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Method for determining thallium content of agricultural product by flame atomic absorption spectrometry

A technology of flame atomic absorption and spectrometry, which is applied in the field of determination of thallium content in agricultural products by flame atomic absorption spectrometry, can solve the problems of undeveloped thallium content detection standards and safety limit standards, etc., and achieve good application effect and good practicability , to ensure the effect of quality

Inactive Publication Date: 2015-09-16
GUIZHOU INSPECTION & QUARANTINE TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In recent years, there have been frequent incidents of thallium poisoning, but my country has yet to formulate detection standards and safety limit standards for thallium content in food

Method used

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  • Method for determining thallium content of agricultural product by flame atomic absorption spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Weigh 2 g of cabbage sample (accurate to 0.001 g), put it in a 250 mL Erlenmeyer flask, add 20 mL of nitric acid + perchloric acid solution (4+1, V+V), cover and soak overnight, and then put it on a heating plate for digestion , until white smoke comes out, the solution is colorless, transparent or slightly yellow, continue to wash the acid until the digestion solution is about 0.5 mL, then remove it, cool to room temperature, transfer it to a 25 mL volumetric flask with pure water, and dilute to the mark , shake well, place to be tested, and make reagent blank at the same time.

[0068] The working conditions of the flame atomic absorption spectrometer are: integral measurement and concentration calibration mode, deuterium lamp buckle background mode, measurement time 5.0s, reading delay 3.0s, analysis line 276.8 nm, slit width 0.5 nm, lamp current 10 mA, air The flow rate is 3.5 L / min, and the flow rate of acetylene is 1.5 L / min.

Embodiment 2

[0070] Weigh 3 g of sweet potato samples (accurate to 0.001 g), put them in a 250 mL Erlenmeyer flask, add 20 mL of nitric acid + perchloric acid solution (4+1, V+V), cover and soak overnight, then put it on a heating plate for digestion , until white smoke comes out, the solution is colorless, transparent or slightly yellow, continue to wash the acid until the digestion solution is about 0.5 mL, then remove it, cool to room temperature, transfer it to a 25 mL volumetric flask with pure water, and dilute to the mark , shake well, place to be tested, and make reagent blank at the same time.

[0071] The working conditions of the flame atomic absorption spectrometer are: integral measurement and concentration calibration mode, deuterium lamp buckle background mode, measurement time 5.0s, reading delay 3.0s, analysis line 276.8 nm, slit width 0.5 nm, lamp current 10 mA, air The flow rate is 3.5 L / min, and the flow rate of acetylene is 1.5 L / min.

Embodiment 3

[0073] Weigh 4g of coix seed sample (accurate to 0.001g), put it in a 250 mL Erlenmeyer flask, add 20 mL of nitric acid + perchloric acid solution (4+1, V+V), cover it and soak overnight, put it on the electric heating plate Digest until white smoke is emitted, the solution is colorless, transparent or slightly yellow, continue to rinse the acid until the digestion solution is about 0.5 mL, then remove it, cool to room temperature, transfer it to a 25 mL volumetric flask with pure water, and dilute to Scale, shake well, place to be tested, and make reagent blank at the same time.

[0074] The working conditions of the flame atomic absorption spectrometer are: integral measurement and concentration calibration mode, deuterium lamp buckle background mode, measurement time 5.0s, reading delay 3.0s, analysis line 276.8 nm, slit width 0.5 nm, lamp current 10 mA, air The flow rate is 3.5 L / min, and the flow rate of acetylene is 1.5 L / min.

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Abstract

The invention discloses a method for determining thallium content of an agricultural product by flame atomic absorption spectrometry. The method comprises the steps of carrying out sample digestion, drawing a work curve, testing a sample, weighing 2-5g (accurately 0.001g) of samples, adding mixed acid of nitric acid and perchloric acid (4+1), carrying out wet digestion, wherein the mass concentration and the absorbancy of thallium have good linear relationship. According to the method, the related coefficient is as follows: r is equal to 0.9999; the detection limit (3s / k) is 0.066mg / kg; the degree of precision is tested as follows: the digestion of the sample is carried out by the test method, seven times of parallel test of the sample is implemented, the result shows that the relative standard deviation of the thallium content of the sample measured by the method is between 1.6%-3.2%; the recovery rate of the added thallium standard solution is 91.6%-95.5%. According to the method, the thallium content of the agricultural product can be measured accurately and rapidly, the precision is good, the accuracy is high, the application effect is good, and the method provides the reference for the formulation of the detection standard of the thallium content of the food in China.

Description

technical field [0001] The invention belongs to the technical field of testing and analysis, and in particular relates to the determination of thallium content in agricultural products by flame atomic absorption spectrometry. Background technique [0002] Thallium is a rare and widely distributed highly toxic and high-risk heavy metal element. Its appearance is similar to tin, and its surface layer is easy to form oxides in the air. It is widely used in the fields of medicine and health, electronic communications, and chemical catalytic materials. Thallium and its compounds are highly toxic and highly water-soluble, and can be easily absorbed through the skin, or through the hair follicles all over the body surface, mucous membranes of the respiratory tract, etc. Cause chronic damage, toxicity far exceeds that of lead, arsenic, mercury, cadmium, etc. [0003] Geological researchers discovered red thallium deposits in Huilong Village, Xingren County, Qianxinan Pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31G01N1/44
Inventor 蔡秋刘康书梁艺馨李娜
Owner GUIZHOU INSPECTION & QUARANTINE TECH CENT
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