GB/T 3260.9-2000 Chemical analysis method for tin - Determination of lead, copper and zinc content
Some standard content:
GB/T 3260.9--2000
This standard is a reconfirmation of GB/T3260.91982 "Chemical analysis method of tin - Determination of lead, copper and zinc by atomic absorption spectrophotometry", and the determination range has been revised:
Lead content 0.015%~0.80% has been revised to 0.001 0%~0.10%; copper content 0.0005%0.12% has been revised to 0.00020%~~0.020%; zinc content 0.0010%~0.0040% has been revised to 0.000 20%~-0.005 0%. It is also clarified that: when the lead content is 0.0010%~0.010%, the copper content is 0.00020%~0.0030%, and the zinc content is 0.00020%0.00050%, the sample is increased and most of the tin is removed by volatilization with hydrochloric acid-hydrobromic acid, and then the atomic absorption spectrometry is performed. The allowable differences for the determination of these three elements have been supplemented and revised accordingly, and the entire text has been edited. GB/T3260.8--1982 "Chemical Analysis Method for Tin, PAN Photometric Determination of Zinc" is no longer implemented. This standard complies with:
GB/T1.1-1993 Guidelines for Standardization Unit 1: Rules for Drafting and Presenting Standards Part 1: Basic Regulations for Standardization
GB/T1.4-1988 Guidelines for Standardization Rules for Chemical Analysis Methods GB/T1467--1978 General Principles and General Rules for Chemical Analysis Methods for Metallurgical Products GB/T7728-1987 General Principles for Flame Atomic Absorption Spectrometry for Chemical Analysis of Metallurgical Products GB/T17433-1998 Basic Terminology for Chemical Analysis of Metallurgical Products Appendix A in this standard is a reminder appendix.
From the date of implementation, this standard will replace GB/T3260.8-1982 and GB/T3260.9-1982. 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 Industry Company and Liuzhou Huaxi Group Co., Ltd. This standard was drafted by Yunnan Entry-Exit Inspection and Quarantine Bureau and Yunnan Tin Company Research and Design Institute. The main drafters of this standard are Lei Xinheng, Fang Zheng, Cao Runeng, Lin Qingquan and Su Aiping. 84
1 Scope
National Standard of the People's Republic of China
Methods for chemical analysis of tinDelermination of lead, copper and zinc contentThis standard specifies the method for determination of lead, copper and zinc content in tin. GB/T 3260. 9 --2000
Replaces GB/T 3240.K: 1582
GB/T 3260. 4
This standard is applicable to the determination of lead, copper and zinc content in tin. Determination range: lead 0.0010%~0.10%; copper 0.0020%~0.020%; zinc 0.00020%~~0.0050%. 2 Method Summary
The sample is dissolved with hydrochloric acid and hydrogen peroxide, and the absorbance of lead, copper and zinc is measured by atomic absorption spectrometer at 283.3nm, 324.8nm and 213.9nm with air-acetylene flame in hydrochloric acid medium. 4 When the lead content is 0.0010%~~0.010%, the copper content is 0.00020%~0.0030%, and the zinc content is 0.00020%~0.00050%, the sample weight must be increased, and most of the tin is volatilized with hydrochloric acid-hydrobromic acid. 3 Reagents
The water recorded in this method is deionized water.
3.1 Hydrochloric acid (pl.19g/ml.). Premium purity, 3.2 Nitric acid (ml.42g/mL). Premium purity. 3.3 Hydrobromic acid (pl.48g/mg), premium purity. 3.4 Hydrogen peroxide (30%), premium purity. 3.5 Hydrochloric acid (1→1), premium purity.
3.6 Hydrochloric acid (1+9), premium purity.
3.7 Nitric acid ()→1). Premium purity.
3.8 Hydrochloric acid-nitrogen bromide: Mix equal volumes of hydrochloric acid (3.1) and hydrobromic acid (3.3). 3.9 Aqua regia: Mix 1 volume of nitric acid (3.2) with 3 volumes of hydrochloric acid (3.1). 3.10 Main water (1+1)
3.11 Sulfuric acid (1+1)
3.12 Lead standard stock solution: Weigh 0.5000g of metallic lead (99.99%), cover it in a 200ml beaker, add 201ml of lead warmer (3.7). Heat slightly until completely dissolved. Cool, transfer to a 500ml volumetric flask. Dilute to the mark with water. Mix. This solution is 1ml.! 3.13 Lead standard solution: Transfer 20.00 ml lead standard solution to a 200 ml volumetric flask. Dilute to scale with water. Mix. 1 ml of solution contains 100 μg lead. 3.14 Copper standard storage solution: Weigh 0.5000 g metallic copper (99.99%). Place in a 200 ml beaker, add 20 ml nitric acid (3.00). Heat until completely dissolved. Cool, transfer to a 500 ml volumetric flask and dilute to scale with water. Mix. 1 ml of this solution contains 50 μg copper. 3.15 Copper standard solution: Transfer 10.00 ml copper standard storage solution to a 200 ml volumetric flask. Dilute to scale with water. Mix. Approved by the State Administration of Quality and Technical Supervision on 2000-08-28 and implemented on 20001201. 1 ml of solution contains 50 μg copper.
GB/T 3260. 9--2000
3.16 Zinc standard stock solution: weigh 0.1000g of metallic zinc (99.99%), place it in a 200mL beaker, add 20ml of hydrochloric acid (3.5) to dissolve it completely, transfer it to a 1000mL volumetric flask, dilute it to the mark with water, mix it, and then transfer it to a plastic bottle for storage. This solution contains 100μg zinc per ml.
3.17 Zinc standard solution: transfer 20.00mL of zinc standard stock solution to a 200mL volumetric flask. Dilute it to the mark with water, mix it, and transfer it to a plastic bottle for storage. This solution contains 10ug zinc per ml. 4 Instruments
Atomic absorption spectrometer, with lead, copper and zinc hollow cathode lamps. Under the working conditions of the instrument, any atomic absorption spectrometer that can meet the following indicators can be used. Sensitivity: The characteristic concentrations of lead, copper and zinc should not exceed 0.11ug/ml, 0.018ug/mL and 0.008ug/mL respectively. Precision: The standard deviation of the absorbance measured 11 times with the highest concentration standard solution shall not exceed 1.50% of its average absorbance. The standard deviation of the absorbance measured 11 times with the lowest concentration standard solution (not the "zero" standard solution) shall not exceed 0.50% of the average absorbance of the highest concentration standard solution.
Linearity of working curve: Divide the working curve into 5 sections according to concentration. The ratio of the absorbance difference of the highest section to the absorbance difference of the lowest section shall not be less than 0.90.
See Appendix A (Suggested Appendix) for instrument working conditions. 5 Analysis steps
5.1 Test material
Weigh 0.5g of sample to an accuracy of 0.0001g. Perform 2 independent measurements and take the average value. 5.2 Blank test
Carry out a blank test with the sample
5.3 Determination
5.3.1 Dissolution
5.3.1.1 Samples with lead content of 0.0010%~0.010%, copper content of 0.00020%~0.0030%, and zinc content of 0.00020%0.00050%.
5.3.1.1.1 Weigh 1.000g of the sample and place it in a 250ml beaker. Note: When measuring zinc, a polytetrafluoroethylene beaker or a zinc-free beaker should be used. 5.3.1.1.2 Add 15 mL of aqua regia (3.10) and heat on a low-temperature electric furnace until the sample is completely dissolved. Add 1.0 mL of sulfuric acid (3.11) along the wall of the cup and heat to evaporate until just smoking. Cool slightly and add 5 mL of hydrochloric acid and hydrobromic acid (3.8) along the wall of the cup. Warm and evaporate until smoking, cool, and repeat this operation once to volatilize and remove most of the tin. Note: When lead is not determined, do not add sulfuric acid and evaporate to nearly dryness. 5.3.1.1.3 Add 5 mL of hydrochloric acid (3.5) along the wall of the cup, warm until the residue is completely dissolved, and cool. Transfer to a 25 mL volumetric flask, dilute to the mark with water, and mix well. The following operations are carried out according to 5.3.2. 5.3.1.2 For samples with lead, copper and zinc contents greater than those in 5.3.1.1, place the sample (5.1) in a 100 mL polytetrafluoroethylene beaker or zinc-free beaker, add 7 mL of hydrochloric acid (3.1), add 1 mL of hydrogen peroxide in 4 to 6 portions, warm until the sample is completely dissolved, cool, transfer to a 50 mL volumetric flask, dilute to scale with water, mix well, and proceed as in 5.3.2.
5.3.2 Measurement
At an atomic absorption spectrometer with a wavelength of 283.3 nm324.8nm and 213.9nm, use air-acetylene flame, adjust to zero with water, and measure the absorbance of lead, copper and zinc respectively while measuring the standard solution series, subtract the absorbance of the blank test solution accompanying the sample, and find the corresponding lead, copper and zinc concentrations from the .1 function line 86
. 5.4 Drawing of working curve
GB/T 3260.9--2000
5.4.1 Drawing of lead working curve, transfer 0, 1.00, 2.00, 4.00, 6.00, 8.00, 10.00mL of lead standard solution to 100ml volumetric bottles, dilute to scale with hydrochloric acid (3.6), and mix well. Measure the absorbance of the standard solution under the same conditions as the sample determination, with concentration as the horizontal axis and absorbance (minus the absorbance of the "zero" concentration solution) as the vertical axis, and draw the working curve. 5.4.2 Drawing of copper working curve: Pipette 0, 0.50, 1.00, 2.00, 3.00, 4.00 mL of copper standard solution and place them in a group of 100 mL volumetric flasks, dilute to scale with hydrochloric acid (3.6), and mix well. Measure the absorbance of the standard solution under the same conditions as the sample determination, with the copper concentration as the horizontal axis and the absorbance (minus the absorbance of the "zero" concentration solution) as the vertical axis to draw a working curve. 5.4.3 Drawing of the zinc working curve: weigh 0, 0.50, 1.00, 2.00, 3.00, 4.00, 5.00mL of zinc standard solution into a group of 100mL volumetric flasks, dilute to the scale with hydrochloric acid (3.6), mix, transfer to a plastic bottle for storage, and measure the absorbance of the standard solution under the same conditions as the sample determination, with the zinc concentration as the horizontal axis and the absorbance (minus the absorbance of the "zero" concentration solution) as the vertical axis to draw a curve. Expression of analysis results
Calculate the percentage of lead, copper and zinc according to formula (1): Ph(Cu.Zn)(%) = : V.× 10~
Formula 4: c-..lead, copper, zinc content obtained from the working curve, μg/ml; V.-total volume of the test solution, ml.
m.-mass of the test material, g.
The result is expressed to three decimal places; if the element content is less than 0.010%, it is expressed to four decimal places. Allowable difference
The difference between the analysis results of laboratories should not be greater than the allowable difference listed in Table 1, Table 2, and Table 3. Table 1
0. 001 0~- 0. 003 0
0. 003 0~ 0. 005 0
>0. 005 0~0. 010
0. 010~ 0. 030
*0. 0300.050
>0.050～0.10
Steel containing base
0. 000 20 ~-0. 000 50
0. 000 50~0. 001 0
≥0. 001 0~~ 0. 003 0
0. 003 0~-0. 005 0
0. 005 0~ 0. 010
0. 010~~ 0. 020
Admission difference
Permit coupon
Zinc content
0. 000 20~ 0. 000 50
0. 000 50~ 0. 001 0
2 0. 001 0- 0. 002 0
>0. 002 0~~0. 005 0bZxz.net
GB/T 3260. 92000
Allowance difference
GB/T 3260. 9---2000
Appendix A
(Suggested Appendix)
Instrument working conditions
Use WFX-ID atomic absorption spectrometer to determine the amount of lead, copper and zinc. The reference working conditions are shown in Table A1. Table A1
Determination scheme
Lamp current
Spectral passband
Burner height
Air flow rate
Fast flow point
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