ABSTRACT
We report on a headspace gas chromatographic method for determining the content of 3-chloro-1,2-propanediol in polyamideamine epichlorohydrin resin solution. It was based on quantitatively converting 3-chloro-1,2-propanediol to formaldehyde by periodate oxidation in a closed headspace sample vial at a room temperature for 10 min, and then to methanol by borohydride reduction at 90°C for 40 min followed by the headspace gas chromatographic measurement. The results showed that the present method has an excellent measurement precision (relative standard deviation < 2.60%) and accuracy (recoveries from 96.4-102%) in 3-chloro-1,2-propanediol analysis. The limit of quantitation was 0.031 mg/mL. It is simple and suitable for determining the 3-chloro-1,2-propanediol content in polyamideamine epichlorohydrin resin solution.
ABSTRACT
This paper reports on an ionic-liquid assisted headspace gas chromatographic (HS-GC) for the determination of the content of alkyl ketene dimer (AKD) in its latex samples, in which the GC system was equipped with a thermal conductivity detector (TCD). The method was based on the AKD hydrolysis conducted in 1-butyl-3-methylimidazolium chloride (ionic-liquid) added medium at 100°C for 10min in a closed headspace sample vial, and the measured CO2 (the resulting product of the hydrolysis) by HS-GC. The results showed that the present method has a good measurement precision (RSD <2.3%) and accuracy (recoveries from 96 - 105%), and the limit of quantitation (LOQ) is 0.9%. The present method is very suitable to be used for the routine check of AKD content in its latex sample in mill applications. The study also showed that the content of AKD in the tested commercial latex samples were in the range of 3.5-12%.
Subject(s)
Chemistry Techniques, Analytical/methods , Chromatography, Gas , Ethylenes/analysis , Ketones/analysis , Latex/chemistry , Limit of Detection , Reproducibility of ResultsABSTRACT
This study demonstrated a headspace gas chromatographic (HS-GC) method for the determination of residual epichlorohydrin (ECH) and the by-product 1,3-dichloro-2-propanol (DCP) in polyamine epichlorohydrin (PAE) solution. It was based on the vapor-liquid phase equilibrium of these analytes at 60°C for 30min in a closed headspace sample vial before GC measurement. It was found that matrix of the PAE solution had the effect on the headspace equilibrium of these species and therefore a standard addition must be applied in the method validation. The results showed that the present method has a good measurement precision (RSD <2.90%) and accuracy (recoveries from 93.6 to 105%), and the limit of quantitation (LOQ) is 3.75mg/L for ECH and 0.8g/L for DCP. The present method is suitable to be used for analyzing the chlorinated volatile organic compounds in the commercial PAE resin solutions.
Subject(s)
Chromatography, Gas , Epichlorohydrin/analysis , Polyamines/chemistry , Volatile Organic Compounds/analysis , Limit of Detection , Solutions/chemistry , alpha-Chlorohydrin/analogs & derivatives , alpha-Chlorohydrin/analysisABSTRACT
The current national standard method GB/T 27741-2011, i.e., "quantitative determination of migratable fluorescent whitening agents-UV spectroscopy", overestimates the migratable fluorescent whitening agents (FWA) in the paper based products because of the spectral interference of the leached lignin from the cellulose fibers. To minimize such interference, a spectroscopic method based on dual-wavelength (305 and 348 nm) measurement was proposed. It was observed that the dual-wavelength spectroscopy can effectively subtract the spectral absorption contributed by the leached lignin in the extraction medium, thus more accurately determination of migratable FWA can be performed. The results showed that the present method has a relative standard deviation of 2.17%, the quantitative detection limit of 16.9 mg x kg(-1), and recovery of 98%-103%. Compared with the current alternative standard-HPLC method, the present method possesses advantages of low operation and maintenance costs, simple, and practical in application. Therefore, it is more suitable for the rapid determination of migratable FWA in the product quality control in the production process and sample examination in the commercial market.
