GB/T 15080.1-1994 Chemical analysis methods for antimony concentrates - Determination of antimony content

This standard specifies the determination method of antimony content in antimony concentrate. This standard is applicable to the determination of antimony content in antimony concentrate. Determination range: 5% to 65%. GB/T 15080.1-1994 Chemical analysis method for antimony concentrate Determination of antimony content GB/T15080.1-1994 Standard download decompression password: www.bzxz.net

UDC669.754：543.06
National Standard of the People's Republic of China
GB/T 15080. 1~15080. 9--94
Methods for chemical analysis of antimony concentrates
Issued on May 11, 1994
State Bureau of Technical Supervision
Implementation on December 1, 1994
National Standard of the People's Republic of China
Methods for chemical analysis of antimony concentrates
Determination of antimony content
Antimony concentrates--Determination of antimnony content
1 Subject content and scope of application
This standard specifies the method for determination of antimony content in antimony concentrate: This standard is applicable to the determination of antimony content in antimony concentrate. Determination range: 5% to 65%. 2 Reference standards
GB1.4 Standardization work guidelines Chemical analysis method standard preparation regulations GB1467 General principles and general provisions for chemical analysis methods for metallurgical products 3 Method summary
GB/T 15080.1-94
The sample is decomposed with sulfuric acid-potassium sulfate, with carbon as a reducing agent and auxiliary solvent, in a hydrochloric acid medium, phosphoric acid is added to mask the high-valent iron ions, methyl orange is used as an indicator, and titrated with cerium sulfate standard titration solution at 80 to 90°C until the red color of the solution disappears as the end point. 4 ReagentsWww.bzxZ.net
4.1 Potassium sulfate.
4.2 Sulfuric acid (o1.84 g/mL).
4.3 Phosphoric acid (pl.70 g/mL).
4.4 Hydrochloric acid (1+1).
4.5 Cerium sulfate standard titration solution.
4.5.1 Preparation: Weigh 40.50g sulfuric acid (CCe (S0,) 4H,0), place in a 1000mL beaker, add 30mL sulfuric acid (4.2), stir evenly, gradually heat on an electric stove until it becomes a paste, and white sulfuric acid smoke will be emitted for about 20 minutes, remove and cool slightly, add 140mL sulfuric acid (4.4), then slowly add 400mL water, stir and dissolve until clear, cool, transfer to a 1000mL volumetric flask, dilute to the scale with water, and mix evenly.
4.5.2 Calibration: Weigh three portions of 0.2500g metal antimony (99.99%), place them in 300mL conical flasks respectively, moisten with a small amount of water, add 12mL sulfuric acid (4.2), heat and dissolve until clear, remove and cool. The following operations are carried out according to 6.3.2 and 6.3.3. Perform a blank test along with the calibration.
Calculate the actual concentration of the standard sulfuric acid titration solution (4.5) according to formula (1): m
c = (V, = V.) × 0. 060 88
The actual concentration of the standard sulfuric acid titration solution (4.5), mol/L; Wherein: c—
The mass of metallic antimony, g;
Vl——The volume of the standard cerium sulfate titration solution (4.5) consumed in titrating antimony, mL; Approved by the State Administration of Technical Supervision on May 11, 1994 (1)
Implementation on December 1, 1994
GB/T 15080.1—94
V. -The volume of the standard cerium sulfate solution (4.5) consumed by the blank solution in the calibration, mL; -The mass of 0.060 88-
of antimony in grams equivalent to 1.00 mL of the standard cerium sulfate solution [c(Ce（S0,),)=1.000 mol/L.
The average of the three calibration results is the actual concentration of the standard cerium sulfate solution (4.5). The range of the volume of the standard cerium sulfate solution (4.5) consumed by the parallel calibration should not exceed 0.10 mL. 4.6 Methyl orange indicator (1 g/L).
5 Sample
5.1 The particle size of the sample should be less than 0.100 mm.
5.2 The sample should be dried at 100-105°C for 1 hour and placed in a desiccator to cool to room temperature. 6 Analysis steps
6.1 Test material
Weigh the sample according to Table 1, accurate to 0.0001g. Table 1
Antimony content, %
Carry out two independent determinations and take the average value. 6.2 Blank test
Make a blank test along with the test material.
6.3 Determination
Test material, g
6.3.1 Place the test material (6.1) in a 300mL conical flask, add 2g potassium sulfate (4.1), moisten with a small amount of water, add 15mL sulfuric acid (4.2), place on a hot plate and heat, after most of the sulfur is driven off, cover with surface III, and dissolve for 60min at a temperature that keeps the solution slightly boiling. Remove and cool slightly, add about 3cm2 of qualitative filter paper, continue heating until the filter paper is carbonized and the dark color of the solution disappears, remove and cool. 6.3.2 Add 40 mL of water and 30 mL of hydrochloric acid (4.4), mix, add 10 mL of phosphoric acid (4.3), mix well, and boil. 6.3.3 Add 2 drops of methyl orange indicator (4.6), and titrate with standard titration solution of sodium sulfate (4.5) while keeping the solution at 80-90°C until the red color of the solution disappears, which is the end point. 7 Expression of analysis results
Calculate the percentage of antimony according to formula (2):
Sb(%) × (Vz -V)) × 0. 060 88 mo
Wherein: c--actual concentration of sulfuric acid standard titration solution (4.5), mol/L; V2--volume of cerium sulfate standard titration solution (4.5) consumed by the titration test solution, ml.X 100
V;--volume of cerium sulfate standard titration solution (4.5) consumed by the blank solution in the determination, mL; mo--mass of the sample, g;
0.06088--mass of antimony in grams equivalent to 1.00mL sulfuric acid standard titration solution Cc (Ce (SO.),) = 1.000mol/LJ.
The result should be expressed to two decimal places.
8 Allowable Difference
GB/T 15080.1--94
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 2. Table 2
Antimony content
5.00~~12.00
>12. 00~22, 00
>22.00~～32.00
>32. 00~~42. 00
Additional Notes:
This standard is proposed by China Nonferrous Metals Industry Corporation. This standard is technically managed by Beijing Research Institute of Mining and Metallurgy. This standard is drafted by Xikuangshan Mining Bureau and Hunan Nonferrous Metals Research Institute. This standard is drafted by Xikuangshan Mining Bureau.
The main drafters of this standard are Xie Benchang and Zeng Fusheng. Allowable Difference
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