This standard specifies the determination method of bismuth content in lead and lead alloys. This standard is applicable to the determination of bismuth content in lead and lead alloys. Determination range: 0.0020% to 0.10%. GB/T 4103.5-2000 Chemical analysis method for lead and lead alloys Determination of bismuth content GB/T4103.5-2000 Standard download decompression password: www.bzxz.net

GB/T4103.5--2000
This standard is a revision of GB/T4103.71983 "Chemical analysis method for lead-based alloys - Determination of bismuth content by potassium iodide photometric method" GB/T4103.8--1983 "Chemical analysis method for lead-based alloys - Determination of bismuth content by sulfide dolphine photometric method" and GB/T472.3 [1984 Chemical analysis method for lead - Determination of bismuth content by potassium iodide-strychnine spectrophotometric method". This standard complies with:
Guidelines for standardization work Unit 1: Rules for drafting and expressing standards Part 1: GB/T 1.1-: 1993
Basic provisions
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/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 replaces GB/T4103.7-1983. GB/T4103.8-1983 and GB/T472.3-1984 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 Refinery and Northwest Copper Processing Plant of Baiyin Nonferrous Metals Company. This standard was drafted by Northwest Steel Processing Plant of Ziyin Nonferrous Metals Company. The main drafter of this standard: Ji Chunfang
1 Scope
National Standard of the People's Republic of ChinawwW.bzxz.Net
Chemical analysis method of lead and lead alloys
Determination of bismuth content
Methods for chemical analysis of lead and lead alloys---Determination of bismuth content This standard stipulates "Determination of bismuth content in lead and lead alloys GB/T4103.5 2000" replaces GB/T 4103.7 1983
G3/T A103.8 1983
GB/T 472.31G84
This standard is applicable to the determination of bismuth content in lead and lead alloy. Determination range: 0.0020%~0.10%. 2 Method Summary
The sample is dissolved in nitric acid or nitric acid-tartaric acid. According to the bismuth content, manganese dioxide is used for co-precipitation to enrich bismuth and separate lead, or hydrochloric acid is added after the sample is dissolved to make the lead form lead chloride precipitate and remove most of the lead. Selenium and tellurium interfere with the determination. They are reduced to monomers in a hydrochloric acid medium with stannous chloride and filtered out. Sodium hexametaphosphate, thiourea and potassium fluoride are used to mask the residual lead, copper and silver, as well as tin and antimony, respectively. In a hydrochloric acid medium, potassium iodide is used as a color developer and its absorbance is measured at a wavelength of 450nm on a spectrophotometer. 3 Reagents
3.1 Tartaric acid
3.2 Hydrogen peroxide (μl.10 g/mL). 3.3 Hydrochloric acid (pl.19g/ml).
3.4 ​​Hydrochloric acid (1+1).
3.5 Hydrochloric acid (1+5).
3.6 Hydrochloric acid (1+9).
3.7 Nitric acid (1+4).
3.8 Manganese nitrate solution: Mix 1 volume of manganese nitrate solution (500g/L) with 4 volumes of water. 3.9 Potassium permanganate solution (10g/1.).
3.10 Stannous chloride solution (100g/L): Weigh 10.0g of stannous chloride (SnCl2·20). Dissolve it with 50mL of hydrochloric acid (3.4) with slight heat. Cool. Dilute to 100mL with hydrochloric acid (3.4). Prepare it before use. 3.11 Sodium hexametaphosphate solution (20 0g/1). 3.12 Potassium iodide solution (250g/1).
3.13 Thiourea solution (100g/L).
3.14 Fluorothiocyanate (KF·2H.0) solution (200g/1). 3.15 Nitrate solution (5mg/mL): Weigh 0.500g of pure nitric acid, place in a 200ml beaker, add 20ml of nitric acid (1+1), heat to dissolve, boil to remove nitrogen oxides, and cool. Transfer to a 100ml volumetric flask, dilute to scale with water, mix well, 3.16 Bismuth standard stock solution: Weigh 0.1000g of pure bismuth, place in a 200ml beaker, add 20ml of nitric acid (1+1). Cover 1 meter, heat to dissolve, boil to remove nitrogen oxides, and cool. Transfer to a 1000mL salt bottle, add 90ml of nitric acidFor a test solution containing 0.010% to 0.030%, add 7 mL of hydrochloric acid (3.3) to the volumetric flask, dilute to the mark with water and mix. Transfer 15.00 mL to another 50 mL volumetric flask. Continue with 5.3.2. 5.3.1.2 Test sample containing bismuth > 0.030% to 0.10% 5.3.1.2.1 Place the test sample (5.1) in a 250 mL beaker, add 9 g of tartaric acid and 30 mL of nitric acid, cover with a beaker, heat at low temperature to dissolve, boil to remove nitrogen oxides, and cool. 5.3.1.2.2 Transfer the solution to a 100 mL volumetric flask, add 15 mL of hydrochloric acid (3.3), cool with running water for 5 min. Dilute to the mark with water, mix well, and let stand for 2 min. Filter with medium-speed filter paper and discard the initial filtrate. 5.3.1.2.3 According to the sample composition, perform the following operations: Samples without selenium and tellurium: Pipette 10.00mL of filtrate into a 50mL volumetric flask, add 10ml of hydrochloric acid (3.5). The following is directly carried out according to 5.3.2
Selenium and tellurium samples: Pipette 50.00ml of filtrate into a 250ml beaker. If the sample only contains selenium, add 2.0ml of tellurium solution, add 123
GB/T4103.5—2000
Evaporate to a volume of about 2mL, add 5ml of hydrochloric acid (3.3), evaporate to a volume of about 2ml, and repeat this operation 2~3 times (1~5 times in total). Add 20mL hydrochloric acid (3.4), boil, add 5mL stannous chloride solution, continue to boil until the precipitate condenses, cool, filter with medium-speed filter paper, wash the precipitate and beaker with hydrochloric acid (3.6) 4-5 times, and discard the precipitate. Collect the filtrate and washing liquid in a 50mL volumetric flask, dilute to scale with salt (3.6), and mix well. Transfer 10.00mL solution to a 50mL volumetric flask. Continue with 5.3.2. 5.3.2 Color development
Add 10mL sodium hexametaphosphate solution, 5mL potassium iodide solution, 2.5mL sulfur solution, and 2.5mL potassium fluoride solution to a 50mL volumetric flask, and mix after each reagent is added. Dilute to scale with water, mix. Let stand for 3min. 5.3.3
Place part of the solution into a 5cm absorption dish, and measure its absorbance at a wavelength of 450nm on a spectrophotometer with the blank solution accompanying the sample as a reference. Find the corresponding bismuth amount from working curve 1. 5.4 Drawing of working curve
5.4.1 Take 0.1.00, 2.00, 3.00, 4.00.5.00ml of bismuth standard solution and place it in a set of 50mL volumetric flasks, add 3mL of hydrochloric acid (3.3) and 10ml of water, mix, and proceed as in 5.3.2. 5.4.2 Place part of the solution into a 5cm absorption dish, and measure its absorbance at a wavelength of 450nm on a spectrophotometer with the blank solution as a reference. Draw a working curve with the bismuth amount as the horizontal axis and the absorbance as the vertical axis. 6 Expression of analysis results
Calculate the percentage of bismuth according to formula (1):
Bi(%) = mI:V.=V, X 10-6
Formula; m----the amount of bismuth found from the working curve, g; V.--the volume of the first dilution solution, mL, V2----the volume of the second dilution solution, mL; V--the volume of the first aliquot solution, mL; V--the volume of the second aliquot solution, mL
m. The mass of the sample, g.
(1)
The result is expressed to two decimal places. If the bismuth 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 1. Table 1
Bismuth content
0. 002 0~ 0. 004 0
0. 004 0 ~ 0. 008 0
0. 008 0~ 0. 015
0. 015~0. 050
0.050~0.10
allowable difference
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