SJ 3199-1989 Determination of zinc and lead in vacuum silicon aluminum alloy Atomic absorption spectrophotometry SJ3199-1989 standard download decompression password: www.bzxz.net

Standard of the Ministry of Machinery and Electronics Industry of the People's Republic of China Determination of zinc and lead in vacuum silicon aluminum alloy Atomic absorption spectrophotometry
1 Main content and scope of application
1.1 Subject content
SJ3199--89wwW.bzxz.Net
This standard specifies the materials, instruments, reagents and preparation of lead and zinc standard solutions for the determination of lead and zinc by atomic absorption spectrophotometry.
1.2 Scope of application
This standard is applicable to the determination of zinc and lead in vacuum silicon aluminum alloy, and the determination range is 0.0010～0.010%. 2 Method summary
The sample is dissolved in dilute hydrochloric acid, and after separating silicon, the standard series method is used to determine zinc and the standard addition method is used to determine lead under the best working conditions of the instrument with an air-acetylene flame. 3 Reagents
a. GR hydrochloric acid, 1+1
b, GR nitric acid, 1+2, 1+1,
Zinc standard solution 1.0mg/ml, 0.10mg/mlc
d. Lead standard solution 1.0mg/ml, 0.10mg/ml, 4 Preparation of zinc and lead standard solutions
4.1 Weigh 0.5000g of metallic zinc (purity not less than 99.9%) and heat to dissolve in 20ml hydrochloric acid (1+1), transfer to a 500ml volumetric flask, dilute to scale with water, and shake well. This solution is 1.0mg zinc/ml (solution A). Take 20.0ml of solution (A) in a 200ml volumetric flask, dilute to scale with water, and shake well. This solution is 0.10mg zinc/ml (solution B).
4.2 Weigh 0.5000g of metallic lead (purity not less than 99.9%), heat and dissolve in 20ml (1+2) nitric acid, transfer to a 500ml volumetric flask, dilute to scale with water, and shake well. This solution is 1.0mg lead/ml (solution C). Take 20.0ml of solution (C) in a 200ml volumetric flask, dilute to scale with water, and shake well. This solution is 0.10mg lead/ml (solution D).
5 Equipment
Approved by the Ministry of Machinery and Electronics Industry of the People's Republic of China on February 10, 1989, implemented on March 1, 1989
SJ3199-89
WFX-IE type
a. Atomic absorption spectrophotometer
b, zinc, lead hollow cathode lamp.
6 Analysis steps
Weigh 0.5g of sample into a 150ml beaker, add 10ml of nitric acid, heat to dissolve, add 5ml of nitric acid, boil to remove nitride, evaporate the solution to near dryness, add about 10ml of water, heat to dissolve, transfer to a 50ml container, dilute to scale with water, dry filter and then measure the atomic absorption front. Add 0, 15-1.50mg to the sample and measure according to the best working conditions of the instrument in the table below. Table
Determination of elements
Absorption line wavelength
Energy gain passband width
7 Drawing of working curve
7.1 Determination of zinc
Lamp current
Burner height
Ethanol flow rate
Air vapor
While dissolving the sample, add the same amount of hydrochloric acid and nitric acid as the sample into 5 150ml beakers, add 0.0, 25.0, 50.0, 75.0, and 100.0μg of zinc standard solution (solution B) respectively, heat and evaporate to nearly 300℃, transfer into a 50ml bottle, dilute with water to 600℃, shake, and filter. According to the above conditions, draw a working curve of absorbance against zinc concentration.
7.2 Determination of lead
In five 150ml beakers, weigh 0.5000g of sample, add the same amount of hydrochloric acid and nitric acid as the sample, add 0.0, 150.0, 200.0, 250.0, 300.0μg of lead standard solution (solution D) respectively, heat to dissolve, evaporate to nearly dry, transfer to a 50ml volumetric flask, dilute to scale with water, shake well, dry filter, and draw a standard curve of absorbance versus lead concentration under the above conditions.
8 Calculation of analysis results
-×100%
Where: A-measured zinc (lead) content of the sample (μg) G sample weight (g).
Note: Find the total lead content corresponding to its absorption value from the working curve, deduct the amount of lead added, and the total lead content of the sample is obtained. 9 Method Sugar Content
Z..±5.0×10-
Additional Notes,
SJ3199--89
Pet±8.0×10*
This standard was proposed by the Electronic Standardization Research Institute of the Ministry of Machinery and Electronics Industry. This standard was drafted by the 744th Factory.
The main drafter of this standard: Dai Youyun.
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