Validation of an analytical method by GC-FID for the quantification of styrene and α-methylstyrene

Styrene and α-methylstyrene are substrates of great interest in asymmetric catalysis. Although they have been widely used, known quantification methodologies are restricted to the use of mass spectrometry detectors and are not validated. In the present work, we developed and validated a reliable method by gas chromatography with a flame ionization detector (GC-FID) for the analysis of non-functionalized olefins (styrene and α-methylstyrene) in a liquid matrix using toluene as the internal standard. We explored validation parameters such as selectivity, linearity, detection limit, quantification limit, precision, and accuracy. The results showed an adequate separation of each olefin under the conditions and range of work implemented (6.83x10-4 mol/L - 4.059x10-3 mol/L). The parameters evaluated are within acceptable values indicating that the validated method is selective, linear, precise, and accurate. This work represents an effort to develop a highly safe, efficient, and validated chromatographic method for the quantification of styrene and α-methylstyrene in liquid matrices for their possible application in the field of resins, plasticizers, and polymers where they are mainly involved.

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Gas-Liquid Chromatographic Method for the Analysis of Carbaryl Insecticide Formulations

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/57.4.778 ◽

1974 ◽

Vol 57 (4) ◽

pp. 778-780 ◽

Cited By ~ 1

Author(s):

Lois G Weyer

Keyword(s):

Chromatographic Method ◽

Internal Standard ◽

Direct Analysis ◽

Flame Ionization Detector ◽

Gas Chromatograph ◽

Ionization Detector ◽

Technical Grade ◽

Flame Ionization ◽

Liquid Chromatographic Method ◽

Liquid Chromatographic

Abstract A gas-liquid chromatographic method has been developed for the direct analysis of Sevin (carbaryl, 1-naphthyl N-methylcarbamate) technical grade, Sevin 85, Sevin 80, and Sevin 50 formulations. The method consists of dissolving the sample in chloroform containing Thiodan as an internal standard; an aliquot of the supernate is injected into a gas chromatograph with a flame ionization detector and a column packed with 3% SE-30 on 60-80 mesh Gas- Chrom Q. The method compares favorably in accuracy with older methods, is not subject to interferences, is rapid, and has automation possibilities.

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Determination of Trifluralin in Formulations by Gas Chromatography

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/54.1.125 ◽

1971 ◽

Vol 54 (1) ◽

pp. 125-127

Author(s):

Larry G Hambleton

Keyword(s):

Gas Chromatography ◽

Chromatographic Method ◽

Internal Standard ◽

Flame Ionization Detector ◽

Gas Chromatograph ◽

Ionization Detector ◽

Average Recovery ◽

Flame Ionization ◽

Gas Chromatographic Method

Abstract A gas chromatographic method has been developed that is rapid and specific for trifluralin in formulations. The sample is extracted with acetone, an internal standard is added, and the solution is diluted to volume and injected into a gas chromatograph equipped with a flame ionization detector. Three typical trifluralin formulations were analyzed by both the gas chromatographic method and an ultraviolet method. The gas chromatographic method gave an average recovery of 101.2%.

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Gas-chromatographic method for plasma acetate analysis in acetate-intolerance studies.

Clinical Chemistry ◽

10.1093/clinchem/24.2.348 ◽

1978 ◽

Vol 24 (2) ◽

pp. 348-350 ◽

Cited By ~ 3

Author(s):

L G Nielsen ◽

K O Ash ◽

E Thor

Keyword(s):

Chromatographic Method ◽

Hemodialysis Patients ◽

Flame Ionization Detector ◽

Gas Chromatograph ◽

Ionization Detector ◽

Flame Ionization ◽

Single Column ◽

Gas Chromatographic Method

Abstract We describe a modified gas-chromatographic method for acetate in serum or plasma, intended for use in the investigation of acetate intolerance in hemodialysis patients. The assay may be adapted for use with a single-column gas chromatograph equipped with a flame ionization detector. The analysis, made isothermally, requires only 0.5 ml of plasma or serum. Only one deproteinizing step is required to prepare the sample for analysis. Additionally, we present preliminary findings of an ongoing acetate-intolerance study.

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Determination of Phenothiazine and Several of its Derivatives by Gas-Liquid Chromatography

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/49.4.857 ◽

1966 ◽

Vol 49 (4) ◽

pp. 857-859

Author(s):

C L Bramlett

Keyword(s):

Liquid Chromatography ◽

Internal Standard ◽

Flame Ionization Detector ◽

Gas Liquid Chromatography ◽

Chromatographic Technique ◽

Ionization Detector ◽

Flame Ionization ◽

Hydrogen Flame

Abstract Phenothiazine, promethazine.HCl, chlorpromazine. HCl, promazine.HCl, and levomepromazine. HCl were chromatographed satisfactorily on a column containing 5% Apiezon L coated on Anakrom ABS, 100/110 mesh, using a hydrogen-flame ionization detector. This gas chromatographic technique is rapid and more specific than existing official methods. The use of an internal standard to improve precision will be investigated.

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Collaborative Study of a Gas Chromatographic Method for Ronnel in Feeds

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/52.3.435 ◽

1969 ◽

Vol 52 (3) ◽

pp. 435-438

Author(s):

Albert J Gehrt

Keyword(s):

Chromatographic Method ◽

Collaborative Study ◽

Flame Ionization Detector ◽

Ionization Detector ◽

Flame Ionization ◽

Coefficients Of Variation ◽

Chromatographic Measurement ◽

Cattle Feeds ◽

Gas Chromatographic Method

Abstract A GLC method (flame ionization detector) for ronnel in cattle feeds at levels of 0.038, 0.041, and 0.055% was studied by 11 collaborators. The method involves extraction of ronnel by shaking with acetone followed by direct chromatographic measurement. The method is simple and rapid (no cleanup required), measures true ronnel, and is free from interferences present in the UV methods previously studied. Agreement between laboratories was satisfactory; coefficients of variation were 11.0, 12.0, and 7.2%. Ronnel recoveries were 81.1, 93.5, and 98.0%. Low recovery from the first sample may be due to ronnel hydrolysis or binding during storage (sample was 8 months old). The Associate Keferee recommends that the method be adopted as official first action.

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Determination of volatile alcohols and acetone in serum by non-polar capillary gas chromatography after direct sample injection.

Clinical Chemistry ◽

10.1093/clinchem/30.10.1672 ◽

1984 ◽

Vol 30 (10) ◽

pp. 1672-1674 ◽

Cited By ~ 16

Author(s):

N B Smith

Keyword(s):

Gas Chromatography ◽

Capillary Gas Chromatography ◽

Capillary Column ◽

Internal Standard ◽

Fused Silica ◽

Gas Chromatograph ◽

Ionization Detector ◽

Flame Ionization ◽

Split Ratio

Abstract In this method for detection and quantification of volatile alcohols by capillary gas chromatography, the serum sample is deproteinized, then directly injected into the gas chromatograph with 1-propanol as the internal standard. The capillary column is a 30-m bonded methylsilicone-coated, fused-silica column. With helium as the carrier gas, the injector inlet is set at a split ratio of 1/30 and the average linear velocity in the column is 25 cm/s. Injector and flame-ionization detector temperatures are 280 degrees C, oven temperature 35 degrees C. Chromatography time is less than 3 min.

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Impurity Problems in Chromatographic Method Studies for Fenthion Formulations

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/68.5.925 ◽

1985 ◽

Vol 68 (5) ◽

pp. 925-929

Author(s):

Willard G Boyd

Keyword(s):

Mobile Phase ◽

Chromatographic Method ◽

Collaborative Study ◽

Internal Standard ◽

Flame Ionization Detection ◽

Private Communication ◽

Flame Ionization ◽

Glass Column ◽

Liquid Chromatographic ◽

Chromatographic Mass

Abstract Several gas chromatographic (GC) methods for analyzing fenthion were studied, and flame ionization detection, a glass column packed with SE-52 on Chromosorb GHP, and on-column injection were selected as parameters. No suitable internal standard was found because of coeluting, bias-producing impurities in fenthion. Several liquid chromatographic (LC) methods were also studied, and UV detection, a Zorbax ODS column, and a methanol-water-H3P04 mobile phase were finally selected as parameters. Dipentyl phthalate was selected as internal standard. After testing, this LC method was submitted for collaborative study. During the collaborative study, the manufacturer found an impurity, 3-methyl-4-(methylthio)anisole, co-eluting with fenthion in the collaborative method. The manufacturer's method was then evaluated as an alternative for collaborative study, but a significant unidentified impurity from the formulation blank, used for formulating emulsifiable concentrates, was also found co-eluting with fenthion. The anisole impurity was verified by LC, and the presence of the S-isomer and bis-methylthio-fenthion impurities was found by gas chromatographic- mass spectrometric (GC-MS) analyses. An anisole material obtained from Mobay was also verified by GC-MS analysis. Several other impurities were identified from literature references and from private communication with the manufacturer.

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Gas Chromatographic Determination of Dioxathion and Chlorfenvinphos in Emulsifiable Formulations and Livestock Dips

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/53.3.566 ◽

1970 ◽

Vol 53 (3) ◽

pp. 566-568

Author(s):

J E Paterson

Keyword(s):

Quantitative Determination ◽

Chromatographic Analysis ◽

Chromatographic Method ◽

Silicone Oil ◽

Chromatographic Determination ◽

Ionization Detector ◽

Flame Ionization ◽

Coefficients Of Variation ◽

Gas Chromatographic Method

Abstract A gas chromatographic method is described for the quantitative determination of dioxathion and chlorfenvinphos in emulsifiable concentrates and livestock dips. A convenient quantity of the emulsifiable formulation is dissolved in xylene and the aqueous dip is extracted with xylene for gas chromatographic analysis, using a mixed silicone oil stationary phase and a flame ionization detector. The coefficients of variation for the dioxathion and chlorfenvinphos determinations in the emulsifiable concentrate are 2.4 and 1.0%, respectively. Recoveries of the former from a fouled dip ranged from 97 to 103% and recoveries of the latter ranged from 92 to 97%.

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Effect of grape variety (Vitis vinifera L.) and grape pomace fermentation conditions on some volatile compounds of the produced grape pomace distillate

OENO One ◽

10.20870/oeno-one.2004.38.4.912 ◽

2004 ◽

Vol 38 (4) ◽

pp. 225 ◽

Cited By ~ 1

Author(s):

Maria Gerogiannaki-Christopoulou ◽

Nikolaos V. Kyriakidis ◽

Panagiotis E. Athanasopoulos

Keyword(s):

Citric Acid ◽

Vitis Vinifera ◽

Volatile Compounds ◽

Internal Standard ◽

Grape Pomace ◽

Grape Variety ◽

Ionization Detector ◽

Flame Ionization ◽

Grape Varieties

<p style="text-align: justify;">Agrape pomace distillate was produced from 4 Greek white grape varieties (<em>Vitis vinifera</em> L.). Pomace was fermented with and without addition of citric acid, acting as an antibacterial agent, during fermentation. Fermented grape pomace was distilled in a traditional copper distillation apparatus.. Five major volatile compounds, including methanol, were measured. Pentanol-3 was used as an internal standard. Flame ionization detector (FID) coupled to capillary gas chromatography was used for determination of five volatile distillate components. The addition of citric acid resulted in the reduction of methanol content by about 15%. All the other components studied did not affect in any appreciable degree.</p>

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Direct Blood-Injection Method for Gas Chromatographic Determination of Alcohols and Other Volatile Compounds

Clinical Chemistry ◽

10.1093/clinchem/17.2.82 ◽

1971 ◽

Vol 17 (2) ◽

pp. 82-85 ◽

Cited By ~ 63

Author(s):

Naresh C Jain

Keyword(s):

Sample Preparation ◽

Volatile Compounds ◽

Low Cost ◽

Internal Standard ◽

Chromatographic Determination ◽

Gas Chromatograph ◽

Ionization Detector ◽

Flame Ionization ◽

Blood Injection

Abstract An extremely simple, rapid method is described for simultaneously determining methanol, ethanol, acetone, isopropanol, and low-boiling hydrocarbons associated with glue sniffing. Less than 1 µl of blood, mixed with an internal standard, is injected directly into a low-cost gas chromatograph equipped with a flame-ionization detector. No extraction, distillation, and (or) sample preparation is required, and the method is sensitive to less than 10 µg of alcohol per ml.

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