by an in vitro biomimetic digestion system in this paper. The results showed that the Cd content in fresh AbM was 10.27 mg kg(-1) DM. The cooking treatments of boiling and microwaving with water significantly decreased Cd contents in fresh AbM by 36.4% and 30.2% (P<0.05), respectively. Cd in fresh AbM showed the highest bioaccessibility of 77.8% during the biomimetic digestion in stomach, followed by that of 69.4% from the gastrointestinal digestion. Cooking treatments also significantly lowered the bioaccessibility of Cd (P<0.05). Cd in boiled AbM showed 50.7% and 46.1% bioaccessibility during the gastric and gastrointestinal procedures. While, Cd in microwaved AbM showed 58.2% and 50.4% bioaccessibility. This study confirmed that the health risk assessment of AbM depending on the total Cd levels in fresh AbM was inaccurate, especially for the products domestically cooked. Copyright © 2012 Elsevier Ltd. All rights reserved.

Determination of cobalt species in nutritional supplements using ICP-OES after microwave-assisted extraction and solid-phase extraction.

PubMed

Bartosiak, Magdalena; Jankowski, Krzysztof; Giersz, Jacek

2018-06-05

Cobalt content (as vitamin B 12 and inorganic cobalt) in two nutritional supplements, namely Spirulina platensis and Saccharomyces cerevisiae known as a "superfood", has been determined using inductively coupled plasma optical emission spectrometry (ICP-OES). Several sample pre-treatment protocols have been applied and compared. Microwave-assisted acid digestion efficiently decomposed all cobalt-containing compounds, thus allowed obtaining total cobalt content in supplements examined. Vitamin B 12 was extracted from the samples with acetate buffer and potassium cyanide solution exposed to mild microwave radiation for 30 min, and cyanocobalamin was separated from the extract by on-column solid phase extraction using C-18 modified silica bed. About 100% of cobalt species was extracted using the triple microwave-assisted extraction procedure. Total cobalt content was 20-fold greater in Spirulina tablets than the declared cobalamin content (as Co). The ICP-OES method precision was about 3% and detection limit was 1.9 and 2.7 ng Co mL -1 for inorganic cobalt or cyanocobalamin, respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

[Performance comparison of material tests for cadmium and lead in food contact plastics].

PubMed

Mutsuga, Motoh; Abe, Tomoyuki; Abe, Yutaka; Ishii, Rie; Itoh, Yuko; Ohno, Hiroyuki; Ohno, Yuichiro; Ozaki, Asako; Kakihara, Yoshiteru; Kaneko, Reiko; Kawamura, Yoko; Shibata, Hiroshi; Sekido, Haruko; Sonobe, Hironori; Takasaka, Noriko; Tajima, Yoshiyasu; Tanaka, Aoi; Nomura, Chie; Hikida, Akinori; Matsuyama, Sigetomo; Murakami, Ryo; Yamaguchi, Miku; Wada, Takenari; Watanabe, Kazunari; Akiyama, Hiroshi

2014-01-01

Based on the Japanese Food Sanitation Law, the performances of official and alternative material test methods for cadmium (Cd) and lead (Pb) in food contact plastics were compared. Nineteen laboratories participated to an interlaboratory study, and quantified Cd and Pb in three PVC pellets. in the official method, a sample is digested with H2SO4, taken up in HCl, and evaporated to dryness on a water bath, then measured by atomic absorption spectrometry (AAS) or inductively coupled plasma-optical emission spectrometry (ICP-OES). Statistical treatment revealed that the trueness, repeatability (RSDr) and reproducibility (RSDr) were 86-95%, 3.1-9.4% and 8.6-22.1%, respectively. The values of the performance parameters fulfilled the requirements , and the performances met the test specifications. The combination of evaporation to dryness on a hot plate and measurement by AAS or ICP-OES is applicable as an alternative method. However, the trueness and RSDr were inferior to those of the official method. The performance parameters obtained by using the microwave digestion method (MW method) to prepare test solution were better than those of the official method. Thus, the MW method is available as an alternative method. Induced coupled plasma-mass spectrometry (ICP-MS) is also available as an alternative method. However, it is necessary to ensure complete digestion of the sample.

Accurate determination of bromine and iodine in medicinal plants by inductively coupled plasma-mass spectrometry after microwave-induced combustion

NASA Astrophysics Data System (ADS)

Nascimento, Mariele S.; Mendes, Ana Luiza G.; Henn, Alessandra S.; Picoloto, Rochele S.; Mello, Paola A.; Flores, Erico M. M.

2017-12-01

In this work, a method for the determination of bromine and iodine in medicinal plants by inductively coupled plasma mass spectrometry (ICP-MS) after digestion by microwave-induced combustion (MIC) was developed. Medicinal plants were pressed as pellets and combusted at 20 bar of oxygen. The suitability of absorbing solution (water, 50 mmol L- 1 (NH4)2CO3, 10 mmol L- 1, 25 mmol L- 1, 50 mmol L- 1 or 100 mmol L- 1 NH4OH) was evaluated and a reflux step of 5 min was applied after combustion. The accuracy of the proposed method was evaluated by using certified reference materials (CRMs) of apple leaves and peach leaves and also by spiked samples. Using 50 mmol L- 1 NH4OH as absorbing solution, recoveries close to 100% for bromine and iodine were obtained as well as a low relative standard deviation (5%). No statistical difference (t-test, 95% of confidence level) was observed between the values obtained by ICP-MS after MIC digestion and the certified values. One of the important advantages of the proposed method is that it allowed the use of a relatively high sample mass (1000 mg) of medicinal plant resulting in low limits of quantification (0.033 μg g- 1 and 0.003 μg g- 1 for Br and I, respectively). Blanks were always negligible and only diluted solutions were used, in agreement with current recommendations for analytical methods. A high digestion efficiency was achieved (> 99%) assuring quantitative results. The concentration of analytes in medicinal plants was in the range of 0.17 μg g- 1 to 53.1 μg g- 1 for Br and < 0.003 μg g- 1 to 1.27 μg g- 1 for I. Despite the relatively high Br concentration, it was lower than the maximum limit allowed by the United States Pharmacopeia for medicinal plants (125 μg g- 1).

Analysis of coke beverages by total-reflection X-ray fluorescence

NASA Astrophysics Data System (ADS)

Fernández-Ruiz, Ramón; von Bohlen, Alex; Friedrich K, E. Josue; Redrejo, M. J.

2018-07-01

The influence of the organic content, sample preparation process and the morphology of the depositions of two types of Coke beverage, traditional and light Coke, have been investigated by mean of Total-reflection X-ray Fluorescence (TXRF) spectrometry. Strong distortions of the nominal concentration values, up to 128% for P, have been detected in the analysis of traditional Coke by different preparation methods. These differences have been correlated with the edge X-ray energies of the elements analyzed being more pronounced for the lighter elements. The influence of the organic content (mainly sugar) was evaluated comparing traditional and light Coke analytical TXRF results. Three sample preparation methods have been evaluated as follows: direct TXRF analysis of the sample only adding internal standard, TXRF analysis after open vessel acid digestion and TXRF analysis after high pressure and temperature microwave-assisted acid digestion. Strong correlations were detected between quantitative results, methods of preparation and energies of the X-ray absorption edges of quantified elements. In this way, a decay behavior for the concentration differences between preparation methods and the energies of the X-ray absorption edges of each element were observed. The observed behaviors were modeled with exponential decay functions obtaining R2 correlation coefficients from 0.989 to 0.992. The strong absorption effect observed, and even possible matrix effect, can be explained by the inherent high organic content of the evaluated samples and also by the morphology and average thickness of the TXRF depositions observed. As main conclusion of this work, the analysis of light elements in samples with high organic content by TXRF, i.e. medical, biological, food or any other organic matrixes should be taken carefully. In any case, the direct analysis is not recommended and a previous microwave-assisted acid digestion, or similar, is mandatory, for the correct elemental quantification by TXRF.

The As removal from arsenopyrite-bearing mine waste by microwave

NASA Astrophysics Data System (ADS)

Kim, Hyun Soo; Myung, Eun Ji; Hack Lim, Dae; Kim, Bong Ju; Park, Cheon Young

2016-04-01

Penalties incurred by miners for arsenic in concentrates have increased significantly because the removal and disposal of arsenic is difficult and costly for smelters and because the environmental challenges are increasing worldwide. Typically miners incur penalties on arsenic in concentrates above 0.2% As with smelter rejection limits of 0.5%. Therefore, finding an effective solution for removing As during primary mining activities is necessary to avoid penalty. The aim of this study was to investigate the As removal from mine waste using microwave process. The mine waste samples were characterized by chemical and XRD analysis. To determine of As removal from the microwave experiments, aqua regia digestion was performed according to Korean environmental standard method(KESM) and the As removal effect were evaluated using the standard EPA toxicity characteristic leaching procedure(TCLP, EPA 1311 method). The result of mineralogical character for mine waste using XRD was detected arsenopyrite, pyrite, chalcopyrite, pyrrhotite and quartz. The chemical analysis of As, Pb, Zn contents in the mine waste measured 13,896.0, 896.1 and 1,054.6 mg/kg, respectively. The As removal of experiments was conducted to examine the effects of microwave exposure time(1~15min). The results showed that the As removal in mine waste (exposure time = 10min) was 92.90%, and the temperature of mine waste by microwave heating was 886℃. The TCLP leaching of treated mine waste by microwave measured values were below the EPA's current regulatory threshold(As, Pb, Zn : 5 mg/L). The optimum condition of microwave exposure for As removal from arsenopyrite-bearing mine waste was obtained at 800W, 2450MHz, 10min. Acknowledgment : This work was supported by the Energy and Resources Engineering Program Grant funded by the Ministry of Trade, Industry and Energy, Korea

Total iodine quantification in fluids and tissues from iodine- or iodide-supplemented rats by ion chromatography following microwave-assisted digestion.

PubMed

Delgado, Guadalupe; Muñoz-Torres, Carolina; Orozco-Esquivel, Teresa; Anguiano, Brenda; Aceves, Carmen

2015-03-01

Iodine is a crucial component of thyroid hormones, and several reports have shown that iodine per se is implicated in the physiopathology of other organs. Innovative ion chromatography detection following a four-step temperature ramp microwave digestion in 25-50 mM nitric acid was developed to measure total iodine in biological fluids and tissue samples from female Sprague-Dawley rats supplemented with 0.05% molecular iodine (I2) or 0.05% potassium iodide (I(-)) in drinking water. The reported method allows the measurement of total iodine with a limit of quantification of 13.7 μg L(-1), recoveries of 96.3-100.3%, and intra- and inter-assay variations, of 3.5% and 7.4% respectively. Analysis of biological fluids showed that after 48 hours, iodine-supplemented animals exhibited significantly higher levels of total iodine in both serum and urine compared with those supplemented with iodide. The half-life of iodine in serum and urine measured over the first 48 h showed similar patterns for both the I2 (7.89 and 7.76 hours) and I(-) (8.27 and 8.90 hours) supplements. Differential uptake patterns were observed in tissues after 6 days of supplements, with I(-) preferentially retained by thyroid, lactating mammary gland, and milk, and a slightly but significantly higher capture of I2 in pituitary, ovary, and virgin mammary gland. We developed a rapid, selective, and accurate digestion method to process fluid and tissue samples that permits reproducible measurements of total iodine by ion chromatography; iodine or iodide supplement show a similar serum and urine half-life, but organ-specific uptake depends on the chemical form of the iodine supplement.

Development of a highly precise ID-ICP-SFMS method for analysis of low concentrations of lead in rice flour reference materials.

PubMed

Zhu, Yanbei; Inagaki, Kazumi; Yarita, Takashi; Chiba, Koichi

2008-07-01

Microwave digestion and isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-SFMS) has been applied to the determination of Pb in rice flour. In order to achieve highly precise determination of low concentrations of Pb, the digestion blank for Pb was reduced to 0.21 ng g(-1) after optimization of the digestion conditions, in which 20 mL analysis solution was obtained after digestion of 0.5 g rice flour. The observed value of Pb in a non-fat milk powder certified reference material (CRM), NIST SRM 1549, was 16.8 +/- 0.8 ng g(-1) (mean +/- expanded uncertainty, k = 2; n = 5), which agreed with the certified value of 19 +/- 3 ng g(-1) and indicated the effectiveness of the method. Analytical results for Pb in three brown rice flour CRMs, NIST SRM 1568a, NIES CRM 10-a, and NIES CRM 10-b, were 7.32 +/- 0.24 ng g(-1) (n = 5), 1010 +/- 10 ng g(-1) (n = 5), and 1250 +/- 20 ng g(-1) (n = 5), respectively. The concentration of Pb in a candidate white rice flour reference material (RM) sample prepared by the National Metrology Institute of Japan (NMIJ) was observed to be 4.36 +/- 0.28 ng g(-1) (n = 10 bottles).

Rapid preparation of functional polysaccharides from Pyropia yezoensis by microwave-assistant rapid enzyme digest system.

PubMed

Lee, Ji-Hyeok; Kim, Hyung-Ho; Ko, Ju-Young; Jang, Jun-Ho; Kim, Gwang-Hoon; Lee, Jung-Suck; Nah, Jae-Woon; Jeon, You-Jin

2016-11-20

This study describes a simple preparation of functional polysaccharides from Pyropia yezoensis using a microwave-assistant rapid enzyme digest system (MAREDS) with various carbohydrases, and evaluates their antioxidative effects. Polysaccharide hydrolysates were prepared using MAREDS under different hydrolytic conditions of the carbohydrases and microwave powers. Polysaccharides less than 10kDa (Low molecular weight polysaccharides, LMWP, ≤10kDa) were efficiently obtained using an ultrafiltration (molecular weight cut-off of 10kDa). MAREDS increases AMG activation via an increased degree of hydrolysis; the best AMG hydrolysate was prepared using a 10:1 ratio of substrate to enzyme for 2h in MAREDS with 400W. LMWP consisted of galactose (27.3%), glucose (64.5%), and mannose (8.3%) from the AMG hydrolysate had stronger antioxidant effects than the high molecular weight polysaccharides (>10kDa). We rapidly prepared functional LMWPs by using MAREDS with carbohydrases, and suggest that LMWP might be potentially a valuable algal polysaccharide antioxidant. Copyright © 2016 Elsevier Ltd. All rights reserved.

The aluminium content of breast tissue taken from women with breast cancer.

PubMed

House, Emily; Polwart, Anthony; Darbre, Philippa; Barr, Lester; Metaxas, George; Exley, Christopher

2013-10-01

The aetiology of breast cancer is multifactorial. While there are known genetic predispositions to the disease it is probable that environmental factors are also involved. Recent research has demonstrated a regionally specific distribution of aluminium in breast tissue mastectomies while other work has suggested mechanisms whereby breast tissue aluminium might contribute towards the aetiology of breast cancer. We have looked to develop microwave digestion combined with a new form of graphite furnace atomic absorption spectrometry as a precise, accurate and reproducible method for the measurement of aluminium in breast tissue biopsies. We have used this method to test the thesis that there is a regional distribution of aluminium across the breast in women with breast cancer. Microwave digestion of whole breast tissue samples resulted in clear homogenous digests perfectly suitable for the determination of aluminium by graphite furnace atomic absorption spectrometry. The instrument detection limit for the method was 0.48 μg/L. Method blanks were used to estimate background levels of contamination of 14.80 μg/L. The mean concentration of aluminium across all tissues was 0.39 μg Al/g tissue dry wt. There were no statistically significant regionally specific differences in the content of aluminium. We have developed a robust method for the precise and accurate measurement of aluminium in human breast tissue. There are very few such data currently available in the scientific literature and they will add substantially to our understanding of any putative role of aluminium in breast cancer. While we did not observe any statistically significant differences in aluminium content across the breast it has to be emphasised that herein we measured whole breast tissue and not defatted tissue where such a distribution was previously noted. We are very confident that the method developed herein could now be used to provide accurate and reproducible data on the aluminium content in defatted tissue and oil from such tissues and thereby contribute towards our knowledge on aluminium and any role in breast cancer. Copyright © 2013 Elsevier GmbH. All rights reserved.

Solid State Technology Branch of NASA Lewis Research Center: Fifth Annual Digest

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

Not Available

1993-08-01

The digest is a collection of papers written by the members of the Solid State Technology Branch of NASA Lewis Research Center from June 1992-June 1993. The papers cover a range of topics relating to superconductivity, monolithic microwave integrated circuits (MMIC`s), coplanar waveguide, and material characterization. Individual papers are abstracted separately on the data base.

1988 IEEE Aerospace Applications Conference, Park City, UT, Feb. 7-12, 1988, Digest

NASA Astrophysics Data System (ADS)

The conference presents papers on microwave applications, data and signal processing applications, related aerospace applications, and advanced microelectronic products for the aerospace industry. Topics include a high-performance antenna measurement system, microwave power beaming from earth to space, the digital enhancement of microwave component performance, and a GaAs vector processor based on parallel RISC microprocessors. Consideration is also given to unique techniques for reliable SBNR architectures, a linear analysis subsystem for CSSL-IV, and a structured singular value approach to missile autopilot analysis.

Highly Efficient Proteolysis Accelerated by Electromagnetic Waves for Peptide Mapping

PubMed Central

Chen, Qiwen; Liu, Ting; Chen, Gang

2011-01-01

Proteomics will contribute greatly to the understanding of gene functions in the post-genomic era. In proteome research, protein digestion is a key procedure prior to mass spectrometry identification. During the past decade, a variety of electromagnetic waves have been employed to accelerate proteolysis. This review focuses on the recent advances and the key strategies of these novel proteolysis approaches for digesting and identifying proteins. The subjects covered include microwave-accelerated protein digestion, infrared-assisted proteolysis, ultraviolet-enhanced protein digestion, laser-assisted proteolysis, and future prospects. It is expected that these novel proteolysis strategies accelerated by various electromagnetic waves will become powerful tools in proteome research and will find wide applications in high throughput protein digestion and identification. PMID:22379392

Multielemental analysis in small amounts of environmental reference materials with inductively coupled plasma mass spectrometry.

PubMed

Dombovári, J; Becker, J S; Dietze, H J

2000-07-01

The lowest possible sample weight for performing multielemental trace element analysis on environmental and biological samples by ICP-MS has been investigated. The certified reference materials Bovine Liver NIST SRM 1577b, Human Hair NCS DC 73347 and Oriental Tobacco Leaves CTA-OTL-1 were applied at sample weights (1, 5, 20 and 50 mg aliquots, n = 10) which were significantly lower than those recommended with most recoveries in the range of 95-110%. Samples were digested in a mixture of nitric acid, hydrogen peroxide and hydrogen fluoride by closed-vessel microwave digestion. Multielemental analysis was performed with an optimized ICP-QMS method. Aqueous standard solutions were applied for external calibration with rhodium as the internal standard element. The detection limits varied between 0.02-0.38 microg/g for Li, Na, Cr, Mn, Ni, Cu, Zn, Sr, Cd, Ba and Pb, and up to 1.92 microg/g for Mg, Al, Ca, Fe and Ni. Digested human plasma samples were spiked with multielemental solution (0.5-10 microg/L) to test the analytical method and the recoveries were 95-105% for most analytes. Our results show that in the case of homogeneous SRMs it is possible to use them in very low amounts (1-5 mg) for method development and quality control.

Investigation of Trace Element Content in the Seeds, Pulp, and Peel of Mashui Oranges Using Microwave Digestion and ICP-MS Analysis.

PubMed

Chen, Lingyun; Shen, Mei; Ma, Ande; Han, Weili

2018-03-01

Fresh Mashui orange samples were pretreated with microwave digestion using an HNO 3 -H 2 O 2 system. The levels of Mg, K, Ca, Fe, Mn, Cu, Zn, As, Cd, and Pb in the seeds, pulp, and peel were then determined using inductively coupled plasma mass spectrometry (ICP-MS) combined with collision cell technology (CCT) and kinetic energy discrimination (KED). The standard curve coefficient of determinations of the ten tested elements were between 0.9995 and 0.9999. The instrument detection limit was between 0.112 ng/L and 3.05 ng/mL. The method detection limit was between 0.0281 and 763 ng/g. The average recovery rate was between 85.0 and 117%. The current results showed that Mashui oranges are rich in three elements, namely Mg, K, and Ca. The concentrations of K and Ca were significantly higher than that of Mg in the peel. The content of K was the highest in the seeds. Fe, Mn, Cu, and Zn had the second highest concentrations, and Fe was the highest in the seeds, while Cu was the lowest in the peel. As, Cd, and Pb (hazardous elements) had the lowest concentrations of all the tested elements.

Microwave assisted alkaline pretreatment to enhance enzymatic saccharification of catalpa sawdust.

PubMed

Jin, Shuguang; Zhang, Guangming; Zhang, Panyue; Li, Fan; Wang, Siqi; Fan, Shiyang; Zhou, Shuqiong

2016-12-01

Catalpa sawdust, a promising biofuel production biomass, was pretreated by microwave-water, -NaOH, and -Ca(OH) 2 to enhance enzymatic digestibility. After 48h enzymatic hydrolysis, microwave-Ca(OH) 2 pretreated sample showed the highest reducing sugar yield. The content of hemicellulose and lignin in catalpa sawdust decreased after microwave-alkali pretreatment. SEM observation showed that the catalpa sawdust surface with microwave-Ca(OH) 2 pretreatment suffered the most serious erosion. Crystallinity index of catalpa sawdust increased after all three kinds of pretreatment. The optimum conditions of microwave-Ca(OH) 2 pretreatment were particle size of 40mesh, Ca(OH) 2 dosage of 2.25% (w/v), microwave power of 400W, pretreatment time of 6min, enzyme loading of 175FPU/g, and hydrolysis time of 96h, and the reducing sugar yield of microwave-Ca(OH) 2 pretreated catalpa sawdust reached 402.73mg/g, which increased by 682.15% compared with that of raw catalpa sawdust. The catalpa sawdust with microwave-Ca(OH) 2 pretreatment is promising for biofuel production with great potential. Copyright © 2016 Elsevier Ltd. All rights reserved.

Characterisation of water hyacinth with microwave-heated alkali pretreatment for enhanced enzymatic digestibility and hydrogen/methane fermentation.

PubMed

Lin, Richen; Cheng, Jun; Song, Wenlu; Ding, Lingkan; Xie, Binfei; Zhou, Junhu; Cen, Kefa

2015-04-01

Microwave-heated alkali pretreatment (MAP) was investigated to improve enzymatic digestibility and H2/CH4 production from water hyacinth. SEM revealed that MAP deconstructed the lignocellulose matrix and swelled the surfaces of water hyacinth. XRD indicated that MAP decreased the crystallinity index from 16.0 to 13.0 because of cellulose amorphisation. FTIR indicated that MAP effectively destroyed the lignin structure and disrupted the crystalline cellulose to reduce crystallinity. The reducing sugar yield of 0.296 g/gTVS was achieved at optimal hydrolysis conditions (microwave temperature = 190°C, time = 10 min, and cellulase dosage = 5 wt%). The sequentially fermentative hydrogen and methane yields from water hyacinth with MAP and enzymatic hydrolysis were increased to 63.9 and 172.5 mL/gTVS, respectively. The energy conversion efficiency (40.0%) in the two-stage hydrogen and methane cogeneration was lower than that (49.5%) in the one-stage methane production (237.4 mL/gTVS) from water hyacinth with MAP and enzymatic hydrolysis. Copyright © 2015 Elsevier Ltd. All rights reserved.

Soil Sample Dissolution Development by Ultrawave Digester, Followed by Isotopic Separation and Analysis

DTIC Science & Technology

2017-01-09

uranium, americium, and thorium were analyzed, along with other transition and rare earth metals, utilizing inductively coupled plasma- mass spectrometry...inductively coupled plasma- mass spectrometry and/or alpha spectrometry, following digestion. For validation of the microwave protocol, radioactive... actinide elements. HF is a hazardous acid to work with and it is highly toxic. In this evaluation and validation, the actinides are of particular

Microwave digestion for the quantification of inorganic elements in coal and coal ash using ICP-OES.

PubMed

Low, Fiona; Zhang, Lian

2012-11-15

In this paper, microwave digestion conditions have been optimised to achieve complete recoveries for the ash-forming inorganic elements in coal and coal combustion fly ash, during the analysis by inductively coupled plasma optical emission spectroscopy (ICP-OES). The elements analysed include six major (Al, Ca, Fe, K, Mg and Na) and twelve trace (As, Ba, Be, Co, Cr, Cu, Li, Mn, Ni, Pb, Sr and V). Seven reference samples have been tested, including two standard coal references, SRM1632c and SARM19, their corresponding high-temperature ashes (HTAs), and three coal fly ash references, SRM1633c, SRM2690 and BCR38. The recoveries of individual elements in these samples have been examined intensively, as a function of the amount of hydrofluoric acid (HF, 0-2.0 ml), microwave power (900 W vs. 1200 W) and sample mass (0.05 g vs. 0.1 g). As have been confirmed, the recoveries of these individual elements varied significantly with the microwave digestion condition, elemental type and sample property. For the coal references and their HTAs, the use of HF can be ruled out for most of the elements, except K associated with feldspar, Pb and V. In particular, the recovery of Pb in coal is highly sample-specific and thus unpredictable. The majority of elements in fly ash references require the use of 0.1-0.2 ml HF for a complete recovery. Al in fly ash is the only exceptional element which gave incomplete recoveries throughout, suggesting the use of a complementary technique for its quantification. As has proven to be the only element inconsequential of sample type and digestion conditions, achieving complete recoveries for all cases. On the power parameter, using a higher power such as 1200 W is critical, which has proved to be an ultimatum for the recovery of certain elements, especially in fly ash. Halving sample mass from 0.1 g to 0.05 g was also found to be insignificant. Copyright © 2012 Elsevier B.V. All rights reserved.

Combining autohydrolysis and ionic liquid microwave treatment to enhance enzymatic hydrolysis of Eucalyptus globulus wood.

PubMed

Rigual, Victoria; Santos, Tamara M; Domínguez, Juan Carlos; Alonso, M Virginia; Oliet, Mercedes; Rodriguez, Francisco

2018-03-01

The combination of autohydrolysis and ionic liquid microwave treatments of eucalyptus wood have been studied to facilitate sugar production in a subsequent enzymatic hydrolysis step. Three autohydrolysis conditions (150 °C, 175 °C and 200 °C) in combination with two ionic liquid temperatures (80 °C and 120 °C) were compared in terms of chemical composition, enzymatic digestibility and sugar production. Morphology was measured (using SEM) and the biomass surface was visualized with confocal fluorescence microscopy. The synergistic cooperation of both treatments was demonstrated, enhancing cellulose accessibility. At intermediate autohydrolysis conditions (175 °C) and low ionic liquid temperature (80 °C), a glucan digestibility of 84.4% was obtained. Using SEM micrographs, fractal dimension (as a measure of biomass complexity) and lacunarity (as a measure of homogeneity) were calculated before and after pretreatment. High fractals dimensions and low lacunarities correspond to morphologically complex and homogeneous samples, that are better digested by enzyme cocktails. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effect of roasted pea flour/starch and encapsulated pea starch incorporation on the in vitro starch digestibility of pea breads.

PubMed

Lu, Zhan-Hui; Donner, Elizabeth; Liu, Qiang

2018-04-15

Oven or microwave roasting and alginate encapsulation of pea flour and starch to produce novel pea ingredients for enrichment of slowly digestible starch (SDS) and resistant starch (RS) content in pea bread were investigated. Pea flour treated either by oven roasting (160°C, 30min) or by microwave roasting (1.1kW, 6min) effectively retained its low starch digestibility similar to its native form (∼25% SDS; ∼60% RS). When oven roasting was applied to pea starch, SDS content increased triply compared to the fully boiled counterpart. Alginate encapsulation effectively controlled carbohydrate release to simulated gastric, intestinal and colonic fluids, and thus largely enriched the SDS and RS fractions in starch. Pea bread containing up to 37.5% of encapsulated roasted MPS pea starch not only provided high SDS and RS fractions (23.9% SDS and 30.2% RS) compared to a white bread control (0.2% SDS and 2.5% RS), but also provided an acceptable palatability. Crown Copyright © 2017. Published by Elsevier Ltd. All rights reserved.

Anaerobic digestion of microalgal bacterial flocs from a raceway pond treating aquaculture wastewater: need for a biorefinery.

PubMed

Van Den Hende, Sofie; Laurent, Cedric; Bégué, Marine

2015-11-01

An outdoor raceway pond with microalgal bacterial flocs (MaB-flocs) is a novel sunlight-based system to treat pikeperch aquaculture wastewater while producing biomass. The harvested MaB-floc biomass (33tonTSha(-1)y(-1)) needs further valorization. Therefore, the biochemical methane yield (BMY) of MaB-floc biomass was determined in batch experiments. The results show significant differences between the BMY of MaB-flocs amongst their harvest dates (128-226NLCH4kg(-1)VS), a low anaerobic digestion conversion efficiency (25.0-36.2%), a moderate chlorophyll a removal (51.5-86.9%) and a low biogas profit (<0.01€m(-3)wastewater). None of the pretreatment methods screened (freezing, thermal, microwave, ultrasonic and chlorination, flue gas sparging, and acid) can be recommended due to a low BMY improvement and/or unfavorable energy balance. Therefore, anaerobic digestion of this MaB-floc biomass should only be granted a supporting role within a biorefinery concept. Copyright © 2015 Elsevier Ltd. All rights reserved.

Eating, Diet, and Nutrition for Constipation

MedlinePlus

... some microwavable dinners References [4] U.S. Department of Agriculture and U.S. Department of Health and Human Services. ... Grants & Grant History Research Resources Research at NIDDK Technology Advancement & Transfer Meetings & Workshops Health Information Diabetes Digestive ...

Ultra-low background mass spectrometry for rare-event searches

NASA Astrophysics Data System (ADS)

Dobson, J.; Ghag, C.; Manenti, L.

2018-01-01

Inductively Coupled Plasma Mass Spectrometry (ICP-MS) allows for rapid, high-sensitivity determination of trace impurities, notably the primordial radioisotopes 238U and 232Th, in candidate materials for low-background rare-event search experiments. We describe the setup and characterisation of a dedicated low-background screening facility at University College London where we operate an Agilent 7900 ICP-MS. The impact of reagent and carrier gas purity is evaluated and we show that twice-distilled ROMIL-SpATM-grade nitric acid and zero-grade Ar gas delivers similar sensitivity to ROMIL-UpATM-grade acid and research-grade gas. A straightforward procedure for sample digestion and analysis of materials with U/Th concentrations down to 10 ppt g/g is presented. This includes the use of 233U and 230Th spikes to correct for signal loss from a range of sources and verification of 238U and 232Th recovery through digestion and analysis of a certified reference material with a complex sample matrix. Finally, we demonstrate assays and present results from two sample preparation and assay methods: a high-sensitivity measurement of ultra-pure Ti using open digestion techniques, and a closed vessel microwave digestion of a nickel-chromium-alloy using a multi-acid mixture.

Functional Fe3O4@ZnO magnetic nanoparticle-assisted enrichment and enzymatic digestion of phosphoproteins from saliva.

PubMed

Chen, Wei-Yu; Chen, Yu-Chie

2010-11-01

Saliva contains various proteins, particularly abundant are phosphoproteins, that may be related to disease occurrences and that play significant roles in a biological system. Thus, medical diagnostics will benefit tremendously if disease-related protein biomarkers are discovered from saliva. In this paper, we propose and demonstrate an approach using functional zinc oxide coated iron oxide magnetic nanoparticles (Fe(3)O(4)@ZnO MNPs) as affinity probes to selectively enrich phosphoproteins from complex saliva samples and as microwave absorbers to assist the enrichment and subsequent tryptic digestion of trapped proteins under microwave heating. The target species trapped by MNPs were characterized by matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS) combined with protein database search. Entire analysis time was shortened to less than 20 min. The detection limit of this approach for a monophosphopeptide was as low as 250 pM (10 μL).

In vitro digestibility, protein composition and techno-functional properties of Saskatchewan grown yellow field peas (Pisum sativum L.) as affected by processing.

PubMed

Ma, Zhen; Boye, Joyce I; Hu, Xinzhong

2017-02-01

Saskatchewan grown yellow field pea was subjected to different processing conditions including dehulling, micronization, roasting, conventional/microwave cooking, germination, and combined germination and conventional cooking/roasting. Their nutritional and antinutritional compositions, functional properties, microstructure, thermal properties, in vitro protein and starch digestibility, and protein composition were studied. Processed field peas including conventional cooked yellow peas (CCYP), microwave cooked yellow peas (MCYP), germinated-conventional cooked yellow peas (GCCYP), and germinated-roasted yellow peas (GRYP) exhibited the significantly higher in vitro protein digestibility (IVPD), which was in accordance with their significantly lower trypsin inhibitor activity and tannin content. The SDS-PAGE and size exclusion HPLC profiles of untreated pea proteins and their hydrolysates also confirmed the IVPD result that these four treatments facilitated the hydrolysis of pea proteins to a greater extent. The CCYP, MCYP, GCCYP, and GRYP also exhibited significantly higher starch digestibility which was supported by their lower onset (T o ), peak (T p ), and conclusion (T c ) temperatures obtained from DSC thermogram, their lower pasting properties and starch damage results, as well as their distinguished amorphous flakes' configuration observed on the scanning electron microscopic image. LC/ESI-MS/MS analysis following in-gel digests of SDS-PAGE separated proteins allowed detailed compositional characterization of pea proteins. The present study would provide fundamental information to help to better understand the functionality of field peas as ingredients, and particularly in regards to agri-food industry to improve the process efficiency of field peas with enhanced nutritional and techno-functional qualities. Copyright © 2016 Elsevier Ltd. All rights reserved.

Chlorine and sulfur determination in extra-heavy crude oil by inductively coupled plasma optical emission spectrometry after microwave-induced combustion

NASA Astrophysics Data System (ADS)

Pereira, Juliana S. F.; Mello, Paola A.; Moraes, Diogo P.; Duarte, Fábio A.; Dressler, Valderi L.; Knapp, Guenter; Flores, Érico M. M.

2009-06-01

In this study, microwave-induced combustion (MIC) of extra-heavy crude oil is proposed for further chlorine and sulfur determination by inductively coupled plasma optical emission spectrometry (ICP OES). Combustion was carried out under oxygen pressure (20 bar) in quartz vessels using ammonium nitrate (50 µl of 6 mol l - 1 solution) as ignition aid. Samples were wrapped with polyethylene film and placed on a quartz holder positioned inside the quartz vessels. The need for an additional reflux step after combustion and the type and concentration of absorbing solution (water, 0.02 to 0.9 mmol l - 1 H 2O 2, 10 to 100 mmol l - 1 (NH 4) 2CO 3 or 0.1 to 14 mol l - 1 HNO 3) were studied. The influence of sample mass, O 2 pressure and maximum pressure attained during the combustion process were investigated. Recoveries from 92 to 102% were obtained for Cl and S for all absorbing solutions. For comparison, Cl and S determination was also performed by ion chromatography (IC) using 25 mmol l - 1 (NH 4) 2CO 3 as absorbing solution. Using MIC with a reflux step the agreement was better than 95% for certified reference materials of similar composition (crude oil, petroleum coke, coal and residual fuel oil). Microwave-assisted digestion and water extraction in high pressure closed vessels were also evaluated. Using these procedures the maximum recoveries were 30 and 98% for Cl and S, respectively, using microwave-assisted digestion and 70% for Cl and less than 1% for S by water extraction procedure. Limits of detection by ICP OES were 12 and 5 µg g - 1 for Cl and S, respectively, and the corresponding values by IC were 1.2 and 8 µg g - 1 . Using MIC it was possible to digest simultaneously up to eight samples resulting in a solution suitable for the determination of both analytes with a single combustion step.

Determination of arsenic species in marine samples by HPLC-ICP-MS.

PubMed

Hirata, Shizuko; Toshimitsu, Hideki; Aihara, Masato

2006-01-01

Arsenic speciation analysis in marine samples was performed using high performance liquid chromatography (HPLC) with ICP-MS detection. The separation of eight arsenic species viz. arsenite (As(III)), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), arsenate (As(V)), arsenobetaine, trimethylarsine oxide (TMAO), arsenocholine and tetramethylarsonium ion (TeMAs) was achieved on a Shiseido Capcell Pak C18 column by using an isocratic eluent (pH 3.0), in which condition As(III) and MMA were co-eluted. The entire separation was accomplished in 15 min. The detection limits for 8 arsenic species by HPLC/ICP-MS were in the range of 0.02 - 0.10 microg L(-1) based on 3sigma of blank response (n=9). The precision was calculated to be 3.1-7.3% (RSD) for all eight species. The method then successfully applied to several marine samples e.g., oyster, scallop, fish, and shrimps. For the extraction of arsenic species from seafood products, the low power microwave digestion was employed. The extraction efficiency was in the range of 52.9 - 112.3%. Total arsenic concentrations were analyzed by using the microwave acid digestion. The total arsenics in the certified reference materials (DORM-2 and TORT-2) were analyzed and agreed with the certified values. The concentrations of arsenics in marine samples were in the range 6.6 - 35.1 microg g(-1).

Detection of copper, lead, cadmium and iron in wine using electronic tongue sensor system.

PubMed

Simões da Costa, A M; Delgadillo, I; Rudnitskaya, A

2014-11-01

An array of 10 potentiometric chemical sensors has been applied to the detection of total Fe, Cu, Pb and Cd content in digested wine. As digestion of organic matter of wine is necessary prior to the trace metal detection using potentiometric sensors, sample preparation procedures have been optimized. Different variants of wet and microwave digestion and dry ashing, 14 conditions in total, have been tested. Decomposition of organic matter was assessed using Fourier transform mid-infrared spectroscopy and total phenolic content. Dry ashing was found to be the most effective method of wine digestion. Measurements with sensors in individual solutions of Fe(III), Cu(II), Pb(II) and Cd(II) prepared on different backgrounds have shown that their detection limits were below typical concentration levels of these metals in wines and, in the case of Cu, Pb and Cd below maximum allowed concentrations. Detection of Fe in digested wine samples was possible using discrete iron-sensitive sensors with chalcogenide glass membranes with RMSEP of 0.05 mmol L(-1) in the concentration range from 0.0786 to 0.472 mmol L(-1). Low concentration levels of Cu, Pb and Cd in wine and cross-sensitivity of respective sensors resulted in the non-linearity of their responses, requiring back-propagation neural network for the calibration. Calibration models have been calculated using measurements in the model mixed solutions containing all three metals and a set of digested wine sample. RMSEP values for Cu, Pb and Cd were 3.9, 39 and 1.2 μmol L(-1) in model solutions and 2, 150 and 1 μmol L(-1) in digested wine samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Different techniques for characterizing single-walled carbon nanotube purity

NASA Astrophysics Data System (ADS)

Yuca, Neslihan; Camtakan, Zeyneb; Karatepe, Nilgün

2013-09-01

Transition-metal catalysts, fullerenes, graphitic carbon, amorphous carbon, and graphite flakes are the main impurities in carbon nanotubes. In this study, we demonstrate an easy and optimum method of cleaning SWCNTs and evaluating their purity. The purification method, which employed oxidative heat treatment followed by 6M HNO3, H2SO4, HNO3:H2SO4 and HCl acid reflux for 6h at 120°C and microwave digestion with 1.5M HNO3 for 0.5h at 210°C which was straightforward, inexpensive, and fairly effective. The purified materials were characterized by thermogravimetric analysis and nuclear techniques such as INAA, XRF and XRD.

Fast Enzymatic Processing of Proteins for MS Detection with a Flow-through Microreactor

PubMed Central

Lazar, Iulia M.; Deng, Jingren; Smith, Nicole

2016-01-01

The vast majority of mass spectrometry (MS)-based protein analysis methods involve an enzymatic digestion step prior to detection, typically with trypsin. This step is necessary for the generation of small molecular weight peptides, generally with MW < 3,000-4,000 Da, that fall within the effective scan range of mass spectrometry instrumentation. Conventional protocols involve O/N enzymatic digestion at 37 ºC. Recent advances have led to the development of a variety of strategies, typically involving the use of a microreactor with immobilized enzymes or of a range of complementary physical processes that reduce the time necessary for proteolytic digestion to a few minutes (e.g., microwave or high-pressure). In this work, we describe a simple and cost-effective approach that can be implemented in any laboratory for achieving fast enzymatic digestion of a protein. The protein (or protein mixture) is adsorbed on C18-bonded reversed-phase high performance liquid chromatography (HPLC) silica particles preloaded in a capillary column, and trypsin in aqueous buffer is infused over the particles for a short period of time. To enable on-line MS detection, the tryptic peptides are eluted with a solvent system with increased organic content directly in the MS ion source. This approach avoids the use of high-priced immobilized enzyme particles and does not necessitate any aid for completing the process. Protein digestion and complete sample analysis can be accomplished in less than ~3 min and ~30 min, respectively. PMID:27078683

Fast Enzymatic Processing of Proteins for MS Detection with a Flow-through Microreactor.

PubMed

Lazar, Iulia M; Deng, Jingren; Smith, Nicole

2016-04-06

The vast majority of mass spectrometry (MS)-based protein analysis methods involve an enzymatic digestion step prior to detection, typically with trypsin. This step is necessary for the generation of small molecular weight peptides, generally with MW < 3,000-4,000 Da, that fall within the effective scan range of mass spectrometry instrumentation. Conventional protocols involve O/N enzymatic digestion at 37 ºC. Recent advances have led to the development of a variety of strategies, typically involving the use of a microreactor with immobilized enzymes or of a range of complementary physical processes that reduce the time necessary for proteolytic digestion to a few minutes (e.g., microwave or high-pressure). In this work, we describe a simple and cost-effective approach that can be implemented in any laboratory for achieving fast enzymatic digestion of a protein. The protein (or protein mixture) is adsorbed on C18-bonded reversed-phase high performance liquid chromatography (HPLC) silica particles preloaded in a capillary column, and trypsin in aqueous buffer is infused over the particles for a short period of time. To enable on-line MS detection, the tryptic peptides are eluted with a solvent system with increased organic content directly in the MS ion source. This approach avoids the use of high-priced immobilized enzyme particles and does not necessitate any aid for completing the process. Protein digestion and complete sample analysis can be accomplished in less than ~3 min and ~30 min, respectively.

Heavy metals in atmospheric surrogate dry deposition

PubMed

Morselli; Cecchini; Grandi; Iannuccilli; Barilli; Olivieri

1999-02-01

This paper describes a methodological approach for the assessment of the amount of surrogate dry deposition of several toxic heavy metals (Cd, Cr, Cu, Ni, Pb, V, Zn) associated with atmospheric particulate matter at ground level. The objectives of the study were twofold: i) the evaluation of several techniques for the digestion of dry deposition samples for trace metal analysis; ii) the comparison of the results from two samplers with different collecting surfaces. A dry solid surface sampler (DRY sampler, Andersen--USA) and a water layer surface sampler (DAS sampler--MTX Italy) were employed. The samples were collected over a one-year period in an urban site of Bologna (northern Italy). A description is given of the complete procedure, from sampling to data elaboration, including sample storage, digestion and analytical methods. According to the results obtained with three different digestion techniques (Teflon bomb, microwave digester and Teflon flask with vapour cooling system), the highest recovery rate was achieved by the Teflon bomb procedure employing an NBS 1648 Standard Reference Material; 90-95% of the elements considered were recovered by dissolution in a pressurized Teflon bomb with an HNO3-HF mixture. Given these results, the technique was adopted for dry deposition sample digestion. On the basis of the amount of heavy metals measured as monthly deposition fluxes (microg/m2), the collecting efficiency of the DAS sampler for a number of elements was found to be as much as two to three times greater than that of the DRY sampler.

Determination of total mercury in biological and geological samples

USGS Publications Warehouse

Crock, James G.

2005-01-01

The analytical chemist is faced with several challenges when determining mercury in biological and geological materials. These challenges include widespread mercury contamination, both in the laboratory and the environment, possible losses of mercury during sample preparation and digestion, the wide range of mercury values commonly observed, ranging from the low nanogram per gram or per liter for background areas to hundreds of milligrams per kilogram in contaminated or ore-bearing areas, great matrix diversity, and sample heterogeneity1. These factors can be naturally occurring or anthropogenic, but must be addressed to provide a precise and accurate analysis. Although there are many instrumental methods available for the successful determination of mercury, no one technique will address all problems or all samples all of the time. The approach for the determination of mercury used at the U.S. Geological Survey, Crustal Imaging and Characterization Team, Denver Laboratories, utilizes a suite of complementary instrumental methods when approaching a study requiring mercury analyses. Typically, a study could require the analysis of waters, leachates or selective digestions of solids, vegetation, and biological materials such as tissue, bone, or shell, soils, rocks, sediments, coals, sludges, and(or) ashes. No one digestion or sample preparation method will be suitable for all of these matrices. The digestions typically employed at our laboratories include: (i) a closed-vessel microwave method using nitric acid and hydrogen peroxide, followed by digestion/dilution with a nitric acid/sodium dichromate solution, (ii) a robotic open test-tube digestion with nitric acid and sodium dichromate, (iii) a sealed Teflon? vessel with nitric acid and sodium dichromate, (iv) a sealed glass bottle with nitric acid and sodium dichromate, or (v) open test tube digestion with nitric and sulfuric acids and vanadium pentoxide. The common factor in all these digestions is that they are very oxidative to ensure the conversion of all mercury forms into Hg (II). Each method of digestion has its advantages and limitations. The method of detection used in our laboratories involves a combination of an in-house, custom, classic continuous-flow cold-vapor atomic absorption spectrometry (CVAAS), a commercially available, automated, flow-injection and a continuous flow cold-vapor atomic fluorescence spectrometry (CV-AFS) systems, and a relatively new, automated and integrated approach where solid or liquid samples are thermally decomposed under an oxygen atmosphere (a nitrogen atmosphere is used for coals) and the released mercury vapor trapped onto a gold gauze and then thermally released into an AAS system. Other less frequently used instrumental methods available for the determination of mercury include inductively coupled plasma ? optical emission spectrometry (ICP-OES), inductively couple plasma ? mass spectrometry (ICP-MS) (both solution nebulization and laser ablation), and instrumental neutron activation analysis (INAA). Results from two case studies involving the determination of mercury in the challenging matrices of biological materials will be presented. These will include fillet, liver and stomach-content samples from grayling for a baseline/background study in Alaska, and samples of meat tissue and shell material from Tanner crabs from Glacier Bay, Alaska. These studies show that the method of digestion is more important than a very sensitive detection limit for mercury.

Determination of mercury compounds in fish by microwave-assisted extraction and liquid chromatography-vapor generation-inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Chiou, Chwei-Sheng; Jiang, Shiuh-Jen; Kumar Danadurai, K. Suresh

2001-07-01

A method employing a vapor generation system and LC combined with inductively coupled plasma mass spectrometry (LC-ICP-MS) is presented for the determination of mercury in biological tissues. An open vessel microwave digestion system was used to extract the mercury compounds from the sample matrix. The efficiency of the mobile phase, a mixture of L-cysteine and 2-mercaptoethanol, was evaluated for LC separation of inorganic mercury [Hg(II)], methylmercury (methyl-Hg) and ethylmercury (ethyl-Hg). The sensitivity, detection limits and repeatability of the liquid chromatography (LC) ICP-MS system with a vapor generator were comparable to, or better than, that of an LC-ICP-MS system with conventional pneumatic nebulization, or other sample introduction techniques. The experimental detection limits for various mercury species were in the range of 0.05-0.09 ng ml -1 Hg, based on peak height. The proposed method was successfully applied to the determination of mercury compounds in a swordfish sample purchased from the local market. The accuracy of the method was evaluated by analyzing a marine biological certified reference material (DORM-2, NRCC).

Determination of total mercury in environmental and biological samples by flow injection cold vapour atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Murphy, James; Jones, Phil; Hill, Steve J.

1996-12-01

A simple and accurate method has been developed for the determination of total mercury in environmental and biological samples. The method utilises an off-line microwave digestion stage followed by analysis using a flow injection system with detection by cold vapour atomic absorption spectrometry. The method has been validated using two certified reference materials (DORM-1 dogfish and MESS-2 estuarine sediment) and the results agreed well with the certified values. A detection limit of 0.2 ng g -1 Hg was obtained and no significant interference was observed. The method was finally applied to the determination of mercury in river sediments and canned tuna fish, and gave results in the range 0.1-3.0 mg kg -1.

Total reflection X-ray fluorescence as a convenient tool for determination of trace elements in microscale gasoline and diesel

NASA Astrophysics Data System (ADS)

Zhang, Airui; Jin, Axiang; Wang, Hai; Wang, Xiaokang; Zha, Pengfei; Wang, Meiling; Song, Xiaoping; Gao, Sitian

2018-03-01

Quantitative determination of trace elements like S, Fe, Cu, Mn and Pb in gasoline and S in diesel is of great importance due to the growing concerns over air pollution, human health and engine failure caused by utilization of gasoline and diesel with these harmful elements. A method of total reflection X-ray fluorescence (TXRF) was developed to measure these harmful trace elements in gasoline and diesel. A variety of factors to affect measurement results, including TXRF parameters, microwave-assisted digestion conditions and internal standard element and its addition, were examined to optimize these experimental procedures. The hydrophobic treatment of the surface of quartz reflectors to support the analyte with neutral silicone solutions could prepare thin films of gasoline and diesel digestion solutions for subsequent TXRF analysis. The proposed method shows good potential and reliability to determine the content of harmful trace elements in gasoline and diesel with high sensitivity and accuracy without drawing different standard calibration curves, and can be easily employed to screen gasoline and diesel in routine quality control and assurance.

Soil and sediment sample analysis for the sequential determination of natural and anthropogenic radionuclides.

PubMed

Michel, H; Levent, D; Barci, V; Barci-Funel, G; Hurel, C

2008-02-15

A new sequential method for the determination of both natural (U, Th) and anthropogenic (Sr, Cs, Pu, Am) radionuclides has been developed for application to soil and sediment samples. The procedure was optimised using a reference sediment (IAEA-368) and reference soils (IAEA-375 and IAEA-326). Reference materials were first digested using acids (leaching), 'total' acids on hot plate, and acids in microwave in order to compare the different digestion technique. Then, the separation and purification were made by anion exchange resin and selective extraction chromatography: transuranic (TRU) and strontium (SR) resins. Natural and anthropogenic alpha radionuclides were separated by uranium and tetravalent actinide (UTEVA) resin, considering different acid elution medium. Finally, alpha and gamma semiconductor spectrometer and liquid scintillation spectrometer were used to measure radionuclide activities. The results obtained for strontium-90, cesium-137, thorium-232, uranium-238, plutonium-239+240 and americium-241 isotopes by the proposed method for the reference materials provided excellent agreement with the recommended values and good chemical recoveries. Plutonium isotopes in alpha spectrometry planchet deposits could be also analysed by ICPMS.

Influence of deflocculation on microwave disintegration and anaerobic biodegradability of waste activated sludge.

PubMed

Ebenezer, A Vimala; Kaliappan, S; Adish Kumar, S; Yeom, Ick-Tae; Banu, J Rajesh

2015-06-01

In the present study, the potential benefits of deflocculation on microwave pretreatment of waste activated sludge were investigated. Deflocculation in the absence of cell lysis was achieved through the removal of extra polymeric substances (EPS) by sodium citrate (0.1g sodium citrate/g suspended solids), and DNA was used as a marker for monitoring cell lysis. Subsequent microwave pretreatment yielded a chemical oxygen demand (COD) solubilisation of 31% and 21%, suspended solids (SS) reduction of 37% and 22%, for deflocculated and flocculated sludge, respectively, with energy input of 14,000kJ/kg TS. When microwave pretreated sludge was subjected to anaerobic fermentation, greater accumulation of volatile fatty acid (860mg/L) was noticed in deflocculated sludge, indicating better hydrolysis. Among the samples subjected to BMP (Biochemical methane potential test), deflocculated microwave pretreated sludge showed better amenability towards anaerobic digestion with high methane production potential of 0.615L (gVS)(-1). Copyright © 2015 Elsevier Ltd. All rights reserved.

Impact of temperature, microwave radiation and organic loading rate on methanogenic community and biogas production during fermentation of dairy wastewater.

PubMed

Zielińska, Magdalena; Cydzik-Kwiatkowska, Agnieszka; Zieliński, Marcin; Dębowski, Marcin

2013-02-01

This study analyzed dairy wastewater fermentation in convection- and microwave-heated hybrid reactors at loadings of 1 and 2 kg COD/(m3 d) and temperatures of 35 and 55 °C. The biomass was investigated at a molecular level to determine the links between the operational parameters of anaerobic digestion and methanogenic Archaea structure. The highest production of biogas with methane content of ca. 67% was noted in the mesophilic microwave-heated reactors. The production of methane-rich biogas and the overall diversity of Archaea was determined by Methanosarcinaceae presence. The temperature and the application of microwaves were the main factors explaining the variations in the methanogen community. At 35 °C, the microwave heating stimulated the growth of highly diverse methanogen assemblages, promoting Methanosarcina barkeri presence and excluding Methanosarcina harudinacea from the biomass. A temperature increase to 55 °C lowered Methanosarcinaceae abundance and induced a replacement of Methanoculleus palmolei by Methanosarcina thermophila. Copyright © 2012 Elsevier Ltd. All rights reserved.

In vitro starch digestibility and predicted glycemic index of microwaved and conventionally baked pound cake.

PubMed

Sánchez-Pardo, María Elena; Ortiz-Moreno, Alicia; Mora-Escobedo, Rosalva; Necoechea-Mondragón, Hugo

2007-09-01

The present study compares the effect of baking process (microwave vs conventional oven) on starch bioavailability in fresh pound cake crumbs and in crumbs from pound cake stored for 8 days. Proximal chemical analysis, resistant starch (RS), retrograded starch (RS3) and starch hydrolysis index (HI) were evaluated. The empirical formula suggested by Granfeldt was used to determine the predicted glycemic index (pGI). Pound cake, one of Mexico's major bread products, was selected for analysis because the quality defects often associated with microwave baking might be reduced with the use of high-fat, high-moisture, batted dough. Differences in product moisture, RS and RS3 were observed in fresh microwave-baked and conventionally baked pound cake. RS3 increased significantly in conventionally baked products stored for 8 days at room temperature, whereas no significantly changes in RS3 were observed in the microwaved product. HI values for freshly baked and stored microwaved product were 59 and 62%, respectively (P > 0.05), whereas the HI value for the conventionally baked product decreased significantly after 8 days of storage. A pound cake with the desired HI and GI characteristics might be obtained by adjusting the microwave baking process.

Determination of chiral pharmaceuticals and illicit drugs in wastewater and sludge using microwave assisted extraction, solid-phase extraction and chiral liquid chromatography coupled with tandem mass spectrometry.

PubMed

Evans, Sian E; Davies, Paul; Lubben, Anneke; Kasprzyk-Hordern, Barbara

2015-07-02

This is the first study presenting a multi-residue method allowing for comprehensive analysis of several chiral pharmacologically active compounds (cPACs) including beta-blockers, antidepressants and amphetamines in wastewater and digested sludge at the enantiomeric level. Analysis of both the liquid and solid matrices within wastewater treatment is crucial to being able to carry out mass balance within these systems. The method developed comprises filtration, microwave assisted extraction and solid phase extraction followed by chiral liquid chromatography coupled with tandem mass spectrometry to analyse the enantiomers of 18 compounds within all three matrices. The method was successfully validated for 10 compounds within all three matrices (amphetamine, methamphetamine, MDMA, MDA, venlafaxine, desmethylvenlafaxine, citalopram, metoprolol, propranolol and sotalol), 7 compounds validated for the liquid matrices only (mirtazapine, salbutamol, fluoxetine, desmethylcitalopram, atenolol, ephedrine and pseudoephedrine) and 1 compound (alprenolol) passing the criteria for solid samples only. The method was then applied to wastewater samples; cPACs were found at concentration ranges in liquid matrices of: 1.7 ng L(-1) (metoprolol) - 1321 ng L(-1) (tramadol) in influent,

[Determination of Mineral Elements in Choerospondias Axillaris and Its Extractives by ICP-AES].

PubMed

Zhai, Yu-xin; Chen, Jun; Li, Ti; Liu, Ji-yan; Wang, Xie-yi; Cheng, Chao; Liu, Cheng-mei

2015-04-01

Nine elements in Choerospondias axillaris flesh, peels, aqueous extractives and gastric digesta were determined by the inductively coupled plasma atomic emission spectrometry (ICP-AES) in the present study. The results showed that the contents of Fe, Ca, Zn, Mn, Al, Mg, Cu, K and P in the flesh were 27.37, 269.88, 1.51, 2.45, 1.95, 195.30, 2.45, 2,970.11, and 133.94 µg · g(-1), respectively. They are lower than that in the peels, about 40.31%, 11.70%, 21.68%, 4.27%, 10.58%, 15.76%, 68.72%, 42.04%, and 22.59%, respectively. For microwave assistant extraction, the release rate of Mn was highest (81.68%), while Fe was lowest (4.42%) in the flesh. The release rate of Zn was the highest (79.00%), while that of A1 was the lowest (4.94%) in the peels. Except Fe, Cu and Zn, the release rates of the other elements in flesh were higher than those in the peels. After gastric digestion, the release rates of nine elements were 3.25%-87.51% in the flesh and 7.11%-50.69% in the peels. The release rates of minerals in the flesh were found to be higher than those in the peels except Fe and Cu. Microwave assistant extraction can more efficiently release Fe, Ca, Mn, Mg and K from the flesh than the gastric digestion do. While gastric digestion had a significant effect on the peels, the release rates of elements, except Zn, were higher than those in microwave assistant extraction. Therefore, the difference of distribution and release of mineral elements between peels and flesh of Choerospondias axillaris was understood, which will provide a positive guide for further study of bioavailability of minerals for human body.

Microwave assisted digestion followed by ICP-MS for determination of trace metals in atmospheric and lake ecosystem.

PubMed

Ahmed, Manan; Chin, Ying Hui; Guo, Xinxin; Zhao, Xing-Min

2017-05-01

The study of trace metals in the atmosphere and lake water is important due to their critical effects on humans, aquatic animals and the geochemical balance of ecosystems. The objective of this study was to investigate the concentration of trace metals in atmospheric and lake water samples during the rainy season (before and after precipitation) between November and December 2015. Typical methods of sample preparation for trace metal determination such as cloud point extraction, solid phase extraction and dispersive liquid-liquid micro-extraction are time-consuming and difficult to perform; therefore, there is a crucial need for development of more effective sample preparation procedure. A convection microwave assisted digestion procedure for extraction of trace metals was developed for use prior to inductively couple plasma-mass spectrometric determination. The result showed that metals like zinc (133.50-419.30μg/m 3 ) and aluminum (53.58-378.93μg/m 3 ) had higher concentrations in atmospheric samples as compared to lake samples before precipitation. On the other hand, the concentrations of zinc, aluminum, chromium and arsenic were significantly higher in lake samples after precipitation and lower in atmospheric samples. The relationship between physicochemical parameters (pH and turbidity) and heavy metal concentrations was investigated as well. Furthermore, enrichment factor analysis indicated that anthropogenic sources such as soil dust, biomass burning and fuel combustion influenced the metal concentrations in the atmosphere. Copyright © 2016. Published by Elsevier B.V.

Chemical and mineralogical characterization of chromite ore processing residue from two recent Indian disposal sites.

PubMed

Matern, Katrin; Kletti, Holger; Mansfeldt, Tim

2016-07-01

Chromite ore processing residue (COPR) is a hazardous waste. Nevertheless, deposition of COPR in uncontrolled surface landfills is still common practice in some countries. Whereas old (between at least 40 and 180 years) COPR from the temperate zone has been intensively investigated, information on COPR in other regions is restricted. Relatively young (<25 years) COPR samples obtained from two abandoned landfill sites in India were investigated by a modified total microwave digestion method, X-ray powder diffraction (XRPD), and scanning electron microscopy (SEM) in order to determine their chemical and mineralogical nature. By the use of microwave digestion with acid mixtures of HNO3, H3PO4, and HBF4 (5:3:2 vol), COPR was completely dissolved and element contents similar to those obtained by X-ray fluorescence were found. Total Cr contents of the two COPR accounted for 81 and 74 g kg(-1), of which 20 and 13% were present in the carcinogenic hexavalent form (CrVI). Apart from the common major mineral phases present in COPR reported earlier, a further Cr host mineral, grimaldiite [CrO(OH)], could be identified by XRPD and SEM. Additionally, well soluble Na2CrO4 was present. Improving the effectiveness of chromite ore processing and preventing the migration of Cr(VI) into water bodies are the main challenges when dealing with these COPR. Copyright © 2016 Elsevier Ltd. All rights reserved.

Comparison of various pretreatments for ethanol production enhancement from solid residue after rumen fluid digestion of rice straw.

PubMed

Zhang, Haibo; Zhang, Panyue; Ye, Jie; Wu, Yan; Liu, Jianbo; Fang, Wei; Xu, Dong; Wang, Bei; Yan, Li; Zeng, Guangming

2018-01-01

The rumen digested residue of rice straw contains high residual carbohydrates, which makes it a potential cellulosic ethanol feedstock. This study evaluated the feasibility and effectiveness of applying microwave assisted alkali (MAP), ultrasound assisted alkali (UAP), and ball milling pretreatment (BMP) to enhance ethanol production from two digested residues (2.5%-DR and 10%-DR) after rumen fluid digestion of rice straw at 2.5% and 10.0% solid content. Results revealed that 2.5%-DR and 10%-DR had a cellulose content of 36.4% and 41.7%, respectively. MAP and UAP improved enzymatic hydrolysis of digested residue by removing the lignin and hemicellulose, while BMP by decreasing the particle size and crystallinity. BMP was concluded as the suitable pretreatment, resulting in an ethanol yield of 116.65 and 147.42mgg -1 for 2.5%-DR and 10%-DR, respectively. The integrated system including BMP for digested residue at 2.5% solid content achieved a maximum energy output of 7010kJkg -1 . Copyright © 2017 Elsevier Ltd. All rights reserved.

Investigation of major and trace element distribution in the extraction-transesterification process of fatty acid methyl esters from microalgae Chlorella sp.

PubMed

Soares, Bruno M; Vieira, Augusto A; Lemões, Juliana S; Santos, Clarissa M M; Mesko, Márcia F; Primel, Ednei G; Montes D'Oca, Marcelo G; Duarte, Fábio A

2012-04-01

This work reports, for the first time, the determination of major and trace elements (Al, As, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, La, Mg, Mn, Mo, Na, Ni, P, Pb, S, Se, Sn, Sr, Ti, Tl, U, V, and Zn) in the fractions of the synthesis of fatty acid methyl esters (FAMEs). These include fresh microalgae, residual biomass, lipid fraction, crude FAMEs, insoluble fraction and purified FAMEs from microalgae Chlorella sp. A microwave-assisted digestion procedure in closed vessels was applied for sample digestion and subsequent element determination by inductively coupled plasma-based techniques. The proposed method was suitable for the multielement determination in FAMEs and its fractions obtained from microalgae. The element concentration was compared with results found in the literature and a careful discussion about the use of residual biomass for different applications was performed. Copyright © 2012 Elsevier Ltd. All rights reserved.

Determination of metallo-organic and particulate wear metals in lubricating oils associated with hybrid ceramic bearings by inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Russell, Robin Ann

It is possible to increase both the performance and operating environment of jet engines by using hybrid ceramic bearings. Our laboratory is concerned with investigating lubricating fluids for wear metals associated with silicon nitride ball bearings and steel raceways. Silicon nitride is characterized by low weight, low thermal expansion, high strength, and corrosion resistance. These attributes result in longer engine lifetimes than when metallic ball bearings are used. Before the routine use of ceramic ball bearings can be realized, the wear mechanisms of the materials should be thoroughly understood. One important variable in determining wear degradation is the concentration of metal present in the lubricating oils used with the bearings. A complete method for analyzing used lubricating oils for wear metal content must accurately determine all metal forms present. Oil samples pose problems for routine analysis due to complex organic matrices. Nebulizing these types of samples into an Inductively Coupled Plasma - Mass Spectrometer introduces many problems including clogging of the sample cone with carbon and increasing interferences. In addition, other techniques such as Atomic Absorption Spectrometry and Atomic Emission Spectrometry are particle size dependent. They are unable to analyze particles greater than 10 mum in size. This dissertation describes a method of analyzing lubricating oils for both metallo-organic and particulate species by ICP-MS. Microwave digestion of the oil samples eliminates the need for elaborate sample introduction schemes as well as the use of a modified carrier gas. Al, Cr, Fe, Mg, Mo, Ni, Ti, and Y have been determined in both aqueous and organic media. Metallo-organic solutions of these metals were successfully digested, nebulized into the ICP, and the singly charged ions measured by mass spectrometry. Metal particulates in oil matrices have also been quantitatively determined by the above method. Linear analytical curves were obtained for these elements from the detection limits (˜1 ppb) to greater than 1 ppm. Used lubricating oil samples were also analyzed by microwave digestion ICP-MS. Oil samples were collected from a Rolling Contact Fatigue tester. Two bearing systems were evaluated: M50 steel balls on an M50 steel rod, and Sisb3Nsb4 balls on an M50 steel rod. Improved operating conditions were obtained when the Sisb3Nsb4 balls were used, which corresponds to longer engine lifetimes.

Establishing human heart chromium, cobalt and vanadium concentrations by inductively coupled plasma mass spectrometry.

PubMed

Day, Patrick L; Eckdahl, Steven J; Maleszewski, Joseph J; Wright, Thomas C; Murray, David L

2017-05-01

Chromium, cobalt, and vanadium are used in metallic joint prosthesis. Case studies have associated elevated heart tissue cobalt concentrations with myocardial injury. To document the long term heart metal ion concentrations, a validated inductively coupled plasma mass spectroscopy (ICP-MS) method was needed. The method utilized a closed-vessel microwave digestion system to digest the samples. An ICP-MS method utilizing Universal Cell Technology was used to determine our target analyte concentrations. Accuracy was verified using reference materials. Precision, sensitivity, recovery and linearity studies were performed. This method was used to establish a reference range for a non-implant containing cohort of 80 autopsy human heart tissues RESULTS: This method demonstrated an analytic measurement range of 0.5-100ng/mL for each element. Accuracy was within ±10% of target value for each element. Within-run precision for each element was below 20% CV. The chromium, vanadium and cobalt concentrations (mean±SD) were 0.1523±0.2157μg/g, 0.0094±0.0211μg/g and 0.1039±0.1305μg/g respectively in 80 non-implant containing human heart tissue samples. This method provides acceptable recovery of the chromium, cobalt and vanadium in heart tissue; allowing assessment of the effects of metallic joint prosthesis on myocardial health. Copyright © 2017 Elsevier GmbH. All rights reserved.

Hg speciation by differential photochemical vapor generation at UV-B and UV-C wavelengths

USDA-ARS?s Scientific Manuscript database

Mercury speciation was accomplished by differential photochemical reduction at two UV wavelengths; the resulting Hg(O) vapor was quantified by atomic fluorescence spectrometry. After microwave digestion and centrifugation, analyte solutions were mixed with 20% (v/v) formic acid in a reactor coil, an...

Review of Radar Absorbing Materials

DTIC Science & Technology

2005-01-01

Symposium, 1990. AP-S. Merging technologies for the 90’s. Digest 1990, 3, 1212. (30) Nortier, J. R., Van der Neut , C.A., Baker, D.E. Microwave Journal...1987, 219. (31) Kasevich, R. S.; Broderick, F., US Patent 5223849. 1993. (32) Van Der Plas, G., Barel, A., Schweicher, E. Antennas and Propagation

Effect of Heating Method on Alteration of Protein Molecular Structure in Flaxseed: Relationship with Changes in Protein Subfraction Profile and Digestion in Dairy Cows.

PubMed

Ahmad Khan, Nazir; Booker, Helen; Yu, Peiqiang

2015-02-04

This study evaluated the effect of heating methods on alteration of protein molecular structure in flaxseed (Linum usitatissimum L.) in relation to changes in protein subfraction profile and digestion in dairy cows. Seeds from two flaxseed varieties, sampled from two replicate plots at two locations, were evaluated. The seeds were either maintained in their raw state or heated in an air-draft oven (dry heating) or autoclave (moist heating) for 60 min at 120 °C or by microwave irradiation (MIR) for 5 min. Compared to raw seeds, moist heating decreased (P < 0.05) soluble protein (SP) content [56.5 ± 5.55 to 25.9 ± 6.16% crude protein (CP)] and increased (P < 0.05) rumen undegraded protein (RUP) content (36.0 ± 5.19 to 46.9 ± 2.72% CP) and intestinal digestibility of RUP (61.0 ± 2.28 to 63.8 ± 2.67% RUP). Dry heating did not alter (P > 0.05) the protein subfraction profile and rumen degradation kinetics, whereas MIR increased (P < 0.05) the RUP content from 36.0 ± 5.19 to 40.4 ± 4.67% CP. The MIR and dry heating did not alter (P > 0.05) the amide I to amide II ratio, but moist heating decreased (P < 0.05) both the amide I to amide II ratio and α-helix-to-β-sheet ratio. Regression equations based on protein molecular spectral intensities provided high prediction power for estimation of heat-induced changes in SP (R 2 = 0.62), RUP (R 2 = 0.71), and intestinal digestibility of RUP (R 2 = 0.72). Overall, heat-induced changes in protein nutritive value and digestion were strongly associated with heat-induced alteration in protein molecular structures.

Determination of total arsenic in fish by hydride-generation atomic absorption spectrometry: method validation, traceability and uncertainty evaluation

NASA Astrophysics Data System (ADS)

Nugraha, W. C.; Elishian, C.; Ketrin, R.

2017-03-01

Fish containing arsenic compound is one of the important indicators of arsenic contamination in water monitoring. The high level of arsenic in fish is due to absorption through food chain and accumulated in their habitat. Hydride generation (HG) coupled with atomic absorption spectrometric (AAS) detection is one of the most popular techniques employed for arsenic determination in a variety of matrices including fish. This study aimed to develop a method for the determination of total arsenic in fish by HG-AAS. The method for sample preparation from American of Analytical Chemistry (AOAC) Method 999.10-2005 was adopted for acid digestion using microwave digestion system and AOAC Method 986.15 - 2005 for dry ashing. The method was developed and validated using Certified Reference Material DORM 3 Fish Protein for trace metals for ensuring the accuracy and the traceability of the results. The sources of uncertainty of the method were also evaluated. By using the method, it was found that the total arsenic concentration in the fish was 45.6 ± 1.22 mg.Kg-1 with a coverage factor of equal to 2 at 95% of confidence level. Evaluation of uncertainty was highly influenced by the calibration curve. This result was also traceable to International Standard System through analysis of Certified Reference Material DORM 3 with 97.5% of recovery. In summary, it showed that method of preparation and HG-AAS technique for total arsenic determination in fish were valid and reliable.

Anaerobic digestion of organic fraction of municipal solid waste combining two pretreatment modalities, high temperature microwave and hydrogen peroxide

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

Shahriari, Haleh, E-mail: haleh.shahriari@gmail.com; Warith, Mostafa; Hamoda, Mohamed

2012-01-15

Highlights: Black-Right-Pointing-Pointer Microwave and H{sub 2}O{sub 2} pretreatment were studied to enhance anaerobic digestion of organic waste. Black-Right-Pointing-Pointer The whole waste pretreated at 115 Degree-Sign C or 145 Degree-Sign C had the highest biogas production. Black-Right-Pointing-Pointer Biogas production of the whole waste decreased at 175 Degree-Sign C due to formation of refractory compounds. Black-Right-Pointing-Pointer Pretreatment to 145 Degree-Sign C and 175 Degree-Sign C were the best when considering only the free liquid fraction. Black-Right-Pointing-Pointer H{sub 2}O{sub 2} pretreatment had a lag phase and the biogas production was not higher than MW pretreated samples. - Abstract: In order to enhance anaerobicmore » digestion (AD) of the organic fraction of municipal solid waste (OFMSW), pretreatment combining two modalities, microwave (MW) heating in presence or absence of hydrogen peroxide (H{sub 2}O{sub 2}) were investigated. The main pretreatment variables affecting the characteristics of the OFMSW were temperature (T) via MW irradiation and supplemental water additions of 20% and 30% (SWA20 and SW30). Subsequently, the focus of this study was to evaluate mesophilic batch AD performance in terms of biogas production, as well as changes in the characteristics of the OFMSW post digestion. A high MW induced temperature range (115-175 Degree-Sign C) was applied, using sealed vessels and a bench scale MW unit equipped with temperature and pressure controls. Biochemical methane potential (BMP) tests were conducted on the whole OFMSW as well as the liquid fractions. The whole OFMSW pretreated at 115 Degree-Sign C and 145 Degree-Sign C showed 4-7% improvement in biogas production over untreated OFMSW (control). When pretreated at 175 Degree-Sign C, biogas production decreased due to formation of refractory compounds, inhibiting the digestion. For the liquid fraction of OFMSW, the effect of pretreatment on the cumulative biogas production (CBP) was more pronounced for SWA20 at 145 Degree-Sign C, with a 26% increase in biogas production after 8 days of digestion, compared to the control. When considering the increased substrate availability in the liquid fraction after MW pretreatment, a 78% improvement in biogas production vs. the control was achieved. Combining MW and H{sub 2}O{sub 2} modalities did not have a positive impact on OFMSW stabilization and enhanced biogas production. In general, all samples pretreated with H{sub 2}O{sub 2} displayed a long lag phase and the CBP was usually lower than MW irradiated only samples. First order rate constant was calculated.« less

Improvement of microwave-assisted digestion of milk powder with diluted nitric acid using oxygen as auxiliary reagent

NASA Astrophysics Data System (ADS)

Bizzi, Cezar A.; Barin, Juliano S.; Garcia, Edivaldo E.; Nóbrega, Joaquim A.; Dressler, Valderi L.; Flores, Erico M. M.

2011-05-01

The feasibility of using diluted HNO 3 solutions under oxygen pressure for decomposition of whole and non-fat milk powders and whey powder samples has been evaluated. Digestion efficiency was evaluated by determining the carbon content in solution (digests) and the determination of Ca, Cd, Cu, Fe, K, Mg, Mn, Mo, Na, Pb and Zn was performed by inductively coupled plasma optical emission spectrometry and Hg by chemical vapor generation coupled to inductively coupled plasma mass spectrometry. Samples (up to 500 mg) were digested using HNO 3 solutions (1 to 14 mol L - 1 ) and the effect of oxygen pressure was evaluated between 2.5 and 20 bar. It was possible to perform the digestion of 500 mg of milk powder using 2 mol L - 1 HNO 3 with oxygen pressure ranging from 7.5 to 20 bar with resultant carbon content in digests lower than 1700 mg L - 1 . Using optimized conditions, less than 0.86 mL of concentrated nitric acid (14 mol L - 1 ) was enough to digest 500 mg of sample. The accuracy was evaluated by determination of metal concentrations in certified reference materials, which presented an agreement better than 95% (Student's t test, P < 0.05) for all the analytes.

[Determination of heavy metals in four traditional Chinese medicines by ICP-MS].

PubMed

Wen, Hui-Min; Chen, Xiao-Hui; Dong, Ting-Xia; Zhan, Hua-Qiang; Bi, Kai-Shun

2006-08-01

To establish a ICP-MS method for the determination of heavy metals, including As, Hg, Pb, Cd, in four traditional Chinese medicines. The samples were digested by closed-versel microwave. The four heavy metals were directly analyzed by ICP-MS. Select internal standard element in for the method by which the analyse signal drife is corrected by the signal of another element (internal standard elements) added to both the standard solution and sample. For all of the analyzed heary methals, the correlative coefficient of the calibration curves was over 0.999 2. The recovery rates of the procedure were 97.5%-108.0%, and its RSD was lower than 11.6%. This method was convenient, quick-acquired, accurate and highly sensitive. The method can be used for the quality control of trace elements in traditional Chinese medicines and for the contents determination of traditional Chinese medicines from different habitats and species.

Algal Proteins: Extraction, Application, and Challenges Concerning Production

PubMed Central

Bleakley, Stephen; Hayes, Maria

2017-01-01

Population growth combined with increasingly limited resources of arable land and fresh water has resulted in a need for alternative protein sources. Macroalgae (seaweed) and microalgae are examples of under-exploited “crops”. Algae do not compete with traditional food crops for space and resources. This review details the characteristics of commonly consumed algae, as well as their potential for use as a protein source based on their protein quality, amino acid composition, and digestibility. Protein extraction methods applied to algae to date, including enzymatic hydrolysis, physical processes, and chemical extraction and novel methods such as ultrasound-assisted extraction, pulsed electric field, and microwave-assisted extraction are discussed. Moreover, existing protein enrichment methods used in the dairy industry and the potential of these methods to generate high value ingredients from algae, such as bioactive peptides and functional ingredients are discussed. Applications of algae in human nutrition, animal feed, and aquaculture are examined. PMID:28445408

Anaerobic digestion of organic fraction of municipal solid waste combining two pretreatment modalities, high temperature microwave and hydrogen peroxide.

PubMed

Shahriari, Haleh; Warith, Mostafa; Hamoda, Mohamed; Kennedy, Kevin J

2012-01-01

In order to enhance anaerobic digestion (AD) of the organic fraction of municipal solid waste (OFMSW), pretreatment combining two modalities, microwave (MW) heating in presence or absence of hydrogen peroxide (H(2)O(2)) were investigated. The main pretreatment variables affecting the characteristics of the OFMSW were temperature (T) via MW irradiation and supplemental water additions of 20% and 30% (SWA20 and SW30). Subsequently, the focus of this study was to evaluate mesophilic batch AD performance in terms of biogas production, as well as changes in the characteristics of the OFMSW post digestion. A high MW induced temperature range (115-175°C) was applied, using sealed vessels and a bench scale MW unit equipped with temperature and pressure controls. Biochemical methane potential (BMP) tests were conducted on the whole OFMSW as well as the liquid fractions. The whole OFMSW pretreated at 115°C and 145°C showed 4-7% improvement in biogas production over untreated OFMSW (control). When pretreated at 175°C, biogas production decreased due to formation of refractory compounds, inhibiting the digestion. For the liquid fraction of OFMSW, the effect of pretreatment on the cumulative biogas production (CBP) was more pronounced for SWA20 at 145°C, with a 26% increase in biogas production after 8days of digestion, compared to the control. When considering the increased substrate availability in the liquid fraction after MW pretreatment, a 78% improvement in biogas production vs. the control was achieved. Combining MW and H(2)O(2) modalities did not have a positive impact on OFMSW stabilization and enhanced biogas production. In general, all samples pretreated with H(2)O(2) displayed a long lag phase and the CBP was usually lower than MW irradiated only samples. First order rate constant was calculated. Copyright © 2011 Elsevier Ltd. All rights reserved.

Determination of As, Cd, Hg and Pb in continuous use drugs and excipients by plasma-based techniques in compliance with the United States Pharmacopeia requirements

NASA Astrophysics Data System (ADS)

da Silva, Caroline Santos; Pinheiro, Fernanda Costa; do Amaral, Clarice Dias Britto; Nóbrega, Joaquim Araújo

2017-12-01

Some inorganic impurities are toxic to human health even when present at low concentrations and therefore must be carefully monitored in products as continuous use drugs. This work aimed the development of a simple microwave-assisted digestion procedure for different types of drugs and excipients and the analytical determination of elemental impurities according to the new regulations of the United States Pharmacopeia (USP) 232 and 233 using inductively coupled plasma optical emission spectrometry (ICP-OES) or inductively coupled plasma mass spectrometry (ICP-MS). Eight drugs samples and two excipients of different brands were microwave-assisted digested with inverse aqua regia. Addition and recovery experiments were performed according to J values, once permissible daily exposure value is specific for each element and estimated according to the maximum daily dose of drug indicated by the label. Samples were spiked with values of 1.5J in order to check accuracies for As, Cd, Hg, and Pb. Recoveries obtained by ICP-OES ranged from 75 to 148% and for ICP-MS ranged from 74 to 120%. The limits of detection for ICP-OES ranged from 0.4 to 17 mg kg- 1 and for ICP-MS from 7.4 to 41.6 μg kg- 1. Both analytical methods were adequate in terms of accuracies and sensitivities. Considering the maximum daily dose, all drugs samples and excipients contained As, Cd, Hg and Pb below the maximum limits stipulated by USP since all of them presented contents below respective limits of detection.

[Study on distribution of five heavy metal elements in different parts of Cordyceps sinensis by microwave digestion ICP-MS].

PubMed

Zhou, Li; Hao, Qing-Xiu; Wang, Sheng; Yang, Quan; Kang, Chuan-Zhi; Yang, Wan-Zhen; Guo, Lan-Ping

2017-08-01

The contents of five heavy metals (Cu, Pb, As, Cd, Hg) in 17 batches of Cordyceps sinensis were determined by microwave digestion-ICP-MS, and their distribution in C. sinensis were analyzed. The results showed that the contents of Cu, Pb, Cd and Hg in all batches were in accordance with the international standards of Chinese Medicine-Chinese Herbal Medicine Heavy Metal Limit, with their contents in the stroma higher than that in the caterpillar body, and the excess rate of As, which mainly concentrated in the caterpillar body part of C. sinensis, was 88.24%, as the content of As in the caterpillar body was 7 to 12 fold of that in the stroma. In this study, the distribution of five heavy metals in C. sinensis was clarified, and the existing problems of arsenic limit of heavy metal in C. sinensis were analyzed, and some suggestions were put forward. It is hoped that the reference standard can be provided for the limited standard of arsenic in C. sinensis. Copyright© by the Chinese Pharmaceutical Association.

Determination of sulfur in bovine serum albumin and L-cysteine using high-resolution continuum source molecular absorption spectrometry of the CS molecule

NASA Astrophysics Data System (ADS)

Andrade-Carpente, Eva; Peña-Vázquez, Elena; Bermejo-Barrera, Pilar

2016-08-01

In this study, the content of sulfur in bovine serum albumin and L-cysteine was determined using high-resolution continuum source molecular absorption spectrometry of the CS molecule, generated in a reducing air-acetylene flame. Flame conditions (height above the burner, measurement time) were optimized using a 3.0% (v/v) sulfuric acid solution. A microwave lab station (Ethos Plus MW) was used for the digestion of both compounds. During the digestion step, sulfur was converted to sulfate previous to the determination. Good repeatability (4-10%) and analytical recovery (91-106%) was obtained.

[Determination of 22 inorganic elements in different parts of Lantana camara by ICP-OES].

PubMed

Zhou, Wei-ming; Wang, Ru-yi; Chen, Liu-sheng; Huang, Chuan-bin

2014-09-01

To determine the contents of 22 inorganic elements in different parts of Lantana camara by inductively coupled plasma optical emission spectroscopy (ICP-OES). HNO3-H2 02 digested system was used to completely decomposed the organic compounds effectually by microwave digestion. 22 inorganic elements such as K, Ca, Mg, Fe, Al, Na, Zn, Mn and Cr were determined by ICP-OES under set up working conditions. The contents of K, Ca and Mg were the most in different parts of Lantana camrnara; The contents of K, Ca, Mg, Mn, Sr and Cu in the leaves of Lantana camara were more than that in the root and the branch. The contents of Fe and Na in the root of Lantana camara were more than that in the leaves and the branch. The contents of Pb and Cd were higher than the national standard and Cr had high content in different parts of Lantana camara. The determination method is quick, easy and accurate with high sensitivity,which can determine the contents of 22 inorganic elements accurately in different parts of Lantana camara.

Selenium analysis by an integrated microwave digestion-needle trap device with hydride sorption on carbon nanotubes and electrothermal atomic absorption spectrometry determination

NASA Astrophysics Data System (ADS)

Maratta Martínez, Ariel; Vázquez, Sandra; Lara, Rodolfo; Martínez, Luis Dante; Pacheco, Pablo

2018-02-01

An integrated microwave assisted digestion (MW-AD) - needle trap device (NTD) for selenium determination in grape pomace samples is presented. The NTD was filled with oxidized multiwall carbon nanotubes (oxMWCNTS) where Se hydrides were preconcentrated. Determination was carried out by flow injection-electrothermal atomic absorption spectrometry (FI-ETAAS). The variables affecting the system were established by a multivariate design (Plackett Burman), indicating that the following variables significantly affect the system: sample amount, HNO3 digestion solution concentration, NaBH4 volume and elution volume. A Box-Behnken design was implemented to determine the optimized values of these variables. The system improved Se atomization in the graphite furnace, since only trapped hydrides reached the graphite furnace, and the pyrolysis stage was eliminated according to the aqueous matrix of the eluate. Under optimized conditions the system reached a limit of quantification of 0.11 μg kg- 1, a detection limit of 0.032 μg kg- 1, a relative standard deviation of 4% and a preconcentration factor (PF) of 100, reaching a throughput sample of 5 samples per hour. Sample analysis show Se concentrations between 0.34 ± 0.03 μg kg- 1 to 0.48 ± 0.03 μg kg- 1 in grape pomace. This system provides minimal reagents and sample consumption, eliminates discontinuous stages between samples processing reaching a simpler and faster Se analysis.

Evaluation of sample preparation methods for the detection of total metal content using inductively coupled plasma optical emission spectrometry (ICP-OES) in wastewater and sludge

NASA Astrophysics Data System (ADS)

Dimpe, K. M.; Ngila, J. C.; Mabuba, N.; Nomngongo, P. N.

Heavy metal contamination exists in aqueous wastes and sludge of many industrial discharges and domestic wastewater, among other sources. Determination of metals in the wastewater and sludge requires sample pre-treatment prior to analysis because of certain challenges such as the complexity of the physical state of the sample, which may lead to wrong readings in the measurement. This is particularly the case with low analyte concentration to be detected by the instrument. The purpose of this work was to assess and validate the different sample preparation methods namely, hot plate and microwave-assisted digestion procedures for extraction of metal ions in wastewater and sludge samples prior to their inductively coupled plasma optical emission spectrometric (ICP-OES) determination. For the extraction of As, Al, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Zn, three acid mixtures, that is, HNO3/H2O2, HNO3/HClO4/H2O2 and aqua regia + H2O2, were evaluated. Influent wastewater spiked with the SRM (CWW-TM-B) was used for the optimization of acid mixtures affecting the extraction procedure. After sample digestion, the filtration capabilities of cellulose-acetate filter paper and the acrodisc syringe filter with the pore size of 0.45 μm were compared. In terms of performance, acrodisc syringe filter in terms of the improved recoveries obtained, was found to be the best filtration method compared to the filter paper. Based on the analytical results obtained, microwave-assisted digestion (MAD) using aqua regia + H2O2 mixture was found to be the most suitable method for extraction of heavy metals and major elements in all the sample matrices. Therefore, MAD using aqua regia + H2O2 mixture was used for further investigations. The precision of the developed MAD method expressed in terms of relative standard deviations (% RSD) for different metals was found to be <5%. The limits of detection (LOD) and limits of quantification (LOQ) ranged from 0.12% to 2.18 μg L-1 and 0.61% to 3.43 μg L-1, respectively. The accuracy of the developed method (MAD using aqua regia + H2O2) was verified by analyzing two SRMs (CWW-TM-A and CWW-TM-B) and the obtained results were in agreement with certified values with recoveries ranging from 80% to 104% for CWW-TM-A and 84% to 102% for CWW-TM-B. The accuracy of the developed method was verified also by the recovery test in the spiked sludge samples. The accuracy and spike recovery test for different metal ions were in the range 80-104% and 92-106%, respectively. The developed method was applied for extraction of the As, Al, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Zn in environmental samples, namely wastewater and sludge.

Multielemental composition of suet oil based on quantification by ultrawave/ICP-MS coupled with chemometric analysis.

PubMed

Jiang, Jun; Feng, Liang; Li, Jie; Sun, E; Ding, Shu-Min; Jia, Xiao-Bin

2014-04-10

Suet oil (SO) has been used commonly for food and medicine preparation. The determination of its elemental composition has became an important challenge for human safety and health owing to its possible contents of heavy metals or other elements. In this study, ultrawave single reaction chamber microwave digestion (Ultrawave) and inductively coupled plasma-mass spectrometry (ICP-MS) analysis was performed to determine 14 elements (Pb, As, Hg, Cd, Fe, Cu, Mn, Ti, Ni, V, Sr, Na, Ka and Ca) in SO samples. Furthermore, the multielemental content of 18 SO samples, which represented three different sources in China: Qinghai, Anhui and Jiangsu, were evaluated and compared. The optimal ultrawave digestion conditions, namely, the optimal time (35 min), temperature (210 °C) and pressure (90 bar), were screened by Box-Behnken design (BBD). Eighteen samples were successfully classified into three groups by principal component analysis (PCA) according to the contents of 14 elements. The results showed that all SO samples were rich in elements, but with significant differences corresponding to different origins. The outliers and majority of SO could be discriminated by PCA according to the multielemental content profile. The results highlighted that the element distribution was associated with the origins of SO samples. The proposed ultrawave digestion system was quite efficient and convenient, which could be mainly attributed to its high pressure and special high-throughput for the sample digestion procedure. Our established method could be useful for the quality control and standardization of elements in SO samples and products.

A fast and feasible method for Br and I determination in whole egg powder and its fractions by ICP-MS.

PubMed

Toralles, Isis Gonçalves; Coelho, Gilberto Silva; Costa, Vanize Cadeira; Cruz, Sandra Meinen; Flores, Erico Marlon Moraes; Mesko, Marcia Foster

2017-04-15

A method for Br and I determination in whole egg powder and its fractions (egg white and yolk) was developed by combining microwave-induced combustion (MIC) and inductively coupled plasma mass spectrometry (ICP-MS). Using the MIC method, 350mg of whole egg powder and its fractions were efficiently digested using 50mmolL -1 NH 4 OH as an absorbing solution. The limits of detection for Br and I using the MIC method followed by ICP-MS determination were 0.039 and 0.015μgg -1 , respectively. Using the proposed method, agreements with the reference values between 97 and 104% for Br and I were obtained by analysis of reference material NIST 8435. Finally, it was possible to observe that Br concentration (4.59-5.29μgg -1 ) was higher than I (0.150-2.28μgg -1 ) for all the evaluated samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Low gas flow inductively coupled plasma optical emission spectrometry for the analysis of food samples after microwave digestion.

PubMed

Nowak, Sascha; Gesell, Monika; Holtkamp, Michael; Scheffer, Andy; Sperling, Michael; Karst, Uwe; Buscher, Wolfgang

2014-11-01

In this work, the recently introduced low flow inductively coupled plasma optical emission spectrometry (ICP-OES) with a total argon consumption below 0.7 L/min is applied for the first time to the field of food analysis. One goal is the investigation of the performance of this low flow plasma compared to a conventional ICP-OES system when non-aqueous samples with a certain matrix are introduced into the system. For this purpose, arsenic is determined in three different kinds of fish samples. In addition several nutrients (K, Na, Mg, Ca) and trace metals (Co, Cu, Mn, Cd, Pb, Zn, Fe, and Ni) are determined in honey samples (acacia) after microwave digestion. The precision of the measurements is characterized by relative standard deviations (RSD) and compared to the corresponding precision values achieved using the conventional Fassel-type torch of the ICP. To prove the accuracy of the low flow ICP-OES method, the obtained data from honey samples are validated by a conventional ICP-OES. For the measurements concerning arsenic in fish, the low flow ICP-OES values are validated by conventional Fassel-type ICP-OES. Furthermore, a certified reference material was investigated with the low gas flow setup. Limits of detection (LOD), according to the 3σ criterion, were determined to be in the low microgram per liter range for all analytes. Recovery rates in the range of 96-106% were observed for the determined trace metal elements. It was proven that the low gas flow ICP-OES leads to results that are comparable with those obtained with the Fassel-type torch for the analysis of food samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Analysis of nutrition-relevant trace elements in human blood and serum by means of total reflection X-ray fluorescence (TXRF) spectroscopy

NASA Astrophysics Data System (ADS)

Stosnach, Hagen; Mages, Margarete

2009-04-01

In clinical service laboratories, one of the most common analytical tasks with regard to inorganic traces is the determination of the nutrition-relevant elements Fe, Cu, Zn, and Se. Because of the high numbers of samples and the commercial character of these analyses, a time-consuming sample preparation must be avoided. In this presentation, the results of total reflection X-ray fluorescence measurements with a low-power system and different sample preparation procedures are compared with those derived from analysis with common methods like Atomic Absorption Spectroscopy (AAS) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS). The results of these investigations indicate that the optimal total reflection X-ray fluorescence analysis of the nutrition-relevant elements Fe, Cu, Zn, and Se can be performed by preparing whole blood and serum samples after dilution with ultrapure water and transferring 10 μl of internally standardized sample to an unsiliconized quartz glass sample carrier with subsequent drying in a laboratory oven. Suitable measurement time was found to be 600 s. The enhanced sample preparation by means of microwave or open digestion, in parts combined with cold plasma ashing, led to an improvement of detection limits by a factor of 2 for serum samples while for whole blood samples an improvement was only observed for samples prepared by means of microwave digestion. As the matrix elements P, S, Cl, and for whole blood Fe have a major influence on the detection limits, most probably a further enhancement of analytical quality requires the removal of the organic matrix. However, for the routine analysis of the nutrition-relevant elements, the dilution preparation was found to be sufficient.

U.S. Army Natick Soldier Research, Development & Engineering Center Testing Facilities And Equipment. Second Edition

DTIC Science & Technology

2011-04-01

30 Freeze Dryer ................................................. 30 High-Pressure Processing ............................... 30 Microwave Digestive...PP1 Power Platform Energy Analyzer ..... 41 Quintox Gas Combustion Analyzer .................... 41 FLIR Systems SC2000 Thermacam Handheld IR ...electronically directly to the contractor or printed on plotter paper , oak tag, or on CD. alloy steel, stainless steel, aluminum, copper and copper alloys

Determination of phosphorus in small amounts of protein samples by ICP-MS.

PubMed

Becker, J Sabine; Boulyga, Sergei F; Pickhardt, Carola; Becker, J; Buddrus, Stefan; Przybylski, Michael

2003-02-01

Inductively coupled plasma mass spectrometry (ICP-MS) is used for phosphorus determination in protein samples. A small amount of solid protein sample (down to 1 micro g) or digest (1-10 micro L) protein solution was denatured in nitric acid and hydrogen peroxide by closed-microvessel microwave digestion. Phosphorus determination was performed with an optimized analytical method using a double-focusing sector field inductively coupled plasma mass spectrometer (ICP-SFMS) and quadrupole-based ICP-MS (ICP-QMS). For quality control of phosphorus determination a certified reference material (CRM), single cell proteins (BCR 273) with a high phosphorus content of 26.8+/-0.4 mg g(-1), was analyzed. For studies on phosphorus determination in proteins while reducing the sample amount as low as possible the homogeneity of CRM BCR 273 was investigated. Relative standard deviation and measurement accuracy in ICP-QMS was within 2%, 3.5%, 11% and 12% when using CRM BCR 273 sample weights of 40 mg, 5 mg, 1 mg and 0.3 mg, respectively. The lowest possible sample weight for an accurate phosphorus analysis in protein samples by ICP-MS is discussed. The analytical method developed was applied for the analysis of homogeneous protein samples in very low amounts [1-100 micro g of solid protein sample, e.g. beta-casein or down to 1 micro L of protein or digest in solution (e.g., tau protein)]. A further reduction of the diluted protein solution volume was achieved by the application of flow injection in ICP-SFMS, which is discussed with reference to real protein digests after protein separation using 2D gel electrophoresis.The detection limits for phosphorus in biological samples were determined by ICP-SFMS down to the ng g(-1) level. The present work discusses the figure of merit for the determination of phosphorus in a small amount of protein sample with ICP-SFMS in comparison to ICP-QMS.

Assessment of microbial viability in municipal sludge following ultrasound and microwave pretreatments and resulting impacts on the efficiency of anaerobic sludge digestion.

PubMed

Cella, Monica Angela; Akgul, Deniz; Eskicioglu, Cigdem

2016-03-01

A range of ultrasonication (US) and microwave irradiation (MW) sludge pretreatments were compared to determine the extent of cellular destruction in micro-organisms within secondary sludge and how this cellular destruction translated to anaerobic digestion (AD). Cellular lysis/inactivation was measured using two microbial viability assays, (1) Syto 16® Green and Sytox® Orange counter-assay to discern the integrity of cellular membranes and (2) a fluorescein diacetate assay to understand relative enzymatic activity. A range of MW intensities (2.17-6.48 kJ/g total solids or TS, coinciding temperatures of 60-160 °C) were selected for comparison via viability assays; a range of corresponding US intensities (2.37-27.71 kJ/g TS, coinciding sonication times of 10-60 min at different amplitudes) were also compared to this MW range. The MW pretreatment of thickened waste activated sludge (tWAS) caused fourfold to fivefold greater cell death than non-pretreated and US-pretreated tWAS. The greatest microbial destruction occurred at MW intensities greater than 2.62 kJ/g TS of sludge, after which increased energy input via MW did not appear to cause greater microbial death. In addition, the optimal MW pretreatment (80 °C, 2.62 kJ/g TS) and corresponding US pretreatment (10 min, 60 % amplitude, 2.37 kJ/g TS) were administered to the tWAS of a mixed sludge and fed to anaerobic digesters over sludge retention times (SRTs) of 20, 14, and 7 days to compare effects of feed pretreatment on AD efficiency. The digester utilizing MW-pretreated tWAS (80 °C, 2.62 kJ/g TS) had the greatest fecal coliform removal (73.4 and 69.8 % reduction, respectively), greatest solids removal (44.2 % TS reduction), and highest overall methane production (248.2 L CH4/kg volatile solids) at 14- and 7-day SRTs. However, despite the fourfold to fivefold increases in cell death upon pretreatment, improvements from the digester fed MW-pretreated sludge were marginal (i.e., increases in efficiency of less than 3-10 %) and likely due to a smaller proportion of cells (10-20 %) in the polymeric network and mixed sludge fed to digesters.

The Levels of Trace Elements in Honey and Molasses Samples That Were Determined by ICP-OES After Microwave Digestion Method.

PubMed

Altundag, Huseyin; Bina, Emel; Altıntıg, Esra

2016-04-01

The aim of this study is determining the amount of Al, Cu, Fe, Mn, Ni, Pb and Zn in samples of molasses and honey which were gathered from the Sakarya and Istanbul regions. In this study, trace elements in 8 honey and 20 molasses samples with different botanic features were evaluated. The sample preparation phase was performed via wet decomposition method and microwave digestion system. The accuracy of the method was checked by the standard reference material; tea leaves (INCY-TL-1) and NIST-SRM 1515-apple. The concentrations of essential trace elements (TEs) were observed in the range of 1.61 ± 0.01-287.03 ± 1.07; 0.21 ± 0.01-11.04 ± 0.12; 0.35 ± 0.03-21.71 ± 0.02 and 1.19 ± 0.01-60.90 ± 1.09 μg g(-1) for iron, copper, manganese and zinc ions, respectively, while the toxic element contents were observed in the range of 0.82 ± 0.17-3.06 ± 0.03; 0.04 ± 0.05-1.96 ± 0.03 and 0.62 ± 0.01-120.52 ± 0.10 μg g(-1) for lead, nickel and aluminum ions, respectively. The concentrations of basic TEs iron, copper, manganese and zinc were determined as 3.87 ± 0.04-16.76 ± 0.06; 0.45 ± 0.03-2.15 ± 0.01; 0.13 ± 0.01-15.02 ± 0.14 and 0.80 ± 0.09-12.03 ± 0.19 for honey samples. Also, toxic metal, lead, nickel and aluminum values in the honey samples were determined as 1.21 ± 0.12-2.46 ± 0.21; 0.28 ± 0.14-0.88 ± 0.43 and 2.11 ± 0.02-8.04 ± 0.08. A comparison between gathered data and literature values has performed and it is determined that such findings are suitable with the literature.

The Evaluation on the Cadmium Net Concentration for Soil Ecosystems.

PubMed

Yao, Yu; Wang, Pei-Fang; Wang, Chao; Hou, Jun; Miao, Ling-Zhan

2017-03-12

Yixing, known as the "City of Ceramics", is facing a new dilemma: a raw material crisis. Cadmium (Cd) exists in extremely high concentrations in soil due to the considerable input of industrial wastewater into the soil ecosystem. The in situ technique of diffusive gradients in thin film (DGT), the ex situ static equilibrium approach (HAc, EDTA and CaCl2), and the dissolved concentration in soil solution, as well as microwave digestion, were applied to predict the Cd bioavailability of soil, aiming to provide a robust and accurate method for Cd bioavailability evaluation in Yixing. Moreover, the typical local cash crops-paddy and zizania aquatica-were selected for Cd accumulation, aiming to select the ideal plants with tolerance to the soil Cd contamination. The results indicated that the biomasses of the two applied plants were sufficiently sensitive to reflect the stark regional differences of different sampling sites. The zizania aquatica could effectively reduce the total Cd concentration, as indicated by the high accumulation coefficients. However, the fact that the zizania aquatica has extremely high transfer coefficients, and its stem, as the edible part, might accumulate large amounts of Cd, led to the conclusion that zizania aquatica was not an ideal cash crop in Yixing. Furthermore, the labile Cd concentrations which were obtained by the DGT technique and dissolved in the soil solution showed a significant correlation with the Cd concentrations of the biota accumulation. However, the ex situ methods and the microwave digestion-obtained Cd concentrations showed a poor correlation with the accumulated Cd concentration in plant tissue. Correspondingly, the multiple linear regression models were built for fundamental analysis of the performance of different methods available for Cd bioavailability evaluation. The correlation coefficients of DGT obtained by the improved multiple linear regression model have not significantly improved compared to the coefficients obtained by the simple linear regression model. The results revealed that DGT was a robust measurement, which could obtain the labile Cd concentrations independent of the physicochemical features' variation in the soil ecosystem. Consequently, these findings provide stronger evidence that DGT is an effective and ideal tool for labile Cd evaluation in Yixing.

The Evaluation on the Cadmium Net Concentration for Soil Ecosystems

PubMed Central

Yao, Yu; Wang, Pei-Fang; Wang, Chao; Hou, Jun; Miao, Ling-Zhan

2017-01-01

Yixing, known as the “City of Ceramics”, is facing a new dilemma: a raw material crisis. Cadmium (Cd) exists in extremely high concentrations in soil due to the considerable input of industrial wastewater into the soil ecosystem. The in situ technique of diffusive gradients in thin film (DGT), the ex situ static equilibrium approach (HAc, EDTA and CaCl2), and the dissolved concentration in soil solution, as well as microwave digestion, were applied to predict the Cd bioavailability of soil, aiming to provide a robust and accurate method for Cd bioavailability evaluation in Yixing. Moreover, the typical local cash crops—paddy and zizania aquatica—were selected for Cd accumulation, aiming to select the ideal plants with tolerance to the soil Cd contamination. The results indicated that the biomasses of the two applied plants were sufficiently sensitive to reflect the stark regional differences of different sampling sites. The zizania aquatica could effectively reduce the total Cd concentration, as indicated by the high accumulation coefficients. However, the fact that the zizania aquatica has extremely high transfer coefficients, and its stem, as the edible part, might accumulate large amounts of Cd, led to the conclusion that zizania aquatica was not an ideal cash crop in Yixing. Furthermore, the labile Cd concentrations which were obtained by the DGT technique and dissolved in the soil solution showed a significant correlation with the Cd concentrations of the biota accumulation. However, the ex situ methods and the microwave digestion-obtained Cd concentrations showed a poor correlation with the accumulated Cd concentration in plant tissue. Correspondingly, the multiple linear regression models were built for fundamental analysis of the performance of different methods available for Cd bioavailability evaluation. The correlation coefficients of DGT obtained by the improved multiple linear regression model have not significantly improved compared to the coefficients obtained by the simple linear regression model. The results revealed that DGT was a robust measurement, which could obtain the labile Cd concentrations independent of the physicochemical features’ variation in the soil ecosystem. Consequently, these findings provide stronger evidence that DGT is an effective and ideal tool for labile Cd evaluation in Yixing. PMID:28287500

Determination of mercury in ayurvedic dietary supplements that are not rasa shastra using the hydra-C direct mercury analyzer.

PubMed

Abdalla, Amir A; Smith, Robert E

2013-01-01

Mercury has been determined in Ayurvedic dietary supplements (Trifala, Trifala Guggulu, Turmeric, Mahasudarshan, Yograj, Shatawari, Hingwastika, Shatavari, and Shilajit) by inductively coupled plasma-mass spectrometry (ICP-MS) and direct mercury analysis using the Hydra-C direct mercury analyzer (Teledyne Leeman Labs Hudson, NH, USA). Similar results were obtained from the two methods, but the direct mercury analysis method was much faster and safer and required no microwave digestion (unlike ICP-MS). Levels of mercury ranged from 0.002 to 56  μ g/g in samples of dietary supplements. Standard reference materials Ephedra 3240 and tomato leaves that were from the National Institute of Standard and Technology (NIST) and dogfish liver (DOLT3) that was from the Canadian Research Council were analyzed using Hydra-C method. Average mercury recoveries were 102% (RSD% 0.0018), 100% (RSD% 0.0009), and 101% (RSD% 0.0729), respectively. Hydra-C method Limit Of Quantitation was 0.5 ng.

Determination of Mercury in Ayurvedic Dietary Supplements That Are Not Rasa Shastra Using the Hydra-C Direct Mercury Analyzer

PubMed Central

Abdalla, Amir A.; Smith, Robert E.

2013-01-01

Mercury has been determined in Ayurvedic dietary supplements (Trifala, Trifala Guggulu, Turmeric, Mahasudarshan, Yograj, Shatawari, Hingwastika, Shatavari, and Shilajit) by inductively coupled plasma-mass spectrometry (ICP-MS) and direct mercury analysis using the Hydra-C direct mercury analyzer (Teledyne Leeman Labs Hudson, NH, USA). Similar results were obtained from the two methods, but the direct mercury analysis method was much faster and safer and required no microwave digestion (unlike ICP-MS). Levels of mercury ranged from 0.002 to 56 μg/g in samples of dietary supplements. Standard reference materials Ephedra 3240 and tomato leaves that were from the National Institute of Standard and Technology (NIST) and dogfish liver (DOLT3) that was from the Canadian Research Council were analyzed using Hydra-C method. Average mercury recoveries were 102% (RSD% 0.0018), 100% (RSD% 0.0009), and 101% (RSD% 0.0729), respectively. Hydra-C method Limit Of Quantitation was 0.5 ng. PMID:23710181

Comparison of MP AES and ICP-MS for analysis of principal and selected trace elements in nitric acid digests of sunflower (Helianthus annuus).

PubMed

Karlsson, Stefan; Sjöberg, Viktor; Ogar, Anna

2015-04-01

The use of nitrogen as plasma gas for microwave plasma atomic emission spectroscopy (MP AES) is an interesting development in analytical science since the running cost can be significantly reduced in comparison to the inductively coupled argon plasma. Here, we evaluate the performance of the Agilent 4100 MP AES instrument for the analysis of principal metals (Ca, K, Mg, and Na), lithogenic metals (Al, Fe, and Mn) and selected trace metals (As, Ba, Cd, Co, Cr, Cu, Mo, Ni, Pb, V, and Zn) in nitric acid plant digests. The digests were prepared by microwave-assisted dissolution of dry plant material from sunflower (Helianthus annuus) in concentrated nitric acid. Comparisons are made with analysis of the same solutions with ICP-MS (Agilent 7500cx) using the octopole reaction system (ORS) in the collision mode for As, Fe, and V. The limits of detection were usually in the low µg L(-1) range and all principal and lithogenic metals were successfully determined with the MP AES and provided almost identical results with the ICP-MS. The same applies for the selected trace metals except for As, Co and Mo where the concentrations were below the detection limit with the MP AES. For successful analysis we recommend that (i) only atom lines are used, (ii) ionization is minimized (e.g. addition of CsNO3) and (iii) the use of internal standards should be considered to resolve spectral interferences. Copyright © 2014 Elsevier B.V. All rights reserved.

Bioaccesibility of Cylindrospermopsin from cooked fish muscle after the application of an in vitro digestion model and its bioavailability.

PubMed

Maisanaba, Sara; Saladino, Federica; Font, Guillermina; Jos, Ángeles; Cameán, Ana M; Meca, Giuseppe

2017-12-01

Humans can be exposed to cyanotoxins through the ingestion of contaminated water, food or beverages. In the present work, the bioaccesibility of Cylindrospermopsin (CYN), one of the most relevant cyanotoxins, was evaluated in a pure CYN solution and cooked CYN-contaminated fish muscles (20 μg/mL). An in vitro digestion model including the salivar, gastric, duodenal and colonic phases was performed, being each fraction analyzed by HPLC-MS-MS to evaluate CYN degradation. Moreover, Caco-2/TC7 cells were exposed to the digested duodenal and colonic phases to elucidate the final bioavailability of CYN in an approximation to the real human exposure scenario. The results revealed that CYN bioaccesibility decreased after the digestive process in all the cooked fish samples. The most drastic reductions were observed after lactic acid bacteria exposure. Thus, the highest bioaccesibility values were obtained in fish cooked by steaming (12.5%) and broiling (10.9%) meanwhile CYN was not detected in the colonic phase after boiling and microwaving. Regarding the duodenal and colonic availability, only in CYN pure digested solution the cyanotoxin was identified. The results obtained showed that digestion processes plays a very important role in the degradation of CYN, which should be considered when preparing a risk assessment of CYN. Copyright © 2017 Elsevier Ltd. All rights reserved.

Generation of organic acids and monosaccharides by hydrolytic and oxidative transformation of food processing residues.

PubMed

Fischer, Klaus; Bipp, Hans-Peter

2005-05-01

Carbohydrate-rich biomass residues, i.e. sugar beet molasses, whey powder, wine yeast, potato peel sludge, spent hops, malt dust and apple marc, were tested as starting materials for the generation of marketable chemicals, e.g. aliphatic acids, sugar acids and mono-/disaccharides. Residues were oxidized or hydrolyzed under acidic or alkaline conditions applying conventional laboratory digestion methods and microwave assisted techniques. Yields and compositions of the oxidation products differed according to the oxidizing agent used. Main products of oxidation by 30% HNO(3) were acetic, glucaric, oxalic and glycolic acids. Applying H(2)O(2)/CuO in alkaline solution, the organic acid yields were remarkably lower with formic, acetic and threonic acids as main products. Gluconic acid was formed instead of glucaric acid throughout. Reaction of a 10% H(2)O(2) solution with sugar beet molasses generated formic and lactic acids mainly. Na(2)S(2)O(8) solutions were very inefficient at oxidizing the residues. Glucose, arabinose and galactose were formed during acidic hydrolysis of malt dust and apple marc. The glucose content reached 0.35 g per gram of residue. Important advantages of the microwave application were lower reaction times and reduced reagent demands.

Facile MALDI-MS analysis of neutral glycans in NaOH-doped matrixes: microwave-assisted deglycosylation and one-step purification with diamond nanoparticles.

PubMed

Tzeng, Yan-Kai; Chang, Cheng-Chun; Huang, Chien-Ning; Wu, Chih-Che; Han, Chau-Chung; Chang, Huan-Cheng

2008-09-01

A streamlined protocol has been developed to accelerate, simplify, and enhance matrix-assisted laser desorption/ionization (MALDI) time-of-flight (TOF) mass spectrometry (MS) of neutral underivatized glycans released from glycoproteins. It involved microwave-assisted enzymatic digestion and release of glycans, followed by rapid removal of proteins and peptides with carboxylated/oxidized diamond nanoparticles, and finally treating the analytes with NaOH before mixing them with acidic matrix (such as 2,5-dihydroxybenzoic acid) to suppress the formation of both peptide and potassiated oligosaccharide ions in MS analysis. The advantages of this protocol were demonstrated with MALDI-TOF-MS of N-linked glycans released from ovalbumin and ribonuclease B.

Bioavailability and bioaccumulation characterization of essential and heavy metals contents in R. acetosa, S. oleracea and U. dioica from copper polluted and referent areas.

PubMed

Balabanova, Biljana; Stafilov, Trajče; Bačeva, Katerina

2015-01-01

Bioavailability of metals occurring in soil is the basic source of its accumulation in vegetables and herbs. The impact of soil pollution (due to urban and mining areas) on the food chain presents a challenge for many investigations. Availability of metals in a potentially polluted soil and their possible transfer and bioaccumulation in sorrel (Rumex acetosa), spinach (Spinacia oleracea) and common nettle (Urtica dioica), were examined. Microwave digestion was applied for total digestion of the plant tissues, while on the soil samples open wet digestion with a mixture of acids was applied. Three extraction methods were implemented for the bioavailable metals in the soil. Atomic emission spectrometry with inductively coupled plasma was used for determination of the total contents of 21 elements. Significant enrichments in agricultural soil for As, Pb and Zn (in urban area), Cd, Cu and Ni (in a copper mine area), compared with the respective values from European standards were detected. On the basis of three different extraction methods, higher availability was assumed for both lithogenic and anthropogenic elements. Translocation values >1 were obtained for As, Cd, Cu, Ni, Pb and Zn. Higher bioconcentrating value was obtained only for Cd, while the bioaccumulation values vary from 0.17 for Cd to 0.82 for Zn. The potential availability of hazardous metals in urban and mining soils is examined using DTPA-TEA-CaCl2 (urban) and HCl (Cu-mines areas). Our results suggested that S. oleracea and R. acetosa have a phytostabilization potential for Cd, Cu, Ni and Pb, while U. dioica only for Cu. R. acetosa has a potential for phytoextraction of Cd in urban and copper polluted areas.

Microwave assisted extraction for trace element analysis of plant materials by ICP-AES.

PubMed

Borkowska-Burnecka, J

2000-11-01

Application of microwave assisted extraction for the decomposition and dissolution of plant samples for trace metal determination by ICP-AES was examined. Dried onion, leaves of spinach beet and three reference materials CTA-OTL-1, CTA-VTL-2 and CL-1 were analyzed. Water, EDTA and hydrochloric acid (0.01, 0.10 and 1.0 M, respectively) were used as leaching solutions. The extraction efficiency was investigated by comparison of the results with those obtained after microwave wet digestion. HCl was found to be very suitable for quantitative extraction of B, Ba, Cd, Cu, Mn, Ni, Pb, Sr and Zn from the samples. For reference materials, the measured concentrations are well consistent with the certified values. The use of EDTA led to a complete extraction of B, Cd, Ni, Pb, Sr and Zn. Water was found to be a good leaching solution for boron. For extraction with HCl and EDTA, the RSD values for the concentrations measured were below 8% for most of the elements.

Comparison of autoclave, microwave, IR and UV-C stabilization of whole wheat flour branny fractions upon the nutritional properties of whole wheat bread.

PubMed

Demir, Mustafa Kürşat; Elgün, Adem

2014-01-01

In this study, whole wheat bread (WWB) prepared by whole wheat flour (WWF) which its branny fraction (35 ± 1% w/w whole flour) previously was stabilized with different processes. Branny fractions obtained by milling of two different Bezostaja-1 wheat samples (medium and high strong) at 65 ± 1% wheat flour extraction ratio. These fractions were stabilized using autoclave (AU), microwave (MW), infrared (IR) and ultraviolet-C (UV-C) methods. Then, WWF obtained by remixing of stabilized branny fraction (35 ± 1% w/w) and wheat flour (65 ± 1% w/w) of same wheat samples. Following this process, WWB was made from WWF. WWB were analyzed to determine their nutritional properties as crude protein, in vitro protein digestibility (IVPD), phytic acid content, total and HCl-extractable mineral concentrations, total phenolic content (TPC), antioxidant activity and total dietary fiber (TDF). While IVPD, TPC and antioxidant activity of WWB increased together with all stabilization methods, a significant (P < 0.05) loss was observed on phytic acid content of the WWB. Especially, UV-C and IR treatments had positive effects on TPC and antioxidant activity. AU and MW stabilization methods increased total mineral and HCl-extractable minerals of WWB. As a result of this study, all stabilization processes had an improving effect on nutritional characteristic of WWB.

Adsorption of trimethyltin, arsenic and zinc by palm oil mill sludge biochar prepared by microwave

NASA Astrophysics Data System (ADS)

Lam, Goh Ching; Sum, Klinsmann Ng Weng; Bashir, M. J. K.; Sethupathi, Sumathi

2017-04-01

Palm oil mill sludge (POS) is a type of solid left over after anaerobic digestion of palm oil mill effluent. At present, not much work has been reported in the literature on the feasibility of reutilizing this waste. In this study, biochar was prepared from POS. POS was pyrolyzed using microwave technique. Several types of palm oil mill sludge biochar (POSB) was produced by varying the microwave heating power from 100 W to 500 W and the pyrolysis holding time from 5 min to 25 min. The efficiency of the produced POSB was tested for Trimethyltin (TMT), arsenate (As), and zinc (Zn) adsorption capacity. The results of this study highlighted that POSB is able to adsorb Zn by the functional groups. The adsorption capacity of Zn was recorded as 44.5 mg/g. However, for TMT and As, the adsorption was very minimum i.e. about 3.3 mg/g and 5.6 mg/g respectively. It was suggested that poor performance of POSB was due to the anionic nature of TMT and As. It was concluded that microwave pyrolysis was not suitable for POSB preparation.

[Determination of 22 inorganic elements in different parts of Lantana camara by ICP-OES].

PubMed

Zhou, Wei-ming; Wang, Ru-yi; Chen, Liu-sheng; Huang, Chuan-bin

2014-10-01

To determine the contents of 22 inorganic elements in different parts of Lantana camara by inductively coupled plasma optical emission spectroscopy (ICP-OES). HNO3-H2O2 digested system was used to completely decompose the organic compounds effectually by microwave digestion. The 22 inorganic elements such as K, Ca, Mg, Fe, Al, Na, Zn, Mn and Cr were determined by ICP-OES under set up working conditions. The contents of K, Ca and Mg were the most in different parts of Lantana camara; The contents of K, Ca, Mg, Mn, Sr and Cu in the leaf were more those that in the root and branch; The contents of Fe, Na, Cr and Ni in the root were more than those in the leaf and branch; The contents of Mn, Zn, Sr and Cu in the branch were more than those in the root and the leaf; The contents of Pb and Cd were higher than the national standard and Cr had high content in different parts of Lantana camara. The determination method is quick, easy and accurate with high sensitivity, which can determine the contents of 22 inorganic elements accurately in different parts of Lantana camara.

Systems and methods for remote long standoff biometric identification using microwave cardiac signals

NASA Technical Reports Server (NTRS)

McGrath, William R. (Inventor); Talukder, Ashit (Inventor)

2012-01-01

Systems and methods for remote, long standoff biometric identification using microwave cardiac signals are provided. In one embodiment, the invention relates to a method for remote biometric identification using microwave cardiac signals, the method including generating and directing first microwave energy in a direction of a person, receiving microwave energy reflected from the person, the reflected microwave energy indicative of cardiac characteristics of the person, segmenting a signal indicative of the reflected microwave energy into a waveform including a plurality of heart beats, identifying patterns in the microwave heart beats waveform, and identifying the person based on the identified patterns and a stored microwave heart beats waveform.

Solid State Research.

DTIC Science & Technology

1996-08-01

Failure of Superconducting Microwave Filters: Investigation by Means of Thermal Imaging G. Hampel* P . Kolodner* P . L. Gammel* P . A. Polakos* E...deObaldia* P . M. Mankiewich* A. Anderson R. Slattery D. Zhang* G. C. Liang* C. F. Shih* Appl. Phys. Lett. 69, 571 (1996) Reflective Linearized...Digest Series, Vol. 6 (Optical Society of America, Washington, D.C., 1996), p . 626 Effects of Low-Temperature-Grown GaAs and AlGaAs on the Current

Evaluation of Trace Metal Content by ICP-MS Using Closed Vessel Microwave Digestion in Fresh Water Fish

PubMed Central

Jarapala, Sreenivasa Rao; Kandlakunta, Bhaskarachary; Thingnganing, Longvah

2014-01-01

The objective of the present study was to investigate trace metal levels of different varieties of fresh water fish using Inductively Coupled Plasma Mass Spectrophotometer after microwave digestion (MD-ICPMS). Fish samples were collected from the outlets of twin cities of Hyderabad and Secunderabad. The trace metal content in different varieties of analyzed fish were ranged from 0.24 to 1.68 mg/kg for Chromium in Cyprinus carpio and Masto symbollon, 0.20 to 7.52 mg/kg for Manganese in Labeo rohita and Masto symbollon, 0.006 to 0.07 mg/kg for Cobalt in Rastrelliger kanagurta and Pampus argenteus, 0.31 to 2.24 mg/kg for Copper in Labeo rohita and Penaeus monodon, 3.25 to 14.56 mg/kg for Zinc in Cyprinus carpio and Macrobrachium rosenbergii, and 0.01 to 2.05 mg/kg for Selenium in Rastrelliger kanagurta and Pampus argenteus, respectively. Proximate composition data for the different fishes were also tabulated. Since the available data for different trace elements for fish is scanty, here an effort is made to present a precise data for the same as estimated on ICP-MS. Results were in accordance with recommended daily intake allowance by WHO/FAO. PMID:24744789

The extraction of essential oil from patchouli leaves (Pogostemon cablin Benth) using microwave hydrodistillation and solvent-free microwave extraction methods

NASA Astrophysics Data System (ADS)

Putri, D. K. Y.; Kusuma, H. S.; Syahputra, M. E.; Parasandi, D.; Mahfud, M.

2017-12-01

Patchouli plant (Pogostemon cablin Benth) is one of the important essential oil-producing plant, contributes more than 50% of total exports of Indonesia’s essential oil. However, the extraction of patchouli oil that has been done in Indonesia is generally still used conventional methods that require enormous amount of energy, high solvent usage, and long time of extraction. Therefore, in this study, patchouli oil extraction was carried out by using microwave hydrodistillation and solvent-free microwave extraction methods. Based on this research, it is known that the extraction of patchouli oil using microwave hydrodistillation method with longer extraction time (240 min) only produced patchouli oil’s yield 1.2 times greater than solvent-free microwave extraction method which require faster extraction time (120 min). Otherwise the analysis of electric consumption and the environmental impact, the solvent-free microwave extraction method showed a smaller amount when compared with microwave hydrodistillation method. It is conclude that the use of solvent-free microwave extraction method for patchouli oil extraction is suitably method as a new green technique.

A new separation and preconcentration method for selenium in some foods using modified silica gel with 2,6-diamino-4-phenil-1,3,5-triazine.

PubMed

Mendil, Durali; Demirci, Zafer; Uluozlu, Ozgur Dogan; Tuzen, Mustafa; Soylak, Mustafa

2017-04-15

A novel and simple solid phase extraction method was improved and recommended for selenium. Silica gel was modified with 2,6-diamino-4-phenil-1,3,5-triazine and characterized by FTIR, SEM and elemental analysis and used adsorbent for column solid phase extraction of selenium ions. The experimental parameters (pH, flow rates, amounts of the modified silica gel, concentration and type of eluent, volume of sample, etc.) on the recoveries of selenium were optimized. Standard reference materials were analyzed for validation of method. The present method was successfully applied to the detection of total selenium in water and microwave digested some food samples with quantitative recoveries (> 95%). The relative standard deviations were<8%. Matrix influences were not observed. The adsorption capacity of modified silica gel was 5.90mgg -1 . The LOD was 0.015μgL -1 . Enrichment factor was obtained as 50 for the introduced method. Copyright © 2016 Elsevier Ltd. All rights reserved.

Microwave digestion-assisted HFO/biochar adsorption to recover phosphorus from swine manure.

PubMed

Zhang, Tao; Xu, Haoyu; Li, Huanhuan; He, Xinyue; Shi, Yuanji; Kruse, Andrea

2018-04-15

A sustainable management option for dealing with waste straw is to pyrolyze it to create biochar, which can then be used as a sorbent in pollution treatments, such as the recovery of phosphorus (P) from swine manure. However, the inability to directly capture soluble organic P (OP) and sparingly soluble P and the low selectivity of biochar remain key issues in this process. To overcome these, we investigated a microwave (MW) digestion pretreatment with a HFO/biochar adsorption process. The MW digestion-assisted treatment showed good performance for the solubilization of OP and sparingly soluble P. Optimized conditions (temperature=348K, time=45min, H 2 O 2 =3mL/30mL, HCl=0.13%) achieved an inorganic phosphorus (IP) release ratio of 83.98% and a total phosphorus (TP) release ratio of 91.83%. The P adsorption on the HFO/biochar was confirmed to follow pseudo-second-order kinetics, indicating that the P adsorption process was mainly controlled by chemical processes. The Freundlich model offered the best fit to the experimental data. The maximum amount of P adsorbed on HFO/biochar was in the range of 51.71-56.15mg/g. Thermodynamic calculations showed that the P adsorption process was exothermic, spontaneous, and increased the disorder in the system. Saturated adsorbed HFO/biochar was able to continually release P and was most suitable for use in an alkaline soil. The amount of P released from saturated adsorbed HFO/biochar reached 8.16mg/g after five interval extractions. A P mass balance indicated that 8.76% of the TP was available after the solubilization, capture, and recovery processes. Copyright © 2017 Elsevier B.V. All rights reserved.

Effects of soil characteristics on grape juice nutrient concentrations and other grape quality parameters in Shiraz

NASA Astrophysics Data System (ADS)

Concepción Ramos, Maria; Romero, Maria Paz

2017-04-01

This study investigated the response of grapes to soil properties in the variety Shiraz (SH) cultivated in the Costers de Segre Designation of Origin (NE, Spain). The research was carried out in two areas with differences in vigor, which was examined using the Normalized Difference Vegetation Index (NDVI). Soil properties such as organic matter content, pH, electrical conductivity and nutrients (N, P, K, Ca, Mg, Cu, Zn and Mn) were analysed in the two areas. Soil analyses were limited to the upper 40 cm. Soil N-NO3 was measured in 2M KCl extracts. Assimilable phosphorus was analysed by extraction with 0.5 M NaHCO3 at pH 8.5 using the Olsen method. The available K, Ca and Mg were evaluated in hemaaxinecobalt trichloride extracts and the available fraction of Cu, Zn, Mn and Fe in DTPA- trietanolamine extracts, by spectroscopy atomic emission/absorption. Berry grapes were collected at maturity. Nutrients in grape juice (K, Ca, Mg Cu, Zn, Mn and Fe) were determined after a microwave hydrogen peroxide digestion in a closed vessel microwave digestion system and measured by spectroscopy. Other grape properties that determine grape quality such as pH, berry weight and sugar content were analysed using the methods proposed by the OIV. Differences in soil properties were observed between plots, which determined the differences in vigour. The vines with lower vigour were grown in the soils with higher pH, electrical conductivity and silt content, which had in addition higher Ca, Mg and K available levels as well as higher levels of Fe and Mn than the soil in which vines had higher vigour. However, the available fraction of Cu and Zn was smaller. Similar differences in nutrient concentration in the berry were observed for all nutrients except for Cu. Grape juice pH and total soluble solids (°Brix) were higher in the most vigorous vines. However, the differences in berry weight and total acidity at ripening were not significant. Keywords: acidity; berry weight; nutrients; pH; soil characteristics, sugar content.

A simple and sensitive vortex-assisted ionic liquid-dispersive microextraction and spectrophotometric determination of selenium in food samples.

PubMed

Bağda, Esra; Tüzen, Mustafa

2017-10-01

In the present study, a novel and eco-friendly vortex-assisted ionic liquid-based microextraction method was developed for the determination of selenium in food. The microextraction method is based on the liberation of iodine in the presence of selenium; the liberated iodine reacts with I - to form I 3 - . Anionic I 3 - reacts with cationic crystal violet dye, and the product is extracted into 1-hexyl-3-methylimidazolium hexafluorophosphate phase in the presence of Triton X-114. The proposed method is linear in the range of 2.0-70µgL -1 and has a detection limit of 9.8×10 -2 µgL -1 . Relative standard deviations were 3.67% and 2.89% for the five replicate measurements of 14 and 35µgL -1 Se(IV), respectively. The proposed method was successfully applied to different food samples (NIST SRM 2976 mussel tissue, pepper, ginger, wheat flour, red lentil, traditional soup, cornflour, cornstarch, and garlic) after microwave digestion. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effect of pre-treatment on physicochemical and structural properties, and the bioaccessibility of β-carotene in sweet potato flour.

PubMed

Trancoso-Reyes, Nalleli; Ochoa-Martínez, Luz A; Bello-Pérez, Luis A; Morales-Castro, Juliana; Estévez-Santiago, Rocío; Olmedilla-Alonso, Begoña

2016-06-01

The aim of this research was to evaluate the effect of microwave or steam pre-treatment of raw sweet potato on physicochemical and microstructural properties, and the bioaccessibility of β-carotene in sweet potato flour. This is the first report on using the in vitro digestion model suitable for food, as proposed in a consensus paper, to assess the bioaccessibility of β-carotene in sweet potato flour. The pre-treatments produced a rearrangement of the flour matrix (starch, protein and non-starch polysaccharides), which was greater by using microwaves (M6) conducting to a greater increase in the phase transition temperatures up to 4.14 °C, while the enthalpy presented the higher reduction (4.49 J/g), both parameters in respect to the control. The resistant starch fraction was not modified, with about 3% in all samples. Microwave (M6) and all the steam pre-treatments showed the higher bioaccessibility of β-carotene. This flour can be used in the development of new products with high β-carotene content. Copyright © 2016 Elsevier Ltd. All rights reserved.

Enhancement of sludge anaerobic biodegradability by combined microwave-H2O2 pretreatment in acidic conditions.

PubMed

Eswari, Parvathy; Kavitha, S; Kaliappan, S; Yeom, Ick-Tae; Banu, J Rajesh

2016-07-01

The aim of this study was to increase the sludge disintegration and reduce the cost of microwave (MW) pretreatment. Thermodynamic analysis of MW hydrolysis revealed the best fit with a first-order kinetic model at a specific energy of 18,600 kJ/kg total solids (TS). Combining H2O2 with MW resulted in a significant increment in solubilization from 30 to 50 % at 18,600 kJ/kg TS. The pH of H2O2-assisted MW-pretreated sludge (MW + H2O2) was in the alkaline range (pH 9-10), and it made the sludge unfavorable for subsequent anaerobic digestion and inhibits methane production. In order to nullify the alkaline effect caused by the MW + H2O2 combination, the addition of acid was considered for pH adjustment. H2O2-assisted MW-pretreated sludge in acidic conditions (MW + H2O2 + acid) showed a maximum methane production of 323 mL/g volatile solids (VS) than others during anaerobic biodegradability. A cost analysis of this study reveals that MW + H2O2 + acid was the most economical method with a net profit of 59.90 €/t of sludge.

Characterisation of particulate exposure during fireworks displays

NASA Astrophysics Data System (ADS)

Joly, Alexandre; Smargiassi, Audrey; Kosatsky, Tom; Fournier, Michel; Dabek-Zlotorzynska, Ewa; Celo, Valbona; Mathieu, David; Servranckx, René; D'amours, Réal; Malo, Alain; Brook, Jeffrey

2010-11-01

Little is known about the level and content of exposure to fine particles (PM 2.5) among persons who attend fireworks displays and those who live nearby. An evaluation of the levels of PM 2.5 and their elemental content was carried out during the nine launches of the 2007 Montréal International Fireworks Competition. For each event, a prediction of the location of the firework plume was obtained from the Canadian Meteorological Centre (CMC) of the Meteorological Service of Canada. PM 2.5 was measured continuously with a photometer (Sidepak™, TSI) within the predicted plume location ("predicted sites"), and integrated samples were collected using portable personal samplers. An additional sampler was located on a nearby roof ("fixed site"). The elemental composition of the collected PM 2.5 samples from the "predicted sites" was determined using both a non-destructive energy dispersive ED-XRF method and an ICP-MS method with a near-total microwave-assisted acid digestion. The elemental composition of the "fixed site" samples was determined by the ICP-MS with the near-total digestion method. The highest PM 2.5 levels reached nearly 10 000 μg m -3, roughly 1000 times background levels. Elements such as K, Cl, Al, Mg and Ti were markedly higher in plume-exposed filters. This study shows that 1) persons in the plume and in close proximity to the launch site may be exposed to extremely high levels of PM 2.5 for the duration of the display and, 2) that the plume contains specific elements for which little is known of their acute cardio-respiratory toxicity.

A Review of Microwave-Assisted Reactions for Biodiesel Production

PubMed Central

Nomanbhay, Saifuddin; Ong, Mei Yin

2017-01-01

The conversion of biomass into chemicals and biofuels is an active research area as trends move to replace fossil fuels with renewable resources due to society’s increased concern towards sustainability. In this context, microwave processing has emerged as a tool in organic synthesis and plays an important role in developing a more sustainable world. Integration of processing methods with microwave irradiation has resulted in a great reduction in the time required for many processes, while the reaction efficiencies have been increased markedly. Microwave processing produces a higher yield with a cleaner profile in comparison to other methods. The microwave processing is reported to be a better heating method than the conventional methods due to its unique thermal and non-thermal effects. This paper provides an insight into the theoretical aspects of microwave irradiation practices and highlights the importance of microwave processing. The potential of the microwave technology to accomplish superior outcomes over the conventional methods in biodiesel production is presented. A green process for biodiesel production using a non-catalytic method is still new and very costly because of the supercritical condition requirement. Hence, non-catalytic biodiesel conversion under ambient pressure using microwave technology must be developed, as the energy utilization for microwave-based biodiesel synthesis is reported to be lower and cost-effective. PMID:28952536

A Review of Microwave-Assisted Reactions for Biodiesel Production.

PubMed

Nomanbhay, Saifuddin; Ong, Mei Yin

2017-06-15

The conversion of biomass into chemicals and biofuels is an active research area as trends move to replace fossil fuels with renewable resources due to society's increased concern towards sustainability. In this context, microwave processing has emerged as a tool in organic synthesis and plays an important role in developing a more sustainable world. Integration of processing methods with microwave irradiation has resulted in a great reduction in the time required for many processes, while the reaction efficiencies have been increased markedly. Microwave processing produces a higher yield with a cleaner profile in comparison to other methods. The microwave processing is reported to be a better heating method than the conventional methods due to its unique thermal and non-thermal effects. This paper provides an insight into the theoretical aspects of microwave irradiation practices and highlights the importance of microwave processing. The potential of the microwave technology to accomplish superior outcomes over the conventional methods in biodiesel production is presented. A green process for biodiesel production using a non-catalytic method is still new and very costly because of the supercritical condition requirement. Hence, non-catalytic biodiesel conversion under ambient pressure using microwave technology must be developed, as the energy utilization for microwave-based biodiesel synthesis is reported to be lower and cost-effective.

Chemically coupled microwave and ultrasonic pre-hydrolysis of pulp and paper mill waste-activated sludge: effect on sludge solubilisation and anaerobic digestion.

PubMed

Tyagi, Vinay Kumar; Lo, Shang-Lien; Rajpal, Ankur

2014-05-01

The effects of alkali-enhanced microwave (MW; 50-175 °C) and ultrasonic (US) (0.75 W/mL, 15-60 min) pretreatments, on solubilisation and subsequent anaerobic digestion efficiency of pulp and paper mill waste-activated sludge, were investigated. Improvements in total chemical oxygen demand and volatile suspended solids (VSS) solubilisation were limited to 33 and 39 % in MW pretreatment only (175 °C). It reached 78 and 66 % in combined MW-alkali pretreatment (pH 12 + 175 °C), respectively. Similarly, chemical oxygen demand and VSS solubilisation were 58 and 37 % in US pretreatment alone (60 min) and it improved by 66 and 49 % after US-alkali pretreatment (pH 12 + 60 min), respectively. The biogas yield for US 60 min-alkali (pH 12)-pretreated sludge was significantly improved by 47 and 20 % over the control and US 60 reactors, respectively. The biogas generation for MW (150 °C)-alkali (pH 12)-pretreated sludge was only 6.3 % higher than control; however, it was 8.3 % lower than the MW (150 °C) reactor, which was due to the inhibition of anaerobic activity under harsh thermal-alkali treatment condition.

Pretreatment of Lignocellulosic Wastes to Improve Ethanol and Biogas Production: A Review

PubMed Central

Taherzadeh, Mohammad J.; Karimi, Keikhosro

2008-01-01

Lignocelluloses are often a major or sometimes the sole components of different waste streams from various industries, forestry, agriculture and municipalities. Hydrolysis of these materials is the first step for either digestion to biogas (methane) or fermentation to ethanol. However, enzymatic hydrolysis of lignocelluloses with no pretreatment is usually not so effective because of high stability of the materials to enzymatic or bacterial attacks. The present work is dedicated to reviewing the methods that have been studied for pretreatment of lignocellulosic wastes for conversion to ethanol or biogas. Effective parameters in pretreatment of lignocelluloses, such as crystallinity, accessible surface area, and protection by lignin and hemicellulose are described first. Then, several pretreatment methods are discussed and their effects on improvement in ethanol and/or biogas production are described. They include milling, irradiation, microwave, steam explosion, ammonia fiber explosion (AFEX), supercritical CO2 and its explosion, alkaline hydrolysis, liquid hot-water pretreatment, organosolv processes, wet oxidation, ozonolysis, dilute-and concentrated-acid hydrolyses, and biological pretreatments. PMID:19325822

Total arsenic and selenium analysis in Marcellus shale, high-salinity water, and hydrofracture flowback wastewater.

PubMed

Balaba, Ronald S; Smart, Ronald B

2012-11-01

Trace levels of arsenic and selenium can be toxic to living organisms yet their quantitation in high ionic strength or high salinity aqueous media is difficult due to the matrix interferences which can either suppress or enhance the analyte signal. A modified thiol cotton fiber (TCF) method employing lower flow rates and centrifugation has been used to remove the analyte from complex aqueous media and minimize the matrix interferences. This method has been tested using a USGS (SGR-1b) certified reference shale. It has been used to analyze Marcellus shale samples following microwave digestion as well as spiked samples of high salinity water (HSW) and flow back wastewater (WRF6) obtained from an actual gas well drilling operation. Quantitation of arsenic and selenium is carried out by graphite furnace atomic spectroscopy (GFAAS). Extraction of arsenic and selenium from Marcellus shale exposed to HSW and WRF6 for varying lengths of time is also reported. Copyright © 2012 Elsevier Ltd. All rights reserved.

Effects of Microgravity on Embryonic Quail Eye Development

NASA Technical Reports Server (NTRS)

Barrett, Joyce E.; Wells, Diane C.; Paulsen, Avelina Q.; Conrad, Gary W.

1997-01-01

Immunohistochemical methods were used to stain neurofilament protein in corneal nerves of Embryonic Day 16 (E16) quail eyes that had been fixed in 4% paraformaldehyde at room temperature for several months. Fixation was according to the methods used by the Mir 21/NASA 2 Avian Developmental Biology Flight Experiments for quail embryos incubated on the Mir Space Station. After fixation, corneas were pretreated to improve immunohistochemical visualization of neurofilaments. A sequential combination of three pretreatments [microwave heating in saline G, followed by extraction with sodium dodecyl sulfate (SDS) at 37 C, followed by digestion with hyaluronidase at 37 C], produced increased antibody staining of corneal nerve neurofilament proteins, compared with corneas subjected to no prior pretreatments. Darker nerve staining and increased numbers of fine branches were observed, together with lower background staining after such pretreatments. In contrast, use of any single pretreatment or pair of pretreatments resulted in only slight and inconsistent enhancement of nerve staining. Only the sequential combination of all three pretreatments resulted in consistently better nerve staining.

[Determination of 24 metal elements and their compounds in air of workplace by ICP-AES].

PubMed

Wang, Xiang; Qiu, Jianguo; Zhao, Zhonglin; Guo, Ying

2014-06-01

To establish a method for determination of the levels of 24 metal elements and their compounds in the air of workplace by inductively coupled plasma-atomic emission spectroscopy (ICP- AES). Sampling filters were digested by microwave, and diluted to 25 ml. Twenty-four elements (Mg, Ni, K, Mo, Zn, Ca, Ba, Pb, Mn, Cd, Cr, Co, Cu, Sr, Bi, Tl, Sn, Li, Sb, Zr, In, V, Y, and Be) were simultaneously measured by ICP-AES. The detection limits for 24 elements were 0.001∼0.029 mg/L; liner correlation coefficient r values were all equal to or above 0.9994; the relative standard derivations were less than 5%; the recovery rates were 91.2%∼103.9%; the degradation rates in 7 days were less than 9.7%. ICP-AES technique is a simple, rapid, accurate, and reliable method, which can be used to measure 24 metal elements and their compounds in the air of workplace.

Effects of drying processes on starch-related physicochemical properties, bioactive components and antioxidant properties of yam flours.

PubMed

Chen, Xuetao; Li, Xia; Mao, Xinhui; Huang, Hanhan; Wang, Tingting; Qu, Zhuo; Miao, Jing; Gao, Wenyuan

2017-06-01

The effects of five different drying processes, air drying (AD), sulphur fumigation drying (SFD), hot air drying (HAD), freeze drying (FD) and microwave drying (MWD) for yams in terms of starch-related properties and antioxidant activity were studied. From the results of scanning electron microscopy (SEM), polarized optical microscopy (POM), X-ray diffraction (XRD), and Fourier transform infrared (FT-IR), the MWD sample was found to contain gelatinized starch granules. The FD yam had more slow digestible (SDS) and resistant starches (RS) compared with those processed with other modern drying methods. The bioactive components and the reducing power of the dried yams, were lower than those of fresh yam. When five dried samples were compared by principal component analysis, the HAD and SFD samples were observed to have the highest comprehensive principal component values. Based on our results, HAD would be a better method for yam drying than the more traditional SFD. Copyright © 2016 Elsevier Ltd. All rights reserved.

Analytical Results for Municipal Biosolids Samples from a Monitoring Program near Deer Trail, Colorado (U.S.A.), 2007

USGS Publications Warehouse

Crock, J.G.; Smith, D.B.; Yager, T.J.B.; Berry, C.J.; Adams, M.G.

2008-01-01

Since late 1993, the Metro Wastewater Reclamation District of Denver (Metro District), a large wastewater treatment plant in Denver, Colorado, has applied Grade I, Class B biosolids to about 52,000 acres of nonirrigated farmland and rangeland near Deer Trail, Colorado (U.S.A.). In cooperation with the Metro District in 1993, the U.S. Geological Survey (USGS) began monitoring ground water at part of this site. In 1999, the USGS began a more comprehensive monitoring study of the entire site to address stakeholder concerns about the potential chemical effects of biosolids applications to water, soil, and vegetation. This more comprehensive monitoring program recently has been extended through 2010. Monitoring components of the more comprehensive study include biosolids collected at the wastewater treatment plant, soil, crops, dust, alluvial and bedrock ground water, and streambed sediment. Streams at the site are dry most of the year, so samples of streambed sediment deposited after rain were used to indicate surface-water effects. This report will present only analytical results for the biosolids samples collected at the Metro District wastewater treatment plant in Denver and analyzed during 2007. We have presented earlier a compilation of analytical results for the biosolids samples collected and analyzed for 1999 through 2006. More information about the other monitoring components is presented elsewhere in the literature. Priority parameters for biosolids identified by the stakeholders and also regulated by Colorado when used as an agricultural soil amendment include the total concentrations of nine trace elements (arsenic, cadmium, copper, lead, mercury, molybdenum, nickel, selenium, and zinc), plutonium isotopes, and gross alpha and beta activity. Nitrogen and chromium also were priority parameters for ground water and sediment components. In general, the objective of each component of the study was to determine whether concentrations of priority parameters (1) were higher than regulatory limits, (2) were increasing with time, or (3) were significantly higher in biosolids-applied areas than in a similar farmed area where biosolids were not applied. Previous analytical results indicate that the elemental composition of the biosolids from the Denver plant was consistent during 1999-2006 and this consistency continues with the samples for 2007; total concentrations of regulated trace elements remained consistently lower than the regulatory limits for the entire monitoring period. Our previously reported data (1999-2006) and data presented in this report were used to compile an inorganic-chemical biosolids signature that can be contrasted with the geochemical signature for this site. The biosolids signature and an understanding of the geology and hydrology of the site can be used to separate biosolids effects from natural geochemical effects. Elements of particular interest for a biosolids signature include bismuth, copper, silver, mercury, phosphorus, and silver. An alternative method of digestion of biosolids was also recently investigated, and the results are presented in this report. A microwave digestion using only nitric acid at controlled elevated temperature and pressure was tested to replace the much more time-consuming and labor-intensive, traditional four-acid, hotplate method for the preparation of solutions to be analyzed by inductively coupled plasma-mass spectrometry (ICP-MS). Elements of concern determined by ICP-MS following digestion include cadmium, copper, lead, molybdenum, nickel, and zinc. The microwave 'digestion' proved to be a strong acid leach, and it was less efficient at digesting the biosolids samples with consistently lower recoveries (compared to the four-acid digestion value) for most elements, but especially for the elements of concern - copper, nickel, and zinc. Other elements traditionally associated with the silicate or oxide minerals demonstrated low recoveries, especially titaniu

Accurate quantitation standards of glutathione via traceable sulfur measurement by inductively coupled plasma optical emission spectrometry and ion chromatography

PubMed Central

Rastogi, L.; Dash, K.; Arunachalam, J.

2013-01-01

The quantitative analysis of glutathione (GSH) is important in different fields like medicine, biology, and biotechnology. Accurate quantitative measurements of this analyte have been hampered by the lack of well characterized reference standards. The proposed procedure is intended to provide an accurate and definitive method for the quantitation of GSH for reference measurements. Measurement of the stoichiometrically existing sulfur content in purified GSH offers an approach for its quantitation and calibration through an appropriate characterized reference material (CRM) for sulfur would provide a methodology for the certification of GSH quantity, that is traceable to SI (International system of units). The inductively coupled plasma optical emission spectrometry (ICP-OES) approach negates the need for any sample digestion. The sulfur content of the purified GSH is quantitatively converted into sulfate ions by microwave-assisted UV digestion in the presence of hydrogen peroxide prior to ion chromatography (IC) measurements. The measurement of sulfur by ICP-OES and IC (as sulfate) using the “high performance” methodology could be useful for characterizing primary calibration standards and certified reference materials with low uncertainties. The relative expanded uncertainties (% U) expressed at 95% confidence interval for ICP-OES analyses varied from 0.1% to 0.3%, while in the case of IC, they were between 0.2% and 1.2%. The described methods are more suitable for characterizing primary calibration standards and certifying reference materials of GSH, than for routine measurements. PMID:29403814

Determination of Free and Total Carnitine and Choline in Infant Formulas and Adult Nutritional Products by UPLC/MS/MS: Single-Laboratory Validation, First Action 2014.04.

PubMed

Jing, Wei; Thompson, Joseph J; Jacobs, Wesley A; Salvati, Louis M

2015-01-01

A single-laboratory validation (SLV) has been performed for a method that simultaneously determines choline and carnitine in nutritional products by ultra performance LC (UPLC)/MS/MS. All 11 matrixes from the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) were tested. Depending on the sample preparation, either the added (free, with a water dilution and filtering) or total (after microwave digestion at 120°C in nitric acid and subsequent neutralization with ammonia) species can be detected. For nonmilk containing products, the total carnitine is almost always equal to the free carnitine. A substantial difference was noted between free and total choline in all products. All Standard Method Performance Requirements for carnitine and choline have been met. This report summarizes the material sent to the AOAC Expert Review Panel for SPIFAN nutrient methods for the review of this method, as well as some additional data from an internal validation. The method was granted AOAC First Action status for carnitine in 2014 (2014.04), but the choline data are also being presented. A comparison of choline results to those from other AOAC methods is given.

Toxic metal levels in cocoa powder and chocolate by ICP-MS method after microwave-assisted digestion.

PubMed

Lo Dico, Gianluigi Maria; Galvano, Fabio; Dugo, Giacomo; D'ascenzi, Carlo; Macaluso, Andrea; Vella, Antonio; Giangrosso, Giuseppe; Cammilleri, Gaetano; Ferrantelli, Vincenzo

2018-04-15

The Commission Regulation (EC) Regulation N. 488/2014, established the concentration limits for cadmium in specific products based on cocoa and chocolate products as from January 2019. Based on this information there is a need to determine ultratrace levels of elements that might be presents in cocoa and chocolate products. In this work, the concentrations of Arsenic, Antimony, Cadmium, Chromium, Lead, Selenium and Vanadium were evaluated in cocoa powder and chocolate by the validation of an ICP-MS method. Good selectivity/specificity, recovery, repeatability and within-laboratory reproducibility, LOD, LOQ, range of linearity, standard measurement uncertainty parameters for method validation were achieved, in accordance with Commission Regulation. The cocoa powder revealed the maximum metal concentrations of 0.303 ± 0.035 mg/kg for cadmium, 1.228 ± 0.146 mg/kg for lead and 0.094 ± 0.013 mg/kg for arsenic. A significant difference was found between cocoa powder and chocolate samples (p < .05). Copyright © 2017 Elsevier Ltd. All rights reserved.

Quantitative and qualitative studies of silica in different rice samples grown in north of Iran using UV-vis, XRD and IR spectroscopy techniques.

PubMed

Samadi-Maybodi, Abdolraouf; Atashbozorg, Ebrahim

2006-11-15

Silicon is an essential trace element and is found in vegetables, fruits, cereals, water, pasta and rice (Oryza sativa). In this work, the silica content of different types of rice grains were measured. Here, we used the heteropoly blue photometric method with a double beam UV-vis spectrophotometer to determine the amount of silicon in rice samples (n=7) that were collected in the north of Iran. The samples were digested with wet-ashing method by microwave-assisted heating and then treated with ammonium molybdate to produce a yellow color compound in acidic solution (ca. pH 1.2) and then reduced to give a heteropoly compound with a blue color. Analyses were performed using standard addition method and absorbance values were measured with double beam UV-vis spectrophotometer at lambda(max)=815nm. Results indicated that the silica content was 307-451mg/kg for the samples. X-ray diffraction patterns and infra-red spectra were obtained from rice samples without any sample treatment.

Recovery of failed solid-state anaerobic digesters.

PubMed

Yang, Liangcheng; Ge, Xumeng; Li, Yebo

2016-08-01

This study examined the performance of three methods for recovering failed solid-state anaerobic digesters. The 9-L digesters, which were fed with corn stover, failed at a feedstock/inoculum (F/I) ratio of 10 with negligible methane yields. To recover the systems, inoculum was added to bring the F/I ratio to 4. Inoculum was either added to the top of a failed digester, injected into it, or well-mixed with the existing feedstock. Digesters using top-addition and injection methods quickly resumed and achieved peak yields in 10days, while digesters using well-mixed method recovered slowly but showed 50% higher peak yields. Overall, these methods recovered 30-40% methane from failed digesters. The well-mixed method showed the highest methane yield, followed by the injection and top-addition methods. Recovered digesters outperformed digesters had a constant F/I ratio of 4. Slow mass transfer and slow growth of microbes were believed to be the major limiting factors for recovery. Copyright © 2016 Elsevier Ltd. All rights reserved.

Biological Effects of Nonionizing Electromagnetic Radiation. Volume 7, Number 2-4, July thru December 1982.

DTIC Science & Technology

1983-07-01

MICROWAVE IRRA- dichotomy in MW susceptibility between two strains DIATION ON MA%4MALIAN CELLS INCUBATED IN congenic at the H- 2 Tla region on chromosome 17...Marsden Hosp., Fulham Road, London or the system is tlerant to typically 2 )1 errors in SW 3, England); Jotes, C. H. Strahlentherapie 158(6): -he phases...A Biological Effects of Nonionizing Electromagnetic Radiation Volume VII. Number 2 -4 (July Thru Decemoer 1982) July 1983 A Digest of Current

QA/QC Guidance for Sampling and Analysis of Sediments, Water, and Tissues for Dredged Material Evaluations: Chemical Evaluations

DTIC Science & Technology

1995-04-01

J. Biochem. Physiol. 37:911-917. Bloom, N.S., E.A. Crecelius, and S . Berman . 1983. Determination of mercury in seawater at sub-nanogram per liter...procedure for determination of trace metal in seawater by atomic absorption spectrometry with electrothermal atomization. Anal. Chern. Acta 98:47-55...Nakashima, S ., R.E. Sturgeon, S.N. Willie, and S.S. Berman . 1988. Acid digestion of marine sample for trace element analysis using microwave heating

An Improved Rectenna for Wireless Power Transmission for Unmanned Air Vehicles

DTIC Science & Technology

2011-09-01

Ohno, “A Microwave Powered High Altitude Platform,” IEEE MTT- S Digest, 1988. [3] M. Mecham, “California’s PG&E links with startup on 200-megawatt...Theory and Techniques, vol. 40, no. 6, pp.1259–1266, June 1992. [23] H.-K. Chiou and I.- S . Chen, “ High -Efficiency Dual- Band On-chip Rectenna for...provides high efficiency, stable output power , and lightweight design. The analysis of rectenna design focuses on four subsystems: (1) the receiving

Wafer Scale Distributed Radio

DTIC Science & Technology

2009-07-01

equation, we can derive: ∆ flock = f0 2Q Ain j A (5.34) with Ain j and A , the relative amplitude of the injecting signal and the oscillator signal, both...center of the line (Ain j = A ), then the locking range is equal to 1250MHz for a 10GHz oscillation frequency. With the architecture previously described...resonator in 90nm CMOS. In 2008 IEEE MTT-S International Microwave Symposium Digest (2008), pp. 775–778. [27] MCLEAN, J . A re-examination of the fundamental

A time domain based method for the accurate measurement of Q-factor and resonance frequency of microwave resonators

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

Gyüre, B.; Márkus, B. G.; Bernáth, B.

2015-09-15

We present a novel method to determine the resonant frequency and quality factor of microwave resonators which is faster, more stable, and conceptually simpler than the yet existing techniques. The microwave resonator is pumped with the microwave radiation at a frequency away from its resonance. It then emits an exponentially decaying radiation at its eigen-frequency when the excitation is rapidly switched off. The emitted microwave signal is down-converted with a microwave mixer, digitized, and its Fourier transformation (FT) directly yields the resonance curve in a single shot. Being a FT based method, this technique possesses the Fellgett (multiplex) and Connesmore » (accuracy) advantages and it conceptually mimics that of pulsed nuclear magnetic resonance. We also establish a novel benchmark to compare accuracy of the different approaches of microwave resonator measurements. This shows that the present method has similar accuracy to the existing ones, which are based on sweeping or modulating the frequency of the microwave radiation.« less

Fast determination of trace elements in organic fertilizers using a cup-horn reactor for ultrasound-assisted extraction and fast sequential flame atomic absorption spectrometry.

PubMed

Teixeira, Leonel Silva; Vieira, Heulla Pereira; Windmöller, Cláudia Carvalhinho; Nascentes, Clésia Cristina

2014-02-01

A fast and accurate method based on ultrasound-assisted extraction in a cup-horn sonoreactor was developed to determine the total content of Cd, Co, Cr, Cu, Mn, Ni, Pb and Zn in organic fertilizers by fast sequential flame atomic absorption spectrometry (FS FAAS). Multivariate optimization was used to establish the optimal conditions for the extraction procedure. An aliquot containing approximately 120 mg of the sample was added to a 500 µL volume of an acid mixture (HNO3/HCl/HF, 5:3:3, v/v/v). After a few minutes, 500 µL of deionized water was added and eight samples were simultaneously sonicated for 10 min at 50% amplitude, allowing a sample throughput of 32 extractions per hour. The performance of the method was evaluated with a certified reference material of sewage sludge (CRM 029). The precision, expressed as the relative standard deviation, ranged from 0.58% to 5.6%. The recoveries of analytes were found to 100%, 109%, 96%, 92%, 101%, 104% and 102% for Cd, Cr, Cu, Mn, Ni, Pb and Zn, respectively. The linearity, limit of detection and limit of quantification were calculated and the values obtained were adequate for the quality control of organic fertilizers. The method was applied to the analysis of several commercial organic fertilizers and organic wastes used as fertilizers, and the results were compared with those obtained using the microwave digestion procedure. A good agreement was found between the results obtained by microwave and ultrasound procedures with recoveries ranging from 80.4% to 117%. Two organic waste samples were not in accordance with the Brazilian legislation regarding the acceptable levels of contaminants. © 2013 Published by Elsevier B.V.

78 FR 7939 - Energy Conservation Program: Test Procedures for Microwave Ovens (Active Mode)

Federal Register 2010, 2011, 2012, 2013, 2014

2013-02-04

...The U.S. Department of Energy (DOE) proposes to revise its test procedures for microwave ovens established under the Energy Policy and Conservation Act. The proposed amendments would add provisions for measuring the active mode energy use for microwave ovens, including both microwave-only ovens and convection microwave ovens. Specifically, DOE is proposing provisions for measuring the energy use of the microwave-only cooking mode for both microwave-only ovens and convection microwave ovens based on the testing methods in the latest draft version of the International Electrotechnical Commission Standard 60705, ``Household microwave ovens--Methods for measuring performance.'' DOE is proposing provisions for measuring the energy use of the convection-only cooking mode for convection microwave ovens based on the DOE test procedure for conventional ovens in our regulations. DOE is also proposing to calculate the energy use of the convection-microwave cooking mode for convection microwave ovens by apportioning the microwave-only mode and convection-only mode energy consumption measurements based on typical consumer use.

A rapid method for quantification of 242Pu in urine using extraction chromatography and ICP-MS

DOE PAGES

Gallardo, Athena Marie; Than, Chit; Wong, Carolyn; ...

2017-01-01

Occupational exposure to plutonium is generally monitored through analysis of urine samples. Typically, plutonium is separated from the sample and other actinides, and the concentration is determined using alpha spectroscopy. Current methods for separations and analysis are lengthy and require long count times. A new method for monitoring occupational exposure levels of plutonium has been developed, which requires fewer steps and overall less time than the alpha spectroscopy method. In this method, the urine is acidified, and a 239Pu internal standard is added. The urine is digested in a microwave oven, and plutonium is separated using an Eichrom TRU Resinmore » column. The plutonium is eluted, and the eluant is injected directly into the Inductively Coupled Plasma–Mass Spectrometer (ICP-MS). Compared to a direct “dilute and shoot” method, a 30-fold improvement in sensitivity is achieved. This method was validated by analyzing several batches of spiked samples. Based on these analyses, a combined standard uncertainty plot, which relates uncertainty to concentration, was produced. As a result, the MDA 95 was calculated to be 7.0 × 10 –7 μg L –1, and the Lc95 was calculated to be 3.5 × 10 –7 μg L –1 for this method.« less

Microwave-emitting rotor, separator apparatus including same, methods of operation and design thereof

DOEpatents

Meikrantz, David H.

2006-12-19

An apparatus for use in separating, at least in part, a mixture, including at least one chamber and at least one microwave generation device configured for communicating microwave energy into the at least one chamber is disclosed. The rotor assembly may comprise an electric generator for generating electricity for operating the microwave generation device. At least one microwave generation device may be positioned within a tubular interior shaft extending within the rotor assembly. At least a portion of the tubular interior shaft may be substantially transparent to microwave energy. Microwave energy may be emitted in an outward radial direction or toward an anticipated boundary surface defined between a mixture and a separated constituent thereof. A method including flowing a mixture through at least one chamber and communicating microwave energy into the at least one chamber while rotating same is disclosed. Methods of operating a centrifugal separator and design thereof are disclosed.

New data on the mobility of Pt emitted from catalytic converters.

PubMed

Fliegel, Daniel; Berner, Zsolt; Eckhardt, Detlef; Stüben, Doris

2004-05-01

The mobility and speciation of Pt was investigated in dust deposited in highway tunnels and in gully sediments. For this, a sequential extraction technique was used in combination with a microwave digestion procedure, followed by detection of Pt with high resolution ICP-MS. A digestion procedure using HNO(3)/HCl/H(2)O(2) was developed and its efficiency tested for environmental materials. Total Pt contents ranged from approximately 100 to 300 microg/kg. The high share of chemically mobile Pt in the tunnel dust (up to about 40%) indicates that Pt is predominantly emitted in a mobile form from the converter. The absence of a mobile fraction in the gully sediment is explained by the elution of Pt by run-off. Except for the mobile and easily mobilised fractions none of the other fractions of the sequential extraction contains Pt, neither in the dust samples nor in the gully sediment.

The function of digestive enzymes on Cu, Zn, and Pb release from soil in in vitro digestion tests.

PubMed

Li, Yi; Demisie, Walelign; Zhang, Ming-kui

2013-07-01

The bioaccessibility of soil heavy metals is the solubility of soil heavy metals in synthetic human digestive juice, which is usually determined using in vitro digestion test. To reveal the effects of digestive enzymes on soil heavy metals bioaccessibility, three representative in vitro digestion tests, Simple Bioaccessibility Extraction Test (SBET), Physiologically Based Extraction Test (PBET), and Simple Gastrointestinal Extraction Test (SGET), were chosen. The bioaccessibility of soil Cu, Zn, and Pb in each method were respectively evaluated with and without digestive enzymes, and the differences were compared. The results showed that the effects of digestive enzymes varied with different methods and elements. Because of digestive enzymes addition, the environmental change from acid gastric phase to neutral intestinal phase of PBET did not result in apparently decrease of the bioaccessibility of soil Cu. However, the solubility of soil Zn and Pb were pH-dependent. For SGET, when digestive enzymes were added, its results reflected more variations resulting from soil and element types. The impacts of digestive enzymes on heavy metal dissolution are mostly seen in the intestinal phase. Therefore, digestive enzyme addition is indispensable to the gastrointestinal digestion methods (PBET and SGET), while the pepsin addition is not important for the methods only comprised of gastric digestion (SBET).

Comparative evaluation of surface porosities in conventional heat polymerized acrylic resin cured by water bath and microwave energy with microwavable acrylic resin cured by microwave energy

PubMed Central

Singh, Sunint; Palaskar, Jayant N.; Mittal, Sanjeev

2013-01-01

Background: Conventional heat cure poly methyl methacrylate (PMMA) is the most commonly used denture base resin despite having some short comings. Lengthy polymerization time being one of them and in order to overcome this fact microwave curing method was recommended. Unavailability of specially designed microwavable acrylic resin made it unpopular. Therefore, in this study, conventional heat cure PMMA was polymerized by microwave energy. Aim and Objectives: This study was designed to evaluate the surface porosities in PMMA cured by conventional water bath and microwave energy and compare it with microwavable acrylic resin cured by microwave energy. Materials and Methods: Wax samples were obtained by pouring molten wax into a metal mold of 25 mm × 12 mm × 3 mm dimensions. These samples were divided into three groups namely C, CM, and M. Group C denotes conventional heat cure PMMA cured by water bath method, CM denotes conventional heat cure PMMA cured by microwave energy, M denotes specially designed microwavable acrylic denture base resin cured by microwave energy. After polymerization, each sample was scanned in three pre-marked areas for surface porosities using the optical microscope. As per the literature available, this instrument is being used for the first time to measure the porosity in acrylic resin. It is a reliable method of measuring area of surface pores. Portion of the sample being scanned is displayed on the computer and with the help of software area of each pore was measured and data were analyzed. Results: Conventional heat cure PMMA samples cured by microwave energy showed maximum porosities than the samples cured by conventional water bath method and microwavable acrylic resin cured by microwave energy. Higher percentage of porosities was statistically significant, but well within the range to be clinically acceptable. Conclusion: Within the limitations of this in-vitro study, conventional heat cure PMMA can be cured by microwave energy without compromising on its property such as surface porosity. PMID:24015000

Combination of alkaline and microwave pretreatment for disintegration of meat processing wastewater sludge.

PubMed

Erden, G

2013-01-01

Meat processing wastewater sludge has high organic content but it is very slow to degrade in biological processes. Anaerobic digestion may be a good alternative for this type of sludge when the hydrolysis, known to be the rate-limiting step of biological sludge anaerobic degradation, could be eliminated by disintegration. This investigation deals with disintegration of meat processing wastewater sludge. Microwave (MW) irradiation and combined alkaline pretreatment and MW irradiation were applied to sludge for disintegration purposes. Disintegration performance of the methods was evaluated with disintegration degree based on total and dissolved organic carbon calculations (DD(TOC)), and the solubilization of volatile solids (S(VS)) in the pretreated sludge. Optimum conditions were found to be 140 degrees C and 30 min for MW irradiation using response surface methodology (RSM) and pH = 13 for combined pretreatment. While DD(TOC) was observed as 24.6% and 54.9, S(VS) was determined as 8.54% and 42.5% for MW pretreated and combined pretreated sludge, respectively. The results clearly show that pre-conditioning of sludge with alkaline pretreatment played an important role in enhancing the disintegration efficiency of subsequent MW irradiation. Disintegration methods also affected the anaerobic biodegradability and dewaterability of sludge. An increase of 23.6% in biogas production in MW irradiated sludge was obtained, comparing to the raw sludge at the end of the 35 days of incubation. This increase was observed as 44.5% combined pretreatment application. While MW pretreatment led to a little improvement of the dewatering performance of sludge, in combined pretreatment NaOH deteriorates the sludge dewaterability.

Sulphur tracer experiments in laboratory animals using 34S-labelled yeast.

PubMed

Martínez-Sierra, J Giner; Moreno Sanz, F; Herrero Espílez, P; Marchante Gayón, J M; Rodríguez Fernández, J; García Alonso, J I

2013-03-01

We have evaluated the use of (34)S-labelled yeast to perform sulphur metabolic tracer experiments in laboratory animals. The proof of principle work included the selection of the culture conditions for the preparation of sulphur labelled yeast, the study of the suitability of this labelled yeast as sulphur source for tracer studies using in vitro gastrointestinal digestion and the administration of the (34)S-labelled yeast to laboratory animals to follow the fate and distribution of (34)S in the organism. For in vitro gastrointestinal digestion, the combination of sodium dodecyl sulphate-polyacrylamide gel electrophoresis and high-performance liquid chromatography and inductively coupled plasma mass spectrometry (HPLC-ICP-MS) showed that labelled methionine, cysteine and other low molecular weight sulphur-containing biomolecules were the major components in the digested extracts of the labelled yeast. Next, in vivo kinetic experiments were performed in healthy Wistar rats after the oral administration of (34)S-labelled yeast. The isotopic composition of total sulphur in tissues, urine and faeces was measured by double-focusing inductively coupled plasma mass spectrometry after microwave digestion. It was observed that measurable isotopic enrichments were detected in all samples. Finally, initial investigations on sulphur isotopic composition of serum and urine samples by HPLC-ICP-MS have been carried out. For serum samples, no conclusive data were obtained. Interestingly, chromatographic analysis of urine samples showed differential isotope enrichment for several sulphur-containing biomolecules.

Interaction of microwaves with carbon nanotubes to facilitate modification

NASA Technical Reports Server (NTRS)

Tour, James M. (Inventor); Dyke, Christopher A. (Inventor); Stephenson, Jason J. (Inventor); Yakobson, Boris I. (Inventor)

2011-01-01

The present invention is directed toward methods of crosslinking carbon nanotubes to each other using microwave radiation, articles of manufacture produced by such methods, compositions produced by such methods, and applications for such compositions and articles of manufacture. The present invention is also directed toward methods of radiatively modifying composites and/or blends comprising carbon nanotubes with microwaves, and to the compositions produced by such methods. In some embodiments, the modification comprises a crosslinking process, wherein the carbon nanotubes serve as a conduit for thermally and photolytically crosslinking the host matrix with microwave radiation.

Determination of free amino acids and 18 elements in freeze-dried strawberry and blueberry fruit using an Amino Acid Analyzer and ICP-MS with micro-wave digestion.

PubMed

Zhang, Hua; Wang, Zhen-Yu; Yang, Xin; Zhao, Hai-Tian; Zhang, Ying-Chun; Dong, Ai-Jun; Jing, Jing; Wang, Jing

2014-03-15

The objective of this study was to investigate the level of 18 trace elements of two freeze-dried samples from the Blueberry (Vaccinium corymbosum) and the Strawberry (Fragaria × Ananassa). The total free amino acid composition in the blueberry and strawberry was determined by an Amino Acid Analyzer. Eleven free amino acids were found in both berries. The trace elements in each dried fruit sample were determined by ICP-MS with microwave digestion. The linearity range of the standard curves was 0-1250.0 μg L(-1) (Mg, P, K, Ca),while in all cases, except for B, Na, Al, Cr, Mn, Fe, Ni, Cu, Zn, Se, Cd, Pb, Ge and As, which was 125.0 μg mL(-1), all related coefficients were above 0.9999; recovery was in the range of 79.0-106.8%. Minor concentrations of nutritional elements were found in each freeze-dried berry. In sum, the toxic trace element analysis found the content of toxic trace elements in each freeze-dried berry sample was safe for human consumption and that the overall quality of the blueberry surpassed that of the strawberry. The results certify that the two freeze-dried berries have potential for human consumption in value-added products and have a certain theoretical and practical significance. Crown Copyright © 2013. Published by Elsevier Ltd. All rights reserved.

Method and apparatus for selectively annealing heterostructures using microwave

NASA Technical Reports Server (NTRS)

Atwater, Harry A. (Inventor); Brain, Ruth A. (Inventor); Barmatz, Martin B. (Inventor)

1998-01-01

The present invention discloses a process for selectively annealing heterostructures using microwaves. A heterostructure, comprised of a material having higher microwave absorption and a material having lower microwave absorption, is exposed to microwaves in the cavity. The higher microwave absorbing material absorbs the microwaves and selectively heats while the lower microwave absorbing material absorbs small amounts of microwaves and minimally heats. The higher microwave absorbing material is thereby annealed onto the less absorbing material which is thermally isolated.

Method and apparatus for selectively annealing heterostructures using microwaves

NASA Technical Reports Server (NTRS)

Atwater, Harry A. (Inventor); Brain, Ruth A. (Inventor); Barmatz, Martin B. (Inventor)

1998-01-01

The present invention discloses a process for selectively annealing heterostructures using microwaves. A heterostructure, comprised of a material having higher microwave absorption and a material having lower microwave absorption, is exposed to microwaves in the cavity. The higher microwave absorbing material absorbs the microwaves and selectively heats while the lower microwave absorbing material absorbs small amounts of microwaves and minimally heats. The higher microwave absorbing material is thereby annealed onto the less absorbing material which is thermally isolated.

[Agreement between animal and vegetable protein digestibility measured in vivo and in vitro and its effect on the chemical score].

PubMed

Carias, D; Cioccia, A M; Hevia, P

1995-06-01

Protein digestibility is a key factor in the determination of protein quality using the chemical score. Since there are several methods available for determining protein digestibility the purpose of this study was to compare three methods in vitro (pH drop, pH stat and pepsin digestibility) and two methods in vivo (true and apparent digestibility in rats) in the determination of the protein digestibility of: casein, soy protein isolate, fish meal, black beans, corn meal and wheat flour. The results showed that in the case of highly digestible proteins all methods agreed very well. However, this agreement was much less apparent in the case of protein with digestibilities below 85%. As a result, the chemical score of these proteins varied substantially depending upon the method used to determine its digestibility. Thus, when the chemical score of the proteins analyzed was corrected by the true protein digestibility measured in rats, they ranked as: casein 83.56, soy 76.11, corn-beans mixtures (1:1) 58.14, fish meal 55.25, black beans 47.93, corn meal 46.06 and wheat flour 32.77. In contrast, when the chemical score of these proteins was corrected by the pepsin digestibility method, the lowest quality was assigned to fish meal. In summary, this results pointed out that for non conventional proteins of for known proteins which have been subjected to processing, protein digestibility should be measured in vivo.

Distribution of copper, iron, and zinc in biological samples (scalp hair, serum, blood, and urine) of Pakistani viral hepatitis (A-E) patients and controls.

PubMed

Kolachi, Nida Fatima; Kazi, Tasneem Gul; Afridi, Hassan Imran; Kazi, Naveed; Kandhro, Ghulam Abbas; Shah, Abdul Qadir; Baig, Jameel Ahmed; Wadhwa, Sham Kumar; Khan, Sumaira; Shah, Faheem; Jamali, Mohammad Khan; Arain, Mohammad Balal

2011-10-01

The aim of the present study was to compare the level of copper (Cu), iron (Fe) and zinc (Zn) in biological samples (serum, blood, urine, and scalp hair) of patients suffering from different viral hepatitis (A, B, C, D, and E; n = 521) of both gender age ranged 31-45 years. For comparative study, 255 age-matched control subjects, of both genders residing in the same city were selected as referents. The elements in the biological samples were analyzed by flame atomic absorption spectrophotometry, prior to microwave-assisted acid digestion. The validity and accuracy of the methodology was checked by using certified reference materials (CRMs) and with those values obtained by conventional wet acid digestion method on same CRMs. The results of this study showed that the mean values of Cu and Fe were higher in blood, sera, and scalp hair samples of hepatitis patients, while Zn level was found to be lower than age-matched control subjects. The urinary levels of these elements were found to be higher in the hepatitis patients than in the age-matched healthy controls (p < 0.05). These results are consistent with literature-reported data, confirming that the deficiency of zinc and hepatic iron and copper overload can directly cause lipid peroxidation and eventually hepatic damage.

Coupled microwave/photoassisted methods for environmental remediation.

PubMed

Horikoshi, Satoshi; Serpone, Nick

2014-11-05

The microwave-induced acceleration of photocatalytic reactions was discovered serendipitously in the late 1990s. The activity of photocatalysts is enhanced significantly by both microwave radiation and UV light. Particularly relevant, other than as a heat source, was the enigmatic phenomenon of the non-thermal effect(s) of the microwave radiation that facilitated photocatalyzed reactions, as evidenced when examining various model contaminants in aqueous media. Results led to an examination of the possible mechanism(s) of the microwave effect(s). In the present article we contend that the microwaves' non-thermal effect(s) is an important factor in the enhancement of TiO2-photoassisted reactions involving the decomposition of organic pollutants in model wastewaters by an integrated (coupled) microwave-/UV-illumination method (UV/MW). Moreover, such coupling of no less than two irradiation methods led to the fabrication and ultimate investigation of microwave discharged electrodeless lamps (MDELs) as optimal light sources; their use is also described. The review focuses on the enhanced activity of photocatalytic reactions when subjected to microwave radiation and concentrates on the authors' research of the past few years.

Digital communications: Microwave applications

NASA Astrophysics Data System (ADS)

Feher, K.

Transmission concepts and techniques of digital systems are presented; and practical state-of-the-art implementation of digital communications systems by line-of-sight microwaves is described. Particular consideration is given to statistical methods in digital transmission systems analysis, digital modulation methods, microwave amplifiers, system gain, m-ary and QAM microwave systems, correlative techniques and applications to digital radio systems, hybrid systems, digital microwave systems design, diversity and protection switching techniques, measurement techniques, and research and development trends and unsolved problems.

Apparatus and method for microwave processing of materials

DOEpatents

Johnson, A.C.; Lauf, R.J.; Bible, D.W.; Markunas, R.J.

1996-05-28

Disclosed is a variable frequency microwave heating apparatus designed to allow modulation of the frequency of the microwaves introduced into a furnace cavity for testing or other selected applications. The variable frequency heating apparatus is used in the method of the present invention to monitor the resonant processing frequency within the furnace cavity depending upon the material, including the state thereof, from which the workpiece is fabricated. The variable frequency microwave heating apparatus includes a microwave signal generator and a high-power microwave amplifier or a microwave voltage-controlled oscillator. A power supply is provided for operation of the high-power microwave oscillator or microwave amplifier. A directional coupler is provided for detecting the direction and amplitude of signals incident upon and reflected from the microwave cavity. A first power meter is provided for measuring the power delivered to the microwave furnace. A second power meter detects the magnitude of reflected power. Reflected power is dissipated in the reflected power load. 10 figs.

Sulfur-based absolute quantification of proteins using isotope dilution inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Lee, Hyun-Seok; Heun Kim, Sook; Jeong, Ji-Seon; Lee, Yong-Moon; Yim, Yong-Hyeon

2015-10-01

An element-based reductive approach provides an effective means of realizing International System of Units (SI) traceability for high-purity biological standards. Here, we develop an absolute protein quantification method using double isotope dilution (ID) inductively coupled plasma mass spectrometry (ICP-MS) combined with microwave-assisted acid digestion for the first time. We validated the method and applied it to certify the candidate protein certified reference material (CRM) of human growth hormone (hGH). The concentration of hGH was determined by analysing the total amount of sulfur in hGH. Next, the size-exclusion chromatography method was used with ICP-MS to characterize and quantify sulfur-containing impurities. By subtracting the contribution of sulfur-containing impurities from the total sulfur content in the hGH CRM, we obtained a SI-traceable certification value. The quantification result obtained with the present method based on sulfur analysis was in excellent agreement with the result determined via a well-established protein quantification method based on amino acid analysis using conventional acid hydrolysis combined with an ID liquid chromatography-tandem mass spectrometry. The element-based protein quantification method developed here can be generally used for SI-traceable absolute quantification of proteins, especially pure-protein standards.

Adhesive bonding using variable frequency microwave energy

DOEpatents

Lauf, Robert J.; McMillan, April D.; Paulauskas, Felix L.; Fathi, Zakaryae; Wei, Jianghua

1998-01-01

Methods of facilitating the adhesive bonding of various components with variable frequency microwave energy are disclosed. The time required to cure a polymeric adhesive is decreased by placing components to be bonded via the adhesive in a microwave heating apparatus having a multimode cavity and irradiated with microwaves of varying frequencies. Methods of uniformly heating various articles having conductive fibers disposed therein are provided. Microwave energy may be selectively oriented to enter an edge portion of an article having conductive fibers therein. An edge portion of an article having conductive fibers therein may be selectively shielded from microwave energy.

Adhesive bonding using variable frequency microwave energy

DOEpatents

Lauf, R.J.; McMillan, A.D.; Paulauskas, F.L.; Fathi, Z.; Wei, J.

1998-08-25

Methods of facilitating the adhesive bonding of various components with variable frequency microwave energy are disclosed. The time required to cure a polymeric adhesive is decreased by placing components to be bonded via the adhesive in a microwave heating apparatus having a multimode cavity and irradiated with microwaves of varying frequencies. Methods of uniformly heating various articles having conductive fibers disposed therein are provided. Microwave energy may be selectively oriented to enter an edge portion of an article having conductive fibers therein. An edge portion of an article having conductive fibers therein may be selectively shielded from microwave energy. 26 figs.

Adhesive bonding using variable frequency microwave energy

DOEpatents

Lauf, R.J.; McMillan, A.D.; Paulauskas, F.L.; Fathi, Z.; Wei, J.

1998-09-08

Methods of facilitating the adhesive bonding of various components with variable frequency microwave energy are disclosed. The time required to cure a polymeric adhesive is decreased by placing components to be bonded via the adhesive in a microwave heating apparatus having a multimode cavity and irradiated with microwaves of varying frequencies. Methods of uniformly heating various articles having conductive fibers disposed therein are provided. Microwave energy may be selectively oriented to enter an edge portion of an article having conductive fibers therein. An edge portion of an article having conductive fibers therein may be selectively shielded from microwave energy. 26 figs.

Comparison of microwave hydrodistillation and solvent-free microwave extraction of essential oil from Melaleuca leucadendra Linn

NASA Astrophysics Data System (ADS)

Ismanto, A. W.; Kusuma, H. S.; Mahfud, M.

2017-12-01

The comparison of solvent-free microwave extraction (SFME) and microwave hydrodistillation (MHD) in the extraction of essential oil from Melaleuca leucadendra Linn. was examined. Dry cajuput leaves were used in this study. The purpose of this study is also to determine optimal condition (microwave power). The relative electric consumption of SFME and MHD methods are both showing 0,1627 kWh/g and 0,3279 kWh/g. The results showed that solvent-free microwave extraction methods able to reduce energy consumption and can be regarded as a green technique for extraction of cajuput oil.

Kinetic and Mechanism Study of Vanadium Acid Leaching from Black Shale Using Microwave Heating Method

NASA Astrophysics Data System (ADS)

Wang, Jing-peng; Zhang, Yi-min; Huang, Jing; Liu, Tao

2018-04-01

The leaching kinetics of the vanadium leaching process were investigated by the comparison of microwave heating and conventional heating methods. Microwave heating with CaF2 had a synergistic effect and improved the vanadium leaching efficiency. In contrast to conventional heating leaching, microwave heating accelerated the vanadium leaching rate by approximately 1-3% and by approximately 15% when CaF2 was also used. The kinetics analysis showed that the calculated activation energy decreased in the microwave heating method in the presence and absence of CaF2. The control procedure of leaching also changed from a chemical reaction control step to a mixed chemical diffusion control step upon the addition of CaF2. Microwave heating was shown to be suitable for leaching systems with diffusion or mixed chemical diffusion control steps when the target mineral does not have a microwave absorbing ability.

Kinetic and Mechanism Study of Vanadium Acid Leaching from Black Shale Using Microwave Heating Method

NASA Astrophysics Data System (ADS)

Wang, Jing-peng; Zhang, Yi-min; Huang, Jing; Liu, Tao

2018-06-01

The leaching kinetics of the vanadium leaching process were investigated by the comparison of microwave heating and conventional heating methods. Microwave heating with CaF2 had a synergistic effect and improved the vanadium leaching efficiency. In contrast to conventional heating leaching, microwave heating accelerated the vanadium leaching rate by approximately 1-3% and by approximately 15% when CaF2 was also used. The kinetics analysis showed that the calculated activation energy decreased in the microwave heating method in the presence and absence of CaF2. The control procedure of leaching also changed from a chemical reaction control step to a mixed chemical diffusion control step upon the addition of CaF2. Microwave heating was shown to be suitable for leaching systems with diffusion or mixed chemical diffusion control steps when the target mineral does not have a microwave absorbing ability.

Comparison of amino acid digestibility of feedstuffs determined with the precision-fed cecectomized rooster assay and the standardized ileal amino acid digestibility assay.

PubMed

Kim, E J; Utterback, P L; Applegate, T J; Parsons, C M

2011-11-01

The objective of this study was to evaluate and compare amino acid digestibility of several feedstuffs using 2 commonly accepted methods: the precision-fed cecectomized rooster assay (PFR) and the standardized ileal amino acid assay (SIAAD). Six corn, 6 corn distillers dried grains with or without solubles (DDGS/DDG), one wet distillers grains, one condensed solubles, 2 meat and bone meal (MBM) and a poultry byproduct meal were evaluated. Due to insufficient amounts, the wet distillers grains and condensed solubles were only evaluated in roosters. Standardized amino acid digestibility varied among the feed ingredients and among samples of the same ingredient for both methods. For corn, there were generally no differences in amino acid digestibility between the 2 methods. When differences did occur, there was no consistent pattern among the individual amino acids and methods. Standardized amino acid digestibility was not different between the 2 methods for 4 of the DDG samples; however, the PFR yielded higher digestibility values for a high protein DDG and a conventionally processed DDGS. The PFR yielded higher amino acid digestibility values than the SIAAD for several amino acids in 1 MBM and the poultry byproduct meal, but it yielded lower digestibility values for the other MBM. Overall, there were no consistent differences between methods for amino acid digestibility values. In conclusion, the PFR and SIAAD methods are acceptable for determining amino acid digestibility. However, these procedures do not always yield similar results for all feedstuffs evaluated. Thus, further studies are needed to understand the underlying causes in this variability.

Microwave assisted esterification of acidified oil from waste cooking oil by CERP/PES catalytic membrane for biodiesel production.

PubMed

Zhang, Honglei; Ding, Jincheng; Zhao, Zengdian

2012-11-01

The traditional heating and microwave assisted method for biodiesel production using cation ion-exchange resin particles (CERP)/PES catalytic membrane were comparatively studied to achieve economic and effective method for utilization of free fatty acids (FFAs) from waste cooking oil (WCO). The optimal esterification conditions of the two methods were investigated and the experimental results showed that microwave irradiation exhibited a remarkable enhanced effect for esterification compared with that of traditional heating method. The FFAs conversion of microwave assisted esterification reached 97.4% under the optimal conditions of reaction temperature 60°C, methanol/acidified oil mass ratio 2.0:1, catalytic membrane (annealed at 120°C) loading 3g, microwave power 360W and reaction time 90min. The study results showed that it is a fast, easy and green way to produce biodiesel applying microwave irradiation. Copyright © 2012 Elsevier Ltd. All rights reserved.

Method and apparatus for thickness measurement using microwaves

DOEpatents

Woskov, Paul [Bedford, MA; Lamar, David A [West Richland, WA

2001-01-01

The method for measuring the thickness of a material which transmits a detectable amount of microwave radiation includes irradiating the material with coherent microwave radiation tuned over a frequency range. Reflected microwave radiation is detected, the reflected radiation having maxima and minima over the frequency range as a result of coherent interference of microwaves reflected from reflecting surfaces of the material. The thickness of the material is determined from the period of the maxima and minima along with knowledge of the index of refraction of the material.

International Conference on Infrared and Millimeter Waves, 13th, Honolulu, HI, Dec. 5-9, 1988, Conference Digest

NASA Astrophysics Data System (ADS)

Temkin, Richard J.

Recent advances in IR and mm-wave (MMW) physics, astrophysics, devices, and applications are examined in reviews and reports. Sections are devoted to MMW sources, MMW modulation of light, MMW antennas, FELs, MMW optical technology, astronomy, MMW systems, microwave-optical interactions, MMW waveguides, MMW detectors and mixers, plasma diagnostics, and atmospheric physics. Also considered are gyrotrons, guided propagation, high-Tc superconductors, sub-MMW detectors and related devices, ICs, near-MMW measurements and techniques, lasers, material characterization, semiconductors, and atmospheric propagation.

Production of large resonant plasma volumes in microwave electron cyclotron resonance ion sources

DOEpatents

Alton, Gerald D.

1998-01-01

Microwave injection methods for enhancing the performance of existing electron cyclotron resonance (ECR) ion sources. The methods are based on the use of high-power diverse frequency microwaves, including variable-frequency, multiple-discrete-frequency, and broadband microwaves. The methods effect large resonant "volume" ECR regions in the ion sources. The creation of these large ECR plasma volumes permits coupling of more microwave power into the plasma, resulting in the heating of a much larger electron population to higher energies, the effect of which is to produce higher charge state distributions and much higher intensities within a particular charge state than possible in present ECR ion sources.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; comparison of a nitric acid in-bottle digestion procedure to other whole-water digestion procedures

USGS Publications Warehouse

Garbarino, John R.; Hoffman, Gerald L.

1999-01-01

A hydrochloric acid in-bottle digestion procedure is used to partially digest wholewater samples prior to determining recoverable elements by various analytical methods. The use of hydrochloric acid is problematic for some methods of analysis because of spectral interference. The inbottle digestion procedure has been modified to eliminate such interference by using nitric acid instead of hydrochloric acid in the digestion. Implications of this modification are evaluated by comparing results for a series of synthetic whole-water samples. Results are also compared with those obtained by using U.S. Environmental Protection Agency (1994) (USEPA) Method 200.2 total-recoverable digestion procedure. Percentage yields that use the nitric acid inbottle digestion procedure are within 10 percent of the hydrochloric acid in-bottle yields for 25 of the 26 elements determined in two of the three synthetic whole-water samples tested. Differences in percentage yields for the third synthetic whole-water sample were greater than 10 percent for 16 of the 26 elements determined. The USEPA method was the most rigorous for solubilizing elements from particulate matter in all three synthetic whole-water samples. Nevertheless, the variability in the percentage yield by using the USEPA digestion procedure was generally greater than the in-bottle digestion procedure, presumably because of the difficulty in controlling the digestion conditions accurately.

Selection of biological indicator for validating microwave heating sterilization.

PubMed

Sasaki, K; Mori, Y; Honda, W; Miyake, Y

1998-01-01

For the purpose of selecting an appropriate biological indicator for evaluation of the effects of microwave heating sterilization, we examined aerobic bacterial spores to determine whether microwaves have non-thermal sterilization effects. After microwave irradiation on dry bacterial spores (three species), none of the bacterial spores were killed. The survival rate of the spores after microwave irradiation of spore suspensions (twelve species) was compared with that after heating by a conventional method. The order of heat resistance in the bacterial species was similar between the two heating methods. Bacillus stearothermophilus spores were the most heat-resistant. These results suggest that microwaves have no non-thermal sterilization effects on bacterial spores, the specific resistant spores to microwave heating, and microwave heating sterilization can be evaluated in the same way as for conventional heating sterilization. As a biological indicator for evaluation of overkill sterilization, B. stearothermophilus spores may be appropriate for microwave heating sterilization as well as steam sterilization.

Method of nitriding, carburizing, or oxidizing refractory metal articles using microwaves

DOEpatents

Holcombe, Cressie E.; Dykes, Norman L.; Tiegs, Terry N.

1992-01-01

A method of nitriding an article of refractory-nitride-forming metal or metalloids. A consolidated metal or metalloid article is placed inside a microwave oven and nitrogen containing gas is introduced into the microwave oven. The metal or metalloid article is heated to a temperature sufficient to react the metal or metalloid with the nitrogen by applying a microwave energy within the microwave oven. The metal or metalloid article is maintained at that temperature for a period of time sufficient to convert the article of metal or metalloid to an article of refractory nitride. in addition, a method of applying a coating, such as a coating of an oxide, a carbide, or a carbo-nitride, to an article of metal or metalloid by microwave heating.

Method of nitriding, carburizing, or oxidizing refractory metal articles using microwaves

DOEpatents

Holcombe, C.E.; Dykes, N.L.; Tiegs, T.N.

1992-10-13

A method of nitriding an article of refractory-nitride-forming metal or metalloids. A consolidated metal or metalloid article is placed inside a microwave oven and nitrogen containing gas is introduced into the microwave oven. The metal or metalloid article is heated to a temperature sufficient to react the metal or metalloid with the nitrogen by applying a microwave energy within the microwave oven. The metal or metalloid article is maintained at that temperature for a period of time sufficient to convert the article of metal or metalloid to an article of refractory nitride. in addition, a method of applying a coating, such as a coating of an oxide, a carbide, or a carbo-nitride, to an article of metal or metalloid by microwave heating.

Metal Load of the Crops Depending on Land Use, Land Management and Soil Characteristics

NASA Astrophysics Data System (ADS)

Oeztan, Sezin; Duering, Rolf-Alexander

2010-05-01

The increase of pollutant concentrations in soil and in the food chain became very important in the past few decades. Metals of different toxicities (Cd, Zn, As, Cr, Cu, Pb, Ni, Co, V, Tl) occur in soils as a result of weathering, industrial processes, fertilization and atmospheric deposition. Some of them can be absorbed by the plants due to their mobility. The transfer of metals from soil into the plants can be explained by the physicochemical characteristics of the soil such as pH-value, organic matter and clay content. Badly adapted cultivation of the agricultural soils (declining pH-value, application of unsuitable fertilizers) can enhance the mobility of the metals and by the way increase their concentrations in agricultural products. With this study, a field experiment was established and the aim is to test the relations between available metal concentrations in the soil and metal load of the plants depending on the fertilization techniques. The plants and soil samples of the reference sites were taken, heavy metal contents of the soil samples identified by Microwave Assisted Extraction (MAE) and compared to the Aqua Regia Digestion Method for confirming the methodology. For the determination of the metal content in plants, MAE was executed to the selected plant samples and for that procedure, the samples were digested with HNO3 and H2O2 in the microwave oven. Quantation of the metals in soil and in plants was done by ICP-OES Methodology. The evaluation of the first results confirmed that the metal content of the soil is strongly dependent on the properties of different fertilization variants (N,P,K) used and physicochemical characteristics of the soils. According to the fertilization variants, total metal contents of the soil are increased in the soil samples which have high amounts of N, P, K fertilization. Soils which were enforced with high P fertilization degrees had significantly higher total Cd content. Results on the Cd content of the plant samples also revealed that transition of metals from soil to plants depend heavily on the fertilizer since plant samples and soil samples treated with the same fertilizer showed similar results.

Apparatus and method for microwave processing of materials

DOEpatents

Johnson, Arvid C.; Lauf, Robert J.; Bible, Don W.; Markunas, Robert J.

1996-01-01

A variable frequency microwave heating apparatus (10) designed to allow modulation of the frequency of the microwaves introduced into a furnace cavity (34) for testing or other selected applications. The variable frequency heating apparatus (10) is used in the method of the present invention to monitor the resonant processing frequency within the furnace cavity (34) depending upon the material, including the state thereof, from which the workpiece (36) is fabricated. The variable frequency microwave heating apparatus (10) includes a microwave signal generator (12) and a high-power microwave amplifier (20) or a microwave voltage-controlled oscillator (14). A power supply (22) is provided for operation of the high-power microwave oscillator (14) or microwave amplifier (20). A directional coupler (24) is provided for detecting the direction and amplitude of signals incident upon and reflected from the microwave cavity (34). A first power meter (30) is provided for measuring the power delivered to the microwave furnace (32). A second power meter (26) detects the magnitude of reflected power. Reflected power is dissipated in the reflected power load (28).

Alternative to conventional extraction of vetiver oil: Microwave hydrodistillation of essential oil from vetiver roots (Vetiveria zizanioides)

NASA Astrophysics Data System (ADS)

Kusuma, H. S.; Altway, A.; Mahfud, M.

2017-12-01

In this study the extraction of essential oil from vetiver roots (Vetiveria zizanioides) has been carried out by using microwave hydrodistillation. In the extraction of vetiver oil using microwave hydrodistillation method is studied the effect of microwave power, feed to solvent (F/S) ratio and extraction time on the yield of vetiver oil. Besides, in this study can be seen that microwave hydrodistillation method offers important advantages over hydrodistillation, such as shorter extraction time (3 h vs. 24 h for hydrodistillation); better yields (0.49% vs. 0.46% for hydrodistillation); and environmental impact (energy cost is appreciably higher for performing hydrodistillation than that required for extraction using microwave hydrodistillation). Based on the analysis using GC-MS can be seen 19 components on vetiver oil that has been extracted using microwave hydrodistillation. In addition, GC-MS analysis showed that the main components of vetiver oil that has been extracted using microwave hydrodistillation method were β-Gurjunene (30.12%), α-Vetivone (20.12%), 4-(1-cyclohexenyl)-2-trimethylsilymethyl-1-buten-3-yne (13.52%) and δ-Selinene (7.27%).

[Comparative analysis between diatom nitric acid digestion method and plankton 16S rDNA PCR method].

PubMed

Han, Jun-ge; Wang, Cheng-bao; Li, Xing-biao; Fan, Yan-yan; Feng, Xiang-ping

2013-10-01

To compare and explore the application value of diatom nitric acid digestion method and plankton 16S rDNA PCR method for drowning identification. Forty drowning cases from 2010 to 2011 were collected from Department of Forensic Medicine of Wenzhou Medical University. Samples including lung, kidney, liver and field water from each case were tested with diatom nitric acid digestion method and plankton 16S rDNA PCR method, respectively. The Diatom nitric acid digestion method and plankton 16S rDNA PCR method required 20 g and 2 g of each organ, and 15 mL and 1.5 mL of field water, respectively. The inspection time and detection rate were compared between the two methods. Diatom nitric acid digestion method mainly detected two species of diatoms, Centriae and Pennatae, while plankton 16S rDNA PCR method amplified a length of 162 bp band. The average inspection time of each case of the Diatom nitric acid digestion method was (95.30 +/- 2.78) min less than (325.33 +/- 14.18) min of plankton 16S rDNA PCR method (P < 0.05). The detection rates of two methods for field water and lung were both 100%. For liver and kidney, the detection rate of plankton 16S rDNA PCR method was both 80%, higher than 40% and 30% of diatom nitric acid digestion method (P < 0.05), respectively. The laboratory testing method needs to be appropriately selected according to the specific circumstances in the forensic appraisal of drowning. Compared with diatom nitric acid digestion method, plankton 16S rDNA PCR method has practice values with such advantages as less quantity of samples, huge information and high specificity.

Apparatus and method for microwave processing of materials using field-perturbing tool

DOEpatents

Tucker, Denise A.; Fathi, Zakaryae; Lauf, Robert J.

2001-01-01

A variable frequency microwave heating apparatus designed to allow modulation of the frequency of the microwaves introduced into a multi-mode microwave cavity for heating or other selected applications. A field-perturbing tool is disposed within the cavity to perturb the microwave power distribution in order to apply a desired level of microwave power to the workpiece.

Microwave thawing apparatus and method

DOEpatents

Fathi, Zakaryae; Lauf, Robert J.; McMillan, April D.

2004-06-01

An apparatus for thawing a frozen material includes: a microwave energy source; a microwave applicator which defines a cavity for applying microwave energy from the microwave source to a material to be thawed; and a shielded region which is shielded from the microwave source, the shielded region in fluid communication with the cavity so that thawed material may flow from the cavity into the shielded region.

Production of large resonant plasma volumes in microwave electron cyclotron resonance ion sources

DOEpatents

Alton, G.D.

1998-11-24

Microwave injection methods are disclosed for enhancing the performance of existing electron cyclotron resonance (ECR) ion sources. The methods are based on the use of high-power diverse frequency microwaves, including variable-frequency, multiple-discrete-frequency, and broadband microwaves. The methods effect large resonant ``volume`` ECR regions in the ion sources. The creation of these large ECR plasma volumes permits coupling of more microwave power into the plasma, resulting in the heating of a much larger electron population to higher energies, the effect of which is to produce higher charge state distributions and much higher intensities within a particular charge state than possible in present ECR ion sources. 5 figs.

Microwaving of normally opaque and semi-opaque substances

DOEpatents

Sheinberg, Haskell; Meek, Thomas T.; Blake, Rodger D.

1990-01-01

Method of heating small particles using microwave radiation which are not normally capable of being heated by microwaves. The surfaces of the particles are coated with a material which is transparent to microwave radiation in order to cause microwave coupling to the particles and thus accomplish heating of the particles.

Evaluation of microwave and ultrasound extraction procedures for arsenic speciation in bivalve mollusks by liquid chromatography-inductively coupled plasma-mass spectrometry

NASA Astrophysics Data System (ADS)

Santos, Clarissa M. M.; Nunes, Matheus A. G.; Barbosa, Isa S.; Santos, Gabriel L.; Peso-Aguiar, Marlene C.; Korn, Maria G. A.; Flores, Erico M. M.; Dressler, Valderi L.

2013-08-01

Liquid chromatography-inductively coupled plasma-mass spectrometry (LC-ICP-MS) was used for arsenic speciation analysis in tissues of bivalve mollusks (Anomalocardia brasiliana sp. and Macoma constricta sp.). Microwave and ultrasound radiation, combined with different extraction conditions (solvent, sample amount, time, and temperature), were evaluated for As-species extraction from the mollusks' tissues. Accuracy, extraction efficiency, and the stability of As species were evaluated by analyzing certified reference materials (DORM-2, dogfish muscle; BCR-627, tuna fish tissue; and SRM 1566b, oyster tissue) and analyte recovery tests. The best conditions were found to be microwave-assisted extraction using 200 mg of samples and water at 80 °C for 6 min. The agreement of As-species concentration in samples ranged from 97% to 102%. Arsenobetaine (AsB) was the main species present in bivalve mollusk tissues, while monomethylarsonic acid (MMA) and arsenate (As(V)) were below the limit of quantification (0.001 and 0.003 μg g- 1, respectively). Two unidentified As species also were detected and quantified. The sum of the As-species concentration was in agreement (90 to 104%), with the total As content determined by ICP-MS after sample digestion.

A comparison of essential oils obtained from lavandin via different extraction processes: Ultrasound, microwave, turbohydrodistillation, steam and hydrodistillation.

PubMed

Périno-Issartier, Sandrine; Ginies, Christian; Cravotto, Giancarlo; Chemat, Farid

2013-08-30

A total of eight extraction techniques ranging from conventional methods (hydrodistillation (HD), steam distillation (SD), turbohydrodistillation (THD)), through innovative techniques (ultrasound assisted extraction (US-SD) and finishing with microwave assisted extraction techniques such as In situ microwave-generated hydrodistillation (ISMH), microwave steam distillation (MSD), microwave hydrodiffusion and gravity (MHG), and microwave steam diffusion (MSDf)) were used to extract essential oil from lavandin flowers and their results were compared. Extraction time, yield, essential oil composition and sensorial analysis were considered as the principal terms of comparison. The essential oils extracted using the more innovative processes were quantitatively (yield) and qualitatively (aromatic profile) similar to those obtained from the conventional techniques. The method which gave the best results was the microwave hydrodiffusion and gravity (MHG) method which gave reduced extraction time (30min against 220min for SD) and gave no differences in essential oil yield and sensorial perception. Copyright © 2013 Elsevier B.V. All rights reserved.

Monitoring digestibility of forages for herbivores: a new application for an old approach

USGS Publications Warehouse

Vansomeren, Lindsey L.; Barboza, Perry S.; Thompson, Daniel P.; Gustine, David D.

2015-01-01

Ruminant populations are often limited by how well individuals are able to acquire nutrients for growth, maintenance, and reproduction. Nutrient supply to the animal is dictated by the concentration of nutrients in feeds and the efficiency of digesting those nutrients (i.e., digestibility). Many different methods have been used to measure digestibility of forages for wild herbivores, all of which rely on collecting rumen fluid from animals or incubation within animals. Animal-based methods can provide useful estimates, but the approach is limited by the expense of fistulated animals, wide variation in digestibility among animals, and contamination from endogenous and microbial sources that impairs the estimation of nutrient digestibility. We tested an in vitro method using a two-stage procedure using purified enzymes. The first stage, a 6 h acid–pepsin treatment, was followed by a combined 72 h amylase–cellulase or amylase–Viscozyme treatment. We then validated our estimates using in sacco and in vivo methods to digest samples of the same forages. In vitro estimates of dry matter (DM) digestibility were correlated with estimates of in sacco and in vivo DM digestibility (both P < 0.01). The in vitro procedure using Viscozyme (r2 = 0.77) was more precise than the in vitro procedure using cellulase (r2 = 0.59). Both procedures can be used to predict in sacco digestibility after correcting for the biases of each method. We used the in vitro method to measure digestibility of nitrogen (N; 0.07–0.95 g/g), which declined to zero as total N content declined below 0.03–0.06 g/g of DM. The in vitro method is well suited to monitoring forage quality over multiple years because it is reproducible, can be used with minimal investment by other laboratories without animal facilities, and can measure digestibility of individual nutrients such as N.

Computer-Aided Design of Low-Noise Microwave Circuits

NASA Astrophysics Data System (ADS)

Wedge, Scott William

1991-02-01

Devoid of most natural and manmade noise, microwave frequencies have detection sensitivities limited by internally generated receiver noise. Low-noise amplifiers are therefore critical components in radio astronomical antennas, communications links, radar systems, and even home satellite dishes. A general technique to accurately predict the noise performance of microwave circuits has been lacking. Current noise analysis methods have been limited to specific circuit topologies or neglect correlation, a strong effect in microwave devices. Presented here are generalized methods, developed for computer-aided design implementation, for the analysis of linear noisy microwave circuits comprised of arbitrarily interconnected components. Included are descriptions of efficient algorithms for the simultaneous analysis of noisy and deterministic circuit parameters based on a wave variable approach. The methods are therefore particularly suited to microwave and millimeter-wave circuits. Noise contributions from lossy passive components and active components with electronic noise are considered. Also presented is a new technique for the measurement of device noise characteristics that offers several advantages over current measurement methods.

Below and above boiling point comparison of microwave irradiation and conductive heating for municipal sludge digestion under identical heating/cooling profiles.

PubMed

Hosseini Koupaie, E; Eskicioglu, C

2015-01-01

This research provides a comprehensive comparison between microwave (MW) and conductive heating (CH) sludge pretreatments under identical heating/cooling profiles at below and above boiling point temperatures. Previous comparison studies were constrained to an uncontrolled or a single heating rate due to lack of a CH equipment simulating MW under identical thermal profiles. In this research, a novel custom-built pressure-sealed vessel which could simulate MW pretreatment under identical heating/cooling profiles was used for CH pretreatment. No statistically significant difference was proven between MW and CH pretreatments in terms of sludge solubilization, anaerobic biogas yield and organics biodegradation rate (p-value>0.05), while statistically significant effects of temperature and heating rate were observed (p-value<0.05). These results explain the contradictory results of previous studies in which only the final temperature (not heating/cooling rates) was controlled. Copyright © 2015 Elsevier Ltd. All rights reserved.

Total and inorganic arsenic in fish samples from Norwegian waters.

PubMed

Julshamn, Kaare; Nilsen, Bente M; Frantzen, Sylvia; Valdersnes, Stig; Maage, Amund; Nedreaas, Kjell; Sloth, Jens J

2012-01-01

The contents of total arsenic and inorganic arsenic were determined in fillet samples of Northeast Artic cod, herring, mackerel, Greenland halibut, tusk, saithe and Atlantic halibut. In total, 923 individual fish samples were analysed. The fish were mostly caught in the open sea off the coast of Norway, from 40 positions. The determination of total arsenic was carried out by inductively coupled plasma mass spectrometry following microwave-assisted wet digestion. The determination of inorganic arsenic was carried out by high-performance liquid chromatography-ICP-MS following microwave-assisted dissolution of the samples. The concentrations found for total arsenic varied greatly between fish species, and ranged from 0.3 to 110 mg kg(-1) wet weight. For inorganic arsenic, the concentrations found were very low (<0.006 mg kg(-1)) in all cases. The obtained results question the assumptions made by the European Food Safety Authority (EFSA) on the inorganic arsenic level in fish used in the recent EFSA opinion on arsenic in food.

Final report on CCQM-K125: elements in infant formula

NASA Astrophysics Data System (ADS)

Merrick, J.; Saxby, D.; Dutra, E. S.; Sena, R. C.; Araújo, T. O.; Almeida, M. D.; Yang, L.; Pihillagawa, I. G.; Mester, Z.; Sandoval, S.; Wei, C.; Castillo, M. E. D.; Oster, C.; Fisicaro, P.; Rienitz, O.; Pape, C.; Schulz, U.; Jährling, R.; Görlitz, V.; Lampi, E.; Kakoulides, E.; Sin, D. W. M.; Yip, Y. C.; Tsoi, Y. T.; Zhu, Y.; Okumu, T. O.; Yim, Y. H.; Heo, S. W.; Han, M.; Lim, Y.; Osuna, M. A.; Regalado, L.; Uribe, C.; Buzoianu, M. M.; Duta, S.; Konopelko, L.; Krylov, A.; Shin, R.; Linsky, M.; Botha, A.; Magnusson, B.; Haraldsson, C.; Thiengmanee, U.; Klich, H.; Can, S. Z.; Coskun, F. G.; Tunc, M.; Entwisle, J.; O'Reilly, J.; Hill, S.; Goenaga-Infante, H.; Winchester, M.; Rabb, S. A.; Pérez, R.

2017-01-01

CCQM-K125 was organized by the Inorganic Analysis Working Group (IAWG) of CCQM to assess and document the capabilities of the national metrology institutes (NMIs) or the designated institutes (DIs) to measure the mass fractions of trace elements (K, Cu and I) in infant formula. Government Laboratory, Hong Kong SAR (GLHK) acted as the coordinating laboratory. In CCQM-K125, 25 institutes submitted the results for potassium, 24 institutes submitted the results for copper and 8 institutes submitted the results for iodine. For examination of potassium and copper, most of the participants used microwave-assisted acid digestion methods for sample dissolution. A variety of instrumental techniques including inductively coupled plasma mass spectrometry (ICP-MS), isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS), inductively coupled plasma optical emission spectrometry (ICP-OES), atomic absorption spectrometry (AAS), flame atomic emission spectrometry (FAES) and microwave plasma atomic emission spectroscopy (MP-AES) were employed by the participants for determination. For analysis of iodine, most of the participants used alkaline extraction methods for sample preparation. ICP-MS and ID-ICP-MS were used by the participants for the determination. Generally, the participants' results of CCQM-K125 were found consistent for all measurands according to their equivalence statements. Except with some extreme values, most of the participants obtained the values of di/U(di) within +/- 1 for the measurands. Main text To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

Interlaboratory evaluation of trace element determination in workplace air filter samples by inductively coupled plasma mass spectrometry†‡

PubMed Central

Shulman, Stanley A.; Brisson, Michael J.; Howe, Alan M.

2015-01-01

Inductively coupled plasma mass spectrometry (ICP-MS) is becoming more widely used for trace elemental analysis in the occupational hygiene field, and consequently new ICP-MS international standard procedures have been promulgated by ASTM International and ISO. However, there is a dearth of interlaboratory performance data for this analytical methodology. In an effort to fill this data void, an interlaboratory evaluation of ICP-MS for determining trace elements in workplace air samples was conducted, towards fulfillment of method validation requirements for international voluntary consensus standard test methods. The study was performed in accordance with applicable statistical procedures for investigating interlaboratory precision. The evaluation was carried out using certified 37-mm diameter mixed-cellulose ester (MCE) filters that were fortified with 21 elements of concern in occupational hygiene. Elements were spiked at levels ranging from 0.025 to 10 μg filter−1, with three different filter loadings denoted “Low”, “Medium” and “High”. Participating laboratories were recruited from a pool of over fifty invitees; ultimately twenty laboratories from Europe, North America and Asia submitted results. Triplicates of each certified filter with elemental contents at three different levels, plus media blanks spiked with reagent, were conveyed to each volunteer laboratory. Each participant was also provided a copy of the test method which each participant was asked to follow; spiking levels were unknown to the participants. The laboratories were requested to prepare the filters by one of three sample preparation procedures, i.e., hotplate digestion, microwave digestion or hot block extraction, which were described in the test method. Participants were then asked to analyze aliquots of the prepared samples by ICP-MS, and to report their data in units of μg filter−1. Most interlaboratory precision estimates were acceptable for medium- and high-level spikes (RSD <25%), but generally yielded greater uncertainties than were anticipated at the outset of the study. PMID:22038017

Optimization of enzymes-microwave-ultrasound assisted extraction of Lentinus edodes polysaccharides and determination of its antioxidant activity.

PubMed

Yin, Chaomin; Fan, Xiuzhi; Fan, Zhe; Shi, Defang; Gao, Hong

2018-05-01

Enzymes-microwave-ultrasound assisted extraction (EMUE) method had been used to extract Lentinus edodes polysaccharides (LEPs). The enzymatic temperature, enzymatic pH, microwave power and microwave time were optimized by response surface methodology. The yields, properties and antioxidant activities of LEPs from EMUE and other extraction methods including hot-water extraction, enzymes-assisted extraction, microwave-assisted extraction and ultrasound-assisted extraction were evaluated. The results showed that the highest LEPs yield of 9.38% was achieved with enzymatic temperature of 48°C, enzymatic pH of 5.0, microwave power of 440W and microwave time of 10min, which correlated well with the predicted value of 9.79%. Additionally, LEPs from different extraction methods possessed typical absorption peak of polysaccharides, which meant different extraction methods had no significant effects on type of glycosidic bonds and sugar ring of LEPs. However, SEM images of LEPs from different extraction methods were significantly different. Moreover, the different LEPs all showed antioxidant activities, but LEPs from EMUE showed the highest reducing power when compared to other LEPs. The results indicated LEPs from EMUE can be used as natural antioxidant component in the pharmaceutical and functional food industries. Copyright © 2018 Elsevier B.V. All rights reserved.

Investigating the fate of activated sludge extracellular proteins in sludge digestion using sodium dodecyl sulfate polyacrylamide gel electrophoresis.

PubMed

Park, Chul; Helm, Richard F; Novak, John T

2008-12-01

The fate of activated sludge extracellular proteins in sludge digestion was investigated using three different cation-associated extraction methods and sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE). Extraction methods used were the cation exchange resin (CER) method for extracting calcium (Ca2+) and magnesium (Mg2+), sulfide extraction for removing iron, and base treatment (pH 10.5) for dissolving aluminum. Extracellular polymeric substances extracted were then subjected to SDS-PAGE, and the resultant protein profiles were examined before and after sludge digestion. The SDS-PAGE results showed that three methods led to different SDS-PAGE profiles for both undigested and digested sludges. The results further revealed that CER-extracted proteins remained mainly undegraded in anaerobic digestion, but were degraded in aerobic digestion. While the fate of sulfide- and base-extracted proteins was not clear for aerobic digestion, their changes in anaerobic digestion were elucidated. Most sulfide-extracted proteins were removed by anaerobic digestion, while the increase in protein band intensity and diversity was observed for base-extracted proteins. These results suggest that activated sludge flocs contain different fractions of proteins that are distinguishable by their association with certain cations and that each fraction undergoes different fates in anaerobic and aerobic digestion. The proteins that were resistant to degradation and generated during anaerobic digestion were identified by liquid chromatography tandem mass spectrometry. Protein identification results and their putative roles in activated sludge and anaerobic digestion are discussed in this study.

Method of sintering materials with microwave radiation

DOEpatents

Kimrey, Jr., Harold D.; Holcombe, Jr., Cressie E.; Dykes, Norman L.

1994-01-01

A method of sintering ceramic materials following: A compacted article comprising inorganic particles coated with carbon is provided, the carbon providing improved microwave coupling. The compacted article is then heated by microwave radiation to a temperature and for a period of time sufficient to sinter the compacted article.

Comparison of Two Static in Vitro Digestion Methods for Screening the Bioaccessibility of Carotenoids in Fruits, Vegetables, and Animal Products.

PubMed

Rodrigues, Daniele B; Chitchumroonchokchai, Chureeporn; Mariutti, Lilian R B; Mercadante, Adriana Z; Failla, Mark L

2017-12-27

In vitro digestion methods are routinely used to assess the bioaccessibility of carotenoids and other dietary lipophilic compounds. Here, we compared the recovery of carotenoids and their efficiency of micellarization in digested fruits, vegetables, egg yolk, and salmon and also in mixed-vegetable salads with and without either egg yolk or salmon using the static INFOGEST method22 and the procedure of Failla et al.16 Carotenoid stability during the simulated digestion was ≥70%. The efficiencies of the partitioning of carotenoids into mixed micelles were similar when individual plant foods and salad meals were digested using the two static methods. Furthermore, the addition of cooked egg or salmon to vegetable salads increased the bioaccessibility of some carotenoids. Our findings showed that the two methods of in vitro digestion generated similar estimates of carotenoid retention and bioaccessibility for diverse foods.

Microwave-Assisted Drying for the Conservation of Honeybee Pollen.

PubMed

Canale, Angelo; Benelli, Giovanni; Castagna, Antonella; Sgherri, Cristina; Poli, Piera; Serra, Andrea; Mele, Marcello; Ranieri, Annamaria; Signorini, Francesca; Bientinesi, Matteo; Nicolella, Cristiano

2016-05-12

Bee pollen is becoming an important product thanks to its nutritional properties, including a high content of bioactive compounds such as essential amino acids, antioxidants, and vitamins. Fresh bee pollen has a high water content (15%-30% wt %), thus it is a good substrate for microorganisms. Traditional conservation methods include drying in a hot air chamber and/or freezing. These techniques may significantly affect the pollen organoleptic properties and its content of bioactive compounds. Here, a new conservation method, microwave drying, is introduced and investigated. The method implies irradiating the fresh pollen with microwaves under vacuum, in order to reduce the water content without reaching temperatures capable of thermally deteriorating important bioactive compounds. The method was evaluated by taking into account the nutritional properties after the treatment. The analyzed parameters were phenols, flavonoids, with special reference to rutin content, and amino acids. Results showed that microwave drying offers important advantages for the conservation of bee pollen. Irrespective of microwave power and treatment time, phenol and flavonoid content did not vary over untreated fresh pollen. Similarly, rutin content was unaffected by the microwave drying, suggesting that the microwave-assisted drying could be a powerful technology to preserve bioprotective compounds in fresh pollen.

[Condition optimization experiment of microwave extaction of flavonoids in rhizome of Drynaria fortunei].

PubMed

Yang, Bin; Hu, Fu-chao; Chen, Gong-xi; Jiang, Dao-song

2009-12-01

The experiment extracted flavonoids in rhizome of Drynaria fortunei by microwave extraction, and determined the extraction rate through colorimetry. Through the single factor experiment and orthogonal method, the optimum extraction conditions were as follows: ethanol concentration was 40%, solid-liquid ratio was 1:20 (g/mL), microwave power was 325 W, extraction time was 40 s. Under these conditions, the extraction rate reached 1.73%. In all condtions, microwave power has the most significant effect on extraction rate. Microwave extraction has obvious advantages in comparison with traditional sovent refluxing method.

No major differences found between the effects of microwave-based and conventional heat treatment methods on two different liquid foods.

PubMed

Géczi, Gábor; Horváth, Márk; Kaszab, Tímea; Alemany, Gonzalo Garnacho

2013-01-01

Extension of shelf life and preservation of products are both very important for the food industry. However, just as with other processes, speed and higher manufacturing performance are also beneficial. Although microwave heating is utilized in a number of industrial processes, there are many unanswered questions about its effects on foods. Here we analyze whether the effects of microwave heating with continuous flow are equivalent to those of traditional heat transfer methods. In our study, the effects of heating of liquid foods by conventional and continuous flow microwave heating were studied. Among other properties, we compared the stability of the liquid foods between the two heat treatments. Our goal was to determine whether the continuous flow microwave heating and the conventional heating methods have the same effects on the liquid foods, and, therefore, whether microwave heat treatment can effectively replace conventional heat treatments. We have compared the colour, separation phenomena of the samples treated by different methods. For milk, we also monitored the total viable cell count, for orange juice, vitamin C contents in addition to the taste of the product by sensory analysis. The majority of the results indicate that the circulating coil microwave method used here is equivalent to the conventional heating method based on thermal conduction and convection. However, some results in the analysis of the milk samples show clear differences between heat transfer methods. According to our results, the colour parameters (lightness, red-green and blue-yellow values) of the microwave treated samples differed not only from the untreated control, but also from the traditional heat treated samples. The differences are visually undetectable, however, they become evident through analytical measurement with spectrophotometer. This finding suggests that besides thermal effects, microwave-based food treatment can alter product properties in other ways as well.

No Major Differences Found between the Effects of Microwave-Based and Conventional Heat Treatment Methods on Two Different Liquid Foods

PubMed Central

Géczi, Gábor; Horváth, Márk; Kaszab, Tímea; Alemany, Gonzalo Garnacho

2013-01-01

Extension of shelf life and preservation of products are both very important for the food industry. However, just as with other processes, speed and higher manufacturing performance are also beneficial. Although microwave heating is utilized in a number of industrial processes, there are many unanswered questions about its effects on foods. Here we analyze whether the effects of microwave heating with continuous flow are equivalent to those of traditional heat transfer methods. In our study, the effects of heating of liquid foods by conventional and continuous flow microwave heating were studied. Among other properties, we compared the stability of the liquid foods between the two heat treatments. Our goal was to determine whether the continuous flow microwave heating and the conventional heating methods have the same effects on the liquid foods, and, therefore, whether microwave heat treatment can effectively replace conventional heat treatments. We have compared the colour, separation phenomena of the samples treated by different methods. For milk, we also monitored the total viable cell count, for orange juice, vitamin C contents in addition to the taste of the product by sensory analysis. The majority of the results indicate that the circulating coil microwave method used here is equivalent to the conventional heating method based on thermal conduction and convection. However, some results in the analysis of the milk samples show clear differences between heat transfer methods. According to our results, the colour parameters (lightness, red-green and blue-yellow values) of the microwave treated samples differed not only from the untreated control, but also from the traditional heat treated samples. The differences are visually undetectable, however, they become evident through analytical measurement with spectrophotometer. This finding suggests that besides thermal effects, microwave-based food treatment can alter product properties in other ways as well. PMID:23341982

Organic trace analysis of lignin phenols in speleothems using UHPLC-ESI-HRMS and their use as vegetation proxy

NASA Astrophysics Data System (ADS)

Hitzemann, Inken; Hoffmann, Thorsten

2016-04-01

To understand the climate of the past, it is necessary to get information not only about temperature and precipitation, but also about the vegetation. In contrast to the vegetation proxies used in speleothems so far, like δ13C, the analysis of lignin can provide information not only about the quantity, but also about the type of the regional vegetation. Lignin is widely used as vegetation proxy in sediment samples and natural waters,[1] but there are no methods to analyse lignin in speleothems yet. Lignin is one of the main constituents of wood and woody plants. It is a biopolymer that consists mainly of three monomers, p-coumaryl alcohol, coniferyl alcohol and sinapyl alcohol. The proportion of these three monomers varies with the type of vegetation, for example gymnosperms, angiosperms or herbaceous plants.[2] To analyse the composition of lignin particles in speleothems, it is necessary to extract the speleothem samples, to digest the lignin polymer in order to split it into its monomers, also called lignin phenols, and then to enrich and quantify these lignin phenols. In the method we are presenting here, stalagmite samples are acid digested and the acidic solution is extracted by solid phase extraction. The resulting organic fraction is submitted to an alkaline cupric oxide oxidation using a microwave digestion system.[3] The oxidation products are enriched by solid phase extraction and analysed by ultra high performance liquid chromatography coupled to electrospray high resolution mass spectrometry. We present the limits of detection and quantification, reproducibility and recovery rates as well as first proof-of-principle results from stalagmite samples from the Herbstlabyrinth-Adventshöhle in Germany. References: [1] S. M. Tareq, H. Kitagawa, K. Ohta, Holocene Lake Records: Patterns, Impacts, Causes And Societal Response Selected Papers from the 3rd LIMPACS Conference, Chandigarh, India 2011, 229, 47-56. [2] C. N. Jex, G. H. Pate, A. J. Blyth, R. G. Spencer, P. J. Hernes, S. J. Khan, A. Baker, Quaternary Science Reviews 2014, 87, 46-59. [3] M. A. Goñi, S. Montgomery, Analytical chemistry 2000, 72, 3116-3121.

Method of sintering materials with microwave radiation

DOEpatents

Kimrey, H.D. Jr.; Holcombe, C.E. Jr.; Dykes, N.L.

1994-06-14

Disclosed is a method of sintering ceramic materials. A compacted article comprising inorganic particles coated with carbon is provided, the carbon providing improved microwave coupling. The compacted article is then heated by microwave radiation to a temperature and for a period of time sufficient to sinter the compacted article. No Drawings

Minerals and Trace Elements in Milk, Milk Products, Infant Formula, and Adult/Pediatric Nutritional Formula, ICP-MS Method: Collaborative Study, AOAC Final Action 2015.06, ISO/DIS 21424, IDF 243.

PubMed

Pacquette, Lawrence H; Thompson, Joseph J; Malaviole, I; Zywicki, R; Woltjes, F; Ding, Y; Mittal, A; Ikeuchi, Y; Sadipiralla, B; Kimura, S; Veltman, H; Miura, A

2018-03-01

AOAC Final Action Official MethodSM 2015.06 "Minerals and Trace Elements in Milk, Milk Products, Infant Formula and Adult/Pediatric Nutritional Formula, ICP-MS Method" was collaboratively studied. Note that "milk, milk products" has now been added to the title of the Final Action method because whole milk and several dairy ingredients were successfully incorporated into the collaborative study for the purpose of developing an International Organization for Standardization/International Dairy Federation standard (ISO/DIS 21424; in progress). The method determines sodium, magnesium, phosphorus, potassium, calcium, iron, manganese, zinc, copper, chromium, molybdenum, and selenium by inductively coupled plasma (ICP)-MS after microwave digestion. Ten laboratories participated in the study, and data from five different model ICP-MS units were represented. Thirteen products, five placebo products, and six dairy samples were tested as blind duplicates in this study, along with a standard reference material, for a total 50 samples. The overall repeatability and reproducibility for all samples met Standard Method Performance Requirements put forth by the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals, with a few exceptions. Comparisons are made to ICP-atomic emission data from a collaborative study of AOAC Official Method 2011.14 carried out concurrently on these same samples.

Enrichment of serum biomarkers by magnetic metal-organic framework composites.

PubMed

Wei, Ji-Ping; Wang, Heng; Luo, Tao; Zhou, Zhi-Jiang; Huang, Yan-Feng; Qiao, Bin

2017-03-01

Highly efficient extraction of peptides from serum is critical for finding serum biomarkers using mass spectrometry, which still remains a great challenge. Currently, a bottom-up proteomics approach has been applied to discover serum biomarkers. However, the approach was labor intensive, time and cost consuming, and cannot meet the requirements for clinical application. In this work, Fe 3 O 4 /C@MIL-100 composites were synthesized to efficiently capture peptides from microwave-assisted formic acid digests of BSA and human serum prior to MALDI-TOF MS analysis. Fe 3 O 4 /C@MIL-100 composites exhibited size-selective adsorption performance, thus providing a rapid and convenient approach to enrich low-abundance peptides. Notably, the peptides' mass fingerprinting of serum digestions between type 2 diabetes mellitus (T2DM) and healthy persons were distinguishable, which indicated the potential ability of this technique for T2DM diagnosis and rapid biomarker discovery. Graphical Abstract Efficient extraction and identification of serum biomarkers using Fe 3 O 4 /C@MIL-100 composites from acid hydrolysate.

Bioaccessibility of Ca, Cu, Fe, Mg, Zn, and crude protein in beef, pork and chicken after thermal processing.

PubMed

Menezes, Eveline A; Oliveira, Aline F; França, Celia J; Souza, Gilberto B; Nogueira, Ana Rita A

2018-02-01

The bioaccessibility of Ca, Cu, Fe, Mg, Zn, and crude protein was evaluated after submitting beef, pork, and chicken to five different thermal treatments. The bioaccessibility of crude protein and metals were simulated by using in vitro enzymatic digestion with a gastric fluid solution and dialysability approach. Inductively coupled plasma optical spectrometry was used to quantify the dialyzable fraction and the total mineral content after microwave-assisted digestion. Graphite furnace atomic absorption spectrometry quantified Cu in chicken dialyzable fraction. The increase of temperature and heat exposure period decreased the protein bioaccessibility. Considering the total and dialyzable fraction, beef is an important source of Cu, Fe, Mg, and Zn to the human diet. The results of Fourier-transform infrared spectroscopy indicated physical changes in the treated samples related to protein denaturation, which was probably responsible for the decreased bioaccessibility of minerals and protein, mainly at higher temperatures. Copyright © 2017 Elsevier Ltd. All rights reserved.

Anisotropic Dielectric Properties of Carbon Fiber Reinforced Polymer Composites during Microwave Curing

NASA Astrophysics Data System (ADS)

Zhang, Linglin; Li, Yingguang; Zhou, Jing

2018-01-01

Microwave cuing technology is a promising alternative to conventional autoclave curing technology in high efficient and energy saving processing of polymer composites. Dielectric properties of composites are key parameters related to the energy conversion efficiency during the microwave curing process. However, existing methods of dielectric measurement cannot be applied to the microwave curing process. This paper presented an offline test method to solve this problem. Firstly, a kinetics model of the polymer composites under microwave curing was established based on differential scanning calorimetry to describe the whole curing process. Then several specially designed samples of different feature cure degrees were prepared and used to reflect the dielectric properties of the composite during microwave curing. It was demonstrated to be a feasible plan for both test accuracy and efficiency through extensive experimental research. Based on this method, the anisotropic complex permittivity of a carbon fiber/epoxy composite during microwave curing was accurately determined. Statistical results indicated that both the dielectric constant and dielectric loss of the composite increased at the initial curing stage, peaked at the maximum reaction rate point and decreased finally during the microwave curing process. Corresponding mechanism has also been systematically investigated in this work.

Multi-elements determination in medical and edible Alpinia oxyphylla and Morinda officinalis and their decoctions by ICP-MS.

PubMed

Zhao, Xiangsheng; Wei, Jianhe; Shu, Xiaoyan; Kong, Weijun; Yang, Meihua

2016-12-01

Contents of twenty elements (Mg, K, Ca, Na, Fe, Al, Zn, Ba, Mn, Cu, Mo, Cr, Ni, As, Se, Cd, Hg, Tl, Pb and V) in two medical and edible plant species, Alpinia oxyphylla and Morinda officinalis were simultaneously determined by inductively coupled plasma-mass spectrometry (ICP-MS) method after microwave digestion with HNO 3 -H 2 O 2 (6:1, v/v) as the digestion solvent. Certified standard reference material Poplar leaf was used to assess the accuracy of the method. The greatest contents of Mg, K, Ca, Al, Fe and Na were found in dried Alpinia oxyphylla and Morinda officinalis samples. The contents of five heavy metals including Pb, Cd, As, Hg and Cu in Alpinia oxyphylla did not exceed the limits. The contents of Pb in 76.67% samples and Cd in two batches of Morinda officinalis samples exceeded the limits set by Chinese Pharmacopeia. The contents of the selected elements in different parts (leaves, stems, roots and fruits) of Alpinia oxyphylla varied considerably. The highest concentrations of Mg, Ca, Mn and Se were found in the leaves of Alpinia oxyphylla, at the same time, while, the contents of 9 elements including Cd, Cr, Cu, As, Pb in the roots were the highest. The transfer ratios of selected elements from both species of herbs into their decoctions were reduced. Especially for the heavy metals, the transfer ratios were below 30% except As (79.73%) in Morinda officinalis. The results showed that decoction of the samples may reduce the intake of heavy metals. Copyright © 2016 Elsevier Ltd. All rights reserved.

Gravimetric preparation and characterization of primary reference solutions of molybdenum and rhodium.

PubMed

Kaltenbach, Angela; Noordmann, Janine; Görlitz, Volker; Pape, Carola; Richter, Silke; Kipphardt, Heinrich; Kopp, Gernot; Jährling, Reinhard; Rienitz, Olaf; Güttler, Bernd

2015-04-01

Gravimetrically prepared mono-elemental reference solutions having a well-known mass fraction of approximately 1 g/kg (or a mass concentration of 1 g/L) define the very basis of virtually all measurements in inorganic analysis. Serving as the starting materials of all standard/calibration solutions, they link virtually all measurements of inorganic analytes (regardless of the method applied) to the purity of the solid materials (high-purity metals or salts) they were prepared from. In case these solid materials are characterized comprehensively with respect to their purity, this link also establishes direct metrological traceability to The International System of Units (SI). This, in turn, ensures the comparability of all results on the highest level achievable. Several national metrology institutes (NMIs) and designated institutes (DIs) have been working for nearly two decades in close cooperation with commercial producers on making an increasing number of traceable reference solutions available. Besides the comprehensive characterization of the solid starting materials, dissolving them both loss-free and completely under strict gravimetric control is a challenging problem in the case of several elements like molybdenum and rhodium. Within the framework of the European Metrology Research Programme (EMRP), in the Joint Research Project (JRP) called SIB09 Primary standards for challenging elements, reference solutions of molybdenum and rhodium were prepared directly from the respective metals with a relative expanded uncertainty associated with the mass fraction of U rel(w) < 0.05 %. To achieve this, a microwave-assisted digestion procedure for Rh and a hotplate digestion procedure for Mo were developed along with highly accurate and precise inductively coupled plasma optical emission spectrometry (ICP OES) and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) methods required to assist with the preparation and as dissemination tools.

Determination of rare earth and concomitant elements in magnesium alloys by inductively coupled plasma optical emission spectrometry.

PubMed

Fariñas, Juan C; Rucandio, Isabel; Pomares-Alfonso, Mario S; Villanueva-Tagle, Margarita E; Larrea, María T

2016-07-01

An Inductively Coupled Plasma Optical Emission Spectrometry method for simultaneous determination of Al, Ca, Cu, Fe, In, Mn, Ni, Si, Sr, Y, Zn, Zr and rare earth elements (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu) in magnesium alloys, including the new rare earth elements-alloyed magnesium, has been developed. Robust conditions have been established as nebulizer argon flow rate of 0.5mLmin(-1) and RF incident power of 1500W, in which matrix effects were significantly reduced around 10%. Three acid digestion procedures were performed at 110°C in closed PFA vessels heated in an oven, in closed TFM vessels heated in a microwave furnace, and in open polypropylene tubes with reflux caps heated in a graphite block. The three digestion procedures are suitable to put into solution the magnesium alloys samples. From the most sensitive lines, one analytical line with lack or low spectral interferences has been selected for each element. Mg, Rh and Sc have been studied as internal standards. Among them, Rh was selected as the best one by using Rh I 343.488nm and Rh II 249.078nm lines as a function of the analytical lines. The trueness and precision have been established by using the Certified Reference Material BCS 316, as well as by means of recovery studies. Quantification limits were between 0.1 and 9mgkg(-1) for Lu and Pr, respectively, in a 2gL(-1) magnesium matrix solution. The method developed has been applied to the commercial alloys AM60, AZ80, ZK30, AJ62, WE54 and AE44. Copyright © 2016 Elsevier B.V. All rights reserved.

Investigation of chemical modifiers for the direct determination of arsenic in fish oil using high-resolution continuum source graphite furnace atomic absorption spectrometry.

PubMed

Pereira, Éderson R; de Almeida, Tarcísio S; Borges, Daniel L G; Carasek, Eduardo; Welz, Bernhard; Feldmann, Jörg; Campo Menoyo, Javier Del

2016-04-01

High-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) has been applied for the development of a method for the determination of total As in fish oil samples using direct analysis. The method does not use any sample pretreatment, besides dilution with 1-propanole, in order to decrease the oil viscosity. The stability and sensitivity of As were evaluated using ruthenium and iridium as permanent chemical modifiers and palladium added in solution over the sample. The best results were obtained with ruthenium as the permanent modifier and palladium in solution added to samples and standard solutions. Under these conditions, aqueous standard solutions could be used for calibration for the fish oil samples diluted with 1-propanole. The pyrolysis and atomization temperatures were 1400 °C and 2300 °C, respectively, and the limit of detection and characteristic mass were 30 pg and 43 pg, respectively. Accuracy and precision of the method have been evaluated using microwave-assisted acid digestion of the samples with subsequent determination by HR-CS GF AAS and ICP-MS; the results were in agreement (95% confidence level) with those of the proposed method. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of Chromium, Selenium, and Molybdenum in Infant Formula and Adult Nutritional Products by Inductively Coupled Plasma/Mass Spectrometry: Collaborative Study, Final Action 2011.19.

PubMed

Pacquette, Lawrence H; Thompson, Joseph J

2015-01-01

AOAC First Action Method 2011.19: Chromium, Selenium, and Molybdenum in Infant Formula and Adult Nutritional Products, was collaboratively studied. This method uses microwave digestion of samples with nitric acid, hydrogen peroxide, and internal standard followed by simultaneous detection of the elements by an inductively coupled plasma (ICP)/MS instrument equipped with a collision/reaction cell. During this collaborative study, nine laboratories from four different countries, using seven different models of ICP/MS instruments, analyzed blind duplicates of seven infant, pediatric, and adult nutritional formulas. One laboratory's set of data was rejected in its entirety. The method demonstrated acceptable repeatability and reproducibility and met the AOAC Stakeholder Panel on Infant Formula and Adult Nutritionals (SPIFAN) Standard Method Performance Requirements (SMPRs®) for almost all of the matrixes analyzed. The Cr, Mo, and Se SPIFAN requirement for repeatability was ≤5% RSD. The SMPR called for a reproducibility of ≤15% RSD for products with ultratrace element concentrations above the targeted LOQ of 20 μg/kg Cr/Mo and 10 μg/kg Se (as ready-to-feed). During this collaborative study, RSDr ranged from 1.0 to 7.0% and RSDR ranged from 2.5 to 13.4% across all three ultratrace elements.

Assessment of the trace element distribution in soils in the parks of the city of Zagreb (Croatia).

PubMed

Roje, Vibor; Orešković, Marko; Rončević, Juraj; Bakšić, Darko; Pernar, Nikola; Perković, Ivan

2018-02-07

This paper presents the results of the preliminary testing of the selected trace elements in the soils of several parks in the city of Zagreb, Republic of Croatia. In each park, the samples were taken from several points-at various distances from the roads. The samples were taken at two different depths: 0-5 and 30-45 cm. Composite samples were done for each sampling point. Microwave-assisted wet digestion of the soil samples was performed and the determination by ICP-AES technique was done. Results obtained for Al, As, Ba, Mn, Ti, V, and K are in a good agreement with the results published in the scientific literature so far. The mass fraction values of Cd, Cr, Cu, Ni, Pb, and Zn are somewhat higher than the maximum values given in the Croatian Directive on agricultural land protection against pollution. Be, Mo, Sb, Se, and Tl in the samples were present in the concentrations that are lower than their method detection limit values.

Determination of nickel in hydrogenated fats and selected chocolate bars in Czech Republic.

PubMed

Dohnalova, Lucie; Bucek, Pavel; Vobornik, Petr; Dohnal, Vlastimil

2017-02-15

Nickel is a metal that can be present in products containing hardened edible oils, possibly as leftover catalyst from the vegetable oil hardening process. Nickel may cause toxic effects including the promotion of cancer and contact allergy. In this work, nickel content was determined in hydrogenated vegetable fats and confectionery products, made with these fats, available on the Czech market using newly developed method combining microwave digestion and graphite furnace AAS. While concentrations of 0.086±0.014mg.kg(-1) or less were found in hydrogenated vegetable fats, the Ni content in confectionery products was significantly higher, varying between 0.742±0.066 and 3.141±0.217mg.kg(-1). Based on an average consumer basket, daily intake of nickel from vegetable fats is at least twice as low as intake from confectionery products. Based on results, the levels of nickel in neither vegetable fats nor confectionery products, do not represent a significant health risk. Copyright © 2016 Elsevier Ltd. All rights reserved.

Cadmium and lead in chocolates commercialized in Brazil.

PubMed

Villa, Javier E L; Peixoto, Rafaella R A; Cadore, Solange

2014-08-27

Cadmium (Cd) and lead (Pb) concentrations and their relationship to the cocoa content of chocolates commercialized in Brazil were evaluated by graphite furnace atomic absorption spectrometry (GF AAS) after microwave-assisted acid digestion. Several chemical modifiers were tested during method development, and analytical parameters, including the limits of detection and quantification as well as the accuracy and precision of the overall procedure, were assessed. The study examined 30 chocolate samples, and the concentrations of Cd and Pb were in the range of <1.7-107.6 and <21-138.4 ng/g, respectively. The results indicated that dark chocolates have higher concentrations of Cd and Pb than milk and white chocolates. Furthermore, samples with five different cocoa contents (ranging from 34 to 85%) from the same brand were analyzed, and linear correlations between the cocoa content and the concentrations of Cd (R(2) = 0.907) and Pb (R(2) = 0.955) were observed. The results showed that chocolate might be a significant source of Cd and Pb ingestion, particularly for children.

New method for estimating digestion of Paracoccidioides brasiliensis by phagocytic cells in vitro.

PubMed Central

Goihman-Yahr, M; Essenfeld-Yahr, E; Albornoz, M C; Yarzábal, L; de Gómez, M H; San Martín, B; Ocanto, A; Convit, J

1979-01-01

We describe a method by which phagocytosis and digestion of Paracoccidioides brasiliensis yeast cells by polymorphonuclear leukocytes or other phagocytic cells may be estimated. Suspensions of P. brasiliensis in its yeastlike phase were sonicated, counted, and incubated with known numbers of peripheral blood polymorphonuclear leukocytes. At given intervals, cytocentrifuge droplets were stained by a variation of Papanicolaou's method. Stained preparations were examined with phase-contrast optics. Digested organisms showed total or partial disappearance of protoplasm. Green-stained cell walls resisted digestion. The proportion of digested cells as a function of time was estimated. Images PMID:90683

Microwave processing heats up

USDA-ARS?s Scientific Manuscript database

Microwaves are a common appliance in many households. In the United States microwave heating is the third most popular domestic heating method food foods. Microwave heating is also a commercial food processing technology that has been applied for cooking, drying, and tempering foods. It's use in ...

Molecular basis of processing-induced changes in protein structure in relation to intestinal digestion in yellow and green type pea (Pisum sativum L.): A molecular spectroscopic analysis.

PubMed

Yu, Gloria Qingyu; Warkentin, Tom; Niu, Zhiyuan; Khan, Nazir A; Yu, Peiqiang

2015-12-05

The objectives of this study were (1) to quantify the protein inherent molecular structural features of green cotyledon (CDC Striker) and yellow cotyledon (CDC Meadow) pea (Pisum sativum L.) seeds using molecular spectroscopic technique (FT/IR-ATR); (2) measure the denaturation of protein molecular makeup in the two types of pea during dry roasting (120°C for 60 min), autoclaving (120°C for 60 min) or microwaving (for 5 min); and (3) correlate the heat-induced changes in protein molecular makeup to the corresponding changes in protein digestibility determined using modified three-step in vitro procedure. Compared with yellow-type, the green-type peas had higher (P<0.05) ratios of amide I to II peak height (1.698 vs. 1.805) and area (1.843 vs. 2.017). A significant correlation was observed between the amide I and II peak height (r=0.48) and peak area (r=-0.42) ratio with protein content. Compared with yellow-type, the green-type peas had lower (P<0.05) α-helix:β-sheet ratio (1.015 vs. 0.926), indicating varietal difference in protein secondary structure makeup. All processing applications increased α-helix:β-sheet ratio, with the largest (P<0.05) increase being observed with roasting and microwaving. The heat-induced changes in α-helix:β-sheet ratio was strongly correlated to intestinal digestibility of protein within the green (r=-0. 86) and yellow (r=0.81) pea-types. However, across the pea types the correlation was not significant. Principal component and hierarchical cluster analyses on the entire spectral data from the amide region (ca. 1727-1480 cm(-1)) were able to visualize and discriminate the structural difference between pea varieties and processing treatments. This study shows that the molecular spectroscopy can be used as a rapid tool to screen the protein value of raw and heat-treated peas. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of copper and iron in biological samples of viral hepatitis (A-E) female patients.

PubMed

Afridi, Hassan Imran; Kazi, Tasneem Gul; Kazi, Naveed Gul; Jamali, Mohammad Khan; Sarfaraz, Raja Adil; Arain, Mohammad Balal; Kandhro, Ghulam Abbas; Shah, Abdul Qadir; Baig, Jamil Ahmed; Jalbani, Nusrat; Ansari, Rehana

2009-01-01

There is accumulative evidence that the metabolism of iron and copper is altered in viral hepatic diseases, and these nutrients might have specific roles in their pathogenesis and progress. The aim of present study was to compare the level of copper (Cu) and iron (Fe) in biological samples (serum, urine, and scalp hair) of female patients suffering from different viral hepatitis (A, B, C, D, and E; n = 253) of age range 31-45 years. For comparative study, 95 healthy females of the same age group residing in the same city were selected. The elements in the biological samples were analyzed by flame atomic absorption spectrophotometry, prior to microwave-assisted acid digestion. The validity and accuracy of the methodology was checked by using certified reference materials (CRMs) and with those values obtained by conventional wet acid digestion method on same CRMs. The results of this study showed that the mean values of Cu and Fe were higher in sera and scalp hair samples of hepatitis patients than age-matched control subjects, while the difference was significant (p < 0.001), in the cases of viral hepatitis B and viral hepatitis C as compared to viral hepatitis A, D, and E. The urinary levels of these elements were found higher in the hepatitis patients than in the age-matched healthy controls (p < 0.05). These results are consistent with literature-reported data, confirming that hepatic iron and copper overload can directly cause lipid peroxidation and eventually hepatic damage.

1998 Conference on Precision Electromagnetic Measurements Digest. Proceedings.

NASA Astrophysics Data System (ADS)

Nelson, T. L.

The following topics were dealt with: fundamental constants; caesium standards; AC-DC transfer; impedance measurement; length measurement; units; statistics; cryogenic resonators; time transfer; QED; resistance scaling and bridges; mass measurement; atomic fountains and clocks; single electron transport; Newtonian constant of gravitation; stabilised lasers and frequency measurements; cryogenic current comparators; optical frequency standards; high voltage devices and systems; international compatibility; magnetic measurement; precision power measurement; high resolution spectroscopy; DC transport standards; waveform acquisition and analysis; ion trap standards; optical metrology; quantised Hall effect; Josephson array comparisons; signal generation and measurement; Avogadro constant; microwave networks; wideband power standards; antennas, fields and EMC; quantum-based standards.

Effects of Microwave Radiation on Oil Recovery

NASA Astrophysics Data System (ADS)

Esmaeili, Abdollah

2011-12-01

A variety of oil recovery methods have been developed and applied to mature and depleted reservoirs in order to improve the efficiency. Microwave radiation oil recovery method is a relatively new method and has been of great interest in the recent years. Crude oil is typically co-mingled with suspended solids and water. To increase oil recovery, it is necessary to remove these components. The separation of oil from water and solids using gravitational settling methods is typically incomplete. Oil-in-water and oil-water-solid emulsions can be demulsified and separated into their individual layers by microwave radiation. The data also show that microwave separation is faster than gravity separation and can be faster than conventional heating at many conditions. After separation of emulsion into water and oil layers, water can be discharged and oil is collected. High-frequency microwave recycling process can recover oil and gases from oil shale, residual oil, drill cuttings, tar sands oil, contaminated dredge/sediments, tires and plastics with significantly greater yields and lower costs than are available utilizing existing known technologies. This process is environmentally friendly, fuel-generating recycler to reduce waste, cut emissions, and save energy. This paper presents a critical review of Microwave radiation method for oil recovery.

Method of nitriding refractory metal articles

DOEpatents

Tiegs, Terry N.; Holcombe, Cressie E.; Dykes, Norman L.; Omatete, Ogbemi O.; Young, Albert C.

1994-01-01

A method of nitriding a refractory-nitride forming metal or metalloid articles and composite articles. A consolidated metal or metalloid article or composite is placed inside a microwave oven and nitrogen containing gas is introduced into the microwave oven. The metal or metalloid article or composite is heated to a temperature sufficient to react the metal or metalloid with the nitrogen by applying a microwave energy within the microwave oven. The metal or metalloid article or composite is maintained at that temperature for a period of time sufficient to convert the article of metal or metalloid or composite to an article or composite of refractory nitride. In addition, a method of applying a coating, such as a coating of an oxide, a carbide, or a carbo-nitride, to an article of metal or metalloid by microwave heating.

Method of nitriding refractory metal articles

DOEpatents

Tiegs, T.N.; Holcombe, C.E.; Dykes, N.L.; Omatete, O.O.; Young, A.C.

1994-03-15

A method of nitriding a refractory-nitride forming metal or metalloid articles and composite articles. A consolidated metal or metalloid article or composite is placed inside a microwave oven and nitrogen containing gas is introduced into the microwave oven. The metal or metalloid article or composite is heated to a temperature sufficient to react the metal or metalloid with the nitrogen by applying a microwave energy within the microwave oven. The metal or metalloid article or composite is maintained at that temperature for a period of time sufficient to convert the article of metal or metalloid or composite to an article or composite of refractory nitride. In addition, a method of applying a coating, such as a coating of an oxide, a carbide, or a carbo-nitride, to an article of metal or metalloid by microwave heating.

Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

PubMed Central

Lovingood, Derek D.; Owens, Jeffrey R.; Seeber, Michael; Kornev, Konstantin G.; Luzinov, Igor

2013-01-01

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan δ solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials' morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by Stöber's methods, which have smooth surfaces. PMID:24379052

La Disciplina Positiva (Positive Discipline). ERIC Digest.

ERIC Educational Resources Information Center

ERIC Clearinghouse on Elementary and Early Childhood Education, Urbana, IL.

This ERIC Digest suggests methods and language that can be used in handling difficult, but common, situations involving young children. The digest explains 12 methods of disciplining children that promote children's self-worth. These methods are: (1) showing children that the reasons for their actions are understood; (2) stating reasons; (3)…

Effects of different drying methods on the product quality and volatile compounds of whole shiitake mushrooms.

PubMed

Tian, Yuting; Zhao, Yingting; Huang, Jijun; Zeng, Hongliang; Zheng, Baodong

2016-04-15

Various drying methods play important roles in the preservation of foods. However, how the different drying methods affect the quality of some foods is not clear. This paper evaluates the effects of hot air, vacuum, microwave, and microwave vacuum drying techniques on important qualities and volatile compounds of whole shiitake (Lentinus edodes) mushrooms. These four drying methods resulted in a significantly (p<0.05) increase in the content of total free amino acids and the relative content of sulfur compounds of dried products. Microwave vacuum drying helped to maintain larger amounts of taste-active amino acids, and improved nutrient retention and color attributes. Furthermore, the uniform honeycomb network created by microwave vacuum drying along with a less collapsed structure of dried samples can be used to explain the observed high rehydration ratio. Therefore, microwave vacuum drying should be a potential method for obtaining high-quality dried mushrooms. Copyright © 2015 Elsevier Ltd. All rights reserved.

Study of the optimisation of puffing characteristics of potato cubes by spouted bed drying enhanced with microwave.

PubMed

Yan, Wei-qiang; Zhang, Min; Huang, Lue-lue; Tang, Juming; Mujumdar, Arun S; Sun, Jin-cai

2010-06-01

In commercial deep-fat frying of potato chips, the oil content of the final products ranges from 35 to 45 g 100 g(-1) (wet basis). High-temperature frying may cause the formation of acrylamide, making the products unhealthy to the consumer. The aim of this research was to explore a new method, spouted bed microwave drying, to produce healthier puffed snack potato cubes as possible alternatives to oil-fried potato chips. The influence of drying conditions of the spouted bed microwave drying on puffing characteristics of potato cubes were studied and compared with the direct microwave and hot air drying method. Tandem combination drying of microwave-enhanced spouted bed drying (MWSB) could achieve a good expansion ratio, breaking force and rehydration ratio. The puffing characteristics of potato cubes were significantly affected (P < 0.05) by moisture content before starting microwave power in spouted bed microwave drying, by microwave (MW) power, and by the original size of potato cubes. The optimum processing parameters were the moisture content at the start of microwave power (60%), the size of potato cubes (10-12 mm), and microwave power (2-2.5 W g(-1)) Copyright (c) 2010 Society of Chemical Industry.

Microwave mediated synthesis of ZnS spherical nanoparticles for IR optical ceramics

NASA Astrophysics Data System (ADS)

Ravichandran, D.; Wharton, T.; Devan, B.; Korenstein, R.; Tustison, R.; Komarneni, S.

2011-06-01

The existing material choice for long-wave infrared (LWIR) and semi-active laser domes is multispectral zinc sulfide (ZnS), made by chemical vapor deposition. An alternative route to make more erosion-resistant ZnS could be through hot pressing ZnS nanoparticles into small-grain material. We have attempted to produce ZnS nanoparticles both by microwave and microwave-hydrothermal methods. Microwave route produced ultrahigh purity, homogeneous, well dispersed, and uniformly spherical ZnS nanoparticles. Microwave-hydrothermal route produced equiaxed cubic-faceted nanoparticles. The powder X-ray diffraction patterns of ZnS shows the presence of broad reflections corresponding to the (1 1 1), (2 2 0), and (3 1 1) planes of the cubic crystalline ZnS material. The domain size of the particles estimated from the Debye-Scherrer formula for the main reflection (111) gives a value of 2.9 and 2.5 for the microwave and microwave-hydrothermal methods respectively.

Method for heat treating and sintering metal oxides with microwave radiation

DOEpatents

Holcombe, Cressie E.; Dykes, Norman L.; Meek, Thomas T.

1989-01-01

A method for microwave sintering materials, primarily metal oxides, is described. Metal oxides do not normally absorb microwave radiation at temperatures ranging from about room temperature to several hundred degrees centrigrade are sintered with microwave radiation without the use of the heretofore required sintering aids. This sintering is achieved by enclosing a compact of the oxide material in a housing or capsule formed of a oxide which has microwave coupling properties at room temprature up to at least the microwave coupling temperature of the oxide material forming the compact. The heating of the housing effects the initial heating of the oxide material forming the compact by heat transference and then functions as a thermal insulator for the encased oxide material after the oxide material reaches a sufficient temperature to adequately absorb or couple with microwave radiation for heating thereof to sintering temperature.

Detection of contraband using microwave radiation

DOEpatents

Toth, Richard P.; Loubriel, Guillermo M.; Bacon, Larry D.; Watson, Robert D.

2002-01-01

The present invention relates to a method and system for using microwave radiation to detect contraband hidden inside of a non-metallic container, such as a pneumatic vehicle tire. The method relies on the attenuation, retardation, time delay, or phase shift of microwave radiation as it passes through the container plus the contraband. The method is non-invasive, non-destructive, low power, and does not require physical contact with the container.

Microwave assisted centrifuge and related methods

DOEpatents

Meikrantz, David H [Idaho Falls, ID

2010-08-17

Centrifuge samples may be exposed to microwave energy to heat the samples during centrifugation and to promote separation of the different components or constituents of the samples using a centrifuge device configured for generating microwave energy and directing the microwave energy at a sample located in the centrifuge.

Method and apparatus for component separation using microwave energy

DOEpatents

Morrow, Marvin S.; Schechter, Donald E.; Calhoun, Jr., Clyde L.

2001-04-03

A method for separating and recovering components includes the steps of providing at least a first component bonded to a second component by a microwave absorbent adhesive bonding material at a bonding area to form an assembly, the bonding material disposed between the components. Microwave energy is directly and selectively applied to the assembly so that substantially only the bonding material absorbs the microwave energy until the bonding material is at a debonding state. A separation force is applied while the bonding material is at the debonding state to permit disengaging and recovering the components. In addition, an apparatus for practicing the method includes holders for the components.

Uniform batch processing using microwaves

NASA Technical Reports Server (NTRS)

Barmatz, Martin B. (Inventor); Jackson, Henry W. (Inventor)

2000-01-01

A microwave oven and microwave heating method generates microwaves within a cavity in a predetermined mode such that there is a known region of uniform microwave field. Samples placed in the region will then be heated in a relatively identical manner. Where perturbations induced by the samples are significant, samples are arranged in a symmetrical distribution so that the cumulative perturbation at each sample location is the same.

Methods for producing extracted and digested products from pretreated lignocellulosic biomass

DOEpatents

Chundawat, Shishir; Sousa, Leonardo Da Costa; Cheh, Albert M.; Balan; , Venkatesh; Dale, Bruce

2017-05-16

Methods for producing extracted and digested products from pretreated lignocellulosic biomass are provided. The methods include converting native cellulose I.sub..beta. to cellulose III.sub.I by pretreating the lignocellulosic biomass with liquid ammonia under certain conditions, and performing extracting or digesting steps on the pretreated/converted lignocellulosic biomass.

Evaluation of status of calcium, magnesium, potassium, and sodium levels in biological samples in children of different age groups with normal vision and night blindness.

PubMed

Afridi, Hassan Imran; Kazi, Tasneem Gul; Kazi, Naveed; Kandhro, Ghulam Abbas; Baig, Jameel Ahmed; Shah, Abdul Qadir; Khan, Sumaira; Kolachi, Nida Fatima; Wadhwa, Sham Kumar; Shah, Faheem

2011-01-01

The most common cause of blindness in developing countries is vitamin A deficiency. The World Health Organization (WHO) estimates 13.8 million children have some degree of visual loss related to vitamin A deficiency. The causes of night blindness in children are multifactorial and particular consideration has been given to childhood nutritional deficiency, which is the most common problem found in underdeveloped countries. Such deficiency can result in physiological and pathological processes that in turn influence biological sample composition. Vitamin and mineral deficiency prevents more than two billion people from achieving their full intellectual and physical potential. This study was designed to compare the levels of magnesium (Mg), calcium (Ca), potassium (K), and sodium (Na) in scalp hair, serum, blood, and urine of night blindness children in two age groups, (1-5) and (6-10) years, of both genders comparing them to sex- and age-matched controls. A microwave assisted wet acid digestion procedure was developed as a sample pretreatment for the determination of Mg, Ca, K, and Na in biological samples of children with night blindness. The proposed method was validated by using conventional wet digestion and certified reference samples of hair, serum, blood, and urine. The digests of all biological samples were analysed for Mg, Ca, K, and Na by flame atomic absorption spectrometry (FAAS) using an air/acetylene flame. The results indicated significantly lower levels of Mg, Ca, and K in the biological samples (blood, serum, and scalp hair) of male and female children with night blindness and higher values of Na compared with control subjects of both genders. These data present guidance to clinicians and other professionals investigating deficiency of essential mineral elements in biological samples (scalp hair, serum, and blood) of children with night blindness.

Assessing oral bioaccessibility of trace elements in soils under worst-case scenarios by automated in-line dynamic extraction as a front end to inductively coupled plasma atomic emission spectrometry.

PubMed

Rosende, María; Magalhães, Luis M; Segundo, Marcela A; Miró, Manuel

2014-09-09

A novel biomimetic extraction procedure that allows for the in-line handing of ≥400 mg solid substrates is herein proposed for automatic ascertainment of trace element (TE) bioaccessibility in soils under worst-case conditions as per recommendations of ISO norms. A unified bioaccessibility/BARGE method (UBM)-like physiological-based extraction test is evaluated for the first time in a dynamic format for accurate assessment of in-vitro bioaccessibility of Cr, Cu, Ni, Pb and Zn in forest and residential-garden soils by on-line coupling of a hybrid flow set-up to inductively coupled plasma atomic emission spectrometry. Three biologically relevant operational extraction modes mimicking: (i) gastric juice extraction alone; (ii) saliva and gastric juice composite in unidirectional flow extraction format and (iii) saliva and gastric juice composite in a recirculation mode were thoroughly investigated. The extraction profiles of the three configurations using digestive fluids were proven to fit a first order reaction kinetic model for estimating the maximum TE bioaccessibility, that is, the actual worst-case scenario in human risk assessment protocols. A full factorial design, in which the sample amount (400-800 mg), the extractant flow rate (0.5-1.5 mL min(-1)) and the extraction temperature (27-37°C) were selected as variables for the multivariate optimization studies in order to obtain the maximum TE extractability. Two soils of varied physicochemical properties were analysed and no significant differences were found at the 0.05 significance level between the summation of leached concentrations of TE in gastric juice plus the residual fraction and the total concentration of the overall assayed metals determined by microwave digestion. These results showed the reliability and lack of bias (trueness) of the automatic biomimetic extraction approach using digestive juices. Copyright © 2014 Elsevier B.V. All rights reserved.

Personalizing Protein Nourishment

PubMed Central

DALLAS, DAVID C.; SANCTUARY, MEGAN R.; QU, YUNYAO; KHAJAVI, SHABNAM HAGHIGHAT; VAN ZANDT, ALEXANDRIA E.; DYANDRA, MELISSA; FRESE, STEVEN A.; BARILE, DANIELA; GERMAN, J. BRUCE

2016-01-01

Proteins are not equally digestible—their proteolytic susceptibility varies by their source and processing method. Incomplete digestion increases colonic microbial protein fermentation (putrefaction), which produces toxic metabolites that can induce inflammation in vitro and have been associated with inflammation in vivo. Individual humans differ in protein digestive capacity based on phenotypes, particularly disease states. To avoid putrefaction-induced intestinal inflammation, protein sources and processing methods must be tailored to the consumer’s digestive capacity. This review explores how food processing techniques alter protein digestibility and examines how physiological conditions alter digestive capacity. Possible solutions to improving digestive function or matching low digestive capacity with more digestible protein sources are explored. Beyond the ileal digestibility measurements of protein digestibility, less invasive, quicker and cheaper techniques for monitoring the extent of protein digestion and fermentation are needed to personalize protein nourishment. Biomarkers of protein digestive capacity and efficiency can be identified with the toolsets of peptidomics, metabolomics, microbial sequencing and multiplexed protein analysis of fecal and urine samples. By monitoring individual protein digestive function, the protein component of diets can be tailored via protein source and processing selection to match individual needs to minimize colonic putrefaction and, thus, optimize gut health. PMID:26713355

Evaluation of Amino Acid and Energy Utilization in Feedstuff for Swine and Poultry Diets

PubMed Central

Kong, C.; Adeola, O.

2014-01-01

An accurate feed formulation is essential for optimizing feed efficiency and minimizing feed cost for swine and poultry production. Because energy and amino acid (AA) account for the major cost of swine and poultry diets, a precise determination of the availability of energy and AA in feedstuffs is essential for accurate diet formulations. Therefore, the methodology for determining the availability of energy and AA should be carefully selected. The total collection and index methods are 2 major procedures for estimating the availability of energy and AA in feedstuffs for swine and poultry diets. The total collection method is based on the laborious production of quantitative records of feed intake and output, whereas the index method can avoid the laborious work, but greatly relies on accurate chemical analysis of index compound. The direct method, in which the test feedstuff in a diet is the sole source of the component of interest, is widely used to determine the digestibility of nutritional components in feedstuffs. In some cases, however, it may be necessary to formulate a basal diet and a test diet in which a portion of the basal diet is replaced by the feed ingredient to be tested because of poor palatability and low level of the interested component in the test ingredients. For the digestibility of AA, due to the confounding effect on AA composition of protein in feces by microorganisms in the hind gut, ileal digestibility rather than fecal digestibility has been preferred as the reliable method for estimating AA digestibility. Depending on the contribution of ileal endogenous AA losses in the ileal digestibility calculation, ileal digestibility estimates can be expressed as apparent, standardized, and true ileal digestibility, and are usually determined using the ileal cannulation method for pigs and the slaughter method for poultry. Among these digestibility estimates, the standardized ileal AA digestibility that corrects apparent ileal digestibility for basal endogenous AA losses, provides appropriate information for the formulation of swine and poultry diets. The total quantity of energy in feedstuffs can be partitioned into different components including gross energy (GE), digestible energy (DE), metabolizable energy (ME), and net energy based on the consideration of sequential energy losses during digestion and metabolism from GE in feeds. For swine, the total collection method is suggested for determining DE and ME in feedstuffs whereas for poultry the classical ME assay and the precision-fed method are applicable. Further investigation for the utilization of ME may be conducted by measuring either heat production or energy retention using indirect calorimetry or comparative slaughter method, respectively. This review provides information on the methodology used to determine accurate estimates of AA and energy availability for formulating swine and poultry diets. PMID:25050031

Evaluation of amino Acid and energy utilization in feedstuff for Swine and poultry diets.

PubMed

Kong, C; Adeola, O

2014-07-01

An accurate feed formulation is essential for optimizing feed efficiency and minimizing feed cost for swine and poultry production. Because energy and amino acid (AA) account for the major cost of swine and poultry diets, a precise determination of the availability of energy and AA in feedstuffs is essential for accurate diet formulations. Therefore, the methodology for determining the availability of energy and AA should be carefully selected. The total collection and index methods are 2 major procedures for estimating the availability of energy and AA in feedstuffs for swine and poultry diets. The total collection method is based on the laborious production of quantitative records of feed intake and output, whereas the index method can avoid the laborious work, but greatly relies on accurate chemical analysis of index compound. The direct method, in which the test feedstuff in a diet is the sole source of the component of interest, is widely used to determine the digestibility of nutritional components in feedstuffs. In some cases, however, it may be necessary to formulate a basal diet and a test diet in which a portion of the basal diet is replaced by the feed ingredient to be tested because of poor palatability and low level of the interested component in the test ingredients. For the digestibility of AA, due to the confounding effect on AA composition of protein in feces by microorganisms in the hind gut, ileal digestibility rather than fecal digestibility has been preferred as the reliable method for estimating AA digestibility. Depending on the contribution of ileal endogenous AA losses in the ileal digestibility calculation, ileal digestibility estimates can be expressed as apparent, standardized, and true ileal digestibility, and are usually determined using the ileal cannulation method for pigs and the slaughter method for poultry. Among these digestibility estimates, the standardized ileal AA digestibility that corrects apparent ileal digestibility for basal endogenous AA losses, provides appropriate information for the formulation of swine and poultry diets. The total quantity of energy in feedstuffs can be partitioned into different components including gross energy (GE), digestible energy (DE), metabolizable energy (ME), and net energy based on the consideration of sequential energy losses during digestion and metabolism from GE in feeds. For swine, the total collection method is suggested for determining DE and ME in feedstuffs whereas for poultry the classical ME assay and the precision-fed method are applicable. Further investigation for the utilization of ME may be conducted by measuring either heat production or energy retention using indirect calorimetry or comparative slaughter method, respectively. This review provides information on the methodology used to determine accurate estimates of AA and energy availability for formulating swine and poultry diets.

Headspace single drop microextraction coupled with microwave extraction of essential oil from plant materials.

PubMed

Zhai, Yujuan; Sun, Shuo; Wang, Ziming; Zhang, Yupu; Liu, He; Sun, Ye; Zhang, Hanqi; Yu, Aimin

2011-05-01

Headspace single drop microextraction (HS-SDME) coupled with microwave extraction (ME) was developed and applied to the extraction of the essential oil from dried Syzygium aromaticum (L.) Merr. et Perry and Cuminum cyminum L. The operational parameters, such as microdrop volume, microwave absorption medium (MAM), extraction time, and microwave power were optimized. Ten microliters of decane was used as the microextraction solvent. Ionic liquid and carbonyl iron powder were used as MAM. The extraction time was less than 7 min at the microwave power of 440 W. The proposed method was compared with hydrodistillation (HD). There were no obvious differences in the constituents of essential oils obtained by the two methods.

Plasma-assisted microwave processing of materials

NASA Technical Reports Server (NTRS)

Barmatz, Martin (Inventor); Jackson, Henry (Inventor); Ylin, Tzu-yuan (Inventor)

1998-01-01

A microwave plasma assisted method and system for heating and joining materials. The invention uses a microwave induced plasma to controllably preheat workpiece materials that are poorly microwave absorbing. The plasma preheats the workpiece to a temperature that improves the materials' ability to absorb microwave energy. The plasma is extinguished and microwave energy is able to volumetrically heat the workpiece. Localized heating of good microwave absorbing materials is done by shielding certain parts of the workpiece and igniting the plasma in the areas not shielded. Microwave induced plasma is also used to induce self-propagating high temperature synthesis (SHS) process for the joining of materials. Preferably, a microwave induced plasma preheats the material and then microwave energy ignites the center of the material, thereby causing a high temperature spherical wave front from the center outward.

Bioimaging of isosteric osmium and ruthenium anticancer agents by LA-ICP-MS.

PubMed

Klose, Matthias H M; Theiner, Sarah; Kornauth, Christoph; Meier-Menches, Samuel M; Heffeter, Petra; Berger, Walter; Koellensperger, Gunda; Keppler, Bernhard K

2018-03-01

Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) was used to study the spatial distribution of two metallodrugs with anticancer activities in vivo, namely the organoruthenium plecstatin-1 (1) and its isosteric osmium analogue (2), in liver, kidneys, muscles and tumours of treated mice bearing a CT-26 tumour after single-dose i.p. administration. To the best of our knowledge, this is the first time that the spatial distribution of an osmium drug candidate has been investigated using LA-ICP-MS in tissues. Independent measurements of the average ruthenium and osmium concentration via microwave digestion and ICP-MS in organs and tumours were in good agreement with the LA-ICP-MS results. Matrix-matched standards (MMS) ranging from 1 to 30 μg g -1 were prepared to quantify the spatial distributions of the metals and the average metal content of the MMS samples was additionally quantified by ICP-MS after microwave digestion. The recoveries for osmium and ruthenium in the MMS were 105% and 101% on average, respectively, validating the sample preparation procedure of the MMS. Preparation of MMS was carried out under an argon atmosphere to prevent oxidation of osmium-species to the volatile OsO 4 . The highest metal concentrations were found in the liver, followed by kidney, lung and tumour tissues, while muscles displayed only very low quantities of the respective metal. Both metallodrugs accumulated in the cortex of the kidneys more strongly compared to the medulla. Interestingly, osmium from 2 was largely located at the periphery and tissue edges, whereas ruthenium from 1 was observed to penetrate deeper into the organs and tumours.

[Physical and mechanical properties of the thermosetting resin for crown and bridge cured by micro-wave heating].

PubMed

Kaneko, K

1989-09-01

A heating method using micro-waves was utilized to obtain strong thermosetting resin for crown and bridge. The physical and mechanical properties of the thermosetting resin were examined. The resin was cured in a shorter time by the micro-waves heating method than by the conventional heat curing method and the working time was reduced markedly. The base resins of the thermosetting resin for crown and bridge for the micro-waves heating method were 2 PA and diluent 3 G. A compounding volume of 30 wt% for diluent 3 G was considered good the results of compressive strength, bending strength and diametral tensile strength. Grams of 200-230 of the filler compounded to the base resins of 2 PA-3 G system provided optimal compressive strength, bending strength and diametral tensile strength. A filler gram of 230 provided optimal hardness and curing shrinkage rate, the coefficient of thermal expansion became smaller with the increase of the compounding volume of the filler. The trial thermosetting resin for crown and bridge formed by the micro-waves heating method was not inferior to the conventional resin by the heat curing method or the light curing method.

[Analysis of triterpenoids in Ganoderma lucidum by microwave-assisted continuous extraction].

PubMed

Lu, Yan-fang; An, Jing; Jiang, Ye

2015-04-01

For further improving the extraction efficiency of microwave extraction, a microwave-assisted contijuous extraction (MACE) device has been designed and utilized. By contrasting with the traditional methods, the characteristics and extraction efficiency of MACE has also been studied. The method was validated by the analysis of the triterpenoids in Ganoderma lucidum. The extraction conditions of MACE were: using 95% ethanol as solvent, microwave power 200 W and radiation time 14.5 min (5 cycles). The extraction results were subsequently compared with traditional heat reflux extraction ( HRE) , soxhlet extraction (SE), ultrasonic extraction ( UE) as well as the conventional microwave extraction (ME). For triterpenoids, the two methods based on the microwaves (ME and MACE) were in general capable of finishing the extraction in 10, 14.5 min, respectively, while other methods should consume 60 min and even more than 100 min. Additionally, ME can produce comparable extraction results as the classical HRE and higher extraction yield than both SE and UE, however, notably lower extraction yield than MASE. More importantly, the purity of the crud extract by MACE is far better than the other methods. MACE can effectively combine the advantages of microwave extraction and soxhlet extraction, thus enabling a more complete extraction of the analytes of TCMs in comparison with ME. And therefore makes the analytic result more accurate. It provides a novel, high efficient, rapid and reliable pretreatment technique for the analysis of TCMs, and it could potentially be extended to ingredient preparation or extracting techniques of TCMs.

Determination of rare earth elements in tomato plants by inductively coupled plasma mass spectrometry techniques.

PubMed

Spalla, S; Baffi, C; Barbante, C; Turetta, C; Turretta, C; Cozzi, G; Beone, G M; Bettinelli, M

2009-10-30

In recent years identification of the geographical origin of food has grown more important as consumers have become interested in knowing the provenance of the food that they purchase and eat. Certification schemes and labels have thus been developed to protect consumers and genuine producers from the improper use of popular brand names or renowned geographical origins. As the tomato is one of the major components of what is considered to be the healthy Mediterranean diet, it is important to be able to determine the geographical origin of tomatoes and tomato-based products such as tomato sauce. The aim of this work is to develop an analytical method to determine rare earth elements (RRE) for the control of the geographic origin of tomatoes. The content of REE in tomato plant samples collected from an agricultural area in Piacenza, Italy, was determined, using four different digestion procedures with and without HF. Microwave dissolution with HNO3 + H2O2 proved to be the most suitable digestion procedure. Inductively coupled plasma quadrupole mass spectrometry (ICPQMS) and inductively coupled plasma sector field plasma mass spectrometry (ICPSFMS) instruments, both coupled with a desolvation system, were used to determine the REE in tomato plants in two different laboratories. A matched calibration curve method was used for the quantification of the analytes. The detection limits (MDLs) of the method ranged from 0.03 ng g(-1) for Ho, Tm, and Lu to 2 ng g(-1) for La and Ce. The precision, in terms of relative standard deviation on six replicates, was good, with values ranging, on average, from 6.0% for LREE (light rare earth elements) to 16.5% for HREE (heavy rare earth elements). These detection limits allowed the determination of the very low concentrations of REE present in tomato berries. For the concentrations of REE in tomato plants, the following trend was observed: roots > leaves > stems > berries. Copyright 2009 John Wiley & Sons, Ltd.

Fast Microwave-assisted Pretreatment for Bioconversion of Sawdust Lignocellulose to Glucose

NASA Astrophysics Data System (ADS)

Nyoman Sudiana, I.; Mitsudo, Seitaro; Endang Susilowati, Prima; Ketut Sutiari, Desak; Widana Arsana, Made; Zamrun Firihu, Muhammad; Ode Ngkoimani, La; Aba, La; Sahaluddin Hasan, Erzam; Cahyono, Edi; Sabchevski, Svilen; Aripin, Haji; Gde Suastika, Komang

2017-05-01

A preliminary study of application microwave energy for bioconversion of cellulosic sawdust to glucose was performed. The effects of the microwave were compared to those of the conventional method for each solvent. It was expected that a broader mechanism responsible for the microwave effects on the chemical processes, especially the pretreatment on the hydrolysis of cellulose can be explained. Reagents used were an acid (HCl), an alkali (NaOH), and distilled water (H2O). The experimental results showed that the microwave-assisted pretreatment on the lignocellulosic sawdust faster than by using conventional heating (hotplate). Moreover by using microwave a higher glucose content compared to the conventional method was found. With microwave during hydrolisis, high temperatures and high reagent concentrations were not required. Pretreatment with a microwave at 800 Watt and solvent NaOH 22,50 mg/mL at a temperature of 120°c appeared to be most efficient found in this experiment. These results indicate that microwave effective for bioconversion of cellulosic sawdust to glucose. The microstructure evaluation by using SEM and XRD should be performed to understand more detail the effect especially on their cellulosic structural evolution.

Effect of Zn doping on the microwave absorption of BFO multiferroic materials

NASA Astrophysics Data System (ADS)

Bi, S.; Li, J.; Mei, B.; Su, X. J.; Ying, C. Z.; Li, P. H.

2018-01-01

The microwave absorbing materials were firstly used in the Second World War. And the BiFeO3 (BFO) based microwave absorbers have been widely applied into the microwave absorbing area due to its possession of excellent electromagnetic properties. Various methods have been conducted to improve the microwave absorption performance of the BFO based materials. In the work, the sol-gel method were used to prepare the BFO, and the Zn were doped into the BFO to prepare the Bi1-xZnxFeO3 nanoparticles. The X-ray diffraction, scanning electron microscope, and vector network analysis (VNA) were conducted to characterize the microstructure and electromagnetic properties of the as-prepared samples. The results indicate that the Bi1-xZnxFeO3 nanoparticles were successfully gained and the as-prepared samples possess excellent microwave absorption properties.

Measuring the content of 17 elements in the flesh of Prunus cerasifera and its cultivars by ICP-MS.

PubMed

Shen, Jing; Xue, Hai-Yan; Li, Gai-Ru; Lu, Yi; Yao, Jun

2014-09-01

The present study compared the contents of inorganic elements in the pulp of purple, red, and yellow Prunus cerasifera with its cultivars. A method was established for the analysis of 17 kinds of trace elements (K, Ca, Mg, Na, Fe, Mn, Cu, Zn, Be, Li, Se, Sr, Cr, Pb, Cd, As and Hg) in the flesh of Prunus cerasifera by microwave digestion-ICP-MS. The detection method is simple and quick, yet shoes high precision and high sensitivity. The recovery rate of 17 elements ranged, from 93.5% to 110.4%. The analysis results showed that the contents of 17 elements in the flesh of purple, red, and yellow Prunus cerasifera and its cultivars are similar, containing extremely rich K elements (as high as 1 per thousand) and higher contents of Ca, Mg, Na, Fe and Mn. The contents of Cu, Zn, Li, Se, Sr and Cr are also present. The contents of Pb, Cd, As, Hg and other harmful element are either very low or not detectable. The experimental results for the study of trace elements in pulp of Prunus cerasifera and its cultivars provide empirical data for. future research in this area.

[Analysis and Evaluation of Inorganic Elements in Euryale Semen from Different Habitats by Microwave Digestion-ICP-OES].

PubMed

Wang, Hong; Wu, Qi-nan; Wu, Cheng-ying; Fan, Xiu-he; Jiang, Zheng; Gu, Wei; Yue, Wei

2015-01-01

To establish a simple, rapid and efficient method for determination of different inorganic elements in Euryale Semen from different habitats. Inductively coupled plasma-optical emission spectrometry(ICP-OES) was applied to determine inorganic elements in Euryale Semen, and the results were analyzed by principal component analysis. Euryale Semen from different habitats contained the kind of inorganic elements ranging from 22 to 26, including micronutrient elements like Iron, Zinc, Selenium, Copper, Molybdenum, Chrome and Cobalt, as well as macronutrient elements such as Potassium, Calcium, Sodium, Magnesium and Phosphorus. Five factors were extracted and used to comprehensively evaluate Euryale Semen from 20 different habitats covered almost China. The comprehensive function was F = 0. 38828F1 + 0. 25603F2 + 0. 07617F3 + 0. 06860F4 + 0. 04868F5, which resulted in the top three samples coming from Jiangsu Gaoyou, Hunan Xiangxi and Jiangsu Suzhou respectively. The study indicates that ICP-OES is a quick, accurate and sensitive method to determine the contents of inorganic elements in Euryale Semen,which provides scientific and reliable reference for its quality control and safety assessment.

Pretreatment methods to improve nerve immunostaining in corneas from long-term fixed embryonic quail eyes

NASA Technical Reports Server (NTRS)

Barrett, J. E.; Wells, D. C.; Conrad, G. W.

1999-01-01

Pretreatment methods were used to improve neurofilament immunostaining in corneas from embryonic day 16 Japanese quail corneas that had been stored in fixative solution for several months. A sequential combination of the following three pretreatments: brief microwave heating in saline, followed by extraction with sodium dodecyl sulfate (SDS) at 37 degrees C, followed by digestion with hyaluronidase at 37 degrees C, produced significantly increased antibody staining of corneal neurofilament proteins, compared with embryonic corneas subjected to no prior pretreatments or to single or two-step protocols. After applying the sequence of all three pretreatments, darkest nerve staining and increased numbers of fine branches were observed, together with lower background staining. Thus, the result of applying the three-step pretreatment sequence is better than that of applying any of its component single pretreatments or even combinations of any two of them. These findings therefore suggest that each of these three pretreatments causes a unique effect, beneficial to immunostaining of neurofilament proteins, and that their individual effects are independent and additive. In addition to embryonic corneas, the three-step procedure also may be useful for immunostaining of nerves in other very delicate, highly-hydrated tissues containing an abundance of extracellular matrix.

[Determination of Heavy Metal Elements in Diatomite Filter Aid by Inductively Coupled Plasma Mass Spectrometry].

PubMed

Nie, Xi-du; Fu, Liang

2015-11-01

This study established a method for determining Be, Cr, Ni, As, Cd, Sb, Sn, Tl, Hg and Pb, total 10 heavy metals in diatomite filter aid. The diatomite filter aid was digested by using the mixture acid of HNO₃ + HF+ H₃PO₄ in microwave system, 10 heavy metals elements were determined by inductively coupled plasma mass spectrometry (ICP-MS). The interferences of mass spectrometry caused by the high silicon substrate were optimized, first the equipment parameters and isotopes of test metals were selected to eliminate these interferences, the methane was selected as reactant gas, and the mass spectral interferences were eliminated by dynamic reaction cell (DRC). Li, Sc, Y, In and Bi were selected as the internal standard elements to correct the interferences caused by matrix and the drift of sensitivity. The results show that the detection limits for analyte is in the range of 3.29-15.68 ng · L⁻¹, relative standard deviations (RSD) is less than 4.62%, and the recovery is in the range of 90.71%-107.22%. The current method has some advantages such as, high sensitivity, accurate, and precision, which can be used in diatomite filter aid quality control and safety estimations.

Hazardous impact of arsenic on tissues of same fish species collected from two ecosystem.

PubMed

Shah, Abdul Qadir; Kazi, Tasneem Gul; Arain, Mohammad Balal; Baig, Jameel Ahmed; Afridi, Hassan Imran; Kandhro, Ghulam Abbas; Khan, Sumaira; Jamali, Mohammad Khan

2009-08-15

The purpose of this paper is to develop a database of fish tissues and to evaluate concentration of arsenic (As) in five tissues of fish species collected from Manchar Lake Pakistan and to compare concentration of As in fish tissues of same fish species collected from the Indus River, Pakistan. A sensitive and precise, hydride generation atomic absorption spectrometry (HG AAS) method is presented for the determination of total Arsenic (As). Microwave acid-assisted digestion (MAD) procedure based on the mixture HNO(3)/H(2)O(2) was evaluated. The method was successfully validated against CRM DORM-2 (dogfish muscle). Quantitative As recovery in CRM (DORM-2) was obtained and no statistical differences were found at 95% level by applying the t-test. The limit of detection (LOD) and limit of quantitation (LOQ), for As were established as 0.022 and 0.063 microg g(-1), respectively. The results of this study indicated that As concentration in fish tissues from the Indus River are generally lower than in tissues of fishes from Manchar Lake. Arsenic concentrations in fish tissues of Indus River are although above the respective human health-based concentrations.

Alternate Methods for Disposal of Nitrocellulose Fines

DTIC Science & Technology

1985-07-22

13 Microwave ..................................... 14 Plasma ........................................ 14V Laser pyrolysis...would either be backflushed (not expected to be too successful) or replaced. Microwave Thermal Degradation The use of microwave heating has been...with microwave heating, new designs would be needed if a practical, cost effective system is to be developed. Considerable additional research would be

Microwave reflection, transmission, and absorption by human brain tissue

NASA Astrophysics Data System (ADS)

Ansari, M. A.; Akhlaghipour, N.; Zarei, M.; Niknam, A. R.

2018-04-01

These days, the biological effects of electromagnetic (EM) radiations on the brain, especially in the frequency range of mobile communications, have caught the attention of many scientists. Therefore, in this paper, the propagation of mobile phone electromagnetic waves in the brain tissues is investigated analytically and numerically. The brain is modeled by three layers consisting of skull, grey and white matter. First, we have analytically calculated the microwave reflection, transmission, and absorption coefficients using signal flow graph technique. The effect of microwave frequency and variations in the thickness of layers on the propagation of microwave through brain are studied. Then, the penetration of microwave in the layers is numerically investigated by Monte Carlo method. It is shown that the analytical results are in good agreement with those obtained by Monte Carlo method. Our results indicate the absorbed microwave energy depends on microwave frequency and thickness of brain layers, and the absorption coefficient is optimized at a number of frequencies. These findings can be used for comparing the microwave absorbed energy in a child's and adult's brain.

[Determination of benzo(alpha)pyrene in food with microwave-assisted extraction].

PubMed

Zhou, Na; Luo, He-Dong; Li, Na; Li, Yao-Qun

2014-03-01

Coupling derivative technique and constant-energy synchronous fluorescence scanning technique, a method of determining benzo[alpha] pyrene in foods by second derivative constant-energy synchronous spectrofluorimetry after microwave-assisted treatment of samples was established using domestic microwave oven. The main factors of influencing the efficiency of microwave extraction were discussed, including the extraction solvent types and amounts, the microwave extraction time, microwave radiation power and cooling time. And the comparison with ultrasonic extraction was made. Low-fat food samples, which were just microwave-extracted with mixed-solvents, could be analyzed immediately by the spectrofluorimetric technique. For high-fat food samples, microwave-assisted saponification and extraction were made at the same time, thus simplifying operation steps and reducing sample analysis time. So the whole sample analysis process could be completed within one hour. This method was simple, rapid and inexpensive. In consequence, it was applied to determine benzo(a)pyrene in food with good reproducibility and the recoveries of benzo(alpha) pyrene ranged from 90.0% to 105.0% for the low fat samples and 83.3% to 94.6% for high-fat samples.

Microwave-induced electrostatic etching: generation of highly reactive magnesium for application in Grignard reagent formation.

PubMed

van de Kruijs, Bastiaan H P; Dressen, Mark H C L; Meuldijk, Jan; Vekemans, Jef A J M; Hulshof, Lumbertus A

2010-04-07

A detailed study regarding the influence of microwave irradiation on the formation of a series of Grignard reagents in terms of rates and selectivities has revealed that these heterogeneous reactions may display a beneficial microwave effect. The interaction between microwaves and magnesium turnings generates violent electrostatic discharges. These discharges on magnesium lead to melting of the magnesium surface, thus generating highly active magnesium particles. As compared to conventional operation the microwave-induced discharges on the magnesium surface lead to considerably shorter initiation times for the insertion of magnesium in selected substrates (i.e. halothiophenes, halopyridines, octyl halides, and halobenzenes). Thermographic imaging and surface characterization by scanning electron microscopy showed that neither selective heating nor a "specific" microwave effect was causing the reduction in initiation times. This novel and straightforward initiation method eliminates the use of toxic and environmentally adverse initiators. Thus, this initiation method limits the formation of by-products. We clearly demonstrated that microwave irradiation enables fast Grignard reagent formation. Therefore, microwave technology is promising for process intensification of Grignard based coupling reactions.

Effective moisture diffusivity and activation energy of rambutan seed under different drying methods to promote storage stability

NASA Astrophysics Data System (ADS)

Ahmad, So'bah; Shamsul Anuar, Mohd; Saleena Taip, Farah; Shamsudin, Rosnah; M, Siti Roha A.

2017-05-01

The effects of two drying methods, oven and microwave drying on the effective moisture diffusivity and activation energy of rambutan seed were studied. Effective moisture diffusivity and activation energy are the main indicators used for moisture movement within the material. Hence, it is beneficial to determine an appropriate drying method to attain a final moisture content of rambutan seed that potentially could be used as secondary sources in the industry. An appropriate final moisture content will provide better storage stability that can extend the lifespan of the rambutan seed. The rambutan seeds were dried with two drying methods (oven and microwave) at two level of the process variables (oven temperature; 40°C and 60°C and microwave power; 250W and 1000W) at constant initial moisture contents. The result showed that a higher value of effective moisture diffusivity and less activation energy were observed in microwave drying compared to oven drying. This finding portrays microwave drying expedites the moisture removal to achieve the required final moisture content and the most appropriate drying method for longer storage stability for rambutan seed. With respect to the process variables; higher oven temperatures and lower microwave powers also exhibit similar trends. Hopefully, this study would provide a baseline data to determine an appropriate drying method for longer storage period for turning waste to by-products.

Measurement of protein digestibility in humans by a dual-tracer method.

PubMed

Devi, Sarita; Varkey, Aneesia; Sheshshayee, M S; Preston, Thomas; Kurpad, Anura V

2018-06-01

Recent evaluations of the risk of dietary protein deficiency have indicated that protein digestibility may be a key limiting factor in the provision of indispensable amino acids (IAAs), particularly for vulnerable populations living in challenging environments where intestinal dysfunction may exist. Since the digestion of protein occurs only in the small intestine, and the metabolic activity of colonic bacteria confounds measurements at the fecal level, there is a need to develop noninvasive protein digestibility measurements at the ileal level. We used a dual-tracer method with stable isotopes to characterize the digestibility of uniformly labeled [13C]-spirulina protein as a standard protein, in comparison to a mixture of 2H-labeled crystalline amino acids, and then demonstrated the use of this standard protein to measure the digestibility of selected legumes (chick pea and mung bean) through the use of proteins that were intrinsically labeled with 2H. The digestibility of uniformly labeled [13C]-spirulina was first measured in 6 healthy volunteers (3 males and 3 females) by feeding it along with a standard mixture of 2H-labeled amino acids, in a dual-tracer, plateau-fed test meal approach. Next, intrinsically labeled legume protein digestibility was studied with a similar dual-tracer approach, with uniformly labeled [13C]-spirulina as the standard, when processed differently before consumption. The average digestibility of IAA in spirulina protein was 85.2%. The average IAA digestibility of intrinsically 2H-labeled chick pea and mung bean protein was 56.6% and 57.7%, respectively. Dehulling of mung bean before ingestion increased the average IAA digestibility by 9.9% in comparison to whole mung bean digestibility. An innovative, minimally invasive "dual-stable-isotope" method was developed to measure protein digestibility, in which the ingestion of an intrinsically 2H-labeled test protein along with a 13C-labeled standard protein of known digestibility allows for an accurate measure of digestion and absorption of the intrinsically labeled protein. This minimally invasive method is critical to redefining protein quality and will aid in revisiting human protein requirements in different settings and in vulnerable populations. This trial was registered at Clinical Trials Registry-India as CTRI/2017/11/010468.

Synthesis of hexagonal wurtzite Cu{sub 2}ZnSnS{sub 4} prisms by an ultrasound-assisted microwave solvothermal method

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

Long, Fei, E-mail: long.drf@gmail.com; Chi, Shangsen; Institute of Advanced Materials and Technology, University of Science and Technology Beijing, Beijing 100083

Wurtzite Cu{sub 2}ZnSnS{sub 4} (CZTS) hexagonal prisms were synthesized by a simple ultrasound-microwave solvothermal method. The product was characterized by XRD, FESEM, EDS, TEM, Raman and UV–vis spectrometer. The hexagonal prisms were 0.5–2 μm wide and 5–12 μm long. The PVP played an important role in the formation of the CZTS hexagonal prisms. In addition, the ultrasound-assisted microwave process was helpful for synthesis of wurtzite rather than kesterite phase CZTS. A nucleation–dissolution–recrystallization mechanism was also proposed to explain the growth of the CZTS hexagonal prisms. - Graphical abstract: Wurtzite Cu{sub 2}ZnSnS{sub 4} hexagonal prisms were synthesized by ultrasound-microwave solvothermal method.more » The ultrasound-assisted microwave process and PVP were useful to the growth of CZTS. A nucleation–dissolution–recrystallization growth mechanism was also proposed. - Highlights: • Wurtzite Cu{sub 2}ZnSnS{sub 4} was prepared by ultrasound-assisted microwave solvothermal method. • The wurtzite CZTS hexagonal prisms are demonstrated a band gap of 1.49 eV. • Synergistic effect of ultrasound and microwave is helpful to prepare Wurtzite CZTS. • PVP plays an important role in the formation of the CZTS hexagonal prisms. • Nucleation–dissolution–recrystallization growth mechanism of the CZTS was proposed.« less

Rapid micro-scale proteolysis of proteins for MALDI-MS peptide mapping using immobilized trypsin

NASA Astrophysics Data System (ADS)

Gobom, Johan; Nordhoff, Eckhard; Ekman, Rolf; Roepstorff, Peter

1997-12-01

In this study we present a rapid method for tryptic digestion of proteins using micro-columns with enzyme immobilized on perfusion chromatography media. The performance of the method is exemplified with acyl-CoA-binding protein and reduced carbamidomethylated bovine serum albumin. The method proved to be significantly faster and yielded a better sequence coverage and an improved signal-to-noise ratio for the MALDI-MS peptide maps, compared to in-solution- and on-target digestion. Only a single sample transfer step is required, and therefore sample loss due to adsorption to surfaces is reduced, which is a critical issue when handling low picomole to femtomole amounts of proteins. An example is shown with on-column proteolytic digestion and subsequent elution of the digest into a reversed-phase micro-column. This is useful if the sample contains large amounts of salt or is too diluted for MALDI-MS analysis. Furthermore, by step-wise elution from the reversedphase column, a complex digest can be fractionated, which reduces signal suppression and facilitates data interpretation in the subsequent MS-analysis. The method also proved useful for consecutive digestions with enzymes of different cleavage specificity. This is exemplified with on-column tryptic digestion, followed by reversed-phase step-wise elution, and subsequent on-target V8 protease digestion.

Several methods to determine heavy metals in the human brain

NASA Astrophysics Data System (ADS)

Andrási, Erzsébet; Igaz, Sarolta; Szoboszlai, Norbert; Farkas, Éva; Ajtony, Zsolt

1999-05-01

The determination of naturally occurring heavy metals in various parts of the human brain is discussed. The patients had no diseases in their central nervous systems (five individuals, mean age 70 years). Twenty brain parts were selected from both hemispheres. The analysis was carried out by graphite furnace atomic absorption spectrometry, inductively coupled plasma atomic emission spectrometry and instrumental neutron activation analysis methods. Accuracy and precision of the applied techniques were tested by using standard reference materials. Two digestion methods were used to dissolve the brain samples for ICP-AES and GF-AAS. One was performed in a Parr-bomb and the second in a microwave oven. The present results show a non-homogeneous distribution of the essential elements (Cu, Fe, Mn, Zn) in normal human brain. Corresponding regions in both hemispheres showed an almost identical concentration of these elements. In the case of toxic elements (Pb, Cd) an average value in different brain regions can not be established because of the high variability of individual data. This study indicates that beside differences in Pb and Cd intake with foods or cigarette smoke inhalation, the main factors of the high inter-individual variability of these element concentrations in human brain parts may be a marked difference in individual elimination or accumulation capabilities.

Direct determination of cadmium in foods by solid sampling electrothermal vaporization inductively coupled plasma mass spectrometry using a tungsten coil trap

NASA Astrophysics Data System (ADS)

Zhang, Ying; Mao, Xuefei; Liu, Jixin; Wang, Min; Qian, Yongzhong; Gao, Chengling; Qi, Yuehan

2016-04-01

In this work, a solid sampling device consisting of a tungsten coil trap, porous carbon vaporizer and on-line ashing furnace of a Ni-Cr coil was interfaced with inductively coupled plasma mass spectrometry (ICP-MS). A modified double gas circuit system was employed that was composed of carrier and supplemental gas lines controlled by separate gas mass flow controllers. For Cd determination in food samples using the assembled solid sampling ICP-MS, the optimal ashing and vaporization conditions, flow rate of the argon-hydrogen (Ar/H2) (v:v = 24:1) carrier gas and supplemental gas, and minimum sampling mass were investigated. Under the optimized conditions, the limit of quantification was 0.5 pg and the relative standard deviation was within a 10.0% error range (n = 10). Furthermore, the mean spiked recoveries for various food samples were 99.4%-105.9% (n = 6). The Cd concentrations measured by the proposed method were all within the certified values of the reference materials or were not significantly different (P > 0.05) from those of the microwave digestion ICP-MS method, demonstrating the good accuracy and precision of the solid sampling ICP-MS method for Cd determination in food samples.

Microwave absorption properties of gold nanoparticle doped polymers

NASA Astrophysics Data System (ADS)

Jiang, C.; Ouattara, L.; Ingrosso, C.; Curri, M. L.; Krozer, V.; Boisen, A.; Jakobsen, M. H.; Johansen, T. K.

2011-03-01

This paper presents a method for characterizing microwave absorption properties of gold nanoparticle doped polymers. The method is based on on-wafer measurements at the frequencies from 0.5 GHz to 20 GHz. The on-wafer measurement method makes it possible to characterize electromagnetic (EM) property of small volume samples. The epoxy based SU8 polymer and SU8 doped with gold nanoparticles are chosen as the samples under test. Two types of microwave test devices are designed for exciting the samples through electrical coupling and magnetic coupling, respectively. Measurement results demonstrate that the nanocomposites absorb a certain amount of microwave energy due to gold nanoparticles. Higher nanoparticle concentration results in more significant absorption effect.

Microwave-Assisted Hydro-Distillation of Essential Oil from Rosemary: Comparison with Traditional Distillation

PubMed Central

Moradi, Sara; Fazlali, Alireza; Hamedi, Hamid

Background: Hydro-distillation (HD) method is a traditional technique which is used in most industrial companies. Microwave-assisted Hydro-distillation (MAHD) is an advanced HD technique utilizing a microwave oven in the extraction process. Methods: In this research, MAHD of essential oils from the aerial parts (leaves) of rosemary (Rosmarinus officinalis L.) was studied and the results were compared with those of the conventional HD in terms of extraction time, extraction efficiency, chemical composition, quality of the essential oils and cost of the operation. Results: Microwave hydro-distillation was superior in terms of saving energy and extraction time (30 min, compared to 90 min in HD). Chromatography was used for quantity analysis of the essential oils composition. Quality of essential oil improved in MAHD method due to an increase of 17% in oxygenated compounds. Conclusion: Consequently, microwave hydro-distillation can be used as a substitute of traditional hydro-distillation. PMID:29296263

Evaluation of a High Intensity Focused Ultrasound-Immobilized Trypsin Digestion and 18O-Labeling Method for Quantitative Proteomics

PubMed Central

López-Ferrer, Daniel; Hixson, Kim K.; Smallwood, Heather; Squier, Thomas C.; Petritis, Konstantinos; Smith, Richard D.

2009-01-01

A new method that uses immobilized trypsin concomitant with ultrasonic irradiation results in ultra-rapid digestion and thorough 18O labeling for quantitative protein comparisons. The reproducible and highly efficient method provided effective digestions in <1 min with a minimized amount of enzyme required compared to traditional methods. This method was demonstrated for digestion of both simple and complex protein mixtures, including bovine serum albumin, a global proteome extract from the bacteria Shewanella oneidensis, and mouse plasma, as well as 18O labeling of such complex protein mixtures, which validated the application of this method for differential proteomic measurements. This approach is simple, reproducible, cost effective, rapid, and thus well-suited for automation. PMID:19555078

Electric field measurement in microwave discharge ion thruster with electro-optic probe.

PubMed

Ise, Toshiyuki; Tsukizaki, Ryudo; Togo, Hiroyoshi; Koizumi, Hiroyuki; Kuninaka, Hitoshi

2012-12-01

In order to understand the internal phenomena in a microwave discharge ion thruster, it is important to measure the distribution of the microwave electric field inside the discharge chamber, which is directly related to the plasma production. In this study, we proposed a novel method of measuring a microwave electric field with an electro-optic (EO) probe based on the Pockels effect. The probe, including a cooling system, contains no metal and can be accessed in the discharge chamber with less disruption to the microwave distribution. This method enables measurement of the electric field profile under ion beam acceleration. We first verified the measurement with the EO probe by a comparison with a finite-difference time domain numerical simulation of the microwave electric field in atmosphere. Second, we showed that the deviations of the reflected microwave power and the beam current were less than 8% due to inserting the EO probe into the ion thruster under ion beam acceleration. Finally, we successfully demonstrated the measurement of the electric-field profile in the ion thruster under ion beam acceleration. These measurements show that the electric field distribution in the thruster dramatically changes in the ion thruster under ion beam acceleration as the propellant mass flow rate increases. These results indicate that this new method using an EO probe can provide a useful guide for improving the propulsion of microwave discharge ion thrusters.

Evaluation of the PrioCHECK™ Trichinella AAD Kit for the digestion and recovery of larvae in pork, horse meat and wild meat.

PubMed

Konecsni, Kelly; Scheller, Cheryl; Scandrett, Brad; Buholzer, Patrik; Gajadhar, Alvin

2017-08-30

The artificial digestion magnetic stirrer method using pepsin protease and hydrochloric acid is the standard assay for the detection of Trichinella larvae in muscle of infected animals. Recently, an alternative enzyme, serine protease, was employed in the development of a commercially available digestion kit (PrioCHECK™ Trichinella AAD Kit). This assay requires a higher digestion temperature of 60°C which kills the larvae during the digestion process, mitigating the risk of environmental contamination from the parasite. The present study was conducted to determine the performance of the PrioCHECK™ Trichinella AAD Kit compared to the conventional pepsin/HCl digestion. Replicate paired 115g samples of Trichinella-negative pork diaphragm and masseter, and of horse tongue and masseter, were used to compare the two methods for tissue digestibility. Similarly, paired 100g samples of pork diaphragm and horse tongue were spiked with proficiency samples containing known numbers of Trichinella spiralis first stage larvae to compare larval recoveries for the two methods. Masseter samples from wild bears and wolves naturally infected with Trichinella nativa or T6 were also used to compare the performance of the methods. The results of the study showed that the PrioCHECK™ Trichinella AAD Kit, when used according to the manufacturer's instructions, was effective in detecting Trichinella infection in all samples that contained 0.05 or more larvae per gram of tissue. Although there was no significant difference between the Kit method and the standard pepsin/HCl digestion procedure in the average number of larvae recovered from spiked pork diaphragm, 38% fewer larvae were recovered from similarly spiked samples of horse tongue by digestion using serine protease (one way ANOVA, P value <0.001). Additional clarification was also more often required for both horse meat and pork when using the Kit compared to the pepsin/HCl method. The results of testing wildlife samples were similar for the two methods. Overall, the performance of the Kit method was suitable for the digestion of muscle samples and recovery of Trichinella larvae, according to international standards. It also provides advantages of faster digestion, safer reagents and recovered parasites that are non-hazardous for analysts and the environment. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

Research progress on the effect of microwave sterilization on agricultural products quality

NASA Astrophysics Data System (ADS)

Zhu, Xiang-hao; Yang, Yu-xia; Duan, Zhen-hua

2018-02-01

Different sterilization methods have different effects on the quality of agricultural products, microwave sterilization inhibited or eliminated microorganism by the use of microwave thermal effects and non-thermal. In this paper, the effects of microwave sterilization on the quality of fruits and vegetables, dairy, meat, grain, aquatic products and other agricultural products were introduced, and the possible development trends of microwave sterilization in agricultural products processing application were put forward.

Microbial communities in liquid and fiber fractions of food waste digestates are differentially resistant to inhibition by ammonia.

PubMed

Peng, Wei; Lü, Fan; Shao, Liming; He, Pinjing

2015-04-01

The effect of different concentrations of ammonia (1.0-7.0 g/L) during mesophilic anaerobic digestion with fiber or liquid digestate as inoculum was examined. Evolution of microbial community within fiber and liquid digestates was quantitatively assessed by the intact lipid analysis methods and qualitatively by DNA fingerprint methods in order to determine their resistance to ammonia inhibition. The results showed that an increased level of total ammonia nitrogen prolonged the lag phase of fiber digestates while reduced the metabolic rate of liquid digestates. Fiber digestates had 19.6-50.9-fold higher concentrations of phospholipid fatty acids (PLFA) compared to liquid digestates, whereas concentrations of phospholipid ether lipids (PLEL) in the fiber digestates were only 2.91-17.6-fold higher compared to liquid digestates. Although the cell concentration in liquid fraction was far lower than that in the fiber one, the ammonia-resistant ability and the methanization efficiency of the liquid digestate was superior to the fiber digestate. The bacterial profiles were affected more by the type of digestate inoculum compared to the concentration of ammonia. Principal component analysis indicated that the lipids technique was superior to the DNA technique for bacterial quantification but detected less archaeal diversity.

An Evaluation of Partial Digestion Protocols for the Extraction and Measurement of Trace Metals of Environmental Concern in Marine and Estuarine Sediments

NASA Astrophysics Data System (ADS)

Winters, S. J.; Krahforst, C.; Sherman, L.; Kehm, K.

2013-12-01

As part of a broad study of the fate and transport of trace metals in estuarine sediments (Krahforst et al., 2013), the efficacy of commonly-used partial digestion protocols, including ISO 11466 (treatment with aqua regia), EPA 3050B (nitric acid followed by H2O2) and a modified rock digestion method ('RD' method- H2O2 followed by nitric), were evaluated for two NIST SRM materials, marine sediment 2702 and estuarine sediment 1646a. Unlike so-called total sediment digestions, the methods studied in this work do not employ hydrofluoric acid and are thought to leave silicates substantially or wholly intact. These methods can in principle compliment studies based on total digestions by providing information about trace metals in phases that are potentially more labile in the marine environment. Samples were digested in ~150 mg aliquots. Application of ISO 11466 and EPA 3050B followed published protocols except that digestions were carried out in trace-metal clean 15 mL capped Teflon vessels in an Al block digester and, at the end of the procedure, the supernatant was decanted from undigested material following repeated centrifugation in 2% nitric acid. Digested solutions were analyzed for Al, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Ag, Cd, Sn and Pb content by ICPMS. All elements were analyzed in collision reaction cell mode to minimize isobaric interferences, except Cd and Ag, which were analyzed in standard mode. Instrument performance was monitored in-run by analyzing the SRM 1643e and several quality-check standards. Two repeated digestions of SRM 2702 and SRM 1646a using EPA 3050B produced identical yields, within the standard deviation of repeated analyses (0 - 5%), for all analyzed elements except Cu, which varied by 30% for SRM 2702. The same was true for ISO 11466, although the standard deviation of repeated analyses for this digestion series tended to be larger (< ~15%). The RD method, which consists of pre-treatment with H2O2 followed by repeated treatments with nitric acid, produced the highest average yields for all elements, ranging from 50% of the Al in SRM 2702 up to ~100% for Cd and Pb. The higher recoveries for the RD method may indicate that pre-treatment with H2O2 more effectively removes organics compared with the conventional methods. Yields for ISO 11466 digestions typically range from 5 - 15% higher than EPA 3050B for all studied elements. Comparisons between the two sediments demonstrated that the acid-extractable fraction differs for several elements. For example results from all three digestion methods confirm a ~40% difference in yield for Mn between SRM 2702 and SRM 1646a. Overall, the results indicate that yields for trace element analyses of marine and estuarine sediments resulting from partial digestion are sensitive to the digestion technique, and in particular the methods employed for removal of organic phases. This work was supported by NSF Grant EAR-0922733 and a Maryland Sea Grant Program Development Award.

A Blade Tip Timing Method Based on a Microwave Sensor

PubMed Central

Zhang, Jilong; Duan, Fajie; Niu, Guangyue; Jiang, Jiajia; Li, Jie

2017-01-01

Blade tip timing is an effective method for blade vibration measurements in turbomachinery. This method is increasing in popularity because it is non-intrusive and has several advantages over the conventional strain gauge method. Different kinds of sensors have been developed for blade tip timing, including optical, eddy current and capacitance sensors. However, these sensors are unsuitable in environments with contaminants or high temperatures. Microwave sensors offer a promising potential solution to overcome these limitations. In this article, a microwave sensor-based blade tip timing measurement system is proposed. A patch antenna probe is used to transmit and receive the microwave signals. The signal model and process method is analyzed. Zero intermediate frequency structure is employed to maintain timing accuracy and dynamic performance, and the received signal can also be used to measure tip clearance. The timing method uses the rising and falling edges of the signal and an auto-gain control circuit to reduce the effect of tip clearance change. To validate the accuracy of the system, it is compared experimentally with a fiber optic tip timing system. The results show that the microwave tip timing system achieves good accuracy. PMID:28492469

A Blade Tip Timing Method Based on a Microwave Sensor.

PubMed

Zhang, Jilong; Duan, Fajie; Niu, Guangyue; Jiang, Jiajia; Li, Jie

2017-05-11

Blade tip timing is an effective method for blade vibration measurements in turbomachinery. This method is increasing in popularity because it is non-intrusive and has several advantages over the conventional strain gauge method. Different kinds of sensors have been developed for blade tip timing, including optical, eddy current and capacitance sensors. However, these sensors are unsuitable in environments with contaminants or high temperatures. Microwave sensors offer a promising potential solution to overcome these limitations. In this article, a microwave sensor-based blade tip timing measurement system is proposed. A patch antenna probe is used to transmit and receive the microwave signals. The signal model and process method is analyzed. Zero intermediate frequency structure is employed to maintain timing accuracy and dynamic performance, and the received signal can also be used to measure tip clearance. The timing method uses the rising and falling edges of the signal and an auto-gain control circuit to reduce the effect of tip clearance change. To validate the accuracy of the system, it is compared experimentally with a fiber optic tip timing system. The results show that the microwave tip timing system achieves good accuracy.

Microwave-assisted routes for rapid and efficient modification of layered perovskites.

PubMed

Akbarian-Tefaghi, S; Wiley, J B

2018-02-27

Recent advances in exploiting microwave radiation in the topochemical modification of layered oxide perovskites are presented. Such methods work well for rapid bulk synthetic steps used in the production of novel inorganic-organic hybrids (protonation, grafting, intercalation, and in situ click reactions), exfoliation to produce dispersed nanosheets, and post-exfoliation processing to rapidly vary nanosheet surface groups. Compared to traditional methods that often take days, microwave methods can produce quality products in as little as 1-2 h.

Advanced Method of Boundary-Layer Control Based on Localized Plasma Generation

DTIC Science & Technology

2009-05-01

measurements, validation of experiments, wind-tunnel testing of the microwave / plasma generation system , preliminary assessment of energy required...and design of a microwave generator , electrodynamic and multivibrator systems for experiments in the IHM-NAU wind tunnel: MW generator and its high...equipped with the microwave - generation and protection systems to study advanced methods of flow control (Kiev) Fig. 2.1,a. The blade

Microwave heating inactivates Shiga Toxin (Stx2) in reconstituted fat-free Milk and adversely affects the nutritional value of cell culture medium

USDA-ARS?s Scientific Manuscript database

Microwave exposure is a convenient and widely used method for defrosting, heating, and cooking numerous foods. Microwave cooking is also reported to kill pathogenic microorganisms that often contaminate food. Microwaves act by causing polar molecules in food, such as water, to rapidly rotate, thus...

Performance Evaluation of Existing Wedgewater and Vacuum-Assisted Bed Dewatering Systems

DTIC Science & Technology

1992-01-01

prior to dewatering by the wedgewater method. Of the 20 satisfied users, 11 preferred aerobic digestion , two employed anaerobic digestion, and seven...did not further process their sludge. Of the seven dissatisfied users, four used aerobic digestion and three employed anaerobic digestion. A meelic...queried, 11 employed aerobic digestion , two employed anaerobic digestion, and three did not process their sludge. Eight dissatisfied users employed

Method for curing polymers using variable-frequency microwave heating

DOEpatents

Lauf, R.J.; Bible, D.W.; Paulauskas, F.L.

1998-02-24

A method for curing polymers incorporating a variable frequency microwave furnace system designed to allow modulation of the frequency of the microwaves introduced into a furnace cavity is disclosed. By varying the frequency of the microwave signal, non-uniformities within the cavity are minimized, thereby achieving a more uniform cure throughout the workpiece. A directional coupler is provided for detecting the direction of a signal and further directing the signal depending on the detected direction. A first power meter is provided for measuring the power delivered to the microwave furnace. A second power meter detects the magnitude of reflected power. The furnace cavity may be adapted to be used to cure materials defining a continuous sheet or which require compressive forces during curing. 15 figs.

In vitro digestibility of goat milk and kefir with a new standardised static digestion method (INFOGEST cost action) and bioactivities of the resultant peptides.

PubMed

Nehir El, Sedef; Karakaya, Sibel; Simsek, Sebnem; Dupont, Didier; Menfaatli, Esra; Eker, Alper Tolga

2015-07-01

The hydrolysis degrees of goat milk and kefir during simulated gastrointestinal digestion and some bioactivities of the resulting peptides after fermentation and digestion were studied. A static in vitro digestion method by the COST FA1005 Action INFOGEST was used and goat milk and kefir were partially hydrolyzed during the gastric phase and had above 80% hydrolysis after duodenal digestion. There were no differences between the digestibility of goat milk and kefir (p > 0.05). Goat milk and kefir displayed about 7-fold antioxidant activity after digestion (p < 0.05). Fermentation showed no effect on the calcium-binding capacity of the samples (p > 0.05), however, after in vitro digestion calcium-binding capacity of the goat milk and kefir increased 2 and 5 fold, respectively (p < 0.05). Digested goat milk and kefir showed a higher dose-dependent inhibitory effect on α-amylase compared to undigested samples (p < 0.05). α-Glucosidase inhibitory activities and in vitro bile acid-binding capacities of the samples were not determined at the studied concentrations.

Microwave-assisted extraction of pectin from cocoa peel

NASA Astrophysics Data System (ADS)

Sarah, M.; Hanum, F.; Rizky, M.; Hisham, M. F.

2018-02-01

Pectin is a polymer of d-galacturonate acids linked by β-1,4 glycosidic bond. This study isolates pectin from cocoa peel (Theobroma cacao) using citric acid as solvent by microwave-assisted extraction method. Cocoa peels (moisture content of 10%) with citric acid solution (pH of 1.5) irradiated by microwave energy at various microwave power (180, 300, 450 and 600 W) for 10, 15, 20, 25 and 30 minutes respectively. Pectin obtained from this study was collected and filtrated by adding 96% ethanol to precipitate the pectin. The best results obtained from extraction process using microwave power of 180 Watt for 30 minutes. This combination of power and time yielded 42.3% pectin with moisture content, ash content, weight equivalent, methoxyl content and galacturonate levels were 8.08%, 5%, 833.33 mg, 6.51% and 58,08%, respectively. The result finding suggested that microwave-assisted extraction method has a great potency on the commercial pectin production.

Green procedure with a green solvent for fats and oils' determination. Microwave-integrated Soxhlet using limonene followed by microwave Clevenger distillation.

PubMed

Virot, Matthieu; Tomao, Valérie; Ginies, Christian; Visinoni, Franco; Chemat, Farid

2008-07-04

Here is described a green and original alternative procedure for fats and oils' determination in oleaginous seeds. Extractions were carried out using a by-product of the citrus industry as extraction solvent, namely d-limonene, instead of hazardous petroleum solvents such as n-hexane. The described method is achieved in two steps using microwave energy: at first, extractions are attained using microwave-integrated Soxhlet, followed by the elimination of the solvent from the medium using a microwave Clevenger distillation in the second step. Oils extracted from olive seeds were compared with both conventional Soxhlet and microwave-integrated Soxhlet extraction procedures performed with n-hexane in terms of qualitative and quantitative determination. No significant difference was obtained between each extract allowing us to conclude that the proposed method is effective and valuable.

Comparison of three methods for the detection of Trichinella spiralis infections in pigs by five European laboratories*

PubMed Central

Kohler, G.; Ruitenberg, E. J.

1974-01-01

Three methods employed in the diagnosis of trichinosis (trichinoscopy, digestion method, and immunofluorescence technique) were compared by laboratories in 5 countries of the European economic community. For this purpose, material from 32 pigs infected with 50, 150, 500, and 1 500 T. spiralis larvae was examined. With none of the three methods was it possible to detect with sufficient reliability a T. spiralis infection in pigs infected with 50 larvae. The digestion method and the immunofluorescence technique yielded more reliable results when the infection dose was 150 larvae or more. With trichinoscopy, reliable results were obtained in pigs infected with 500 and 1 500 larvae. With the digestion method and trichinoscopy, the onset of infections was detectable from 3 weeks post infection, the digestion method being more reliable; the immunofluorescence technique yielded positive results from approximately 4-6 weeks post infection. The immunofluorescence technique is applicable for epidemiological surveys. As a routine diagnostic procedure in the slaughterhouse, trichinoscopy and the digestion method are possible alternatives, the latter being more sensitive. PMID:4616776

Quantitative Assessment of In-solution Digestion Efficiency Identifies Optimal Protocols for Unbiased Protein Analysis*

PubMed Central

León, Ileana R.; Schwämmle, Veit; Jensen, Ole N.; Sprenger, Richard R.

2013-01-01

The majority of mass spectrometry-based protein quantification studies uses peptide-centric analytical methods and thus strongly relies on efficient and unbiased protein digestion protocols for sample preparation. We present a novel objective approach to assess protein digestion efficiency using a combination of qualitative and quantitative liquid chromatography-tandem MS methods and statistical data analysis. In contrast to previous studies we employed both standard qualitative as well as data-independent quantitative workflows to systematically assess trypsin digestion efficiency and bias using mitochondrial protein fractions. We evaluated nine trypsin-based digestion protocols, based on standard in-solution or on spin filter-aided digestion, including new optimized protocols. We investigated various reagents for protein solubilization and denaturation (dodecyl sulfate, deoxycholate, urea), several trypsin digestion conditions (buffer, RapiGest, deoxycholate, urea), and two methods for removal of detergents before analysis of peptides (acid precipitation or phase separation with ethyl acetate). Our data-independent quantitative liquid chromatography-tandem MS workflow quantified over 3700 distinct peptides with 96% completeness between all protocols and replicates, with an average 40% protein sequence coverage and an average of 11 peptides identified per protein. Systematic quantitative and statistical analysis of physicochemical parameters demonstrated that deoxycholate-assisted in-solution digestion combined with phase transfer allows for efficient, unbiased generation and recovery of peptides from all protein classes, including membrane proteins. This deoxycholate-assisted protocol was also optimal for spin filter-aided digestions as compared with existing methods. PMID:23792921

Performance analysis of FET microwave devices by use of extended spectral-element time-domain method

NASA Astrophysics Data System (ADS)

Sheng, Yijun; Xu, Kan; Wang, Daoxiang; Chen, Rushan

2013-05-01

The extended spectral-element time-domain (SETD) method is employed to analyse field effect transistor (FET) microwave devices. In order to impose the contribution of the FET microwave devices into the electromagnetic simulation, the SETD method is extended by introducing a lumped current term into the vector Helmholtz equation. The change of currents on each lumped component can be expressed by the change of voltage via corresponding models of equivalent circuit. The electric fields around the lumped component must be influenced by the change of voltage on each lumped component, and vice versa. So a global coupling about the EM-circuit can be built directly. The fully explicit solving scheme is maintained in this extended SETD method and the CPU time can be saved spontaneously. Three practical FET microwave devices are analysed in this article. The numerical results demonstrate the ability and accuracy of this method.

Microwave-assisted Derivatization of Fatty Acids for Its Measurement in Milk Using High-Performance Liquid Chromatography.

PubMed

Shrestha, Rojeet; Miura, Yusuke; Hirano, Ken-Ichi; Chen, Zhen; Okabe, Hiroaki; Chiba, Hitoshi; Hui, Shu-Ping

2018-01-01

Fatty acid (FA) profiling of milk has important applications in human health and nutrition. Conventional methods for the saponification and derivatization of FA are time-consuming and laborious. We aimed to develop a simple, rapid, and economical method for the determination of FA in milk. We applied a beneficial approach of microwave-assisted saponification (MAS) of milk fats and microwave-assisted derivatization (MAD) of FA to its hydrazides, integrated with HPLC-based analysis. The optimal conditions for MAS and MAD were determined. Microwave irradiation significantly reduced the sample preparation time from 80 min in the conventional method to less than 3 min. We used three internal standards for the measurement of short-, medium- and long-chain FA. The proposed method showed satisfactory analytical sensitivity, recovery and reproducibility. There was a significant correlation in the milk FA concentrations between the proposed and conventional methods. Being quick, economic, and convenient, the proposed method for the milk FA measurement can be substitute for the convention method.

Rapid determination of the volatile components in tobacco by ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction with gas chromatography-mass spectrometry.

PubMed

Yang, Yanqin; Chu, Guohai; Zhou, Guojun; Jiang, Jian; Yuan, Kailong; Pan, Yuanjiang; Song, Zhiyu; Li, Zuguang; Xia, Qian; Lu, Xinbo; Xiao, Weiqiang

2016-03-01

An ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction was first employed to determine the volatile components in tobacco samples. The method combined the advantages of ultrasound, microwave, and headspace solid-phase microextraction. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, several experimental parameters, such as fiber type, ultrasound power, and irradiation time, were optimized to improve sampling efficiency. Under the optimal conditions, there were 37, 36, 34, and 36 components identified in tobacco from Guizhou, Hunan, Yunnan, and Zimbabwe, respectively, including esters, heterocycles, alkanes, ketones, terpenoids, acids, phenols, and alcohols. The compound types were roughly the same while the contents were varied from different origins due to the disparity of their growing conditions, such as soil, water, and climate. In addition, the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method was compared with the microwave-assisted extraction coupled to headspace solid-phase microextraction and headspace solid-phase microextraction methods. More types of volatile components were obtained by using the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method, moreover, the contents were high. The results indicated that the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction technique was a simple, time-saving and highly efficient approach, which was especially suitable for analysis of the volatile components in tobacco. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ciliate ingestion and digestion: flow cytometric measurements and regrowth of a digestion-resistant campylobacter jejuni

USDA-ARS?s Scientific Manuscript database

We developed a method to measure ingestion and digestion rates of bacterivorous protists feeding on pathogenic bacteria. We tested this method using the enteric bacteria Campylobacter jejuni and a freshwater colpodid ciliate. Campylobacter and a non-pathogenic bacteria isolated from the environment ...

Microwave-assisted solid phase conversion study of Meldrum's acid to ethylenetetracarboxylic dianhydride (C 6O 6)

NASA Astrophysics Data System (ADS)

Taherpour, Avat (Arman)

2010-01-01

Utilization of microwave irradiation provides an effective method for fast synthesizing of some important compounds. Microwave-assisted solid phase is an especial class in chemical synthesis. By the use of MW-irradiation on chemicals, sometimes interesting results can be seen. The synthesis of the interesting molecule ethylenetetracarboxylic dianhydride (C 6O 6) was attempted with a few different methods. In this study, the microwave-assisted solid phase conversion of Meldrum's acid to ethylenetetracarboxylic dianhydride was reported. This conversion was characterized by FT-IR, GC/MS and NMR spectroscopy results.

In vitro dynamic model simulating the digestive tract of 6-month-old infants.

PubMed

Passannanti, Francesca; Nigro, Federica; Gallo, Marianna; Tornatore, Fabio; Frasso, Annalisa; Saccone, Giulia; Budelli, Andrea; Barone, Maria V; Nigro, Roberto

2017-01-01

In vivo assays cannot always be conducted because of ethical reasons, technical constraints or costs, but a better understanding of the digestive process, especially in infants, could be of great help in preventing food-related pathologies and in developing new formulas with health benefits. In this context, in vitro dynamic systems to simulate human digestion and, in particular, infant digestion could become increasingly valuable. To simulate the digestive process through the use of a dynamic model of the infant gastroenteric apparatus to study the digestibility of starch-based infant foods. Using M.I.D.A (Model of an Infant Digestive Apparatus), the oral, gastric and intestinal digestibility of two starch-based products were measured: 1) rice starch mixed with distilled water and treated using two different sterilization methods (the classical method with a holding temperature of 121°C for 37 min and the HTST method with a holding temperature of 137°C for 70 sec) and 2) a rice cream with (premium product) or without (basic product) an aliquot of rice flour fermented by Lactobacillus paracasei CBA L74. After the digestion the foods were analyzed for the starch concentration, the amount of D-glucose released and the percentage of hydrolyzed starch. An in vitro dynamic system, which was referred to as M.I.D.A., was obtained. Using this system, the starch digestion occurred only during the oral and intestinal phase, as expected. The D-glucose released during the intestinal phase was different between the classical and HTST methods (0.795 grams for the HTST versus 0.512 for the classical product). The same analysis was performed for the basic and premium products. In this case, the premium product had a significant difference in terms of the starch hydrolysis percentage during the entire process. The M.I.D.A. system was able to digest simple starches and a more complex food in the correct compartments. In this study, better digestibility of the premium product was revealed.

1989 IEEE Aerospace Applications Conference, Breckenridge, CO, Feb. 12-17, 1989, Conference Digest

NASA Astrophysics Data System (ADS)

Recent advances in electronic devices for aerospace applications are discussed in reviews and reports. Topics addressed include large-aperture mm-wave antennas, a cross-array radiometer for spacecraft applications, a technique for computing the propagation characteristics of optical fibers, an analog light-wave system for improving microwave-telemetry data communication, and a ground demonstration of an orbital-debris radar. Consideration is given to a verifiable autonomous satellite control system, Inmarsat second-generation satellites for mobile communication, automated tools for data-base design and criteria for their selection, and a desk-top simulation work station based on the DSP96002 microprocessor chip.

Optimization of microwave assisted extraction of essential oils from Iranian Rosmarinus officinalis L. using RSM.

PubMed

Akhbari, Maryam; Masoum, Saeed; Aghababaei, Fahimeh; Hamedi, Sepideh

2018-06-01

In this study, the efficiencies of conventional hydro-distillation and novel microwave hydro-distillation methods in extraction of essential oil from Rosemary officinalis leaves have been compared. In order to attain the best yield and also highest quality of the essential oil in the microwave assisted method, the optimal values of operating parameters such as extraction time, microwave irradiation power and water volume to plant mass ratio were investigated using central composite design under response surface methodology. Optimal conditions for obtaining the maximum extraction yield in the microwave assisted method were predicted as follows: extraction time of 85 min, microwave power of 888 W, and water volume to plant mass ratio of 0.5 ml/g. The extraction yield at these predicted conditions was computed as 0.7756%. The qualities of the obtained essential oils under designed experiments were optimized based on total contents of four major compounds (α-pinene, 1,8-cineole, camphor and verbenone) which determined by gas chromatography equipped with mass spectroscopy (GC-MS). The highest essential oil quality (55.87%) was obtained at extraction time of 68 min; microwave irradiation power of 700 W; and water volume to plant mass ratio of zero.

Method and apparatus for measuring butterfat and protein content using microwave absorption techniques

DOEpatents

Fryer, Michael O.; Hills, Andrea J.; Morrison, John L.

2000-01-01

A self calibrating method and apparatus for measuring butterfat and protein content based on measuring the microwave absorption of a sample of milk at several microwave frequencies. A microwave energy source injects microwave energy into the resonant cavity for absorption and reflection by the sample undergoing evaluation. A sample tube is centrally located in the resonant cavity passing therethrough and exposing the sample to the microwave energy. A portion of the energy is absorbed by the sample while another portion of the microwave energy is reflected back to an evaluation device such as a network analyzer. The frequency at which the reflected radiation is at a minimum within the cavity is combined with the scatter coefficient S.sub.11 as well as a phase change to calculate the butterfat content in the sample. The protein located within the sample may also be calculated in a likewise manner using the frequency, S.sub.11 and phase variables. A differential technique using a second resonant cavity containing a reference standard as a sample will normalize the measurements from the unknown sample and thus be self-calibrating. A shuttered mechanism will switch the microwave excitation between the unknown and the reference cavities. An integrated apparatus for measuring the butterfat content in milk using microwave absorption techniques is also presented.

Microwave Sterilization in School Microbiology.

ERIC Educational Resources Information Center

Wynn, Brian; Dixon, Angela

1988-01-01

Described are two investigations carried out in a high school biology department using a domestic microwave oven to compare the relative attributes of the autoclave and microwave oven in school use. Discussed are equipment, methods, and results of each investigation. (Author/CW)

Development of microwave assisted spectrophotometric method for the determination of glucose

NASA Astrophysics Data System (ADS)

Ali, Asif; Hussain, Zahid; Arain, Muhammad Balal; Shah, Nasrullah; Khan, Khalid Mohammad; Gulab, Hussain; Zada, Amir

2016-01-01

A spectrophotometric method was developed based on the microwave assisted synthesis of Maillard product. Various conditions of the reaction were optimized by varying the relative concentration of the reagents, operating temperature and volume of solutions used in the reaction in the microwave synthesizer. The absorbance of the microwave synthesized Maillard product was measured in the range of 360-740 nm using UV-Visible spectrophotometer. Based on the maximum absorbance, 370 nm was selected as the optimum wave length for further studies. The LOD and LOQ of glucose was found 3.08 μg mL- 1 and 9.33 μg mL- 1 with standard deviation of ± 0.05. The developed method was also applicable to urine sample.

Environmentally friendly chemical recycling of poly(bisphenol-A carbonate) through phase transfer-catalysed alkaline hydrolysis under microwave irradiation.

PubMed

Tsintzou, Georgia P; Antonakou, Eleni V; Achilias, Dimitris S

2012-11-30

The various and widespread uses of polycarbonate (PC) polymers require a meaningful and environmentally friendly disposal method. In this study, depolymerisation of polycarbonate with water in a microwave reactor is suggested as a recycling method. Hydrolysis was investigated in an alkaline (NaOH) solution using a phase-transfer catalyst. All of the experiments were carried out in a sealed microwave reactor, in which the reaction pressure, temperature and microwave power were continuously controlled and recorded. In the hydrolysis products, bisphenol-A monomer was obtained and identified by FTIR measurements. PC degradation higher than 80% can be obtained at 160°C after a microwave irradiation time of either 40 min or 10 min using either a 5 or 10% (w/v) NaOH solution, respectively. GPC, TGA and DSC measurements of the PC residues revealed that surface erosion is the degradation mechanism. First-order reaction kinetics were estimated by implementing a simple kinetic model. Finally, greater than 85% degradation was achieved when waste CDs were treated with the same method. The results confirm the importance of the microwave power technique as a promising recycling method for PC-based waste plastics, resulting in monomer recovery in addition to substantial energy savings. Copyright © 2012 Elsevier B.V. All rights reserved.

1997 Technology Applications Report,

DTIC Science & Technology

1997-01-01

handle high -power loads at microwave radio frequencies , microwave vacuum tubes remain the chosen technology to amplify high power. Aria Microwave...structure called the active RF cavity amplifier (ARFCA). With this design , the amplifier handles high -power loads at radio and microwave frequencies ...developed this technology using BMDO-funded modeling methods designed to simulate the dynamics of large space-based structures. Because it increases

Effects of Low-Dose Microwave on Healing of Fractures with Titanium Alloy Internal Fixation: An Experimental Study in a Rabbit Model

PubMed Central

Zhang, Han; Fu, Tengfei; Jiang, Lan; Bai, Yuehong

2013-01-01

Background Microwave is a method for improving fracture repair. However, one of the contraindications for microwave treatment listed in the literature is surgically implanted metal plates in the treatment field. The reason is that the reflection of electromagnetic waves and the eddy current stimulated by microwave would increase the temperature of magnetic implants and cause heat damage in tissues. Comparing with traditional medical stainless steel, titanium alloy is a kind of medical implants with low magnetic permeability and electric conductivity. But the effects of microwave treatment on fracture with titanium alloy internal fixation in vivo were not reported. The aim of this article was to evaluate the security and effects of microwave on healing of a fracture with titanium alloy internal fixation. Methods Titanium alloy internal fixation systems were implanted in New Zealand rabbits with a 3.0 mm bone defect in the middle of femur. We applied a 30-day microwave treatment (2,450MHz, 25W, 10 min per day) to the fracture 3 days after operation. Temperature changes of muscle tissues around implants were measured during the irradiation. Normalized radiographic density of the fracture gap was measured on the 10th day and 30th day of the microwave treatment. All of the animals were killed after 10 and 30 days microwave treatment with histologic and histomorphometric examinations performed on the harvested tissues. Findings The temperatures did not increase significantly in animals with titanium alloy implants. The security of microwave treatment was also supported by histology of muscles, nerve and bone around the implants. Radiographic assessment, histologic and histomorphometric examinations revealed significant improvement in the healing bone. Conclusion Our results suggest that, in the healing of fracture with titanium alloy internal fixation, a low dose of microwave treatment may be a promising method. PMID:24086626

Quality factors in beef, pork, and lamb cooked by microwaves.

PubMed

Korschgen, B M; Baldwin, R E; Snider, S

1976-12-01

Three cooking treatments were applied to the longissimus muscle of beef and of pork and to deboned leg of lamb. Cooking treatments included: Intermittent energy application (3-min. cycle) with a microwave range operated at 220V and intermittent energy application (6-min. cycle) with a microwave range operated at 115V. Control roasts were cooked in a conventional gas oven (163+/-3 degrees C.). Cooking was adjusted so that roasts achieved an internal temperature of 70 degrees C. when cut for analyses. Cooking losses were significantly greater for microwave than for conventionally cooked beef. However, microwave cooking resulted in beef, pork, and lamb roasts with flavor of interior portions similar to those prepared conventionally. Flavor differences in samples from the edge of the slices of lamb and of pork and tenderness of lamb appeared to be related to cooking method. For these attributes, meat cooked conventionally was superior. In contrast, patterns in significant differences in tenderness and juiciness of beef and of pork were not consistent and were not related solely to method of cookery. Neither creatine nor creatinine was a good index of flavor of meat cooked by these methods. Aside from the time-saving aspect of microwave heating, there was no major advantage of one method of cooking over another. Thus, either high- or low- powered microwave equipment, operated at 2450 MHz, can be used satisfactorily for cooking tender cuts of beef, pork, and lamb.

First detection of lead in black paper from intraoral film: an environmental concern.

PubMed

Guedes, Débora F C; Silva, Reginaldo S; da Veiga, Márcia A M S; Pecora, Jesus D

2009-10-30

Lead (Pb) contamination in the black paper that recovers intraoral films (BKP) has been investigated. BKP samples were collected from the Radiology Clinics of the Dental School of Ribeirão Preto, University of São Paulo, Brazil. For sake of comparison, four different methods were used. The results revealed the presence of high lead levels, well above the maximum limit allowed by the legislation. Pb contamination levels achieved after the following treatments: paper digestion in nitric acid, microwave treatment, DIN38414-54 method and TCLP method were 997 microg g(-1), 189 microg g(-1), 20.8 microg g(-1), and 54.0 microg g(-1), respectively. Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma mass spectrometry (ICP-MS) were employed for lead determination according to the protocols of the applied methods. Lead contamination in used BKP was confirmed by scanning electron microscopy coupled with energy dispersive X-ray microanalysis (SEM-EDS). All the SEM imaging was carried out in the secondary electron mode (SE) and backscattered-electron mode (QBSD) following punctual X-ray fluorescence spectra. Soil contamination derived from this product revealed the urgent need of addressing this problem. These elevated Pb levels, show that a preliminary treatment of BKP is mandatory before it is disposed into the common trash. The high lead content of this material makes its direct dumping into the environment unwise.

The study on air pollution with nickel and vanadium in Croatia by using moss biomonitoring and ICP-AES.

PubMed

Vučković, Ivana; Špirić, Zdravko; Stafilov, Trajče; Kušan, Vladimir; Bačeva, Katerina

2013-10-01

Moss samples were collected from 121 sampling sites all over Croatia during the summer and autumn of 2010. They were totally digested by using microwave digestion system and analysed by using atomic emission spectrometry with inductively coupled plasma (ICP-AES). Descriptive statistics and maps of distribution were made. The data obtained in this study were compared with those from the study in 2006 and additionally with the data obtained in the similar studies in neighbouring countries and Norway as pristine area. The median value of nickel is 3.16 mg kg(-1) and the content varies from 1.04 to 14.66 mg kg(-1). The content of vanadium ranges between 0.23 and 37.26 mg kg(-1) with the median value of 2.55 mg kg(-1). High contents of these elements are found in the vicinity of Rijeka, Zagreb and Sisak as a result of their emission from oil refinery, thermal power plant and industrial processes.

Characterization of Toxic Metals in Tobacco, Tobacco Smoke, and Cigarette Ash from Selected Imported and Local Brands in Pakistan

PubMed Central

Ajab, Huma; Malik, Salman Akbar; Junaid, Muhammad; Yasmeen, Sadia; Abdullah, Mohd Azmuddin

2014-01-01

In this study, concentrations of Cd, Ni, Pb, and Cr were determined in tobacco, tobacco smoke-condensate, and cigarette ash for selected brands used in Pakistan. Smoking apparatus was designed for metal extraction from cigarette smoke. Samples were digested through microwave digester and then analyzed by flame atomic absorption spectrophotometer (FAAS). Higher concentration of Ni was detected in imported brands than the counterparts in the local brands. Pb levels were however higher in local brands while significant concentration of Cd was observed in both brands. For Cr, the level in tobacco of local brands was higher than their emitted smoke, whereas imported brands showed higher level in smoke than in tobacco. The cigarette ash retained 65 to 75% of the metal and about 25 to 30% went into the body. While this study revealed the serious requirement to standardize the manufacturing of tobacco products, more importantly is the urgent need for stronger enforcements to put in place to alert the general population about the hazardous effects of cigarettes and the health risks associated with these toxic metals. PMID:24672317

Occurrence of antibiotic resistance genes and mobile genetic elements in enterococci and genomic DNA during anaerobic digestion of pharmaceutical waste sludge with different pretreatments.

PubMed

Tong, Juan; Lu, XueTing; Zhang, JunYa; Sui, Qianwen; Wang, Rui; Chen, Meixue; Wei, Yuansong

2017-07-01

Pharmaceutical waste sludge harbors large amounts of antibiotic resistance genes (ARGs) and mobile genetic elements (MGEs), and it is necessary to study the reduction of ARGs and MGEs during sludge treatment. Therefore, the antibiotic resistance phenotypes and genotypes of enterococci, and the ARGs and MGEs in genomic DNA were investigated during anaerobic digestion (AD) with microwave (MW), thermal hydrolysis (TH) and ozone pretreatment. Results showed that sludge pretreatment increased the occurrence of the resistance phenotypes and genotypes of enterococci. During AD, the resistance of enterococci to macrolides decreased, except for in the MW-pretreated sludge. Horizontal gene transfer and co-occurrence of ermB and tetM in enterococci resulted in increased tetracycline resistance of enterococci throughout the sludge treatment. MGEs such as intI1, ISCR1 and Tn916/1545 had a significant effect on the distribution of ARGs. AD with pretreatment, especially TH pretreatment, resulted in greater ARGs and MGEs reduction and improved methane production. Copyright © 2017. Published by Elsevier Ltd.

Using microwave heating to improve the desorption efficiency of high molecular weight VOC from beaded activated carbon.

PubMed

Fayaz, Mohammadreza; Shariaty, Pooya; Atkinson, John D; Hashisho, Zaher; Phillips, John H; Anderson, James E; Nichols, Mark

2015-04-07

Incomplete regeneration of activated carbon loaded with organic compounds results in heel build-up that reduces the useful life of the adsorbent. In this study, microwave heating was tested as a regeneration method for beaded activated carbon (BAC) loaded with n-dodecane, a high molecular weight volatile organic compound. Energy consumption and desorption efficiency for microwave-heating regeneration were compared with conductive-heating regeneration. The minimum energy needed to completely regenerate the adsorbent (100% desorption efficiency) using microwave regeneration was 6% of that needed with conductive heating regeneration, owing to more rapid heating rates and lower heat loss. Analyses of adsorbent pore size distribution and surface chemistry confirmed that neither heating method altered the physical/chemical properties of the BAC. Additionally, gas chromatography (with flame ionization detector) confirmed that neither regeneration method detectably altered the adsorbate composition during desorption. By demonstrating improvements in energy consumption and desorption efficiency and showing stable adsorbate and adsorbent properties, this paper suggests that microwave heating is an attractive method for activated carbon regeneration particularly when high-affinity VOC adsorbates are present.

In vitro versus in vivo protein digestibility techniques for calculating PDCAAS (protein digestibility-corrected amino acid score) applied to chickpea fractions.

PubMed

Tavano, Olga Luisa; Neves, Valdir Augusto; da Silva Júnior, Sinézio Inácio

2016-11-01

Seven different in vitro methods to determine the protein digestibility for chickpea proteins were considered and also the application of these methodologies for calculating PDCAAS (protein digestibility-corrected amino acid score), seeking their correlations with the in vivo methodology. In vitro digestibility of raw and heated samples were determined using pepsin-pancreatin hydrolysis, considering soluble nitrogen via Kjeldahl (ppKJ) and hydrolysed peptide linkages using trinitrobenzenesulfonic acid and o-phthaldialdehyde. In vitro digestibility was also determined using trypsin, chymotrypsin and peptidase (3-Enz) or trypsin, chymotrypsin, peptidase and pronase solution (4-Enz). None of the correlations between in vitro and in vivo digestibilities were significant (at p<0.0500), but, strong correlations were observed between PDCAAS calculated by in vitro and in vivo results. PDCAAS-ppKJ, PDCAAS-3-Enz and PDCAAS-4-Enz presented the highest correlations with in vivo method, r=0.9316, 0.9442 and 0.9649 (p<0.0500), respectively. The use of in vitro methods for calculating PDCAAS may be promising and deserves more discussions. Copyright © 2016 Elsevier Ltd. All rights reserved.

Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Elements in Whole-Water Digests Using Inductively Coupled Plasma-Optical Emission Spectrometry and Inductively Coupled Plasma-Mass Spectrometry

USGS Publications Warehouse

Garbarino, John R.; Struzeski, Tedmund M.

1998-01-01

Inductively coupled plasma-optical emission spectrometry (ICP-OES) and inductively coupled plasma-mass spectrometry (ICP-MS) can be used to determine 26 elements in whole-water digests. Both methods have distinct advantages and disadvantages--ICP-OES is capable of analyzing samples with higher elemental concentrations without dilution, however, ICP-MS is more sensitive and capable of determining much lower elemental concentrations. Both techniques gave accurate results for spike recoveries, digested standard reference-water samples, and whole-water digests. Average spike recoveries in whole-water digests were 100 plus/minus 10 percent, although recoveries for digests with high dissolved-solid concentrations were lower for selected elements by ICP-MS. Results for standard reference-water samples were generally within 1 standard deviation of hte most probable values. Statistical analysis of the results from 43 whole-water digest indicated that there was no significant difference among ICP-OES, ICP-MS, and former official methods of analysis for 24 of the 26 elements evaluated.

Ignition methods and apparatus using microwave energy

DOEpatents

DeFreitas, Dennis Michael; Migliori, Albert

1997-01-01

An ignition apparatus for a combustor includes a microwave energy source that emits microwave energy into the combustor at a frequency within a resonant response of the combustor, the combustor functioning as a resonant cavity for the microwave energy so that a plasma is produced that ignites a combustible mixture therein. The plasma preferably is a non-contact plasma produced in free space within the resonant cavity spaced away from with the cavity wall structure and spaced from the microwave emitter.

Novel Multistatic Adaptive Microwave Imaging Methods for Early Breast Cancer Detection

NASA Astrophysics Data System (ADS)

Xie, Yao; Guo, Bin; Li, Jian; Stoica, Petre

2006-12-01

Multistatic adaptive microwave imaging (MAMI) methods are presented and compared for early breast cancer detection. Due to the significant contrast between the dielectric properties of normal and malignant breast tissues, developing microwave imaging techniques for early breast cancer detection has attracted much interest lately. MAMI is one of the microwave imaging modalities and employs multiple antennas that take turns to transmit ultra-wideband (UWB) pulses while all antennas are used to receive the reflected signals. MAMI can be considered as a special case of the multi-input multi-output (MIMO) radar with the multiple transmitted waveforms being either UWB pulses or zeros. Since the UWB pulses transmitted by different antennas are displaced in time, the multiple transmitted waveforms are orthogonal to each other. The challenge to microwave imaging is to improve resolution and suppress strong interferences caused by the breast skin, nipple, and so forth. The MAMI methods we investigate herein utilize the data-adaptive robust Capon beamformer (RCB) to achieve high resolution and interference suppression. We will demonstrate the effectiveness of our proposed methods for breast cancer detection via numerical examples with data simulated using the finite-difference time-domain method based on a 3D realistic breast model.

Preparation and microwave absorption properties of honeycomb core structures coated with composite absorber

NASA Astrophysics Data System (ADS)

Luo, Hui; Chen, Fu; Wang, Fang; Wang, Xian; Dai, Weiyong; Hu, Sheng; Gong, Rongzhou

2018-05-01

Honeycomb structure coated with paraffin filled with composite of graphene and flaky carbonyl iron powder (FCIP) as lossy filler have been studied. The composite of graphene/FCIP with different weight ratio were synthesized via mechanical milling, the electromagnetic properties of the samples were measured by transmission/reflection method in the frequency range of 8-12 GHz. The microwave absorbing properties of the microwave absorbing honeycomb structure (MAHS) and microwave absorbing honeycomb sandwich structure (MAHSS) were studied based on the Finite Element Method with periodical boundary conditions. The matching layer on the top of the honeycomb sandwich structure can enhanced the microwave absorption properties. It was shown that a light weight and broadband MAHSS could be implemented with the use of the magnetic material and dielectric material.

Method for curing polymers using variable-frequency microwave heating

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

Lauf, R.J.; Bible, D.W.; Paulauskas, F.L.

1998-02-24

A method for curing polymers incorporating a variable frequency microwave furnace system designed to allow modulation of the frequency of the microwaves introduced into a furnace cavity is disclosed. By varying the frequency of the microwave signal, non-uniformities within the cavity are minimized, thereby achieving a more uniform cure throughout the workpiece. A directional coupler is provided for detecting the direction of a signal and further directing the signal depending on the detected direction. A first power meter is provided for measuring the power delivered to the microwave furnace. A second power meter detects the magnitude of reflected power. Themore » furnace cavity may be adapted to be used to cure materials defining a continuous sheet or which require compressive forces during curing. 15 figs.« less

Method for curing polymers using variable-frequency microwave heating

DOEpatents

Lauf, Robert J.; Bible, Don W.; Paulauskas, Felix L.

1998-01-01

A method for curing polymers (11) incorporating a variable frequency microwave furnace system (10) designed to allow modulation of the frequency of the microwaves introduced into a furnace cavity (34). By varying the frequency of the microwave signal, non-uniformities within the cavity (34) are minimized, thereby achieving a more uniform cure throughout the workpiece (36). A directional coupler (24) is provided for detecting the direction of a signal and further directing the signal depending on the detected direction. A first power meter (30) is provided for measuring the power delivered to the microwave furnace (32). A second power meter (26) detects the magnitude of reflected power. The furnace cavity (34) may be adapted to be used to cure materials defining a continuous sheet or which require compressive forces during curing.

Immobilized monolithic enzymatic reactor and its application for analysis of in-vitro fertilization media samples.

PubMed

Chen, Wei-Qiang; Obermayr, Philipp; Černigoj, Urh; Vidič, Jana; Panić-Janković, Tanta; Mitulović, Goran

2017-11-01

Classical proteomics approaches involve enzymatic hydrolysis of proteins (either separated by polyacrylamide gels or in solution) followed by peptide identification using LC-MS/MS analysis. This method requires normally more than 16 h to complete. In the case of clinical analysis, it is of the utmost importance to provide fast and reproducible analysis with minimal manual sample handling. Herein we report the method development for online protein digestion on immobilized monolithic enzymatic reactors (IMER) to accelerate protein digestion, reduce manual sample handling, and provide reproducibility to the digestion process in clinical laboratory. An integrated online digestion and separation method using monolithic immobilized enzymatic reactor was developed and applied to digestion and separation of in-vitro-fertilization media. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The microwave Hall effect measured using a waveguide tee

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

Coppock, J. E.; Anderson, J. R.; Johnson, W. B.

2016-03-14

This paper describes a simple microwave apparatus to measure the Hall effect in semiconductor wafers. The advantage of this technique is that it does not require contacts on the sample or the use of a resonant cavity. Our method consists of placing the semiconductor wafer into a slot cut in an X-band (8–12 GHz) waveguide series tee, injecting microwave power into the two opposite arms of the tee, and measuring the microwave output at the third arm. A magnetic field applied perpendicular to the wafer gives a microwave Hall signal that is linear in the magnetic field and which reverses phasemore » when the magnetic field is reversed. The microwave Hall signal is proportional to the semiconductor mobility, which we compare for calibration purposes with d.c. mobility measurements obtained using the van der Pauw method. We obtain the resistivity by measuring the microwave reflection coefficient of the sample. This paper presents data for silicon and germanium samples doped with boron or phosphorus. The measured mobilities ranged from 270 to 3000 cm{sup 2}/(V s).« less

The healing process of intracorporeally and in situ devitalized distal femur by microwave in a dog model and its mechanical properties in vitro.

PubMed

Ji, Zhenwei; Ma, Yunlei; Li, Wei; Li, Xiaoxiang; Zhao, Guangyi; Yun, Zhe; Qian, Jixian; Fan, Qingyu

2012-01-01

Limb-salvage surgery has been well recognized as a standard treatment and alternative to amputation for patients with malignant bone tumors. Various limb-sparing techniques have been developed including tumor prosthesis, allograft, autograft and graft-prosthesis composite. However, each of these methods has short- and long-term disadvantages such as nonunion, mechanical failures and poor limb function. The technique of intracorporeal devitalization of tumor-bearing bone segment in situ by microwave-induced hyperthermia after separating it from surrounding normal tissues with a safe margin is a promising limb-salvage method, which may avoid some shortcomings encountered by the above-mentioned conventional techniques. The purpose of this study is to assess the healing process and revitalization potential of the devitalized bone segment by this method in a dog model. In addition, the immediate effect of microwave on the biomechanical properties of bone tissue was also explored in an in vitro experiment. We applied the microwave-induced hyperthermia to devitalize the distal femurs of dogs in situ. Using a monopole microwave antenna, we could produce a necrotic bone of nearly 20 mm in length in distal femur. Radiography, bone scintigraphy, microangiography, histology and functional evaluation were performed at 2 weeks and 1, 2, 3, 6, 9 and 12 months postoperatively to assess the healing process. In a biomechanical study, two kinds of bone specimens, 3 and 6 cm in length, were used for compression and three-point bending test respectively immediately after extracorporeally devitalized by microwave. An in vivo study showed that intracorporeally and in situ devitalized bone segment by microwave had great revitalization potential. An in vitro study revealed that the initial mechanical strength of the extracorporeally devitalized bone specimen may not be affected by microwave. Our results suggest that the intracorporeal microwave devitalization of tumor-bearing bone segment in situ may be a promising limb-salvage method.

40 CFR Appendix D to Part 136 - Precision and Recovery Statements for Methods for Measuring Metals

Code of Federal Regulations, 2012 CFR

2012-07-01

... water and three effluents. These samples were digested by the total digestion procedure, 4.1.3 in this.... These samples were digested by the total digestion procedure, 4.1.3 in this manual. Results for the...

40 CFR Appendix D to Part 136 - Precision and Recovery Statements for Methods for Measuring Metals

Code of Federal Regulations, 2014 CFR

2014-07-01

... water and three effluents. These samples were digested by the total digestion procedure, 4.1.3 in this.... These samples were digested by the total digestion procedure, 4.1.3 in this manual. Results for the...

40 CFR Appendix D to Part 136 - Precision and Recovery Statements for Methods for Measuring Metals

Code of Federal Regulations, 2013 CFR

2013-07-01

... water and three effluents. These samples were digested by the total digestion procedure, 4.1.3 in this.... These samples were digested by the total digestion procedure, 4.1.3 in this manual. Results for the...

Reflection measurement of waveguide-injected high-power microwave antennas.

PubMed

Yuan, Chengwei; Peng, Shengren; Shu, Ting; Zhang, Qiang; Zhao, Xuelong

2015-12-01

A method for reflection measurements of High-power Microwave (HPM) antennas excited with overmoded waveguides is proposed and studied systemically. In theory, principle of the method is proposed and the data processing formulas are developed. In simulations, a horn antenna excited by a TE11 mode exciter is examined and its reflection is calculated by CST Microwave Studio and by the method proposed in this article, respectively. In experiments, reflection measurements of two HPM antennas are conducted, and the measured results are well consistent with the theoretical expectations.

Microwave sintering of sol-gel derived abrasive grain

DOEpatents

Plovnick, Ross; Celikkaya, Ahmet; Blake, Rodger D.

1997-01-01

A method is provided for making microwave-sintered, free flowing alpha alumina-based ceramic abrasive grain, under conditions effective to couple microwaves with calcined alpha alumina-based abrasive gain precursor and sinter it at a temperature of at least about 1150.degree. C.

A Microwave Method for Measuring Moisture Content, Density, and Grain Angle of Wood.

DTIC Science & Technology

1985-03-01

Livermore, CA 94550. James, William L; Yen , You - Hsin ; King, Ray J. A microwave method for measuring moisture content,density, and grain angle of wood...Note S FPL-0250 March 1985 Density, and Grain 8 Angle of Wood William L. James, Physicist Forest Products Laboratory, Madison, WI You -Hain Yen ... Yen . You -1tsin. Microwave electromagnetic nondestructive testing of wood in real- time. Madison. WI: Department of Electronic and Computer

Methods for microwave heat treatment of manufactured components

DOEpatents

Ripley, Edward B.

2010-08-03

An apparatus for heat treating manufactured components using microwave energy and microwave susceptor material. Heat treating medium such as eutectic salts may be employed. A fluidized bed introduces process gases which may include carburizing or nitriding gases. The process may be operated in a batch mode or continuous process mode. A microwave heating probe may be used to restart a frozen eutectic salt bath.

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

Sudiana, I. Nyoman, E-mail: sudiana75@yahoo.com; Ngkoimani, La Ode; Usman, Ida

Microwave sintering of materials has attracted much research interest because of its significant advantages (e.g. reduced sintering temperatures and soaking times) over the conventional heating. Most researchers compared processes that occurred during the microwave and conventional heating at the same temperature and time. The enhancements found in the former method are indicated as a 'non-thermal effect' which is usually used for explaining the phenomena in microwave processing. Numerous recent studies have been focused on the effect to elucidate the microwave interaction mechanism with materials. Moreover, recent progress on microwave sources such as gyrotrons has opened the possibility for processing materialsmore » by using a higher microwave frequency. Therefore, the technology is expected to exhibit a stronger non-thermal effect. This paper presents results from a series of experiments to study the non-thermal effect on microwave sintered alumina. Sintering by using a wide rage of microwave frequencies up to 300 GHz as well as a conventional furnace was carried out. The linear shrinkages of samples for each sintering method were measured. Pores and grains taken from scanning electron microstructure (SEM) images of cut surfaces were also examined. The results of a comparative study of the shrinkages and microstructure evolutions of the sintered samples under annealing in microwave heating systems and in an electric furnace were analyzed. A notably different behavior of the shrinkages and microstructures of alumina after being annealed was found. The results suggested that microwave radiations provided an additional force for mass transports. The results also indicated that the sintering process depended on microwave frequencies.« less

Low temperature vapor phase digestion of graphite

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

Pierce, Robert A.

2017-04-18

A method for digestion and gasification of graphite for removal from an underlying surface is described. The method can be utilized to remove graphite remnants of a formation process from the formed metal piece in a cleaning process. The method can be particularly beneficial in cleaning castings formed with graphite molding materials. The method can utilize vaporous nitric acid (HNO.sub.3) or vaporous HNO.sub.3 with air/oxygen to digest the graphite at conditions that can avoid damage to the underlying surface.

Method and apparatus for melting metals

DOEpatents

Moore, Alan F.; Schechter, Donald E.; Morrow, Marvin Stanley

2006-03-14

A method and apparatus for melting metals uses microwave energy as the primary source of heat. The metal or mixture of metals are placed in a ceramic crucible which couples, at least partially, with the microwaves to be used. The crucible is encased in a ceramic casket for insulation and placed within a microwave chamber. The chamber may be evacuated and refilled to exclude oxygen. After melting, the crucible may be removed for pouring or poured within the chamber by dripping or running into a heated mold within the chamber. Apparent coupling of the microwaves with softened or molten metal produces high temperatures with great energy savings.

Diagnosis of femtosecond plasma filament by channeling microwaves along the filament

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

Alshershby, Mostafa; Ren, Yu; Qin, Jiang

2013-05-20

We introduce a simple, fast, and non-intrusive experimental method to obtain the basic parameters of femtosecond laser-generated plasma filament. The method is based on the channeling of microwaves along both a plasma filament and a well-defined conducting wire. By comparing the detected microwaves that propagate along the plasma filament and a copper wire with known conductivity and spatial dimension, the basic parameters of the plasma filament can be easily obtained. As a result of the possibility of channeling microwave radiation along the plasma filament, we were then able to obtain the plasma density distribution along the filament length.

Exploring microwave resonant multi-point ignition using high-speed schlieren imaging

NASA Astrophysics Data System (ADS)

Liu, Cheng; Zhang, Guixin; Xie, Hong; Deng, Lei; Wang, Zhi

2018-03-01

Microwave plasma offers a potential method to achieve rapid combustion in a high-speed combustor. In this paper, microwave resonant multi-point ignition and its control method have been studied via high-speed schlieren imaging. The experiment was conducted with the microwave resonant ignition system and the schlieren optical system. The microwave pulse in 2.45 GHz with 2 ms width and 3 kW peak power was employed as an ignition energy source to produce initial flame kernels in the combustion chamber. A reflective schlieren method was designed to illustrate the flame development process with a high-speed camera. The bottom of the combustion chamber was made of a quartz glass coated with indium tin oxide, which ensures sufficient microwave reflection and light penetration. Ignition experiments were conducted at 2 bars of stoichiometric methane-air mixtures. Schlieren images show that flame kernels were generated at more than one location simultaneously and flame propagated with different speeds in different flame kernels. Ignition kernels were discussed in three types according to their appearances. Pressure curves and combustion duration also show that multi-point ignition plays a significant role in accelerating combustion.

Exploring microwave resonant multi-point ignition using high-speed schlieren imaging.

PubMed

Liu, Cheng; Zhang, Guixin; Xie, Hong; Deng, Lei; Wang, Zhi

2018-03-01

Microwave plasma offers a potential method to achieve rapid combustion in a high-speed combustor. In this paper, microwave resonant multi-point ignition and its control method have been studied via high-speed schlieren imaging. The experiment was conducted with the microwave resonant ignition system and the schlieren optical system. The microwave pulse in 2.45 GHz with 2 ms width and 3 kW peak power was employed as an ignition energy source to produce initial flame kernels in the combustion chamber. A reflective schlieren method was designed to illustrate the flame development process with a high-speed camera. The bottom of the combustion chamber was made of a quartz glass coated with indium tin oxide, which ensures sufficient microwave reflection and light penetration. Ignition experiments were conducted at 2 bars of stoichiometric methane-air mixtures. Schlieren images show that flame kernels were generated at more than one location simultaneously and flame propagated with different speeds in different flame kernels. Ignition kernels were discussed in three types according to their appearances. Pressure curves and combustion duration also show that multi-point ignition plays a significant role in accelerating combustion.

Effect of blanching treatments on antioxidant activity of frozen green capsicum (Capsicum annuum L. var bell pepper) using radical scavenging activity (DPPH) assay

NASA Astrophysics Data System (ADS)

Azizzuddin, Norafida; Abdullah, Aminah

2016-11-01

Blanching treatments are needed to deactivate enzymes in frozen vegetables. Antioxidant activity using DPPH radical scavenging activity assay were evaluated in steaming, boiling water, and microwave blanching at different temperature, time and microwave power level on frozen green capsicum. Green capsicum was chosen for frozen treatment compared to other capsicum with different maturity index because of the firm texture. The objective of this study was to compare the antioxidant activity of frozen green capsicum between conventional and Oxi Count Kit® assay for DPPH radical scavenging activity. Results showed frozen green capsicum blanched using microwave at high level/90 seconds (sample J) contained higher level of DPPH in both conventional method and Oxi Count Kit® compared to other treatments. However, there were no significant differences between sample J and fresh sample (sample A). Overall, the sequences from highest to lowest in blanching treatments for both DPPH conventional method, and DPPH Oxi Count Kit® were J (microwave high level/90 seconds) > A (Fresh) > H (Microwave Medium Level/120 seconds) > D (Boiling Water 80°C/150 seconds) > K (Microwave High Level/120 seconds) > I (Microwave Medium Level/150 seconds) > F (Microwave Low Level/150 seconds)> B (Steam 100°C/150 seconds) > E (Boiling Water 100°C /120 seconds) > G (Microwave Low Level /180 seconds)> C (Steam 100°C/180 seconds). Almost all frozen green capsicum samples showed no significant differences for comparison between test using DPPH conventional method and Oxi Count Kit®. Frozen storage for 0, and 3rd months showed no significant differences which indicate no changes on antioxidant activity during frozen storage at -18°C.

Microwave Nondestructive Evaluation of Dielectric Materials with a Metamaterial Lens

NASA Technical Reports Server (NTRS)

Shreiber, Daniel; Gupta, Mool; Cravey, Robin L.

2008-01-01

A novel microwave Nondestructive Evaluation (NDE) sensor was developed in an attempt to increase the sensitivity of the microwave NDE method for detection of defects small relative to a wavelength. The sensor was designed on the basis of a negative index material (NIM) lens. Characterization of the lens was performed to determine its resonant frequency, index of refraction, focus spot size, and optimal focusing length (for proper sample location). A sub-wavelength spot size (3 dB) of 0.48 lambda was obtained. The proof of concept for the sensor was achieved when a fiberglass sample with a 3 mm diameter through hole (perpendicular to the propagation direction of the wave) was tested. The hole was successfully detected with an 8.2 cm wavelength electromagnetic wave. This method is able to detect a defect that is 0.037 lambda. This method has certain advantages over other far field and near field microwave NDE methods currently in use.

A novel method to augment extraction of mangiferin by application of microwave on three phase partitioning.

PubMed

Kulkarni, Vrushali M; Rathod, Virendra K

2015-06-01

This work reports a novel approach where three phase partitioning (TPP) was combined with microwave for extraction of mangiferin from leaves of Mangifera indica . Soxhlet extraction was used as reference method, which yielded 57 mg/g in 5 h. Under optimal conditions such as microwave irradiation time 5 min, ammonium sulphate concentration 40% w/v, power 272 W, solute to solvent ratio 1:20, slurry to t -butanol ratio 1:1, soaking time 5 min and duty cycle 50%, the mangiferin yield obtained was 54 mg/g by microwave assisted three phase partitioning extraction (MTPP). Thus extraction method developed resulted into higher extraction yield in a shorter span, thereby making it an interesting alternative prior to down-stream processing.

Microwave-assisted synthesis of sensitive silver substrate for surface-enhanced Raman scattering spectroscopy

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

Xia Lixin; Wang Haibo; Wang Jian

A sensitive silver substrate for surface-enhanced Raman scattering (SERS) spectroscopy is synthesized under multimode microwave irradiation. The microwave-assisted synthesis of the SERS-active substrate was carried out in a modified domestic microwave oven of 2450 MHz, and the reductive reaction was conducted in a polypropylene container under microwave irradiation with a power of 100 W for 5 min. Formaldehyde was employed as both the reductant and microwave absorber in the reductive process. The effects of different heating methods (microwave dielectric and conventional) on the properties of the SERS-active substrates were investigated. Samples obtained with 5 min of microwave irradiation at amore » power of 100 W have more well-defined edges, corners, and sharper surface features, while the samples synthesized with 1 h of conventional heating at 40 deg. C consist primarily of spheroidal nanoparticles. The SERS peak intensity of the {approx}1593 cm{sup -1} band of 4-mercaptobenzoic acid adsorbed on silver nanoparticles synthesized with 5 min of microwave irradiation at a power of 100 W is about 30 times greater than when it is adsorbed on samples synthesized with 1 h of conventional heating at 40 deg. C. The results of quantum chemical calculations are in good agreement with our experimental data. This method is expected to be utilized for the synthesis of other metal nanostructural materials.« less

Calibration and standardization of microwave ovens for fixation of brain and peripheral nerve tissue.

PubMed

Login, G R; Leonard, J B; Dvorak, A M

1998-06-01

Rapid and reproducible fixation of brain and peripheral nerve tissue for light and electron microscopy studies can be done in a microwave oven. In this review we report a standardized nomenclature for diverse fixation techniques that use microwave heating: (1) microwave stabilization, (2) fast and ultrafast primary microwave-chemical fixation, (3) microwave irradiation followed by chemical fixation, (4) primary chemical fixation followed by microwave irradiation, and (5) microwave fixation used in various combinations with freeze fixation. All of these methods are well suited to fix brain tissue for light microscopy. Fast primary microwave-chemical fixation is best for immunoelectron microscopy studies. We also review how the physical characteristics of the microwave frequency and the dimensions of microwave oven cavities can compromise microwave fixation results. A microwave oven can be calibrated for fixation when the following parameters are standardized: irradiation time; water load volume, initial temperature, and placement within the oven; fixative composition, volume, and initial temperature; and specimen container shape and placement within the oven. Using two recently developed calibration tools, the neon bulb array and the agar-saline-Giemsa tissue phantom, we report a simple calibration protocol that identifies regions within a microwave oven for uniform microwave fixation. Copyright 1998 Academic Press.

Photocatalytic degradation of RhB with microwave prepared PbMoO4.

PubMed

Hernández-Uresti, Diana B; Aguilar-Garib, Juan A; Martínez-de la Cruz, Azael

2012-01-01

Synthesized PbMoO4 from H2MoO4 and Pb(NO3)2 with microwaves was compared, in terms of its photocatalytic activity as catalyzer for decomposing rhodamine B (RhB), against samples prepared by hydrothermal and sonochemical methods from the same precursors. Microwave synthesis lasted 20 minutes; hydrothermal, 10 minutes and sonochemical method, 1 hour. Xrays diffraction patterns show that PbMoO4 prepared by these three routes is compounded by the same phase. It is found that microwave synthesized PbMoO4 particles are rounder, in an intermediate size (250 nm), compared to sonochemical (100 nm) and hydrothermal (500 nm) routes; microwave particles also exhibit higher photocatalytic activity for degradation of RhB under a xenon lamp. This difference is not explicable in terms of surface area measurements, but could be explained by UV Light scattering by the rounder particles produced by means of the microwave processing, which are about one half size compared to the wavelength.

Large-scale synthesis and microwave absorption enhancement of actinomorphic tubular ZnO/CoFe2O4 nanocomposites.

PubMed

Cao, Jing; Fu, Wuyou; Yang, Haibin; Yu, Qingjiang; Zhang, Yanyan; Liu, Shikai; Sun, Peng; Zhou, Xiaoming; Leng, Yan; Wang, Shuangming; Liu, Bingbing; Zou, Guangtian

2009-04-09

Actinomorphic tubular ZnO/CoFe(2)O(4) nanocomposites were fabricated in large scale via a simple solution method at low temperature. The phase structures, morphologies, particle size, shell thickness, chemical compositions of the composites have been characterized by X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), energy dispersive X-ray spectroscopy (EDS), and transmission electron microscopy (TEM). The as-synthesized nanocomposites were uniformly dispersed into the phenolic resin then the mixture was pasted on metal plate with the area of 200 mm x 200 mm as the microwave absorption test plate. The test of microwave absorption was carried out by the radar-absorbing materials (RAM) reflectivity far field radar cross-section (RCS) method. The range of microwave absorption is from 2 to 18 Hz and the best microwave absorption reach to 28.2 dB at 8.5 Hz. The results indicate that the composites are of excellence with respect to microwave absorption.

Assessment of trace element contents of chicken products from Turkey.

PubMed

Uluozlu, Ozgur Dogan; Tuzen, Mustafa; Mendil, Durali; Soylak, Mustafa

2009-04-30

Due to the consumption of chicken and chicken products in Turkey at high ratio, trace metal content of chicken and chicken products from Turkey were determined by atomic absorption spectrometry after microwave digestion. The accuracy of the method was confirmed by analysis of standard reference material (NIST SRM 1577b Bovine liver). Trace element content in various parts of chicken samples and chicken products were to be in the range of 0.10-114 microg/g for copper, 0.25-6.09 microg/kg for cadmium, 0.01-0.40 microg/g for lead, 0.10-0.91 microg/g for selenium, 0.05-3.91 microg/g for manganese, 0.06-0.10 microg/g for arsenic, 0.01-0.72 microg/g for chromium, 0.01-2.08 microg/g for nickel, 0.01-0.02 microg/g for cobalt, 0.10-1.90 microg/g for aluminium, 1.21-24.3 microg/g for zinc, 2.91-155 microg/g for iron. The levels of lead in some analyzed chicken products were higher than the recommended legal limits for human consumption.

Characterization and Leaching Tests of the Fluidized Bed Steam Reforming (FBSR) Waste Form for LAW Immobilization

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

Neeway, James J.; Qafoku, Nikolla; Brown, Christopher F.

2013-10-01

Several supplemental technologies for treating and immobilizing Hanford low activity waste (LAW) have been evaluated. One such immobilization technology is the Fluidized Bed Steam Reforming (FBSR) granular product. The FBSR granular product is composed of insoluble sodium aluminosilicate (NAS) feldspathoid minerals. Production of the FBSR mineral product has been demonstrated both at the industrial and laboratory scale. Pacific Northwest National Laboratory (PNNL) was involved in an extensive characterization campaign. This goal of this campaign was study the durability of the FBSR mineral product and the mineral product encapsulated in a monolith to meet compressive strength requirements. This paper gives anmore » overview of results obtained using the ASTM C 1285 Product Consistency Test (PCT), the EPA Test Method 1311 Toxicity Characteristic Leaching Procedure (TCLP), and the ASTMC 1662 Single-Pass Flow-Through (SPFT) test. Along with these durability tests an overview of the characteristics of the waste form has been collected using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), microwave digestions for chemical composition, and surface area from Brunauer, Emmett, and Teller (BET) theory.« less

Characterization and Leaching Tests of the Fluidized Bed Steam Reforming (FBSR) Waste Form for LAW Immobilization - 13400

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

Neeway, James J.; Qafoku, Nikolla P.; Peterson, Reid A.

2013-07-01

Several supplemental technologies for treating and immobilizing Hanford low activity waste (LAW) have been evaluated. One such immobilization technology is the Fluidized Bed Steam Reforming (FBSR) granular product. The FBSR granular product is composed of insoluble sodium aluminosilicate (NAS) feldspathoid minerals. Production of the FBSR mineral product has been demonstrated both at the industrial and laboratory scale. Pacific Northwest National Laboratory (PNNL) was involved in an extensive characterization campaign. The goal of this campaign was to study the durability of the FBSR mineral product and the encapsulated FBSR product in a geo-polymer monolith. This paper gives an overview of resultsmore » obtained using the ASTM C 1285 Product Consistency Test (PCT), the EPA Test Method 1311 Toxicity Characteristic Leaching Procedure (TCLP), and the ASTMC 1662 Single-Pass Flow-Through (SPFT) test. Along with these durability tests an overview of the characteristics of the waste form has been collected using Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), microwave digestions for chemical composition, and surface area from Brunauer, Emmett, and Teller (BET) theory. (authors)« less

Preliminary studies of laser-induced breakdown spectrometry for the determination of Ba, Cd, Cr and Pb in toys

NASA Astrophysics Data System (ADS)

Godoi, Quienly; Santos, Dario, Jr.; Nunes, Lidiane C.; Leme, Flávio O.; Rufini, Iolanda A.; Agnelli, José A. M.; Trevizan, Lilian C.; Krug, Francisco J.

2009-06-01

The performance of laser-induced breakdown spectrometry (LIBS) for the determination of Ba, Cd, Cr and Pb in toys has been evaluated by using a Nd:YAG laser operating at 1064 nm and an Echelle spectrometer with intensified charge-coupled device detector. Samples were purchased in different cities of São Paulo State market and analyzed directly without sample preparation. Laser-induced breakdown spectrometry experimental conditions (number of pulses, delay time, integration time gate and pulse energy) were optimized by using a Doehlert design. Laser-induced breakdown spectrometry signals correlated reasonably well with inductively coupled plasma optical emission spectrometry (ICP OES) concentrations after microwave-assisted acid digestion of selected samples. Thermal analysis was used for polymer identification and scanning electron microscopy to visualize differences in crater geometry of different polymers employed for toy fabrication. Results indicate that laser-induced breakdown spectrometry can be proposed as a rapid screening method for investigation of potentially toxic elements in toys. The unique application of laser-induced breakdown spectrometry for identification of contaminants in successive layers of ink and polymer is also demonstrated.

Evaluation of the impact of food matrix change on the in vitro bioaccessibility of carotenoids in pumpkin (Cucurbita moschata) slices during two drying processes.

PubMed

Zhang, Zhongyuan; Wang, Xiaoyan; Li, Yixiang; Wei, Qiuyu; Liu, Chunju; Nie, Meimei; Li, Dajing; Xiao, Yadong; Liu, Chunquan; Xu, Lang; Zhang, Min; Jiang, Ning

2017-12-13

The food matrix is a limiting factor in determining the bioaccessibility of carotenoids. The impact of food matrix change on the bioaccessibility of carotenoids during drying processes is still unknown. The effect of intermittent microwave vacuum-assisted drying (IMVD) and hot air drying (HAD) on the in vitro liberation and micellization of carotenoids in pumpkin slices was studied. This variable depended on the changes of the matrix driven by the drying process. Different changes in the cell morphology and carotenoid distribution of pumpkin slices during the two processing methods were observed. For IMVD, cell wall degradation and complete chromoplast organelle disruption contributed to the improvement in the liberation and micellization of carotenoids. In the HAD-dried sample, large pigment aggregates hindered the liberation of carotenoids. The carotenoid level in the micellar fraction appeared to be lower than that in the aqueous supernatant during the two processes, suggesting that the new obstacles formed during processing and/or digestion hindered the incorporation of carotenoids in mixed micelles.

Determination of arsenic species and arsenosugars in marine samples by HPLC-ICP-MS.

PubMed

Hirata, Shizuko; Toshimitsu, Hideki

2005-10-01

Arsenic-speciation analysis in marine samples was performed by high-pressure liquid chromatography (HPLC) with ICP-MS detection. Separation of eight arsenic species--As(III), MMA, DMA, As(V), AB, TMAO, AC and TeMAs(+)--was achieved on a C(18) column with isocratic elution (pH 3.0), under which conditions As(III) and MMA co-eluted. The entire separation was accomplished in 15 min. The HPLC-ICP-MS detection limits for the eight arsenic species were in the range 0.03-0.23 microg L(-1) based on 3 sigma for the blank response (n=5). The precision was calculated to be 2.4-8.0% (RSD) for the eight species. The method was successfully applied to several marine samples, e.g. oysters, fish, shrimps, and marine algae. Low-power microwave digestion was employed for extraction of arsenic from seafood products; ultrasonic extraction was employed for the extraction of arsenic from seaweeds. Separation of arsenosugars was achieved on an anion-exchange column. Concentrations of arsenosugars 2, 3, and 4 in marine algae were in the range 0.18-9.59 microg g(-1).

[Analysis of biological material originating from the body of general Władysław Sikorski for inorganic poisons and diatoms presence].

PubMed

Sadlik, Józefa Krystyna; Brozek-Mucha, Zuzanna

2009-01-01

Results of the analysis of biological materials originating from the body of general Sikorski are presented in the paper. Samples of the liver, kidney, intestine and lung were analysed for metals and As content, and samples of the lung, liver, kidney, stomach, intestine and bone marrow--for diatoms presence. The analysis for metals and As was performed by atomic absorption spectrometry (AAS) and inductively coupled plasma optical emission spectrometry (ICP-OES). Before the analysis, the samples were wet digested by the classic and microwave assisted method. The analysis did not result in detecting the presence of As, Co, Ni, and Tl in any of the studied materials, while Hg was not revealed in the liver, intestines and lung and Pb in the intestines and lung. The content of Ba, Cd, Cr, Cu, Fe, Mn, Sr and Zn in all the studied materials, Hg in the kidney, and Pb in the liver and kidney did not indicate poisoning by the above-mentioned metals or arsenic. No diatoms were found in the studied materials.

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.

Improved conventional and microwave-assisted silylation protocols for simultaneous gas chromatographic determination of tocopherols and sterols: Method development and multi-response optimization.

PubMed

Poojary, Mahesha M; Passamonti, Paolo

2016-12-09

This paper reports on improved conventional thermal silylation (CTS) and microwave-assisted silylation (MAS) methods for simultaneous determination of tocopherols and sterols by gas chromatography. Reaction parameters in each of the methods developed were systematically optimized using a full factorial design followed by a central composite design. Initially, experimental conditions for CTS were optimized using a block heater. Further, a rapid MAS was developed and optimized. To understand microwave heating mechanisms, MAS was optimized by two distinct modes of microwave heating: temperature-controlled MAS and power-controlled MAS, using dedicated instruments where reaction temperature and microwave power level were controlled and monitored online. Developed methods: were compared with routine overnight derivatization. On a comprehensive level, while both CTS and MAS were found to be efficient derivatization techniques, MAS significantly reduced the reaction time. The optimal derivatization temperature and time for CTS found to be 55°C and 54min, while it was 87°C and 1.2min for temperature-controlled MAS. Further, a microwave power of 300W and a derivatization time 0.5min found to be optimal for power-controlled MAS. The use of an appropriate derivatization solvent, such as pyridine, was found to be critical for the successful determination. Catalysts, like potassium acetate and 4-dimethylaminopyridine, enhanced the efficiency slightly. The developed methods showed excellent analytical performance in terms of linearity, accuracy and precision. Copyright © 2016 Elsevier B.V. All rights reserved.

Understanding microwave vessel contamination by chloride species.

PubMed

Recchia, Sandro; Spanu, Davide; Bianchi, Davide; Dossi, Carlo; Pozzi, Andrea; Monticelli, Damiano

2016-10-01

Microwaves are widely used to assist digestion, general sample treatment and synthesis. The use of aqua regia is extensively adopted for the closed vessel mineralization of samples prior to trace element detection, leading to the contamination of microwave vessels by chlorine containing species. The latter are entrapped in the polymeric matrix of the vessels, leading to memory effects that are difficult to remove, among which the risk of silver incomplete recoveries by removal of the sparingly soluble chloride is the predominant one. In the present paper, we determined by mass spectrometry that hydrogen chloride is the species entrapped in the polymeric matrix and responsible for vessel contamination. Moreover, several decontamination treatments were considered to assess their efficiency, demonstrating that several cleaning cycles with water, nitric acid or silver nitrate in nitric acid were inefficient in removing chloride contamination (contamination reduction around 90%). Better results (≈95% decrease) were achieved by a single decontamination step in alkaline environment (sodium hydroxide or ammonia). Finally, a thermal treatment in a common laboratory oven (i.e. without vacuum and ventilation) was tested: a one hour heating at 150°C leads to a 98.5% decontamination, a figure higher than the ones obtained by wet treatments which requires comparable time. The latter treatment is a major advancement with respect to existing treatments as it avoids the need of a vacuum oven for at least 17h as presently proposed in the literature. Copyright © 2016 Elsevier B.V. All rights reserved.

Microwave-assisted Facile and Ultrafast Growth of ZnO Nanostructures and Proposition of Alternative Microwave-assisted Methods to Address Growth Stoppage

NASA Astrophysics Data System (ADS)

Rana, Abu Ul Hassan Sarwar; Kang, Mingi; Kim, Hyun-Seok

2016-04-01

The time constraint in the growth of ZnO nanostructures when using a hydrothermal method is of paramount importance in contemporary research, where a long fabrication time rots the very essence of the research on ZnO nanostructures. In this study, we present the facile and ultrafast growth of ZnO nanostructures in a domestic microwave oven within a pressurized environment in just a few minutes. This method is preferred for the conventional solution-based method because of the ultrafast supersaturation of zinc salts and the fabrication of high-quality nanostructures. The study of the effect of seed layer density, growth time, and the solution’s molar concentration on the morphology, alignment, density, and aspect ratio of ZnO nanorods (ZNRs) is explored. It is found in a microwave-assisted direct growth method that ~5 mins is the optimum time beyond which homogeneous nucleation supersedes heterogeneous nucleation, which results in the growth stoppage of ZNRs. To deal with this issue, we propound different methods such as microwave-assisted solution-replacement, preheating, and PEI-based growth methods, where growth stoppage is addressed and ZNRs with a high aspect ratio can be grown. Furthermore, high-quality ZnO nanoflowers and ZnO nanowalls are fabricated via ammonium hydroxide treatment in a very short time.

Development of new UV-vis spectroscopic microwave-assisted method for determination of glucose in pharmaceutical samples

NASA Astrophysics Data System (ADS)

Mabood, Fazal; Hussain, Z.; Haq, H.; Arian, M. B.; Boqué, R.; Khan, K. M.; Hussain, K.; Jabeen, F.; Hussain, J.; Ahmed, M.; Alharasi, A.; Naureen, Z.; Hussain, H.; Khan, A.; Perveen, S.

2016-01-01

A new UV-Visible spectroscopic method assisted with microwave for the determination of glucose in pharmaceutical formulations was developed. In this study glucose solutions were oxidized by ammonium molybdate in the presence of microwave energy and reacted with aniline to produce a colored solution. Optimum conditions of the reaction including wavelength, temperature, and pH of the medium and relative concentration ratio of the reactants were investigated. It was found that the optimal wavelength for the reaction is 610 nm, the optimal reaction time is 80 s, the optimal reaction temperature is 160 °C, the optimal reaction pH is 4, and the optimal concentration ratio aniline/ammonium molybdate solution was found to be 1:1. The limits of detection and quantification of the method are 0.82 and 2.75 ppm for glucose solution, respectively. The use of microwaves improved the speed of the method while the use of aniline improved the sensitivity of the method by shifting the wavelength.

Microwave-assisted extraction of rutin and quercetin from the stalks of Euonymus alatus (Thunb.) Sieb.

PubMed

Zhang, Fan; Yang, Yi; Su, Ping; Guo, Zhenku

2009-01-01

Euonymus alatus (Thunb.) has been used as one of traditional Chinese medicines for several thousand years. Conventional methods for the extraction of rutin and quercetin from E. alatus, including solvent extraction, Soxhlet extraction and heat reflux extraction are characterised by long extraction times and consumption of large amounts of solvents. To develop a simple and rapid method for the extraction of rutin and quercetin from the stalks of Euonymus alatus (Thunb.) Sieb using microwave-assisted extraction (MAE) technique. MAE experiments were performed with a multimode microwave extraction system. The experimental variables that affect the MAE process, such as the concentration of ethanol solution, extractant volume, microwave power and extraction time were optimised. Yields were determined by HPLC. The results were compared with that obtained by classical Soxhlet and ultrasonic-assisted extraction (UAE). From the optimised conditions for MAE of rutin and quercetin it can be concluded that the solvent is 50% ethanol (v/v) solution, the extractant volume is 40 mL, microwave power is 170 W and irradiation time is 6 min. Compared with Soxhlet extraction and ultrasonic extraction, microwave extraction is a rapid method with a higher yield and lower solvent consumption. The results showed that MAE can be used as an efficient and rapid method for the extraction of the active components from plants.

The effect of drying method temperature, collection method, and marker type on apparent ileal amino acid digestibility in 21-day-old broilers fed corn-soybean meal-barley based diet.

PubMed

Olojede, O C; Ford, M J; Jacob, J P; Ao, T; Pescatore, A J; Adedokun, S A

2018-06-01

For accurate estimation of nutrient digestibility, an ideal drying and sampling method is required to preserve the quality of the digesta. A standard corn-soybean meal (corn-SBM) broiler starter diet was fed from d 0 to 10 before birds were placed on the experimental diets until d 21. One hundred and sixty-eight male Cobb 500 broiler chicks were used to evaluate the effect of two drying methods (freeze-dryer vs. forced air-oven) and two drying temperatures (40 vs. 55°C) (Exp 1), while ninety-six chicks were used to evaluate the effect of flushing and squeezing as well as marker types (titanium vs. chromium) on apparent ileal DM, N, Ca, P, and AA digestibility (Exp 2). There were seven (Exp 1) or eight (Exp 2) replicate cages per treatment with 6 birds/cage. Digesta from the distal two thirds of the ileum was obtained from birds following euthanasia on d 21 by squeezing (Exp 1) and squeezing or flushing (Exp 2). Samples collected were stored in the freezer at -20°C until they were either freeze-dried (FD) or oven-dried (OD) at 40 or 55°C. There were no interactions between the drying methods and drying temperatures (Exp 1) on apparent ileal DM, N, and AA digestibility. Met had the highest (92.3%) while Cys had the lowest (73.8%) digestibility value. In Exp 2, no interaction between sampling methods and marker types was observed. The effect of sampling methods was not significant except for Arg and Met where squeezing resulted in higher (P < 0.05) digestibility values. Furthermore, apparent ileal His, Ile, Cys, Ser, and Tyr digestibility tended to be higher (P < 0.1) in squeezed digesta compared to the flushed digesta. Results from these studies showed that OD ileal digesta at 40 or 55°C had no negative effect on apparent ileal AA digestibility. Likewise, marker type did not influence apparent ileal AA digestibility values.

Process for microwave sintering boron carbide

DOEpatents

Holcombe, C.E.; Morrow, M.S.

1993-10-12

A method of microwave sintering boron carbide comprises leaching boron carbide powder with an aqueous solution of nitric acid to form a leached boron carbide powder. The leached boron carbide powder is coated with a glassy carbon precursor to form a coated boron carbide powder. The coated boron carbide powder is consolidated in an enclosure of boron nitride particles coated with a layer of glassy carbon within a container for microwave heating to form an enclosed coated boron carbide powder. The enclosed coated boron carbide powder is sintered within the container for microwave heating with microwave energy.

Process for microwave sintering boron carbide

DOEpatents

Holcombe, Cressie E.; Morrow, Marvin S.

1993-01-01

A method of microwave sintering boron carbide comprises leaching boron carbide powder with an aqueous solution of nitric acid to form a leached boron carbide powder. The leached boron carbide powder is coated with a glassy carbon precursor to form a coated boron carbide powder. The coated boron carbide powder is consolidated in an enclosure of boron nitride particles coated with a layer of glassy carbon within a container for microwave heating to form an enclosed coated boron carbide powder. The enclosed coated boron carbide powder is sintered within the container for microwave heating with microwave energy.

Microwave Energy Increases Fatty Acid Methyl Ester Yield in Human Whole Blood Due to Increased Sphingomyelin Transesterification.

PubMed

Metherel, Adam H; Aristizabal Henao, Juan J; Ciobanu, Flaviu; Taha, Ameer Y; Stark, Ken D

2015-09-01

Dried blood spots (DBS) by fingertip prick collection for fatty acid profiling are becoming increasingly popular due to ease of collection, minimal invasiveness and its amenability to high-throughput analyses. Herein, we assess a microwave-assisted direct transesterification method for the production of fatty acid methyl esters (FAME) from DBS. Technical replicates of human whole blood were collected and 25-μL aliquots were applied to chromatography strips prior to analysis by a standard 3-h transesterification method or microwave-assisted direct transesterification method under various power (variable vs constant), time (1-5 min) and reagent (1-10% H2SO4 in methanol) conditions. In addition, a standard method was compared to a 5-min, 30-W power microwave in 1% H2SO4 method for FAME yield from whole blood sphingomyelin, and sphingomyelin standards alone and spiked in whole blood. Microwave-assisted direct transesterification yielded no significant differences in both quantitative (nmol/100 µL) and qualitative (mol%) fatty acid assessments after as little as 1.5- and 1-min reaction times, respectively, using the variable power method and 5% H2SO4 in methanol. However, 30-W power for 5 min increased total FAME yield of the technical replicates by 14%. This increase appears largely due to higher sphingomyelin-derived FAME yield of up to 109 and 399% compared to the standard method when determined from whole blood or pure standards, respectively. In conclusion, microwave-assisted direct transesterification of DBS achieved in as little as 1-min, and 5-min reaction times increase total fatty acids primarily by significantly improving sphingomyelin-derived fatty acid yield.

In vitro dynamic model simulating the digestive tract of 6-month-old infants

PubMed Central

Gallo, Marianna; Tornatore, Fabio; Frasso, Annalisa; Saccone, Giulia; Budelli, Andrea; Barone, Maria V.

2017-01-01

Background In vivo assays cannot always be conducted because of ethical reasons, technical constraints or costs, but a better understanding of the digestive process, especially in infants, could be of great help in preventing food-related pathologies and in developing new formulas with health benefits. In this context, in vitro dynamic systems to simulate human digestion and, in particular, infant digestion could become increasingly valuable. Objective To simulate the digestive process through the use of a dynamic model of the infant gastroenteric apparatus to study the digestibility of starch-based infant foods. Design Using M.I.D.A (Model of an Infant Digestive Apparatus), the oral, gastric and intestinal digestibility of two starch-based products were measured: 1) rice starch mixed with distilled water and treated using two different sterilization methods (the classical method with a holding temperature of 121°C for 37 min and the HTST method with a holding temperature of 137°C for 70 sec) and 2) a rice cream with (premium product) or without (basic product) an aliquot of rice flour fermented by Lactobacillus paracasei CBA L74. After the digestion the foods were analyzed for the starch concentration, the amount of D-glucose released and the percentage of hydrolyzed starch. Results An in vitro dynamic system, which was referred to as M.I.D.A., was obtained. Using this system, the starch digestion occurred only during the oral and intestinal phase, as expected. The D-glucose released during the intestinal phase was different between the classical and HTST methods (0.795 grams for the HTST versus 0.512 for the classical product). The same analysis was performed for the basic and premium products. In this case, the premium product had a significant difference in terms of the starch hydrolysis percentage during the entire process. Conclusions The M.I.D.A. system was able to digest simple starches and a more complex food in the correct compartments. In this study, better digestibility of the premium product was revealed. PMID:29261742

Toward the establishment of standardized in vitro tests for lipid-based formulations, part 1: method parameterization and comparison of in vitro digestion profiles across a range of representative formulations.

PubMed

Williams, Hywel D; Sassene, Philip; Kleberg, Karen; Bakala-N'Goma, Jean-Claude; Calderone, Marilyn; Jannin, Vincent; Igonin, Annabel; Partheil, Anette; Marchaud, Delphine; Jule, Eduardo; Vertommen, Jan; Maio, Mario; Blundell, Ross; Benameur, Hassan; Carrière, Frédéric; Müllertz, Anette; Porter, Christopher J H; Pouton, Colin W

2012-09-01

The Lipid Formulation Classification System Consortium is an industry-academia collaboration, established to develop standardized in vitro methods for the assessment of lipid-based formulations (LBFs). In this first publication, baseline conditions for the conduct of digestion tests are suggested and a series of eight model LBFs are described to probe test performance across different formulation types. Digestion experiments were performed in vitro using a pH-stat apparatus and danazol employed as a model poorly water-soluble drug. LBF digestion (rate and extent) and drug solubilization patterns on digestion were examined. To evaluate cross-site reproducibility, experiments were conducted at two sites and highly consistent results were obtained. In a further refinement, bench-top centrifugation was explored as a higher throughput approach to separation of the products of digestion (and compared with ultracentrifugation), and conditions under which this method was acceptable were defined. Drug solubilization was highly dependent on LBF composition, but poorly correlated with simple performance indicators such as dispersion efficiency, confirming the utility of the digestion model as a means of formulation differentiation. Copyright © 2012 Wiley Periodicals, Inc.

Starch digestibility: past, present, and future.

PubMed

Bello-Perez, Luis A; Flores-Silva, Pamela C; Agama-Acevedo, Edith; Tovar, Juscelino

2018-02-10

In the last century, starch present in foods was considered to be completely digested. However, during the 1980s, studies on starch digestion started to show that besides digestible starch, which could be rapidly or slowly hydrolysed, there was a variable fraction that resisted hydrolysis by digestive enzymes. That fraction was named resistant starch (RS) and it encompasses those forms of starch that are not accessible to human digestive enzymes but can be fermented by the colonic microbiota, producing short-chain fatty acids. RS has been classified into five types, depending on the mechanism governing its resistance to enzymatic hydrolysis. Early research on RS was focused on the methods to determine its content in foods and its physiological effects, including fermentability in the large intestine. Later on, due to the interest of the food industry, methods to increase the RS content of isolated starches were developed. Nowadays, the influence of RS on the gut microbiota is a relevant research topic owing to its potential health-related benefits. This review summarizes over 30 years of investigation on starch digestibility, its relationship with human health, the methods to produce RS and its impact on the microbiome. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

Examining Dense Data Usage near the Regions with Severe Storms in All-Sky Microwave Radiance Data Assimilation and Impacts on GEOS Hurricane Analyses

NASA Technical Reports Server (NTRS)

Kim, Min-Jeong; Jin, Jianjun; McCarty, Will; El Akkraoui, Amal; Todling, Ricardo; Gelaro, Ron

2018-01-01

Many numerical weather prediction (NWP) centers assimilate radiances affected by clouds and precipitation from microwave sensors, with the expectation that these data can provide critical constraints on meteorological parameters in dynamically sensitive regions to make significant impacts on forecast accuracy for precipitation. The Global Modeling and Assimilation Office (GMAO) at NASA Goddard Space Flight Center assimilates all-sky microwave radiance data from various microwave sensors such as all-sky GPM Microwave Imager (GMI) radiance in the Goddard Earth Observing System (GEOS) atmospheric data assimilation system (ADAS), which includes the GEOS atmospheric model, the Gridpoint Statistical Interpolation (GSI) atmospheric analysis system, and the Goddard Aerosol Assimilation System (GAAS). So far, most of NWP centers apply same large data thinning distances, that are used in clear-sky radiance data to avoid correlated observation errors, to all-sky microwave radiance data. For example, NASA GMAO is applying 145 km thinning distances for most of satellite radiance data including microwave radiance data in which all-sky approach is implemented. Even with these coarse observation data usage in all-sky assimilation approach, noticeable positive impacts from all-sky microwave data on hurricane track forecasts were identified in GEOS-5 system. The motivation of this study is based on the dynamic thinning distance method developed in our all-sky framework to use of denser data in cloudy and precipitating regions due to relatively small spatial correlations of observation errors. To investigate the benefits of all-sky microwave radiance on hurricane forecasts, several hurricane cases selected between 2016-2017 are examined. The dynamic thinning distance method is utilized in our all-sky approach to understand the sources and mechanisms to explain the benefits of all-sky microwave radiance data from various microwave radiance sensors like Advanced Microwave Sounder Unit (AMSU-A), Microwave Humidity Sounder (MHS), and GMI on GEOS-5 analyses and forecasts of various hurricanes.

Spectrophotometric determination of low levels arsenic species in beverages after ion-pairing vortex-assisted cloud-point extraction with acridine red.

PubMed

Altunay, Nail; Gürkan, Ramazan; Kır, Ufuk

2016-01-01

A new, low-cost, micellar-sensitive and selective spectrophotometric method was developed for the determination of inorganic arsenic (As) species in beverage samples. Vortex-assisted cloud-point extraction (VA-CPE) was used for the efficient pre-concentration of As(V) in the selected samples. The method is based on selective and sensitive ion-pairing of As(V) with acridine red (ARH(+)) in the presence of pyrogallol and sequential extraction into the micellar phase of Triton X-45 at pH 6.0. Under the optimised conditions, the calibration curve was highly linear in the range of 0.8-280 µg l(-1) for As(V). The limits of detection and quantification of the method were 0.25 and 0.83 µg l(-1), respectively. The method was successfully applied to the determination of trace As in the pre-treated and digested samples under microwave and ultrasonic power. As(V) and total As levels in the samples were spectrophotometrically determined after pre-concentration with VA-CPE at 494 nm before and after oxidation with acidic KMnO4. The As(III) levels were calculated from the difference between As(V) and total As levels. The accuracy of the method was demonstrated by analysis of two certified reference materials (CRMs) where the measured values for As were statistically within the 95% confidence limit for the certified values.

Real Time Monitoring of Flooding from Microwave Satellite Observations

NASA Technical Reports Server (NTRS)

Galantowicz, John F.; Frey, Herb (Technical Monitor)

2002-01-01

We have developed a new method for making high-resolution flood extent maps (e.g., at the 30-100 m scale of digital elevation models) in real-time from low-resolution (20-70 km) passive microwave observations. The method builds a "flood-potential" database from elevations and historic flood imagery and uses it to create a flood-extent map consistent with the observed open water fraction. Microwave radiometric measurements are useful for flood monitoring because they sense surface water in clear-or-cloudy conditions and can provide more timely data (e.g., compared to radars) from relatively wide swath widths and an increasing number of available platforms (DMSP, ADEOS-II, Terra, NPOESS, GPM). The chief disadvantages for flood mapping are the radiometers' low resolution and the need for local calibration of the relationship between radiances and open-water fraction. We present our method for transforming microwave sensor-scale open water fraction estimates into high-resolution flood extent maps and describe 30-day flood map sequences generated during a retrospective study of the 1993 Great Midwest Flood. We discuss the method's potential improvement through as yet unimplemented algorithm enhancements and expected advancements in microwave radiometry (e.g., improved resolution and atmospheric correction).

Sub-second carbon-nanotube-mediated microwave sintering for high-conductivity silver patterns on plastic substrates

NASA Astrophysics Data System (ADS)

Jung, Sunshin; Chun, Su Jin; Han, Joong Tark; Woo, Jong Seok; Shon, Cha-Hwa; Lee, Geon-Woong

2016-02-01

A method of microwave sintering that is mediated by carbon nanotubes (CNTs) has been developed to obtain high-conductivity Ag patterns on the top of heat-sensitive plastic substrates within a short time. The Ag patterns are printed on CNTs formed on plastic substrates and rapidly heated to a great extent by the heat transferred from the microwave-heated CNTs. The conductivity of the microwave-sintered Ag patterns reaches ~39% that of bulk Ag within 1 s without substrate deformation. Furthermore, microwave sintering enhances the adhesion of Ag patterns to the thermoplastic substrates because the sintering causes interfacial fusion between the Ag patterns and the substrates, and CNTs physically connect the patterns with the substrates.A method of microwave sintering that is mediated by carbon nanotubes (CNTs) has been developed to obtain high-conductivity Ag patterns on the top of heat-sensitive plastic substrates within a short time. The Ag patterns are printed on CNTs formed on plastic substrates and rapidly heated to a great extent by the heat transferred from the microwave-heated CNTs. The conductivity of the microwave-sintered Ag patterns reaches ~39% that of bulk Ag within 1 s without substrate deformation. Furthermore, microwave sintering enhances the adhesion of Ag patterns to the thermoplastic substrates because the sintering causes interfacial fusion between the Ag patterns and the substrates, and CNTs physically connect the patterns with the substrates. Electronic supplementary information (ESI) available: Temperature difference in Ag/CNT/PC samples; the carbon content and electrical performance after microwave sintering; microwave sintering of Ag/CNT patterns; physical connection between the substrate and sintered Ag lines; touch-piano (figure and movie). See DOI: 10.1039/c5nr08082g

A Method of Treatment of Purulent-Inflammatory Diseases of the Hand in Outpatient Clinic with Using Electromagnetic Microwave Field

NASA Astrophysics Data System (ADS)

Rabenok, L.; Grimalsky, V.; De La Hidalga-W., J.

2006-09-01

The report is devoted to applications of the microwave therapy. 50 patients with acute purulent-inflammatory diseases of the hand were examined with using our method of treatment with electromagnetic (EM) microwave field in an outpatient clinic. We used a portable apparatus that operates in the millimeter (mm) wave range in 4 regimes. The intensity of EM radiation was 2-10 mW/cm2. A peculiarity of the method was an absence of any antibacterial medicine during the treatment. We conclude that using EM microwave fields seems very efficient in a complex treatment of acute purulent-inflammatory diseases of the hand in an outpatient clinic. An interpretation of the obtained results is given due to the resonant character of the interaction of EM radiation with molecular and cellular structures.

A novel image processing method to determine the nutritional condition of lobsters.

PubMed

Berillis, P; Simon, C; Mente, E; Sofos, F; Karapanagiotidis, I T

2013-02-01

The digestive gland of crustacean is involved in various metabolic activities, including the synthesis and secretion of digestive enzymes that begin the process of food digestion, intracellular digestion and absorption of nutrients, storage of reserves, and disposal of waste products. It consists of two glandular lobes which extensively subdivide to form a complex of blind-ending tubules, whose size, surface area, and digestive cells are associated with intracellular digestion and the nutritional status of the organism. The aim of this paper was to study the morphology of the digestive gland in various lobster species and calculate the surface area of tubules, lumen and digestive cells (R-, F-, and B-cells) and their ratios to total tubule surface area. The similarity in ratios obtained in this study between individual lobsters suggests that the method developed in this study can be successfully applied to a range of species. This study describes a novel image processing algorithm for the automatic measurement of the hepatopancreas structure using stained cross sections of digestive gland tubules. The proposed new methodology could be used for studying the physiology and nutrient metabolism of lobsters and other crustaceans. The computer-aided analysis described in this paper is accurate for the quantitative assessment of the lobster's digestive gland structure. Copyright © 2012 Elsevier Ltd. All rights reserved.

The electromagnetic-trait imaging computation of traveling wave method in breast tumor microwave sensor system.

PubMed

Tao, Zhi-Fu; Han, Zhong-Ling; Yao, Meng

2011-01-01

Using the difference of dielectric constant between malignant tumor tissue and normal breast tissue, breast tumor microwave sensor system (BRATUMASS) determines the detected target of imaging electromagnetic trait by analyzing the properties of target tissue back wave obtained after near-field microwave radicalization (conelrad). The key of obtained target properties relationship and reconstructed detected space is to analyze the characteristics of the whole process from microwave transmission to back wave reception. Using traveling wave method, we derive spatial transmission properties and the relationship of the relation detected points distances, and valuate the properties of each unit by statistical valuation theory. This chapter gives the experimental data analysis results.

A Novel Method of Preparation of Inorganic Glasses by Microwave Irradiation

NASA Astrophysics Data System (ADS)

Vaidhyanathan, B.; Ganguli, Munia; Rao, K. J.

1994-12-01

Microwave heating is shown to provide an extremely facile and automatically temperature-controlled route to the synthesis of glasses. Glass-forming compositions of several traditional and novel glasses were melted in a kitchen microwave oven, typically within 5 min and quenched into glasses. This is only a fraction of the time required in normal glass preparation methods. The rapidity of melting minimizes undesirable features such as loss of components of the glass, variation of oxidation states of metal ions, and oxygen loss leading to reduced products in the glass such as metal particles. This novel procedure of preparation is applicable when at least one of the components of the glass-forming mixture absorbs microwaves.

On the importance of simultaneous infrared/fiber-optic temperature monitoring in the microwave-assisted synthesis of ionic liquids.

PubMed

Obermayer, David; Kappe, C Oliver

2010-01-07

The temperature profiles obtained from both an external infrared and internal fiber-optic sensor were compared for heating and synthesizing the ionic liquid 1-butyl-3-methylimidazolium bromide (bmimBr) under microwave conditions. Utilizing a single-mode microwave reactor that allows simultaneous infrared/fiber-optic temperature measurements, significant differences between the two methods of temperature monitoring were revealed. Due to the strong microwave absorptivity of ionic liquids and the delay experienced in monitoring temperature on the outer surface of a heavy-walled glass vial, external infrared temperature sensors can not be used to accurately control the temperature in the heating of ionic liquids under microwave conditions. The use of internal fiber-optic probes allows the monitoring and control of the heating behavior in a much better way. In order to prevent the strong exotherm in the synthesis of bmimBr under microwave conditions the use of a reaction vessel made out of silicon carbide is the method of choice. Because of the high thermal conductivity and effusivity of silicon carbide, the heat generated during the ionic liquid formation is efficiently exchanged with the comparatively cool air in the microwave cavity via the silicon carbide ceramic.

Microwave sintering of multiple articles

DOEpatents

Blake, Rodger D.; Katz, Joel D.

1993-01-01

Apparatus and method for producing articles of alumina and of alumina and silicon carbide in which the articles are sintered at high temperatures using microwave radiation. The articles are placed in a sintering container which is placed in a microwave cavity for heating. The rates at which heating and cooling take place is controlled.

Nuke 'Em! Library Pest Control Using a Microwave.

ERIC Educational Resources Information Center

Brezner, Jerome; Luner, Philip

1989-01-01

Discusses the threats to books and periodicals posed by such insects as book lice, termites, cockroaches, silverfish, firebrats, and beetles; reviews past methods of pest control; and describes a technique for insect control using microwaves. The results of tests of microwave effects on publications are reported, necessary precautions are…

Ex situ themo-catalytic upgrading of biomass pyrolysis vapors using a traveling wave microwave reactor

USDA-ARS?s Scientific Manuscript database

Microwave heating offers a number of advantages over conventional heating methods, such as, rapid and volumetric heating, precise temperature control, energy efficiency and lower temperature gradient. In this article we demonstrate the use of 2450 MHz microwave traveling wave reactor to heat the cat...

Computer-Generated Microwave Holograms.

ERIC Educational Resources Information Center

Leming, Charles W.; Hastings, Orestes Patterson, III

1980-01-01

Described is the phasor method of superposition of waves. The intensity pattern from a system of microwave sources is calculated point by point on a plane corresponding to a film emulsion, and then printed and directly converted to a hologram for 3-cm microwaves. Calculations, construction, and viewing of holograms are included. (Author/DS)

Anaerobic digestibility of beef hooves with swine manure or slaughterhouse sludge.

PubMed

Xia, Yun; Wang, Ding-Kang; Kong, Yunhong; Ungerfeld, Emilio M; Seviour, Robert; Massé, Daniel I

2015-04-01

Anaerobic digestion is an effective method for treating animal by-products, generating at the same time green energy as methane (CH4). However, the methods and mechanisms involved in anaerobic digestion of α-keratin wastes like hair, nails, horns and hooves are still not clear. In this study we investigated the feasibility of anaerobically co-digesting ground beef hooves in the presence of swine manure or slaughterhouse sludge at 25 °C using eight 42-L Plexiglas lab-scale digesters. Our results showed addition of beef hooves statistically significantly increased the rate of CH4 production with swine manure, but only increased it slightly with slaughterhouse sludge. After 90-day digestion, 73% of beef hoof material added to the swine manure-inoculated digesters had been converted into CH4, which was significantly higher than the 45% level achieved in the slaughterhouse sludge inoculated digesters. BODIPY-Fluorescent casein staining detected proteolytic bacteria in all digesters with and without added beef hooves, and their relative abundances corresponded to the rate of methanogenesis of the digesters with the different inocula. Fluorescence in situ hybridization in combination with BODIPY-Fluorescent casein staining identified most proteolytic bacteria as members of genus Alkaliphilus in the subfamily Clostridiaceae 2 of family Clostridiaceae. They thus appear to be the bacteria mainly responsible for digestion of beef hooves. Crown Copyright © 2014. Published by Elsevier Ltd. All rights reserved.

Microwave Sensors for Breast Cancer Detection

PubMed Central

2018-01-01

Breast cancer is the leading cause of death among females, early diagnostic methods with suitable treatments improve the 5-year survival rates significantly. Microwave breast imaging has been reported as the most potential to become the alternative or additional tool to the current gold standard X-ray mammography for detecting breast cancer. The microwave breast image quality is affected by the microwave sensor, sensor array, the number of sensors in the array and the size of the sensor. In fact, microwave sensor array and sensor play an important role in the microwave breast imaging system. Numerous microwave biosensors have been developed for biomedical applications, with particular focus on breast tumor detection. Compared to the conventional medical imaging and biosensor techniques, these microwave sensors not only enable better cancer detection and improve the image resolution, but also provide attractive features such as label-free detection. This paper aims to provide an overview of recent important achievements in microwave sensors for biomedical imaging applications, with particular focus on breast cancer detection. The electric properties of biological tissues at microwave spectrum, microwave imaging approaches, microwave biosensors, current challenges and future works are also discussed in the manuscript. PMID:29473867

Microwave Sensors for Breast Cancer Detection.

PubMed

Wang, Lulu

2018-02-23

Breast cancer is the leading cause of death among females, early diagnostic methods with suitable treatments improve the 5-year survival rates significantly. Microwave breast imaging has been reported as the most potential to become the alternative or additional tool to the current gold standard X-ray mammography for detecting breast cancer. The microwave breast image quality is affected by the microwave sensor, sensor array, the number of sensors in the array and the size of the sensor. In fact, microwave sensor array and sensor play an important role in the microwave breast imaging system. Numerous microwave biosensors have been developed for biomedical applications, with particular focus on breast tumor detection. Compared to the conventional medical imaging and biosensor techniques, these microwave sensors not only enable better cancer detection and improve the image resolution, but also provide attractive features such as label-free detection. This paper aims to provide an overview of recent important achievements in microwave sensors for biomedical imaging applications, with particular focus on breast cancer detection. The electric properties of biological tissues at microwave spectrum, microwave imaging approaches, microwave biosensors, current challenges and future works are also discussed in the manuscript.

Microwave-Assisted Synthesis of Phenothiazine and Quinoline Derivatives

PubMed Central

Găină, Luiza; Cristea, Castelia; Moldovan, Claudia; Porumb, Dan; Surducan, Emanoil; Deleanu, Călin; Mahamoud, Abdalah; Barbe, Jacques; Silberg, Ioan A.

2007-01-01

Application of a dynamic microwave power system in the chemical synthesis of some phenothiazine and quinoline derivatives is described. Heterocyclic ring formation, aromatic nucleophilic substitution and heterocyclic aldehydes/ketones condensation reactions were performed on solid support, or under solvent free reaction conditions. The microwave-assisted Duff formylation of phenothiazine was achieved. Comparison of microwave-assisted synthesis with the conventional synthetic methods demonstrates advantages related to shorter reaction times and in some cases better reaction yields.

Photocatalytic oxidation of ammonia by cadmium sulfide/titanate nanotubes synthesised by microwave hydrothermal method.

PubMed

Chen, Y-C; Lo, S-L; Ou, H-H; Chen, C-H

2011-01-01

CdS/Titanate nanotubes (TNTs) were successfully synthesised by a simple, rapid, and reliable microwave hydrothermal method. The CdS nanoparticles synthesised using a 140-W microwave irradiation power at 423 K photodegraded 26% ammonia in water, while the photocatalytic efficiency increased to 52.3% using the synthesised CdS/TNTs composites. The results indicated that the CdS/TNTs photocatalysts possess improved photocatalytic activity than that of CdS or TNTs materials alone.

Synthesis of ultrafine powders by microwave heating

DOEpatents

Meek, T.T.; Sheinberg, H.; Blake, R.D.

1987-04-24

A method of synthesizing ultrafine powders using microwaves is described. A water soluble material is dissolved in water and the resulting aqueous solution is exposed to microwaves until the water has dissolved. The resulting material is an ultrafine powder. This method can be used to make Al/sub 2/O/sub 3/, NiO /plus/ Al/sub 2/O/sub 3/ and NiO as well as a number of other materials including GaBa/sub 2/Cu/sub 3/O/sub x/. 1 tab.

Synthesis of ultrafine powders by microwave heating

DOEpatents

Meek, Thomas T.; Sheinberg, Haskell; Blake, Rodger D.

1988-01-01

A method of synthesizing ultrafine powders using microwaves is described. A water soluble material is dissolved in water and the resulting aqueous solution is exposed to microwaves until the water has been removed. The resulting material is an ultrafine powder. This method can be used to make Al.sub.2 O.sub.3, NiO+Al.sub.2 O.sub.3 and NiO as well as a number of other materials including GaBa.sub.2 Cu.sub.3 O.sub.x.

[Development of ICP-OES, ICP-MS and GF-AAS Methods for Simultaneous Quantification of Lead, Total Arsenic and Cadmium in Soft Drinks].

PubMed

Kataoka, Yohei; Watanabe, Takahiro; Hayashi, Tomoko; Teshima, Reiko; Matsuda, Rieko

2015-01-01

In this study, we developed methods to quantify lead, total arsenic and cadmium contained in various kinds of soft drinks, and we evaluated their performance. The samples were digested by common methods to prepare solutions for measurement by ICP-OES, ICP-MS and graphite furnace atomic absorption spectrometry (GF-AAS). After digestion, internal standard was added to the digestion solutions for measurements by ICP-OES and ICP-MS. For measurement by GF-AAS, additional purification of the digestion solution was conducted by back-extraction of the three metals into nitric acid solution after extraction into an organic solvent with ammonium pyrrolidine dithiocarbamate. Performance of the developed methods were evaluated for eight kinds of soft drinks.

Cd–cysteine precursor nanowire templated microwave-assisted transformation route to CdS nanotubes

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

Liu, Xiao-Lin, E-mail: liu_x_l@sina.cn; Zhu, Ying-Jie; Zhang, Qian

2012-12-15

Graphical abstract: Cadmium sulfide polycrystalline nanotubes have been successfully synthesized by microwave-assisted transformation method using Cd–cysteine precursor nanowires as the source material and template in ethylene glycol at 160 °C or ethanol at 60 °C. Display Omitted Highlights: ► Cd–cysteine precursor nanowires were successfully synthesized in alkaline solution. ► CdS nanotubes were prepared by templated microwave-assisted transformation method. ► CdS nanotubes can well duplicate the size and morphology of precursor nanowires. ► This method has the advantages of the simplicity and low cost. -- Abstract: We report the Cd–cysteine precursor nanowire templated microwave-assisted transformation route to CdS nanotubes. In thismore » method, the Cd–cysteine precursor nanowires are synthesized using CdCl{sub 2}·2.5H{sub 2}O, L-cysteine and ethanolamine in water at room temperature. The Cd–cysteine precursor nanowires are used as the source material and template for the subsequent preparation of CdS nanotubes by a microwave-assisted transformation method using ethylene glycol or ethanol as the solvent. This method has the advantages of the simplicity and low cost, and may be extended to the synthesis of nanotubes of other compounds. The products are characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM).« less

Rapid analysis of the essential oil components of dried Zanthoxylum bungeanum Maxim by Fe2O3-magnetic-microsphere-assisted microwave distillation and simultaneous headspace single-drop microextraction followed by GC-MS.

PubMed

Ye, Qing

2013-06-01

In this work, microwave distillation assisted by Fe2 O3 magnetic microspheres (FMMS) and headspace single-drop microextraction were combined, and developed for determination of essential oil compounds in dried Zanthoxylum bungeanum Maxim (ZBM). The FMMS were used as microwave absorption solid medium for dry distillation of dried ZBM. Using the proposed method, isolation, extraction, and concentration of essential oil compounds can be carried out in a single step. The experimental parameters including extraction solvent, solvent volume, microwave power, irradiation time, and the amount of added FMMS, were studied. The optimal analytical conditions were: 2.0 μL decane as the extraction solvent, microwave power of 300 W, irradiation time of 2 min, and the addition of 0.1 g FMMS to ZBM. The method precision was from 4 to 10%. A total of 52 compounds were identified by the proposed method. The conventional steam distillation method was also used for the analysis of essential oil in dried ZBM and only 31 compounds were identified by steam distillation method. It was found that the proposed method is a simple, rapid, reliable, and solvent-free technique for the determination of volatile compounds in Chinese herbs. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The Use of Mouse Models of Breast Cancer and Quantitative Image Analysis to Evaluate Hormone Receptor Antigenicity after Microwave-assisted Formalin Fixation

PubMed Central

Engelberg, Jesse A.; Giberson, Richard T.; Young, Lawrence J.T.; Hubbard, Neil E.

2014-01-01

Microwave methods of fixation can dramatically shorten fixation times while preserving tissue structure; however, it remains unclear if adequate tissue antigenicity is preserved. To assess and validate antigenicity, robust quantitative methods and animal disease models are needed. We used two mouse mammary models of human breast cancer to evaluate microwave-assisted and standard 24-hr formalin fixation. The mouse models expressed four antigens prognostic for breast cancer outcome: estrogen receptor, progesterone receptor, Ki67, and human epidermal growth factor receptor 2. Using pathologist evaluation and novel methods of quantitative image analysis, we measured and compared the quality of antigen preservation, percentage of positive cells, and line plots of cell intensity. Visual evaluations by pathologists established that the amounts and patterns of staining were similar in tissues fixed by the different methods. The results of the quantitative image analysis provided a fine-grained evaluation, demonstrating that tissue antigenicity is preserved in tissues fixed using microwave methods. Evaluation of the results demonstrated that a 1-hr, 150-W fixation is better than a 45-min, 150-W fixation followed by a 15-min, 650-W fixation. The results demonstrated that microwave-assisted formalin fixation can standardize fixation times to 1 hr and produce immunohistochemistry that is in every way commensurate with longer conventional fixation methods. PMID:24682322

Evaluation of collection method and diet effects on apparent digestibility and energy values of swine diets.

PubMed

Li, Y S; Tran, H; Bundy, J W; Burkey, T E; Kerr, B J; Nielsen, M K; Miller, P S

2016-06-01

Two experiments were conducted to investigate the effects of collection method and diet type on digestibility coefficients. In Exp. 1, 24 barrows were fed either a corn-soybean meal (CSBM) diet or CSBM with 20% dried distillers' grains with solubles (CSBM-DDGS). In Exp. 2, the effects of basal diet and collection method on determination of dried distillers' grains with solubles (DDGS) digestibility were studied using 24 barrows. The 4 diets used in Exp. 2 were: a CSBM (basal 1) , a barley-canola meal (BCM; basal 2), 80% basal 1 with 20% DDGS (CSBM-DDGS), and 80% basal 2 with 20% DDGS (BCM-DDGS). In both experiments, feces were collected using a time-based collection method (DY) or a "marker-to-marker" collection method (MM). Diets contained 0.5% of titanium dioxide (TiO) for estimating digestibility using the index marker approach (IM). The apparent total tract digestibility (ATTD) of DM and GE were lower ( < 0.05) in the CSBM-DDGS diet than in the CSBM diet in Exp. 1 but were not different in Exp. 2. All the estimates of BCM-based diets were consistently lower ( < 0.05) than those of CSBM-based diets. In Exp. 1, digestibility coefficients determined by the DY and MM were not different from each other, whereas those estimates were lower ( < 0.05) using the IM than those using the total collection approach (TC; DY and MM). In Exp. 2, interactions ( < 0.05) were observed between diet type and method for dietary digestibility coefficients. Digestibility and energy values estimated by the DY and MM were not different in pigs fed CSBM-based diets and the BCM-DDGS diet, whereas those estimates were greater ( < 0.05) using the DY than those using the MM in pigs fed the BCM. There were no interactions between basal diet and method for estimating DDGS digestibility. The ATTD of DM and GE of DDGS using the MM were greater ( < 0.05) than those using the IM, and ATTD of N tended to be greater ( < 0.10) using the MM than that using the IM. All estimates using the DY were not different from those using the MM or the IM, except that DE of DDGS was greater ( < 0.05) using the DY than when using the IM. Digestibility estimates of DDGS were not affected by basal diets. The mean DE and ME (as-fed basis) of DDGS were 3,994 and 3,688 kcal/kg, respectively, when estimated using the basal 1 diet and were 3,919 and 3,547 kcal/kg, respectively, when estimated using the basal 2 diet. In conclusion, both collection methods can be used to estimate energy and nutrient digestibility of diets and DDGS when using CSBM-based diets.

Estimating Apparent Nutrient Digestibility of Diets Containing Leucaena leucocephala or Moringa oleifera Leaf Meals for Growing Rabbits by Two Methods

PubMed Central

Safwat, A. M.; Sarmiento-Franco, L.; Santos-Ricalde, R. H.; Nieves, D.; Sandoval-Castro, C. A.

2015-01-01

This study aimed to evaluate the nutrient digestibility of growing rabbits fed diets with different levels of either Leucaena leucocephala (LLM) or Moringa oleifera (MOLM) leaf meals and also to compare total collection and TiO2 marker methods for estimating digestibility. A total of 30 California growing rabbits (1.81±0.19 kg live weight on average) were randomly distributed into five experimental groups of six rabbits each and were housed in individual cages. The groups were control, 30% LLM, 40% LLM, 30% MOLM, and 40% MOLM. All groups received pelleted diets for two weeks; diets also contained 4 g/kg titanium dioxide as dietary marker. Daily feed intake was recorded during the whole experimental period and total feces were collected daily and weighed individually during four days. The results showed that there were no difference (p>0.05) in feed, dry matter (DM), organic matter (OM), crude protein (CP), digestible energy, and crude fiber (CF) intake between the control group and the other experimental groups. The apparent digestibility values of DM, OM, CP, CF, acid detergent fiber, and gross energy were the highest for control group (p = 0.001), meanwhile MOLM diets had generally higher nutrient digestibility coefficients than LLM diets. Increasing the inclusion level of leaf meal in the diet from 30% to 40% improved the digestibility of CF from 45.02% to 51.69% for LLM and from 48.11% to 55.89% for MOLM. Similar results for apparent nutrient digestibility coefficients were obtained when either total collection or indigestible marker method was used. In conclusion, the digestibility of MOLM containing diets were better than LLM diets, furthermore TiO2 as an external marker could be used as a simple, practical and reliable method to estimate nutrients digestibility in rabbit diets. PMID:26104524

Estimating Apparent Nutrient Digestibility of Diets Containing Leucaena leucocephala or Moringa oleifera Leaf Meals for Growing Rabbits by Two Methods.

PubMed

Safwat, A M; Sarmiento-Franco, L; Santos-Ricalde, R H; Nieves, D; Sandoval-Castro, C A

2015-08-01

This study aimed to evaluate the nutrient digestibility of growing rabbits fed diets with different levels of either Leucaena leucocephala (LLM) or Moringa oleifera (MOLM) leaf meals and also to compare total collection and TiO2 marker methods for estimating digestibility. A total of 30 California growing rabbits (1.81±0.19 kg live weight on average) were randomly distributed into five experimental groups of six rabbits each and were housed in individual cages. The groups were control, 30% LLM, 40% LLM, 30% MOLM, and 40% MOLM. All groups received pelleted diets for two weeks; diets also contained 4 g/kg titanium dioxide as dietary marker. Daily feed intake was recorded during the whole experimental period and total feces were collected daily and weighed individually during four days. The results showed that there were no difference (p>0.05) in feed, dry matter (DM), organic matter (OM), crude protein (CP), digestible energy, and crude fiber (CF) intake between the control group and the other experimental groups. The apparent digestibility values of DM, OM, CP, CF, acid detergent fiber, and gross energy were the highest for control group (p = 0.001), meanwhile MOLM diets had generally higher nutrient digestibility coefficients than LLM diets. Increasing the inclusion level of leaf meal in the diet from 30% to 40% improved the digestibility of CF from 45.02% to 51.69% for LLM and from 48.11% to 55.89% for MOLM. Similar results for apparent nutrient digestibility coefficients were obtained when either total collection or indigestible marker method was used. In conclusion, the digestibility of MOLM containing diets were better than LLM diets, furthermore TiO2 as an external marker could be used as a simple, practical and reliable method to estimate nutrients digestibility in rabbit diets.

High-Power Microwave Transmission and Mode Conversion Program

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

Vernon, Ronald J.

2015-08-14

This is a final technical report for a long term project to develop improved designs and design tools for the microwave hardware and components associated with the DOE Plasma Fusion Program. We have developed basic theory, software, fabrication techniques, and low-power measurement techniques for the design of microwave hardware associated gyrotrons, microwave mode converters and high-power microwave transmission lines. Specifically, in this report we discuss our work on designing quasi-optical mode converters for single and multiple frequencies, a new method for the analysis of perturbed-wall waveguide mode converters, perturbed-wall launcher design for TE0n mode gyrotrons, quasi-optical traveling-wave resonator design formore » high-power testing of microwave components, and possible improvements to the HSX microwave transmission line.« less

The microwave-assisted ionic-liquid method: a promising methodology in nanomaterials.

PubMed

Ma, Ming-Guo; Zhu, Jie-Fang; Zhu, Ying-Jie; Sun, Run-Cang

2014-09-01

In recent years, the microwave-assisted ionic-liquid method has been accepted as a promising methodology for the preparation of nanomaterials and cellulose-based nanocomposites. Applications of this method in the preparation of cellulose-based nanocomposites comply with the major principles of green chemistry, that is, they use an environmentally friendly method in environmentally preferable solvents to make use of renewable materials. This minireview focuses on the recent development of the synthesis of nanomaterials and cellulose-based nanocomposites by means of the microwave-assisted ionic-liquid method. We first discuss the preparation of nanomaterials including noble metals, metal oxides, complex metal oxides, metal sulfides, and other nanomaterials by means of this method. Then we provide an overview of the synthesis of cellulose-based nanocomposites by using this method. The emphasis is on the synthesis, microstructure, and properties of nanostructured materials obtained through this methodology. Our recent research on nanomaterials and cellulose-based nanocomposites by this rapid method is summarized. In addition, the formation mechanisms involved in the microwave-assisted ionic-liquid synthesis of nanostructured materials are discussed briefly. Finally, the future perspectives of this methodology in the synthesis of nanostructured materials are proposed. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Adaptive and robust statistical methods for processing near-field scanning microwave microscopy images.

PubMed

Coakley, K J; Imtiaz, A; Wallis, T M; Weber, J C; Berweger, S; Kabos, P

2015-03-01

Near-field scanning microwave microscopy offers great potential to facilitate characterization, development and modeling of materials. By acquiring microwave images at multiple frequencies and amplitudes (along with the other modalities) one can study material and device physics at different lateral and depth scales. Images are typically noisy and contaminated by artifacts that can vary from scan line to scan line and planar-like trends due to sample tilt errors. Here, we level images based on an estimate of a smooth 2-d trend determined with a robust implementation of a local regression method. In this robust approach, features and outliers which are not due to the trend are automatically downweighted. We denoise images with the Adaptive Weights Smoothing method. This method smooths out additive noise while preserving edge-like features in images. We demonstrate the feasibility of our methods on topography images and microwave |S11| images. For one challenging test case, we demonstrate that our method outperforms alternative methods from the scanning probe microscopy data analysis software package Gwyddion. Our methods should be useful for massive image data sets where manual selection of landmarks or image subsets by a user is impractical. Published by Elsevier B.V.

Metal concentrations of wild edible mushrooms from Turkey.

PubMed

Sarikurkcu, Cengiz; Tepe, Bektas; Solak, Mehmet Halil; Cetinkaya, Serap

2012-01-01

In the present study, the contents of Zn, Fe, Cu, Mn, Co, Ni, Pb, Cd, Cr, Al, Ca, Mg, and K in Agaricus campestris, Agrocybe cylindracea, Collybia dryophila, Helvella leucopus, Russula delica, Tricholoma auratum, Amanita ovoidea, Melanoleuca excissa, Rhizopogon roseolus, Russula chloroides, Volvoriella gloiocephala, Lyophyllum decastes, Morcella angusticeps, Morchella esculenta and Morcella eximia collected from Isparta, Mugla, and Osmaniye provinces (Turkey) were determined by inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave digestion. The intake of heavy metals (Pb, Cd) and other metals (Fe, Cu, Zn) by consumption of 30 g dry weight of mushrooms daily poses no risk at all except in A. cylindracea and H. leucopus (for Cd) for the consumer.

Fast microwave-assisted extraction of rotenone for its quantification in seeds of yam bean (Pachyrhizus sp.).

PubMed

Lautié, Emmanuelle; Rasse, Catherine; Rozet, Eric; Mourgues, Claire; Vanhelleputte, Jean-Paul; Quetin-Leclercq, Joëlle

2013-02-01

The aim of this study was to find if fast microwave-assisted extraction could be an alternative to the conventional Soxhlet extraction for the quantification of rotenone in yam bean seeds by SPE and HPLC-UV. For this purpose, an experimental design was used to determine the optimal conditions of the microwave extraction. Then the values of the quantification on three accessions from two different species of yam bean seeds were compared using the two different kinds of extraction. A microwave extraction of 11 min at 55°C using methanol/dichloromethane (50:50) allowed rotenone extraction either equivalently or more efficiently than the 8-h-Soxhlet extraction method and was less sensitive to moisture content. The selectivity, precision, trueness, accuracy, and limit of quantification of the method with microwave extraction were also demonstrated. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Smelting Magnesium Metal using a Microwave Pidgeon Method

PubMed Central

Wada, Yuji; Fujii, Satoshi; Suzuki, Eiichi; Maitani, Masato M.; Tsubaki, Shuntaro; Chonan, Satoshi; Fukui, Miho; Inazu, Naomi

2017-01-01

Magnesium (Mg) is a lightweight metal with applications in transportation and sustainable battery technologies, but its current production through ore reduction using the conventional Pidgeon process emits large amounts of CO2 and particulate matter (PM2.5). In this work, a novel Pidgeon process driven by microwaves has been developed to produce Mg metal with less energy consumption and no direct CO2 emission. An antenna structure consisting of dolomite as the Mg source and a ferrosilicon antenna as the reducing material was used to confine microwave energy emitted from a magnetron installed in a microwave oven to produce a practical amount of pure Mg metal. This microwave Pidgeon process with an antenna configuration made it possible to produce Mg with an energy consumption of 58.6 GJ/t, corresponding to a 68.6% reduction when compared to the conventional method. PMID:28401910

Microwave modification of surface hydroxyl density for g-C3N4 with enhanced photocatalytic activity

NASA Astrophysics Data System (ADS)

An, Na; Zhao, Yang; Mao, Zhiyong; Agrawal, Dinesh Kumar; Wang, Dajian

2018-03-01

Microwave modification was performed on graphitic carbon nitride (g-C3N4) photocatalysts to tail the surface hydroxyl content for enhanced photocatalytic activity in this work. The influence of microwave heating on the surface hydroxyl density was investigated by a suite of characterization methods. The microwave treated g-C3N4 (MT-g-C3N4) delivered a higher photocatalytic activity in degradation of Rhodamine B (RhB) under visible light irradiation than pristine g-C3N4 due to its improved separation efficiency of photogenerated charge carries and promoted absorption capacity of RhB reactants on surface, which resulted from the increased surface hydroxyl density induced by microwave treatment. This study provides a simple and convenient method to modify g-C3N4 materials with enhanced photocatalytic activity for the potential application in photocatalytic elimination of environmental pollutants.

Microwave-Assisted Hydro-Distillation of Essential Oil from Rosemary: Comparison with Traditional Distillation.

PubMed

Moradi, Sara; Fazlali, Alireza; Hamedi, Hamid

2018-01-01

Hydro-distillation (HD) method is a traditional technique which is used in most industrial companies. Microwave-assisted Hydro-distillation (MAHD) is an advanced HD technique utilizing a microwave oven in the extraction process. In this research, MAHD of essential oils from the aerial parts (leaves) of rosemary ( Rosmarinus officinalis L. ) was studied and the results were compared with those of the conventional HD in terms of extraction time, extraction efficiency, chemical composition, quality of the essential oils and cost of the operation. Microwave hydro-distillation was superior in terms of saving energy and extraction time (30 min , compared to 90 min in HD). Chromatography was used for quantity analysis of the essential oils composition. Quality of essential oil improved in MAHD method due to an increase of 17% in oxygenated compounds. Consequently, microwave hydro-distillation can be used as a substitute of traditional hydro-distillation.

Microwave hemorrhagic stroke detector

DOEpatents

Haddad, Waleed S.; Trebes, James E.

2002-01-01

The microwave hemorrhagic stroke detector includes a low power pulsed microwave transmitter with a broad-band antenna for producing a directional beam of microwaves, an index of refraction matching cap placed over the patients head, and an array of broad-band microwave receivers with collection antennae. The system of microwave transmitter and receivers are scanned around, and can also be positioned up and down the axis of the patients head. The microwave hemorrhagic stroke detector is a completely non-invasive device designed to detect and localize blood pooling and clots or to measure blood flow within the head or body. The device is based on low power pulsed microwave technology combined with specialized antennas and tomographic methods. The system can be used for rapid, non-invasive detection of blood pooling such as occurs with hemorrhagic stroke in human or animal patients as well as for the detection of hemorrhage within a patient's body.

Microwave hemorrhagic stroke detector

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

Haddad, Waleed S; Trebes, James E

The microwave hemorrhagic stroke detector includes a low power pulsed microwave transmitter with a broad-band antenna for producing a directional beam of microwaves, an index of refraction matching cap placed over the patients head, and an array of broad-band microwave receivers with collection antennae. The system of microwave transmitter and receivers are scanned around, and can also be positioned up and down the axis of the patients head. The microwave hemorrhagic stroke detector is a completely non-invasive device designed to detect and localize blood pooling and clots or to measure blood flow within the head or body. The device ismore » based on low power pulsed microwave technology combined with specialized antennas and tomographic methods. The system can be used for rapid, non-invasive detection of blood pooling such as occurs with hemorrhagic stoke in human or animal patients as well as for the detection of hemorrhage within a patient's body.« less

Microwave fixation versus formalin fixation of surgical and autopsy tissue.

PubMed

Login, G R

1978-05-01

Microwave irradiation of surgical and autopsy tissue penetrates, fixes, and hardens the tissue almost immediately (the fluid media used in the microwave consisted of saline, ten percent phosphate buffered formalin, and distilled water). Tissue sections from a representative sample of organs were tested. Comparable sections were simultaneously fixed in a phosphate buffered ten percent formalin bath in a vaccum oven as a control. Hematoxylin and eosin were used to stain the sections. Results equal to and superior to the control method were obtained. Saline microwave fixation was superior to formalin microwave fixation. Tissues placed in Zenker's solution and fixed in standard microwave oven (for approximately one minute) yielded results at least equal to conventional Zenker fixation (approximately two hours). No tissue hardening resulted from Zenker microwave fixation. A unique time versus temperature graph (microwave heating curve) reduces individual variation with this technique.

Remote measurement of microwave distribution based on optical detection

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

Ji, Zhong; Ding, Wenzheng; Yang, Sihua

2016-01-04

In this letter, we present the development of a remote microwave measurement system. This method employs an arc discharge lamp that serves as an energy converter from microwave to visible light, which can propagate without transmission medium. Observed with a charge coupled device, quantitative microwave power distribution can be achieved when the operators and electronic instruments are in a distance from the high power region in order to reduce the potential risk. We perform the experiments using pulsed microwaves, and the results show that the system response is dependent on the microwave intensity over a certain range. Most importantly, themore » microwave distribution can be monitored in real time by optical observation of the response of a one-dimensional lamp array. The characteristics of low cost, a wide detection bandwidth, remote measurement, and room temperature operation make the system a preferred detector for microwave applications.« less

System to continuously produce carbon fiber via microwave assisted plasma processing

DOEpatents

White, Terry L; Paulauskas, Felix L; Bigelow, Timothy S

2014-03-25

A method for continuously processing carbon fiber including establishing a microwave plasma in a selected atmosphere contained in an elongated chamber having a microwave power gradient along its length defined by a lower microwave power at one end and a higher microwave power at the opposite end of the elongated chamber. The elongated chamber having an opening in each of the ends of the chamber that are adapted to allow the passage of the fiber tow while limiting incidental gas flow into or out of said chamber. A continuous fiber tow is introduced into the end of the chamber having the lower microwave power. The fiber tow is withdrawn from the opposite end of the chamber having the higher microwave power. The fiber to is subjected to progressively higher microwave energy as the fiber is being traversed through the elongated chamber.

Evaluation of Wet Chemical ICP-AES Elemental Analysis Methods usingSimulated Hanford Waste Samples-Phase I Interim Report

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

Coleman, Charles J.; Edwards, Thomas B.

2005-04-30

The wet chemistry digestion method development for providing process control elemental analyses of the Hanford Tank Waste Treatment and Immobilization Plant (WTP) Melter Feed Preparation Vessel (MFPV) samples is divided into two phases: Phase I consists of: (1) optimizing digestion methods as a precursor to elemental analyses by ICP-AES techniques; (2) selecting methods with the desired analytical reliability and speed to support the nine-hour or less turnaround time requirement of the WTP; and (3) providing baseline comparison to the laser ablation (LA) sample introduction technique for ICP-AES elemental analyses that is being developed at the Savannah River National Laboratory (SRNL).more » Phase II consists of: (1) Time-and-Motion study of the selected methods from Phase I with actual Hanford waste or waste simulants in shielded cell facilities to ensure that the methods can be performed remotely and maintain the desired characteristics; and (2) digestion of glass samples prepared from actual Hanford Waste tank sludge for providing comparative results to the LA Phase II study. Based on the Phase I testing discussed in this report, a tandem digestion approach consisting of sodium peroxide fusion digestions carried out in nickel crucibles and warm mixed-acid digestions carried out in plastic bottles has been selected for Time-and-Motion study in Phase II. SRNL experience with performing this analytical approach in laboratory hoods indicates that well-trained cell operator teams will be able to perform the tandem digestions in five hours or less. The selected approach will produce two sets of solutions for analysis by ICP-AES techniques. Four hours would then be allocated for performing the ICP-AES analyses and reporting results to meet the nine-hour or less turnaround time requirement. The tandem digestion approach will need to be performed in two separate shielded analytical cells by two separate cell operator teams in order to achieve the nine-hour or less turnaround time. Because of the simplicity of the warm mixed-acid method, a well-trained cell operator team may in time be able to perform both sets of digestions. However, having separate shielded cells for each of the methods is prudent to avoid overcrowding problems that would impede a minimal turnaround time.« less

The aluminium content of infant formulas remains too high

PubMed Central

2013-01-01

Background Recent research published in this journal highlighted the issue of the high content of aluminium in infant formulas. The expectation was that the findings would serve as a catalyst for manufacturers to address a significant problem of these, often necessary, components of infant nutrition. It is critically important that parents and other users have confidence in the safety of infant formulas and that they have reliable information to use in choosing a product with a lower content of aluminium. Herein, we have significantly extended the scope of the previous research and the aluminium content of 30 of the most widely available and often used infant formulas has been measured. Methods Both ready-to-drink milks and milk powders were subjected to microwave digestion in the presence of 15.8 M HNO3 and 30% w/v H2O2 and the aluminium content of the digests was measured by TH GFAAS. Results Both ready-to-drink milks and milk powders were contaminated with aluminium. The concentration of aluminium across all milk products ranged from ca 100 to 430 μg/L. The concentration of aluminium in two soya-based milk products was 656 and 756 μg/L. The intake of aluminium from non-soya-based infant formulas varied from ca 100 to 300 μg per day. For soya-based milks it could be as high as 700 μg per day. Conclusions All 30 infant formulas were contaminated with aluminium. There was no clear evidence that subsequent to the problem of aluminium being highlighted in a previous publication in this journal that contamination had been addressed and reduced. It is the opinion of the authors that regulatory and other non-voluntary methods are now required to reduce the aluminium content of infant formulas and thereby protect infants from chronic exposure to dietary aluminium. PMID:24103160

Determination of trace rare earth elements in gadolinium aluminate by inductively coupled plasma time of flight mass spectrometry

NASA Astrophysics Data System (ADS)

Saha, Abhijit; Deb, S. B.; Nagar, B. K.; Saxena, M. K.

An analytical methodology was developed for the precise quantification of ten trace rare earth elements (REEs), namely, La, Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, and Tm, in gadolinium aluminate (GdAlO3) employing an ultrasonic nebulizer (USN)-desolvating device based inductively coupled plasma mass spectrometry (ICP-MS). A microwave digestion procedure was optimized for digesting 100 mg of the refractory oxide using a mixture of sulphuric acid (H2SO4), phosphoric acid (H3PO4) and water (H2O) with 1400 W power, 10 min ramp and 60 min hold time. An USN-desolvating sample introduction system was employed to enhance analyte sensitivities by minimizing their oxide ion formation in the plasma. Studies on the effect of various matrix concentrations on the analyte intensities revealed that precise quantification of the analytes was possible with matrix level of 250 mg L- 1. The possibility of using indium as an internal standard was explored and applied to correct for matrix effect and variation in analyte sensitivity under plasma operating conditions. Individual oxide ion formation yields were determined in matrix matched solution and employed for correcting polyatomic interferences of light REE (LREE) oxide ions on the intensities of middle and heavy rare earth elements (MREEs and HREEs). Recoveries of ≥ 90% were achieved for the analytes employing standard addition technique. Three real samples were analyzed for traces of REEs by the proposed method and cross validated for Eu and Nd by isotope dilution mass spectrometry (IDMS). The results show no significant difference in the values at 95% confidence level. The expanded uncertainty (coverage factor 1σ) in the determination of trace REEs in the samples were found to be between 3 and 8%. The instrument detection limits (IDLs) and the method detection limits (MDLs) for the ten REEs lie in the ranges 1-5 ng L- 1 and 7-64 μg kg- 1 respectively.

An efficient microwave-assisted synthesis method for the production of water soluble amine-terminated Si nanoparticles.

PubMed

Atkins, Tonya M; Louie, Angelique Y; Kauzlarich, Susan M

2012-07-27

Silicon nanoparticles can be considered a green material, especially when prepared via a microwave-assisted method without the use of highly reactive reducing agents or hydrofluoric acid. A simple solution synthesis of hydrogen-terminated Si- and Mn-doped Si nanoparticles via microwave-assisted synthesis is demonstrated. The reaction of the Zintl salt, Na(4)Si(4), or Mn-doped Na(4)Si(4), Na(4)Si(4(Mn)), with ammonium bromide, NH(4)Br, produces small dispersible nanoparticles along with larger particles that precipitate. Allylamine and 1-amino-10-undecene were reacted with the hydrogen-terminated Si nanoparticles to provide water solubility and stability. A one-pot, single-reaction process and a one-pot, two-step reaction process were investigated. Details of the microwave-assisted process are provided, with the optimal synthesis being the one-pot, two-step reaction procedure and a total time of about 15 min. The nanoparticles were characterized by transmission electron microscopy (TEM), x-ray diffraction, and fluorescence spectroscopies. The microwave-assisted method reliably produces a narrow size distribution of Si nanoparticles in solution.

Computational fluid dynamics and frequency-dependent finite-difference time-domain method coupling for the interaction between microwaves and plasma in rocket plumes

NASA Astrophysics Data System (ADS)

Kinefuchi, K.; Funaki, I.; Shimada, T.; Abe, T.

2012-10-01

Under certain conditions during rocket flights, ionized exhaust plumes from solid rocket motors may interfere with radio frequency transmissions. To understand the relevant physical processes involved in this phenomenon and establish a prediction process for in-flight attenuation levels, we attempted to measure microwave attenuation caused by rocket exhaust plumes in a sea-level static firing test for a full-scale solid propellant rocket motor. The microwave attenuation level was calculated by a coupling simulation of the inviscid-frozen-flow computational fluid dynamics of an exhaust plume and detailed analysis of microwave transmissions by applying a frequency-dependent finite-difference time-domain method with the Drude dispersion model. The calculated microwave attenuation level agreed well with the experimental results, except in the case of interference downstream the Mach disk in the exhaust plume. It was concluded that the coupling estimation method based on the physics of the frozen plasma flow with Drude dispersion would be suitable for actual flight conditions, although the mixing and afterburning in the plume should be considered depending on the flow condition.

Numerical Analysis of Microwave Heating on Saponification Reaction

NASA Astrophysics Data System (ADS)

Huang, Kama; Jia, Kun

2005-01-01

Currently, microwave is widely used in chemical industry to accelerate chemical reactions. Saponification reaction has important applications in industry; some research results have shown that microwave heating can significantly accelerate the reaction [1]. But so far, no efficient method has been reported for the analysis of the heating process and design of an efficient reactor powered by microwave. In this paper, we present a method to study the microwave heating process on saponification reaction, where the reactant in a test tube is considered as a mixture of dilute solution. According to the preliminary measurement results, the effective permittivity of the mixture is approximately the permittivity of water, but the conductivity, which could change with the reaction, is derived from the reaction equation (RE). The electromagnetic field equation and reaction equation are coupled by the conductivity. Following that, the whole heating processes, which is described by Maxwell's equations, the reaction equation and heat transport equation (HTE), is analyzed by finite difference time domain (FDTD) method. The temperature rising in the test tube are measured and compared with the computational results. Good agreement can be seen between the measured and calculated results.

Microwave-Assisted Synthesis of High Dielectric Constant CaCu3Ti4O12 from Sol-Gel Precursor

NASA Astrophysics Data System (ADS)

Ouyang, Xin; Cao, Peng; Huang, Saifang; Zhang, Weijun; Huang, Zhaohui; Gao, Wei

2015-07-01

CaCu3Ti4O12 (CCTO) powders derived from sol-gel precursors were calcined and sintered via microwave radiation. The obtained CCTO powders were compared with that obtained via a conventional heating method. For microwave heating, 89.1 wt.% CCTO was achieved from the sol-gel precursor, after only 17 min at 950°C. In contrast, the conventional calcination method required 3 h to generate 87.6 wt.% CCTO content at 1100°C. In addition, the CCTO powders prepared through 17 min of microwave calcination exhibited a small particle size distribution of D50 = 3.826 μm. It was found that a lengthy hold time of 1 h by microwave sintering is required to obtain a high dielectric constant (3.14 × 103 at 102 Hz) and a reasonably low dielectric loss (0.161) in the sintered CCTO ceramic. Based upon the distinct microstructures, the dielectric responses of the CCTO samples sintered by different methods are attributed to space charge polarization and internal barrier layer capacitor mechanism.

[Study on friction and wear properties of dental zirconia ceramics processed by microwave and conventional sintering methods].

PubMed

Guoxin, Hu; Ying, Yang; Yuemei, Jiang; Wenjing, Xia

2017-04-01

This study evaluated the wear of an antagonist and friction and wear properties of dental zirconia ceramic that was subjected to microwave and conventional sintering methods. Ten specimens were fabricated from Lava brand zirconia and randomly assigned to microwave and conventional sintering groups. A profile tester for surface roughness was used to measure roughness of the specimens. Wear test was performed, and steatite ceramic was used as antagonist. Friction coefficient curves were recorded, and wear volume were calculated. Finally, optical microscope was used to observe the surface morphology of zirconia and steatite ceramics. Field emission scanning electron microscopy was used to observe the microstructure of zirconia. Wear volumes of microwave and conventionally sintered zirconia were (6.940±1.382)×10⁻², (7.952±1.815) ×10⁻² mm³, respectively. Moreover, wear volumes of antagonist after sintering by the considered methods were (14.189±4.745)×10⁻², (15.813±3.481)×10⁻² mm³, correspondingly. Statistically significant difference was not observed in the wear resistance of zirconia and wear volume of steatite ceramic upon exposure to two kinds of sintering methods. Optical microscopy showed that ploughed surfaces were apparent in zirconia. The wear surface of steatite ceramic against had craze, accompanied by plough. Scanning electron microscopy showed that zirconia was sintered compactly when subjected to both conventional sintering and microwave methods, whereas grains of zirconia sintered by microwave alone were smaller and more uniform. Two kinds of sintering methods are successfully used to produce dental zirconia ceramics with similar friction and wear properties.
.

Current perspective on assessing site of digestion in ruminants.

PubMed

Merchen, N R; Elizalde, J C; Drackley, J K

1997-08-01

The site of nutrient digestion in the gastrointestinal tract of ruminants affects nutrient availability and the nature of digestive end-products supplied to the host animal. Methods to study site of digestion in vivo provide a tool to obtain data that enhance the ability to interpret or predict animal responses to some feeding practices. Examples are discussed for which site of digestion data provided insights that might not have been evident from other approaches. The use of site of digestion techniques may provide interpretation regarding digestion of N by ruminants different from those derived from measurement of total tract N digestion. Site of digestion measurements have been particularly important in studying effects of heat processing of protein sources and in understanding the nature of digestion of N in high-quality, fresh forages. Moreover, site of digestion techniques have been instrumental in interpreting the influences of supplemental fat sources on ruminal digestion and ruminal biohydrogenation and small intestinal digestion of long-chain fatty acids.

Geometry for web microwave heating or drying to a desired profile in a waveguide

DOEpatents

Habeger, Jr., Charles C.; Patterson, Timothy F.; Ahrens, Frederick W.

2005-11-15

A microwave heater and/or dryer has a nonlinear or curvilinear relative slot profile geometry. In one embodiment, the microwave dryer has at least one adjustable field modifier making it possible to change the geometry of the heater or dryer when drying different webs. In another embodiment, the microwave dryer provides more uniform drying of a web when the field modifier is adjusted in response to a sensed condition of the web. Finally, a method of microwave heating and/or drying a web achieves a uniform heating and/or drying profile.

Microwave-assisted Maillard reactions for the preparation of advanced glycation end products (AGEs).

PubMed

Visentin, Sonja; Medana, Claudio; Barge, Alessandro; Giancotti, Valeria; Cravotto, Giancarlo

2010-05-21

The application of microwaves as an efficient form of volumetric heating to promote organic reactions was recognized in the mid-1980 s. It has a much longer history in the food research and industry where microwave irradiation was studied in depth to optimize food browning and the development of desirable flavours from Maillard reactions. The microwave-promoted Maillard reaction is a challenging synthetic method to generate molecular diversity in a straightforward way. In this paper we present a new rapid and efficient one-pot procedure for the preparation of pentosidine and other AGEs under microwave irradiation.

Feasibility of Rare Earth Element Determination in Low Concentration in Crude Oil: Direct Sampling Electrothermal Vaporization-Inductively Coupled Plasma Mass Spectrometry.

PubMed

Silva, Jussiane Souza; Schneider Henn, Alessandra; Dressler, Valderi Luiz; Mello, Paola Azevedo; Flores, Erico Marlon Moraes

2018-06-05

A comprehensive study was developed showing the feasibility of determination of rare earth elements (REE) in low concentration in crude oil by using direct sampling electrothermal vaporization system coupled to inductively coupled plasma mass spectrometry (ETV-ICP-MS). The effect of organic modifier on the REE signal was evaluated and the use of 6 mg of citric acid allowed calibration using aqueous reference solutions (selected pyrolysis and vaporization temperatures were 700 and 2200 °C, respectively). Because of the facility of REE in forming refractory compounds inside the graphite furnace during the heating step, the use of a modifier gas (Freon R-12, 3.0 mL min -1 ) was necessary to allow quantitative vaporization of these elements. A flow rate of 0.40 L min -1 was selected for both bypass and carrier gases. Under optimized conditions, the influence of sample mass was evaluated, and even using a relatively high mass of crude oil (up to 18 mg), accurate results were obtained. The accuracy was evaluated by the comparison of results by ETV-ICP-MS with those obtained by ICP-MS with ultrasonic nebulizer (USN) after high-pressure microwave-assisted wet digestion (MAWD) and microwave-induced combustion (MIC) and no statistical difference was observed between the results. The limits of quantification for REE by ETV-ICP-MS were lower (0.02-0.8 ng g -1 ) than those obtained by USN-ICP-MS after MAWD and MIC (0.6-5.1 ng g -1 ). Negligible blank values and relative standard deviations lower than 12% show the feasibility of the proposed ETV-ICP-MS method for routine analysis of crude oil.

Digestibility of gluten proteins is reduced by baking and enhanced by starch digestion

PubMed Central

Pan, Xiaoyan; Bellido, Vincent; Toole, Geraldine A.; Gates, Fred K.; Wickham, Martin S. J.; Shewry, Peter R.; Bakalis, Serafim; Padfield, Philip; Mills, E. N. Clare

2015-01-01

Scope Resistance of proteins to gastrointestinal digestion may play a role in determining immune‐mediated adverse reactions to foods. However, digestion studies have largely been restricted to purified proteins and the impact of food processing and food matrices on protein digestibility is poorly understood. Methods and results Digestibility of a total gliadin fraction (TGF), flour (cv Hereward), and bread was assessed using in vitro batch digestion with simulated oral, gastric, and duodenal phases. Protein digestion was monitored by SDS‐PAGE and immunoblotting using monoclonal antibodies specific for celiac‐toxic sequences (QQSF, QPFP) and starch digestion by measuring undigested starch. Whereas the TGF was rapidly digested during the gastric phase the gluten proteins in bread were virtually undigested and digested rapidly during the duodenal phase only if amylase was included. Duodenal starch digestion was also slower in the absence of duodenal proteases. Conclusion The baking process reduces the digestibility of wheat gluten proteins, including those containing sequences active in celiac disease. Starch digestion affects the extent of protein digestion, probably because of gluten‐starch complex formation during baking. Digestion studies using purified protein fractions alone are therefore not predictive of digestion in complex food matrices. PMID:26202208

Observations of cloud liquid water path over oceans: Optical and microwave remote sensing methods

NASA Technical Reports Server (NTRS)

Lin, Bing; Rossow, William B.

1994-01-01

Published estimates of cloud liquid water path (LWP) from satellite-measured microwave radiation show little agreement, even about the relative magnitudes of LWP in the tropics and midlatitudes. To understand these differences and to obtain more reliable estimate, optical and microwave LWP retrieval methods are compared using the International Satellite Cloud Climatology Project (ISCCP) and special sensor microwave/imager (SSM/I) data. Errors in microwave LWP retrieval associated with uncertainties in surface, atmosphere, and cloud properties are assessed. Sea surface temperature may not produce great LWP errors, if accurate contemporaneous measurements are used in the retrieval. An uncertainty of estimated near-surface wind speed as high as 2 m/s produces uncertainty in LWP of about 5 mg/sq cm. Cloud liquid water temperature has only a small effect on LWP retrievals (rms errors less than 2 mg/sq cm), if errors in the temperature are less than 5 C; however, such errors can produce spurious variations of LWP with latitude and season. Errors in atmospheric column water vapor (CWV) are strongly coupled with errors in LWP (for some retrieval methods) causing errors as large as 30 mg/sq cm. Because microwave radiation is much less sensitive to clouds with small LWP (less than 7 mg/sq cm) than visible wavelength radiation, the microwave results are very sensitive to the process used to separate clear and cloudy conditions. Different cloud detection sensitivities in different microwave retrieval methods bias estimated LWP values. Comparing ISCCP and SSM/I LWPs, we find that the two estimated values are consistent in global, zonal, and regional means for warm, nonprecipitating clouds, which have average LWP values of about 5 mg/sq cm and occur much more frequently than precipitating clouds. Ice water path (IWP) can be roughly estimated from the differences between ISCCP total water path and SSM/I LWP for cold, nonprecipitating clouds. IWP in the winter hemisphere is about 3 times the LWP but only half the LWP in the summer hemisphere. Precipitating clouds contribute significantly to monthly, zonal mean LWP values determined from microwave, especially in the intertropical convergence zone (ITCZ), because they have almost 10 times the liquid water (cloud plus precipitation) of nonprecipitating clouds on average. There are significant differences among microwave LWP estimates associated with the treatment of precipitating clouds.

Integrated microwave processing system for the extraction of organophosphorus pesticides in fresh vegetables.

PubMed

Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

2015-03-01

A simple and efficient integrated microwave processing system (IMPS) was firstly assembled and validated for the extraction of organophosphorus pesticides in fresh vegetables. Two processes under microwave irradiation, dynamic microwave-assisted extraction (DMAE) and microwave-accelerated solvent elution (MASE), were integrated for simplifying the pretreatment of the sample. Extraction, separation, enrichment and elution were finished in a simple step. The organophosphorus pesticides were extracted from the fresh vegetables into hexane with DMAE, and then the extract was directly introduced into the enrichment column packed with active carbon fiber (ACF). Subsequently, the organophosphorus pesticides trapped on the ACF were eluted with ethyl acetate under microwave irradiation. No further filtration or cleanup was required before analysis of the eluate by gas chromatography-mass spectrometry. Some experimental parameters affecting extraction efficiency were investigated and optimized, such as microwave output power, kind and volume of extraction solvent, extraction time, amount of sorbent, elution microwave power, kind and volume of elution solvent, elution solvent flow rate. Under the optimized conditions, the recoveries were in the range of 71.5-105.2%, and the relative standard deviations were lower than 11.6%. The experiment results prove that the present method is a simple and effective sample preparation method for the determination of pesticides in solid samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Active microwave water equivalence

NASA Technical Reports Server (NTRS)

Boyne, H. S.; Ellerbruch, D. A.

1980-01-01

Measurements of water equivalence using an active FM-CW microwave system were conducted over the past three years at various sites in Colorado, Wyoming, and California. The measurement method is described. Measurements of water equivalence and stratigraphy are compared with ground truth. A comparison of microwave, federal sampler, and snow pillow measurements at three sites in Colorado is described.

Microwave sintering of single plate-shaped articles

DOEpatents

Katz, Joel D.; Blake, Rodger D.

1995-01-01

Apparatus and method for high temperature sintering of plate-shaped articles of alumina, magnesia, silica, yttria, zirconia, and mixtures thereof using microwave radiation. An article is placed within a sintering structure located within a sintering container which is placed in a microwave cavity for heating. The rates at which heating and cooling take place is controlled.