Soil alkali fusion pretreatment method

An alkaline melting and soil technology, applied in the field of analytical chemistry, can solve the problems of inability to detect and high risk, and achieve the effect of improving efficiency, increasing the number of samples, and expanding the scope of detection

Pending Publication Date: 2019-04-26
宁波市环境监测中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the detection accuracy of heavy metal elements in soil, Publication No. 107167361A discloses a method for analyzing heavy metal content in soil, which is determined through steps such as alkali hydrolysis, acid hydrolysis, concentration, and determination, but its essence is alkaline solution treatment and acid solution It is not well adapted to the detection of some elements, and it is more dangerous

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Experimental program
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Embodiment 1

[0060] (1) Sample treatment: Air-dry, grind, and mix the four samples of standard soil GBW07405 (GSS-5), standard soil GBW07453 (GSS-24), standard sediment GBW07311 (GSD-11), and actual soil, respectively. Sieve and measure the moisture content respectively;

[0061] (2) Digestion: Weigh 0.5g of 4 kinds of samples with known moisture content and place them in corundum crucibles respectively, place the crucibles on the alkali fusion weighing device respectively, first weigh 1.0g of sodium carbonate and place them at the bottom of the crucible, then Add 0.1g of lithium tetraborate and 0.4g of lithium metaborate, transfer the crucibles one by one to the heating box of the temperature-adjustable heating and digestion device with the mechanical arm, heat at 1000°C for 30min, and cool to 300°C to obtain 4 kinds of digestion samples ;

[0062] (4) Post-processing: transfer the 4 kinds of digestion samples to the alkali fusion weighing device one by one by using the mechanical arm, a...

Embodiment 2

[0075] (1) Sample treatment: Air-dry, grind, and mix the four samples of standard soil GBW07405 (GSS-5), standard soil GBW07453 (GSS-24), standard sediment GBW07312 (GSD-12), and actual soil, respectively. Sieve and measure the moisture content respectively;

[0076] (2) Pre-digestion: Weigh 0.5g of 4 kinds of samples with known moisture content and place them in corundum crucibles, place the crucibles on the alkali fusion weighing device, add 10ml of hydrofluoric acid dropwise to the crucibles, and use the mechanical arm to Transfer the crucibles one by one to the heating box of the temperature-adjustable heating and digestion device, heat at 100°C for 20 minutes, and cool for 20 minutes to room temperature to obtain the pre-digestion sample;

[0077] (3) Re-digestion: transfer the pre-digested samples to the alkali fusion weighing device respectively, add 5 g of sodium peroxide to the crucible, and then transfer the crucibles one by one to the heating box of the temperature-...

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Abstract

The invention belongs to the technical field of analytical chemistry, and particularly relates to a soil alkali fusion pretreatment method. The pretreatment method comprises the steps of sample treatment, pre-digestion, re-digestion, post-treatment and the like; the pretreatment method is simple and feasible, most of the pretreatment method is automatically controlled by a system, the error degreeof manual operation can be greatly reduced, in the actual treatment process, selective operation can be carried out according to the difference of metal elements such as manganese and barium, alkalifusion pretreatment can be directly carried out by omitting the pre-digestion step, while the metal elements such as tin need to be strictly implemented according to the steps, and thus the actual detection range of the method is extended. By simplifying the pretreatment step and making the simplified step blended into a specific instrument, the efficiency of sample pretreatment is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a soil alkali melting pretreatment method. Background technique [0002] Among metal elements, heavy metal elements cannot be decomposed by microorganisms in soil and sediment, but can accumulate continuously and be enriched by organisms, passing through the food chain, posing a threat to humans, and even some heavy metals can be transformed by microorganisms in soil and sediment for more toxic compounds. [0003] At present, most of the determination of metals in environmental monitoring adopts acid digestion system, using sulfuric acid, perchloric acid, nitric acid and hydrofluoric acid to fully digest the soil, and finally using inductively coupled plasma atomic emission spectrometer or atomic fluorescence instrument, etc. The instrument performs the measurement. However, the dissolution efficiency of some elements such as metal tin, potassium, sodiu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28
CPCG01N1/28
Inventor 沈碧君朱丽波杨惠傅晓钦潘双叶冯加永李琦钱成薛令楠
Owner 宁波市环境监测中心
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