GB/T 3260.1-2000 Chemical analysis method for tin - Determination of copper content

This standard specifies the determination method of copper content in tin. This standard is applicable to the determination of copper content in tin. Determination range: 0.00030% to 0.10%. GB/T 3260.1-2000 Chemical analysis method for tin Determination of copper content GB/T3260.1-2000 Standard download decompression password: www.bzxz.net

GB/T3260.1—2000
This standard is a revision of GB/T3260.1-—1982 "Chemical Analysis Methods of Tin - Determination of Copper by New Copper Reagent Photometric Method". The main contents of the revision are:
Change the organic phase photometric determination by dichloromethane extraction to the direct photometric determination by aqueous phase color development; Change the sample weight from 0.5~1 to (.5~2 more); and specify the sampling volume and test solution volume for different copper contents; Change the absorption blood from 2 cm to 3 cmt
Add 0.5mL of thiourea solution (50g/L) and hydroxylamine solution before color development; Change the new copper reagent solution from 5 mL to 3 mL. This standard complies with:
CB/T1.1-1993 Standardization Guidelines Unit 1: Rules for drafting and expressing standards Part 1: Basic provisions for standard writing
GB/T1.4-1988 Standardization Guidelines Provisions for the preparation of chemical analysis methods GB/T1467-1978 General principles and general provisions for chemical analysis methods for metallurgical products G13/T7729-1987 General principles for spectrophotometric methods for chemical analysis of metallurgical products GR/T17433-1998 Fundamentals of chemical analysis of metallurgical products Terminology This standard shall replace GB/T3260.1·-1982 from the date of implementation. This standard is 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 the Yunnan Tin Company Research and Design Institute. The main drafters of this standard are: Bai Jiayuan and Yang Bokang. 1 Scope
National Standard of the People's Republic of China
Chemical analysis method of tinDetermination of copper content
Methods fur chenical analysis of tinDetermination of copper contentThis standard specifies the determination method of tin content: This standard is applicable to the determination of copper content in tin. Determination range: 0.00030%~0.10. 2 Method summary
GB/T 3260.1-2000
Replaces GB/T 3260.1-1982
The sample is dissolved with hydrochloric acid and hydrogen peroxide, and copper () is reduced to copper () with hydroxylamine hydrochloride at pH 5~-7 to form a yellow complex with the new copper reagent. The absorbance of the aqueous phase is directly measured at a wavelength of 460nm in the spectrophotometer. Ammonium citrate is added to prevent the hydrolysis of tin and other gold ions, and thiourea is added to prevent silver from forming silver chloride precipitation. Tin and its coexisting elements do not interfere with the determination.
3 Reagents
Hydrochloric acid (ol.19 g/mL)
Hydrogen peroxide (30%).
Hydrochloric acid (1+19),
Ammonia water (2+1).
Hydroxylamine hydrochloride solution (100g/1.):
Thiodol solution (50g/L)
3.7Ammonium citrate solution (500g/L),
3.82,9-dimethyl-1,10-phenanthroline (neucoporin) solution (1g/L); weigh 0.1g of neucoporin and dissolve it in 100ml of anhydrous ethanol. Www.bzxZ.net
3.9 Copper standard stock solution: Weigh 0.1000g of copper (299.99%) and place it in a 100ml beaker, add 5ml of hydrochloric acid (3.1), cover with table III, add 1m hydrogen peroxide, heat until completely dissolved and boil to drive off free chlorine, cool slightly, blow water to wash the table and the wall of the cup. After cooling, transfer to a 100ml volumetric bottle, dilute to the mark with old water, and mix. This solution contains 100 μg of copper in 1 mL. 3.10 Copper standard solution: Transfer 50.00ml of copper standard stock solution to a 1000mL volumetric flask, add 2mL of hydrochloric acid (3.1), dilute to the mark with water, and mix. This solution contains 5 pg of copper in 1 mL. 4 Analysis steps
4.1 Test materials
Weigh the sample according to Table 1, accurate to 0.0001 g. Approved by the State Administration of Quality and Technical Supervision on 200008-28 2
Implemented on 2000-12-01
Steel content, %
U. 000 30-~0. 000 50
>0. 000 50 ~0, 005 0
>0, 005 0~0. 010
0. 010~0. 060
>0. 060-0. 10
Sample quantity,
Carry out 2 independent measurements and take the average value. 4.2 Blank test
Carry out a blank test with the sample.
4.3 Determination
GB/T 3260. 1 2000
Add hydrochloric acid during decomposition, mL
Total volume of test solution, mL
Taken volume, ml
Full determination
Full determination
Full determination
4.3.1 Place the sample (4.1) in a 100mL beaker, cover with blood, add 10~15mL hydrochloric acid (3.1), add hydrogen peroxide drop by drop until the sample is completely dissolved and then add 3 drops of excess, heat and boil until there are no small bubbles, remove blood. Evaporate to about 1 mL, remove and cool. Note: When the copper base in the weighed sample is less than 50%, proceed from 4.3.3 below. 4.3.2 Transfer to a 50 or 100 mL volumetric flask, wash the beaker with hydrochloric acid (3.3) several times, and transfer to a sudden volumetric flask and dilute to the mark, stir with a spoon, transfer 5.00 ml of the test solution to a 100 mL beaker, and place it on a low-temperature electric stove to evaporate to about 1 ml. 4.3.3 Add 10 mL of ammonium citrate solution, mix to dissolve soluble salts, add 3 ml of hydroxylamine hydrochloride solution, 0.5 ml of thiourea solution, mix well, neutralize with nitrogen water to about pH 6.2 (test with precision pH test paper), add 3 mL of new copper reagent solution and mix well. 4.3.4 Transfer to a 25 ml colorimetric tube, dilute to the mark with water, mix well, and let stand for 5 minutes. 4.3.5 Transfer part of the test solution into a 3 cm absorbent tube and use the blank test solution accompanying the test sample as a reference. Measure its absorbance at 460 nm on a spectrophotometer and find out the corresponding copper amount from the working curve. Draw the following curve: 4.4T
4.4.1 Transfer 0, 0.50, 1.00, 2.00, 4.00, 6.00, 8.00 and 10.00 mL of copper standard solution into a 100 mL beaker and evaporate it to about 1 mL on a low temperature electric stove. Remove the beaker and cool it slightly. Proceed as in 4.3.3 to 4.3.4. 4.4.2 Under the same conditions as for the test sample, use the reagent blank as a reference and measure the absorbance of the standard solution. Use the copper amount as the abscissa and the absorbance as the ordinate to draw the following curve.
5 Expression of analysis results
Calculate the percentage of copper according to formula (1):
Cu(%) = m:V.× 10-s
Wherein: m1—the amount found from the working curve,: Vr
—the volume of the test solution, ml.:
the total volume of the test solution, mL,
—the mass of the test material, 8,
The result is expressed to two decimal places. If the copper content is less than 0.10%, it is expressed to three decimal places; if it is less than 0.010%, it is expressed to four decimal places; if it is less than 0.001 0%, it is expressed to five decimal places. 6 Allowable difference
The difference between the analysis results of laboratories should not be greater than the allowable difference listed in Table 2. Copper content
0. 000 30 ~0. 000 50
>0.000 50~0. 001 0
>0.001 ~1.003 0
20. 003 0-~0. 005 0
GB/T 3260. 1—2000
Allowance
0. 000 20
0. 000 30
Copper content
>0.C050~0,010
>0. 010--0. C30
>0. 030~-0. 060
2*0. 060~-[h. 10
Allowable difference
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