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YS/T 273.5-2006 English PDF (YST273.5-2006)

YS/T 273.5-2006 English PDF (YST273.5-2006)

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YS/T 273.5-2006: Chemical analysis methods and physical properties of cryolite. Part 5: Determination of sodium by flame atomic absorption spectrometric method

This Part specifies the method for the determination of sodium content in cryolite. This Part applies to the determination of sodium content in cryolite. Determination range: 20%~35%. 2 Method summary After the test portion is dissolved with sulfuric acid, it is heated to remove fluorine, and the precipitate is dissolved with hydrochloric acid and water; the sodium content of the test solution is determined at the wavelength of 589.0 nm or 589.6 nm of an atomic absorption spectrometer by the use of an air-acetylene fuel-lean flame. 3 Reagents 3.1 Sulfuric acid (???? 1.84 g/mL). 3.2 Hydrochloric acid (???? 1.19 g/mL). 3.3 Sodium standard solution: Weigh 3.089 g of anhydrous sodium sulfate that has been dried at 120 ????C and cooled in a desiccator, place it in a 250 mL beaker, and add 100 mL of water to dissolve; then, add 10 mL of hydrochloric acid (3.2), transfer the solution to a 1000 mL volumetric flask, dilute to volume with water, mix well, and transfer it to a polyethylene bottle. 1 mL of this solution contains 1.000 mg of sodium. 4 Apparatus 4.1 Platinum dish: The diameter is 80 mm, and the height is 35 mm. 4.2 Atomic absorption spectrometer: It is equipped with a sodium hollow cathode lamp. Any instrument that can meet the following indicators under the best working conditions can be used. YS/T 273.5-2006 www.ChineseStandard.net ? Buy True-PDF ? A and quot;delivery Page 6 of 8 -- Characteristic concentration: In a solution consistent with the matrix of the measured sample, the characteristic concentration of sodium shall not be
YS/T 273.5-2006
YS
NONFERROUS METAL INDUSTRY STANDARD
OF THE PEOPLE'S REPUBLIC OF CHINA
ICS 71.100.10
H 21
Replacing YS/T 273.5-1994
Chemical analysis methods and physical properties of
cryolite - Part 5: Determination of sodium by flame atomic
absorption spectrometric method
ISSUED ON: MAY 25, 2006
IMPLEMENTED ON: DECEMBER 1, 2006
Issued by: National Development and Reform Commission of PRC
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Method summary ... 5
3 Reagents ... 5
4 Apparatus ... 5
5 Sample ... 6
6 Analysis procedure ... 6
7 Calculation of analysis results ... 7
8 Precision ... 8
9 Quality assurance and control ... 8
Foreword
YS/T 273 "Chemical analysis methods and physical properties of cryolite" is divided into 13 parts:
-- Part 1: Determination of moisture content - Gravimetric method;
-- Part 2: Determination of ignition loss;
-- Part 3: Determination of fluoride content;
-- Part 4: Determination of aluminum content - EDTA titration method;
-- Part 5: Determination of sodium by flame atomic absorption spectrometric method;
-- Part 6: Determination of silica content by the molybdenum blue photometric; -- Part 7: Determination of iron content by orthophenantholine photometric method; -- Part 8: Determination of sulfate content - Barium sulfate gravimetric method; -- Part 9: Determination of phosphorus pentoxide content - Molybdenum blue photometric method;
-- Part 10: Determination of alumina content by gravimetric method;
-- Part 11: Determination of sulphur content by X-ray fluorescence spectrometric method;
-- Part 12: The atomic absorption spectrophotometric method for the determination of calcium oxide content;
-- Part 13: Preparation and storage of test samples.
This Part is Part 5.
This part is a revision of YS/T 273.5-1994. In addition to editorial modification, two chapters on Precision AND Quality Assurance and Control have been added. Other changes include:
-- The measuring wavelength of the instrument is changed from the most sensitive 589.0 nm to the hypo-sensitive 589.6 nm;
-- The length of the working curve is shortened, and the concentration of the highest concentration standard solution in the working curve is reduced from 10.0 ??g/mL to 5.00 ??g/mL;
Chemical analysis methods and physical properties of
cryolite - Part 5: Determination of sodium by flame atomic
absorption spectrometric method
1 Scope
This Part specifies the method for the determination of sodium content in cryolite. This Part applies to the determination of sodium content in cryolite. Determination range: 20%~35%.
2 Method summary
After the test portion is dissolved with sulfuric acid, it is heated to remove fluorine, and the precipitate is dissolved with hydrochloric acid and water; the sodium content of the test solution is determined at the wavelength of 589.0 nm or 589.6 nm of an atomic absorption spectrometer by the use of an air-acetylene fuel-lean flame. 3 Reagents
3.1 Sulfuric acid (?? 1.84 g/mL).
3.2 Hydrochloric acid (?? 1.19 g/mL).
3.3 Sodium standard solution: Weigh 3.089 g of anhydrous sodium sulfate that has been dried at 120 ??C and cooled in a desiccator, place it in a 250 mL beaker, and add 100 mL of water to dissolve; then, add 10 mL of hydrochloric acid (3.2), transfer the solution to a 1000 mL volumetric flask, dilute to volume with water, mix well, and transfer it to a polyethylene bottle. 1 mL of this solution contains 1.000 mg of sodium. 4 Apparatus
4.1 Platinum dish: The diameter is 80 mm, and the height is 35 mm.
4.2 Atomic absorption spectrometer: It is equipped with a sodium hollow cathode lamp. Any instrument that can meet the following indicators under the best working conditions can be used.
-- Characteristic concentration: In a solution consistent with the matrix of the measured sample, the characteristic concentration of sodium shall not be greater than 0.07 ug/mL.
-- Precision: Use the standard solution with the highest concentration to measure the absorbance 10 times, and the standard deviation shall not exceed 1.0% of the average absorbance; use the standard solution with the lowest concentration (not the "zero" concentration standard solution) to measure the absorbance 10 times, and the standard deviation shall not exceed 0.5% of the average
absorbance of the highest concentration standard solution.
-- Working curve linearity: Divide the working curve into 5 equal segments according to concentration, and the ratio of the absorbance difference in the highest segment to the absorbance difference in the lowest segment is not less than 0.85.
5 Sample
The sample shall comply with the requirements of 3.3 in YS/T 273.13.
6 Analysis procedure
6.1 Test portion
Weigh 0.5 g of test sample (5), accurate to 0.0001 g.
6.2 Number of determinations
Two determinations shall be carried out independently and the average value shall be taken.
6.3 Blank test
Do a blank test along with the sample test.
6.4 Determination
6.4.1 Place the test portion (6.1) in the platinum dish (4.1), add 5 mL of sulfuric acid (3.1), and slowly dissolve it in a sand bath (15 min~20 min) to remove fluorine; then, heat it to evaporate until the thick smoke emits; remove the test portion and cool it to room temperature; add 3 mL of hydrochloric acid (3.2) and 30 mL of water, and heat in a low-temperature sand bath until all salts are dissolved. After cooling, transfer the solution to a 500 mL volumetric flask, dilute to volume with water, and mix well. 6.4.2 According to Table 1, take the test solution (6.4.1), place it in a 500 mL volumetric

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