Method for detecting normal hexane and cyclohexanone in retired plot soil

A detection method, the technology of n-hexane, applied in the field of detection of n-hexane and cyclohexanone in soil, can solve the problems of lack of detection methods for n-hexane and cyclohexanone, and achieve low detection limit, high extraction efficiency and precision and accurate and reliable results

Active Publication Date: 2022-03-18
杭州中一检测研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, purge and trap-gas chromatography-mass spectrometry did not detect n-hexane and cyclohexanone in the soil, so there is a lack of a method for the detection of n-hexane and cyclohexanone in the soil of decommissioned plots

Method used

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  • Method for detecting normal hexane and cyclohexanone in retired plot soil
  • Method for detecting normal hexane and cyclohexanone in retired plot soil
  • Method for detecting normal hexane and cyclohexanone in retired plot soil

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Experimental program
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Effect test

Embodiment 1

[0047] see Figure 1-9 , a kind of detection method of n-hexane and cyclohexanone in decommissioned plot soil, comprises the following steps:

[0048] S1. Sample collection: use HC-Z450 drilling rig special soil sampling and drilling equipment to collect soil samples from a decommissioned plot, use a non-disturbance sampler to collect about 5.00g of soil samples, put them in a 40mL brown purge bottle, and add Magnetic stirring bar, sealed bottle cap;

[0049] Among them, the disturbance of soil samples should be minimized during the collection process, the samples should not be homogenized, and mixed samples should not be collected;

[0050] S2. Sample analysis: The collected samples are transported and stored in a frozen blue ice incubator, transferred to the laboratory, placed in a purge and trap device, and the positive self in the soil is extracted under the best purge and trap conditions. Alkanes and cyclohexanone, the content of n-hexane and cyclohexanone in the soil o...

Embodiment 2

[0089] Purge-and-trap-gas chromatography-mass spectrometry experiments were performed under different purge-and-trap conditions by the control variable method to verify the optimal purge-and-trap conditions:

[0090] Take the solutions with mass concentrations (n-hexane: 250 μg / L; cyclohexanone: 2000 μg / L; toluene-d8: 200 μg / L; chlorobenzene-d5: 50 μg / L) through the purge and trap instrument and gas chromatography-mass spectrometry Injection analysis of the hyphenated instrument, its ion flow diagram is obtained in the full scan mode to verify the feasibility of the experimental results under different purge and trap conditions;

[0091] see Figure 4 , is the total ion current chromatogram of normal hexane, cyclohexanone, toluene-d8 and chlorobenzene-d5 under standard solution sample test;

[0092] When implementing step 3, the following data can be used for the purge and trap conditions under the control variable method:

[0093] Fix other purge and trap conditions unchang...

Embodiment 3

[0109] Preliminary investigation and environmental testing on the soil pollution status of decommissioned plots of a Zhejiang Biotechnology Co., Ltd. involved the use of n-hexane and cyclohexanone in the raw materials of the company's products. The detection method is very necessary, including the following steps:

[0110] S1. Sample collection: use HC-Z450 drilling rig special soil sampling and drilling equipment to collect soil samples S24-1 (0-0.5m) and S15-1 (0-0.5m) of the decommissioned plot. Minimize the disturbance of the soil samples, collect about 5.00g soil samples with a non-disturbance sampler, do not homogenize the samples, do not collect mixed samples, collect 6 parallel samples of the same point sample, and place them in a 40mL brown purge In the bottle, add a magnetic stir bar and seal the bottle cap;

[0111] Among them, for high-concentration samples (preliminary estimate of the content of the analyte greater than 1000μg / kg, the data comes from the photoion...

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Abstract

The invention discloses a method for detecting normal hexane and cyclohexanone in retired plot soil. The method comprises the following steps: S1, collecting a sample; s2, extracting and analyzing n-hexane and cyclohexanone in the soil under the optimal purging and trapping condition; s3, under the experimental conditions of the step S2, obtaining a linear regression equation and correlation coefficients of normal hexane, cyclohexanone and toluene-d8, and determining the detection limit of the normal hexane and cyclohexanone method; and S4, under the experimental conditions of the step S2, performing precision and correctness tests on the labeled sample. According to the method, the detection limits of the method for determining the n-hexane and the cyclohexanone in the soil are 1.2 mu g / kg and 13.0 mu g / kg respectively, the standard recovery ranges of actual samples are 75.7%-96.8% and 81.5%-123% respectively, and the relative standard deviations are 5.8%-7.6% and 3.8%-4.7% respectively; and S5, under the experimental conditions of the steps S1 to S4, performing whole-process step parallel determination on the soil sample of the retired plot for 6 times, and enabling the relative standard deviations of repeated determination results to be less than 10%. The method has the advantages of being environmentally friendly, free of pollution, high in extraction efficiency, low in detection limit, good in repeatability, reliable in precision and accuracy and the like, and can be suitable for analysis of determination of n-hexane and cyclohexanone in retired plot soil.

Description

technical field [0001] The invention relates to the technical field of detection of n-hexane and cyclohexanone in soil, in particular to a detection method for n-hexane and cyclohexanone in the soil of decommissioned plots. Background technique [0002] n-Hexane is a colorless liquid with a faint special smell. It is volatile, almost insoluble in water, and easily soluble in chloroform, ether, and ethanol. It is used as an important organic solvent, including vegetable oil extraction solvent, propylene polymerization solvent, rubber and Paint solvents, pigment thinners, etc. Cyclohexanone is a clear, colorless liquid with an earthy, and when it contains traces of phenol, a minty odour. The impurity is light yellow, and with the storage time, it can form impurities and develop color, from water white to grayish yellow, with a strong pungent odor. In industry, it is mainly used as raw material and solvent for organic synthesis, for example, it can dissolve nitrocellulose, pa...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): G01N30/02G01N30/06G01N1/08G01N1/38
CPCG01N30/02G01N30/06G01N1/08G01N1/38
Inventor王瑞包苏英翁咪娜王利蔡阳勇来航桦杨毅唐山凤
Owner杭州中一检测研究院有限公司