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Method for quantitatively analyzing perfluorocarboxylic acid compounds through precolumn derivatization-gas chromatography

A gas chromatographic separation and perfluorocarboxylic acid technology, which is used in analytical materials, measuring devices, material separation, etc., can solve the problems of low detection cost, high detection limit and high detection cost, and achieve strong anti-interference ability and high precision. , the effect of low detection limit

Active Publication Date: 2017-01-04
ZHEJIANG WANLI UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

However, due to potential contamination problems in the LC system (such as fluoropolymer coating on the seal), this technique is difficult to obtain ideal blank analysis results, and the detection cost is high
Compared with liquid chromatography analysis, gas chromatography (GC) detection cost is lower and is more popular, but perfluorocarboxylic acid has polar groups, high boiling point, difficult to volatilize, cannot be directly determined by gas chromatography, must After the derivatization step is converted into volatile derivatives, Yang Yulin, Wang Hong et al. Gas chromatography analysis of PFOA in plasma, Chromatography, 2012,20(1):66-68 pointed out that methanol esterified PFOA is easy to gas Quantitative analysis of perfluorooctanoic acid in plasma by gas chromatography detection, this method is easy to operate, but the detection limit is high, it is difficult to detect low levels of perfluorooctanoic acid
The current derivatization methods have problems such as unstable derivatives, poor reproducibility, and high detection limits.
This series of problems has led to the lack of a set of more popular methods for analyzing PFCAs in water bodies.

Method used

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  • Method for quantitatively analyzing perfluorocarboxylic acid compounds through precolumn derivatization-gas chromatography
  • Method for quantitatively analyzing perfluorocarboxylic acid compounds through precolumn derivatization-gas chromatography
  • Method for quantitatively analyzing perfluorocarboxylic acid compounds through precolumn derivatization-gas chromatography

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Experimental program
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Effect test

Embodiment 1

[0028] Prepare standard curve

[0029] (1) Configuration of standard samples: Accurately measure nine kinds of samples, including chromatographically pure PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnA and PFDoA, and use n-hexane as the solvent to configure them into 0.001mol / L PFCAs standard stock solution. Accurately pipette 10mL of each of the nine PFCAs standard stock solutions into a 100mL volumetric flask, and dilute to 100mL with n-hexane to prepare a 0.0001mol / L mixed standard mother solution containing nine PFCAs. At the same time, prepare 0.0001mol / L 2,4-difluoroaniline (DFA) solution and N,N'-dicyclohexylcarbodiimide (DCC) solution with n-hexane. The prepared solutions above were stored at 4°C in the dark. Before use, accurately weigh 2 μL, 4 μL, 6 μL, 8 μL and 10 μL of PFCAS mixed standard mother solution, add 2,4-DFA solution and DCC solution, and the molar ratio of PFCAs mixed standard, 2,4-DFA, DCC It is 1:100:25. Use n-hexane to make up the volume in a ...

Embodiment 2

[0036] Detection of PFCAs Compound Type and Content in a Sewage Treatment Plant in Ningbo

[0037] (1) Sample preparation: collect water samples from a sewage treatment plant in Ningbo, filter the water samples to be tested through a 0.45 μm aqueous microporous membrane, adjust the pH value to 6 with 1mol / L NaOH, and then carry out solidification. phase extraction. Install the WAX ​​cartridge, and use 4mL methanol solution containing 0.5% ammonia water, 4mL methanol, and 4mL high-purity water to pass through the WAX ​​cartridge sequentially for activation and equilibrium. Pass the filtered water sample through the WAX ​​column at a flow rate of 5mL / min. After the sample passes through the column, wash the column with 4mL of 25mmol / L sodium acetate solution, and continue vacuuming to remove water; Rinse with methanol and 4mL methanol solution containing 0.5% ammonia, and collect in a stoppered glass graduated centrifuge tube. The eluent was blown off with high-purity nitrogen...

Embodiment 3

[0046] Determination of the types and contents of PFCAs in a surface water sample in Ningbo

[0047] (1) Sample preparation: Water samples were collected from a surface in Ningbo, filtered through a 0.45 μm water phase microporous membrane, and then adjusted to pH 6 with 1 mol / L NaOH, followed by solid-phase extraction. Install the WAX ​​column, and use 8mL of methanol solution containing 0.5% ammonia water, 8mL of methanol, and 8mL of high-purity water to pass through the WAX ​​column in sequence for activation and equilibrium. Pass the filtered water sample through the WAX ​​column at a flow rate of 8mL / min. After the sample passes through the column, wash the column with 8mL of 30mmol / L sodium acetate solution, and continue vacuuming to remove water; Rinse with methanol and 8mL methanol solution containing 0.5% ammonia, and collect in a stoppered glass graduated centrifuge tube. The eluent was blown off with high-purity nitrogen gas (50°C constant temperature water bath) t...

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Abstract

The invention relates to a method for quantitatively analyzing perfluorocarboxylic acid compounds through precolumn derivatization-gas chromatography. The determination method comprises the following steps that standard curves of nine perfluorocarboxylic acid compounds are formulated; a water sample is subjected to derivatization with 2,4-difluoroaniline and DCC after being subjected to solid-phase extraction pretreatment, after filtering is conducted through an organic microfiltration membrane, determination is conducted through gas chromatograph, and the variety and content of the perfluorocarboxylic acid compounds in the to-be-determined sample are obtained by contrasting the standard curves and regression equations. The correlation coefficients (R2) of the regression equations of the standard curves of the nine perfluorocarboxylic acid compounds are all larger than 0.99, the relative standard deviations (RSD) of the regression equations range from 1.3% to 7.5%, the accuracy is high, and the perfluorocarboxylic acid compounds in the sample are accurately and quantitatively analyzed through the linear regression equations on the basis of qualitative analysis. By means of the method, the nine perfluorocarboxylic acid compounds can be determined and analyzed simultaneously, and the method has the advantages of being high in precision and anti-jamming capability, low in detection limit and good in reproducibility.

Description

technical field [0001] The invention relates to a method for measuring perfluorocarboxylic acid compounds, in particular to a pre-column derivatization-gas chromatography quantitative analysis method for perfluorocarboxylic acid compounds, which belongs to the field of analytical chemistry. Background technique [0002] Perfluorochemicals (Perfluorochemicals, PFCs) are a series of artificially synthesized organic compounds in which all hydrogen atoms connected to carbon atoms are replaced by fluorine atoms. Because the structure contains a large number of C-F bonds, it can exist stably in the environment for a long time. PFCs have good chemical stability, thermal stability, surface activity, and both hydrophobic and oleophobic properties, and are widely used in various fields such as paper, textiles, leather, and carpets. Studies have shown that PFCs have multiple biotoxic effects such as developmental toxicity, immunotoxicity, and endocrine disruption; in addition, long-cha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/70G01N30/06G01N30/86
CPCG01N30/06G01N30/70G01N30/8634
Inventor 夏静芬唐力杨国靖袁凯王冬波胡煜钗罗薇楠沙昊雷
Owner ZHEJIANG WANLI UNIV
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