This standard specifies the determination method of mercury in bismuth. This standard is applicable to the determination of mercury in bismuth. Determination range: 0.00003%~0.00006%. GB/T 8220.11-1998 Chemical analysis method for bismuth Determination of mercury content by cold vapor atomic absorption spectrometry GB/T8220.11-1998 Standard download decompression password: www.bzxz.net

GB/T8220.11--1998
This standard is a revision of Appendix J of GB/T915-1995 "Bismuth". This standard complies with:
Guidelines for Standardization Work - Provisions for the Preparation of Chemical Analysis Methods GB/T 1.4-1988
GB/T 1467-1978
, General Principles and General Provisions for Chemical Analysis Methods for Metallurgical Products GB/T7729-1987 General Rules for Spectrophotometric Methods for Chemical Analysis of Metallurgical Products This standard is a supporting standard of GB/T915-1995 "Bismuth" Unit 1: Rules for Drafting and Presentation of Standards The preparation method of this standard complies with the provisions of GB/T1.1-1993 "Guidelines for Standardization Work - Part 1: Basic Provisions for the Preparation of Standards". From the date of implementation, this standard will also replace Appendix J of GB/T915--1995 "Bismuth". This standard was proposed by China Nonferrous Metals Industry Corporation. This standard is under the jurisdiction of the Standardization and Metrology Research Institute of China Nonferrous Metals Industry Corporation. This standard was drafted by Zhuzhou Smelter. The main drafters of this standard are Yang Mingchen and Yan Jiliang. 353
1 Scope
: National Standard of the People's Republic of China
Chemical analysis method of bismuth
Determination of mercury content by cold vapor atomic absorption spectrometric methodMeihods for chemical analysis of hismuth--Determination af mercury contentCold vapour atomic absorplion spectrometric methodThis standard specifies the method for the determination of mercury content in bismuth. This standard is applicable to the determination of mercury content in bismuth. Determination range: 0.00003% to 0.00006%. 2 Summary of the method
GB/T 8220.117998
The sample is dissolved in nitric acid. In nitric acid solution, use stannous chloride as reducing agent and nitrogen (or dry air) as carrier gas, and introduce the generated atomic vapor into the vapor measuring instrument for measurement. When the amount is less than 14 times the amount, it will not interfere with the measurement. 3 Reagents
3.1 Nitric acid (ol.42g/ml), high-grade pure. 3.2 Nitric acid (1+1). High-grade pure.
3.3 Stannous chloride solution (100g/L): weigh 10g stannous chloride (SnCl2H2O). Dissolve in 10)mL hydrochloric acid (1-11): prepare it when used,
3.4 ​​Palladium dichromate solution (50g/1.). bZxz.net
3.5 Standard stock solution: Weigh 0.1354 g of mercury chloride solution that has been dried for 24 hours with phosphorus pentoxide. Add 50 mL of nitric acid (3.1) and 10 mL of potassium dichromate solution (3.4), transfer to a 1000 mL volumetric flask, dilute to scale with water, and mix. 1 mL of this solution contains 0.1 ng mercury.
3.6 Standard solution: Transfer 10.00 mL of mercury standard stock solution (4.5) to a 100 mL volumetric flask, add 1 mL of nitric acid (3.1) and 1 mL of potassium dichromate solution (3.4), dilute to scale with water, and mix. 1 mL of this solution contains 101 g mercury. 3.7 Standard solution: Transfer 1.00 mL of mercury standard solution (3.6) to a 100 mL volumetric flask, add 5 mL of nitric acid (3.1) and 1 mL of potassium dichromate solution (3.4), dilute to scale with water, and mix. This solution contains 0.1μg of mercury in 1ml. 4 Apparatus
Crystal absorption mercury meter.
5 Analysis steps
5.7 Sample
Weigh 2.000g of sample.
5.2 Room white test
Approved by the State Administration of Quality and Technical Supervision on August 19, 1998 356
19990301 implementation
Carry out a blank test with the sample.
5.3 Determination
GB/T 8220.11-1998
5.3.1 Place the sample (5.1) in a 150ml beaker, add 30ml nitric acid (3.1), cover Table III. until the sample is completely dissolved, add 50mL water, heat and boil on a hot plate to drive off nitrogen oxides. When the test solution becomes clear and there is no brown gas in the beaker, add 1ml potassium chromate solution (3.4), continue to boil. If the solution fades, add potassium dichromate dropwise until the color does not fade. Remove, cool, transfer to a 100)ml volumetric flask, dilute to the scale with water, and mix well. 5.3.2 Stabilize the instrument in advance, adjust the zero point, and adjust the carrier gas flow rate to 1.31./min. 5.3.3 Take 5.00ml of the test solution (5.3.1) in a 10mL colorimetric tube, dilute it to the scale with water, and mix it. 5.3.4 Transfer the test solution (5.3.3) into the reactor, quickly add 1.5mL of tin chloride solution (3.3), cover the reactor tightly, pass nitrogen (or dry air), and record the maximum reading displayed on the instrument. 5.4 Drawing of the working curve
5.4.1 Stabilize the instrument in advance, adjust the zero point, and adjust the gas flow rate to 1.3L/min. 5.4.2 Take 0, 0.20, 0.40, 0.60, 0.80, 1.00mL of mercury standard solution (3.7) and place them in a set of 10mL colorimetric tubes respectively, add 2mL of nitric acid (3.2) and 1 drop of potassium dichromate solution (3.4), dilute with water to the scale and mix well. The following is carried out according to 5.3.4. With the amount to be measured as the abscissa and the reading value as the ordinate, draw a working curve. 6 Calculation and expression of analysis results
Calculate the percentage of mercury according to the following formula:
Hg(%) = (m= - m). Vo× 10*5m..V.
Where: m2--the amount of mercury in the sample solution obtained from the working curve, g; × 100
m1--the amount of mercury in the empty solution accompanying the sample obtained from the working curve, ug; V. —Total volume of test solution, mL;
V,—-Volume of test solution taken, mL;
mo—Mass of test material, g.
Analysis results should retain two significant figures. 7 Allowable difference
The difference in analysis results between laboratories should not be greater than 0.00002%. 357
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