This standard specifies the determination method of calcium in lead alloys. This standard is applicable to the determination of calcium in lead alloys. Determination range: 0.010% to 0.15%. GB/T 4103.9-2000 Chemical analysis method for lead and lead alloys Determination of calcium content GB/T4103.9-2000 Standard download decompression password: www.bzxz.net

GB/T4103.9-2000
This standard is a revision of GB/T4103.11--1983 "Chemical analysis method of lead-based alloys - Determination of calcium content by atomic absorption spectrophotometry".
This standard complies with:
GB/T1.1--1993 Guidelines for standardization work
Unit 1: Rules for drafting and expressing standards Part 1: Basic provisions for standard writing
GB/T1.4--1988 Guidelines for standardization work - Provisions for writing standards for chemical analysis methods GB/T1467-1978 General principles and general provisions for standards for chemical analysis methods of metallurgical products GB3/T7728-1987 General principles for chemical analysis of metallurgical products by flame atomic absorption spectrometry GB/T17433-1998 Basic terms for chemical analysis of metallurgical products Appendix A of this standard is a prompt appendix.
This standard replaces GB/T4103.11-1983 from the date of 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 Zhuzhou Smelter.
The main drafters of this standard are Zhang Liping and Chen Ke. 137
1 Scope
National Standard of the People's Republic of China
Chemical analysis methods of lead and lead alloys
Determination of calcium content
Methods for chemical analysis of lead and lead alloys--Determination of calcium content This standard specifies the determination method of calcium in lead alloys. This standard is applicable to the determination of calcium in lead alloys. Determination range: 0.010%~~0.15%. 2 Method Summary
GB/T4103.9.2000
Replaces GB/T1113.J11933
The sample is dissolved with nitric acid and tartaric acid. In dilute nitric acid medium, lanthanum salt is used as a release agent, and air·acetylene flame is used to measure the absorbance of calcium at a wavelength of 422.7nm on an original absorption spectrometer. 3 Reagents
The water used in this method is double distilled water or deionized water. 3.1 Sample dissolving acid: Weigh 30g of tartaric acid and dissolve it in 500mL nitric acid (1+2). Mix well. 3.2 Lanthanum solution (50g/L): Weigh 5.87g of lanthanum oxide, place it in a 250ml beaker, add 10ml of nitric acid (o1.42g/ml. high-grade pure), heat to dissolve and dilute to 100ml, mix well. 3.3 Lead solution: Weigh 10.0g of pure lead (99.99%), place in a 250ml beaker, add 30ml of nitric acid (112), and dissolve completely at low temperature. Remove, cool, transfer to a 100mL volumetric flask, dilute to scale with water, and mix. This solution contains 0.1g in 1ml. 3.4 Aluminum bath: Weigh 0.100g of aluminum flakes (aluminum ≥ 99.9※, calcium <0.01%) in a 250ml beaker, slowly add 20ml of hydrochloric acid (1 + 1), heat at low temperature until completely dissolved, cool, transfer to a 1000ml volumetric flask, dilute to full scale with water, and mix. This solution contains 100 μg Aluminum,
3.5 Calcium standard stock solution: Accurately weigh 2.4972g of high-grade pure calcium carbonate (pre-heated at 105~~110 (dry for 1h in a desiccator. Cool to room temperature) in a 250ml beaker, add 60ml nitric acid (112), heat at low temperature to dissolve, boil, cool, transfer to a 100ml volumetric flask, dilute to scale with water, and mix. This solution contains 1mg calcium in 1mL. 3.6 Calcium standard solution: Transfer 10.00mL of calcium standard stock solution to a 100ml volumetric flask. Dilute to scale with nitric acid (!! 99). Mix. This solution contains 100μg calcium in 1ml.
4 Instrument
Atomic absorption spectrometry Instrument, with a calcium 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 calcium should not be greater than 0.12ug/ml. Precision: When the absorbance is measured 10 times with the standard solution of the highest concentration, its standard deviation should not exceed 1.0% of the average absorbance; when the absorbance is measured 10 times with the standard solution of the lowest concentration (not the "zero" standard solution), its standard deviation should not exceed 0.5% of the average absorbance of the highest standard solution.
CB/T 4103.9--2000
1 Linear curve: Divide the working curve into 5 sections according to the concentration. The ratio of the absorbance difference of the highest section to the absorbance difference of the lowest section shall not be less than 0.85
For instrument working conditions, see Appendix A (Suggested Appendix). 5 Analysis steps
5.1 Test materials
Weigh the test materials according to Table 1, accurate to 0.0001g. Table 1
0.010 ~0.040
-0. 040-- 0. 15
Carry out 2 independent determinations and take the average value. 5.2 Blank testbZxz.net
Test material
Weigh the pure lead (99.99%) that is equivalent to the test material. Add an equivalent amount of aluminum solution (3.4). Perform a blank test together with the test material. 5.3 Determination
5.3.1 Place the test material (5.1) in a 100ml beaker, add 10ml of dissolving acid, heat at low temperature until completely dissolved, remove and cool. 5.3.2 Transfer the test solution (5.3.1) into a 100ml volumetric flask, add 10.0ml of solution, dilute to the mark with water, and mix well. 5.3. 3 Use air: acetylene flame = - atomic absorption spectrometer at wavelength 422.7nm, adjust to zero with water, measure the absorbance of the test solution, subtract the absorbance of the blank solution accompanying the sample, and find the corresponding calcium concentration from the working curve. 5.4 Drawing of working curve
5.4.1 Working curve of calcium content 0.010%~0.040% 5.4.1.1 Take 0.1.00, 2.00, 3.00, 4.00.5.00mL of calcium standard solution and place them in 100ml volumetric flasks respectively, add 10.0mL of lead solution, 10ml of dissolving acid, and 10.0ml of lanthanum solution. Add an equivalent amount of aluminum solution to the sample, dilute to the mark with water, mix,
5.4.1.2 Under the same conditions as the sample, measure the absorbance of the standard solution, subtract the absorbance of the "zero" standard solution. Draw a working curve with calcium concentration as the horizontal axis and absorbance as the vertical axis. 5.4.2 Working curve for calcium content > 0.040% to 0.15% Take 0, 1.50, 3.00.4.50, 6.00, 7.50mL of calcium standard solution and place them in a group of 100mL volumetric flasks, add 5.0mL of lead solution, 10mL of sample dissolving acid, and 10.0mL of lanthanum solution. Add an equivalent amount of aluminum solution to the sample, dilute to the mark with water, and mix. The following is carried out according to 5.4.1.2.
6 Expression of analysis results
Calculate the percentage of calcium according to formula (1): V× 10-Ca(%) →
Where: - the concentration of calcium obtained from the curve, #g/ml; V, --- the total volume of the test solution, mL;
m the mass of the test material, g.
The result should be expressed to two decimal places. If the calcium content is less than 0.10%, it should be expressed to 1 decimal place. 139
Allowable difference
GB/T4103.9--2000
The difference between the analysis results of laboratories should not be greater than the allowable difference listed in Table 2. Table 2
Calcium content
0. 010--0. 040
>0.040~0.080
0. 080-~0. 15
Allowance difference
GB/T4103.9--2000
Appendix A
(Suggestive appendix)
Instrument working conditions
The working conditions for measuring calcium using WFX-1C atomic absorption spectrometer are shown in Table A1: Table A1
Lamp current
Spectral passband
Burner height
Air flow
Burner flow
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