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Method for extracting and analyzing valence antimony in soil

An analysis method and extraction technology, which is applied in the field of quantitative analysis of trivalent antimony and pentavalent antimony by plasma mass spectrometry, can solve the problems of increasing operational complexity and pollution, and achieve flexible arrangements, high extraction rates, and parallelism Good results

Inactive Publication Date: 2022-04-12
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the main extractant is nitric acid, the complexity and pollution of the operation are increased

Method used

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  • Method for extracting and analyzing valence antimony in soil
  • Method for extracting and analyzing valence antimony in soil
  • Method for extracting and analyzing valence antimony in soil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] refer to figure 1 According to the procedure provided, the road soil of a section of Hutai Road in Shanghai was selected for the determination of valence antimony content.

[0041] Do the soil treatment first. Remove gravel particles, animal and plant residues, plastic bags and other sundries in the soil samples and then freeze-dry them to prevent the loss of volatile Sb; sieve; the second time is fine grinding, using the quartering method to select part of the samples from the first grinding for secondary grinding, and passing through a 100-mesh sieve to obtain the Hutai Road soil sample.

[0042] Weigh 1.5g of the treated soil sample in a 50mL centrifuge tube, add 15mL of pH 2 concentration of 400mmol L -1 citric acid solution, put the centrifuge tube into a constant temperature water bath shaker at 80°C, oscillate at a constant temperature for 2 hours at a vibration frequency of 300 r·min-1, and extract once; -1 After centrifugation for 30 min, pass through a 0.22...

Embodiment 2

[0048] Based on the method established by the invention, the valence state antimony concentration level of the soil on the main traffic road is monitored. According to the comprehensive analysis of road conditions, typical roads in the central urban area of ​​the inner, middle and outer rings in Shanghai were selected to sample the soil on both sides of the road.

[0049] A total of 16 sampling points were set in the 3 research sections, including 6 in the inner ring, 5 in the middle ring and 5 in the outer ring. Collect surface soil samples, seal them in ziplock bags, and freeze-dry them as soon as possible after returning to the laboratory. take advantage of figure 1 The process provided and the valence state extraction and analysis method established are used to analyze the valence state of road soil Sb.

[0050] Soil pretreatment is carried out first. The debris in the soil sample was removed and then freeze-dried to prevent the loss of volatile Sb; then two grindings w...

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Abstract

The invention provides a method for extracting and analyzing valence antimony in soil, which comprises the following steps: (1) pretreating a soil sample to facilitate subsequent extraction and analysis; (2) extracting trivalent antimony and pentavalent antimony from the pretreated soil sample by using an extracting agent; (3) purifying and storing the extract liquor; and (4) carrying out chromatographic column separation on the extract, and carrying out quantitative analysis in an inductively coupled plasma mass spectrometer. The method is reasonable in design, clear in step, accurate in result, good in reproducibility, suitable for extraction and quantitative analysis of trivalent antimony and pentavalent antimony in various soils, high in sensitivity and good in accuracy. The distribution of the valence antimony in the soil is measured through the method, the occurrence, migration and transformation characteristics of Sb in the soil can be known, the environmental soil Sb pollution condition can be evaluated, the ecological risk caused by Sb to the environment can be evaluated, and a theoretical basis is provided for formulating urban environmental policies and standards.

Description

technical field [0001] The invention relates to the technical field of environmental monitoring, in particular to extracting trivalent antimony and pentavalent antimony in soil by using an extractant, separating them with a chromatographic column, and finally using inductively coupled plasma mass spectrometry to quantitatively analyze the trivalent antimony and pentavalent antimony content method. Background technique [0002] Antimony (Sb) is a heavy metal element in Group VA of the fifth cycle, and its properties are similar to arsenic. Sb is widely distributed in the environment, and the Sb content in the environment has increased significantly in the past few hundred years, indicating that Sb pollution has affected people's living environment. [0003] Sb has certain toxicity to organisms, and has certain toxic effects on immune, nervous and developmental systems. Similar to many elements, the toxicity of antimony and its compounds depends on the form in which they exi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/34G01N27/626G01N1/28
Inventor 陈皓陈玲刘硕勋颜耕周磊杨超
Owner TONGJI UNIV
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