GB/T 26524-2011 English PDF (GBT26524-2011)
GB/T 26524-2011 English PDF (GBT26524-2011)
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GB/T 26524-2011: Refined nickel sulfates
GB/T 26524-2011
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.50
G 12
Refined Nickel Sulfates
精制硫酸镍
ISSUED ON: MAY 12, 2011
IMPLEMENTED ON: DECEMBER 1, 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 Classification ... 5
5 Requirements ... 5
6 Test Method ... 6
7 Inspection Rules ... 35
8 Marking and Labeling ... 36
9 Packaging, Transportation and Storage ... 36
Appendix A (informative) Method of Processing Mercury-containing Waste
Liquid ... 38
Refined Nickel Sulfates
1 Scope
This Standard specifies the classification, requirements, test method, inspection rules,
marking, labeling, packaging, transportation and storage of refined nickel sulfates.
This Standard is applicable to refined nickel sulfates that are mainly used for pre-plated
nickel, nickel-plating, nickel-plated iron alloy, nickel-cobalt-plated alloy, zinc-plated
nickel-iron alloy, electroformed nickel and electroless nickel plating, etc.
2 Normative References
The following documents are indispensable to the application of this document. In
terms of references with a specified date, only versions with a specified date are
applicable to this document. In terms of references without a specified date, the latest
version (including all the modifications) is applicable 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 and Expression and
Judgement of Limiting Values
HG/T 3696.1 Inorganic Chemicals for Industrial Use - Preparations of Standard and
Reagent Solutions for Chemical Analysis - Part 1: Preparations of Standard
Volumetric Solutions
HG/T 3696.2 Inorganic Chemicals for Industrial Use - Preparations of Standard and
Reagent Solutions for Chemical Analysis - Part 2: Preparations of Standard
Solutions for Impurity
GB/T 3696.3 Inorganic Chemicals for Industrial Use - Preparations of Standard and
Reagent Solutions for Chemical Analysis - Part 3: Preparations of Reagent
Solutions
accordance with the stipulations of HG/T 3696.1, HG/T 3696.2 and HG/T 3696.3.
6.3 Appearance Inspection
Under natural light, visually determine the appearance.
6.4 Determination of Nickel Content
6.4.1 Weight method (arbitration method)
6.4.1.1 Method summary
In ammonia solution, add tartaric acid and impurities (iron and aluminum, etc.) to form
a soluble complex, so as to eliminate the interference. Use dimethylglyoxime and
nickel to generate red dimethylglyoxime nickel precipitation. Filter it, rinse it, dry and
weigh it. Thus, calculate the nickel content.
6.4.1.2 Reagents
6.4.1.2.1 Ethanol solution: 1 + 4.
6.4.1.2.2 Hydrochloric acid solution: 1 + 1.
6.4.1.2.3 Ammonia solution: 1 + 1.
6.4.1.2.4 Ammonium chloride solution: 200 g/L.
6.4.1.2.5 Tartaric acid solution: 200 g/L.
6.4.1.2.6 Dimethylglyoxime ethanol solution: 10 g/L.
6.4.1.3 Instrument
Sintered-glass filter crucible: 5 μm ~ 15 μm.
6.4.1.4 Analytical procedures
Weigh-take around 2 g of sample, accurate to 0.0002 g. Place it in a 250 mL beaker.
Add 1 mL of hydrochloric acid solution and 50 mL of water; heat it up, till the sample
dissolves. Then, cool it down to room temperature. Completely transfer it into a 100
mL volumetric flask; use water to dilute to the scale; shake it well.
Use a transfer pipette to transfer-take 10 mL of test solution, place it in a 400 mL beaker.
Then, add 150 mL of water, 5 mL of ammonium chloride solution and 5 mL of tartaric
acid solution. Cover it with a watch glass; heat it up, till it boils. When it cools down to
70 °C ~ 80 °C, keep stirring it, slowly add 30 mL of dimethylglyoxime solution; dropwise
add ammonia solution to adjust the pH of the solution to 8 ~ 9 (check with precision
pH test paper). Then, add another 1 mL ~ 2 mL. At 70 °C ~ 80 °C, preserve the heat
6.4.2.2.5 Potassium sodium tartrate solution: 150 g/L.
6.4.2.2.6 Sodium thiosulfate solution: 500 g/L.
6.4.2.2.7 Ethylene Diamine Tetra-acetic Acid (EDTA) standard titration solution: c
(EDTA) 0.02 mol/L.
6.4.2.2.8 Ammonium purpurate indicator: mix 1 g of ammonium purpurate with 100 g
of sodium chloride, which is dried at 105 °C ~ 110 °C for 2 h, in a mortar; mix and grind
it.
6.4.2.3 Analytical procedures
6.4.2.3.1 Preparation of test solutions
Weigh-take around 1 g of sample, accurate to 0.0002 g. Place it in a 250 mL beaker.
Add 50 mL of water and 20 mL of hydrochloric acid solution; heat it up and dissolve it.
Cool it down to room temperature, then, completely transfer it to a 250 mL volumetric
flask. Use water to dilute to the scale; shake it well.
6.4.2.3.2 Determination
Transfer 25 mL of test solution, place it in a 500 mL conical flask. Add 1 g ~ 2 g of
ammonium fluoride, 10 mL of potassium sodium tartrate solution, 15 mL of sodium
thiosulfate solution and 0.1 g of ammonium purpurate indicator. After shaking it well,
dropwise add ammonia solution, until the solution manifests yellow. Use Ethylene
Diamine Tetra-acetic Acid (EDTA) standard titration solution to titrate it, until the
solution becomes orange-yellow, then, dropwise add ammonia solution, until the
solution turns yellow. Then, continue to use the Ethylene Diamine Tetra-acetic Acid
(EDTA) standard titration solution for titration. After the color of the solution becomes
darker, dropwise add ammonia solution, until the solution becomes yellow. Then, use
the Ethylene Diamine Tetra-acetic Acid (EDTA) standard titration solution for titration.
Repeat it, until the solution manifests purple red.
6.4.2.4 Result calculation
Nickel content, counted by the mass fraction w1 of nickel (Ni), shall be expressed in
(%) and calculated in accordance with Formula (2):
Where,
c---accurate value of the concentration of Ethylene Diamine Tetra-acetic Acid (EDTA)
standard titration solution, expressed in (mol/L);
Accurately transfer-take 0 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL and 10.00 mL
cobalt standard solutions. Respectively place them in six 250 mL beakers, which
already hold 1.2 mL of nickel standard solution; add water to 40 mL. Add 10 mL of
sodium acetate solution, heat it up, till it boils. Then, add 10 mL of 1-nitroso-2-naphthol-
3,6-disulfonate sodium solution; boil for 2 min ~ 3 min. Add 10 mL of nitric acid solution,
then, slightly boil it for 2 min; cool it down. Transfer it into a 100 mL volumetric flask;
use water to dilute to the scale, shake it well. Use the spectrophotometer, at a
wavelength of 550 nm, use 1 cm absorption cell; use water as a reference to measure
its absorbance. Take cobalt mass (mg) as the x-coordinate; take the corresponding
absorbance as the y-coordinate; draw a working curve.
6.5.1.4.2 Preparation of test solution and blank test solution
Weigh-take around 1 g of sample, accurate to 0.001 g; place it in a 250 mL beaker.
Add 2 mL of hydrochloric acid solution and 50 mL of water. Heat it up, till the sample ...
Get QUOTATION in 1-minute: Click GB/T 26524-2011
Historical versions: GB/T 26524-2011
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GB/T 26524-2011: Refined nickel sulfates
GB/T 26524-2011
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.060.50
G 12
Refined Nickel Sulfates
精制硫酸镍
ISSUED ON: MAY 12, 2011
IMPLEMENTED ON: DECEMBER 1, 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 Classification ... 5
5 Requirements ... 5
6 Test Method ... 6
7 Inspection Rules ... 35
8 Marking and Labeling ... 36
9 Packaging, Transportation and Storage ... 36
Appendix A (informative) Method of Processing Mercury-containing Waste
Liquid ... 38
Refined Nickel Sulfates
1 Scope
This Standard specifies the classification, requirements, test method, inspection rules,
marking, labeling, packaging, transportation and storage of refined nickel sulfates.
This Standard is applicable to refined nickel sulfates that are mainly used for pre-plated
nickel, nickel-plating, nickel-plated iron alloy, nickel-cobalt-plated alloy, zinc-plated
nickel-iron alloy, electroformed nickel and electroless nickel plating, etc.
2 Normative References
The following documents are indispensable to the application of this document. In
terms of references with a specified date, only versions with a specified date are
applicable to this document. In terms of references without a specified date, the latest
version (including all the modifications) is applicable 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 and Expression and
Judgement of Limiting Values
HG/T 3696.1 Inorganic Chemicals for Industrial Use - Preparations of Standard and
Reagent Solutions for Chemical Analysis - Part 1: Preparations of Standard
Volumetric Solutions
HG/T 3696.2 Inorganic Chemicals for Industrial Use - Preparations of Standard and
Reagent Solutions for Chemical Analysis - Part 2: Preparations of Standard
Solutions for Impurity
GB/T 3696.3 Inorganic Chemicals for Industrial Use - Preparations of Standard and
Reagent Solutions for Chemical Analysis - Part 3: Preparations of Reagent
Solutions
accordance with the stipulations of HG/T 3696.1, HG/T 3696.2 and HG/T 3696.3.
6.3 Appearance Inspection
Under natural light, visually determine the appearance.
6.4 Determination of Nickel Content
6.4.1 Weight method (arbitration method)
6.4.1.1 Method summary
In ammonia solution, add tartaric acid and impurities (iron and aluminum, etc.) to form
a soluble complex, so as to eliminate the interference. Use dimethylglyoxime and
nickel to generate red dimethylglyoxime nickel precipitation. Filter it, rinse it, dry and
weigh it. Thus, calculate the nickel content.
6.4.1.2 Reagents
6.4.1.2.1 Ethanol solution: 1 + 4.
6.4.1.2.2 Hydrochloric acid solution: 1 + 1.
6.4.1.2.3 Ammonia solution: 1 + 1.
6.4.1.2.4 Ammonium chloride solution: 200 g/L.
6.4.1.2.5 Tartaric acid solution: 200 g/L.
6.4.1.2.6 Dimethylglyoxime ethanol solution: 10 g/L.
6.4.1.3 Instrument
Sintered-glass filter crucible: 5 μm ~ 15 μm.
6.4.1.4 Analytical procedures
Weigh-take around 2 g of sample, accurate to 0.0002 g. Place it in a 250 mL beaker.
Add 1 mL of hydrochloric acid solution and 50 mL of water; heat it up, till the sample
dissolves. Then, cool it down to room temperature. Completely transfer it into a 100
mL volumetric flask; use water to dilute to the scale; shake it well.
Use a transfer pipette to transfer-take 10 mL of test solution, place it in a 400 mL beaker.
Then, add 150 mL of water, 5 mL of ammonium chloride solution and 5 mL of tartaric
acid solution. Cover it with a watch glass; heat it up, till it boils. When it cools down to
70 °C ~ 80 °C, keep stirring it, slowly add 30 mL of dimethylglyoxime solution; dropwise
add ammonia solution to adjust the pH of the solution to 8 ~ 9 (check with precision
pH test paper). Then, add another 1 mL ~ 2 mL. At 70 °C ~ 80 °C, preserve the heat
6.4.2.2.5 Potassium sodium tartrate solution: 150 g/L.
6.4.2.2.6 Sodium thiosulfate solution: 500 g/L.
6.4.2.2.7 Ethylene Diamine Tetra-acetic Acid (EDTA) standard titration solution: c
(EDTA) 0.02 mol/L.
6.4.2.2.8 Ammonium purpurate indicator: mix 1 g of ammonium purpurate with 100 g
of sodium chloride, which is dried at 105 °C ~ 110 °C for 2 h, in a mortar; mix and grind
it.
6.4.2.3 Analytical procedures
6.4.2.3.1 Preparation of test solutions
Weigh-take around 1 g of sample, accurate to 0.0002 g. Place it in a 250 mL beaker.
Add 50 mL of water and 20 mL of hydrochloric acid solution; heat it up and dissolve it.
Cool it down to room temperature, then, completely transfer it to a 250 mL volumetric
flask. Use water to dilute to the scale; shake it well.
6.4.2.3.2 Determination
Transfer 25 mL of test solution, place it in a 500 mL conical flask. Add 1 g ~ 2 g of
ammonium fluoride, 10 mL of potassium sodium tartrate solution, 15 mL of sodium
thiosulfate solution and 0.1 g of ammonium purpurate indicator. After shaking it well,
dropwise add ammonia solution, until the solution manifests yellow. Use Ethylene
Diamine Tetra-acetic Acid (EDTA) standard titration solution to titrate it, until the
solution becomes orange-yellow, then, dropwise add ammonia solution, until the
solution turns yellow. Then, continue to use the Ethylene Diamine Tetra-acetic Acid
(EDTA) standard titration solution for titration. After the color of the solution becomes
darker, dropwise add ammonia solution, until the solution becomes yellow. Then, use
the Ethylene Diamine Tetra-acetic Acid (EDTA) standard titration solution for titration.
Repeat it, until the solution manifests purple red.
6.4.2.4 Result calculation
Nickel content, counted by the mass fraction w1 of nickel (Ni), shall be expressed in
(%) and calculated in accordance with Formula (2):
Where,
c---accurate value of the concentration of Ethylene Diamine Tetra-acetic Acid (EDTA)
standard titration solution, expressed in (mol/L);
Accurately transfer-take 0 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL and 10.00 mL
cobalt standard solutions. Respectively place them in six 250 mL beakers, which
already hold 1.2 mL of nickel standard solution; add water to 40 mL. Add 10 mL of
sodium acetate solution, heat it up, till it boils. Then, add 10 mL of 1-nitroso-2-naphthol-
3,6-disulfonate sodium solution; boil for 2 min ~ 3 min. Add 10 mL of nitric acid solution,
then, slightly boil it for 2 min; cool it down. Transfer it into a 100 mL volumetric flask;
use water to dilute to the scale, shake it well. Use the spectrophotometer, at a
wavelength of 550 nm, use 1 cm absorption cell; use water as a reference to measure
its absorbance. Take cobalt mass (mg) as the x-coordinate; take the corresponding
absorbance as the y-coordinate; draw a working curve.
6.5.1.4.2 Preparation of test solution and blank test solution
Weigh-take around 1 g of sample, accurate to 0.001 g; place it in a 250 mL beaker.
Add 2 mL of hydrochloric acid solution and 50 mL of water. Heat it up, till the sample ...