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. Safety assessment of MIBK (methyl isobutyl ketone).


    Johnson, Wilbur


    MIBK (Methyl Isobutyl Ketone) is an aliphatic ketone that functions as both a denaturant and solvent in cosmetic products. Current use in cosmetic products is very limited, but MIBK is reported to be used in one nail correction pen (volume = 3 ml) at a concentration of 21%. The maximum percutaneous absorption rate in guinea pigs is 1.1 micromol/min/cm2 at 10 to 45 min. Metabolites include 4-hydroxy-4-methyl-2-pentanone (oxidation product) and 4-methyl-2-pentanol (4-MPOL) (reduction product). Values for the serum half-life and total clearance time of MIBK in animals were 66 min and 6 h, respectively. In clinical tests, most of the absorbed MIBK had been eliminated from the body 90 min post exposure. MIBK was not toxic via the oral or dermal route of exposure in acute, short-term, or subchronic animal studies, except that nephrotoxicity was observed in rats dosed with 1 g/kg in a short-term study. MIBK was an ocular and skin irritant in animal tests. Ocular irritation was noted in 12 volunteers exposed to 200 ppm MIBK for 15 min in a clinical test. A depression of the vestibulo-oculomotor reflex was seen with intravenous infusion of MIBK (in an emulsion) at 30 microM/kg/min in female rats. The no-observed-effect level in rats exposed orally to MIBK was 50 mg/kg. Both gross and microscopic evidence of lung damage were reported in acute inhalation toxicity studies in animals. Short-term and subchronic inhalation exposures (as low as 100 ppm) produced effects in the kidney and liver that were species and sex dependent. Dermal doses of 300 or 600 mg/kg for 4 months in rats produced reduced mitotic activity in hair follicles, increased thickness of horny and granular cell layers of the epidermis, a decrease in the number of reactive centers in follicles (spleen), an increase in the number of iron-containing pigments in the area of the red pulp (spleen), and a reduction in the lipid content of the cortical layer of the adrenal glands. Neuropathological changes in the most distal portions of the tibial and ulnar nerves were observed in young adult rats which inhaled 1500 ppm MIBK for up to 5 months. No adverse effects were seen in any other neurological end point by any route of exposure in other studies using rats or other animal species. Clinical tests demonstrated a threshold for MIBK-induced irritation of the lungs at 0.03 to 0.1 mg/L after 1 min of respiration. MIBK was not mutagenic in the Ames test or in a mitotic gene-conversion assay in bacteria. Mammalian mutagenicity test results were also negative in the following assays: mouse lymphoma, unscheduled DNA synthesis, micronucleus, cell transformation, and chromosome damage. MIBK did not induce any treatment-related increases in embryotoxicity or fetal malformations in pregnant Fischer 344 rats or CD-1 mice that inhaled MIBK at concentrations of 300, 1000, or 3000 ppm. There was evidence of treatment-related maternal toxicity only at the highest concentration tested. MIBK applied to the tail of rats daily at doses of 300 or 600 mg/kg for 4 months produced changes in the testes, including a reduction in the number of spermatocytes, spermatids, and spermatozoa. An ongoing carcinogenicity study of MIBK being conducted by the National Toxicology Program will be considered when the results are available. On the basis of the information that is currently available, MIBK is considered safe as used in nail polish removers and as an alcohol denaturant in cosmetic products. PMID:15162837

  3. Biofiltration for removal of methyl isobutyl ketone (MIBK): experimental studies and kinetic modelling.


    Raghuvanshi, Smita; Babu, B V


    The present study deals with the biofiltration of methyl isobutyl ketone (MIBK), which is considered to be a highly toxic volatile organic compound. It is released from the paint and petrochemical industries and is one of the major contributors to air pollution. The biofiltration study was carried out on a lab scale for two months in the presence of acclimated mixed culture. The performance of the biofilter column was evaluated for different inlet loads of MIBK at air flow rates ranging from 0.18 to 0.3 m3 h(-1). The maximum removal efficiency of 93% was obtained after 60 days of biofilter operation for an inlet MIBK concentration of 0.45 g m(-3), and a microbial concentration of 2.36 x 10(8) CFU g(-1) of packing material was obtained. This led to a study of shock loadings for 20 days, by varying the inlet MIBK load and air flow rate after every five days, to observe the behaviour of the biofilter column in removing sudden loads of MIBK. The biokinetic constants r(max) and Ks were obtained using the Michaelis-Menten kinetics and were found to be 1.046 g m(-3) and 0.115 g m(-3) h(-1),respectively, with a coefficient of determination (R2) of 0.993. The obtained experimental results were validated with the Ottengraf and Van den Oever kinetic model. The critical inlet concentration, critical inlet load and biofilm thickness were also estimated using the results obtained from the model predictions. PMID:20232676

  4. Methyl isobutyl ketone (MIBK)

    Integrated Risk Information System (IRIS)

    EPA / 635 / R - 03 / 002 TOXICOLOGICAL REVIEW OF METHYL ISOBUTYL KETONE ( CAS No . 108 - 10 - 1 ) In Support of Summary Information on the Integrated Risk Information System ( IRIS ) March 2003 U.S . Environmental Protection Agency Washington DC DISCLAIMER This document has been reviewed in accordan

  5. Methyl isobutyl ketone as a solvent for wax deoiling

    SciTech Connect

    Larikov, V.I.; Pereverzev, A.N.; Roshchin, Y.N.; Sokolova, S.P.


    The solvency of methyl isobutyl ketone (MIBK) for use in deoiling and cold-fractionation of solid paraffin waxes is investigated by a visual polytherm method in the temperature interval 0-36 C. The capability of MIBK for precipitating solid hydrocarbons from solution was found to be greater than acetone/toluene or MEK/toluene, with only MEK better in this respect than MIBK. The quantity of wax remaining in the filtrate is examined. The critical solution temperatures are investigated and it is shown that MIBK surpasses MEK. The results obtained indicate that MIBK is extremely promising for use in processes of deoiling and cold fractionation of waxes.

  6. Solvent extraction for treating phenolic wastewater

    SciTech Connect

    Medzadourian, M.L.; Durlofsky, L.J.; Thomason, T.B.


    A two-stage solvent extraction of phenolic wastewater was investigated. In the first step, phenolics are extracted with methylisobutyl ketone (MIBK). In the second step, MIBK (1 to 2 wt %), which dissolves in the wastewater is recovered by extraction with hexane. The phenolics were modeled in this study as phenol and resorcinol. For the first extraction step, the distribution coefficient K/sub D/ for resorcinol in the MIBK-water system was experimentally determined as a function of temperature and resorcinol concentration. The process was simulated on the computer with the ASPEN program, and the results were used to determine the effects of temperature and the MIBK/water ratio in the first extracter on process economics. Of the four cases studied, a water MIBK ratio of 5 and extraction temperatures of 303 K (30/sup 0/C) required the smallest capital and operating costs.

  7. Tissue concentrations of methyl isobutyl ketone, methyl n-butyl ketone and their metabolites after oral or inhalation exposure.


    Duguay, A B; Plaa, G L


    Quantitative relationships between plasma, liver and lung methyl isobutyl ketone (MiBK) and methyl n-butyl ketone (MnBK) concentrations after oral or inhalation exposure were established. Their respective metabolites (4-methyl-2-pentanol, 4-hydroxy-methyl isobutyl ketone, 2-hexanol, and 2,5-hexanedione) were also quantified. Male Sprague-Dawley rats were exposed for 3 days to MiBK or MnBK vapors (4 h/day) or treated orally for 3 days with a MiBK- or MnBK-corn oil solution. Both ketones and their respective metabolites in plasma or tissue concentrations were determined by gas chromatography. MiBK and MnBK plasma and tissue concentrations increased in a dose-related manner with the administered dose irrespective of the route of administration. Metabolite concentrations, however, were influenced by the route of administration. PMID:7863537

  8. 40 CFR Table 8 to Subpart Ffff of... - Partially Soluble Hazardous Air Pollutants

    Code of Federal Regulations, 2010 CFR


    ...-Trichlorophenol 95954 10. 1,4-Dichlorobenzene 106467 11. 2-Nitropropane 79469 12. 4-Methyl-2-pentanone (MIBK.... Bromomethane 74839 22. Butadiene 106990 23. Carbon disulfide 75150 24. Chlorobenzene 108907 25. Chloroethane.... Styrene 100425 50. Tetrachloroethylene (perchloroethylene) 127184 51. Tetrachloromethane...

  9. Metabolic fate of methyl n-butyl ketone, methyl isobutyl ketone and their metabolites in mice.


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


    The metabolic fate of methyl n-butyl ketone (MnBK) and its isomer methyl isobutyl ketone (MiBK) was studied in mice. The concentrations of both ketones and their metabolites in blood and brain were measured at different time intervals after their administration. The principal metabolites of MnBK were 2-hexanol (2-HOL) and 2,5-hexanedione (2,5-HD), while those of MiBK were 4-methyl-2-pentanol (4-MPOL) and 4-hydroxy-4 methyl-2-pentanone (HMP). The administration of 2-hexanol by itself led to the appearance of both MnBK and 2,5-hexanedione which, when administered by itself, did not lead to the appearance of either MnBK or 2-hexanol. The administration of 4-methyl-2-pentanol resulted in the appearance of MiBK and HMP. The administration of HMP did not result in the appearance of MiBK or 4-MPOL. These results indicate that the metabolic fate of MnBK and MiBK is similar to that reported in other species. PMID:8284793

  10. 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.

  11. 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.

  12. 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.

  13. 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

  14. Use of long chain alkylamines for preconcentration and determination of traces of molybdenum, tungsten and rhenium by atomic-absorption spectroscopy--III. Tungsten in geological samples.


    Kim, C H; Alexander, P W; Smythe, L E


    Tungsten is determined by atomic-absorption spectroscopy after its reduction to the W(V)-thiocyanate complex with tin metal and extraction with Alamine 336 into chloroform. Atomic absorbance is measured on a final MIBK solution after evaporation of the chloroform and redissolution of the residue in MIBK. Interference effects are shown to be negligible for diverse cations and anions, including Fe, Cu, Cr, Co, Mo, Al and Bi. Analysis of geological samples with an exceptionally wide range of W content from 2.8 ppm to 10% is achieved with relative standard deviations better than 5%. PMID:18961931

  15. 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.

  16. 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.

  17. 40 CFR Appendix B to Part 80 - Test Methods for Lead in Gasoline

    Code of Federal Regulations, 2012 CFR


    ... g) of Aliquat 336 (Aldrich Chemical Co., Milwaukee, Wisconsin) with MIBK (Burdick & Jackson Lab...): Dissolve and dilute 3.0 g iodine crystals (American Chemical Society) with toluene (Burdick & Jackson Lab... unleaded gasoline (Phillips Chemical Co., Borger, Texas) or iso-octane (Burdick & Jackson Lab,...

  18. 40 CFR Appendix B to Part 80 - Test Methods for Lead in Gasoline

    Code of Federal Regulations, 2010 CFR


    ... g) of Aliquat 336 (Aldrich Chemical Co., Milwaukee, Wisconsin) with MIBK (Burdick & Jackson Lab...): Dissolve and dilute 3.0 g iodine crystals (American Chemical Society) with toluene (Burdick & Jackson Lab... unleaded gasoline (Phillips Chemical Co., Borger, Texas) or iso-octane (Burdick & Jackson Lab,...

  19. 40 CFR Appendix B to Part 80 - Test Methods for Lead in Gasoline

    Code of Federal Regulations, 2011 CFR


    ... g) of Aliquat 336 (Aldrich Chemical Co., Milwaukee, Wisconsin) with MIBK (Burdick & Jackson Lab...): Dissolve and dilute 3.0 g iodine crystals (American Chemical Society) with toluene (Burdick & Jackson Lab... unleaded gasoline (Phillips Chemical Co., Borger, Texas) or iso-octane (Burdick & Jackson Lab,...

  20. 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.

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

    PubMed Central

    Zelinkovß, Hana; ?ervenka, Rostislav; Komßrek, 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

  2. Methyl isobutyl ketone exposure-related increases in specific measures of ?2u-globulin (?2u) 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 ?2u nephropathy-mediated mode of action, the objective of this study is to evaluate the ability of MIBK to induce measures of ?2u 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), ?2u staining of hyaline droplets, renal cell proliferation, and to quantitate renal ?2u concentration. There was an exposure-related increase in all measures of ?2u nephropathy in male, but not female rat kidneys. The hyaline droplets present in male rat kidney stained positively for ?2u. The changes in HDA and ?2u concentration were comparable to d-limonene, an acknowledged inducer of ?2u nephropathy. In a separate in vitro study using a two-compartment vial equilibration model to assess the interaction between MIBK and ?2u, the dissociation constant (Kd) was estimated to be 1.27Î10(-5)M. This Kd is within the range of other chemicals known to bind to ?2u and cause nephropathy. Together, the exposure-related increase in measures of ?2u nephropathy, sustained increase in renal cell proliferation along with an indication of reversible binding of MIBK to ?2u, support the inclusion of MIBK in the category of chemicals exerting renal effects through a protein droplet ?2u nephropathy-mediated mode of action (MoA). PMID:25797582

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. Pharmacodynamic and metabolic interactions between ethanol and two industrial solvents (methyl n-butyl ketone and methyl isobutyl ketone) and their principal metabolites in mice.


    Sharkawi, M; Granvil, C; Faci, A; Plaa, G L


    MnBK and MiBK prolong the duration of ketamine-, pentobarbital-, thiopental- and ethanol-induced loss of righting reflex (LRR) in mice. In equimolar doses, (5 mmol/kg i.p.), both isomers were equipotent with respect to the enhancement of ketamine-, pentobarbital-, and thiopental-induced LRR. However, MnBK was significantly more effective (twice as effective) than its isomer with respect to enhancing ethanol-induced LRR. An attempt to explain the difference in effectiveness between the two isomers was carried out. The effects of both ketones and their principal metabolites, (2-hexanol (2-HOL), 2,5-hexanedione (2,5-HD), 4-methyl-2-pentanol (4-MPOL) and 4-hydroxy 4-methyl-2-pentanone (HMP)) on ethanol-induced LRR and ethanol elimination were studied in mice. The ketones and their metabolites were dissolved in corn oil and injected intraperitoneally 30 min before 4 g/kg ethanol for LRR and 2 g/kg for ethanol elimination. Ethanol-induced LRR was significantly prolonged by the following dosages (mmol/kg), MnBK, 5; MiBK, 5; 2-HOL, 2.5; 4-MPOL, 2.5; and HMP, 2.5; 2,5-HD, 2.5, however exerted no effect. Concentrations of ethanol in blood or brain upon return of the righting reflex were similar in solvent-treated and control animals. The mean elimination rate of ethanol was slower in groups pretreated with MnBK or 2-HOL as compared to control animals. Ethanol elimination in animals pretreated with MiBK, HMP, 4-MPOL, or 2,5-HD was similar to that in control animals. These ketones are known to have some central depressant action on their own. This by itself could lead to prolongation of ethanol-induced LRR. However, MnBK, as well as one of its principal metabolites, (2-HOL), markedly reduced ethanol elimination. This could explain the observation that MnBK has a greater potentiating effect on ethanol-induced LRR that its isomer, MiBK, which does not affect ethanol elimination. PMID:7801321

  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. 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.

  10. Evaluation of solvent selectivity in dewaxing and deoiling

    SciTech Connect

    Al'perovich, N.V.; Leonidov, A.N.; Sokolova, S.P.


    Previous literature on the efficiency of solvents used in removing paraffin wax by decrystallization is insufficient. A method for evaluating selectivity and mixtures of solvents is offered. General solvents MEK, acetone, MIBK are tested in various raw materials, then graphed. It is found that the ratio of the slope of the curve for the temperature of equal solubility (TES) as a function of the content of the solvent (that is, the solubility curve) to the slope of the corresponding denormalization curve is constant. This ratio gives a formula, and is therefore a criterion for selectivity. The greater the ratio, the higher the selectivity. The ratio is also generalized to solvents of any composition.

  11. Severe cutaneous reaction to CS gas.


    Varma, S; Holt, P J


    Tear gas is used throughout the World for control of riots and civil disobedience. CS gas as used by the UK police force is issued as a 'spray' and is 5% CS in methylisobutylketone (MIBK), a potent irritant. Assaults on police officers in forces issued with CS spray have fallen significantly over the past 3 years, whilst having risen in areas without it. Thus, CS gas appears to be an effective deterrent. However, significant cutaneous reactions can occur as a result of exposure. We report a severe contact dermatitis to CS gas to highlight the clinical features. The nature of CS gas and potential cutaneous adverse reactions are discussed. PMID:11422166

  12. Use of long-chain alkylamines for preconcentration and determination of traces of molybdenum, tungsten and rhenium by atomic-absorption spectroscopy-II: molybdenum in soils, sediments and natural waters.


    Kim, C H; Alexander, P W; Smythe, L E


    Molybdenum is extracted as the thiocyanate complex with the quaternary long-chain aliphatic amine Aliquat 336 in chloroform, followed by evaporation of the solvent, dissolution in MIBK, and atomic-absorption spectroscopy. The method is simple, rapid and sensitive, with few interference problems for the determination of the Mo content of soils and sediments in the range 0.1-1.0 ppm with a relative standard deviation better than 5% when 1-g samples are used. Quantitative extraction from large volumes of aqueous solution has also been confirmed, allowing the determination of Mo in natural waters in the ppM range. PMID:18961838

  13. Cineangiographically determined coronary artery disease and plasma chromium level for 150 subjects

    NASA Astrophysics Data System (ADS)

    Simonoff, M.; Llabador, Y.; Simonoff, G. N.; Besse, P.; Conri, C.


    Proton induced X-ray emission (PIXE) analysis, following enrichment by APDC-MIBK extraction, is used to measure chromium concentration in blood plasma from patients submitted to selective coronary artery cineangiography. The yield of the chromium preconcentration is determined with carrier-free 51Cr. From the catheterism results the patients are classified into three populations: coronary artery disease (CAD), heart disease (HD) and normal arteries (N). The first two groups, CAD and HD, have significantly lower chromium concentrations than does the group with normally patent arteries. The present analytical method and the results obtained provide an interesting contribution to the difficult problem of chromium determination in biological media.

  14. 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.

  15. A comparative study of fungal and bacterial biofiltration treating a VOC mixture.


    Estrada, Jos├ę M; Hern├índez, Sergio; Mu├▒oz, Ra├║l; Revah, Sergio


    Bacterial biofilters usually exhibit a high microbial diversity and robustness, while fungal biofilters have been claimed to better withstand low moisture contents and pH values, and to be more efficient coping with hydrophobic volatile organic compounds (VOCs). However, there are only few systematic evaluations of both biofiltration technologies. The present study compared fungal and bacterial biofiltration for the treatment of a VOC mixture (propanal, methyl isobutyl ketone-MIBK, toluene and hexanol) under the same operating conditions. Overall, fungal biofiltration supported lower elimination capacities than its bacterial counterpart (27.7 ┬▒ 8.9 vs 40.2 ┬▒ 5.4 gCm(-3) reactor h(-1)), which exhibited a final pressure drop 60% higher than that of the bacterial biofilter due to mycelial growth. The VOC mineralization ratio was also higher in the bacterial bed (Ôëł 63% vs Ôëł 43%). However, the substrate biodegradation preference order was similar for both biofilters (propanal>hexanol>MIBK>toluene) with propanal partially inhibiting the consumption of the rest of the VOCs. Both systems supported an excellent robustness versus 24h VOC starvation episodes. The implementation of a fungal/bacterial coupled system did not significantly improve the VOC removal performance compared to the individual biofilter performances. PMID:23454457

  16. A novel approach for an automated liquid/liquid extraction system--principle and application for the determination of several trace contaminants in highly alloyed steels and base alloys.


    Wiltsche, Helmar; Prattes, Karl; Knapp, GŘnter


    A novel automated liquid/liquid extraction system was developed for the determination of trace contaminants in unalloyed, alloyed and highly alloyed steels and super alloys. In the presented batch extraction system the aqueous phase and the non-water miscible organic phase were brought into close phase contact by high-speed stirring with a magnetic stir bar. Iodide complexes of Ag, Bi, Cd, Pb, Sb, Sn, Tl, and Zn were extracted from aqueous steel digests into 4-methylpentan-2-one (MIBK) containing 20 g L(-1) trioctylphosphine oxide. Ag, Bi, Cd, Pb, and Tl were extracted quantitatively whereas the extraction yields of Sb, Sn, and Zn were 83%, 61% and 75% respectively. Using high resolution continuum source flame AAS (HR-CS-FAAS) for analyte quantification the method was validated using 21 certified steel reference materials (CRMs). PMID:21301824

  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. 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.

  20. Syn/anti isomerization of 2,4-dinitrophenylhydrazones in the determination of airborne unsymmetrical aldehydes and ketones using 2,4-dinitrophenylhydrazine derivation.


    Binding, N; MŘller, W; Witting, U


    Aldehydes and ketones readily react with 2,4-dinitrophenylhydrazine (2,4-DNPH) to form the corresponding hydrazones. This reaction has been frequently used for the quantification of airborne carbonyl compounds. Since unsymmetrical aldehydes and ketones are known to form isomeric 2,4-dinitrophenylhydrazones (syn/ anti-isomers), the influence of isomerization on the practicability and accuracy of the 2,4-DNPH-method using 2,4-dinitrophenylhydrazine-coated solid sorbent samplers has been studied with three ketones (methyl ethyl ketone (MEK), methyl isopropyl ketone (MIPK), and methyl isobutyl ketone (MIBK)). With all three ketones the reaction with 2,4-DNPH resulted in mixtures of the isomeric hydrazones which were separated by HPLC and GC and identified by mass spectroscopy and (1)H nuclear magnetic resonance spectroscopy. The isomers show similar chromatographic behaviour in HPLC as well as in GC, thus leading to problems in quantification and interpretation of chromatographic results. PMID:15045231

  1. 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

  2. Atomic absorption spectrophotometric determination of microgram levels of Co, Ni, Cu, Pb, and Zn in soil and sediment extracts containing large amounts of Mn and Fe

    USGS Publications Warehouse

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


    An atomic absorption spectrophotometric method has been developed for the determination of seven metal ions in the hydroxylamine extract of soils and sediments. Mn, Fe, and Zn are directly determined in the aqueous extract upon dilution. Co, Ni, Cu, and Pb in a separate aliquot of the extract are chelated with APDC (ammonium pyrrolidine dithiocarbamate) and extracted into MIBK (methyl isobutyl ketone) before determination. Data are presented to show the quantitative recovery of microgram levels of Co, Ni, Cu, and Pb by APDC-MIBK chelation-extraction from synthetic solutions containing as much as 2,000 ug/ml (micrograms per milliliter) Mn or 50 ug/ml Fe. Recovery of known amounts of the metal ions from sample solutions is equally satisfactory. Reproducible results are obtained by replicate analyses of two sediment samples for the seven metals.

  3. A Bio-Catalytic Approach to Aliphatic Ketones

    PubMed Central

    Xiong, Mingyong; Deng, Jin; Woodruff, Adam P.; Zhu, Minshan; Zhou, Jun; Park, Sun Wook; Li, Hui; Fu, Yao; Zhang, Kechun


    Depleting oil reserves and growing environmental concerns have necessitated the development of sustainable processes to fuels and chemicals. Here we have developed a general metabolic platform in E. coli to biosynthesize carboxylic acids. By engineering selectivity of 2-ketoacid decarboxylases and screening for promiscuous aldehyde dehydrogenases, synthetic pathways were constructed to produce both C5 and C6 acids. In particular, the production of isovaleric acid reached 32 g/L (0.22 g/g glucose yield), which is 58% of the theoretical yield. Furthermore, we have developed solid base catalysts to efficiently ketonize the bio-derived carboxylic acids such as isovaleric acid and isocaproic acid into high volume industrial ketones: methyl isobutyl ketone (MIBK, yield 84%), diisobutyl ketone (DIBK, yield 66%) and methyl isoamyl ketone (MIAK, yield 81%). This hybrid ÔÇťBio-Catalytic conversionÔÇŁ approach provides a general strategy to manufacture aliphatic ketones, and represents an alternate route to expanding the repertoire of renewable chemicals. PMID:22416247

  4. 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.

  5. Simultaneous determination of trace heavy metals in waters by atomic absorption spectrometry after preconcentration by solvent extraction

    SciTech Connect

    Saran, R. ); Basu Baul, T.S.; Srinivas, P.; Khathing, D.T. )


    A simple and rapid method for the simultaneous extraction of heavy metals using a new reagent 5-(2{prime}-carbomethoxyphenyl) azo-8-quinolinol (R) into methyl isobutyl ketone (MIBK) and their subsequent determination by flame atomic absorption spectrometry is described. The method has been applied to the determination of Cu, Pb, Ni, Fe, Cr, Co, and Mo in drinking and bore well waters. The extraction has been carried out with an aqueous to organic phase ratio to achieve around 30 fold preconcentration of metals. Extraction parameters and the influence of diverse ions have been studied. The detection limits (36) for Cu, Pb, Ni, Fe, Cr, Co and Mo are 0.07, 0.23, 0.15, 0.09, 0.22, 0.17, 0.38, {mu}g/1, respectively. Higher preconcentration factors can be achieved by using a higher aqueous to organic phase ratio and lower concentration of metals can be determined.

  6. The use of long-chain alkylamines for preconcentration of traces of molybdenum, tungsten and rhenium in their determination by atomic-absorption spectroscopy-I General studies.


    Kim, C H; Alexander, P W; Smythe, L E


    Long-chain alkylamines are used for the preconcentration of traces of molybdenum, tungsten and rhenium as thiocyanate complexes, in their determination by atomic-absorption spectroscopy. General studies of factors, influencing the extraction show that the thiocyanate complexes can be extracted into chloroform containing a low concentration of Amberlite LA1. Detection limits are 0.02 ppm Mo, 0.75 ppm W and 0.34 ppm Re in the final MIBK solution and are improved by a factor of 5-10 over those obtained by using current extraction methods. Serious interelement effects are eliminated and a range of other cations and anions are shown to have little effect on the absorption. PMID:18961721

  7. 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.

  8. 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.

  9. Recovery of poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) from Ralstonia eutropha cultures with non-halogenated solvents.


    Riedel, Sebastian L; Brigham, Christopher J; Budde, Charles F; Bader, Johannes; Rha, Chokyun; Stahl, Ulf; Sinskey, Anthony J


    Reduced downstream costs, together with high purity recovery of polyhydroxyalkanoate (PHA), will accelerate the commercialization of high quality PHA-based products. In this work, a process was designed for effective recovery of the copolymer poly(hydroxybutyrate-co-hydroxyhexanoate) (P(HB-co-HHx)) containing high levels of HHx (>15?mol%) from Ralstonia eutropha biomass using non-halogenated solvents. Several non-halogenated solvents (methyl isobutyl ketone, methyl ethyl ketone, and butyl acetate and ethyl acetate) were found to effectively dissolve the polymer. Isoamyl alcohol was found to be not suitable for extraction of polymer. All PHA extractions were performed from both dry and wet cells at volumes ranging from 2?mL to 3?L using a PHA to solvent ratio of 2% (w/v). Ethyl acetate showed both high recovery levels and high product purities (up to 99%) when using dry cells as starting material. Recovery from wet cells, however, eliminates a biomass drying step during the downstream process, potentially saving time and cost. When wet cells were used, methyl isobutyl ketone (MIBK) was shown to be the most favorable solvent for PHA recovery. Purities of up to 99% and total recovery yields of up to 84% from wet cells were reached. During polymer recovery with either MIBK or butyl acetate, fractionation of the extracted PHA occurred, based on the HHx content of the polymer. PHA with higher HHx content (17-30?mol%) remained completely in solution, while polymer with a lower HHx content (11-16?mol%) formed a gel-like phase. All PHA in solution could be precipitated by addition of threefold volumes of n-hexane or n-heptane to unfiltered PHA solutions. Effective recycling of the solvents in this system is predicted due to the large differences in the boiling points between solvent and precipitant. Our findings show that two non-halogenated solvents are good candidates to replace halogenated solvents like chloroform for recovery of high quality PHA. PMID:22903730

  10. Cold-development tool and technique for the ultimate resolution of ZEP520A to fabricate an EB master mold for nano-imprint lithography for 1Tbit/inch2 BPM development

    NASA Astrophysics Data System (ADS)

    Kobayashi, Hideo; Iyama, Hiromasa; Kagatsume, Takeshi; Watanabe, Tsuyoshi


    Cold-development is well-known for resolution enhancement on ZEP520A. Dipping a wafer in a developer solvent chilled by a freezer, such a typical method had been employed. But, it is obvious that the dip-development method has several inferiorities such as developer temperature instability, temperature inconsistency between developer and a wafer, water-condensation on drying. We then built a single wafer spin-develop tool, and established a process sequence, to solve those difficulties. And, we tried to see their effect down to -10degC over various developers. In specific, we tried to make hole patterns in hexagonal closest packing in 40nm, 35nm, 30nm, 25nm pitch, and examined holes pattern quality and resolution limit by varying setting temperature from room temperature to -10degC in the cold-development, as well as varying developer chemistry from the standard developer ZED N-50 (n-amyl acetate, 100%) to MiBK and IPA mixture which was a rinsing solvent mixture originally. We also examined the other developer (poor solvent mixture) we designed, N-50 and fluorocarbon (FC) mixture, MiBK and FC mixture, and IPA+FC mixture. This paper describes cold-development tool and technique, and its results down to minus (-) 10degC, for ZEP520A resolution enhancement to obtain 1Xnm bits (holes) in 25nm pitch to fabricate an EB master mold for Nano-Imprinting Lithography for 1Tbit/in2 bit patterned media (BPM) in HDD development and production.

  11. Sensitive assay for oxygen solubility in molten alkali metal carbonates by indirect flame atomic absorption spectrometric Cr(VI) determination.


    Scaccia, Silvera; Frangini, Stefano


    A precise and accurate indirect analytical method for the assessment of O(2) solubility in molten (Li(0.62)K(0.38))(2)CO(3) and (Li(0.52)Na(0.48))(2)CO(3) is described. The method is based on the oxidation of Cr(2)(SO(4))(3) (added in excess to the melt) by the oxygenate species, which are formed inside the melt when it is in contact with oxygen gas, and subsequent determination of trace amount of Cr(VI) in withdrawn frozen melts by flame atomic absorption spectrometry (FAAS). The samples (1.0-2.0g) are dissolved in dilute hydrochloric acid at room temperature. The speciation of Cr(VI) is carried out by complexation with ammonium pyrrolidine dithiocarbamate (APDC), followed by extraction into methyl isobutyl ketone (MIBK), which is introduced directly into the flame. Optimisation of the flame composition provided maximum Cr signal in organic phase under lean acetylene-air flame. The separation and preconcentration parameters such as sample volume/extractant volume ratio, pH sample solution, chelating concentration and extraction time are evaluated. Under the optimised conditions Cr(VI) is efficiently separated from Cr(III), which exceeded 200-folds. The results of the analysis of synthetic samples using standards in MIBK medium give rise to recoveries of 98-99%. The Cr(VI) detection limit of 4x10(-6)gL(-1) using 12.5-fold preconcentration and relative standard deviation of 1% at the 0.10mgL(-1) level are obtained. The sampling-to-sampling reproducibility was typically 3-5% relative standard deviation. By changing the preconcentration factor and the dilution of the sample melt, it is possible to analyse oxygen concentrations in molten alkali metal carbonates as low as 1.5x10(-9)mol O(2) per gram melt. PMID:18969674

  12. 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.

  13. Determination of Nickel, Vanadium and Iron in Crude Oil by Three-Phase Plasma Arc Spectrometry

    NASA Astrophysics Data System (ADS)

    Ghatass, Zekry F.


    Three-phase plasma arc (TPPA) with ultrasonic nebulizer is developed for simultaneous determination of trace elements in crude oil samples. Ultrasonic nebulizer is used instead of pneumatic nebulizer in order to minimize the problems caused by the oil viscosity during the operation. This system was used for determination of some trace elements (V, Ni, and Fe) in a crude oil samples. Methyl isobutyl ketone (MIBK) was used to dilute the oil samples. The TPPA instrument offers several advantages including a low cost power supply with no radio frequency, linear dynamic ranges from 4 to 5 of orders of magnitude, and detection limits (0.121, 0.313 and 0.242 (╬╝g/ml) for Ni, V and Fe respectively. The average concentrations were 31 ┬▒ 0.45 (╬╝g/ml) for Ni, 40 ┬▒ 0.88 (╬╝g/ml) for V and 8 ┬▒ 0.74 (╬╝g/ml) for Fe at Balaaiem fields and 2 ┬▒ 0.05 (╬╝g/ml) for Ni, 4.8 ┬▒ 0.25 (╬╝g/ml) for V and 2 ┬▒ 0.10 (╬╝g/ml) for Fe at Wastern Desert fields.

  14. New phase separator for extraction-spectrophotometric determination of anionic surfactants with Malachite Green by flow injection analysis.


    Sakai, T; Harada, H; Liu, X; Ura, N; Takeyoshi, K; Sugimoto, K


    A simple flow injection spectrophotometric method for the determination of anionic surfactants in river water was studied. A three-channel flow system was assembled. The distilled water as a carrier and 5x10(-5) mol l(-1) Malachite Green (MG) dissolved in 0.1 mol l(-1) CH(3)COONa-CH(3)COOH buffer solution (pH 5) were delivered at 1.94 ml min(-1). The mixed solvent (toluene+methylisobutyl ketone (MIBK)=1+1) was pumped at 0.78 ml min(-1). Other conditions were the extraction coil 0.5 mm i.d.x3 m, the reaction temperature 20 degrees C and the sample size 200 mul. The calibration graph was linear in the range 0.1-0.4 ppm at 626 nm. The detection limit (S/N=3) was 18 ppb and a sample frequency of 20 h(-1) was attained. The relative standard deviation (n=7) for 0.4 ppm standard sodium dodecylsulfate (SDS) solutions was 1.1%. And also, new phase separator with a convenient connector was designed. This Fl method was applied to the determination of anionic surfactants in river water. PMID:18967035

  15. Gases and organic solvents in urine as biomarkers of occupational exposure: a review.


    Imbriani, M; Ghittori, S


    A brief review of urine analysis in studies of occupational exposure to volatile organic compounds and gases is provided. Analysis of exhaled breath for volatile compounds does not have a long history in occupational medicine. A number of studies has been undertaken since the 1980s, and the methods are well enough accepted to be put forward as biological equivalents of threshold limit values (TLVs) for some volatile organic compounds (VOCs) such as acetone; methanol; methyl ethyl ketone (MEK); methyl isobutyl ketone (MIBK); tetrahydrofurane; dichloromethane. In the last 20 years many scientific articles have shown that the urinary concentrations of unchanged solvents are correlated with environmental exposure and could be used for biological monitoring. The use of urine analysis of unchanged solvents in occupational applications is not yet widespread. Nonetheless, in the short time since its application, a number of important discoveries has been made, and the future appears bright for this branch of analysis. In this paper, the basic concepts and methodology of urine analysis are briefly presented with a critical revision of the literature on this matter. The excretion mechanisms of organic solvents in urine are discussed, with regard to biological variability, and the future directions of research are described. PMID:15592680

  16. Organic-inorganic hybrid resists for EUVL

    NASA Astrophysics Data System (ADS)

    Singh, Vikram; Kalyani, Vishwanath; Satyanarayana, V. S. V.; Pradeep, Chullikkattil P.; Ghosh, Subrata; Sharma, Satinder; Gonsalves, Kenneth E.


    Herein, we describe preliminary results on organic-inorganic hybrid photoresists, capable of showing line patterns up to 16 nm under e-beam exposure studies, prepared by incorporating polyoxometalates (POMs) clusters into organic photoresist materials. Various Mo and W based clusters such as (TBA)2[Mo6O19], (TBA)5(H)[P2V3W15O62] and (TBA)4[P2Mo18O61] (where TBA = tetrabutyl ammonium counter ion) have been incorporated into PMMA matrix by mixing POM solutions and standard PMMA polymer in anisole (MW ~ 95000, MicroChem) in 1:33 w/v ratio. E-beam exposure followed by development with MIBK solutions showed that these new organic-inorganic hybrid photoresists show good line patterns upto 16 nm, which were not observed in the case of control experiments done on pure PMMA polymer resist. The observed enhancement of resist properties in the case of hybrid resists could possibly be due to a combination of features imparted to the resist by the POM clusters such as increased sensitivity, etch resistance and thermal stability.

  17. 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)

  18. 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.

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


    Marfil, Rocio; Cabrera-Vique, Carmen; GimÚnez, Rafael; Bouzas, Paula R; MartÝnez, Olga; Sßnchez, 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

  20. Complex reaction networks in high temperature hydrocarbon chemistry.


    Mutlay, ?brahim; 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

  1. Predicting Optimal Resolving Power for Ambient Pressure Ion Mobility Spectrometry (IMS)

    PubMed Central

    Kanu, Abu B.; Gribb, Molly M.; Hill, Herbert H


    Although diffusion theory predicts that IMS resolving power increases with the square root of the voltage applied across the drift tube, in practice there exists an optimum voltage above which resolving power decreases. This optimum voltage was determined to be both compound and initial ion pulse width-dependent. A ôconditionalö resolving power equation is introduced that can be used to quickly approximate realistic resolving powers for specific instrumental operating parameters and compounds. Using four common environmental contaminants [trichloroethylene (TCE), tetrachloroethylene (PCE), methyl tert-butyl ether (MTBE) and methyl iso-butyl ketone (MIBK)], diffusion-limited (theoretical), Rd, conditional, Rc, and actual (or measured), Rm, IMS resolving powers were determined and compared for a small IMS instrument designed for subsurface measurements. Detection limits determined at the optimal resolving power for the environmental contaminants ranged from 18 parts per trillion volume-to-volume (pptv) to 80 parts per billion volume-to-volume (ppbv). The maximal measured resolving power for our small, ambient-pressure stand-alone IMS ranged from 42 to 54, yielding an IMS resolving power efficiency, defined as Rm/Rc Î 100%, of 56 to 74% of the maximal conditional resolving power possible. PMID:18683951

  2. 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.

  3. Nickel and strontium nitrates as modifiers for the determination of selenium in wine by Zeeman electrothermal atomic absorption spectrometry.


    Cvetkovi─ç, J; Stafilov, T; Mihajlovi─ç, D


    A mixed matrix modifier of nickel and strontium nitrates was used as a chemical modifier for the determination of selenium in wines by Zeeman electrothermal atomic absorption spectrometry. Wine samples were heated on a boiling water bath with small amounts of nitric acid and hydrogen peroxide. For complete elimination of interference, especially from sulfates and phosphates, selenium is complexed with ammonium pyrolidinedithiocarbamate (APDTC), extracted into methyl isobutyl ketone (MIBK), and measured by ETAAS. The graphite furnace temperature program was optimized for both aqueous and organic solutions. Pyrolysis temperatures of 1300 degrees C and 800 degrees C were chosen for aqueous and organic solutions, respectively; 2700 degrees C and 2100 degrees C were used as optimum atomization temperatures for aqueous and organic solutions, respectively. The optimum modifier mass established is markedly lower than those presented in the literature. The platform atomization ensures pretreatment stabilization up to 1100 degrees C and 1600 degrees C, respectively, for organic and aqueous selenium solutions. The procedure was verified by the method of standard addition. The investigated wine samples originated from the different regions of the Republic of Macedonia. The selenium concentration varied from not detectable to 0.93 microg L(-1). PMID:11583090

  4. 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.

  5. Simulation of the breakthrough behavior of volatile organic compounds against sorbent tube sampler as a function of concentration level and sampling volume.


    Kim, Ki-Hyun; Lee, Min-Hee; Szulejko, Jan E


    The breakthrough (BT) properties of Tenax TA sorbent were challenged by gaseous standards containing a suite of 13 volatile organic compounds (VOC): (1) aromatic hydrocarbons: benzene (B), toluene (T), p-xylene (p-X), and styrene (S), (2) aldehydes: acetaldehyde (AA), propionaldehyde (PA), butyraldehyde (BA), isovaleraldehyde (IA), and valeraldehyde (VA), (3) ketones: methyl ethyl ketone (MEK) and methyl isobutyl ketone (MIBK), and (4) two others: isobutyl alcohol (i-BuAl) and butyl acetate (BuAc). To this end, 1-3 L of standards (10-50 ppb) were loaded on the two sorbent tubes (ST) connected in series at 100 mL min(-1). The front ST-1 was used for calibration purposes, while the ST-2 for breakthrough (recovery criterion of <1% with p-xylene as the key datum point). Although aromatic hydrocarbons generally met such criterion, benzene was readily distinguishable with the maximum BT. The BT for the aldehydes exhibited ~100% (AA) ? 85% (PA) ? 45% (BA) ? 30% (VA and IVA). There is good correlation between ST-2 recovery vs. carbon number for >CO entity (aldehydes, ester, and ketones). As such, BT is essentially concentration independent and relatively predictable across different functional groups and between the homologues. However, the BT behavior of ppb level VOCs is no longer consistent for certain species (like benzene or MEK) relative their ppm counterparts. This variation is explained by the Langmuir equation in which the 1/BTV is proportional to analyte gas-phase concentration, if the gas-phase/sorbent partition coefficient is large. PMID:24952628

  6. Fate of 14C-Pyrene in soil-plant system amended with pig manure compost and Tween 80: a growth chamber study.


    Cheng, Ka Yu; Wong, Jonathan W C


    This paper evaluated the effects of a pig manure compost (PMC) and a nonionic surfactant Tween 80 on the fate of 14C-Pyrene (Pyr) in a soil-plant system (Agropyron elongatum). Soils spiked with 14C-4, 5, 9, 10-Pyr were amended with 7.5% (w/w) PMC together with or without 100mgkg(-1) of Tween 80. Unplanted soil without amendments was set as the control. Gas phases of the systems were monitored for 14CO2 over a 60 days period. The impact of PMC and Tween 80 on the apparent loss of the PAH and the distribution of 14C-activity in the systems was studied. 14C-activity associated with different soil fractions was further examined by using methyl-isobutyl-ketone (MIBK) fractionation method. The results showed that the addition of PMC could increase the dissipation of Pyr in vegetated soil from 12.1% to 58.7%, while the co-addition of Tween 80 and PMC could further enhance the dissipation to 90.3%. Pyr dissipation in soil was correlated with the mineralization of 14C-Pyr, indicating that Pyr dissipation was mainly due to mineralization. A higher formation of water-extractable metabolites was observed in soil amended with PMC and Tween 80, and this was correlated with a higher biomass accumulation of 14C-activity and higher bound residue formation in the soil. Overall, this study suggested that the co-application of PMC and Tween 80 could improve phytoremediation of Pyr-contaminated soil. PMID:18400492

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


    Demirta?, ?lknur; Bak?rdere, 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 Ág/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 ÁL 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 the certified value using SQT-AT-FAAS and Ta coated-SQT. PMID:25863394


    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, self-supporting thin films and have, therefore, been used for adhesives, safety glass, and finishes. If the bacterial culture produces the L-lactic acid enanatiomer form exclusively, the L-lactide prepared from this form can be used for making polymers with good fiber-forming properties. We have not currently achieved the exclusive production of L-lactate in our efforts. However, markets in films and structural shapes are available for polymers and copolymers prepared from the mixed D,L-lactide forms that result from processing the D,L-lactic acid obtained from fermentation such as that occurring naturally in sugar beet wastewater. These materials are slowly biodegraded to harmless compounds in the environment, and they burn with a clean blue flame when incinerated. These materials represent excellent opportunities for utilization of the D,L-lactic mixture produced from natural fermentation of the ACS flume water. Esters can be converted into a lactide, and the alcohol released from the ester can be recycled with no net consumption of the alcohol. Lactide intermediates could be produced locally and shipped to polymer producers elsewhere. The polymer and copolymer markets are extremely large, and the role of lactides in these markets is continuously expanding. The overall process can be readily integrated into existing factory wastewater operations. There are several environmental benefits that would be realized at the factories with incorporation of the lactate recovery process. The process reduces the organic loading to the existing wastewater treatment system that should result in enhanced operability with respect to both solids handling and treated-water quality. A higher-quality treated water will also help reduce odor levels from holding ponds. Several water reuse opportunities are probable, depending on the quality of treated water from the FT process.