A method for quantitatively detecting perfluorooctanoic acid and its salts 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: 2011-12-07
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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  • A method for quantitatively detecting perfluorooctanoic acid and its salts in fluororubber
  • A method for quantitatively detecting perfluorooctanoic acid and its salts in fluororubber
  • A method for quantitatively detecting perfluorooctanoic acid and its salts in fluororubber

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Experimental program
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Effect test

Embodiment 1

[0022] 1. Instrument

[0023] American Agilent 6892-5973N gas spectrometer;

[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°C;

[0028] Vaporization chamber: 260°C;

[0029] Ion source: 150°C;

[0030] Quadrupole: 230°C;

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

[0032] SIM ions: Monitoring m / z 59, 69, 131 started 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 by the prepared PFOA standard.

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

[003...

Embodiment 2

[0043] Prepare a 1.00mg / L perfluorooctanoic acid aqueous solution, select CHROMABOND EASY and HR-P SPE cartridges from MN Company in Germany, and BESEP Carbon carbon black cartridges 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 1 ml / min, and the eluate was collected in a headspace bottle with a volume of 10 ml, purged with nitrogen, and concentrated to 2 ml. Add 0.2 g of analytically pure concentrated sulfuric acid to the concentrated eluate, seal it, place it in a water bath at 70°C for 60 min, and cool it down. Extract with 2ml of n-hexane, constant volume, analyze with GC / MS, carry out recovery determination, the result is shown in Table 2.

[0044] Table 2 SPE average recovery

[0045]

[0046] It can be seen from this example that better solid-phase extraction efficiency can be obtained by using CHROMABOND EASY solid-phase extraction cartridges. ...

Embodiment 3

[0048] Acetyl chloride and absolute ethanol were prepared as a derivatization reagent at a volume ratio of 1:20.

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

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

[0051] The derivatization efficiencies of two different acidification systems are shown in Table 3, and the trend diagrams are shown in image 3 shown.

[0052] Table 3 Derivatization efficiency of different derivatization systems

[0053]

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

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Abstract

The invention provides a method for quantitatively detecting perfluorooctanoic acid and its salts in fluororubber, comprising the steps of dissolving, settling, solid-phase extracting and derivatizing a sample, and then measuring the derivatized product by gas chromatography-mass spectrometry. Calculated on the basis of S / N=10, the quantitative detection limit of the method of the present invention is 0.04 mg / kg, and the correlation coefficient is 0.9991. The method of the invention has the advantages of fast sample processing, high extraction efficiency, simple derivatization steps, little 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 (Perfluorooctanoic Acid, PFOA) is a kind of surfactant with excellent performance, which has good foaming effect, and is widely used in fluorine industry, detergent, fire extinguishing agent and other fields. The European Commission - the European Parliament and the Council pointed out in the "Restriction on the Sales and Use of Perfluorooctane Sulfonate PFOS": PFOA may have similar hazards to PFOS, therefore, it is necessary to continue to conduct risk assessments and find relevant alternatives And consider developing measures to reduce its harm. [0003] Fluorine rubber is widely used in cutting-edge scientific and technological fields such as automobiles, aviation, missiles...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/72
Inventor 刘斌蔡醇洋
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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