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Headspace gas chromatography-mass spectrometry determination method of 2-chloroethanol in water

A technique of headspace gas chromatography and a determination method, which is applied in the field of 2-chloroethanol headspace gas chromatography-mass spectrometry in water, can solve the problems of insufficient sensitivity and low response value of 2-chloroethanol, and achieve good specificity , low detection limit and wide application range

Inactive Publication Date: 2018-08-21
ZHEJIANG QICAI ECO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the detection of 2-chloroethanol by simple gas chromatography still has the disadvantages of low response value and insufficient sensitivity.

Method used

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  • Headspace gas chromatography-mass spectrometry determination method of 2-chloroethanol in water
  • Headspace gas chromatography-mass spectrometry determination method of 2-chloroethanol in water
  • Headspace gas chromatography-mass spectrometry determination method of 2-chloroethanol in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1 This embodiment illustrates detection range and detection limit

[0037] Determination of standard curve:

[0038] Weigh 4 g of sodium chloride into each headspace vial.

[0039] Weigh 0.9950g of 2-chloroethanol, dilute to 100mL with deionized water, shake well to prepare a standard stock solution with a concentration of 9950mg / L, then take 10mL of the stock solution and dilute to 100mL with deionized water to prepare Get 995.0mg / L standard solution, and then dilute with deionized water 1000, 200, 100, 20, 10, 2 times respectively to obtain concentrations of 0.995mg / L, 4.975mg / L, 9.95mg / L, 49.75mg / L, 99.75mg / L, and 497.5mg / L standard solutions, respectively accurately sample 10mL into headspace bottles containing sodium chloride, and shake for a while to fully dissolve sodium chloride.

[0040] Detect standard samples of each concentration to obtain the SIM total ion chromatogram of 2-chloroethanol in water, see figure 1 ; SCAN total ion chromatogram of...

Embodiment 2

[0043] Embodiment 2 This embodiment illustrates the accuracy of 2-chloroethanol content determination

[0044] Standard curve determination is the same as in Example 1.

[0045] Dilute the 995.0mg / L standard solution by 50 times to obtain a calibration solution with an actual concentration of 19.9mg / L. Take 4 samples respectively, and accurately measure 10mL of water samples into headspace bottles containing 4g of sodium chloride. After shaking for a while, analysis was carried out, and the peak areas of quantified ion 31 were 281309, 281294, 281300, 281289, respectively, and the average value 281298 was substituted into the above-mentioned standard curve, and the concentration of 2-chloroethanol was 19.8997 mg / L, calculated to obtain the actual recovery The rate is 100.0%, indicating that the method of the present invention is accurate and reliable.

Embodiment 3

[0046] Embodiment 3 This embodiment illustrates the mensuration of 2-chloroethanol content in the para-ester production waste water

[0047]Standard curve determination is the same as in Example 1.

[0048] First, the para-ester production wastewater was diluted 1000 times with deionized water, and 10 mL of water sample was accurately measured into a headspace bottle containing 4 g of sodium chloride, and analyzed after shaking for a while. Obtain the mass spectrum of the sample at 2.740min as Figure 5 , it can be seen that the peak at about 2.740min is the peak of 2-chloroethanol.

[0049] The peak area of ​​quantitative ion 31 is 342854, which is brought into the above standard curve to obtain the concentration of 2-chloroethanol in the sample as 24.15mg / L, multiplied by the dilution factor of the sample, and the concentration of 2-chloroethanol in the original water sample can be obtained as 24150mg / L .

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Abstract

The invention discloses a headspace gas chromatography-mass spectrometry determination method of 2-chloroethanol in water. The headspace gas chromatography-mass spectrometry determination method comprises the following steps: 1), preparing a sample liquid: adding a water ample and sodium chloride into a headspace bottle, and sealing; 2), preparing a standard sample liquid: adding 2-chloroethanol with different concentrations and sodium chloride into headspace bottles, and sealing; 3), drawing a standard curve: analyzing the standard sample liquid prepared in the step 2) by headspace gas chromatography-mass spectrometry, and drawing the standard curve by using the concentration as an abscissa and the peak area as an ordinate; 4), detecting the sample liquid: analyzing the sample liquid by headspace gas chromatography-mass spectrometry to obtain the peak area, and substituting the peak area into a regression equation of the standard curve to obtain the concentration of the 2-chloroethanol in water. The determination method has the advantages of a large response value, a short detection time, good specificity, high sensitivity and the like.

Description

technical field [0001] The invention belongs to the technical field of water treatment, in particular to a method for determining 2-chloroethanol headspace gas chromatography-mass spectrometry in water. Background technique [0002] 2-Chloroethanol is a colorless or pale yellow liquid with slight ether fragrance; molecular weight is 80.52; vapor pressure is 1.33kPa / 30.3°C; flash point is 60°C; melting point is -63°C; boiling point is 129°C; soluble in water , acid, ether; relative density (water = 1) is 1.20; relative density (air = 1) is 2.78; it is an important organic solvent and organic synthesis raw material, often used in the manufacture of ethylene glycol, ethylene oxide, and medicine, Synthesis of dyes and pesticides, etc. [0003] 2-Chloroethanol reacts with sodium sulfide to obtain thiodiethylene glycol, which is a printing and dyeing solvent for textiles, and also a plasticizer for vat dyes and polyalkylene dichlorides. 2-Chloroethanol can be used to synthesize ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 付玲玲张清义宋亿文杨强杨莹莹
Owner ZHEJIANG QICAI ECO TECH CO LTD
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