GB/T 3260.3-2000 Chemical analysis method for tin - Determination of bismuth content
Some standard content:
GB/T 3260.3--2000
This standard is a reconfirmation of (B/T3260.3-1982 "Chemical analysis method of tin - determination of bismuth by potassium iodide photometry", and makes clear provisions on the sample weighing and test solution separation. 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 the preparation of chemical analysis method standards
GB/T1467---1978 General principles and general provisions for chemical analysis method standards for metallurgical products GB/T7728--1987 General principles for chemical analysis of metallurgical products by flame atomic absorption spectrometry GB/T7729--1987 General principles for chemical analysis of metallurgical products by flame atomic absorption spectrometry General rules for chemical analysis spectrophotometry GB/T17433-1998 Basic terminology for chemical analysis methods of metallurgical products Appendix A in this standard is the standard appendix, and Appendix B is the indicative appendix. From the date of implementation, this standard will replace GB/T3260.3--1982. 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 Guangzhou Smelter and Yunnan Tin Company Research and Design Institute. The main drafters of this standard are: Fang Xiurui, Liu Shuhan, Deng Jianguang, Su Aiping, Lin Qingquan. 60
1 Scope
National Standard of the People's Republic of China
Chemical analysis methods for tin
Determination of quantity
Methods for chemical analysis of tinDetermination of bismuth contentThis standard specifies the determination method of bismuth content in tin. This standard is applicable to the determination of bismuth content in tin. Determination range: 0.0010%~0.080%. 2 Method summary
GB/T 3260. 3 2000
Replaces GB/T 3260.3:1982
The sample is decomposed with dry water, and tin, antimony, etc. are eliminated with hydrochloric acid-hydrobromic acid in the presence of sulfuric acid. Then, in the hydrochloric acid medium, bismuth forms a yellow complex with potassium iodide, and its absorbance is measured at a wavelength of 460nm on a spectrophotometer. The color developing solution contains 2.5mg lead, 0.3mg nickel, less than 20mg tin (V), 0.5mg iron, copper, arsenic. 0.04mg tin. Zinc, indium, antimony and citrate, sulfate and chloride do not interfere with the determination. 3 Reagents
3.1 Hydrochloric acid (pl.19 g/mL).
3.2 Aminobromic acid (pl.49 g/ml.).
3.3 Nitric acid (ol.42 g/mL).
3.4 Nitric acid (1+2).
3.5 Sulfuric acid (1+1).
3.6 Hydrochloric acid (1-4.9).
3.7 Aqua regia: Mix 1 volume of nitric acid (3.3) and 3 volumes of hydrochloric acid (3.1). 3.8 Hydrochloric acid and hydrobromic acid: Mix equal volumes of hydrochloric acid (3.1) and oxybromic acid (3.6). 3.9 Citric acid solution (500 g/L).
3.10 Potassium iodide solution (200 g/1.).
3.11 Thiourea solution (100 g/L).
Sodium chloride solution (200g/L): Prepare 3.13 Bismuth standard stock solution with hydrochloric acid (3.6): Weigh 0.1000g of metallic bismuth (99.99%), put it in a 250mL beaker, add 1ml of nitric acid (3.4), heat and dissolve it completely, add 20mL of sulfuric acid (3.5), heat and evaporate until white smoke appears, cool, purge the cup wall with a little water. Evaporate again until smoke appears, cool, dissolve with hydrochloric acid (3.6), transfer to a 1000mm volumetric flask, dilute to scale, and mix. This solution contains 100g bismuth in 1ml.
3.14 Bismuth standard solution: Transfer 100.00mL of bismuth standard stock solution to a 500mL volumetric flask, dilute to scale with hydrochloric acid (3.6), and mix. This solution contains 20μg bismuth in 1ml.
Approved by the State Administration of Quality and Technical Supervision on 2000-08-28, implemented on 200012-01
4 Analysis steps
4.1 Test sample
Weigh the test sample according to Table 1, accurate to 0.0001g. Content of chromium
0. 001 0- 0. 005 0
-0. 005 0~0. 010
0. 010 -- 0. 020
0, 020~- 0. 080
GB/T 3260.3 2000
Test sample quantity
Carry out 2 independent determinations and take the average value. 4.2 Blank test
Carry out a blank test along with the test sample.
4.3 Determination
Total volume of test solution, ml.
Full determination
Full determination
Full determination
Volume of fraction, ml
4.3.1 Place the sample (4.1) in a 150mL beaker, add 8-15mL aqua regia according to the sample weight, cover with a beaker, warm and dissolve completely, remove the beaker, add 1mL sulfuric acid, heat and evaporate until white smoke appears, cool, add 5mL hydrochloric acid-hydrobromic acid, heat and evaporate until white smoke appears, repeat this operation 1~~2 times, then add 1 drop of nitric acid (3.3), continue to evaporate until white smoke appears, cool. Add about 5mL hydrochloric acid (3.6). Heat slightly to dissolve soluble salts, cool.
Note: If the amount of lead in the sample exceeds 3mg, use 5mL sodium chloride solution instead of hydrochloric acid (3.6). 4.3.2 Use hydrochloric acid (3.6) to transfer the test solution into a 50ml volumetric flask and dilute to the mark, mix well. Transfer 10.00ml of the test solution into a 25ml volumetric flask,
Note: If the bismuth content in the sample is less than 0.020%, it is not necessary to proceed to 4.3.2. Transfer all the test solution into a 25ml volumetric flask and proceed from 4.3.3.
4.3.3 Add 1ml of citric acid solution, 3ml of thiourea solution, and 5ml of potassium iodide solution. Mix well after adding each reagent, dilute to the mark with hydrochloric acid (3.6), and mix well.
4.3.4 Transfer part of the test solution into a 3cm absorption III, use the empty test solution accompanying the sample as a reference, and measure the absorbance at a wavelength of 460nm on a spectrophotometer. Find the corresponding bismuth content from the working curve. 4.4 Drawing of the curve
4.4.1 Transfer 0, 1.00, 2.00, 3.00, 4.00, 5.00, 6.00 ml of the bismuth standard solution to a set of 25 ml volumetric flasks, add hydrochloric acid (3.6) to about 10 ml, and proceed as in 4.3.3. 4.4.2 Under the same conditions as the test sample, measure the absorbance of the standard solution with the reagent blank as the reference. Draw the working curve with bismuth as the abscissa and absorbance as the ordinate.
5 Expression of analysis results
Calculate the percentage of bismuth according to formula (1):
m -V, × 10\
Bi(%)=
Wherein: m·the amount of bismuth found from the working curve, μg; V. -Total volume of test wave, mL
Volume of test solution, mL.
---Mass of sample for photometric determination·&mo.V
The result is expressed to three decimal places. If the content is less than 0.010%, it is expressed to four decimal places. 62
6 Allowable difference
GB/T3260.3--2000
The difference between the analysis results of the experimental cases should not be greater than the allowable difference listed in Table 2. Table 2
Bi content
0.0010~0.0050
≥0. 005 0~ 0. 010
>0.010~~0.030
>0.030~0.060
>0.0600.080
Allowable difference
A1 range
GB/T3260.3—-2000
Appendix A
(Appendix to the standard)
Determination of bismuth content by flame atomic absorption spectrometry
This standard specifies the determination method of bismuth content in tin. This standard is applicable to the determination of bismuth content in tin. Determination range: 0.00030%~0.020%. A2 Method Summary
The sample is decomposed with dilute aqua regia in the presence of a small amount of sulfuric acid and sodium salt, and tin is removed with hydrochloric acid-hydrobromic acid. The absorbance of bismuth is measured at a wavelength of 223.06nm using an air-acetylene flame in the dilute aqua regia medium on an atomic absorption spectrometer. A3 Reagents
A3.1 Hydrochloric acid (pl.19 g/mL).
A3.2 Nitric acid (μl.42g/ml),
A3.3 Nitric acid (1-1).
A3.4 Nitric acid (2+3).
A3.5 Sulfuric acid (1+1).
A3.6 Hydrochloric acid-hydrobromic acid mixture: Mix equal volumes of hydrochloric acid (A3.1) and hydrobromic acid (p1.38g/mL) to prepare A3.7 Soil and water: Mix 3 volumes of hydrochloric acid (A3.1) and 1 volume of nitric acid (A3.2). A3.8 T water (1-1)
A3.9 Sodium chloride solution (100g/L).
A3.10 Bismuth standard stock solution: Pipette 0.5000g of metallic bismuth (≥99.99%) into a 250ml beaker, add 20ml of nitric acid (A3.3) and cover with a watch glass. Slightly heat until completely dissolved, wash the watch glass and the beaker wall with water, and cool. Pour into a 500ml volumetric flask, add 50ml of nitric acid (A3.2), dilute to the mark with water, and mix. This solution contains 1000ug bismuth in 1ml. A3.11 Bismuth standard solution: Pipette 25.00mL of bismuth standard stock solution into a 250ml volumetric flask containing 25ml of nitric acid (A3.2), dilute to the mark with water, and mix. This solution contains 100μg bismuth in 1mL. A4 Instrument
Atomic absorption spectrometer with bismuth hollow cathode lamp. Under the best working conditions of the instrument, any atomic absorption spectrometer that can achieve the following indicators can be used. Sensitivity: The characteristic concentration should not be greater than 0.16μg/ml. Precision: When measuring the absorbance 11 times with the highest concentration standard solution, the standard deviation should not exceed 1.50% of the average absorbance; when measuring the absorbance 11 times with the lowest concentration standard solution (not the "zero" standard solution), the standard deviation should not exceed 0.50% of the average absorbance of the highest concentration standard solution.
Linearity of working curve: 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.
For instrument working conditions, see Appendix B (Suggested Appendix). A5 Analysis steps
A5.1 Test material
GB/T 3260.3-2000
Weigh the sample according to Table A1, accurate to 0.0001g: Table A1
Bismuth content, %
0. 000 30 ~0. 005 0
≥0. 005 0~ 0. 02
Carry out 2 independent determinations and take the average value. A5.2 Blank test
Carry out a blank test with the test material.
A5.3 Determination
Test material·g
Test solution volume m
A5.3.1 Place the test material (A5.1) in a 250ml beaker, add 0.5ml sodium fluoride solution and 20ml aqua regia (A3.8). Cover with table blood. Decompose completely on a low-temperature electric furnace, remove the table glass, add 1.Cml sulfuric acid along the wall of the cup and mix well, heat and evaporate until white smoke appears, cool slightly, slide the wall of the cup and add 5mL hydrochloric acid-hydrobromic acid mixture, mix well, heat and evaporate until white smoke appears, cool slightly. Repeat adding hydrochloric acid and hydrobromic acid mixture 23 times, until all the tin is gone and all the white smoke appears, and cool.
A5.3.2 Add 1.0~2.5mL of positive water (A3.7) and rinse the cup wall with a small amount of water, heat slightly, cool to room temperature, and transfer to a 1025ml volumetric flask with water, which contains 10% (V/V) aqua regia, and dilute to the scale and mix. A5.3.3 Use air-acetylene flame, at the wavelength of 223.06nm of the atomic absorption spectrometer, and adjust to zero with water to measure the absorbance of bismuth in the test solution at the same time as the standard solution series. Subtract the absorbance of the blank test solution from the measured absorbance, and find the corresponding bismuth concentration from the working curve. A5.4 Drawing of working curve
Put 0, 1.00, 3.00, 5.00, 10.00, 15.00, 20.00 ml of bismuth standard solution into a 100 ml volumetric flask. Add 10 ml of aqua regia (A3.7) and 2.0 ml of sodium chloride solution to dilute to the mark with water and mix. Measure the absorbance of the standard solution under the conditions of the test sample. With bismuth concentration as the abscissa and absorbance (minus the absorbance of the "zero" concentration solution) as the ordinate, draw a working curve. A6 Expression of analysis results
Calculate the percentage of bismuth according to formula (A1):
Bi (%) = CV × 10* 6
Where: (—— Bismuth concentration μug/ml obtained from the working curve; V.—Total volume of the test solution, ml.
m—-The mass of the test material, g.
The result is expressed to three decimal places; if the bismuth content is less than 0.010%, it is expressed to four decimal places; if it is less than 0.0010%, it is expressed to five decimal places.
A7 Allowable difference
The difference between the analysis results of the laboratory should not be too large. The allowable difference listed in Table A2. Table A2
0. 000 30 -- 0. 001 0
≥ 0. 001 0~- 0. 005 0
≥0. 005 0~ 0. 010
20. 010~0. 920
Tolerance
.00020
GB/T 3260. 3---2000
Appendix BbZxz.net
(Suggestive Appendix)
Instrument Working Conditions
Use WFX-1D original absorption spectrometer to determine bismuth content. Working conditions are shown in Table B1Table B1
Lamp current, mA
Spectral passband, mm
Burner height, mm
Air flow, L/min
Fast flow, min2 Add 1.0~2.5mL. positive water (A3.7) and blow the cup wall with a small amount of water, heat slightly, cool to room temperature, and then transfer it into a 1025ml volumetric flask with water, which contains 10% (V/V) aqua regia, and dilute to the scale, and mix. A5.3.3 Use air-acetylene flame, at the wavelength of 223.06nm of the atomic absorption spectrometer, and adjust the absorbance of bismuth in the test solution with water at zero at the same time as the standard solution series. Subtract the absorbance of the blank test solution from the measured absorbance, and find the corresponding bismuth concentration from the working curve. A5.4 Drawing of the working curve
Put 0, 1.00, 3.00, 5.00, 10.00, 15.00, and 20.00ml. Bismuth standard solution into a 100ml volumetric flask. Add 10ml of aqua regia (A3.7) respectively, and add 2.0ml. Sodium chloride solution to dilute to the scale with water and mix. Under the same conditions as the sample, measure the absorbance of the standard solution. With bismuth concentration as the abscissa and absorbance (minus the absorbance of the "zero" concentration solution) as the ordinate, draw a working curve. A6 Expression of analysis results
Calculate the percentage of bismuth according to formula (A1):
Bi (%) = CV × 10* 6
Where: (—— Bismuth concentration μug/ml obtained from the working curve; V.—Total volume of the test solution, ml.
m—-The mass of the test material, g.
The result is expressed to three decimal places; if the bismuth content is less than 0.010%, it is expressed to four decimal places; if it is less than 0.0010%, it is expressed to five decimal places.
A7 Allowable difference
The difference between the analysis results of the laboratory should not be too large. The allowable difference listed in Table A2. Table A2
0. 000 30 -- 0. 001 0
≥ 0. 001 0~- 0. 005 0
≥0. 005 0~ 0. 010
20. 010~0. 920
Tolerance
.00020
GB/T 3260. 3---2000
Appendix B
(Suggestive Appendix)
Instrument Working Conditions
Use WFX-1D original absorption spectrometer to determine bismuth content. Working conditions are shown in Table B1Table B1
Lamp current, mA
Spectral passband, mm
Burner height, mm
Air flow, L/min
Fast flow, min2 Add 1.0~2.5mL. positive water (A3.7) and blow the cup wall with a small amount of water, heat slightly, cool to room temperature, and then transfer it into a 1025ml volumetric flask with water, which contains 10% (V/V) aqua regia, and dilute to the scale, and mix. A5.3.3 Use air-acetylene flame, at the wavelength of 223.06nm of the atomic absorption spectrometer, and adjust the absorbance of bismuth in the test solution with water at zero at the same time as the standard solution series. Subtract the absorbance of the blank test solution from the measured absorbance, and find the corresponding bismuth concentration from the working curve. A5.4 Drawing of the working curve
Put 0, 1.00, 3.00, 5.00, 10.00, 15.00, and 20.00ml. Bismuth standard solution into a 100ml volumetric flask. Add 10ml of aqua regia (A3.7) respectively, and add 2.0ml. Sodium chloride solution to dilute to the scale with water and mix. Under the same conditions as the sample, measure the absorbance of the standard solution. With bismuth concentration as the abscissa and absorbance (minus the absorbance of the "zero" concentration solution) as the ordinate, draw a working curve. A6 Expression of analysis results
Calculate the percentage of bismuth according to formula (A1):
Bi (%) = CV × 10* 6
Where: (—— Bismuth concentration μug/ml obtained from the working curve; V.—Total volume of the test solution, ml.
m—-The mass of the test material, g.
The result is expressed to three decimal places; if the bismuth content is less than 0.010%, it is expressed to four decimal places; if it is less than 0.0010%, it is expressed to five decimal places.
A7 Allowable difference
The difference between the analysis results of the laboratory should not be too large. The allowable difference listed in Table A2. Table A2
0. 000 30 -- 0. 001 0
≥ 0. 001 0~- 0. 005 0
≥0. 005 0~ 0. 010
20. 010~0. 920
Tolerance
.00020
GB/T 3260. 3---2000
Appendix B
(Suggestive Appendix)
Instrument Working Conditions
Use WFX-1D original absorption spectrometer to determine bismuth content. Working conditions are shown in Table B1Table B1
Lamp current, mA
Spectral passband, mm
Burner height, mm
Air flow, L/min
Fast flow, min
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