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GB/T 6009-2014 PDF in English


GB/T 6009-2014 (GB/T6009-2014, GBT 6009-2014, GBT6009-2014)
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GB/T 6009-2014: PDF in English (GBT 6009-2014)

GB/T 6009-2014
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.50
G 12
Replacing GB/T 6009-2003
Anhydrous sodium sulfate for industrial use
工业无水硫酸钠
ISSUED ON: JULY 08, 2014
IMPLEMENTED ON: DECEMBER 01, 2014
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Molecular formula and relative molecular mass ... 5 
4 Classification ... 5 
5 Requirements ... 5 
6 Test methods ... 6 
7 Inspection rules ... 22 
8 Markings and labels ... 23 
9 Packaging, transportation, storage ... 23 
Anhydrous sodium sulfate for industrial use
1 Scope
This standard specifies the classification, requirements, test methods,
inspection rules, marking, labeling, packaging, transportation, storage of
anhydrous sodium sulfate for industrial use.
This standard applies to anhydrous sodium sulfate for industrial use. This
product is mainly used as the industrial raw materials such as battery, optical
glass, printing-dyeing, synthetic detergent, vinylon, dye, ordinary glass, paper
industry, fiber production, inorganic salt, etc.
2 Normative references
The following documents are essential to the application of this document. For
the dated documents, only the versions with the dates indicated are applicable
to this document; for the undated documents, only the latest version (including
all the amendments) are applicable to this standard.
GB/T 191-2008 Packaging - Pictorial marking for handling of goods
GB/T 3049-2006 Chemical products for industrial use - General method for
determination of iron content - 1 10-Phenanthroline spectrophotometric
method
GB/T 3051-2000 Inorganic chemical products for industrial use - General
method for determination of chloride content - Mercurimetric method
GB/T 6678 General principles for sampling chemical products
GB/T 6682-2008 Water for analytical laboratory use - Specification and test
methods
GB/T 8170 Rules for rounding off for numerical values & expression and
judgement of limiting values
GB/T 23769-2009 Inorganic chemical products - General method for the
determination of pH values
GB/T 23774-2009 Inorganic chemical products - General method for
determination of whiteness
Use water to dissolve the sample and filter the insoluble matter. Under acidic
conditions, add cerium chloride to react with the sulfate ion in the test solution
to form barium sulfate precipitate. Filter it. Ash it. Burn it. Weigh it. Make
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: 122 g/L.
6.3.1.2.3 Silver nitrate solution: 20 g/L.
6.3.1.3 Instruments
High-temperature furnace: The temperature can be controlled at 800 °C ± 20 °C.
6.3.1.4 Analytical procedures
6.3.1.4.1 Preparation of test solution
Weigh approximately 5 g of the specimen, accurate to 0.0002 g. Place it in a
250 mL beaker. Add 100 mL of water. Heat to dissolve it. Use a medium speed
quantitative filter paper to filter the solution into a 500 mL (V1) volumetric flask.
Use water to rinse it until there is no sulfate ions (tested by barium chloride
solution). Cool it. Use water to dilute it to the mark. Shake it uniformly.
6.3.1.4.2 Determination
Pipette 25 mL (V2) of test solution. Place it in a 500 mL beaker. Add 5 mL of
hydrochloric acid solution and 270 mL of water. Heat to slight boiling. Add
dropwise 10 mL of ruthenium chloride solution whilst stirring it. The addition
time is about 1.5 min. Continue stirring and keep slight boiling for 2 min ~ 3 min.
Cover the watch glass. Continue keeping slight boiling for 5 min. Then place
the beaker in the boiling water bath for thermal insulation for 2 h. Remove the
beaker. Cool it to room temperature. Use the slow-speed quantitative filter
paper to filter it. Use warm water to rinse the precipitate until there is no chloride
ion (take 5 mL of rinsing solution; add 5 mL of silver nitrate solution; mix it
uniformly; place it for 5 min; there is no turbidity). Transfer the precipitate
together with the filter paper into a porcelain crucible which had been burned at
800 °C ± 20 °C to a constant mass. Dry it on an electric furnace and ash it.
Place it in a high-temperature furnace. Burn it at 800 °C ± 20 °C until the mass
is constant.
6.3.1.5 Calculation of results
The sodium sulfate content is calculated based on the mass fraction w1 of
w3 - The exact value of the mass fraction of calcium and magnesium (in
terms of Mg) as measured in 6.5;
w4 - The exact value of the mass fraction of chloride (in terms of Cl) as
measured in 6.6;
w5 - The exact value of the mass fraction of iron (Fe) as measured in 6.7;
w6 - The exact value of the mass fraction of moisture as measured in 6.8;
w7 - The exact value of the mass fraction (calculated as H2SO4) or alkalinity
(calculated as Na2CO3) as measured in 6.11;
4.951 - The factor of converting magnesium (Mg) to magnesium sulfate
(MgSO4);
1.648 - The factor of converting chlorine (Cl) to sodium chloride (NaCl);
3.580 - The factor of converting iron (Fe) 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 5 μm ~ 15 μm.
6.4.1.2 Electrothermal constant temperature drying oven: The temperature can
be controlled at 105 °C ± 2 °C.
6.4.2 Analytical procedures
Weight approximately 20 g of the specimen, accurate to 0.01 g. Place it in a
250 mL beaker. Add 100 mL of water. Heat to dissolve it. Use a clean and dry
suction filter bottle and a glass mortar that has been dried at 105 °C ± 2 °C to
a constant mass to filter it. Use water to rinse it until there is no sulfate ion. Use
barium chloride solution (see 6.3.1.2.2) for inspection. Place the glass mortar
in an electrothermal constant temperature drying oven. Dry it at 105 °C ± 2 °C
until the mass is constant.
After cooling the filtrate, transfer it into a 500 mL (V1) volumetric flask. Use water
to dilute it to the mark. Shake it uniformly. This solution is the test solution A.
Keep this solution for the determination by titration of calcium and magnesium
as well as the determination of chloride content.
6.4.3 Calculation of results
The water insoluble content is calculated based on the mass fraction w2 through
the formula (3):
6.5.1.2.6 Water: The grade II water which complies with the requirements of
GB/T 6682-2008.
6.5.1.3 Instruments
Flame atomic absorption spectrophotometer: It is equipped with calcium and
magnesium cathode hollow lamps.
6.5.1.4 Analytical procedures
6.5.1.4.1 Preparation of test solution
Weigh a certain amount of specimen (about 10 g for category-I superior
products; about 1 g for category-II products; about 0.5 g for category-III
products; about 0.3 g for category-III products), accurate to 0.01 g. Place it in a
250 mL beaker. Add 50 mL of water and 20 mL of nitric acid solution. Heat to
dissolve it. Continue boiling it for 5 min. After cooling it, transfer it all into a 500
mL (V1) volumetric flask. Use water to dilute it to the mark. Shake it uniformly.
Dry filter it. Prepare for use.
6.5.1.4.2 Drawing of working curve
Pipette 0.00 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL, 10.00 mL of calcium and
magnesium standard solution into six 100 mL volumetric flasks. Add 1.0 mL of
nitric acid solution, 2.0 mL of lanthanum chloride solution, 1.5 mL of cesium
chloride solution. Use water to dilute it to the mark. Shake it uniformly. Calcium
is measured at a wavelength of 422.6 nm and magnesium at a wavelength of
286.2 nm using water as a reference by a flame atomic absorption
spectrophotometer. Use the mass of calcium and magnesium as the abscissa
and the corresponding absorbance as the ordinate to draw the working curve.
6.5.1.4.3 Determination
Pipette 25 mL (V2) of test solution. Place it in a 100 mL volumetric flask. Add
2.0 mL of lanthanum chloride solution and 1.5 mL of cesium chloride solution.
Use water to dilute it to the mark. Shake it uniformly. Make determination
together with the standard solution. Based on the absorbance of the sample
solution, find the mass of calcium and magnesium in the specimen from the
working curve.
6.5.1.5 Calculation of results
The calcium content is calculated based on the mass fraction of calcium (Ca)
wCa through the formula (4):
6.5.1.4.3;
wMg - The exact value of the mass fraction of magnesium (Mg) as measured
in 6.5.1.4.3;
0.606 - The factory of converting calcium (Ca) to magnesium (Mg).
6.5.2 Titration method
6.5.2.1 Summary of method
Using chrome black T as an indicator. Use the standard titration solution of
disodium edetate to titrate the calcium and magnesium in the test solution.
6.5.2.2 Reagents
6.5.2.2.1 Triethanolamine solution: 1 + 3.
6.5.2.2.2 Sodium sulfide solution: 20 g/L.
6.5.2.2.3 Ammonia-ammonium chloride buffer solution A: pH ≈ 10.
6.5.2.2.4 Ethylenediaminetetraacetic acid disodium (EDTA) standard titration
solution: c (EDTA) ≈ 0.02 mol/L.
6.5.2.2.5 Chrome black T indicator.
6.5.2.3 Instruments
Micro-burette: The index value is 0.01 mL or 0.02 mL.
6.5.2.4 Analytical procedures
Pipette 25 mL (V2) of test solution A (see 6.4.2). Place it in a 250 mL conical
flask. Add 25 mL of water and 2 mL of triethanolamine solution. If there is
interference by copper, add another 1 mL of sodium sulfide solution. Add 5 mL
of ammonia-ammonium chloride buffer solution A and about 0.1 g of chrome
black T indicator. Use the standard titration solution of disodium edetate to
titrate it until the solution changes from magenta to blue, which is the end point.
6.5.2.5 Calculation of results
The calcium and magnesium contents are calculated based on the mass
fraction of magnesium (Mg), w3, through the formula (7):
6.6.1.4 Analytical procedures
Pipette 25 mL (V2) of test solution A (see 6.4.2). Place it in a 250 mL conical
flask. Add water to 100 mL. Add 3 drops of bromophenol blue indicator solution.
If the solution is blue, add a nitric acid solution (1 mol/L) until the solution turns
yellow. Add another 1 mL. If the solution is yellow, add dropwise sodium
hydroxide solution (1 mol/L) until the solution turns blue. Then add dropwise the
nitric acid solution (1 mol/L) until the solution turns yellow. Add another 1 mL.
Add 1 mL of diphenyl azo carbazide indicator solution. Use the 0.05 mol/L
mercury nitrate standard titration solution to titrate it until it changes into purple
red which is same as that of the reference solution. This is the end point. The
treatment of mercury-containing waste liquid is carried out according to
Appendix D of GB/T 3051-2000.
6.6.1.5 Calculation of results
The chloride is calculated according to the mass fraction of chlorine (Cl), w4,
through the formula (8):
Where:
V - The value of the volume of the standard titration solution of mercury
nitrate as consumed in the measurement, in milliliters (mL);
V0 - The volume of the standard titration solution of mercury nitrate as
consumed in the preparation of the reference solution, in milliliters (mL);
V1 - The value of the volume of test solution A in 6.4.2, in milliliters (mL);
V2 - The value of the volume of test solution A in 6.6.1.4, in milliliters (mL);
c - The exact value of the concentration of the standard titration solution of
mercury nitrate, in moles per liter (mol/L);
m - The value of the mass of the sample as contained in test solution A in
6.4.2, in grams (g);
M - The molar mass of chlorine (M = 35.45), in grams per mole (g/mol).
Take the arithmetic mean of the results of two parallel determinations as the
measurement result. The absolute difference of the parallel determination
results is not more than 0.005% for the category-I superior products, not more
than 0.02% for the category-I first grade products and category-II products, not
more than 0.05% for the category-III products.
Take the arithmetic mean of the results of two parallel determinations as the
measurement result. The absolute difference of the parallel determination
results is not more than 0.005% for the category-I superior products, not more
than 0.02% for the category-I first grade products and category-II products, not
more than 0.05% for the category-III products.
6.7 Determination of iron content
6.7.1 Summary of method
Same as Chapter 3 of GB/T 3049-2006.
6.7.2 Reagents
6.7.2.1 Hydrochloric acid.
6.7.2.2 Ammonia solution: 1 + 1.
Others are the same as Chapter 4 of GB/T 3049-2006.
6.7.3 Instruments and equipment
Spectrophotometer: Equipped with cuvettes which have a thicknesses of 2 cm
and 5 cm.
6.7.4 Drawing of working curve
According to the provisions of 6.3 of GB/T 3049-2006, use 2 cm and 5 cm
cuvettes and the corresponding iron standard solution to draw the working
curve, respectively.
6.7.5 Analytical procedures
6.7.5.1 Preparation of test solution
Weigh approximately 10 g of the specimen, accurate to 0.01 g. Place it in a 250
mL beaker. Add 50 mL of water and 25 mL of hydrochloric acid (see 6.7.2.1).
Heat to boiling and completely dissolve it. Continue boiling it for 5 min. After
cooling, transfer it all into a 500 mL (V1) volumetric flask. Use water to dilute it
to the mark. Shake it uniformly. Dry filter it to prepare for use.
6.7.5.2 Preparation of blank test solution
Add 50 mL of water and 25 mL of hydrochloric acid (see 6.7.2.1) to a 250 mL
beaker. Heat to boil it for 5 min. After cooling, transfer it into a 500 mL volumetric
flask. Dilute it to the mark. Shake it uniformly.
6.7.5.3 Determination
6.8.1.2 Electrothermal constant temperature drying oven: The temperature can
be controlled at 105 °C ± 2 °C.
6.8.2 Analytical procedures
Use the weighing bottle which had been dried at 105 °C ± 2 °C to a constant
mass to weigh 5 g ~ 20 g of specimen, accurate to 0.0002 g. Place it in an
electrothermal constant temperature drying oven. Dry it at 105 °C ± 2 °C until
the mass is constant.
6.8.3 Calculation of results
The moisture mass fraction w6 is calculated according to formula (11):
Where:
m1 - The mass of the sample after drying, in grams (g);
m - The mass of the sample, in grams (g).
Take the arithmetic mean of the results of two parallel determinations as the
measurement result. The absolute difference of the parallel determination
results is not more than 0.005% for the category-I products, not more than 0.02%
for the category-I first grade products, category-II and category-III superior
products, not more than 0.05% for the category-III first-grade products.
6.9 Determination of whiteness
6.9.1 Instruments
Same as Chapter 4 of GB/T 23774-2009.
6.9.2 Analytical procedures
The determination is carried out in accordance with the provisions of Chapter 5
of GB/T 23774-2009.
6.9.3 Calculation of results
It is calculated according to the provisions of 6.1 of GB/T 23774-2009.
Take the arithmetic mean of the parallel measurement results as the
measurement result. The absolute difference of the parallel determination
results is not more than 0.6%.
6.10 Determination of pH
......
 
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