GB/T 4375.11-1984 Chemical analysis of gallium - Determination of mercury by cold atomic absorption spectrophotometry GB/T4375.11-1984 standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Chemical Analysis Methods
Methods for chemical analysis of galliumThe cold vapor atomic absorption spectrophotomectric method forthe determination of mcrcury contentThis standard applies to the determination of mercury in gallium. Determination range: 0.000020~0.00010%. UDC 669.871 : 543
42 : 56,49
GB 4375.11..-84
This standard complies with GB1467--78 "General Principles and General Regulations for Chemical Analysis Methods of Metallurgical Products". 1 Method Summary
The sample is dissolved in nitric acid and sulfuric acid, with chlorine as the reducing agent and air as the carrier gas, and the generated vapor is introduced into the gas measuring instrument for measurement.
2 Reagents
2.1 Nitric acid, high purity (specific gravity 1.42). 2.2 Hydrochloric acid, high purity (1+1).
2.3 Sulfuric acid, high purity (1+35)
2.4 Stannous chloride solution (10%): Weigh 10g of stannous chloride (SmCl21,0) and dissolve it in 10Hml of hydrochloric acid (1+1). Prepare it before use.
2.5 Mercury standard storage solution: Weigh Take 1.000g pure mercury (more than 99.9%), put it in a 250ml beaker, add 20~30ml magnetic acid (1+1), put it in a fume hood and slowly heat to dissolve, after it is completely dissolved, dilute it with water, put it into a 100ml volumetric flask, dilute it to the mark with water, and mix it. This solution contains 1.0mg of water in 1ml. 2.6 Polymer standard solution: Take 10.00ml of mercury standard storage solution (2.), put it in a 1ml volumetric flask, add 1ml phosphoric acid (2.1), dilute it to the mark with water, and mix it. This solution contains 100μg mercury in 1ml. 2.7 Mercury standard solution: Take 10.00ml of permanent standard solution (2.6), put it in a 100ml volumetric flask, add 1ml nitric acid (2.1), dilute it to the mark with water, and mix it. This solution contains 10μg of mercury in 1ml. 2.8 Mercury standard solution: Take 10.00ml of the standard solution (2.7), put it into a 100ml volumetric flask, add 1ml of nitric acid (2.1), dilute it with water to 1/3 inch, and mix it. This solution contains 1ml of mercury. 2.9 Compressed gas (packed in a steel cylinder, or produced by an electric pneumatic machine), 3 Instruments and volume
Mercury vapor "detector and accessory devices are shown in the figure. National Bureau of Standards 1984-04-30 Issued 1985-04-01 Implementation
GB 4375.11-84
Mercury vapor detection technology and accessory devices Figure
[一 Use narrow 2-mil 3-way piston: 4-reactor; 5·Calcium chloride section, 1-unused device (make way, once the non-Chinese museum measuring instrument to the following indicators:
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Minimum sensitivity: "The absorption reading of the highest concentration standard solution of the equal concentration standard solution used in the line should not be lower than" 1. Curve curve: In the concentration range, the difference between the absorption readings of the highest and second concentration standard solutions should not be less than 1/2 times of the absorption readings of the lowest concentration standard solution and the zero concentration solution. Minimum precision: The coefficient of variation of the absorption readings obtained by multiple measurements of the highest concentration standard solution and the second concentration standard solution used in the line to the average absorption reading of the highest concentration standard solution, Should be less than 4.5, 1.6: Calculation of coefficient of variation in stability (supplementary)
4 Analysis steps
41 Determination number
Weigh the two samples for adjustment and take the average load.
4.a Empty door test
Avoid the same sample for hollow test,
4.4 Determination
4.4.1 Place the sample (4.2) in a volume of 11 ml without burning, 2 ml acid (2.1), 1ml sulfuric acid (2.2), cover with a screw cap, and after the violent reaction stops, move to about 100°C to heat the test solution to make it gradually dissolve, continue to heat the test solution to remove nitrogen oxides, and after the test solution becomes full and softened, take the beaker and leave it for a while, transfer the liquid to the colorimetric tube with water and dilute to 2.2. The liquid should be stabilized in advance, avoid zero point, and adjust the gas flow to 51min. Transfer the test solution (4.4.1) into the reaction chamber, quickly add 1 tin chloride solution (2.) immediately, turn on the sound box, and turn the reaction chamber to the reaction chamber. Air is passed through the reactor and the maximum reading is recorded. The line is calculated from the result. 4.51 Test line
Take 4.05, D.12, 0.20, 0.3ml water standard (2.8), respectively, and place them in colorimetric tubes! Dilute with sulfuric acid (2.3) to 29.0m. The following is carried out according to 1.1.2. With the result as the reference, draw a line with the reading value as the ordinate. ate
5 Calculation of analysis results
Calculate the percentage of the maximum content of the result according to the following formula:
GB 4375.11—84
He(%) =
mg×10t
× 10)
Formula: m is the sample rate in liquid obtained from the working curve, m, is the blank rolling liquid of the sample obtained from the white curve, a
6 is the allowable difference
sample volume, for consideration.
The difference in analytical results between laboratories should not be too large. The following table lists the allowable and acceptable values.
0.004002~0.00m5
: u.t10005 -0.0001u
GB4375.11--84
Appendix A
Calculation of the minimum stability coefficient of variation
(Supplement)
The calculation formula for the coefficient of variation between the absorbance of the highest concentration standard solution and the zero concentration drop solution is as follows S.
E(CC)2
E(0-0)2
Where: S. — coefficient of variation of absorbance of the highest concentration standard solution: C—— absorbance variation of the highest concentration standard solution: C——average value of absorbance of the highest concentration standard solution; n——number of measurements:
S, — coefficient of variation of absorbance of zero concentration solution (—absorbance of zero concentration solution: bzxZ.net
0average value of absorbance of zero concentration solution.
Additional remarks:
This standard was proposed by the General Nonferrous Metals Industry Corporation. This standard was drafted by the Nonferrous Metals Research Institute of the Nonferrous Metals Industry Corporation. The main drafter of this standard is Liu Long.
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