This standard specifies the determination method of aluminum content in lead and lead alloys. This standard is applicable to the determination of aluminum content in lead, lead-calcium alloys, lead-tin and lead-calcium bearing alloys. Determination range: 0.0050% to 0.10%. GB/T 4103.13-2000 Chemical analysis method for lead and lead alloys Determination of aluminum content GB/T4103.13-2000 Standard download decompression password: www.bzxz.net

GB/T 4103.13-2000
This standard is formulated for the first time.
This standard complies with:
GB/T 1. 1--1993
Guidelines for standardization work
Basic provisions
GB/T1.4-1988Guidelines for standardization work
Unit 1: Rules for drafting and expressing standards Part 1: Rules for writing standards
Rules for writing standards for chemical analysis methods
GB/T1467—1978 General principles and general provisions for chemical analysis methods for 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 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 Shenyang Smelter.
The main drafters of this standard are Liu Guohong and Zhang Quan.
1 Scope
National Standard of the People's Republic of China
Chemical analysis method of lead and lead alloys
Determination of aluminium content
Methods for chemical analysis of lead and lead alloys-Determination of aluminium content This standard specifies the method for determination of aluminium content in lead and lead alloys. GB/T 4103.13—2000
This standard is applicable to the determination of aluminium content in lead, lead-calcium alloy, lead-tin and lead-calcium bearing alloy. Determination range: 0.0050%~0.10%. 2 Method Summary
The sample is dissolved in nitric acid, and the matrix lead is separated in the form of lead sulfate precipitation. In the hydrochloric acid (c(HCL)=0.6mol/L) medium, aluminum and chrome azuro blue S form a red complex, and its absorbance is measured at a wavelength of 545nm on a spectrophotometer. 3 Reagents
3.1 Hydrochloric acid (pl.19).
3.2 Hydrochloric acid (1+19).
3.3 Nitric acid (1+2).
3.4 ​​Sulfuric acid (1+1).
3.5 p-Nitrophenol solution (1g/1.).
3.6 Ammonium hydroxide (1+5).
3.7 Ascorbic acid solution (10g/L).
3.8 Thiourea solution (100g/L).
3.9 Chrome azuro blue S solution (1g/L): Weigh 0.100g of Chrome azuro blue S and dissolve it in 100mL of ethanol (1+1) solution. 3.10 Hexamethylenetetramine solution (400g/L), adjust to pH6.0 with a pH meter. 3.11 Aluminum standard stock solution: Weigh 0.1000g of pure aluminum (99.9%), add 10ml of hydrochloric acid (3.1), heat to dissolve. After cooling, transfer to a 1000mL volumetric flask, dilute to scale with water, and mix. This solution contains 100μg aluminum in 1ml. 3.12 Aluminum standard solution: Transfer 10mL of aluminum standard stock solution (3.11), place in a 500mL volumetric flask, add 5mL of hydrochloric acid (1+1), dilute to scale with water, and mix. This solution contains 2μg aluminum in 1ml. 4 Instruments
721 spectrophotometer.
5 Analysis steps
5.1 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 158
Implemented on December 1, 2000
Aluminum content%
0. 005 0-~0. 030
0. 030 ~0. 050
>0.050~0.10
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
GB/T 4103.13--2000
Sample amount, g
Total volume of solution. ml.
Volume of solution transferred, ml.
5.3.1 Place the sample (5.1) in a 250ml beaker, add 10mlL nitric acid, heat to dissolve, remove and cool. Wash the surface blood and the wall of the cup with water, add 8mL sulfuric acid, cool after precipitation occurs. 5.3.2 Transfer the test solution into the volumetric flask shown in Table 1, dilute to the scale, and mix well. 5.3.3 After the test solution is dry filtered, transfer the test solution according to Table 1 into a 100mL beaker, heat to evaporate thoroughly, remove, and add 5mL hydrochloric acid (3.1). Heat at low temperature to about 2mL and remove. Wash the surface blood and the wall of the cup with water, heat to boil and remove. 5.3.4 Transfer the solution into a 50mL volumetric flask, control the volume to about 15mL, add 2 drops of p-nitrophenol solution, adjust the solution to yellow with ammonium hydroxide, and then neutralize with hydrochloric acid (3.2) until the yellow disappears and an excess of 0.5mL is added. Add 1.0ml of ascorbic acid solution, 2.5ml of thiourea solution, 2.5ml of chrome azuro blue S solution, and 5.0mL of hexamethylenetetramine solution. Mix each reagent. Dilute with water to the mark, stir with a spoon, and let stand for 10 minutes.
5.3.5 Transfer part of the solution (5.3.4) into a 1cm absorption III, and measure its absorbance at a wavelength of 545nm on a spectrophotometer using the blank test solution accompanying the sample as a reference. Find the corresponding amount of aluminum from the working curve. 5.4 Drawing of working curve
5.4.1 Take 0, 1.00, 2.00, 4.00, 6.00, 8.00mL of aluminum standard solution and place them in a group of 50mL volumetric flasks respectively, control the volume to about 15mL, and proceed as per 5.3.4.
5.4.2 Transfer part of the solution (5.4.1) into 1cm absorption III, use the reagent blank as reference, measure its absorbance at a wavelength of 545nm on the spectrophotometer, and draw the working curve with the aluminum content as the horizontal axis and the absorbance as the vertical axis. 6 Expression of analysis resultswwW.bzxz.Net
Calculate the percentage of aluminum according to formula (1):
Al(%) m1 : V. × 10-s
Where: m—the aluminum content obtained from the working curve.ugV. --Total volume of test solution, mL;
V\--Volume of test solution taken, mL;
-Mass of test material, g.
× 100
The result is expressed to two decimal places. If the aluminum 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.
7 Allowable difference
The difference between the analysis results of laboratories should not be greater than the allowable difference listed in Table 2. 159
Aluminum content
0. 005 0~0. 010
>0. 010~-0. 030
0. 030~~0.060
≥0. 060~0. 10
GB/T 4103.13—2000
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