A pretreatment method for the determination of mercury in plant-derived samples

A plant-derived, element determination technology, applied in the field of heavy metal detection, can solve the problems of high energy consumption and high digestion temperature, and achieve the effects of reducing the amount of strong acid, improving accuracy, and alleviating foaming and splashing

Active Publication Date: 2020-09-08
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

The digestion time is at least 4-5h, the digestion temperature is high (140-170°C), and the energy consumption is large

Method used

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  • A pretreatment method for the determination of mercury in plant-derived samples
  • A pretreatment method for the determination of mercury in plant-derived samples

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A pretreatment method for determination of mercury in plant-derived samples, comprising the following steps:

[0027] 1) Take the onion, pulverize it, beat it, weigh 0.5g of the beaten sample, add 1.0mL of concentrated sulfuric acid with a mass fraction of 70%, place it in a graphite porous electrothermal digestion apparatus, keep the temperature at 10°C, and hold it for 0.3h;

[0028] 2) Add 2.0mL of digestion solution a, and keep the temperature at 90°C until the total volume is reduced by 50%; then add 3.0mL of sulfuric acid solution with a mass fraction of 75% for 0.3h;

[0029] 3) Add 1.0mL of digestion solution b, cool down to 65°C at a rate of 3°C / min, keep it warm for 0.5h, then rinse with acid, constant volume, and test;

[0030] The digestion solution a is HNO 3 and HClO 4 Mixture of HNO 3 with HClO 4 The mass ratio is 3:1;

[0031] The digestion solution b is HNO 3 , HCl and HClO 4 Mixture of HNO 3 , HCl and HClO 4 The mass ratio is 7:2:1.

Embodiment 2

[0033] A pretreatment method for determination of mercury in plant-derived samples, comprising the following steps:

[0034] 1) Take the onion, pulverize it, beat it, weigh 4.0g of the beaten sample, add 1.5mL of concentrated sulfuric acid with a mass fraction of 75%, keep the temperature at 15°C, and hold for 0.5h;

[0035] 2) Add 4.0mL of digestion solution a, and keep the temperature at 105°C until the total volume is reduced by 60%; then add 1.0mL of sulfuric acid solution with a mass fraction of 30% for 0.2h;

[0036] 3) Add 2.0mL of digestion solution b, cool down to 75°C at a rate of 5°C / min, keep it warm for 1.5h, then rinse with acid, constant volume, and test;

[0037] The proportion and dosage of the digestion solutions a and b are the same as in Example 1.

Embodiment 3

[0039] A pretreatment method for determination of mercury in plant-derived samples, comprising the following steps:

[0040] 1) Take the onion, pulverize it, beat it, weigh 2.0g of the beaten sample, add 1.5mL of concentrated sulfuric acid with a mass fraction of 70%, keep the temperature at 15°C, and hold for 0.5h;

[0041] 2) Add 3.0mL of digestion solution a, and keep the temperature at 105°C until the total volume is reduced by 60%; then add 3.0mL of sulfuric acid solution with a mass fraction of 75% for 0.3h;

[0042] 3) Add 2.0mL of digestion solution b, cool down to 65°C at a rate of 3°C / min, keep it warm for 1.0h, then rinse with acid, constant volume, and test;

[0043] The proportion and dosage of the digestion solutions a and b are the same as in Example 1.

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Abstract

The invention provides a pretreatment method for determining mercury element in a plant derived sample, comprising the steps of adding sulfuric acid, digestion solution a, digestion solution b and thelike. According to the pretreatment method for determining mercury element in a plant derived sample, the use amount of the strong acid is reduced, the treatment time is shortened, and the pretreatment efficiency and accuracy of mercury determination are improved through the reduction of the digestion temperature and the segmented use of the polybasic acid; the sulfuric acid solution is added andcooled before digestion, so that the phenomenon of foaming and splashing in the digestion process can be effectively relieved, and the harm to the environment and technicians due to the large amountof solvent volatilization can be prevented, the interference of substances such as fat, wax, cellulose and other substances in the sample to mercury element leaching can also be reduced, so that the accuracy of mercury determination is improved.

Description

technical field [0001] The invention relates to the technical field of heavy metal detection, in particular to a pretreatment method for determining mercury in plant-derived samples. Background technique [0002] Mercury is a heavy metal element that is extremely harmful to the human body. It accumulates in the human body to a certain extent. Once it exceeds the standard, it will seriously damage important organs such as the liver, kidney, heart, and brain. Mercury often enters the human body through food, so the detection of mercury content in food is particularly important. At present, according to [National Food Safety Standard Determination of Total Mercury and Organic Mercury in Food], the pretreatment methods included in the determination method of total mercury in samples include pressure tank digestion method, microwave digestion method, and reflux digestion method. Among them, the pressure tank digestion method and microwave digestion method need to add 5.0-8.0mL c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/44
CPCG01N1/44
Inventor 苏冰霞
Owner ANALYSIS & TESTING CENT CHINESE ACADEMY OF TROPICAL AGRI SCI
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