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Method for quantitatively detecting perfluorooctanoic acid and salts thereof in fluororubber

A technology for the quantitative detection of perfluorooctanoic acid, which is applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of expensive instruments, difficulty in widespread promotion, and high quantitative sensitivity of the SIM method, and achieves less interference from impurities, simple derivatization steps, and reproducible results good sex effect

Inactive Publication Date: 2010-07-07
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the LC / MS method is fast and sensitive to test trace PFOA, it is not easy to be widely used because of the expensive equipment; while the GC / MS method can not only confirm the composition of the sample, but also has a high quantitative sensitivity of the SIM method

Method used

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  • Method for quantitatively detecting perfluorooctanoic acid and salts thereof in fluororubber
  • Method for quantitatively detecting perfluorooctanoic acid and salts thereof in fluororubber
  • Method for quantitatively detecting perfluorooctanoic acid and salts thereof in fluororubber

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Experimental program
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Embodiment 1

[0022] 1. Instrument

[0023] American Agilent 6892-5973N GC / MS;

[0024] Porous vacuum extraction device with large volume sampling tube.

[0025] 2. Chromatographic conditions

[0026] Chromatographic column: DB-1ms 30m×0.32mm×0.10μm;

[0027] Column temperature: 100℃;

[0028] Vaporization chamber: 260℃;

[0029] Ion source: 150℃;

[0030] Quadrupole: 230℃;

[0031] Injection volume: 0.5μL, split ratio 1:10;

[0032] SIM ion: Start monitoring at m / z 59, 69, 131 at 11.8 minutes.

[0033] 3. Sample analysis

[0034] The quantitative method adopts the external standard curve method, and the external standard curve is measured with the preparation of perfluorooctanoic acid standard.

[0035] Prepare perfluorooctanoic acid standard solutions with mass concentrations of 0, 0.1, 0.5, 1.2, 3.5, and 6 mg / L, and perform GC / MS analysis after derivatization. The regression curve is as follows figure 1 As shown, the correlation coefficient is 0.9991, and the equation is as follows:

[0036] Y=24756X

[003...

Embodiment 2

[0043] Prepare 1.00mg / L perfluorooctanoic acid aqueous solution, choose CHROMABOND EASY and HR-P SPE cartridges and BESEP Carbon carbon black cartridges of Germany MN company respectively for solid phase extraction enrichment, dry the extraction cartridge with high-purity nitrogen, and use 5ml methanol The dried extraction column was eluted at a rate of 1ml / min. The eluent was collected in a headspace bottle with a volume of 10ml, and the eluent was purged with nitrogen and concentrated to 2ml. Add 0.2g analytically pure concentrated sulfuric acid to the concentrated eluate, seal it and place it in a 70°C water bath for derivatization for 60 minutes and cool. Extract with 2ml of n-hexane, make the volume constant, analyze by GC / MS, and measure the recovery rate. The results are shown in Table 2.

[0044] Table 2 Average recovery rate of solid phase extraction

[0045]

[0046] It can be seen from this example that the CHROMABOND EASY solid-phase extraction cartridge can obtain bet...

Embodiment 3

[0048] Acetyl chloride and absolute ethanol are formulated into a derivatization reagent in a volume ratio of 1:20.

[0049] Carry out 3 parallel experiments, add 10%wt analytically pure concentrated sulfuric acid to 2ml of 1.00mg / L PFOA methanol solution, seal it and place it in a 70°C water bath for derivatization for 60 minutes, and cool. Extract with 2ml n-hexane, make the volume constant, and analyze by GC / MS.

[0050] Carry out 3 parallel experiments, add 2ml acetyl chloride acidified methanol derivatization reagent to 2ml 1.00mg / L PFOA methanol solution, seal it and place it in a water bath at 70°C for 60min derivatization and cool. Extract with 2ml n-hexane, make the volume constant, and analyze by GC / MS.

[0051] The derivatization efficiency of the two different acidification systems is shown in Table 3, and the trend chart is shown as image 3 Shown.

[0052] Table 3 Derivatization efficiency of different derivatization systems

[0053]

[0054] It can be seen from Table 3 ...

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Abstract

The invention provides a method for quantitatively detecting perfluorooctanoic acid and salts thereof in fluororubber. The method comprises steps of dissolving, depositing, solid phase extracting and deriving a sample, and then carrying out gas phase chromatography-mass spectrography measurement on the derivative. Counted as S / N=10, the limit of quantitative detection in the method of the invention is 0.04mg / kg, and related coefficient is 0.9991. The method in the invention has the characteristics of fast sample processing, high extraction efficiency, simple derivation step, small impurity interference and high sensitivity.

Description

Technical field [0001] The invention relates to a method for quantitatively detecting perfluorooctanoic acid and its salts, in particular to a method for quantitatively detecting trace amounts of perfluorooctanoic acid and its salts in fluororubber. Background technique [0002] Perfluorooctanoic Acid (PFOA) is a surfactant with excellent performance and has good foaming effect. It is widely used in the fluorine industry, detergents, fire extinguishing agents and other fields. The Commission of the European Communities-European Parliament and the Council pointed out in the "Regarding Restrictions on the Sale and Use of Perfluorooctane Sulfonic Acid PFOS" that PFOA may have similar hazards to PFOS. Therefore, it is necessary to continue to conduct risk assessments and find relevant substitutes. And consider formulating measures to reduce its harm. [0003] Because fluorine rubber has good high temperature resistance, oil resistance and resistance to various chemicals, it is widely ...

Claims

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Application Information

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IPC IPC(8): G01N30/72
Inventor 刘斌蔡醇洋
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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