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Method for rapid determination for minim antimony of steel

A rapid determination and micro-quantity technology, applied in the preparation of test samples, electrical excitation analysis, material excitation analysis, etc., can solve the problems of uneven sample injection, high detection limit of analysis, and large fluctuation of spectral line intensity, etc., to achieve Effects of improving assay sensitivity, optimizing assay conditions, and enlarging test range

Inactive Publication Date: 2008-09-17
725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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AI Technical Summary

Problems solved by technology

[0006] But there are following problems when this method is used to measure the antimony in hull steel: (1) spectral line is selected as Sb206.819nm, and analysis detection limit is higher, is 0.0073ug / mL
(2) The reduction inhibitor used in the article is 10g / L KBH 4 +5g / L thiourea+5g / L ascorbic acid+2g / L KI, found in actual use, from KBH in dry solution 4 Continued decomposition, continuous hydrogen overflow, so that the injection is extremely uneven, and the intensity of the spectral line fluctuates greatly. (3) In this paper, there are few experiments on interfering elements in low alloy steel, mainly Fe, Ni, Cr, Cu, Co interference, but no interference test and interference elimination test were done for Mo, which has the most serious interference

Method used

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  • Method for rapid determination for minim antimony of steel
  • Method for rapid determination for minim antimony of steel
  • Method for rapid determination for minim antimony of steel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1 mixed interference test

[0033] Matrix Fe interferes with antimony. The standard curve of the mixed interference test invented is based on 4-6mg / mL iron as the matrix, 40-60mL mixed acid as the medium, the antimony content of the added standard solution is 0ug, 5ug, 50ug, 100ug, 300ug, and the volume is 100mL. The data are shown in Table 1, attached figure 1 ,Table 2. The amount of antimony added in the interference test is equivalent to 0.01% by mass of antimony.

Embodiment 2

[0034] Embodiment 2 determines the linear relationship between the spectral line intensity of the antimony standard concentration solution and the working curve

[0035] Detection limit test: Carry out ten consecutive measurements on the blank sample, and multiply the average value of the standard deviation (SD) of 10 tests by three to obtain a detection limit of 0.0000991% (0.004955ug / mL), which is lower than << The detection limit of antimony described in the paper "ICP-AES Determination of As, Sn, Pb, Sb, Bi in ordinary carbon steel and low alloy steel" in Metallurgical Analysis (Volume 25, Issue 2) is 0.0073ug / mL .

[0036] The linear relationship of the working curve: Weigh six parts of 0.4-0.6000g high-purity iron into a 250mL beaker, dissolve with 40-60mL mixed acid (HCl:HNO3:H2O=1:2:7), remove, cool, and transfer to a 100mL volumetric flask , add 0ug, 5ug, 50ug, 100ug, 300ug of antimony respectively, dilute to the mark with high-purity water, and shake well. Under th...

Embodiment 3

[0041] Weigh six parts of 0.4900g high-purity iron into 250mL beakers respectively, and use 45mL mixed acid (HCl:HNO 3 :H 2 (0=1:2:7) dissolves, removes, cools, transfers into 100mL volumetric flask, adds the antimony of corresponding content respectively according to accompanying drawing 3, dilutes to scale with high-purity water, shakes up. Under the selected working conditions of the instrument, measure its intensity value to antimony standard solution, and carry out linear regression calculation, the results are shown in Table 4 and attached figure 2 .

[0042] Weigh 0.4850g sample 1 in a 250mL Erlenmeyer flask, add 45mL mixed acid (HCl: HNO 3 :H 2 (0=1: 2: 7), low-temperature heating to dissolve the sample, after the dissolution is complete, remove it, cool it, transfer it into a 100mL volumetric flask, and analyze its antimony content to be 0.0017%.

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Abstract

The invention relates to a method for quickly measuring the trace antimony in steel, using the hydride generator-plasma atomic emission spectrometer and solution containing NaBH 4 as reducer, the mixed liquor containing thiourea, ascorbic acid and potassium iodide as masking inhibitor and alkali or alkali salt in the reducer as NaBH4 restraint decomposer. Preferably the masking inhibitor is the mixture of 8.0-13.0g / L NaBH 4, 4.0-8.0g / L NaOH, 4.0-8.0g / Lthiourea, 4.0-8.0g / Lascorbic acid and 2.0-5.5g / L KI and the analytical line of the antimony is 217.581(154)nm. The invention reduces the testing time and increases the measurement sensitivity and reduces the analysis detection limit.

Description

technical field [0001] The invention relates to a method for measuring trace amount of antimony in steel, in particular to a method for measuring trace amount of antimony in hull steel by using a hydride generator-plasma atomic emission spectrometer. Background technique [0002] Trace amounts of arsenic, tin, antimony, lead, bismuth and other low melting point elements ("five harmful" elements) in steel have a great influence on the properties of materials. In the process of smelting and using steel, it is of great significance to strictly measure and control their content. The main source of antimony is the raw material for steelmaking. The increase of antimony in steel will reduce the impact toughness of steel, enhance the brittleness of steel, and form severe segregation. It is a harmful element and must be strictly controlled. The content of antimony in steel is generally required to be controlled at 0.05%. the following. [0003] The content analysis of trace amounts...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/66G01N1/28
Inventor 高国林李治亚杜米芳
Owner 725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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