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Analysis Of Alkyl Sulfonate By High Performance Liquid Chromatography With Indirect Ultraviolet Detection

Posted on:2018-06-15Degree:MasterType:Thesis
Country:ChinaCandidate:D ZhaoFull Text:PDF
GTID:2321330542483428Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
An investigation into analysis of alkyl sulfonate without ultraviolet absorption by high performance liquid chromatography / indirect UV detection was carried out.The purpose is to develop simple,rapid and accurate analysis method to detect alkyl sulfonate,and study the factors that influence the separation mechanism.The research contents mainly include the following three parts:Firstly,a method was established for the determination of three kinds of alkyl sulfonates without ultraviolet absorption using 4-aminophenol hydrochloride as the background ultraviolet absorption reagent by high performance liquid chromatography with indirect ultraviolet detection Chromatographic separation was performed on a reversed-phase C18 column using 4-aminophenol hydrochloride-acetonitrile as mobile phases.The separation and detection of three alkyl sulfonates were realized.The effect of the ultraviolet absorption reagent,organic solvent,4-aminophenol hydrochloride concentration,detection wavelength and other factors on the separation and determination of alkyl sulfonates were investigated.The retention rules of alkyl sulfonates were discussed and the chromatographic conditions were optimized.The optimized chromatographic conditions for the determination of three kinds of alkyl sulfonates were as follow: 0.7 mmol/L of 4-aminophenol hydrochloride-acetonitrile(70:30)as mobile phase,column temperature 30°C,flow rate 1 m L/min,detection wavelength 210 nm.Under these condition,three kinds of alkyl sulfonate can be completely detected and separated in 15 min.The linear range of standard curve of octane-1-sulfonate,decane-1-sulfonate and twelve alkyl sulfonate were 0.43-100 mg/L,0.40-100 mg/L and 3.23-100 mg/L.The linear coefficients were all above 0.999.The detection limits were 0.13mg/L,0.12mg/L,0.97mg/L.The method was applied to the determination of 84 disinfectant,and the recovery after spiking was more than 91%.The method was accurate and reliable,and could meet the requirement of quantitative analysis.Secondly,the influence of different classes of background ultraviolet absorption reagents on the determination of alkyl benzene sulfonate without ultraviolet absorption was studied.In this study,two kinds of alkyl sulfonates were separated using background ultraviolet absorption reagents-organic solvent as mobile phase on reversed-phase C18 column by high performance liquid chromatography with indirect ultraviolet detection.The separation rule and mechanism of different background ultraviolet absorption reagent in separation and determination of alkyl sulfonates were investigate.The experimental results show that the peak of sample was positive when alkyl sulfonate was detected using by the cationic,and the peak of sample was inverted when the anionic and alkyl sulfonate was detected using by the anionic or the amphiprotic.The separation mechanism is followed by ion pair separation mode,ion exchange model and equilibrium disturbance model.Finally obtained by comparison,it was concluded that the chromatogram was better for the determination of alkyl sulfonate using by the cationic,and the separation effect using imidazole ionic liquid was the best.Finally,a method of solid phase extraction and high performance liquid chromatography with indirect ultraviolet detection was developed for the determination of alkyl sulfonates.In this experiment,a strong anion exchange column for was used for separation and enrichment.The taget was eluted by 0.02mmol/L hydrochloric acid-methanol(10:90,v/v),and then the eluent can be chromatographic analysis.The final selection of chromatographic detection conditions: reversed-phase C18 column,0.5 mmol/L 1-ethyl 3-methyl imidazole tetrafluoroborate aqueous solution-methanol(65:35,v/v)as mobile phase,detection wavelength 210 nm,flow rate 1 m L/min,indirect ultraviolet detection,column temperature 30°C,sample volume 20 L.In range of 0.16-100mg/L,0.50-100 mg/L,the correlation coefficient of the linear regression equation was good.The detection limit was 0.047 mg/L,0.15 mg/L.The relative standard deviations were all below 2.5%.The method is simple,low cost and can meet the requirements of quantitative analysis of alkyl sulfonates.
Keywords/Search Tags:high performance liquid chromatography, ionic liquids, indirect ultraviolet detection, solid phase extraction, alkyl sulfonate
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