Determination of Ethylene Oxide in Ethoxylated Surfactants and Demulsifiers by Headspace
Gas Chromatography

Abstract A headspace gas chromatographic method for the determination of traces of ethylene oxide in ethoxylated surfactants and demulsifiers was developed. Samples are analyzed directly by the technique to a 1.0 ppm (w/w) quantitation limit. The procedure also performs well for propylene oxide, acetaldehyde, and 1,4-dioxane. It is simple, sensitive, and linear. The percent relative standard deviations for 0.5 and 30 ppm ethylene oxide in the surfactant were 2.8 and 8.3%, respectively.

Download Full-text

Determination of Residual Ethylene Oxide in Spectinomycin Hydrochloride Bulk Drug by Dynamic Headspace Gas Chromatography

Journal of AOAC International ◽

10.1093/jaoac/76.2.313 ◽

1993 ◽

Vol 76 (2) ◽

pp. 313-319

Author(s):

Tore Ramstad ◽

Lisa S Miller ◽

Virginia N Thomas

Keyword(s):

Detection Limit ◽

Ethylene Oxide ◽

Chromatographic Method ◽

Headspace Gas Chromatography ◽

Dynamic Headspace ◽

Relative Standard ◽

Headspace Gas ◽

Bulk Drug ◽

Gas Chromatographic Method

Abstract A dynamic headspace gas chromatographic method was developed for the determination of residual ethylene oxide (EtO) in a pharmaceutical bulk drug, spectinomycin hydrochloride. The recommended column is PoraPLOT Q; PoraPLOT U was demonstrated to be equivalent. A detection limit of 2 ppb was achieved, and linearity was established to the highest value tested (5 ppm). The detection limit was 2-3 orders of magnitude lower than that achieved in previously published methods for EtO in pharmaceutical bulk drugs. Precision studies yielded relative standard deviations ranging from 2 to 10% over the 10-575 ppb concentration range. The method was applied to support EtO sterilization studies conducted at The Upjohn Company and was implemented for routine use. The sterilization studies demonstrated that residual levels of EtO <10 ppb are achievable.

Download Full-text

Determination of total phosphorus in soil and sludge by an effective headspace gas chromatographic method

RSC Advances ◽

10.1039/c9ra07228d ◽

2019 ◽

Vol 9 (70) ◽

pp. 40961-40965

Author(s):

Yukai Zheng ◽

Weide Fu ◽

Rencheng Zhu ◽

Zhanbo Hu ◽

Gang Chen ◽

...

Keyword(s):

Gas Chromatography ◽

Total Phosphorus ◽

Chromatographic Method ◽

Headspace Gas Chromatography ◽

Headspace Gas ◽

Novel Method ◽

Gas Chromatographic Method

This paper reported a novel method for the determination of total phosphorus (TP) content in soil and sludge by a headspace gas chromatography (HS-GC) method.

Download Full-text

Determination of 1,3-Dichloropropanol in Soy Sauce and Related Products by Headspace Gas Chromatography with Mass Spectrometric Detection: Interlaboratory Study

Journal of AOAC International ◽

10.1093/jaoac/88.5.1404 ◽

2005 ◽

Vol 88 (5) ◽

pp. 1404-1412 ◽

Cited By ~ 4

Author(s):

Sarah Hasnip ◽

Colin Crews ◽

Nicholas Potter ◽

Paul Brereton ◽

Henri Diserens ◽

...

Keyword(s):

Gas Chromatography ◽

Standard Deviation ◽

Relative Standard Deviation ◽

Internal Standard ◽

Mass Spectrometric ◽

Soy Sauce ◽

Headspace Gas Chromatography ◽

Relative Standard ◽

Headspace Gas

Abstract An interlaboratory study was performed to evaluate the effectiveness of a headspace gas chromatography (GC) method for the determination of 1,3-dichloro-propan-2-ol (1,3-DCP) in soy sauce and related products at levels above 5 ng/g. The test portion is mixed with an internal standard (d5-1,3-DCP) and ammonium sulfate in a sealed headspace vial. After achieving equilibrium, the headspace is sampled either by gas-tight syringe or solid-phase microextraction (SPME) and analyzed by GC with mass spectrometric detection. 1,3-DCP is detected in the selected-ion mode (monitoring m/z 79 and 81 for 1,3-DCP and m/z 82 for the deuterated internal standard) and quantified by measurement against standards. Test materials comprising soy, dark soy, mushroom soy, and teriyaki sauces, both spiked and naturally contaminated, were sent to 9 laboratories in Europe, Japan, and the United States; of these, 5 used SPME and 4 used syringe headspace analysis. Test portions were spiked at 5.0, 10.0, 20.0, 100.0, and 500.0 ng/g. The average recovery for spiked blank samples was 108% (ranging from 96–130%). Based on results for spiked samples (blind pairs at 5, 10, 20, 100, and 500 ng/g) as well as a naturally contaminated sample (split-level pair at 27 and 29 ng/g), the relative standard deviation for repeatability (RSDr) ranged from 2.9–23.2%. The relative standard deviation for reproducibility (RSDR) ranged from 20.9–35.3%, and HorRat values of between 1.0 and 1.6 were obtained.

Download Full-text

Determination of Styrene Migration from Food-Contact Polymers into Margarine, Using Azeotropic Distillation and Headspace Gas Chromatography

Journal of AOAC INTERNATIONAL ◽

10.1093/jaoac/66.5.1067 ◽

1983 ◽

Vol 66 (5) ◽

pp. 1067-1073

Author(s):

Sandra L Varner ◽

Charles V Breder ◽

Thomas Fazio

Keyword(s):

Gas Chromatography ◽

Azeotropic Distillation ◽

Flame Ionization Detector ◽

Headspace Gas Chromatography ◽

Ionization Detector ◽

Migration Studies ◽

Flame Ionization ◽

Quantitation Limit ◽

Headspace Gas

Abstract Migration studies were conducted to determine the quantity of styrene that migrates from polymers into fatty foods, specifically margarine. Azeotropic distillation was used to isolate styrene from the margarine. Headspace gas chromatography with a Chromosorb 104 column and a flame ionization detector was used for quantitation. The quantitation limit for the method was about 25 ppb (wt/wt) styrene in margarine. On the average, greater than 90% of the styrene was recovered. Several commercial margarines were examined. The method and results of the migration studies are presented. There was no detectable migration of styrene into margarine.

Download Full-text

Determination of pinene content in black liquor by solvent-assisted/pyrogallol-protected headspace gas chromatography (HS-GC)

Holzforschung ◽

10.1515/hf-2018-0031 ◽

2018 ◽

Vol 72 (11) ◽

pp. 973-978

Author(s):

Hui-Chao Hu ◽

Tong Zeng ◽

Shaokai Zhang ◽

Lihui Chen ◽

Liulian Huang ◽

...

Keyword(s):

Gas Chromatography ◽

Good Accuracy ◽

Black Liquor ◽

Kraft Pulping ◽

Headspace Gas Chromatography ◽

Complete Dissolution ◽

Sample Storage ◽

Relative Standard ◽

Headspace Gas

Abstract A solvent-assisted and pyrogallol (PG)-protected headspace gas chromatography (HS-GC) method was developed to determine the pinene (α- and β-pinene) content in the kraft pulping black liquor (BL). Ethanol (EtOH) addition eliminated pinene’s micelles in BL by complete dissolution in the EtOH/BL medium. PG was applied to protect pinene from oxidation during the sample storage and measurement. The results showed that, with a 25% (v/v) of EtOH content and a 0.1 g of PG in 5-ml of sample solution, a rapid and stable pinene HS extraction can be obtained in 20 min at 80°C. The method has high precision with relative standard deviations within 4.2%. The sensitivity [limits of quantification (LOQ) are ~140 μg l−1] was high, and a good accuracy (recovery=96.0–104%) was typical for the pinene detection. The presented method is simple, rapid, accurate and is suitable for pinene quantification in biorefinery related processes and it leads to the preparation of high-value chemicals.

Download Full-text