This standard specifies the method for determining the content of antimony trioxide in antimony trioxide. This standard is applicable to the determination of the content of antimony trioxide in antimony trioxide. Determination range: 98.000% to 99.95%. GB/T 3254.1-1998 Chemical analysis method for antimony trioxide Determination of antimony trioxide content GB/T3254.1-1998 Standard download decompression password: www.bzxz.net

GB/T 3254.1~3254.6—1998
This standard is a revision of GB3254.1~-3254.4-82. The original standard includes three determination items and one analysis method, among which the determination of the main component antimony trioxide has two analysis methods, which is only applicable to products produced with metallic antimony as raw material; this standard includes 6 determination items and 7 analysis methods, which is applicable to the analysis of various antimony trioxide products produced. The new standard not only fully meets the requirements of production and users, but also meets the international standards, and simplifies the analysis procedures and saves analysis costs.
This standard is applicable to the determination of the chemical composition content of various grades of antimony dioxide products in GB/T4062-1998, among which the determination methods of antimony monoxide and arsenic content and the method of Appendix A (determination of lead content by disulfide spectrophotometry) of GB/T3254.3 are revised. The determination methods of lead, copper, iron and selenium content are newly formulated methods. There are two methods for the determination of lead content in this standard, among which "atomic absorption spectrometry" is the preferred method in arbitration analysis. Appendix A (determination of lead content by dithiol spectrophotometry) is based on the fact that most production units currently lack atomic absorption spectrometers, and these units have been using them for a long time, have skilled operating techniques, and have obtained accurate results after revision and improvement. The two methods are included in the standard.
From the date of entry into force, this standard will replace Appendix A of GB3254.13254.4--82GB/T3254.31998 as the standard appendix, and Appendix B as the reminder appendix. This standard was proposed by China Nonferrous Metals Industry Corporation and is under the jurisdiction of the Standard Metrology Institute of China Nonferrous Metals Industry Corporation. This standard was drafted by Xikuangshan Mining Bureau. The main drafting unit of this standard: Xikuangshan Mining Bureau. The main drafters of this standard: Zeng Fusheng, Cai Xu, Peng Yongquan, Wu Donghua, Fang Hanchen, Li Wenmei. 27www.bzxz.net
National Standard of the People's Republic of China
Chemical analysis method of antimony trioxide
Determination of antimony trioxide content
Antimony trioxide-Determination of antimony trioxide content1 Scope
This standard specifies the method for determining the content of antimony trioxide in antimony trioxide. GB/T3254.. 1998
Replaces GB3251.13254.282
This standard is applicable to the determination of antimony trioxide content in antimony trioxide. Determination range: 98.00%～99.95%. 2 Referenced standards
The provisions included in the following standards constitute the provisions of this standard through their use in this standard. When this standard is published, the versions shown are valid. All standards are subject to revision, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB1.4-88 Guidelines for Standardization Work Provisions for the Preparation of Chemical Analysis Methods GB1467-78 General Principles and General Provisions for Chemical Analysis Methods for Metallurgical Products 3 Method Summary
The sample is dissolved in tartaric acid, and in a sodium bicarbonate buffer solution, starch is used as an indicator, and the iodine standard solution is dripped until the purple-blue color is the end point. The percentage of antimony trioxide is calculated by accurately weighing the mass of the consumed iodine standard solution. Arsenic dioxide quantitatively interferes with the determination, and the results should be corrected after independent determination. 4 Reagents
4.1 Sodium bicarbonate.
4.2 Tartaric acid solution (200g/L).
4.3 Sodium hydroxide solution (230g/L).
4.4 Iodine standard titration solution
4.4.1 Preparation
Weigh 10.45g iodine and place it in a 1000mL beaker, add 100g potassium iodide. Dissolve it in 200ml water, transfer it into a 1000ml brown volumetric flask, dilute it to the mark with water, and mix it well. 4.4.2 Calibration
Carry out a blank test along with the calibration.
Weigh 0.40000g antimony trioxide (99.99% or more) according to 7.1, place it in a 500mL conical flask, moisten it with a small amount of water, add 50ml tartaric acid solution (4.2), and proceed as per 7.3.2. Calculate the actual concentration of the iodine standard solution according to formula (1): r
0. 072 88 x (ml -
ma -- m)
Where: the actual concentration of the iodine standard titration solution. mol/kgm·mass of trioxide-_·g;
Approved by the State Administration of Quality and Technical Supervision on July 15, 199828
Implementation on February 1, 1999
GB/T3254.1--1998
-The mass of the weighing titration bottle containing the iodine standard titration solution before calibration, &: m2—-The mass of the weighing titration bottle containing the remaining iodine standard titration solution after calibration, g: m
0.072 88-
-The mass of iodine standard solution consumed by the blank test solution calibrated at random; - The mass of antimony trioxide equivalent to 1.0000g of iodine standard titration solution [c (12/2) = 1.0000mo1/kg], kg/mol.
Three parallel calibrations, the extreme value of the mass of iodine standard titration solution consumed does not exceed 0.0200g. Take the average value. Otherwise, recalibrate.
4.5 Starch indicator (10g/1.): Weigh 1g of soluble starch, put it in a 250mL beaker, add a small amount of water to make a paste, add 100ml of boiling water under constant stirring, let it stand, and cool. Use clear solution. 5 Instruments
5.1 Weighing titration bottle (about 100mL), see Figure 1. $12.5×32
Figure! Weighing titration bottle
5.2 Analytical balance, sensitivity 100,000ths-
5.3 Electromagnetic stirrer.
6 Sample
No. 2 siphon 4.5×23
Hole 40. 6 ~ 0. 75
The sample should be dried at 100C～105 (after 1h, placed in a dryer and cooled to room temperature. 7 Analysis steps
7.1 Sample
Weigh 0.40000g of sample, accurate to 0.00001g. When weighing the sample, use a heat-resistant plastic of about 2mm thick to make a small blood with a groove in the middle with a size of α×b.cm:2×4, and the sample is added to the small blood for weighing. Perform two independent measurements and take the average value. 7.2 Blank test 7.3 Determination 7.3.1 Transfer the sample and the small bottle into a 500ml conical flask and moisten it with a small amount of water. While analyzing the sample, titrate the 29 solution with standard iodine. GB/T3254.1-1998 7.3.2 Add 50ml tartaric acid solution, shake the sample, cover the surface III, heat, and keep the solution slightly boiling. Dissolve for 0.5h in a state. Shake the conical flask 2-3 times during the dissolution process, remove it, and cool it to room temperature. 7.3.3 Add 20mL of sodium hydroxide solution to neutralize most of the tartaric acid, then add sodium bicarbonate to neutralize the remaining tartaric acid until no obvious gas is generated, and add about 4g of excess. Add 40ml of water and keep the solution temperature between 15C and 40C. Add 2mL of starch indicator. 7.3.4 Weigh the mass of the weighing titration bottle containing the iodine standard titration solution, and fill it with Titrate the sample solution with iodine standard titration solution at the mouth of the conical bottle under constant stirring until the solution turns a stable purple-blue color. This is the end point. Then weigh the mass of the weighing titration bottle containing the remaining iodine standard titration solution. The difference between the two weighing results is the consumption of iodine standard titration solution. 7.3.5 Determine the arsenic content and calibrate the results in accordance with GB/T3254.2. 8 Expression of analysis results
Calculate the percentage of antimony monoxide according to formula (2): Sb:0(%) :(mm=m)X.0.072 88 × 100 - As% × 1. 945 m.
Wherein: - the actual concentration of the iodine standard titration solution.mol/kg; the mass of the weighing titration bottle containing the iodine standard titration solution before the measurement; m.
the mass of the weighing titration bottle containing the remaining iodine standard titration solution after the measurement·g; machine. --During the measurement. The mass of the iodine standard titration solution consumed by titrating the blank test solution accompanying the sample, gm
0. 072 88 -- --
Mass of the sample, nominal;
equivalent to 1.0000g of iodine standard titration solution [c (1/2) 1.0000mol/kg = mass of iodine. kg/mol;
1.945% converted to the coefficient of iodine disulfide
The result is expressed to two decimal places.
Allowable difference
The difference between the analysis results of laboratories should not be less than 0.12%. 30
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