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Method of determining mercury in soil through water bath digestion-atomic fluorescence method

An atomic fluorescence and water bath digestion technology, which is used in fluorescence/phosphorescence, preparation of test samples, material excitation analysis, etc., can solve problems such as the inability to process large quantities of soil samples quickly, and achieve simple operation, accurate detection results, and digestion. fast effect

Inactive Publication Date: 2016-03-23
SUZHOU GUOHUAN ENVIRONMENT DETECTION
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, none of the above digestion methods can quickly process large quantities of soil samples.

Method used

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  • Method of determining mercury in soil through water bath digestion-atomic fluorescence method
  • Method of determining mercury in soil through water bath digestion-atomic fluorescence method
  • Method of determining mercury in soil through water bath digestion-atomic fluorescence method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Instrument: Hydride atomic fluorescence photometer: AFS-830 type, Beijing Jitian Instrument Co., Ltd.; mercury hollow cathode lamp: Beijing Nonferrous Metal Research Institute; intermittent flow automatic sampling system; adjustable constant temperature electric hot water bath (max. Adjust the temperature at 100°C); soak all glassware in 20% hydrochloric acid solution for more than 24 hours before each use, rinse with tap water, and wash with distilled water and double distilled water.

[0022] Reagents: The reagents used in the experiment are of analytical grade or superior grade, and the water used is Millipore ultrapure water.

[0023] Mercury standard stock solution: 1000μg / ml, National Nonferrous Metals and Electronic Materials Analysis and Testing Center, GSB04-1729-2004, 13527-2, validity period: 2013.5-2015.5.

[0024] Mercury standard use solution: take 10ml, 1000μg / ml mercury standard stock solution and dilute to 100μg / L step by step, for use in preparing merc...

Embodiment 2

[0053] Sample pretreatment:

[0054] Water bath digestion:

[0055] Accurately weigh 0.5g of air-dried soil sample (200 mesh) into a 50ml stoppered colorimetric tube, add a little water to moisten the sample, add 12.5ml (3:1) aqua regia, shake well after plugging, and place in a boiling water bath Digest for 100 minutes, during which shake once every 20 minutes. After the digestion is complete, take it out and cool it, add 5ml of hydrochloric acid, dilute to the mark with ultrapure water, shake well and let stand, take the supernatant for testing. At the same time, do sample blank processing.

[0056] Instrument Conditions:

[0057] Mercury: lamp current: 40mA; negative high voltage: 280V; atomizer height: 8mm; carrier gas flow: 300ml / min; shielding gas flow: 800ml / min; injection volume: 0.5ml; measurement method: standard curve method; reading Method: Peak Area.

[0058] Reductant: Potassium borohydride solution with a concentration of 12g / L is prepared, dissolved in 0.5% ...

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Abstract

The invention discloses a method of determining mercury in soil through a water bath digestion-atomic fluorescence method. The method is characterized by comprising the first step of preparation of a test substance solution, the second step of preparation of a standard substance solution, the third step of drawing of a standard curve and the fourth step of detection of test substances, wherein an appropriate amount of supernate of the test substance solution and sample blank are taken and placed into a clean colorimetric tube, and the colorimetric tube is placed in an automatic sampler of an atomic fluorescence spectrometer for detection of mercury content. Through the method of determining mercury in soil through the water bath digestion-atomic fluorescence method, operation is easy and convenient, sensitivity is high, detection time is short, and soil samples can be detected quickly in batch.

Description

technical field [0001] The invention relates to a water-bath digestion-atomic fluorescence method for determining mercury in soil, and belongs to the technical field of environmental monitoring methods. Background technique [0002] Mercury and its compounds are highly toxic substances that can invade the human body through different channels such as the respiratory tract, skin or digestive tract. Inorganic mercury ions entering the water body can be transformed into more toxic organic mercury, which enters the human body through the food chain and causes systemic poisoning. [0003] Colorimetric method, atomic absorption method and atomic fluorescence method are commonly used in soil analysis to determine mercury content. The results of the first two methods are relatively stable, but the disadvantages are cumbersome operation, long analysis time, low sensitivity, quantitative results cannot be obtained for samples with low content, and cannot meet the requirements of envi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/44G01N21/64
Inventor 刘欢欢周杰张雷
Owner SUZHOU GUOHUAN ENVIRONMENT DETECTION
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