Method for determining nickel content in soil by microwave digestion-flame atomic absorption spectrometry

A flame atomic absorption and microwave digestion technology, which is used in the measurement of color/spectral properties and the preparation of samples for testing, can solve the problems of large solvent consumption, environmental pollution, and low sensitivity, and achieves less solvent consumption and environmental pollution. The effect of lowering and heating up

Inactive Publication Date: 2014-02-05
SUZHOU GUOHUAN ENVIRONMENT DETECTION
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AI Technical Summary

Problems solved by technology

[0003] At present, for the determination of nickel in soil, the sample treatment method in the national standard is wet digestion, which is determined by flame atomic absorption spectrometry. This method takes a long time, has low sensitivity, consumes a large amount of solvent, and causes environmental pollution caused by solvent. serious

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050]The soil of the plow layer of the vegetable base was collected according to the diagonal distribution method, and the collected soil was air-dried naturally, and after removing animal and plant residues and gravel, it was ground through a nylon sieve with a pore size of 2 mm, and then divided by quartering and further crushed with agate. Grind it through a 0.25mm pore nylon sieve with a mortar, mix well, and obtain a soil sample; accurately weigh 0.25g of the soil sample and place it in a clean microwave digestion tank, add a few drops of ultrapure water to moisten it, and add a volume ratio of 15 : 2:5 mixed solution of 65% nitric acid, 38% hydrofluoric acid, and 11 mL of 25% hydrogen peroxide is used as a digestion solvent, that is, the digestion solvent is a mixture of 65% nitric acid 7.5 mL, 38% hydrofluoric acid 1 mL, and 25% hydrogen peroxide 2.5 mL. Soak solution and soil samples in the digestion solvent for 40~45min, then cover and seal them into a microwave diges...

Embodiment 2

[0058] The only difference from Example 1 is that the digestion program is set as follows: under a digestion pressure of 2.5 MPa, heat at 140°C for 10 minutes, 210°C for 5 minutes, and 230°C for 20 minutes.

[0059] Other experimental conditions are the same as in Example 1, prepare 6 parallel sample solutions and digestion solutions, add 2.5mL of 1.5% surfactant polyoxyethylene castor oil glyceryl ether to the sample solution after digestion, dilute with 1.0% nitric acid To measure the absorbance of the nickel element in the sample with the help of a spectrometer, respectively calculate the content of the nickel element in the 6 samples according to the linear regression equation, and take the average value. The measured nickel element contents are: 180.38 ug / L, 179.45 ug / L, 178.23 ug / L, 179.26 ug / L, 180.24 ug / L, 180.31 ug / L, and the calculated average value is: 179.65 ug / L, relative In Example 1, the content of nickel element in the measured soil is low, and comprehensive an...

Embodiment 3

[0061] The only difference from Example 1 is that the digestion program is set as follows: under a digestion pressure of 2.5 MPa, heat at 180°C for 10 minutes, 210°C for 5 minutes, and 230°C for 20 minutes.

[0062] Other experimental conditions are the same as in Example 1, prepare 6 parallel sample solutions and digestion solutions, add 2.5mL of 1.5% surfactant polyoxyethylene castor oil glyceryl ether to the sample solution after digestion, dilute with 1.0% nitric acid To measure the absorbance of the nickel element in the sample with the help of a spectrometer, respectively calculate the content of the nickel element in the 6 samples according to the linear regression equation, and take the average value. The measured nickel element contents are: 189.67 ug / L, 184.61 ug / L, 187.04 ug / L, 187.46 ug / L, 186.98 ug / L, 187.23 ug / L, and the calculated average value is: 187.165 ug / L, relative Example 1, the test results are consistent with Example 1, showing that as long as the tempe...

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Abstract

The invention provides a method for determining a nickel content in soil by microwave digestion-flame atomic absorption spectrometry, wherein the method is characterized by: pretreating a soil sample by combining long-time immersion and stepedly heated microwave digestion, using polyoxyethylene castor oil glycerin ether as an activator, raising atomization efficiency of nickel atoms in flame, raising determination sensitivity, thereby raising sensitivity; based on linear relation of absorbance and nickel content determined by a flame atomic abserption spectrometer by a standard solution, measuring and calculating to obtain the content of nickel atoms in soil. The method provided by the invention solves problems that a method for determining trace elements by traditional atomic absorption spectrometry has disadvantages long time consumption, low sensitivity, large solvent consumption amount, and severe environment pollution caused by a solvent, and the method provided by the invention has advantages of good precision, high recovery rate, accuracy, reliability, rapidness and convenience.

Description

technical field [0001] The invention relates to a method for measuring nickel content in soil, in particular to a method for measuring nickel content in soil by means of microwave digestion and polyoxyethylene castor oil glyceryl ether as an activator by means of flame atomic absorption spectrometry. Background technique [0002] Nickel is mainly used in alloys (such as nickel steel and nickel silver) and as a catalyst in chemical production, which can be used to make currency, etc. Nickel is also an essential trace element for the human body; at the same time, nickel is also one of the important environmental pollutants. my country's soil environment The quality standard clearly stipulates that the maximum allowable concentration of nickel in the soil is 0.2mg / L. If the content of nickel in the soil exceeds the standard, it will affect the crops, and then cause harm to animals and humans through the food chain. Nickel is even carcinogenic. Therefore, the determination The con...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/33G01N1/44
Inventor 徐晓华
Owner SUZHOU GUOHUAN ENVIRONMENT DETECTION
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