Sample records for mibk

  1. Methyl isobutyl ketone (MIBK)

    Integrated Risk Information System (IRIS)

    Methyl Isobutyl Ketone ( MIBK ) ; CASRN 108 - 10 - 1 ; Human health assessment information on a chemical substance is included in the IRIS database only after a comprehensive review of toxicity data , as outlined in the IRIS assessment development process . Sections I ( Health Hazard Assessments for

  2. Influence of Salts on the Partitioning of 5-Hydroxymethylfurfural in Water/MIBK.


    Mohammad, Sultan; Held, Christoph; Altuntepe, Emrah; Köse, Tülay; Sadowski, Gabriele


    This study investigates the influence of electrolytes on the performance of extracting 5-hydroxymethylfurfural (HMF) from aqueous media using methyl isobutyl ketone (MIBK). For that purpose, liquid-liquid phase equilibria (LLE) of quaternary systems containing HMF, water, MIBK and salts were measured at atmospheric pressure and 298.15 K. The salts under investigation were composed of one of the anions NO(3-), SO4(2-), Cl(-), or CH3COO(-) and of one of the alkali cations Li(+), Na(+), or K(+). On the basis of these LLE data, the partition coefficient of HMF between the aqueous and the MIBK phase KHMF was determined. It could be shown that KHMF significantly depends on the kind and concentration of the added salt. Weak electrolytes (e.g., sulfates, acetates) caused salting-out, whereas nitrates caused salting-in of HMF to the aqueous phase. Unexpectedly, LiCl caused salting-out at low LiCl concentrations and salting-in at LiCl concentrations higher than 3 mol/kgH2O. The model electrolyte perturbed-chain SAFT (ePC-SAFT) was used to predict the salt influence on the LLE in the quaternary systems water/MIBK/HMF/salt in good agreement with the experimental data. On the basis of ePC-SAFT, it could be concluded that the different salting-out/salting-in behavior of the various salts is mainly caused by their different tendency to form ion pairs in aqueous solutions. PMID:27027570

  3. Analytical validation applied to simultaneous determination of solvents dichloromethane (DCM), methyl isobutyl ketone (MIBK), tetrahydrofuran (THF) and toluene (TOL) in urine by headspace extraction and injection on chromatographic system with a flame ionization detector

    NASA Astrophysics Data System (ADS)

    Muna, E. D. M.; Pereira, R. P.


    The determination of the volatile organic solvents dichloromethane (DCM), methyl isobutyl ketone (MIBK), tetrahydrofuran (THF) and toluene (TOL) is applied on toxicological monitoring of employees in various industrial activities. The gas chromatography technique with flame ionization detector and headspace injection system has been applied. The analytical procedure developed allows the simultaneous determination of the above-mentioned solvents and the accuracy of the method was tested following the INMETRO guidelines through the DOQ-CGRE 008 Rev.04-July/2011.

  4. Solvent extraction of N-Cyclohexyl-N-Nitrosohydroxylamine (cnha) into some organic solvents and of the Cu(II)-cnha complex into methyl isobutyl ketone.


    Rauret, G; Pineda, L; Ventura, M; Compaño, R


    The distribution equilibria of N-cyclohexyl-N-nitrosohydroxylamine (cnha) in the water-chloroform, water-hexane, water-methyl isobutyl ketone (MIBK) and water-isopentyl alcohol systems, and of the Cu(II)-cnha complex in the water-MIBK system have been studied. From the distribution data the dissociation and distribution constants of the reagent have been calculated; their values are pK(a) = 5.55 +/- 0.10; log K(DR) = 2.46 +/- 0.05 (chloroform), 1.76 +/- 0.11 (MIBK), 1.06 +/- 0.07 (hexane) and 1.48 +/- 0.06 (isopentyl alcohol). In the same way the values of the distribution and stability constants of the Cu(II) complex have been obtained; log K(DC) = 3.51; log beta(1) = 7.23 +/- 0.10 and log beta(2) = 12.00 +/- 0.08. For the determination of cnha in the aqueous phase saturated with MIBK, a spectrophotometric method based on the coloured complex formed by the reagent with Fe(III) has been established. Finally, an analytical method for Cu(II) by atomic-absorption spectrometry after its extraction with cnha into MIBK, is proposed. Its detection limit is 4.6 mug l ., its precision +/- 2.1% and its accuracy 97.5%. This method has been applied to the determination of the copper content in the surface water of the Congest River of Catalonia (Spain). PMID:18964050

  5. Treatment of biomass gasification wastewaters using liquid-liquid extraction

    SciTech Connect

    Bell, N.E.


    Pacific Northwest Laboratory (PNL) investigated liquid-liquid extraction as a treatment method for biomass gasification wastewaters (BGW). Distribution coefficients for chemical oxygen demand (COD) removal were determined for the following solvents: methylisobutyl ketone (MIBK), n-butyl acetate, n-butanol, MIBK/n-butyl acetate (50:50 vol), MIBK/n-butanol (50:50 vol), tri-butyl phosphate, tri-n-octyl phosphine oxide (TOPO)/MIBK (10:90 wt), TOPO/kerosene (10:90 wt), kerosene, and toluene. The best distribution coefficient of 1.3 was given by n-butanol. Chemical analysis of the wastewater by gas chromatography (GC) showed acetic acid and propionic acid concentrations of about 4000 mg/1. Methanol, ethanol, and acetone were identified in trace amounts. These five compounds accounted for 45% of the measured COD of 29,000 mg/1. Because of the presence of carboxylic acids, pH was expected to affect extraction of the wastewater. At low pH the acids should be in the acidic form, which increased extraction by MIBK. Extraction by n-butanol was increased at high pH, where the acids should be in the ionic form.

  6. Identification and separation of the organic compounds in coal-gasification condensate waters. [5,5 dimethyl hydantoin, dihydroxy benzenes, acetonitrile

    SciTech Connect

    Mohr, D.H. Jr.; King, C.J.


    A substantial fraction of the organic solutes in condensate waters from low-temperature coal-gasification processes are not identified by commonly employed analytical techniques, have low distriution coefficients (K/sub C/) into diisopropyl ether (DIPE) or methyl isobutyl ketone (MIBK), and are resistant to biological oxidation. These compounds represent an important wastewater-treatment problem. Analytical techniques were developed to detect these polar compounds, and the liquid-liquid phase equilibria were measured with several solvents. A high-performance liquid - chromatography (HPLC) technique was employed to analyze four condensate-water samples from a slagging fixed-bed gasifier. A novel sample-preparation technique, consisting of an azeotropic distillation with isopropanol, allowed identification of compounds in the HPLC eluant by combined gas chromatography and mass spectrometry. 5,5-dimethyl hydantoin and related compounds were identified in condensate waters for the first time, and they account for 1 to 6% of the chemical oxygen demand (COD). Dimethyl hydatoin has a K/sub D/ of 2.6 into tributyl phosphate (TBP) and much lower K/sub D/ values into six other solvents. It is also resistant to biological oxidation. Phenols (59 to 76% of the COD), dihydroxy benzenes (0.02 to 9.5% of the COD), and methanol, acetonitrile, and acetone (15% of the COD in one sample) were also detected. Extraction with MIBK removed about 90% of the COD. MIBK has much higher K/sub D/ values than DIPE for dihydroxy benzenes. Chemical reactions occurred during storage of condensate-water samples. The reaction products had low K/sub D/ values into MIBK. About 10% of the COD had a K/sub D/ of nearly zero into MIBK. These compounds were not extracted by MIBK over a wide range of pH. 73 references, 6 figures, 35 tables.

  7. The determination of aluminum, copper, iron, and lead in glycol formulations by atomic absorption spectroscopy

    NASA Technical Reports Server (NTRS)


    Initial screening tests and the results obtained in developing procedures to determine Al, Cu, Fe, and Pb in glycol formulations are described. Atomic absorption completion was selected for Cu, Fe and Pb, and after comparison with emission spectroscopy, was selected for Al also. Before completion, carbon, iron, and lead are extracted with diethyl dithio carbamate (DDC) into methyl isobutyl ketone (MIBK). Aluminum was also extracted into MIBK using 8-hydroxyquinoline as a chelating agent. As little as 0.02 mg/l carbon and 0.06 mg/l lead or iron may be determined in glycol formulations. As little as 0.3 mg/l aluminum may be determined.

  8. The direct conversion of sugars into 2,5-furandicarboxylic acid in a triphasic system.


    Yi, Guangshun; Teong, Siew Ping; Zhang, Yugen


    A one-pot conversion of sugars into 2,5-furandicarboxylic acid (FDCA) is demonstrated in a triphasic system: tetraethylammonium bromide (TEAB) or water-methyl isobutyl ketone (MIBK)-water. In this reaction, sugars are first converted into 5-hydroxymethylfurfural (HMF) in TEAB or water (Phase I). The HMF in Phase I is then extracted to MIBK (Phase II) and transferred to water (Phase III), where HMF is converted into FDCA. Phase II plays multiple roles: as a bridge for HMF extraction, transportation and purification. Overall FDCA yields of 78 % and 50 % are achieved from fructose and glucose respectively. PMID:25766123

  9. Determination of silver in soils, sediments, and rocks by organic-chelate extraction and atomic absorption spectrophotometry

    USGS Publications Warehouse

    Chao, T.T.; Ball, J.W.; Nakagawa, H.M.


    A useful method for the determination of silver in soil, sediment, and rock samples in geochemical exploration has been developed. The sample is digested with concentrated nitric acid, and the silver extracted with triisooctyl thiophosphate (TOTP) in methyl isobutyl ketone (MIBK) after dilution of the acid digest to approximately 6 M. The extraction of silver into the organic extractant is quantitative and not affected by the nitric acid concentration from 4 M to 8 M, or by different volumes of TOTP-MIBK. The extracted silver is stable and remains in the organic phase up to several days. The silver concentration is determined by atomic absorption spectrophotometry. ?? 1971.

  10. Stabilizing Agents for Calibration in the Determination of Mercury Using Solid Sampling Electrothermal Atomic Absorption Spectrometry

    PubMed Central

    Zelinková, Hana; Červenka, Rostislav; Komárek, Josef


    Tetramethylene dithiocarbamate (TMDTC), diethyldithiocarbamate (DEDTC), and thiourea were investigated as stabilizing agents for calibration purposes in the determination of mercury using solid sampling electrothermal atomic absorption spectrometry (SS-ETAAS). These agents were used for complexation of mercury in calibration solutions and its thermal stabilization in a solid sampling platform. The calibration solutions had the form of methyl isobutyl ketone (MIBK) extracts or MIBK-methanol solutions with the TMDTC and DEDTC chelates and aqueous solutions with thiourea complexes. The best results were obtained for MIBK-methanol solutions in the presence of 2.5 g L−1 TMDTC. The surface of graphite platforms for solid sampling was modified with palladium or rhenium by using electrodeposition from a drop of solutions. The Re modifier is preferable due to a higher lifetime of platform coating. A new SS-ETAAS procedure using the direct sampling of solid samples into a platform with an Re modified graphite surface and the calibration against MIBK-methanol solutions in the presence of TMDTC is proposed for the determination of mercury content in solid environmental samples, such as soil and plants. PMID:22654606

  11. Manganese dioxide causes spurious gold values in flame atomic-absorption readings from HBr-Br2 digestions

    USGS Publications Warehouse

    Campbell, W.L.


    False readings, apparently caused by the presence of high concentrations of manganese dioxide, have been observed in our current flame atomic-absorption procedure for the determination of gold. After a hydrobromic acid (HBr)-bromine (Br2) leach, simply heating the sample to boiling to remove excess Br2 prior to extraction with methyl-isobutyl-ketone (MIBK) eliminates these false readings. ?? 1981.

  12. 40 CFR Table 2 to Subpart Ggg of... - Partially Soluble HAP

    Code of Federal Regulations, 2014 CFR


    ... (mek) Ethylene oxide 1,4-Dichlorobenzene Hexachlorobenzene 2-Nitropropane Hexachlorobutadiene 4-Methyl-2-pentanone (MIBK) Hexachloroethane Acetaldehyde Methyl methacrylate Acrolein Methyl-t-butyl ether... GGG of Part 63—Partially Soluble HAP 1,1,1-Trichloroethane (methyl chloroform) Chloroform...

  13. 40 CFR Table 7 to Subpart Vvvvvv... - Partially Soluble HAP

    Code of Federal Regulations, 2014 CFR


    .... Hexachlorobutadiene 87683 39. Hexachloroethane 67721 40. Methyl methacrylate 80626 41. Methyl-t-butyl ether 1634044 42...-Trichloroethane (methyl chloroform) 71556 2. 1,1,2,2-Tetrachloroethane 79345 3. 1,1,2-Trichloroethane 79005 4. 1,1...-Dichlorobenzene 106467 11. 2-Nitropropane 79469 12. 4-Methyl-2-pentanone (MIBK) 108101 13. Acetaldehyde 75070...

  14. Stabilizing agents for calibration in the determination of mercury using solid sampling electrothermal atomic absorption spectrometry.


    Zelinková, Hana; Červenka, Rostislav; Komárek, Josef


    Tetramethylene dithiocarbamate (TMDTC), diethyldithiocarbamate (DEDTC), and thiourea were investigated as stabilizing agents for calibration purposes in the determination of mercury using solid sampling electrothermal atomic absorption spectrometry (SS-ETAAS). These agents were used for complexation of mercury in calibration solutions and its thermal stabilization in a solid sampling platform. The calibration solutions had the form of methyl isobutyl ketone (MIBK) extracts or MIBK-methanol solutions with the TMDTC and DEDTC chelates and aqueous solutions with thiourea complexes. The best results were obtained for MIBK-methanol solutions in the presence of 2.5 g L(-1) TMDTC. The surface of graphite platforms for solid sampling was modified with palladium or rhenium by using electrodeposition from a drop of solutions. The Re modifier is preferable due to a higher lifetime of platform coating. A new SS-ETAAS procedure using the direct sampling of solid samples into a platform with an Re modified graphite surface and the calibration against MIBK-methanol solutions in the presence of TMDTC is proposed for the determination of mercury content in solid environmental samples, such as soil and plants. PMID:22654606

  15. Studies on the interaction between ethanol and two industrial solvents (methyl isobutyl ketone) in mice

    SciTech Connect

    Granvil, C.P.; Sharkawi, M.; Plaa, G.L. )


    Methyl n-butyl ketone (MnBK) and methyl isobutyl ketone (MiBK) prolong the duration of ethanol-induced loss of righting reflex (EILRR) in mice. MnBK was almost twice as potent in this regard. To explain this difference, the metabolism of both ketones was studied in male CD-1 mice using GC. MiBK was converted to 4-methyl-2-pentanol (4MPOL) and 4-hydroxy methyl isobutyl ketone (HMP). MnBK metabolites were 2-hexanol (2HOL) and 2,5-hexanedione (2,5HD). The effects of both ketones and metabolites on EILRR and ethanol (E) elimination were studied in mice. The ketones and their metabolites were dissolved in corn oil and injected intraperitoneally 30 min before E 4g/kg for EILRR and 2g/kg for E elimination. In the following doses: MnBK, 5; MiBK, 5; 2HOL, 2.5; 4MPOL, 2.5; and HMP 2.5, significantly prolonged EILRR. Concentrations of E in blood and brain upon return of the righting reflex were similar in solvent-treated and control animals. The mean elimination rate of E was slower in groups given MnBK or 2HOL than in control animals. No change in E elimination was observed with MiBK, HMP, 4MPOL, or 2, 5HD.

  16. Removal of iron interferences by solvent extraction for geochemical analysis by atomic-absorption spectrophotometry

    USGS Publications Warehouse

    Zhou, L.; Chao, T.T.; Sanzolone, R.F.


    Iron is a common interferent in the determination of many elements in geochemical samples. Two approaches for its removal have been taken. The first involves removal of iron by extraction with methyl isobutyl ketone (MIBK) from hydrochloric acid medium, leaving the analytes in the aqueous phase. The second consists of reduction of iron(III) to iron(II) by ascorbic acid to minimize its extraction into MIBK, so that the analytes may be isolated by extraction. Elements of interest can then be determined using the aqueous solution or the organic extract, as appropriate. Operating factors such as the concentration of hydrochloric acid, amounts of iron present, number of extractions, the presence or absence of a salting-out agent, and the optimum ratio of ascorbic acid to iron have been determined. These factors have general applications in geochemical analysis by atomic-absorption spectrophotometry. ?? 1985.

  17. Flame and flameless atomic-absorption determination of tellurium in geological materials

    USGS Publications Warehouse

    Chao, T.T.; Sanzolone, R.F.; Hubert, A.E.


    The sample is digested with a solution of hydrobromic acid and bromine and the excess of bromine is expelled. After dilution of the solution to approximately 3 M in hydrobromic acid, ascorbic acid is added to reduce iron(III) before extraction of tellurium into methyl isobutyl ketone (MIBK). An oxidizing air-acetylene flame is used to determine tellurium in the 0.1-20 ppm range. For samples containing 4-200 ppb of tellurium, a carbon-rod atomizer is used after the MIBK extract has been washed with 0.5 M hydrobromic acid to remove the residual iron. The flame procedure is useful for rapid preliminary monitoring, and the flameless procedure can determine tellurium at very low concentrations. ?? 1978.

  18. SML resist processing for high-aspect-ratio and high-sensitivity electron beam lithography

    NASA Astrophysics Data System (ADS)

    Mohammad, Mohammad Ali; Dew, Steven K.; Stepanova, Maria


    A detailed process characterization of SML electron beam resist for high-aspect-ratio nanopatterning at high sensitivity is presented. SML contrast curves were generated for methyl isobutyl ketone (MIBK), MIBK/isopropyl alcohol (IPA) (1:3), IPA/water (7:3), n-amyl acetate, xylene, and xylene/methanol (3:1) developers. Using IPA/water developer, the sensitivity of SML was improved considerably and found to be comparable to benchmark polymethylmethacrylate (PMMA) resist without affecting the aspect ratio performance. Employing 30-keV exposures and ultrasonic IPA/water development, an aspect ratio of 9:1 in 50-nm half-pitch dense grating patterns was achieved representing a greater than two times improvement over PMMA. Through demonstration of 25-nm lift-off features, the pattern transfer performance of SML is also addressed.

  19. Optimization of clean fractionation processing as a pre-treatment technology for prairie cordgrass.


    Brudecki, Grzegorz; Cybulska, Iwona; Rosentrater, Kurt; Julson, James


    The main objective of this study was to fractionate prairie cordgrass (PCG) obtaining the highest cellulose digestibility. Following clean fractionation (CF) processing, the PCG lignocellulosic biomass was fractionated into three main building blocks: cellulose, hemicellulose and lignin. Effects of processing factors such as time, temperature, catalyst concentration and organic solvent mixture composition were evaluated. Organic solvent-aqueous mixture contained methyl isobutyl ketone (MIBK), ethanol and water in different proportions. Sulfuric acid was used as a catalyst. In order to evaluate the degree of pre-treatment, enzymatic saccharification was employed on the cellulose fraction obtained from the CF process. Response surface methodology was used for process optimization and statistical analysis. Optimal conditions (39 min, 154°C, 0.69% catalyst and 9% MIBK) resulted in 84% glucose yield and 87% acid insoluble lignin (AIL). PMID:22244901

  20. Toxicity and carcinogenicity of methyl isobutyl ketone in F344N rats and B6C3F1 mice following 2-year inhalation exposure.


    Stout, Matthew D; Herbert, Ronald A; Kissling, Grace E; Suarez, Fernando; Roycroft, Joseph H; Chhabra, Rajendra S; Bucher, John R


    Methyl isobutyl ketone (MIBK) is primarily used as a denaturant for rubbing alcohol, as a solvent and in the manufacture of methyl amyl alcohol. Inhalation of vapors is the most likely route of exposure in the work place. In order to evaluate the potential of MIBK to induce toxic and carcinogenic effects following chronic exposure, groups of 50 male and 50 female F344/N rats and B6C3F1 mice were exposed to MIBK at concentrations of 0, 450, 900, or 1800ppm by inhalation, 6h/day, 5 days per week for 2 years. Survival was decreased in male rats at 1800ppm. Body weight gains were decreased in male rats at 900 and 1800ppm and in female mice at 1800ppm. The primary targets of MIBK toxicity and carcinogenicity were the kidney in rats and the liver in mice. In male rats, there was increased mineralization of the renal papilla at all exposure concentrations. The incidence of chronic progressive nephropathy (CPN) was increased at 1800ppm and the severity was increased in all exposed groups. There were also increases in renal tubule hyperplasia at all exposure concentrations, and in adenoma and adenoma or carcinoma (combined) at 1800ppm; these lesions are thought to represent a continuum in the progression of proliferative lesions in renal tubule epithelium. These increases may have resulted from the increased severity of CPN, either through alpha2micro-globulin-dependent or -independent mechanisms. An increase in mononuclear cell leukemia at 1800ppm was an uncertain finding. Adrenal medulla hyperplasia was increased at 1800ppm, and there was a positive trend for increases in benign or malignant pheochromocytomas (combined). In female rats, there were increases in the incidence of CPN in all exposure concentrations and in the severity at 1800ppm, indicating that CPN was increased by mechanisms in addition to those related to alpha2micro-globulin. There were renal mesenchymal tumors, which have not been observed in historical control animals, in two female rats at 1800ppm. The

  1. Methyl isobutyl ketone exposure-related increases in specific measures of α2u-globulin (α2u) nephropathy in male rats along with in vitro evidence of reversible protein binding.


    Borghoff, S J; Poet, T S; Green, S; Davis, J; Hughes, B; Mensing, T; Sarang, S S; Lynch, A M; Hard, G C


    Chronic exposure to methyl isobutyl ketone (MIBK) resulted in an increase in the incidence of renal tubule adenomas and occurrence of renal tubule carcinomas in male, but not female Fischer 344 rats. Since a number of chemicals have been shown to cause male rat renal tumors through the α2u nephropathy-mediated mode of action, the objective of this study is to evaluate the ability of MIBK to induce measures of α2u nephropathy including renal cell proliferation in male and female F344 rats following exposure to the same inhalation concentrations used in the National Toxicology Program (NTP) cancer bioassay (0, 450, 900, or 1800ppm). Rats were exposed 6h/day for 1 or 4 weeks and kidneys excised approximately 18h post exposure to evaluate hyaline droplet accumulation (HDA), α2u staining of hyaline droplets, renal cell proliferation, and to quantitate renal α2u concentration. There was an exposure-related increase in all measures of α2u nephropathy in male, but not female rat kidneys. The hyaline droplets present in male rat kidney stained positively for α2u. The changes in HDA and α2u concentration were comparable to d-limonene, an acknowledged inducer of α2u nephropathy. In a separate in vitro study using a two-compartment vial equilibration model to assess the interaction between MIBK and α2u, the dissociation constant (Kd) was estimated to be 1.27×10(-5)M. This Kd is within the range of other chemicals known to bind to α2u and cause nephropathy. Together, the exposure-related increase in measures of α2u nephropathy, sustained increase in renal cell proliferation along with an indication of reversible binding of MIBK to α2u, support the inclusion of MIBK in the category of chemicals exerting renal effects through a protein droplet α2u nephropathy-mediated mode of action (MoA). PMID:25797582

  2. Development Characteristics of PMMA in alternative alcohol:water mixtures

    NASA Astrophysics Data System (ADS)

    Ocola, Leonidas E.


    The most widely used resist in electron beam lithography is polymethylmethacrylate (PMMA). The standard developers used are solution mixtures of isopropanol (IPA) and methyl isobutyl ketone (MIBK) in a ratio of 3:1 and mixtures of IPA and water (H2O) in a ratio of 7:3. The Globally Harmonized System (GHS) classification entry for IPA includes: Specific target organ toxicity - single exposure (Category 3). MIBK is much more hazardous than IPA. The only GHS classification entry for Ethanol is: Flammable liquids (Category 2), i.e. more environmentally safe. Using Ethanol/H2O as a developer will therefore enable lower hazardous waste disposal costs to cleanrooms. We find Ethanol/H2O at 85% volume (2:1 molar) exhibits excellent lithography results as good as with IPA/H2O, and better contrast and sensitivity than IPA/H2O and MIBK/IPA developers. Lithographic data shows trends similar to published cosolvency data, but differ too much to be explained by it. In addition, unusual development at 50% volume concentrations for both IPA and Ethanol in H2O show dramatic pothole formation instead of uniform thickness loss found in standard contrast curve exposures. We believe local pockets of concentrated alcohol water molar mixtures are responsible for such behavior. This work was supported by the Department of Energy under Contract No. DE-AC02-06CH11357. Use of the Center for Nanoscale Materials was supported by the U. S. Department of Energy, Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357.

  3. Modification and optimization of a 50 MHz inductively coupled argon plasma with special reference to analyses using organic solvents

    NASA Astrophysics Data System (ADS)

    Boumans, P. W. J. M.; Lux-Steiner, M. Ch.

    The torch and nebulizer of an existing argon ICP system were modified and the system was (re-) optimized for aqueous and organic liquids. The paper describes the design considerations and construction of (1) a new, streamlined torch including a torch base used in this study, where a demountable rather than a prealigned version of the torch was preferred; (2) a cross-flow pneumatic nebulizer with adjustable teflon capillaries including a spray chamber with flow spoiler, concentric aerosol pick-up tube, and "U" tube with unequal legs to smooth the flow of wasted liquid to the drain. The (re)-optimization of the ICP system for analysis of aqueous solutions with inorganic matter or with both inorganic and organic matter is discussed in the light of earlier work in this laboratory regarding the selection of "compromise conditions" and the choice of representative spectral lines and measurement criteria for establishing such compromise conditions. In this context the authors consider the concepts of norm temperature and "hard" and "soft" lines, as well as recent results of measurements of spatial distributions in ICPs. The authors further describe experiments aimed at the optimization of the operating conditions of an "organic ICP" using methyl isobutyl ketone (MIBK) as organic solvent. Trends of net line and background signals and signal-to-background ratios with the ICP parameters (power; outer, intermediate and carrier gas flow; observation height; liquid feed rate) are reported, and a rational choice of compromise conditions for the ICP is argued. Performance characteristics of the modified ICP system, such as detection limits, precision and interference level, achieved under compromise conditions, have been communicated in a previous report [ Spectrochim. Acta36B, 1031 (1981)] to demonstrate the capabilities of the system for analysis of aqueous solutions. Detection limits in MIBK and oil diluted in MIBK are reported in the present work as an illustration of the

  4. Effect of standard phase differences between gas and liquid and the resulting experimental bias in the analysis of gaseous volatile organic compounds.


    Kim, Yong-Hyun; Kim, Ki-Hyun


    Liquid- or gas-phase standards can be used for the analysis of VOCs in air. Once the accuracy is secured in the standard preparation stage, the use of gas-phase standard should be more reliable with the least matrix effect. However, it is not difficult to find that the liquid-phase standard is used more preferably in many laboratories for several reasons (e.g., low expense, easy handling, etc.). As such, one needs to accurately evaluate any possible bias stemming from the use of different standard phases. To this end, standards for 8 VOCs consisting of 4 aromatic compounds (benzene (B), toluene (T), styrene (S) and p-xylene (p-X)) and 4 others (methyl ethyl ketone (MEK), methyl isobutyl ketone (MIBK), butyl acetate (BuAc), and isobutyl alcohol (i-BuAl)) were prepared in both liquid and gas phases. Each standard was analyzed by the initial collection on the adsorption tube and by the combined application of thermal-desorption-gas chromatography-mass spectrometry (TD/GC/MS). The results indicated that experimental bias between the two phases, if expressed in terms of percent difference (PD), was very low in many target VOCs (B (1.09%), T (2.41%), p-X (3.64%), MEK (6.76%), and MIBK (0.17%)), while it was not in some targets (e.g., >10%: e.g., S, i-BuAl, and BuAc). In an ancillary experiment, biases were evaluated further by (1) calibrating gaseous samples against liquid phase standard and via (2) comparison between two different types of gas phase standards. In conclusion, treatment of different standards (e.g., between the same or different phases) will inevitably induce biases in most VOCs, although certain volatiles (e.g., benzene, MIBK, etc.) are virtually unaffected by such variables in a practical sense. PMID:22244142

  5. Simple analysis of total mercury and methylmercury in seafood using heating vaporization atomic absorption spectrometry.


    Yoshimoto, Keisuke; Anh, Hoang Thi Van; Yamamoto, Atsushi; Koriyama, Chihaya; Ishibashi, Yasuhiro; Tabata, Masaaki; Nakano, Atsuhiro; Yamamoto, Megumi


    This study aimed to develop a simpler method for determining total mercury (T-Hg) and methylmercury (MeHg) in biological samples by using methyl isobutyl ketone (MIBK) in the degreasing step. The fat in the samples was extracted by MIBK to the upper phase. T-Hg transferred into the water phase. This was followed by the extraction of MeHg from the water phase using HBr, CuCl2 and toluene. The MeHg fraction was reverse-extracted into L-cysteine-sodium acetate solution from toluene. The concentrations of T-Hg and MeHg were determined by heating vaporization atomic absorption spectrometry. Certified reference materials for T-Hg and MeHg in hair and fish were accurately measured using this method. This method was then applied to determine T-Hg and MeHg concentrations in the muscle, liver and gonads of seafood for the risk assessment of MeHg exposure. The mean T-Hg and MeHg concentrations in squid eggs were 0.023 and 0.022 µg/g, and in squid nidamental glands 0.052 and 0.049 µg/g, respectively. The MeHg/T-Hg ratios in the eggs and nidamental glands of squid were 94.4% and 96.5%, respectively. The mean T-Hg and MeHg concentrations in the gonads of sea urchins were 0.043 and 0.001 µg/g, respectively, with a MeHg/T-Hg ratio of 3.5%. We developed an efficient analytical method for T-Hg and MeHg using MIBK in the degreasing step. The new information on MeHg concentration and MeHg/T-Hg ratios in the egg or nidamental glands of squid and gonads of sea urchin will also be useful for risk assessment of mercury in seafood. PMID:27432235

  6. Continuous exposure of animals to methylisobutylketone

    NASA Technical Reports Server (NTRS)

    Vernot, E. H.; Macewen, J. D.; Harris, E. S.


    Continuous exposure of dogs, monkeys, mice, and rats to MIBK for two weeks and all animals except mice for 90 days resulted in measurable adverse effects only in the case of rats. Rat kidney weights and kidney to body weight ratios were significantly elevated after exposure to 410 mg/cu m for two weeks, and kidney and liver organ weights and organ to body weight ratios were elevated after exposure to 820 mg/cu m for two weeks and to 410 mg/cu m for 90 days.

  7. Purification of biomass-derived 5-hydroxymethylfurfural and its catalytic conversion to 2,5-furandicarboxylic Acid.


    Yi, Guangshun; Teong, Siew Ping; Li, Xiukai; Zhang, Yugen


    A simple and effective water extraction method is presented for the purification 5-hydroxylmethylfurfural (HMF) obtained from a biomass dehydration system. Up to 99% of the HMF can be recovered and the HMF in aqueous solution is directly converted to 2,5-furandicarboxylic acid (FDCA) as the sole product. This purification technique allows an integrated process to produce FDCA from fructose via HMF prepared in an isopropanol monophasic system, with an overall FDCA yield of 83% obtained. From Jerusalem raw artichoke biomass to FDCA via HMF prepared in a water/MIBK (methyl isobutyl ketone) biphasic system, an overall FDCA yield of 55% is obtained. PMID:24889713

  8. Determination of traces of silver in waters by anion exchange and atomic absorption spectrophotometry

    USGS Publications Warehouse

    Chao, T.T.; Fishman, M. J.; Ball, J.W.


    A method has been developed for the accurate determination of 0.1-1 ??g of silver per liter of water. The method permits stabilization of silver in water without loss to container walls. Optimum conditions have been established for the complete recovery of silver from water with an anion-exchange column, for quantitative elution of silver from the resin, and for measurement of silver by atomic absorption spectrophotometry after chelation with ammonium pyrrolidine dithiocarbamate and extraction of the chelate with MIBK. Silver in the 1-10 ??g 1 range can be determined by extraction without pre-concentration on an ion-exchange resin. ?? 1969.

  9. Determination of total tin in silicate rocks by graphite furnace atomic absorption spectrometry

    USGS Publications Warehouse

    Elsheimer, H.N.; Fries, T.L.


    A method is described for the determination of total tin in silicate rocks utilizing a graphite furnace atomic absorption spectrometer with a stabilized-temperature platform furnace and Zeeman-effect background correction. The sample is decomposed by lithium metaborate fusion (3 + 1) in graphite crucibles with the melt being dissolved in 7.5% hydrochloric acid. Tin extractions (4 + 1 or 8 + 1) are executed on portions of the acid solutions using a 4% solution of tricotylphosphine oxide in methyl isobutyl ketone (MIBK). Ascorbic acid is added as a reducing agent prior to extraction. A solution of diammonium hydrogenphosphate and magnesium nitrate is used as a matrix modifier in the graphite furnace determination. The limit of detection is > 10 pg, equivalent to > 1 ??g l-1 of tin in the MIBK solution or 0.2-0.3 ??g g-61 in the rock. The concentration range is linear between 2.5 and 500 ??g l-1 tin in solution. The precision, measured as relative standard deviation, is < 20% at the 2.5 ??g l-1 level and < 7% at the 10-30 ??g l-1 level of tin. Excellent agreement with recommended literature values was found when the method was applied to the international silicate rock standards BCR-1, PCC-1, GSP-1, AGV-1, STM-1, JGb-1 and Mica-Fe. Application was made to the determination of tin in geological core samples with total tin concentrations of the order of 1 ??g g-1 or less.

  10. Solvent sublation and spectrometric determination of iron(II) and total iron using 3-(2-pyridyl)-5,6-bis(4-phenylsulfonic acid)-1,2,4-triazine and tetrabutylammonium bromide.


    Akl, Magda Ali; Mori, Yoshihito; Sawada, Kiyoshi


    Solvent sublation has been studied for the separation and determination of trace iron(II) in various kinds of water samples. A strongly magenta-colored anionic [Fe(FZ)3](4-) complex was formed at pH 5.0 upon adding 3-(2-pyridyl)-5,6-bis(4-phenylsulfonic acid)-1,2,4-triazine (ferrozine, FZ) to the sample solution. Tetrabutylammonium bromide (TBAB) was added in the solution to form the (TBA)4[Fe(FZ)3)] ion pair, and an oleic acid (HOL) surfactant was added. Then, the (TBA)4[Fe(FZ)3] ion pairs were floated by vigorous shaking in the flotation cell and extracted into methyl isobutyl ketone (MIBK) on the surface of the aqueous solution. The iron collected in the MIBK layer was measured directly by spectrophotometry and/or flame atomic-absorption spectrophotometry. Different experimental variables that may affect the sublation efficiency were thoroughly investigated. The molar absorptivity of the (TBA)4[Fe(FZ)3] ion pair was 2.8 x 10(4) l mol(-1) cm(-1) in the aqueous layer. Beer's law held up to 1.0 mg L(-1) Fe(II) in the aqueous as well as in the organic layers. The adopted solvent sublation method was successfully applied for the determination of Fe(II) in natural water samples with a preconcentration factor of 200. The application was extended to determine iron in pharmaceutical samples. PMID:16966804

  11. Development of a test method for carbonyl compounds from stationary source emissions

    SciTech Connect

    Zhihua Fan; Peterson, M.R.; Jayanty, R.K.M.


    Carbonyl compounds have received increasing attention because of their important role in ground-level ozone formation. The common method used for the measurement of aldehydes and ketones is 2,4-dinitrophenylhydrazine (DNPH) derivatization followed by high performance liquid chromatography and ultra violet (HPLC-UV) analysis. One of the problems associated with this method is the low recovery for certain compounds such as acrolein. This paper presents a study in the development of a test method for the collection and measurement of carbonyl compounds from stationary source emissions. This method involves collection of carbonyl compounds in impingers, conversion of carbonyl compounds to a stable derivative with O-2,3,4,5,6-pentafluorobenzyl hydroxylamine hydrochloride (PFBHA), and separation and measurement by electron capture gas chromatography (GC-ECD). Eight compounds were selected for the evaluation of this method: formaldehyde, acetaldehyde, acrolein, acetone, butanal, methyl ethyl ketone (MEK), methyl isobutyl ketone (MIBK), and hexanal.

  12. Evaluation of performance impairment by spacecraft contaminants

    NASA Technical Reports Server (NTRS)

    Geller, I.; Hartman, R. J., Jr.; Mendez, V. M.


    The environmental contaminants (isolated as off-gases in Skylab and Apollo missions) were evaluated. Specifically, six contaminants were evaluated for their effects on the behavior of juvenile baboons. The concentrations of contaminants were determined through preliminary range-finding studies with laboratory rats. The contaminants evaluated were acetone, methyl ethyl ketone (MEK), methyl isobutyl ketone (MIBK), trichloroethylene (TCE), heptane and Freon 21. When the studies of the individual gases were completed, the baboons were also exposed to a mixture of MEK and TCE. The data obtained revealed alterations in the behavior of baboons exposed to relatively low levels of the contaminants. These findings were presented at the First International Symposium on Voluntary Inhalation of Industrial Solvents in Mexico City, June 21-24, 1976. A preprint of the proceedings is included.

  13. A preliminary report on the derivatization-gas chromatographic determination of nalidixic acid and 3,7-dicarboxynalidixic acid in urine.


    Wu, S M; Chen, S H; Wu, H L


    A preliminary study on the gas chromatographic analysis of urine spiked with nalidixic acid and 3,7-dicarboxynalidixic acid is described. The method is based on the transfer of an ion-pair of NA or CNA with tetradecyldimethylbenzylammonium chloride (benzalkonium chloride) from alkaline aqueous solution into methyl isobutyl ketone (MIBK), the organic phase, where these salts are derivatized with pentafluorobenzyl bromide. The derivatives formed by this process are chromatographed on an analytical column packed with 1.5% OV-101 and detected with a flame-ionization detector. Several parameters affecting the transfer and/or derivatization of NA or CNA were investigated. These parameters include the phase transfer catalyst employed, the organic solvent used, the concentration of the acid and base added, the amount of derivatizing agent required, and reaction time and temperature. PMID:2634117

  14. Health-hazard evaluation report HETA 85-256-1716, AMF Head Division, Boulder, Colorado

    SciTech Connect

    Pryor, P.


    A request was made by a representative of AMF Head Division of Boulder, Colorado, for an evaluation to be made of possible employee exposure to methylene-bisphenyl-isocyanate (BDI), methylene-chloride, 1,1,1-trichloroethane, naphtha, sodium-hydroxide, methyl-ethyl-ketone (MEK), and methyl-isobutyl-ketone (MIBK). The author concluded that noise exposure was excessive for employees working in racket stripping, refill, and fill/sand refinishing areas. No dangerous exposure levels were found for the chemicals under study with the exception of methylene chloride, which may be a health hazard for employees directly involved with its use due to its carcinogenicity. It is recommended that employees exposed to 1,1,1-trichloroethane and sodium hydroxide wear proper clothing to prevent direct contact or splashing onto the skin.

  15. Indirect determination of trace phenol in water by atomic-absorption spectrophotometry.


    Bo-Xing, X; Tong-Ming, X; Ming-Neng, S; Yu-Zhi, F


    An indirect method for determination of trace phenol in water by atomic-absorption spectrophotometry (AAS) is described. The phenol is brominated in acidic solution with KBrO(3)-KBr solution at room temperature. The excess of bromine is reacted with KI and the I(2) produced is extracted into cyclohexane and then reduced back to I(-) with ascorbic acid. The I(-) is then complexed with Cd(2+) in sulphuric acid medium and the complex extracted into MIBK. The extract is analysed by flame AAS for Cd (and hence indirectly for phenol). The linear concentration range for determination of phenol is 6 x 10(-7)-0.9 x 10(-5)M in aqueous solution. Several foreign ions and organic substances do not interfere. PMID:18963829

  16. Determination of silver, bismuth, cadmium, copper, lead, and zinc in geologic materials by atomic absorption spectrometry with tricaprylylmethylammonium chloride

    USGS Publications Warehouse

    Viets, J.G.


    Interferences commonly encountered in the determination of silver, bismuth, cadmium, copper, lead, and zinc at crustal abundance levels are effectively eliminated using a rapid, sensitive, organic extraction technique. A potassium chlorate-hydrochloric acid digestion solubilizes the metals not tightly bound in the silicate lattice of rocks, soils, and stream sediments. The six metals are selectively extracted into a 10% Aliquat 336-MIBK organic phase in the presence of ascorbic acid and potassium iodide. Metals in the organic extract are determined by flame atomic absorption spectrometry to the 0.02-ppm level for silver, cadmium, copper, and zinc and to the 0.2-ppm level for bismuth and lead with a maximum relative standard deviation of 18.8% for known reference samples. An additional hydrofluoric acid digestion may be used to determine metals substituted in the silicate lattice.

  17. Determination of gold, indium, tellurium and thallium in the same sample digest of geological materials by atomic-absorption spectroscopy and two-step solvent extraction

    USGS Publications Warehouse

    Hubert, A.E.; Chao, T.T.


    A rock, soil, or stream-sediment sample is decomposed with hydrofluoric acid, aqua regia, and hydrobromic acid-bromine solution. Gold, thallium, indium and tellurium are separated and concentrated from the sample digest by a two-step MIBK extraction at two concentrations of hydrobromic add. Gold and thallium are first extracted from 0.1M hydrobromic acid medium, then indium and tellurium are extracted from 3M hydrobromic acid in the presence of ascorbic acid to eliminate iron interference. The elements are then determined by flame atomic-absorption spectrophotometry. The two-step solvent extraction can also be used in conjunction with electrothermal atomic-absorption methods to lower the detection limits for all four metals in geological materials. ?? 1985.

  18. Determination of trace amounts of tin in geological materials by atomic absorption spectrometry

    USGS Publications Warehouse

    Welsch, E.P.; Chao, T.T.


    An atomic absorption method is described for the determination of traces of tin in rocks, soils, and stream sediments. A dried mixture of the sample and ammonium iodide is heated to volatilize tin tetraiodide -which is then dissolved in 5 % hydrochloric acid, extracted into TOPO-MIBK, and aspirated into a nitrous oxide-acetylene flame. The limit of determination is 2 p.p.m. tin and the relative standard deviation ranges from 2 to 14 %. Up to 20 % iron and 1000 p.p.m. Cu, Pb, Zn, Mn, Hg, Mo, V, or W in the sample do not interfere. As many as 50 samples can be easily analyzed per man-day. ?? 1976.

  19. The determination of vanadium in brines by atomic absorption spectroscopy

    USGS Publications Warehouse

    Crump-Wiesner, Hans J.; Feltz, H.R.; Purdy, W.C.


    A standard addition method is described for the determination of vanadium in brines by atomic absorption spectroscopy with a nitrous oxide-acetylene flame. Sample pH is adjusted to 1.0 with concentrated hydrochloric acid and the vanadium is directly extracted with 5% cupferron in methyl isobutyl ketone (MIBK). The ketone layer is then aspirated into the flame and the recorded absorption values are plotted as a function of the concentration of the added metal. As little as 2.5 ??g l-1 of vanadium can be detected under the conditions of the procedure. Tungsten and tin interfere when present in excess of 5 and 10 ??g ml-1, respectively. The concentrations of the two interfering ions normally found in brines are well below interference levels. ?? 1971.

  20. Selective and recyclable depolymerization of cellulose to levulinic acid catalyzed by acidic ionic liquid.


    Ren, Huifang; Girisuta, Buana; Zhou, Yonggui; Liu, Li


    Cellulose depolymerization to levulinic acid (LA) was catalyzed by acidic ionic liquids (ILs) selectively and recyclably under hydrothermal conditions. The effects of reaction temperature, time, water amount and cellulose intake were investigated. Dilution effect becomes more pronounced at lower cellulose intake, dramatically improving the yield of LA to 86.1%. A kinetic model has been developed based on experimental data, whereby a good fit was obtained and kinetic parameters were derived. The relationships between IL structure, polymeric structure and depolymerization efficiency were established, shedding light on the in-depth catalytic mechanism of IL, inclusive of acidity and hydrogen bonding ability. The LA product can be readily separated through extraction by methyl isobutyl ketone (MIBK) and IL can be reused over five cycles without loss of activity. This environmentally friendly methodology can be applied to selective production of LA from versatile biomass feedstocks, including cellulose and derivatives, glucose, fructose and HMF. PMID:25498672

  1. The determination of specific forms of aluminum in natural water

    USGS Publications Warehouse

    Barnes, R.B.


    A procedure for analysis and pretreatment of natural-water samples to determine very low concentrations of Al is described which distinguishes the rapidly reacting equilibrium species from the metastable or slowly reacting macro ions and colloidal suspended material. Aluminum is complexed with 8-hydroxyquinoline (oxine), pH is adjusted to 8.3 to minimize interferences, and the aluminum oxinate is extracted with methyl isobutyl ketone (MIBK) prior to analysis by atomic absorption. To determine equilibrium species only, the contact time between sample and 8-hydroxyquinoline is minimized. The Al may be extracted at the sample site with a minimum of equipment and the MIBK extract stored for several weeks prior to atomic absorption analysis. Data obtained from analyses of 39 natural groundwater samples indicate that filtration through a 0.1-??m pore size filter is not an adequate means of removing all insoluble and metastable Al species present, and extraction of Al immediately after collection is necessary if only dissolved and readily reactive species are to be determined. An average of 63% of the Al present in natural waters that had been filtered through 0.1-??m pore size filters was in the form of monomeric ions. The total Al concentration, which includes all forms that passed through a 0.1-??m pore size filter, ranged 2-70 ??g/l. The concentration of Al in the form of monomeric ions ranged from below detection to 57 ??g/l. Most of the natural water samples used in this study were collected from thermal springs and oil wells. ?? 1975.

  2. Long-term measurement of volatile organic compounds in ambient air by canister-based one-week sampling method.


    Ochiai, Nobuo; Daishima, Shigeki; Cardin, Daniel B


    A canister-based 1 week sampling method using a mechanical flow controller and a 6 L fused-silica-lined canister was evaluated for the long-term measurement of 47 VOCs in ambient air at pptv (volume/volume) to ppbv levels by use of a three-stage preconcentation method followed by GC-MS analysis. The GC conditions were initially optimized for complete separations of several pptv-level VOCs (e.g. vinyl chloride, 1,3-butadiene, acrylonitrile, 1,2-dichloroethane and chloroform) in ambient air because the selected ions are easily interfered with by coexisting C4-, C5-hydrocarbons and analytes presented at ppbv levels. Thirty-four VOCs determined by the 1 week and 24 h sampling method in December 16-22 (2002) had concentrations of 6.0-15000 pptv per compound. Concentrations of 28 VOCs (including polar VOCs (e.g. methyl isobutyl ketone and butyl acetate)) obtained by the method were approximately equal to the mean values calculated from 24 h sampling (< +/- 10% deviation). Six VOCs that had low concentrations of 6.0-43 pptv showed more than +/- 10% deviation. Thirteen VOCs were not detected during the entire sampling period. The effect of relative humidity or ozone for the specific VOCs (e.g. MIBK, butyl acetate, vinyl chloride, 1,3-butadiene and styrene) was negligible. PMID:14710945

  3. Waterborne coatings for videotape

    SciTech Connect

    Cheng, S.; Fan, H.; Gogineni, N.; Jacobs, B.; Harrell, J.W.; Jefcoat, I.A.; Lane, A.M.; Nikles, D.E.


    Magnetic tape provides a low-cost, high-density information storage medium. There is a problem, however, because current manufacturing technology uses organic solvents to apply the magnetic wailing to the film. Here the authors describe a waterborne formulation that shows promise as a technology for pollution prevention. The organic solvents used in magnetic tape coating formulations include 2-butanone (methylethyl ketone [MEK]), 4-methyl-2-pentanone (methyl-iso-butyl ketone [MIBK]), tetrahydrofuran, toluene, and cyclohexanone. These solvents present an occupational hazard to the workers and emissions hazard to the environment. The authors developed a new waterborne coating formulation and prepared magnetic tape in a pilot coating trial. The tape has mechanical and magnetic properties comparable to those of the commercial VHS tape. There is a clear economic and environmental incentive to consider adopting this waterborne process for magnetic tape manufacture. This process is not commercial, and a development effort by a tape manufacturer is required to bring it to commercial reality. They have not addressed the important issue of long-term reliability of the materials package, an object of current research. However, they have made a case for a reexamination of the use of waterborne coating formulations by the magnetic tape industry.

  4. Determination of dissolved aluminum in water samples

    USGS Publications Warehouse

    Afifi, A.A.


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

  5. Complex reaction networks in high temperature hydrocarbon chemistry.


    Mutlay, İbrahim; Restrepo, Albeiro


    Complex chemical reaction mechanisms of high temperature hydrocarbon decomposition are represented as networks and their underlying graph topologies are analyzed as a dynamic system. As model reactants, 1,3-butadiene, acetylene, benzene, ethane, ethylene, methane, methyl isobutyl ketone (MIBK) and toluene are chosen in view of their importance for the global environment, energy technologies as well as their quantum chemical properties. Accurate kinetic mechanisms are computationally simulated and converted to bipartite graphs for the incremental conversion steps of the main reactant. Topological analysis of the resulting temporal networks reveals novel features unknown to classical chemical kinetics theory. The time-dependent percolation behavior of the chemical reaction networks shows infinite order phase transition and a unique correlation between the percolation thresholds and electron distribution of the reactants. These observations are expected to yield important applications in the development of a new theoretical perspective to chemical reactions and technological processes e.g. inhibition of greenhouse gases, efficient utilization of fossil fuels, and large scale carbon nanomaterial production. PMID:25720589

  6. Methods for collection and analysis of geopressured geothermal and oil field waters

    USGS Publications Warehouse

    Lico, Michael S.; Kharaka, Yousif K.; Carothers, William W.; Wright, Victoria A.


    Present methods are described for the collection, preservation, and chemical analysis of waters produced from geopressured geothermal and petroleum wells. Detailed procedures for collection include precautions and equipment necessary to ensure that the sample is representative of the water produced. Procedures for sample preservation include filtration, acidification, dilution for silica, methyl isobutyl ketone (MIBK) extraction of aluminum, addition of potassium permanganate to preserve mercury, and precipitation of carbonate species as strontium carbonate for stable carbon isotopes and total dissolved carbonate analysis. Characteristics determined at the well site are sulfide, pH, ammonia, and conductivity. Laboratory procedures are given for the analysis of lithium, sodium, potassium, rubidium, cesium, magnesium, calcium, strontium, barium, iron, manganese, zinc, lead, aluminum, .and mercury by atomic absorption and flame emission spectroscopy. Chloride is determined by silver nitrate titration and fluoride by ion-specific electrode. Bromide and iodide concentrations are determined by the hypochlorite oxidation method. Sulfate is analyzed by titration using barium chloride with thorin indicator after pretreatment with alumina. Boron and silica are determined colorimetrically by the carmine and molybdate-blue methods, respectively. Aliphatic acid anions (C2 through C5) are determined by gas chromatography after separation and concentration in a chloroform-butanol mixture.

  7. A rapid, partial leach and organic separation for the sensitive determination of Ag, Bi, Cd, Cu, Mo, Pb, Sb, and Zn in surface geologic materials by flame atomic absorption

    USGS Publications Warehouse

    Viets, J.G.; Clark, J.R.; Campbell, W.L.


    A solution of dilute hydrochloric acid, ascorbic acid, and potassium iodide has been found to dissolve weakly bound metals in soils, stream sediments, and oxidized rocks. Silver, Bi, Cd, Cu, Mo, Pb, Sb, and Zn are selectively extracted from this solution by a mixture of Aliquat 336 (tricaprylyl methyl ammonium chloride) and MIBK (methyl isobutyl ketone). Because potentially interfering major and minor elements do not extract, the organic separation allows interference-free determinations of Ag and Cd to the 0.05 ppm level, Mo, Cu, and Zn to 0.5 ppm, and Bi, Pb, and Sb to 1 ppm in the sample using flame atomic absorption spectroscopy. The analytical absorbance values of the organic solution used in the proposed method are generally enhanced more than threefold as compared to aqueous solutions, due to more efficient atomization and burning characteristics. The leaching and extraction procedures are extremely rapid; as many as 100 samples may be analyzed per day, yielding 800 determinations, and the technique is adaptable to field use. The proposed method was compared to total digestion methods for geochemical reference samples as well as soils and stream sediments from mineralized and unmineralized areas. The partial leach showed better anomaly contrasts than did total digestions. Because the proposed method is very rapid and is sensitive to pathfinder elements for several types of ore deposits, it should be useful for reconnaissance surveys for concealed deposits. ?? 1984.

  8. Atomic absorption spectrometric determination of copper, zinc, and lead in geological materials

    USGS Publications Warehouse

    Sanzolone, R.F.; Chao, T.T.


    An atomic absorption spectrometric method is described for the determination of copper, zinc, and lead in geological materials. The sample is digested with HF-HCl-H2O2; the final solution for analysis is in 10 % (v/v) HCl. Copper and zinc are determined directly by aspirating the solution into an air-acetylene flame. A separate aliquot of the solution is used for determination of lead; lead is extracted into TOPO-MIBK from the acidic solution in the presence of iodide and ascorbic acid. For a 0.50-g sample, the limits of determination are 10-2000 p.p.m. for Cu and Zn, and 5-5000 p.p.m. for Pb. As much as 40 % Fe or Ca. and 10 % Al, Mg, or Mn in the sample do not interfere. The proposed method can be applied to the determination of copper, zinc, and lead in a wide range of geological materials including iron- and manganese-rich, calcareous and carbonate samples. ?? 1976.

  9. Metal content and physicochemical parameters used as quality criteria in virgin argan oil: influence of the extraction method.


    Marfil, Rocio; Cabrera-Vique, Carmen; Giménez, Rafael; Bouzas, Paula R; Martínez, Olga; Sánchez, Jose Antonio


    Metal content was determined in 26 samples of virgin argan oil from Morocco. An ETA-AAS with previous sample dilution with MIBK technique was used. In oil obtained by traditional method, Fe ranged from 0.8 to 4.0 mg/kg, Cu from 160.4 to 695.7 microg/kg, Cr from 10.3 to 55.3 microg/kg, Mn from 18.1 to 70.8 microg/kg, and Pb from 28.5 to 450.0 microg/kg. In oil obtained by a half-industrialized method, Fe ranged from 0.8 to 1.7 mg/kg, Cu from 158.4 to 385.0 microg/kg, Cr from 10.0 to 48.1 microg/kg, Mn from 15.0 to 68.5 microg/kg, and Pb from 32.0 to 100.0 microg/kg. Acidity value, peroxide index, K270 and K232, humidity and sludge volatile, and insoluble sludges in petroleum ether were also determined. A high variability in these quality parameters and a decrease of the quality in the oils obtained by the traditional method were observed. PMID:18662006

  10. An automated flow injection system for metal determination by flame atomic absorption spectrometry involving on-line fabric disk sorptive extraction technique.


    Anthemidis, A; Kazantzi, V; Samanidou, V; Kabir, A; Furton, K G


    A novel flow injection-fabric disk sorptive extraction (FI-FDSE) system was developed for automated determination of trace metals. The platform was based on a minicolumn packed with sol-gel coated fabric media in the form of disks, incorporated into an on-line solid-phase extraction system, coupled with flame atomic absorption spectrometry (FAAS). This configuration provides minor backpressure, resulting in high loading flow rates and shorter analytical cycles. The potentials of this technique were demonstrated for trace lead and cadmium determination in environmental water samples. The applicability of different sol-gel coated FPSE media was investigated. The on-line formed complex of metal with ammonium pyrrolidine dithiocarbamate (APDC) was retained onto the fabric surface and methyl isobutyl ketone (MIBK) was used to elute the analytes prior to atomization. For 90s preconcentration time, enrichment factors of 140 and 38 and detection limits (3σ) of 1.8 and 0.4μgL(-1) were achieved for lead and cadmium determination, respectively, with a sampling frequency of 30h(-1). The accuracy of the proposed method was estimated by analyzing standard reference materials and spiked water samples. PMID:27260436

  11. Kinetics of OH-initiated oxidation of some oxygenated organic compounds in the aqueous phase under tropospheric conditions

    NASA Astrophysics Data System (ADS)

    Poulain, L.; Grubert, S.; François, S.; Monod, A.; Wortham, H.


    The interest for multiphase interactions of Volatile Organic Compounds (VOCs) in the troposphere has increased for a few years. Inside the clouds water droplets, soluble VOCs can be oxidized by free radicals thus modifying the droplet composition. This reactivity has an impact on the tropospheric oxidizing capacity as well as the aerosols' properties. In the present work, we measured aqueous phase OH-initiated oxidation rate constants of several oxygenated organic compounds relevant to the atmosphere or chosen as test compounds (ethanol, t-butanol, 1-butanol, iso-propanol, 1-propanol, acetaldehyde, propionaldehyde, butyraldehyde, valeraldehyde, phenol, ethyl ter-butyl ether (ETBE), n-propyl acetate, acetone, methyl ethyl ketone (MEK), methyl iso-butyl ketone (MIBK), ethyl formate). Experiments took place in an aqueous phase photoreactor. The rate constants were determinated using the relative kinetic method. Different OH-radical sources were tested, as well as different reference compounds in order to detect any artifact. The results have shown validation of the experimental protocol on test compounds. The overall results allowed to propose a structure reactivity method in order to predict OH-oxidation rate constant of new compounds. Finally, tropospheric life times of the studied compounds were compared inside and outside a cloud.

  12. Volatile organic compounds concentrations in residential indoor and outdoor and its personal exposure in Korea.


    Son, Busoon; Breysse, Patrick; Yang, Wonho


    To date, personal volatile organic compounds (VOCs) exposure and residential indoor and outdoor VOCs levels have not been characterized in Korea. In this study, residential indoor and outdoor VOCs concentrations were measured and compared simultaneously with the personal exposure for each of 30 participants in a medium city, Asan, and in a metropolitan city, Seoul. Factors that influence personal VOCs exposures were assessed in relation to house characteristics and time activity information. All VOC concentrations were measured using passive samplers during a 24-h period and analyzed using GC-MS. Ten target VOCs were benzene, trichloroethylene, toluene, o-xylene, p-xylene, ethylbenzene, MIBK, n-octane, styrene, and 1,2-dichlorobenzene. Residential indoor and outdoor VOCs concentrations measured in Seoul were significantly higher than those in Asan. Indoor/outdoor (I/O) ratios for all target compounds ranged from 0.94 to 1.51 and I/O ratios of Asan were a little higher than those of Seoul. Results indicate that time activity information can be used to predict personal exposures, although such predictions will result in an over estimation compared to measured exposures. Factors which influence the indoor VOCs level and its personal exposure in relation to house characteristics included house age, indoor smoking, and house type. PMID:12605940

  13. Methods for collection and analysis of geopressured geothermal and oil field waters

    SciTech Connect

    Lico, M.S.; Kharaka, Y.K.; Carothers, W.W.; Wright, V.A.


    Present methods are described for the collection, preservation, and chemical analysis of waters produced from geopressured geothermal and petroleum wells. Detailed procedures for collection include precautions and equipment necessary to ensure that the sample is representative of the water produced. Procedures for sample preservation include filtration, acidification, dilution for silica, methyl isobutyl ketone (MIBK) extraction of aluminum, addition of potassium permanganate to preserve mercury, and precipitation of carbonate species as strontium carbonate for stable carbon isotopes and total dissolved carbonate analysis. Characteristics determined at the well site are sulfide, pH, ammonia, and conductivity. Laboratory procedures are given for the analysis of lithium, sodium, potassium, rubidium, cesium, magnesium, calcium, strontium, barium, iron, manganese, zinc, lead, aluminum, and mercury by atomic absorption and flame emission spectroscopy. Chloride is determined by silver nitrate titration and fluoride by ion-specific electrode. Bromide and iodide concentrations are determined by the hypochlorite oxidation method. Sulfate is analyzed by titration using barium chloride with thorin indicator after pretreatment with alumina. Boron and silica are determined colorimetrically by the carmine and molybdate-blue methods, respectively. Aliphatic acid anions (C/sub 2/ through C/sub 5/) are determined by gas chromatography after separation and concentration in a chloroform-butanol mixture.

  14. Mechanism of transport and distribution of organic solvents in blood

    NASA Technical Reports Server (NTRS)

    Lam, C. W.; Galen, T. J.; Boyd, J. F.; Pierson, D. L.


    Little is known about the mechanism of transport and distribution of volatile organic compounds in blood. Studies were conducted on five typical organic solvents to investigate how these compounds are transported and distributed in blood. Groups of four to five rats were exposed for 2 hr to 500 ppm of n-hexane, toluene, chloroform, methyl isobutyl ketone (MIBK), or diethyl ether vapor; 94, 66, 90, 51, or 49%, respectively, of these solvents in the blood were found in the red blood cells (RBCs). Very similar results were obtained in vitro when aqueous solutions of these solvents were added to rat blood. In vitro studies were also conducted on human blood with these solvents; 66, 43, 65, 49, or 46%, respectively, of the added solvent was taken up by the RBCs. These results indicate that RBCs from humans and rats exhibited substantial differences in affinity for the three more hydrophobic solvents studied. When solutions of these solvents were added to human plasma and RBC samples, large fractions (51-96%) of the solvents were recovered from ammonium sulfate-precipitated plasma proteins and hemoglobin. Smaller fractions were recovered from plasma water and red cell water. Less than 10% of each of the added solvents in RBC samples was found in the red cell membrane ghosts. These results indicate that RBCs play an important role in the uptake and transport of these solvents. Proteins, chiefly hemoglobin, are the major carriers of these compounds in blood. It can be inferred from the results of the present study that volatile lipophilic organic solvents are probably taken up by the hydrophobic sites of blood proteins.

  15. Catalytic destruction of hazardous organics in aqueous solutions

    SciTech Connect

    Baker, E.G.; Sealock, L.J. Jr.


    Pacific Northwest Laboratory (PNL) is developing a process for destroying hazardous organics and chlorinated organics in aqueous solutions. The process is targeted at liquid waste streams that are difficult and costly to treat with conventional or developing technologies. Examples of these waste streams include contaminated groundwater and surface water and industrial wastewater. Aqueous solutions are treated with a transition metal catalyst at 300/degree/C to 460/degree/C and 2000 to 5000 psig pressure to convert the wastes to innocuous gases. During proof-of-principle tests conducted in a 1-L batch reactor, destruction of over 99/percent/ (in most cases approaching 99.9/percent/) of the organic material was achieved. Hexone (methyl is isobutyl ketone, MIBK), p-cresol, hexane, benzene, and naphthalene were used as model waste materials. The only major product with all of the organic compounds was a gas containing 50/percent/ to 75/percent/ methane, 25/percent/ to 45/percent/ carbon dioxide, and 0/percent) to 5/percent/ hydrogen. Reduced nickel was the only effective catalyst and that the optimal operating conditions for destroying nonchlorinated organics were 350/degree/C to 400/degree/C, 2000 to 4000 psig, and 30/endash/ to 60/endash/min residence time. These tests also indicated that catalyst deactivation or fouling would not be a problem at these conditions. Chlorobenzene and trichloroethylene (TEC), were also tested. Destruction of both compounds was 99/percent/ or greater, but the products were different from those obtained from hydrocarbons. With TCE, the major product was carbon dioxide; with chlorobenzene the major product identified was benzene. In the tests with the chlorinated hydrocarbons, the chlorine was converted to HC1 and the reduced nickel was converted to nickel hydroxide, which may be detrimental to long-term catalyst activity. (15 refs., 8 figs., 6 tabs).

  16. Biofiltration of a mixture of volatile organic compounds on granular activated carbon.


    Aizpuru, A; Malhautier, L; Roux, J C; Fanlo, J L


    The performance of a biofilter packed with Active Carbon (AC) was evaluated. The effluent (alcohol, ketones, esters, aromatic and chlorinated compounds) treated was a representative mixture of most common industrial emissions. To achieve a better knowledge of multicomponent adsorption mechanisms, and to underline the interest of inoculating AC, a control abiotic humidified filter had been operated in the same conditions as the biofilter. For a load of 110 g VOC m(-3) AC h(-1), after 55 days of operation, the removal efficiency was higher in the biotic than in the abiotic filter (85% vs 55%, respectively). Moreover, in the biofilter, at steady state, the elimination of all compounds was almost complete except for chlorinated compounds and p-xylene (removal efficiency of 25% and 64%, respectively). The microbial colonization of AC involved a decrease of the adsorption sites accessibility and enhanced the treatment of VOCs (volatile organic compounds) having a lower affinity for activated carbon. Moreover, while aromatic compounds and MIBK were eliminated along the overall height of the biofilter, pollutants with reduced affinity for AC, such as methanol, acetone, and halogenated compounds were only treated on the second half of the reactor. Thus, the affinity for activated carbon was an important parameter controlling the biodegradation process. Nevertheless, the use of AC as packing material in biofilters treating complex mixtures of VOCs is limited. Actually, similar removal efficiency could be reached, in the same conditions, for a biofilter packed with granular peat. Furthermore, for the biofilter packed with AC, the column height necessary to remove biodegradable compounds, with reduced affinity for the support, was important. PMID:12800142

  17. Concentration levels of metals in vegetables grown in soils irrigated with river water in Addis Ababa, Ethiopia.


    Weldegebriel, Yirgaalem; Chandravanshi, Bhagwan Singh; Wondimu, Taddese


    Samples of vegetables, water and soil were collected from four vegetable farms in Addis Ababa to evaluate the extent and trend of metal accumulation in these systems and health risk concerns to consumers. Vegetable samples were digested in HNO(3) and HClO(4), soil samples in Aqua Regia and water samples were pre-concentrated with methyl isobutyl ketone (MIBK) using the chelating agent ammonium pyrrolidine dithiocarbamate (APDC). All the samples were analyzed for Co, Cr, Cu, Mn, Ni, Zn, Cd and Pb with flame atomic absorption spectrophotometer. The concentrations of Cd (0.12-1.13 mg kg(-1)) and Pb (0.11-0.89 mg kg(-1)) in the vegetables surpassed the maximum recommended levels. The total metal concentrations in soils were (mg kg(-1)): Cr, 9.9-22.8; Co, 28.0-47.3; Cu, 25.1-51.4, Mn, 1000-1054; Ni, 16.4-55.8; Zn, 146-149; Cd, 1.4-1.8 and Pb, 22.0-50.7. The trace metals Cd, Co, Cu, Mn and Ni in most of the water samples collected from Goffa, Kera and Akaki farms also surpassed irrigation water guideline limits, which might be a case for high accumulation of metals in the soils. However, the soil pH (6.5-7.6) and high cation exchange capacity (CEC), 38.41-50.18, coupled with high clay content, 37-51%, of the soil seemed to limit metal uptake by the vegetables. The physical parameters, pH (7.43-7.89) and electrical conductivity (0.33-1.54 dS/m) of irrigation waters measured at 25°C were found within the acceptable range. PMID:22062152

  18. Lead determination at ng/mL level by flame atomic absorption spectrometry using a tantalum coated slotted quartz tube atom trap.


    Demirtaş, İlknur; Bakırdere, Sezgin; Ataman, O Yavuz


    Flame atomic absorption spectrometry (FAAS) still keeps its importance despite the relatively low sensitivity; because it is a simple and economical technique for determination of metals. In recent years, atom traps have been developed to increase the sensitivity of FAAS. Although the detection limit of FAAS is only at the level of µg/mL, with the use of atom traps it can reach to ng/mL. Slotted quartz tube (SQT) is one of the atom traps used to improve sensitivity. In atom trapping mode of SQT, analyte is trapped on-line in SQT for few minutes using ordinary sample aspiration, followed by the introduction of a small volume of organic solvent to effect the revolatilization and atomization of analyte species resulting in a transient signal. This system is economical, commercially available and easy to use. In this study, a sensitive analytical method was developed for the determination of lead with the help of SQT atom trapping flame atomization (SQT-AT-FAAS). 574 Fold sensitivity enhancement was obtained at a sample suction rate of 3.9 mL/min for 5.0 min trapping period with respect to FAAS. Organic solvent was selected as 40 µL of methyl isobutyl ketone (MIBK). To obtain a further sensitivity enhancement inner surface of SQT was coated with several transition metals. The best sensitivity enhancement, 1650 fold enhancement, was obtained by the Ta-coated SQT-AT-FAAS. In addition, chemical nature of Pb species trapped on quartz and Ta surface, and the chemical nature of Ta on quartz surface were investigated by X-ray photoelectron spectroscopy (XPS) and Raman Spectroscopy. Raman spectrometric results indicate that tantalum is coated on SQT surface in the form of Ta2O5. XPS studies revealed that the oxidation state of Pb in species trapped on both bare and Ta coated SQT surfaces is +2. For the accuracy check, the analyses of standard reference material were performed by use of SCP SCIENCE EnviroMAT Low (EU-L-2) and results for Pb were to be in good agreement with


    SciTech Connect

    Daniel J. Stepan; Edwin S. Olson; Richard E. Shockey; Bradley G. Stevens; John R. Gallagher


    This project has shown that the recovery of several valuable lactic acid products is both technically feasible and economically viable. One of the original objectives of this project was to recover lactic acid. However, the presence of a variety of indigenous bacteria in the wastewater stream and technical issues related to recovery and purification have resulted in the production of lactic acid esters. These esters could by hydrolyzed to lactic acid, but only with unacceptable product losses that would be economically prohibitive. The developed process is projected to produce approximately 200,000 lb per day of lactate esters from wastewater at a single factory at costs that compete with conventional solvents. The lactate esters are good solvents for polymers and resins and could replace acetone, methyl ethyl ketone, MIBK, and other polar solvents used in the polymer industry. Because of their low volatility and viscosity-lowering properties, they will be especially useful for inks for jet printers, alkyl resins, and high-solid paints. Owing to their efficiency in dissolving salts and flux as well as oils and sealants, lactate esters can be used in cleaning circuit boards and machine and engine parts. Unlike conventional solvents, lactate esters exhibit low toxicity, are biodegradable, and are not hazardous air pollutants. Another application for lactate esters is in the production of plasticizers. Severe health problems have been attributed to widely used phthalate ester plasticizers. The U.S. Department of Agriculture showed that replacement of these with inexpensive lactate esters is feasible, owing to their superior polymer compatibility properties. A very large market is projected for polymers prepared from lactic acid. These are called polylactides and are a type of polyester. Thermoplastics of this type have a variety of uses, including moldings, fibers, films, and packaging of both manufactured goods and food products. Polylactides form tough, orientable