Instrumental analysis pretreatment method of enriching perfluorinated carboxylic acid compound

A perfluorocarboxylic acid and instrumental analysis technology, applied in the field of analysis and detection, can solve problems such as large amount of organic reagents, influence on analysis results, and hazards to operators, and achieve the effects of less sample loss, high enrichment multiples, and improved accuracy

Active Publication Date: 2017-09-08
ZHEJIANG WANLI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional sample pretreatment techniques, such as Soxhlet extraction, solvent extraction, centrifugation, distillation, chromatography, precipitation, etc., not only have a low enrichment factor, but also use a large amount of toxic organic reagents, and the operation is time-consuming and laborious.
Long-term exposure will not only bring harm to the operator, but also have a certain impact on the environment
In addition, in the extraction process, there will inevitably be phenomena such as emulsification that affect the separation effect, thereby affecting the analysis results. Therefore, the development of simple, fast, efficient, and less-solvent or solvent-free sample pretreatment methods has become an important part of the development of analytical chemistry. the trend of

Method used

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  • Instrumental analysis pretreatment method of enriching perfluorinated carboxylic acid compound
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  • Instrumental analysis pretreatment method of enriching perfluorinated carboxylic acid compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Drawing of standard curve

[0047] (1) Configuration of standard solution: Accurately weigh the appropriate amount of nine kinds of samples including chromatographically pure PFBA, PFPeA, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnA and PFDoA, dissolve them in n-hexane, and configure them into 0.001mol / L PFCA standard stock solution. Accurately pipette 10 mL each of the above nine PFCAs standard stock solutions, mix them into a 100 mL volumetric flask, and dilute to 100 mL with n-hexane to prepare a 0.0001 mol / L mixed standard mother solution containing nine PFCAs.

[0048] At the same time, take DFA and DCC and dissolve them in n-hexane, respectively, to prepare 0.001mol / L DFA stock solution and DCC stock solution, respectively pipette the DFA stock solution and DCC stock solution, place them in a 100mL volumetric flask, and dissolve them with n-hexane Dilute to 0.0001mol / L DFA solution and DCC solution. The prepared solutions above were stored at 4°C in the dark.

[0049]...

Embodiment 2

[0058] Detection of PFCAs Compound Type and Content in a Sewage Treatment Plant in Ningbo

[0059] Water samples were collected from a sewage treatment plant in Ningbo. After the water samples to be tested were filtered through a 0.45 μm aqueous microporous membrane, derivatization, magnetic separation and other pre-treatment processes were performed to obtain derivatives that could be detected on the machine, and then Perform chromatographic assays. The above-mentioned pretreatment and chromatographic determination were carried out according to the method of Example 1.

[0060] See Table 2 for the determination results of the type and content of PFCA in the sample and the recovery calculated after the addition of the standard.

[0061] Table 2: PFCA determination and standard addition recovery results in the water samples of Example 2

[0062]

Embodiment 3

[0064] Collect water sample from the same sewage treatment plant in embodiment 2, and embodiment 2 difference is:

[0065] Standard solution, DFA solution and DCC solution were prepared with ethyl acetate.

[0066] The process of activating the magnetic graphene oxide material is to add 0.15g of the magnetic graphene oxide material and 15ml of ammonia-methanol solution into a conical flask filled with 100mL of high-purity water, and ultrasonically disperse it to obtain the activated magnetic graphene oxide material. , the frequency of ultrasonic dispersion is 26kHz, the power is 5kw, and the time is 1min. .

[0067] When the sample is derivatized, the volume ratio of standard solution, DFA solution, DCC solution and magnetic graphene oxide material is 1:50:5:90, and the Erlenmeyer flask is fixed on the oscillator to fully shake for 20min at a temperature of 18°C. Derivatization process.

[0068] The desorbent added during vortex desorption is ethanol, the vortex oscillation...

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Abstract

The invention relates to an instrumental analysis pretreatment method of enriching a perfluorinated carboxylic acid compound and belongs to the technical field of analysis and detection. The pretreatment method comprises the steps of preparing a DFA solution, a DCC solution and a standard solution, activating a magnetic graphite oxide material, performing incoming magnetic separation after derivatization treatment, blow-drying and dissolving collected desorption liquid, and then performing online detection. The treatment method is simple and quick, has good selectivity for the perfluorinated carboxylic acid compound, is high in enrichment time and reusable, can reduce sample loss and improves detection accuracy.

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and in particular relates to an instrument analysis pretreatment method for enriching perfluorocarboxylic acid compounds. 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-chain PFCs also have a strong tendency to bioaccumulate and biomagnify along t...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/08
CPCG01N30/02G01N30/08
Inventor 唐力杨国靖夏静芬袁凯姚文怡吴亦馨胡煜钗张妮罗浩叶茂烨
Owner ZHEJIANG WANLI UNIV
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