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Environment-friendly high-efficiency acid reflux collection-type element analysis sample digestion method

An elemental analysis and sample technology, which is applied in the field of acid reflux type environmental protection and high-efficiency elemental analysis sample digestion, can solve the problems of increasing sample contamination, and achieve the effects of shortening the time for acid removal, reducing the amount of acid used, and reducing work intensity

Inactive Publication Date: 2013-08-14
ANALYSIS & TESTING CENT CHINESE ACADEMY OF TROPICAL AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the two methods use digestion equipment, the steps of removing acid are the same as the wet digestion method, and they also have the disadvantages of the above-mentioned wet digestion method for removing acid, and when transferring the sample solution in the microwave digestion tube or high-pressure digestion tube In the process of evaporating the acid in the small beaker, manual operation increases the chance of sample contamination

Method used

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  • Environment-friendly high-efficiency acid reflux collection-type element analysis sample digestion method
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  • Environment-friendly high-efficiency acid reflux collection-type element analysis sample digestion method

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Weigh a certain amount (0.2g-5.0g) of solid agricultural product samples into a digestion vessel, add 2.0mL-20.0mL of nitric acid, and cover with a ground cover with an outlet pipe and a condensation chamber; place the digestion vessel on an electric heating plate , turn on the power switch, set the digestion temperature at 100°C to 180°C (depending on the type of sample), heat and digest the sample until the sample is completely digested (the sample solution is clear and transparent). Then raise the temperature of the electric heating plate to 200°C to 350°C (depending on the amount of acid added), and perform evaporation and acid removal treatment until a little acid (about 0.5mL) remains at the bottom of the digestion vessel. Remove the digestion container, add a small amount of deionized water or ultrapure water to dissolve the salt, transfer and constant volume to a volumetric flask, and become the solution to be tested. The acid liquid collected in the condensatio...

Embodiment 2

[0027] Weigh 4 grams of solid samples of agricultural products into the digestion container, add 15 mL of nitric acid solution and 0.5 mL of hydrogen peroxide solution, cover with a ground cover with an air outlet pipe and a condensation chamber; put the digestion container on an electric heating plate , turn on the power switch, set the digestion temperature to 120°C, heat and digest the sample until the sample is completely digested (the sample solution is clear and transparent). Then raise the temperature of the electric heating plate to 250°C, and carry out evaporation and acid removal treatment until a little acid (about 0.3mL) remains at the bottom of the digestion vessel. Remove the digestion container, add a small amount of deionized water or ultrapure water to dissolve the salt, transfer and constant volume to a volumetric flask, and become the solution to be tested. The acid liquid collected in the condensation chamber can be used as washing liquid or re-distilled. ...

Embodiment 3

[0029] Weigh 5.0 grams of food solid samples into a digestion container, add 20.0 mL of nitric acid and 0.6 mL of hydrogen peroxide, cover with a ground cover with an air outlet pipe and a condensation chamber; put the digestion container on an electric heating plate, turn on Turn on the power switch, set the digestion temperature to 150°C, and heat the digestion sample until the sample is completely digested (the sample solution is clear and transparent). Then raise the temperature of the electric heating plate to 300°C, and carry out evaporation and acid removal treatment until a little acid (about 0.3mL) remains at the bottom of the digestion vessel. Remove the digestion container, add a small amount of deionized water or ultrapure water to dissolve the salt, transfer and constant volume to a volumetric flask, and become the solution to be tested. The acid liquid collected in the condensation chamber can be used as washing liquid or re-distilled.

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Abstract

The invention discloses an environment-friendly high-efficiency acid reflux collection-type element analysis sample digestion method. The method comprises the following steps of: (1) preparing a digestion container equipped with an acid reflux collection device; (2) weighting 0.2 to 0.5g of a solid sample in the digestion container, and adding 2.0 to 21.0mL oxide to obtain a sample solution to be measured; (3) placing the digestion device equipped with the acid reflux collection device and containing the sample solution to be measured on an electric heating plate for digestion; (4) raising temperature of the electric heating plate to remove acid by evaporating after the sample is digested completely; and (5) taking down the digestion container, adding a small amount of deionized water or ultrapure water to dissolve salts, transferring and diluting to fix volume in a volumetric flask to obtain the to-be-measured solution. The digestion method provided by the invention is closed completely from the sample digestion to the evaporation acid-removal processes so as to avoid direct contact between the digested sample and ambient air and avoid pollution of ambient dusts to the sample in the digestion container, thereby greatly improving precision and accuracy of an analysis result.

Description

technical field [0001] The invention relates to an acid reflux type liquid-environmental and high-efficiency elemental analysis sample digestion method. Background technique [0002] Elemental analysis is an important part of chemical analysis. Many trace or trace metal elements (such as copper, manganese, zinc, iron, lead, cadmium, chromium, etc.) are important for the quality analysis of agricultural products, food, medicine, feed, etc. technical indicators. During the experiment, most of the samples need to be digested and decomposed with reagents such as nitric acid, perchloric acid, hydrogen peroxide, etc., and the solid sample is changed into a liquid sample solution before the next step of instrument measurement can be carried out. The sample digestion effect is good. Bad directly affects the precision and accuracy of the analysis results. Due to the low content of metal elements in the sample, and metal elements are ubiquitous in the environment, the digested sampl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/44
Inventor 周聪赵敏
Owner ANALYSIS & TESTING CENT CHINESE ACADEMY OF TROPICAL AGRI SCI
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