GB/T 4103.3-2000 Chemical analysis methods for lead and lead alloys - Determination of copper content
Some standard content:
GB/T 4103.3-2000
This standard is a revision of GB/T4103.5--1983 "Chemical analysis method for lead-based alloys - Dicyclohexanone oxalyl spectrophotometric method for the determination of copper content" and GB/T472.1-1984 "Chemical analysis method for lead ingots - Diacetaldehyde oxalyl ditracemetric spectrophotometric method for the determination of copper content". This standard complies with:
Guidelines for Standardization Work Unit 1: Rules for Drafting and Presenting Standards Part 1: Basic Provisions for Standard Writing
GB/T 1.1—1993
Basic Provisions
GBT1.4---1988Guidelines for Standardization Work Provisions for the Preparation of Chemical Analysis Methods Standards GB/T1467-1978General Principles and General Provisions for Chemical Analysis Methods of Metallurgical Products Standards GB/T7729.-1987General Rules for Spectrophotometric Methods for Chemical Analysis of Metallurgical Products GB/T17433-1998Basic Terminology for Chemical Analysis of Metallurgical Products Appendix A of this standard is a reminder appendix.
This standard replaces GB/T4103.5—1983 and GB/T472.1—1984 from the date of its entry into force. 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 Shenyang Smelter and Northwest Copper Processing Plant of Baiyin Nonferrous Metals Company. This standard was drafted by Huludao Zinc Plant.
The main drafter of this standard: Li Chengwen.
1 Scope
National Standard of the People's Republic of China
Chemical analysis method of lead and lead alloys
Determination of copper content
Methods for chemical analysis of lead and lead alloys--Determination of copper content This standard specifies the method for determination of copper content in lead and lead alloys. GB/T 4103. 3 - 2000
Replaces GB/T 4103.5--1983
GB/T 472.1--1984
This standard applies to the determination of copper content in lead and lead alloys. Determination range: 0.00050%~0.60%. 2 Method Summary
The sample is decomposed with nitric acid, and the lead matrix is separated with sulfuric acid. In a dilute acid medium, the absorbance of copper is measured at a wavelength of 324.7nm using an air-acetylene flame on an atomic absorption spectrometer. When the sample contains a large amount of tin and antimony, it is dissolved with a tartaric acid-nitric acid mixture. 3 Reagents
3.1 Tartaric acid.
3.2 Nitric acid (pl.42g/ml).
3.3 Hydrochloric acid (pl.19g/mL).
3.4 Perfluoric acid (pl.67g/ml).
3.5 Sulfuric acid (1+1).
3.6 Nitric acid (1+4).
3.7 Sulfuric acid (2+-98).
3.8 Tartaric acid-nitric acid mixed acid: Weigh 5g tartaric acid (3.1), dissolve in 100ml nitric acid (3.6), and mix. 3.9 Copper standard stock solution: Weigh 5.0000g metallic copper (>99.99%) and place in a 250ml beaker. Add 20ml nitric acid (1+1), cover with a watch glass, place on a hot plate and dissolve completely at low temperature, boil slightly to remove nitrogen oxides, remove, rinse watch III and the wall of the beaker with water, cool to room temperature, transfer to a 250ml volumetric flask, dilute to scale with water, and mix. This solution contains 20mg copper in 1ml. 3.10 Copper standard solution: Transfer 5.00ml copper standard stock solution (3.9) to a 1000ml volumetric flask, dilute to scale with water, and mix. This solution contains 100μg copper in 1ml.
3.11 Copper standard solution: Pipette 10.00mL of copper standard storage solution (3.9) into a 500mL volumetric flask, dilute to scale with water, and mix with a spoon. This solution contains 400μg of copper per ml.
4 Instruments
Atomic absorption spectrometer, with copper hollow cathode lamp. Under the best working conditions of the instrument, any instrument that can meet the following indicators can be used. Sensitivity: In a solution consistent with the matrix of the measurement solution, the characteristic concentration of copper should not exceed 0.045μg/mL Precision: Measure the absorbance 10 times with the highest concentration standard solution, and its standard deviation should not exceed 0.8% of the average absorbance: Measure the absorbance 10 times with the lowest concentration standard solution (not the "zero" standard solution) and its standard deviation should not exceed 0.4% of the average absorbance of the highest standard solution
Working curve linearity: Divide the working curve into 5 sections according to concentration, and the ratio of the absorbance difference of the highest section to the absorbance difference of the lowest section should not be less than 0.9.
Instrument working conditions are shown in Appendix A (Suggested Appendix). 5 Analysis steps
5.1 Test sampleWww.bzxZ.net
Weigh the sample according to Table 1, accurate to 0.0001g. Table 1
Feed content.%
Test sample pad
0.00050~~0.003 0
Carry out 2 independent determinations and take the average value. 5.2 Blank test
Carry out a blank test along with the test sample.
5.3 Determination
5.3.1 Dissolution and treatment of test sample
5.3.1.1 Test sample with a content of 0.00050% to 0.025% 3>0. 003 0~~ 0. 025
-0. 025 .0.
」：（)
5.3.1.1.1 Place the sample (5.1) in a 300mL beaker, add nitric acid (3.6) according to Table 2, cover with Table m, decompose completely on the electric hot plate 1, continue to steam until a large number of crystals appear, remove, rinse Table III and the wall of the cup with water, add a little water, shake to dissolve all the crystals 5.3.1.1.2 Add 5ml sulfuric acid (3.5), mix well, let stand for 15min, filter the precipitate with filter paper, wash the beaker and precipitate with sulfuric acid (3.7) 5 to 6 times, and cover the filtrate in a 300ml beaker. Place the filtrate on the electric hot plate and heat and steam until the white smoke disappears, remove, and cool to room temperature. 5.3.1.1.3 Add 3mL nitric acid (3.2) along the wall of the cup, rinse the wall of the cup with a small amount of water, heat slightly on the electric hot plate until boiling, dissolve the salts, remove, and cool to room temperature. Transfer the solution to the volumetric flask specified in Table 2, dilute to the mark with water, mix well, Table 2
Copper containing disk
0. 000 50~~0. 003 0
>0. 003 0~0. 025
0. 025 ~0. 20
>0. 20~0. 60
Amount of acid added to decompose sample
Total volume of dilution
Volume taken
Base volume measured
5.3.1.1.4 For samples containing impurities such as high tin and antimony, which are not completely decomposed by dilute nitric acid, add tartaric acid-nitric acid mixture according to Table 2, and proceed as per 5.3.1.1.1 to 5.3.1.1.2. When the filtrate is evaporated until the tartaric acid is carbonized, remove it, cool it slightly, add 3 to 5 mL of pernitrogen acid along the wall of the cup, evaporate it on a hot plate until the white smoke is gone and the perchloric acid is completely driven out, remove it, and cool it to room temperature. Add 3mL hydrochloric acid, 0.5~1g tartaric acid and a little water. Heat on a hot plate to dissolve the salts, remove, cool to room temperature, transfer to the volumetric flask specified in Table 2, dilute to scale with water, and mix well. 5.3.1.2 Test materials with copper content > 0.025%~0.60% 5.3.1.2.1 Test materials (such as those containing high tin and high antimony, which are not completely dissolved by dilute nitric acid, need to add 15mL tartaric acid-nitric acid mixed acid) are treated according to 5.3.1.1.1 and cooled to room temperature. Transfer the solution to a 100mL volumetric flask, dilute to scale with water, and mix. 5.3.1.2.2 Take 20.00mL of the solution, transfer to a 100mL volumetric flask, add 3ml of nitric acid (3.2), dilute to scale with water, and mix well.
5.3.2 Measurement
Take the above solutions (5.3.1.1.3 or 5.3.1.1.4; 5.3.1.2.2) and place them in the original absorption spectrometer at a wavelength of 324.7 mm. At the same time as measuring the standard solution series of GB/T 4103. 3-2000
, use a gas-acetylene flame and adjust the zero value with water to measure the absorbance of the sample solution. Find the corresponding copper concentration from the curve below.
5.4 Drawing of the curve
5.4.1 Working curve of the sample with a copper content of 0.00050% to 0.20% 5.4.1.7 Take 0.0.50.1.00.2.00.3.00,4.00.5.00ml. copper standard solution (3.10), respectively in a 100ml volumetric flask: add 3ml nitric acid (3.2) (if the test solution is hydrochloric acid medium, add 3mL hydrochloric acid), dilute with water to the scale, and mix. 5.4-1.2 Under the same conditions as the test solution, measure the absorbance of the standard solution, subtract the absorbance of the "zero" standard solution, and draw a working curve with the steel concentration as the horizontal axis and the absorbance as the vertical axis. 5.4.2 Working curve for samples with copper content > 0.20%~0.60% Only the copper standard solution is transferred as the reagent in 3.11. Follow 5.4.1.1~5.4.1.2. 6 Expression of analysis results
Calculate the percentage of copper according to formula (1):
Cu(%) = (Gi - c)V..V, × 10-6mo.V
Where: -The copper concentration obtained from the curve, μg/ml. The copper concentration of the blank solution accompanying the sample, μg/ml; V.----Total volume of the test solution, mL,
V,…--The volume of the test solution taken, ml.;
V. The volume of the diluted test solution, mI.; m-The mass of the sample, g.
The result is expressed to two decimal places. If the copper content is less than 0.10%, it is expressed to three decimal places: less than 0.010%, it is expressed to four decimal places; less than 0.0010%, it is expressed to five decimal places, 7 Allowable difference
The difference between the analysis results of the experimental rates should not be greater than the allowable difference listed in Table 3. Table 3
0. 000 50~~0. 002 ()
0. 002 0 - 0. 010
>0.010~0. 050
>0.050~~0.10
20. 10~0. 30
≥0. 30 -- 0. 60
Allowed
GB/T4103.3-2000
Appendix A
(Suggested Appendix)
Instrument Working Conditions
Use WFX-1C Atomic Absorption Spectrometer to measure the working conditions of copper as shown in Table A1: Table A1
Lamp Current
Spectral Bandwidth
Burner Height
Air Flow
Heat Flow Hall
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