GB/T 6009-2014 English PDF (GBT6009-2014)

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GB/T 6009-2014: Anhydrous sodium sulfate for industrial use
GB/T 6009-2014
Anhydrous sodium sulfate for industrial use
ICS 71.060.50
G12
National Standards of People's Republic of China
Replace GB/T 6009-2003
Industrial anhydrous sodium sulfate
Released on.2014-07-08
2014-12-01 implementation
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
China National Standardization Administration issued
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB/T 6009-2003 "Industrial anhydrous sodium sulfate", compared with GB/T 6009-2003, except editorial modification
The technical changes are as follows.
---Adjusted the technical requirements of the product, improved the requirements of Class I superior products, and increased the aqueous solution (50g/L)
pH requirements (see 5.2,.2003 edition 4.2);
--- A method of determining the content of calcium and magnesium by atomic absorption (see 6.5, 5.5 of the.2003 edition);
--- The determination of chloride content has been increased by the silver method (see 6.6, 5.6 of the.2003 edition);
--- Increased pH determination method (see 6.10).
This standard was proposed by the China Petroleum and Chemical Industry Federation.
This standard is under the jurisdiction of the Inorganic Chemical Branch of the National Chemical Standardization Technical Committee (SAC/TC63/SC1).
This standard was drafted. Hunan Hengyang Xinyi Chemical Co., Ltd., CNOOC Tianjin Chemical Research and Design Institute, Nanfeng Chemical Group Co., Ltd.
Company, Sichuan Chuanmei Glauber's Salt Co., Ltd., Sichuan Hongyaqing Yijiang Yuanming Powder Co., Ltd., Tongbai Star Chemical Co., Ltd., and
Chang (Pengshan) Chemical Co., Ltd., Jiangsu Yinzhu Chemical Group Co., Ltd., National Salt Chemical Product Quality Supervision and Inspection Center (Jiangsu).
The main drafters of this standard. Liu Jian, Lu Siwei, Chen Aibing, Zou Huarong, Huang Guifang, Wu Guoyu, Zhou Yigang, Wang Yigui, Chen Changyi.
The previous versions of the standards replaced by this standard are.
---GB 6009-1985, GB/T 6009-1992, GB/T 6009-2003.
Industrial anhydrous sodium sulfate
1 Scope
This standard specifies the classification, requirements, test methods, inspection rules, marking, labeling, packaging, transportation and storage of industrial anhydrous sodium sulfate.
This standard applies to industrial anhydrous sodium sulfate. This product is mainly used in battery, optical glass, printing and dyeing, synthetic detergent, vinylon, dyeing
Industrial materials such as materials, ordinary glass, paper industry, fiber production and inorganic salts.
2 Normative references
The following documents are indispensable for the application of this document. For dated references, only dated versions apply to this article.
Pieces. For undated references, the latest edition (including all amendments) applies to this document.
GB/T 191-2008 packaging storage and transportation icon
GB/T 3049-2006 General method for determination of iron content of industrial chemical products 1,10-phenanthroline spectrophotometric method
GB/T 3051-2000 General method for determination of chloride content in inorganic chemical products
General rules for sampling GB/T 6678 chemical products
GB/T 6682-2008 Analytical laboratory water specifications and test methods
GB/T 8170 Numerical Rounding Rules and Representation and Determination of Limit Values
GB/T 23769-2009 General method for the determination of pH in aqueous solutions of inorganic chemical products
GB/T 23774-2009 General method for determination of whiteness of inorganic chemical products
Inorganic chemical products -- Preparation of standard solutions, preparations and products for chemical analysis - Part 1 . standard titration
Liquid preparation
HG/T 3696.2 Preparation of standard solutions, preparations and products for chemical analysis of chemical products - Part 2
Liquid preparation
Preparation of standard solutions, preparations and products for chemical analysis - Part 3. Preparations and preparations
Preparation
3 Molecular formula and relative molecular mass
Molecular formula. Na2SO4.
Relative molecular mass. 142.02 (according to.2011 international relative atomic mass).
4 classification
According to the use of industrial anhydrous sodium sulfate, it is divided into three categories.
---I class superior products, mainly used in batteries, optical glass, printing and dyeing, synthetic detergents, vinylon, fiber production, etc.;
--- Class II, mainly used in ordinary glass, dye, paper and other industries;
--- Class III, mainly used in industrial raw materials such as inorganic salts.
5 requirements
5.1 Appearance. Industrial anhydrous sodium sulfate is white crystalline particles.
5.2 Industrial anhydrous sodium sulfate should meet the requirements of Table 1.
Table 1 Technical requirements
project
index
Class I, Class II, Class III
First-class products, first-class products, first-class products, first-class products, first-class products, qualified products
Sodium sulfate (Na2SO4) w/% ≥ 99.6 99.0 98.0 97.0 95.0 92.0
Water insoluble matter w/% ≤ 0.005 0.05 0.10 0.20 - -
Calcium and magnesium (in Mg) w/% ≤ - 0.15 0.30 0.40 0.6 -
Calcium (Ca) w /% ≤ 0.01 - - - - -
Magnesium (Mg) w /% ≤ 0.01 - - - - -
Chloride (in terms of Cl) w/% ≤ 0.05 0.35 0.70 0.90 2.0
Iron (Fe) w /% ≤ 0.0005 0.002 0.010 0.040 - -
Moisture w/% ≤ 0.05 0.20 0.5 1.0 1.5 -
Whiteness (R457) /% ≥ 88 82 82 - - -
pH (50g/L aqueous solution, 25 ° C) 6~8 - - - - -
6 Test methods
Warning. Some of the reagents used in this test method are toxic or corrosive, and the operator should be cautious if splashed on the skin.
Rinse with water. In severe cases, treat immediately. When using flammable products, it is strictly forbidden to use an open flame.
6.1 General requirements
The reagents and water used in this standard refer to the analytical reagents and the three specified in GB/T 6682-2008 when no other requirements are specified.
Grade water.
Standard titration solutions, impurity standard solutions, preparations and products required in the test, according to HG/T 3696.1, if no other requirements are specified.
HG/T 3696.2, HG/T 3696.3 specifies the preparation.
6.2 Appearance inspection
The appearance was visually judged on a white-surface watch glass or a white porcelain plate under natural light.
6.3 Determination of sodium sulfate content
6.3.1 Weight method (arbitration method)
6.3.1.1 Method summary
Dissolve the sample in water and filter the insoluble matter. Under acidic conditions, add barium chloride and sulfate ions in the test solution to form barium sulfate.
Ding, filtration, ashing, burning, weighing, calculation.
6.3.1.2 Reagents
6.3.1.2.1 Hydrochloric acid solution. 1 1.
6.3.1.2.2 Barium chloride (BaCl2 · 2H2O) solution. 122g/L.
6.3.1.2.3 Silver nitrate solution. 20g/L.
6.3.1.3 Instruments
High temperature furnace. The temperature can be controlled at 800 °C ± 20 °C.
6.3.1.4 Analysis steps
6.3.1.4.1 Preparation of test solution
Approximately 5 g of the sample was weighed to the nearest 0.0002 g, placed in a 250 mL beaker, and 100 mL of water was added and dissolved by heating. Use medium speed
The quantitative filter paper was filtered into a 500 mL (V1) volumetric flask and washed with water until no sulfate ions (tested with barium chloride solution). Cooling, use
Dilute the water to the mark and shake well.
6.3.1.4.2 Determination
Pipette 25mL (V2) test solution, place it in a 500mL beaker, add 5mL hydrochloric acid solution and 270mL water, heat to
Micro boiling. 10mL of ruthenium chloride solution was added dropwise under stirring, and the addition time was about 1.5 minutes. Stirring was continued and the boiling was kept for 2 min~3 min.
Cover the watch glass and continue to hold for 5 min. The beaker was then placed on a boiling water bath for 2 h. Remove the beaker and cool to room temperature. Slowly
Filter the speed quantitative filter paper, wash the precipitate with warm water until there is no chloride ion (take 5mL washing solution, add 5mL silver nitrate solution and mix, place
No turbidity occurred in 5 minutes). Transfer the precipitate together with the filter paper to a porcelain crucible that has been burned at 800 ° C ± 20 ° C to a constant mass in an electric furnace
Dry and ash. Place in a high temperature furnace and burn at 800 °C ± 20 °C until the mass is constant.
6.3.1.5 Calculation of results
The sodium sulfate content is calculated by the formula (1) based on the mass fraction w1 of sodium sulfate (Na2SO4).
W1=
M1-m( )2 ×0.6086
m×V2/V1 ×
100%-5.844w3 (1)
In the formula.
The value of the volume of the test solution in V1 - 6.3.1.4.1, in milliliters (mL);
The value of the volume of the test solution taken in V2 --- 6.3.1.4.2, in milliliters (mL);
M1 --- barium sulfate precipitation and the quality of porcelain crucible, the unit is grams (g);
M2 --- the value of the mass of porcelain crucible, in grams (g);
m --- the value of the sample quality, in grams (g);
W3 --- The exact value of calcium and magnesium (in terms of Mg) measured according to 6.5;
0.6086---the coefficient of conversion of barium sulfate to sodium sulfate;
5.844 --- Calcium and magnesium are converted to the coefficient of sodium sulfate.
The arithmetic mean of the results of two parallel determinations is the measurement result, and the absolute difference of the parallel measurement results is not more than 0.2%.
6.3.2 Calculation method
6.3.2.1 Method summary
Subtracting water insolubles, magnesium sulfate, sodium chloride, ferric sulphate, moisture, and acidity or alkalinity from 100 to obtain sodium sulphate
content.
6.3.2.2 Calculation of results
The sodium sulfate content is calculated by the formula (2) based on the mass fraction w1 of sodium sulfate (Na2SO4).
W1=100%-(w2 4.951w3 1.648w4 3.580w5 w6 w7) (2)
In the formula.
W2 --- The exact value of the water insoluble mass fraction measured by 6.4;
W3 --- The exact value of the mass fraction of calcium and magnesium (in Mg) measured according to 6.5;
W4 --- The exact value of the mass fraction of chloride (in terms of Cl) measured according to 6.6;
W5 --- The exact value of the iron (Fe) mass fraction measured according to 6.7;
W6 --- The exact value of the mass fraction of moisture measured by 6.8;
W7 --- The exact value of the acidity (calculated as H2SO4) or alkalinity (calculated as Na2CO3) measured according to 6.11;
4.951---magnesium (Mg) is converted to the coefficient of magnesium sulfate (MgSO4);
1.648---the coefficient of conversion of chlorine (Cl) to sodium chloride (NaCl);
3.580---The coefficient of iron (Fe) converted to ferric sulfate [Fe2(SO4)3].
6.4 Determination of water insoluble content
6.4.1 Instruments
6.4.1.1 Glass mortar. The filter plate has a pore size of 5μm~15μm.
6.4.1.2 Electrothermal constant temperature drying oven. The temperature can be controlled at 105 °C ± 2 °C.
6.4.2 Analysis steps
Approximately 20 g of the sample was weighed to the nearest 0.01 g, placed in a 250 mL beaker, 100 mL of water was added, and dissolved by heating. Use clean, dry
The filter flask was filtered and filtered through a glass mortar which had been dried at 105 ° C ± 2 ° C to a constant mass. Wash with water until no sulfate ions, use chlorine
Test for phlegm solution (see 6.3.1.2.2). Place the glass mortar in an electric constant temperature drying oven and dry at 105 °C ± 2 °C to the quality
Constant.
The filtrate was cooled and transferred to a 500 mL (V1) volumetric flask, diluted to the mark with water, and shaken. This solution is test solution A, retain this
The solution is used for the determination of calcium and magnesium content titration and the determination of chloride content.
6.4.3 Calculation of results
The water insoluble content is calculated by the formula (3) based on the mass fraction w2.
W2=
M1-m2
m ×100%
(3)
In the formula.
M1---the value of the mass of water insoluble matter and glass mortar, in grams (g);
M2---the value of the mass of the glass mortar, in grams (g);
m --- The value of the mass of the sample in grams (g).
Taking the arithmetic mean of the results of two parallel determinations as the measurement results, the absolute difference of the parallel determination results is not greater than the class I superiority
0.0005%, Class I first class is not more than 0.005%, Class II is not more than 0.01%.
6.5 Determination of calcium and magnesium content
6.5.1 Atomic Absorption Method (Arbitration Law)
6.5.1.1 Method summary
After the sample is dissolved, in the nitric acid medium, the release agent cesium chloride and the deionization agent cesium chloride are used to eliminate the ionization interference, and the calcium and magnesium ions are respectively
The measurement was carried out by a flame atomic absorption spectrophotometer at wavelengths of 422.6 nm and 286.2 nm.
6.5.1.2 Reagents
6.5.1.2.1 Nitric acid solution. 19.
6.5.1.2.2 Barium chloride solution. 0.1g/L.
6.5.1.2.3 Barium chloride solution. 0.4g/L.
6.5.1.2.4 Calcium standard solution. 1mL solution containing calcium (Ca) 0.010mg, pipette 1mL of calcium prepared according to HG/T 3696.2
The standard solution was placed in a 100 mL volumetric flask, diluted to the mark with water, and shaken.
6.5.1.2.5 Magnesium standard solution. 1mL solution containing magnesium (Mg) 0.010mg, pipette 1mL of magnesium prepared according to HG/T 3696.2
The standard solution was placed in a 100 mL volumetric flask, diluted to the mark with water, and shaken.
6.5.1.2.6 Water. It meets the secondary water specified in GB/T 6682-2008.
6.5.1.3 Instruments
Flame atomic absorption spectrophotometer. equipped with calcium and magnesium cathode hollow lamps.
6.5.1.4 Analysis steps
6.5.1.4.1 Preparation of test solution
Weigh a certain amount of samples (about 10g for class I superiors, about 1g for first-class products, about 0.5g for class II, and about 0.5g for class III)
0.3g) sample, accurate to 0.01g, placed in a 250mL beaker, add 50mL water, 20mL nitric acid solution, heat to dissolve and continue to boil
After 5 min, transfer...