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Pretreatment and quantitative analysis method for linear alkylbenzene in soil/sediment

A technology for quantitative analysis of straight-chain alkylbenzene, applied in the direction of analyzing materials, measuring devices, material separation, etc., can solve problems such as easy blockage of pipelines, complicated instrument operation, degradation of target pollutants, etc., achieve simple and easy operation, and save solvents , high recycling efficiency

Pending Publication Date: 2020-03-27
广电计量检测(合肥)有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the eluent is concentrated and fixed to volume, it is quantified by GC-MS. The accelerated solvent extraction instrument is expensive, the operation of the instrument is complicated, and the pipeline is easy to block; because the extraction is carried out under high temperature and high pressure, it is easy to cause the degradation of target pollutants, and it is not suitable for containing For samples with high organic carbon or fat, the silica gel-alumina multi-layer chromatography column is used for purification, the filling material is complicated, the solvent consumption is large, and the recovery efficiency is not high. Therefore, it is necessary to establish a simple, fast and low-consumption Suitable for LABs pretreatment method and instrument quantitative method in soil / sediment

Method used

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  • Pretreatment and quantitative analysis method for linear alkylbenzene in soil/sediment
  • Pretreatment and quantitative analysis method for linear alkylbenzene in soil/sediment
  • Pretreatment and quantitative analysis method for linear alkylbenzene in soil/sediment

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1 A kind of quantitative analysis method of linear alkylbenzene in soil or sediment

[0036] (1) Preparation of standard samples

[0037] Standard solution: decylbenzene, undecylbenzene, dodecylbenzene, tridecylbenzene (purity respectively 99.8%, 99.2%, 99.3%, 99.5%, mass 100mg), commercially available certified standard Substance, AccuStandard.

[0038] Mix 4 kinds of linear alkylbenzene standard solutions with n-hexane to prepare a 10000 mg / L mixed standard stock solution, dilute the standard stock solution, and prepare a standard curve series concentration, the concentration of each point is 5, 50, 100, 500, 1000, 5000μg / L.

[0039] (2) Determination of moisture

[0040] The determination of dry matter content of soil samples is carried out in accordance with HJ613, and the determination of moisture content of sediment samples is carried out in accordance with GB17378.5.

[0041] (3) Sample preparation

[0042] Place the collected soil or sediment sam...

Embodiment 2

[0065] Example 2 Optimization of purification experimental conditions

[0066] In order to optimize the experimental conditions of the purification process, under the premise of ensuring the best recovery efficiency, the elution solvent can be saved, a total of 4 groups of elution schemes with different volumes are set up:

[0067] Scheme 1: The standard solution containing 1000 ppb in 1 mL of n-hexane was transferred to a 3.0 g silica gel chromatography column. The elution conditions were as follows: firstly add 5 mL of n-hexane to elute the chromatography column and discard it; then add 5 mL of n-hexane to elute, The liquid fraction 1 was collected; 5 mL of n-hexane was added to rinse, and the fraction 2 was collected; and 5 mL of n-hexane was added to rinse, and the fraction 3 was collected. Concentrated on-board measurement.

[0068] Scheme 2: Transfer the standard solution containing 1000ppb in 1 mL of n-hexane to a 3.0 g silica gel column, add 5 mL of n-hexane to rinse,...

Embodiment 3

[0072] Example 3 Analysis of blank and blank spiked samples

[0073] Take quartz sand for blank experiment and blank addition experiment respectively, and the blank addition amount is 1000ppb. Extraction, concentration, purification, concentration and constant volume and instrumental analysis are carried out through the step distribution of Example 1, wherein the purification conditions are selected as the final optimized conditions of Example 2. The results of 3 blank experiments and 13 blank addition experiments are as follows figure 2 As shown, LABs were detected in all three blank samples, and the detected concentrations of decylbenzene, undecylbenzene, dodecylbenzene and tridecylbenzene were 4.8±1.2, 3.3±0.4, 2.0 ±0.2 and 3.5±0.4ppb ( figure 2 ), reflecting that the experimental blank of this experimental process is low, and the target pollutants introduced are less, which provides the ability for the analysis of actual samples in the later stage.

[0074] The result...

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Abstract

The invention discloses a sample pretreatment and quantitative analysis method for linear alkylbenzene in soil / sediment. The sample pretreatment comprises the following steps: S1, taking to-be-detected soil / sediment, wrapping the to-be-detected soil / sediment with a glass fiber filter membrane, and putting the wrapped to-be-detected soil / sediment into a sleeve of an automatic soxhlet extractor; S2,adding a dichloromethane solvent into a measuring cup of an automatic Soxhlet extractor, boiling for 60 minutes, leaching for 60 minutes, recovering the solvent for 10 minutes, finishing extraction,collecting an extracting solution, removing water, and concentrating, wherein the mass volume ratio of the to-be-detected soil / sediment to dichloromethane is 10g: 80mL; and S3, concentrating the extracting solution, exchanging a solvent, fixing the volume to 1mL, purifying the concentrated extracting solution by virtue of a chromatographic column, filling the purifying column with 3.0 g of silicagel, leaching the chromatographic column by virtue of 25mL of normal hexane, collecting leacheate, concentrating, fixing the volume to 1.0 mL, and performing subsequent quantitative analysis. The invention establishes an automatic Soxhlet extraction-silica gel purification-gas chromatography-mass spectrometry quantitative method which can be used for quantitative analysis of LABs in soil. Comparedwith the previously reported analysis method, the method is simple and easy to operate, saves the solvent, and is suitable for batch soil sample analysis in actual analysis and detection.

Description

technical field [0001] The invention relates to the technical field of detection of environmental molecular markers, and more specifically, to a method for pretreatment and quantitative analysis of linear alkylbenzenes in soil / sediment. Background technique [0002] LABs are alkane derivatives in which one hydrogen atom on the carbon chain of n-alkanes containing 10 to 14 carbons is substituted by a phenyl group. The different positions of the phenyl substitution form a series of homologues, collectively referred to as linear alkylbenzenes, which are mainly used for industrial synthesis of long chains. Paraffin Sulfonate (LAS) - A major ingredient in anionic detergents that has been widely used since the 1960's. Since there will be a small amount of LABs left in LAS-type detergents during the synthesis process, LABs will enter the environment with the use and subsequent disposal of this type of detergent in daily life, and are usually used as molecular markers for domestic s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 王继忠张席席张迪黄贵凤
Owner 广电计量检测(合肥)有限公司
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