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Test method of micro amount of arsenic or antimony in steel

A detection method and technology for iron and steel, applied in the detection of antimony and trace arsenic in iron and steel, can solve the problems of limited element determination by instruments, harmful operators, expensive instruments, etc., and achieve simple operation, good stability, and little matrix interference. Effect

Inactive Publication Date: 2010-02-17
CHINA YITUO GROUP
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0003] 1. Determination of arsenic content by hydride generation-atomic fluorescence spectrometry (national standard GB / T20127.2-2006), determination of antimony content by hydride generation-atomic fluorescence spectrometry (national standard GB / T20127.8-2006), instrument comparison Expensive, and instrumental determination of elements is limited
[0004] 2. Determination of arsenic by chemical method often adopts distillation separation-molybdenum blue photometric method and n-butanol extraction-arsenic bismuth molybdenum blue photometric method, carrier precipitation-molybdenum blue photometric method to determine antimony content and malachite green-benzene extraction photometric method to determine antimony These methods are cumbersome to operate and harmful to the operator's health

Method used

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  • Test method of micro amount of arsenic or antimony in steel
  • Test method of micro amount of arsenic or antimony in steel

Examples

Experimental program
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Effect test

specific Embodiment 1

[0051] Weigh 0.1000g of a steel sample containing different amounts of arsenic and antimony into a 150mL conical flask, add 10mL of concentrated hydrochloric acid, 3mL of concentrated nitric acid, and 10mL of (1+1) sulfuric acid, heat to dissolve the sample (if insoluble A few drops of hydrofluoric acid can be added dropwise to help dissolve), heated to fume of sulfuric acid for 1-2min, removed and cooled slightly, and dissolved in water with salt (if there is carbide precipitation, filter it out) add 10mL100g·L -1 Tartaric acid solution, 10mL100g·L -1 Citric acid solution, add 200g·L -1 Thiourea-200g·L -1 Ascorbic acid mixed solution 10mL, take it out after slightly heating, transfer it into a 100mL volumetric flask after cooling, dilute to the mark with 5% hydrochloric acid solution, shake well for testing.

[0052] Under the working conditions selected by the instrument, the absorbance value of arsenic and antimony is measured, and the content of arsenic and antimony in t...

specific Embodiment 2

[0053] Operate a sample containing arsenic and antimony in the same manner as in Example 1, dilute it to the mark with 10% hydrochloric acid solution, and shake it up for testing.

[0054] Under the working conditions selected by the instrument, the absorbance value of arsenic and antimony is measured, and the content of arsenic and antimony in the sample is found out from the calibration curve drawn by steel standard samples containing different amounts of arsenic and antimony operated under the same conditions.

specific Embodiment 3

[0055] Operate a sample containing arsenic and antimony in the same manner as in Example 1, dilute it to the mark with 25% hydrochloric acid solution, shake it up to be tested.

[0056] Under the working conditions selected by the instrument, the absorbance value of arsenic and antimony is measured, and the content of arsenic and antimony in the sample is found out from the calibration curve drawn by steel standard samples containing different amounts of arsenic and antimony operated under the same conditions.

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Abstract

The invention relates to a test method of steel, in particular to a test method of a micro amount of arsenic or antimony in steel. The test method is based on a principle of a flow injection-hydride generation-atomic absorption spectroscopic methodology, and experiments are determined in a flow-injection sample-injection mode. The method comprises the following steps: a test solution is reduced bya thiourea-ascorbic acid mixed solution and a hydrochloric acid solution to convert arsenic (V) into arsenic (III), and convert antimony (V) into antimony (III); the test solution reacts with a potassium borohydride solution under a carrier band of a carrier solution to generate a great amount of nascent oxygen which reacts with the arsenic (III) or the antimony (III) to generate gaseous AsH3 orSbH3; the AsH3 or the SbH3 is led into a specially-designed quartz tube by high-purity argon gas as carrier gas and is atomized into ground-state atomic vapor; ground-state electrons which are on theoutermost layer of the atom are excited by the light energy of a light source of a hollow cathode lamp to transit to a high energy level; and the amount of abortion light intensity is directly proportional to the concentration of the atom. Accordingly, the arsenic or antimony content in the test solution can be quantitatively analyzed.

Description

【Technical field】 [0001] The invention relates to a method for detecting iron and steel, in particular to a method for detecting trace amounts of arsenic and antimony in iron and steel, in particular to a method for detecting trace amounts of arsenic and antimony in iron and steel by using flow injection-hydride generation atomic absorption spectrophotometry method. 【technical background】 [0002] It is recognized that arsenic and antimony are harmful elements in steel. When the content of arsenic and antimony in steel is high, it will have obvious adverse effects on the strength and bending resistance of steel, resulting in high temperature brittleness of steel and reducing the strength of steel. A small amount of arsenic and antimony in special steel can improve the corrosion resistance and oxidation resistance of steel to a certain extent, which is beneficial to the wear resistance and corrosion resistance of process casting and later use. Generally, arsenic and antimony ...

Claims

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Application Information

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IPC IPC(8): G01N21/31G01N1/28
Inventor 焦凤菊蔡安克邵经峰高桂琴马春庆靖琦史小阳徐少华
Owner CHINA YITUO GROUP
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