GB/T 3260.5-2000 Chemical analysis method for tin - Determination of antimony content

This standard specifies the determination method of antimony content in tin. This standard is applicable to the determination of antimony content in tin. Determination range: 0.00050% to 0.050%. GB/T 3260.5-2000 Chemical analysis method for tin Determination of antimony content GB/T3260.5-2000 Standard download decompression password: www.bzxz.net

GB/T3260.52000
This standard is a reconfirmation of GB/T3260.5·1982 "Chemical analysis method of tin - determination of antimony by malachite green photometry", with only editorial changes.
Standard compliance:
GB/T1.}--1993 Standardization\I. Basic provisions of guidelines for standardization work
Unit 1: Rules for drafting and expressing standards Part 1: GB/T 1.4-1988
Guidelines for standardization work Provisions for the preparation of chemical analysis methods GB/T1467-1978 General principles and general provisions for chemical analysis methods of metallurgical products GB/T7729~--1987 General principles for spectrophotometric methods for chemical analysis of metallurgical products GB/T17433-1998 Basic terms for chemical analysis of metallurgical products This standard will replace GB/T3260.5--1982 from the date of implementation. This standard was proposed by the State Bureau of Nonferrous Metals Industry. This standard is under the jurisdiction of the China Nonferrous Metals Industry Standard Metrology and Quality Research Institute. This standard was drafted by Yunnan Tin Company and Liuzhou Huaxi Group Co., Ltd. This standard was drafted by Liuzhou Smelter of Liuzhou Huaxi Group Co., Ltd. The main drafters of this standard are Li Zhifang, Wang Shoulai and Chen Xufeng. 72
1 Scope
National Standard of the People's Republic of China
Methods for chemical analysis of tin--Determination of antimony content This standard specifies the method for the determination of antimony content in tin. This standard is applicable to the determination of antimony content in tin. Determination range: 0.00050%~0.050%. 2 Method Summary
GB/T3260.5 ---2000
Replaces GB/T 3260.5-1982
The sample is decomposed with hydrochloric acid and hydrogen peroxide. In the hydrochloric acid medium, the complex anion reacts with malachite green. The resulting green complex is extracted by benzene and its absorbance is measured at a wavelength of 635nm by a spectrophotometer. The extracted solution contains 400mg tin, 0.1mg copper, 1ug ​​gold, and each does not interfere with the determination. 3 Reagents
3.1 Anhydrous sodium sulfate.
3.2 Hydrochloric acid (pl.19g/ml).
3.3 Cyanogen peroxide (30%).
3.4 ​​Benzene.
3.5 Hydrochloric acid (5+3).
3.6 Phosphoric acid (1+9).
3.7 Stannous chloride solution (100g/L): Weigh 10g stannous chloride (SnCl2·2Hz0), add 20mL hydrochloric acid (3.2), warm to dissolve. Cool slightly, dilute with water to 100ml.
3.8 Sodium nitrite solution (140g/1.). 3.9 Urea solution (400g/1.).
3.10 Malachite green solution (2g/1.).
3.11 Antimony standard stock solution: Weigh 0.2742g potassium tartrate (KShOC,H0.·1/2H.0) in a 250ml beaker: 1. Pour 100ml hydrochloric acid (3.5), stir to dissolve. Transfer to a 1000mL volumetric flask, clean the beaker with salt (3.5) and dilute to the mark. Mix well. This solution contains 100g antimony in 1mL.
3.12 Antimony standard solution: Pipette 25.00nL of standard stock solution into a 500m. volumetric flask, dilute to scale with hydrochloric acid (3.5), mix, and this solution contains 5ug antimony in 1mL.
4 Analysis steps
4.1 Test sample
Weigh the sample according to Table 1, accurate to 0.0001g. Approved by the State Administration of Quality and Technical Supervision on August 28, 2000, implemented on December 1, 2000
Antimony content, %
0.00050~0.0050
>0. 005 0-- 0. 020
≥0.020~0. 050
Carry out 2 independent determinations and take the average value. 4.2 Blank test
Carry out a blank test with the test sample.
4.3 Determination
GB/T3260.5—2000
Test material quantity·g
Total volume of test solution, ml
4.3.1 Place the test material (4.1) in a 150ml beaker. Add 20ml of hydrochloric acid (3.2). Cover with blood, add 2~6ml of cyanide peroxide drop by drop, heat to dissolve completely and boil until there are no small bubbles, cool, transfer to a 25 or 50ml volumetric flask with hydrochloric acid (3.5) and dilute to the scale, mix well.
4.3.2 Transfer 5.00ml of test solution, place in a 100ml beaker, add 3ml of hydrochloric acid (3.2), heat to 50~60C, drop 2~4 drops of stannous chloride solution, mix, and cool.
4.3.3 Add 1mL sodium nitrite solution, mix well, and let stand for 2min. Add 1.5mL urea solution, and shake for 0.5-1min while adding to dissipate bubbles.
4.3.4 Transfer to a 125ml separatory funnel pre-filled with 20.00mL benzene, wash the beaker several times with 20mL phosphoric acid, add it to the separatory funnel, and mix. Add 0.5mL malachite green solution, shake for 1min, let stand and separate, and discard the aqueous phase. Add 0.5% anhydrous sodium sulfate to the organic phase and shake for a while.
4.3.5 Transfer part of the organic phase into 1cm absorption III, use the blank test solution accompanying the sample as a reference, measure the absorbance at a wavelength of 635nm on the spectrophotometer, and find out the antimony content from the working curve. 4.4 Drawing of working curve
4.4.1 Transfer 0.1.00, 2.00, 3.00, 4.00, and 5.00mL of antimony standard solution to a group of 100mL beakers, respectively, and make up to 5ml with hydrochloric acid (3.5). The following is carried out according to 1.3.2 to 4.3.4. Transfer part of the organic phase into 1cm absorption III, use the blank test solution as a reference, and measure the absorbance of the standard solution. Draw the working curve with the content as the horizontal axis and the absorbance as the vertical axis. 5 Expression of analysis results
Calculate the percentage of antimony according to formula (1):
Sb(%) = - m: V. X 10-s
? Antimony amount found from the working curve, g; where; m,--
V, the volume of the test solution, mL;
V. Total volume of the test solution, ml.;
--the mass of the sample, g.
The result is expressed to three decimal places. If the antimony content is less than 0.010%, it is expressed to four decimal places, and if it is less than 0.0010%, it is expressed to five decimal places.
6 Allowable differencebzxZ.net
The difference between the analysis results of laboratories shall not be greater than the allowable difference listed in Table 2 below74
0. 000 50~0. 001 0
>G. 001 0~0. 003 0
>0. 003 0~ 0. 005 0
GB/T 3260. 5-2000
Allowed ban
Antimony content
0. 005 0~ 0. 010
0. 010~0. 030
≥0.030~0.050
Allowed difference
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