Determination Of Epichlorohydrin Research Articles

Determination of epichlorohydrin in workplace air by gas chromatograph-electron capture detector

To develop a method for determining epichlorohydrin in the workplace air by gas chromatograph-electron capture detector (GC-ECD). Epichlorohydrin in the workplace air was collected by activated charcoal tubes, desorbed using acetone, and analyzed by GC-ECD. A good linearity was obtained in the range of 1.0-50 µg/mL (r=0.999 7). The detection limit was 0.012 µg/ml, while the recovery rate was 88.1% and relative standard deviation ranged from 1.11% to 3.57%. The samples could be stored for seven days at room temperature. This method effectively eliminates the interferences of alkanes on determination of epichlorohydrin and improves the sensitivity by 1 to 2 orders of magnitude, which can solve the problem of detection limit above standard in GBZ/T 160.58-2004.

Determination of epichlorohydrin in drinking water by isotope dilution gas chromatography-mass spectrometry

To establish a method for determination of the epichlorohydrin in drinking water by isotope dilution gas chromatography-mass spectrometry (GC-MS). The internal standard solution D5-epichlorohydrin was added in drinking water sample. The epichlorohydrin was firstly collected by active carbon, and the adsorbent was then centrifuged at 2739 × g for 10 min to remove water. Finally, the epichlorohydrin was desorbed by dipping the active carbon in 1.0 ml acetone for 1 h. The desorbed solution was tested by GC-MS and quantified with isotopic internal standards. The detection limit, precision and accuracy of the assay were evaluated. This method was adopted to detect the epichlorohydrin in drinking water for 25 batches in a city. The determination method of epichlorohydrin represented a good linear relationship in the range of 0.0645-3.8700 µg/L, the linear regression equation was Y = 2.828X + 4.91 × 10(-2) (r > 0.999). When the epichlorohydrin concentration were 0.0806, 0.3230 and 3.2300 µg/L, the relative standard deviations (RSD) were 7.9%, 4.7% and 3.1%, respectively. The average recoveries were from 95.7% to 98.7%. The limit of detection (LOD) was 0.015 µg/L, limit of quantification (LOQ) was 0.052 µg/L. The content of epichlorohydrin in the 25 cases of drinking water was under the limit of detection. The method is more simple than the national standard method, with high sensitivity, accuracy and good reproducibility, which is suitable for detection of the trace amounts of epichlorohydrin in drinking water.

Development of diffusive solid phase microextraction method for sampling of epichlorohydrin in air

Epichlorohydrin is used frequently in many industrial processes. Exposure to this pollutant could induce harmful effects. The present work developed a novel solid phase microextraction (SPME) method for time weighted average determination of epichlorohydrin in the air by GC/MS. CAR/PDMS in 0.5 cm retracted mode was selected and the effect of environmental parameters on sampling properties of SPME was examined. Experimental sampling rate for epichlorohydrin (8.89 × 10−3 cm3/min) was slightly less than theoretical value (9.059 × 10−3 cm3/min). There was no significant difference among sampling rates at different temperature and velocities but relative humidity had a significant effect on the sampling rate. Limit of detection for SPME method was 0.8 ng per sample, which is good enough in comparison with the NIOSH 1010 method. Comparison of the results between the developed SPME and the NIOSH 1010 method on standard test atmosphere and field showed satisfactory agreement (y = 1.162x + 1.8 r 2 = 0.992 and y = 1.009x+0.76 r 2 = 0.98 respectively).

Determination of Epichlorohydrin in Active Pharmaceutical Ingredients by Gas Chromatography–Mass Spectrometry

During the development of new active pharmaceutical ingredients (API), the control of low level impurities plays a crucial role in the progression of a new compound. Particular attention is given to known or suspected genotoxic impurities, which, to ensure patient safety, have a maximum daily patient exposure limit of 1.5 μg/day for long-term exposure (>12 months).In this communication, we report the development and validation of a part per million (ppm) level GC–MS method to detect epichlorohydrin (ECH) in a new API under development in Chemical Development at GlaxoSmithKline Verona, now an Aptuit Research Centre. GC separation was conducted on a DB-624 column, while MS detection was performed on a single-quad MSD in selected ion monitoring mode. After successful development, the method was validated according to our in-house validation guidelines for ppm level analysis. The method proved to be selective for ECH in drug substance. Sensitivity of the method (limit of quantitation (LOQ)) proved to be as low as 0.8 ppm (w/w) when the API samples were prepared at 45 mg/mL (free base). The precision (% RSD) of five preparations of spiked samples at the concentration of 8 ppm (target analytical level (TAL)) was 1.3, while recovery proved to be 97%, demonstrating the absence of matrix effect.

Determination of epichlorohydrin and 1,3-dichloro-2-propanol in synthesis of cationic etherifying reagent by headspace gas chromatography

This study demonstrates a headspace gas chromatographic(HS-GC) technique for the determination of residual epichlorohydrin (ECH) and generated 1,3-dichloro-2-propanol (DCP) in synthesis process of 3-chloro-2-hydroxypropyltrimethylammonium chloride (CHTAC). By a weight-based sampling method, coupled with significant dilution in 15.8% sodium sulfate and 0.1% silver nitrate mixed solution rapidly, the sample for HS-GC analysis is prepared. Based on the reaction stoichiometry, the conversion ( R) of CHTAC during the synthesis process can be calculated from sampling weight and GC peak area. The results showed that the method has a good measurement precision (RSD < 2.5%) and accuracy (recovery = 101–104%) for the quantification of both ECH and DCP in the process samples. The present method is simple and accurate, which can be used for the efficient determination of the CHTAC conversion in the synthesis research.

Determination of epichlorohydrin in water and sewage samples

The simple, quick and effective methods for the analysis of epichlorohydrin (ECH) in water and sewage samples with the use of gas chromatography have been presented. From among all the methods developed, the procedures for monitoring drinking-water quality and the methods which allow the determination of epichlorohydrin in sewage samples have been selected. The limits of ECH detection have been determined by direct aqueous injection (DAI) into the chromatographic column and an analysis with the application of a flame ionization detector (FID), a mass spectrometry detector (MS), an electron capture detector (ECD) and atomic emission detection (AED) detectors. The method allows the determination of ECH in water samples at the concentration level of 0.1 mg l −1. Moreover, the developed methods of water samples preparation for chromatographic analysis using the following extraction methods: headspace (HS), stripping with adsorption on solid phase, liquid–liquid extraction (LLE), solid phase extraction (SPE) and solid phase microextraction (SPME) have been evaluated. The limits of ECH detection for each procedure with the application of gas chromatography (GC) combined with various detectors have been determined and their statistical evaluation has been presented. The SPME method allowed us to determine ECH in water samples at the concentration levels of 1.0 ng l −1. The results of studies on the choice of the selective methods allowing ECH analysis in sewage samples have been demonstrated. The applied SPME method was found to be a quick and effective technique to determine micro trace amounts of ECH in samples containing high amounts of various organic compounds.

Determination of epichlorohydrin by sulfite derivatization and ion chromatography: characterization of the sulfite derivatives by ion chromatography–mass spectrometry

This work is an upgrade of a previously developed method [J. Chromatogr. A 884 (2000) 251] for epichlorohydrin determination by ion chromatography (IC) and conductivity detection. Here, an ion chromatography–mass spectrometry (IC–MS) coupling has been employed for the separation and the identification of products of epichlorohydrin when reacted with the nucleophilic agent SO 3 2−. The high capacity column (IonPac AS11-HC) used for separation provided good resolution. This allowed evaluation of the IC behavior and mass spectrometric identification of epichlorohydrin sulfite derivatives. By using atmospheric pressure interfaces (ESI and APCI) the following species were tentatively identified: 2,3-dihydroxy-1-propanesulfonic, 2,3-epoxy-1-propanesulfonic, 1,3-dihydroxy-2-propanesulfonic and 3-oxetanesulfonic acids and 2-hydroxy-1,3-propanedisulfonic acid (or its isomer 3-hydroxy-1,2-propanedisulfonic acid). The study showed that chlorine atoms are displaced from epichlorohydrin during the reaction, while mass spectrometry confirmed that none of the products formed contains chlorine atoms.

Determination of epichlorohydrin by ion chromatography

In this work we developed a new method for epichlorohydrin determination with suppressed ion chromatography. The technique is based on a reaction between the analyte and sulfur(IV) to form a product with a terminal sulfonate group that can be analyzed by anion-exchange chromatography. The reaction conditions were optimized as a function of temperature, type and concentrations of reagents and pH. Due to the characteristics of the product formed, the columns used were an IonPac AS11 and AS11-HC with a NaOH eluent. The eluent concentration was optimized in order to achieve a complete separation of epichlorohydrin, chloride and nitrate ions, commonly occurring in drinking waters. In order to improve the detection limits, a preconcentration step, using reversed-phase materials, has been optimized. The method developed was suitable for epichlorohydrin determination in drinking water.

Gas chromatographic determination of epichlorohydrin in workplace atmospheres

A new method has been developed for the determination of trace amounts of epichlorohydrin in workplace atmospheres. Collection is peroormed in two bubblers in series both containing dichloromethane. Optimum conditions for sampling and analysis have been established. The lower limit of determination is 0.05 μg/mL with an RSD of ±5%.

Determination of epichlorohydrin in blood by gas chromatography and selected ion monitoring

Determination of epichlorohydrin in blood by gas chromatography and selected ion monitoring

The determination of epichlorohydrin in aqueous solutions in the presence of glycerin, monochlorohydrin and glycidol

Epichlorohydrin can be extracted from aqueous solutions containing glycerin, monochlorohydrin and glycidol into carbon tetrachloride and determined by infrared spectrophotometry. The high-frequency component of the complex band at a wavenumber 1274 cm–1 is used as the analytical band. A three-fold excess of carbon tetrachloride over the aqueous phase is necessary for the quantitative extraction. A cell thickness of up to 1 mm can be used; the concentration limit of the solute in the aqueous phase is then 0·3 per cent. v/v.