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GB/T 26523-2011 PDF in English


GB/T 26523-2011 (GB/T26523-2011, GBT 26523-2011, GBT26523-2011)
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GB/T 26523-2011: PDF in English (GBT 26523-2011)

GB/T 26523-2011
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.50
G 12
Refined cobaltous sulfates
精制硫酸钴
ISSUED ON: MAY 12, 2011
IMPLEMENTED ON: DECEMBER 01, 2011
Issued by: General Administration of Quality Supervision, Inspection
and Quarantine;
Standardization Administration of the People’s Republic of
China.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Molecular formula and relative molecular mass ... 5 
4 Requirements ... 5 
5 Test method ... 5 
6 Inspection rules ... 24 
7 Marking, labeling ... 25 
8 Packaging, transportation, storage ... 25 
Appendix A (Informative) Method for processing mercury waste liquid ... 26 
Refined cobaltous sulfates
1 Scope
This Standard specifies the requirements, test methods, inspection rules,
marking, labeling, packaging, transportation and storage of refined cobaltous
sulfates.
This Standard applies to refined cobaltous sulfates that are mainly used in
industries such as chemical industry, electroplating industry, battery industry,
chemical reagents.
2 Normative references
The following documents are indispensable for the application of this document.
For dated references, only the dated version applies to this document. For
undated references, the latest edition (including all amendments) applies to this
document.
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 6678, General principles for sampling chemical products
GB/T 6682-2008, Water for analytical laboratory use - Specification and test
methods
GB/T 8170, Rules of rounding off for numerical values & expression and
judgment of limiting values
GB/T 9724-2007, Chemical reagent - General rule for the determination of
pH
GB/T 16488-1996, Water quality - Determination of petroleum oil, animal and
vegetable oils - Infrared photometric method
HG/T 3696.1, Inorganic chemical products - Preparations of standard
volumetric solutions for chemical analysis
HG/T 3696.2, Inorganic chemical products - Preparations of standard
solutions for chemical analysis
immediately with water. In severe cases, treat immediately. When
flammable products are used, it is strictly forbidden to use an open flame
for heating.
5.2 General provisions
The reagents and water that are used in this Standard, when no other
requirements are specified, refer to analytical reagents and grade-III water
which is specified in GB/T 6682-2008. All the reagents and water that are used
in the atomic absorption method in the Standard refer to the guaranteed
reagents and the grade-II water that is specified in GB/T 6682-2008. The
standard titration solutions, impurity standard solutions, preparations and
products that are used in the test shall be prepared in accordance with the
provisions of HG/T 3696.1, HG/T 3696.2, HG/T 3696.3 when no other
requirements are specified.
5.3 Appearance inspection
Under natural light, visually judge the appearance.
5.4 Determination of cobalt content
5.4.1 Method summary
In an acid solution, add hydroxylamine hydrochloride to the test solution to
reduce the iron; cobalt and thiocyanate form cobalt thiocyanate [Co(SCN)4]2-
blue complex; in the presence of acetone, use Ethylene Diamine Tetraacetic
Acid (EDTA) standard titration solution and cobalt to form a complex; when it
reaches the end point, the blue color disappears.
5.4.2 Reagents
5.4.2.1 Hydroxylamine hydrochloride.
5.4.2.2 Ammonium thiocyanate.
5.4.2.3 Acetone.
5.4.2.4 Saturated ammonium acetate solution.
5.4.2.5 Ethylene Diamine Tetraacetic Acid standard titration solution: c(EDTA)
≈ 0.05 mol/L.
5.4.3 Analysis steps
Weigh about 0.35 g ~ 0.40 g of sample, accurate to 0.000 2 g; put in 250 mL
conical flask; add 50 mL of water, 0.25 g of hydroxylamine hydrochloride; add
10 g of ammonium thiocyanate; add 4 mL of saturated ammonium acetate
5.5.2.3 Zinc standard solution: 1 mL of solution contains 0.01 mg of zinc (Zn).
Pipette 1 mL of the zinc standard solution that is prepared according to HG/T
3696.2; place it in a 100 mL volumetric flask; use water to dilute to the mark;
shake well.
5.5.2.4 Iron standard solution: 1 mL of solution contains 0.1 mg of iron (Fe).
Pipette 10 mL of the iron standard solution that is prepared according to HG/T
3696.2; place it in a 100 mL volumetric flask; use water to dilute to the mark;
shake well.
5.5.2.5 Copper standard solution: 1 mL of solution contains 0.1 mg of copper
(Cu).
Pipette 10 mL of the copper standard solution that is prepared according to
HG/T 3696.2; place it in a 100 mL volumetric flask; use water to dilute to the
mark; shake well.
5.5.2.6 Lead standard solution: 1 mL of solution contains 0.1 mg of lead (Pb).
Pipette 10 mL of the lead standard solution that is prepared according to HG/T
3696.2; place it in a 100 mL volumetric flask; use water to dilute to the mark;
shake well.
5.5.2.7 Cadmium standard solution: 1 mL of solution contains 0.01 mg of
cadmium (Cd).
Pipette 1 mL of the cadmium standard solution that is prepared according to
HG/T 3696.2; place it in a 100 mL volumetric flask; use water to dilute to the
mark; shake well.
5.5.2.8 Manganese standard solution: 1 mL of solution contains 0.1 mg of
manganese (Mn).
Pipette 10 mL of the manganese standard solution that is prepared according
to HG/T 3696.2; place it in a 100 mL volumetric flask; use water to dilute to the
mark; shake well.
5.5.2.9 Acetylene: high purity.
5.5.3 Instruments and apparatuses
Atomic absorption spectrophotometer: it is equipped with nickel hollow cathode
lamp, zinc hollow cathode lamp, iron hollow cathode lamp, copper hollow
cathode lamp, lead hollow cathode lamp, cadmium hollow cathode lamp and
manganese hollow cathode lamp.
In sulfuric acid solution, use potassium permanganate to oxidize chromium to
hexavalent; hexavalent chromium forms a purple complex with
diphenylcarbazide in sulfur-phosphorus mixed acid solution; after using isoamyl
alcohol for extraction, at a wavelength of 545 nm, use a spectrophotometer to
measure its absorbance.
5.8.2 Reagents
5.8.2.1 Sodium nitrite solution.
5.8.2.2 Sulfuric acid solution: 1+2.
5.8.2.3 Phosphoric acid solution: 1+2.
5.8.2.4 Urea solution: 200 g/L.
5.8.2.5 Potassium permanganate solution: 40 g/L.
5.8.2.6 Diphenylcarbazide solution: 1 g/L.
Weigh 0.1 g of diphenylcarbazide in 100 mL of acetone that contains 1 mL of
sulfuric acid solution (1+9); store in a brown bottle.
5.8.2.7 Isoamyl alcohol.
5.8.2.8 Chromium standard solution: 1 mL of solution contains 0.005 mg of
chromium (Cr).
Preparation: pipette 1 mL of the chromium standard solution that is prepared
according to HG/T 3696.2; place it in a 100 mL volumetric flask; use water to
dilute to the mark; shake well. Weigh 50 mL in a 100 mL volumetric flask; use
water to dilute to the mark; shake well. Formulate this solution when needed.
5.8.3 Instruments
5.8.3.1 Conical separating funnel: 125 mL.
5.8.3.2 Spectrophotometer: it is equipped with a 1 cm absorption cell.
5.8.4 Analysis steps
5.8.4.1 Preparation of test solution A
Weigh about 2 g of the superior product and about 0.5 g of the first-class product,
accurate to 0.001 g; put them in a 250 mL beaker; add 40 mL of water to
dissolve; add 0.5 mL of sulfuric acid solution; dropwise add potassium
permanganate solution until the solution remains purplish red; carefully heat
and boil for 3 min. After cooling, add 2 mL of urea solution; shake well; add
5.9 Determination of mercury content
5.9.1 Cold atomic absorption spectrometry (arbitration method)
5.9.1.1 Method summary
The sample is dissolved in the acid solution; the contained mercury compound
exists in an ionic state; add a reducing agent to reduce it to an atomic state
(elemental mercury vapor). Bring out the mercury by the airflow; measure the
mercury at a wavelength of 253.7 nm in the quartz tube. The absorption value
is proportional to the mercury content in a certain concentration range. Find the
mercury content from the working curve.
5.9.1.2 Reagents
5.9.1.2.1 Hydrochloric acid solution: 1+4.
5.9.1.2.2 Stannous chloride hydrochloric acid solution: weigh 25 g of stannous
chloride to dissolve in 50 mL of hot concentrated hydrochloric acid; after cooling,
move to a 250 mL volumetric flask; use water to dilute to the mark; shake well.
5.9.1.2.3 Iodine solution: 2.5 g/L.
5.9.1.2.4 Stock solution of mercury standard solution: 1 mL of solution contains
0.1 mg of mercury (Hg).
Pipette 10 mL of the mercury standard solution that is prepared according to
HG/T 3696.2; place it in a 100 mL volumetric flask; dilute to the mark; shake
well.
5.9.1.2.5 Mercury standard solution: 1 mL of solution contains 0.001 mg of
mercury (Hg).
Pipette 1 mL of stock solution of mercury standard solution in a 100 mL
volumetric flask; dilute to the mark; shake well. Prepare this solution when used.
5.9.1.3 Instruments and apparatuses
5.9.1.3.1 Atomic absorption spectrophotometer: with low-pressure mercury
lamp or hollow cathode lamp.
5.9.1.3.2 Quick response recorder.
5.9.1.4 Analysis steps
5.9.1.4.1 Preparation of test solution
Take the arithmetic mean of the parallel determination results as the
determination result; the absolute difference between the parallel determination
results shall not be larger than 0.000 1%.
5.9.2 Cold atomic fluorescence method
5.9.2.1 Method summary
Nitric acid dissolves the sample. In an acid solution, use stannous chloride to
reduce divalent mercury ions to mercury atoms; use high-purity argon gas to
introduce into an atomic fluorescence absorption cell; use the cold atomic
fluorescence method to determine.
5.9.2.2 Reagent
Hydrochloric acid solution (5+95) and reagent in 5.9.1.2.
5.9.2.3 Instruments and apparatuses
Atomic fluorometer: equipped with high-strength mercury hollow cathode lamp
and dual-pump autosampler.
5.9.2.4 Analysis steps
5.9.2.4.1 Drawing of the working curve
Successively take 0.00 mL, 2.00 mL, 4.00 mL, 8.00 mL, and 16.00 mL of
mercury standard solutions; respectively put them into five 50 mL volumetric
flasks; add 5 mL of hydrochloric acid solution (1+1); use water to dilute to the
mark; shake well. Respectively take an appropriate amount on the autosampler;
adjust the instrument to the best working condition; use hydrochloric acid
solution (5+95) as the carrier current; use stannous sulfate hydrochloric acid
solution as the reducing solution; measure the fluorescence value. Subtract the
fluorescence value of the blank test solution from the fluorescence value of
each mercury standard working solution; use the mercury mass as the abscissa
and the fluorescence value as the ordinate, to draw the working curve.
5.9.2.4.2 Determination of samples
Weigh about 1 g of sample for superior products, about 0.5 g of sample for first-
class products, accurate to 0.001 g; place in 100 mL beaker; add water to
dissolve; completely transfer to a 50 mL volumetric flask; add 5 mL of
hydrochloric acid solution (1+1); use water to dilute to the mark; shake well.
Prepare the blank test solution at the same time. Operate the following
according to 5.9.2.4.1; measure its fluorescence value.
5.9.2.5 Result calculation
5.11.3.2 Electrothermal constant-temperature drying oven: the controlling
temperature is 105 °C ± 2 °C.
5.11.4 Analysis steps
Weigh about 20 g of sample to the nearest 0.01 g; place it in a 500 mL beaker.
Use 300 mL of water to dissolve; use a glass mortar of constant quality at
105 °C ~ 110 °C to filter; use water to wash until there is no sulfate in the filtrate
(use barium chloride solution to check); mix well; dry to constant mass at 105 °C
~ 110 °C.
5.11.5 Result calculation
The content of water insoluble matter is calculated by mass fraction w8; the
value is expressed in %; it is calculated according to Formula (8):
Where:
m1 -- the value of the mass of glass mortar, in grams (g);
m2 -- the value of the mass of glass mortar and insoluble matter, in grams (g);
m -- the value of the mass of the sample, in grams (g).
Take the arithmetic mean of the parallel determination results as the
determination result; the absolute difference between the two parallel results
shall not be larger than 0.002%.
5.12 Determination of chloride content
5.12.1 Method summary
Add water; then, heat and boil the sample; after cooling, filter the test solution
in a 100 mL volumetric flask; after washing the funnel and insoluble matter, use
water to set the volume; transfer an appropriate amount of filtrate to the
colorimetric tube; add silver nitrate solution to make it silver chloride turbid liquid;
compare with standard turbid solution.
5.12.2 Reagents
5.12.2.1 Nitric acid solution: 1+4.
5.12.2.2 Silver nitrate solution: 0.1 mol/L.
4 -- the upper end of the glass tube;
5 -- glass cap.
Figure 1 -- Arsenic measuring device
5.13.4 Analysis steps
Weigh 1.00 g ± 0.01 g of sample; add water to dissolve; then, transfer to a 100
mL volumetric flask; dilute to the mark, shake well; then, transfer 10 mL of
superior product, 5 mL of first-class product and place in a conical flask or a
wide-mouth bottle. Add 75 mL of water; add 5 mL of hydrochloric acid, 1 g of
potassium iodide solution, 0.2 mL of stannous chloride solution; shake well;
place at room temperature for 10 min. Then, add 2.5 g of arsenic-free metal
zinc; immediately plug the arsenic measuring tube that is pre-loaded with lead
acetate cotton and mercury bromide test paper; place it in a dark place at about
25 °C for 1 h. Remove the mercury bromide test paper; the color of the arsenic
spots shall not be deeper than the standard.
Respectively pipette 1 mL and 2.5 mL of arsenic standard solutions;
respectively put them in the conical flasks or the wide-mouth bottles; add water
to 75 mL; starting from "add 5 mL of hydrochloric acid...", perform the same
treatment as the sample.
The arsenic spots that are obtained from the superior sample shall not be
deeper than the arsenic spots that are produced by 1 mL of arsenic standard
solution; the arsenic spots that are obtained from the first-class sample shall
not be deeper than the arsenic spots that are produced by 2.5 mL of arsenic
standard solution.
5.14 Determination of pH value
5.14.1 Reagents
5.14.1.1 Carbon dioxide-free water.
5.14.1.2 Ethanol solution: 95% neutral solution.
5.14.2 Instruments
5.14.2.1 Acidity meter: the accuracy is 0.02 pH unit.
5.14.2.2 Magnetic stirrer and stir bar.
5.14.3 Analysis steps
Weigh 1.00 g ± 0.01 g of sample; place it in a 100 mL beaker; add 5 mL of
ethanol to moisten; then, add 100 mL of carbon dioxide-free water; stir to
6.5 Use GB/T 8170 numerical rounding rules and limit values to represent and
determine whether the inspection results meet the standards.
7 Marking, labeling
7.1 There shall be a firm and clear mark on the refined cobaltous sulfates
packaging, including: the name of the manufacturer, the factory address, the
product name, the grade, the net content, the batch number or the date of
production, the serial number of this Standard and the sign of "fear of rain" that
is specified in GB/T 191-2008.
7.2 Each batch of the delivered refined cobaltous sulfates products shall be
accompanied by a quality certificate. The contents include: the name of the
manufacturer, the factory address, the product name, the grade, the net content,
the batch number or the date of production and the serial number of this
Standard.
8 Packaging, transportation, storage
8.1 The refined cobaltous sulfates are packed in plastic woven bags: the inner
packaging is a polyethylene plastic film bag; the inner bag is artificially pierced
with vinylon rope or other equivalent quality rope, or sealed in other ways
equivalent to it; the outer packaging is a plastic woven bag; the outer bag is
tightly sealed with vinylon rope or other thread of equivalent quality. Or align the
inner and outer bag mouths; fold the seams; secure the seams with vinylon
rope or other equivalent threads. When users have special requirements for
packaging, they can be negotiated. The net content of each bag is 25 kg.
8.2 The refined cobaltous sulfates shall be covered during transportation to
prevent sun, rain and moisture. They must not be transported with poisonous
and harmful materials.
8.3 The refined cobaltous sulfates shall be stored in a dry warehouse to prevent
rain, moisture, and sunlight. They must not be stored with poisonous and
harmful materials.
8.4 Under the packaging, transportation and storage conditions that are
stipulated in this Standard, the refined cobaltous sulfates have a shelf life of not
less than 2 years from the date of production.
......
 
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.