This standard specifies the determination method of tellurium content in lead and lead alloys. This standard is applicable to the determination of tellurium content in lead and lead alloys. Determination range: 0.0050% to 1.00%. GB/T 4103.8-2000 Chemical analysis method for lead and lead alloys Determination of tellurium content GB/T4103.8-2000 Standard download decompression password: www.bzxz.net

3-2000
GB/T 4103. 8
This standard is a revision of the method part of GB3/T4103.10:-1983 "Chemical analysis methods for lead-based alloys - Oscillographic polarographic determination of selenium and tellurium in tellurium salts".
This standard complies with:
GB/T 1. 1-- 1993
GB/T 1. 4---1988
Guidelines for standardization work
Unit 1: Rules for the initiation and expression of standards Part 1: Basic provisions for the preparation of standards
Rules for the preparation of chemical analysis methods standards
Guidelines for standardization work
GB/T1467·1978 General principles and general provisions for chemical analysis methods of metallurgical products Basic terminology for chemical analysis of metallurgical products
GB/T 17433—1998
This standard will partially replace GB/T4103.101983 from the date of entry into force
This standard was proposed by the National 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 Xifu Smelter
The main drafters of this standard are Liu Haiyan and Zhang Quan.
1 Scope
National Standard of the People's Republic of China
Chemical Analysis Method of Lead and Lead Alloys
Determination of Tellurium Content
Methods for chemical analysis of lead and lead alloys--Determination of telluriumn content This standard specifies the method for determination of tellurium content in lead and lead alloys. GB/T 4103.82000
Partially replaces GB/T4103.101983
This standard is applicable to the determination of tellurium content in lead and lead alloys. The determination range is 0.0050% to 1.00%. 2 Method Summary
The sample is decomposed with nitric acid and tartaric acid. In the hydrochloric acid medium, formaldehyde is used to remove nitric acid. Arsenic is added as a carrier. Sodium hypophosphite is used to reduce tellurium and stele into monomers. The mixture is filtered and dissolved with nitric acid and perchloric acid. The perchloric acid is used to bubble. In an alkaline electrolyte supported by ammonium sulfate, gum arabic is used to suppress the maximum (wave height). Na.Fr)TA complexes trace impurity elements. Hydrogen (or nitrogen) is passed to remove oxygen. The second-order derivative wave height is determined at a potential of -0.3 to -0.80 V.
3 Reagents
3.1 Sodium hypophosphite.
3.2 Tartaric acid,
3.3 Formaldehyde.
3.4 ​​Nitric acid (ol.42 g/ml).
3.5 Hydrochloric acid (pl.19 g/mL).
3.6 Perchloric acid (ol.67 g/ml).
3.7 Ammonium hydroxide (1+5).
3.8 Washing solution: Dissolve 1g of sodium hypophosphite in 100ml of hydrochloric acid (5+95) and mix well. 3.9 Silver nitrate solution (10g/L).
3.10 Arsenic solution: Weigh 1.3000g of arsenic trioxide in a 100mL beaker, add 15ml of sodium oxychloride solution (100/ml) and dissolve it with slight heat. Transfer it to a 500mL volumetric flask, dilute it to 200mL with water, add 1 drop of phenol ethanol solution (2g/L), neutralize it with hydrochloric acid (111) until the red color disappears, and dilute it to the mark with water. This solution contains 2mg of arsenic in 1ml. 3.11 Ammonium sulfate solution (33g/L).
3.12 Gum arabic solution (1.4g/1). 3.13 Disodium ethylenediaminetetraacetic acid (Naz2EDTA) solution (50g/L). 3.14 Phenol red solution (1g/L): Weigh 0.1g phenol red, dissolve in 20ml ethanol, dilute to 100ml with water, mix. 3.15 Tellurium standard stock solution: Weigh 0.1000g tellurium (99.95%) in 200ml beaker, add 20ml acid (1+1), heat to dissolve, transfer to 1000mL volumetric flask, dilute to scale with water and mix. This solution contains 100ug tellurium in 1ml. 3.16 Tellurium standard solution: Transfer 25.00mL tellurium standard stock solution (3.15) to 500ml volumetric flask, dilute to scale with water, mix. This solution contains 5μg tellurium in 1ml.
4 Instrument
Oscillographic polarograph,
5 Analysis steps
5.1 Test sample
Weigh the sample according to Table 1, accurate to 0.0001g. Tellurium content%
0. 005 0 ~~ 0. 050
0.050~0. 10
≥0.10~0.50
0. 50~1.00
Test sample amount g
Carry out 2 independent determinations and take the average value5.2 Blank testbZxz.net
Carry out a blank test together with the test sample.
GB/T4103.8--2000
Total volume of test solution, ml
Volume of fraction, mL
2. 00~5. 00
2.00~5.00
Measurement volume. ml,
5.3.1 Place the sample (5.1) in a 200mL beaker, add 1g tartaric acid, 10ml water, 4mL nitric acid, cover with table IIIl, and heat until completely dissolved.
5.3.2 Remove, add 50ml hydrochloric acid, and let stand until the solution turns reddish brown, add 1~~2mL formaldehyde each time, shake from time to time until the reddish brown disappears, add 40ml water, then add 2.5mL arsenic solution and 4g sodium hypophosphite in turn, and stir to dissolve. Place on a low-excitation electric hot plate. Heat and slightly boil for 10 minutes, and keep warm in a water bath at 80-~90℃ for 60~120 minutes. 5.3.3 Filter with absorbent cotton while hot, and transfer all the precipitates into the funnel. Wash the tableware and cup with detergent 3 times, precipitate 5 times, and then wash the precipitate with water until the filtrate is checked with silver nitrate solution and no silver chloride white precipitate is generated. Discard the filtrate and washing liquid, transfer the absorbent cotton to the original beaker, rinse the funnel in the original beaker with 10~15mL nitric acid and 4mL perfluoric acid, digest the absorbent cotton on a low-temperature electric hot plate, and dissolve arsenic and tellurium. After dissolution, remove it and transfer it to a volumetric flask according to Table 1. 5.3.4 Take a certain amount of test solution according to Table 1 in a 50mL beaker, add 1mL nitric acid and 0.5ml perfluoric acid, mix the spoon, and place it on a low-temperature electric hot plate to steam until white smoke appears (during the evaporation process, shake the beaker from time to time, and white smoke will appear for about 1 minute). Remove and cool, rinse the table III and the cup wall with a little water, evaporate until white smoke just comes out, remove and cool. 5.3.5 Use a small amount of water to blow the table III and the cup wall, add 1.0mL NazEDTA solution, 3.0mL ammonium sulfate solution, 3.0mL gum arabic solution, add 2 drops of phenol red solution, and adjust with ammonium hydroxide until the solution just turns purple-red, and add 1 drop in excess. Transfer the solution into a 25mL volumetric flask, dilute to the mark with water, and mix.
5.3.6 Take part of the solution (5.3.5) and place it in an electrolytic cell. Pass hydrogen (or nitrogen) for 5 minutes to remove dissolved oxygen. On the oscillographic polarograph, measure the first-order derivative wave height of tellurium at a potential of F(.30~0.80V. And deduct the blank value accompanying the sample. 5.4 Standard reference solution used in direct comparison method Take 3 portions of tellurium standard solution with the same tellurium content as the test sample and place them in 3 50ml beakers. Add 1ml nitric acid to each beaker. Proceed as in 5.3.4~5.3.6. Take the average value and calculate the result by direct comparison method. 6 Expression of analytical results
Calculate the exact percentage content according to formula (1):
GB/T 4103.8- 2000
cV-H, X 10-6
Te(%) =
Wherein: c-concentration of tellurium standard solution, g/mL: V—-volume of tellurium standard solution taken during determination, mL; H,----wave height of test solution, mm
.:wave height of standard solution, mm;
mass of test sample, g.
The result is expressed to one decimal place. If the tellurium content is less than 0.10%, it is expressed to two decimal places: if it is less than 0.010%, it is expressed to four decimal places.
Allowable error
The difference between the analysis results of the experimental cases should not be greater than the allowable error listed in Table 2. Table 2
Tellurium content
0. 005 0~~0. 010
>0. 010~0. 050
>0.050~0.10
≥0. 10~-0.50
>0.50~1.00
Allowable difference
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