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Pretreatment method for heavy metal element detection in solid sample and application of pretreatment method

A heavy metal and sample technology, which is applied in the pretreatment field of heavy metal element detection in solid samples, can solve the problems of long sample digestion time, general accuracy and reproducibility of analysis results, large residual rate, etc. Sample loss, good reproducibility effect

Inactive Publication Date: 2014-01-29
SOUTH CHINA INST OF ENVIRONMENTAL SCI MEP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above method has many steps, the sample digestion time is long, the residual rate is large, and the accuracy and reproducibility of the analysis results are average.

Method used

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  • Pretreatment method for heavy metal element detection in solid sample and application of pretreatment method
  • Pretreatment method for heavy metal element detection in solid sample and application of pretreatment method
  • Pretreatment method for heavy metal element detection in solid sample and application of pretreatment method

Examples

Experimental program
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Effect test

Embodiment 1

[0036] (1) Pre-digestion stage: Weigh 0.2000g soil sample (standard material for soil composition analysis GBW07410) into a 50mL polytetrafluoroethylene crucible; add 10mL nitric acid (excellent grade, mass concentration 65%) into the polytetrafluoroethylene crucible , covered, and digested on an electric heating plate in a fume hood at 240°C for 4 hours to decompose the soil sample;

[0037] (2) Mixed acid digestion stage: After the soil pre-digestion is completed, open the cover, add 10mL of mixed acid A to the polytetrafluoroethylene crucible, cover it, and digest it for 16h on the electric heating plate in the fume hood at 220°C; the mixed acid A It is mixed acid B and hydrofluoric acid whose volume ratio is 1:1; said mixed acid B is nitric acid and perchloric acid whose volume ratio is 1:4, and used nitric acid, perchloric acid, and hydrofluoric acid are excellent-grade pure reagents, The mass concentrations are 65%, 70% and 40% respectively;

[0038] (3)H 2 o 2 Digest...

Embodiment 2

[0052] (1) Pre-digestion stage: Weigh 0.2000g of river sediment sediment sample (standard material for river sediment composition analysis GBW08301) into a 50mL polytetrafluoroethylene crucible; add 6mL nitric acid (excellent grade, mass concentration 65%), covered, and digested on the electric heating plate in the fume hood at 180°C for 4 hours to decompose the sample;

[0053] (2) Mixed acid digestion stage: after the pre-digestion, open the cover, add 6 mL of mixed acid A to the polytetrafluoroethylene crucible, cover it, and digest it on the electric heating plate in the fume hood at 240 ° C for 16 hours; the mixed acid A is the volume Mixed acid B and hydrofluoric acid with a ratio of 7:5; the mixed acid B is nitric acid and perchloric acid with a volume ratio of 1:4, and the nitric acid, perchloric acid and hydrofluoric acid used are all superior grade pure reagents, and the mass concentration 65%, 70% and 40% respectively;

[0054] (3)H 2 o 2 Digestion stage: After t...

Embodiment 3

[0066] (1) Pre-digestion stage: Weigh 0.2000g coal sample (standard substance for analysis of inorganic elements in anthracite GSB06-2097-2007) into a 50mL polytetrafluoroethylene crucible; add 10mL nitric acid (premium pure , with a mass concentration of 65%), covered, and digested on an electric heating plate in a fume hood at 240°C for 6 hours to decompose the sample;

[0067] (2) Mixed acid digestion stage: After the pre-digestion is completed, open the cover, add 14 mL of mixed acid A to the polytetrafluoroethylene crucible, cover it, and digest it on the electric heating plate in the fume hood at 220 ° C for 24 hours; the mixed acid A is the volume Mixed acid B and hydrofluoric acid with a ratio of 7:3; the mixed acid B is nitric acid and perchloric acid with a volume ratio of 1:4, and the nitric acid, perchloric acid and hydrofluoric acid used are all superior grade pure reagents, and the mass concentration 65%, 70% and 40% respectively;

[0068] (3)H 2 o 2 Digestion...

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Abstract

The invention discloses a pretreatment method for heavy metal element detection in a solid sample and an application of the pretreatment method. The pretreatment method mainly comprises the five steps: a pre-decomposition stage, a mixed acid decomposition stage, an H2O2 decomposition stage, an acid catching stage and a volume determining stage, wherein the sample is primarily decomposed by using nitric acid in the pre-decomposition stage; the sample is further decomposed by using nitric acid, perchloric acid and hydrofluoric acid in the mixed acid decomposition stage, and the method comprises the main step that the sample is finally decomposed by using H2O2 in the H2O2 decomposition stage. The pretreatment method can be widely applied to the pretreatment for heavy metal element detection in solid samples such as soil, sludge, sediments at the bottom of a lake and the like, and has the advantages of wide application range, high heavy metal recovery rate, simplicity and feasibility in operation and the like.

Description

technical field [0001] The invention belongs to the field of environmental monitoring, and in particular relates to a pretreatment method for detecting heavy metal elements in solid samples and an application thereof. Background technique [0002] In recent years, while my country's economy has developed rapidly and people's living standards have been greatly improved, my country's environmental conditions have deteriorated day by day, which has not only seriously affected the achievements of my country's reform and opening up, but also poses a serious threat to the health of the broad masses of the people. With the gradual enhancement of people's awareness of environmental protection, the voice for improving the environment and controlling pollution is getting louder and louder. In order to control pollution and improve the environment, our government has issued a series of environmental protection regulations and policies, which have achieved good results. However, there ...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N1/44
Inventor 岑超平唐子君方平陈定盛陈志航陈雄波
Owner SOUTH CHINA INST OF ENVIRONMENTAL SCI MEP
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