GB/T 26524-2023 (GB/T26524-2023, GBT 26524-2023, GBT26524-2023) & related versions
GB/T 26524-2023: PDF in English (GBT 26524-2023)
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 & 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
dissolves. Then, cool it down to room temperature. Transfer it to a 100 mL volumetric
flask; use water to dilute to the scale; shake it well.
Meanwhile, prepare blank test solution. Except that no sample is added, the amount
of added reagent is exactly the same as the amount in the preparation of the test
solution. Process it at the same time and in the same way as the sample.
6.5.1.4.3 Determination
Use a transfer pipette to transfer-take 10 mL of Type-I test solution, 2 mL of Type-II test
solution, and a corresponding amount of blank test solution. Respectively place them
in a 250 mL beaker. The following operation shall comply with the description from “add
water to 40 mL……” to “……, measure its absorbance.” in 6.5.1.4.1.
In accordance with the working curve, find out the mass of cobalt in the test solution
and the blank test solution.
6.5.1.5 Result calculation
Cobalt content, counted by the mass fraction w2 of cobalt (Co), shall be expressed in
(%) and calculated in accordance with Formula (3):
Where,
m1---numerical value of the mass of cobalt in the test solution obtained from the
working curve, expressed in (mg);
m0---numerical value of the mass of cobalt in the blank test solution obtained from the
m---numerical value of the mass of sample weighed in 6.6.4.1, expressed in (g).
Take the arithmetic mean value of the parallel determination results as the
determination result. The absolute difference between two parallel determination
results shall be not more than 0.0003%.
6.8 Determination of Sodium Content
6.8.1 Method summary
Use water to dissolve the sample. On the atomic absorption spectrophotometer, adopt
the standard addition method, at a wavelength of 689.0 nm, use air-acetylene flame
for determination.
6.8.2 Reagents and materials
Sodium standard solution: 1 mL of solution contains 0.01 mg of sodium (Na).
Preparation: use a transfer pipette to transfer-take 1.0 mL of sodium standard solution
(prepared in accordance with HG/T 3696.2); place it in a100 mL volumetric flask. Use
water to dilute it to the scale; shake it well. This solution shall be prepared before usage.
6.8.3 Instrument
Atomic absorption spectrophotometer: equipped with sodium hollow cathode lamp.
6.8.4 Analytical procedures
Respectively transfer-take 1 mL of test solution A (6.6.4.1); place in four 100 mL
volumetric flask. Respectively add 0 mL, 2.00 mL, 4.00 mL and 6.00 mL of sodium
standard solution; use water to dilute to the scale; shake it well. On the atomic
absorption spectrophotometer, use sodium hollow cathode lamp as the light source;
use air-acetylene flame, at a wavelength of 589.0 nm, measure the absorbance of the
above-mentioned solutions. Take the mass of sodium in the sodium standard solution
as the x-coordinate; take the corresponding absorbance as the y-coordinate; draw a
working curve. Extend the curve in reverse and intersect with the x-coordinate, the
intersection point is the mass of sodium in the test solution being determined.
6.8.5 Result calculation
Sodium content, counted by the mass fraction w5 of sodium (Na), shall be expressed
in (%) and calculated in accordance with Formula (8):
Where,
emission spectrometer to determine the lead content in the sample.
6.9.2.2 Reagents
6.9.2.2.1 Hydrochloric acid.
6.9.2.2.2 30% hydrogen peroxide.
6.9.2.2.3 Argon: purity shall be more than 99.9%.
6.9.2.3 Instruments
6.9.2.3.1 Electromagnetic stirrer: equipped with heating device.
6.9.2.3.2 Inductively coupled plasma atomic emission spectrometer.
Stability of the instrument: the short-term stability (RSD) is not more than 2.0%; the
long-term stability (RSD) is not more than 4.0%.
Detection limit of the instrument: the detection limit of the representative element is not
more than 0.005 mg/L.
Calibration working curve: linear correlation coefficient of regression curve, linear
correlation coefficient of each element R ≥ 0.99.
6.9.2.4 Analytical procedures
6.9.2.4.1 Preparation of test solution
Weigh-take 2 g of sample, accurate to 0.001 g; place it in a 250 mL beaker. Add 50 mL
of water, 50 mL of hydrochloric acid and 16 mL of 30% hydrogen peroxide. Place the
electromagnetic stir bar into the beaker; cover it with a watch glass. Place it on the
electromagnetic stirrer; turn on the magnetic stirring and heat up the solution to 60 °C;
stir it, until the sample dissolves or the amount of the insoluble matter remains
unchanged. Cool down the solution to room temperature, then, transfer the solution
and the insoluble matter to a 250 mL volumetric flask; use water to dilute to the scale;
shake it well. Dry-filter the solution; discard 20 mL of the initial filtrate. The retained
filtrate is the test solution for determination.
6.9.2.4.2 Drawing of working curve
In accordance with the requirements in Table 6, respectively transfer-take lead
standard solution (6.9.1.2.2); place into four 100 mL volumetric flasks. Then,
respectively use a transfer pipette to add 25 mL of test solution; use water to dilute to
the scale; shake it well.
Where,
---numerical value of the mass concentration of zinc in the test solution obtained from
the working curve, expressed in (mg/mL);
m---numerical value of the mass of sample weighed in 6.6.4.1, expressed in (g).
Take the arithmetic mean value of the parallel determination results as the
determination result. The absolute difference between two parallel determination
results shall be not more than 0.0003%.
6.11 Determination of Calcium Content
6.11.1 Method summary
Use water to dissolve the sample; add lanthanum salt to eliminate the influence of the
matrix. On the atomic absorption spectrophotometer, at a wavelength of 422.7 nm, use
air-acetylene flame to determine the calcium content.
6.11.2 Reagents and materials
6.11.2.1 Hydrochloric acid: 1 + 1.
6.11.2.2 Lanthanum chloride solution: 1 mL of solution contains 10 mg of lanthanum
(La).
Weigh-take 2.5 g of lanthanum chloride (LaCl36H2O); dissolve it in water; dilute to 100
mL.
6.11.2.3 Calcium standard solution: 1 mL of solution contains 0.05 mg of calcium (Ca).
Use a transfer pipette to transfer-take 5 mL of calcium standard solution (prepared in
accordance with HG/T 3696.2), place it in a 100 ml volumetric flask. Use water to dilute
to the scale; shake it well. This solution shall be prepared before usage.
6.11.3 Instrument
Atomic absorption spectrophotometer: equipped with calcium hollow cathode lamp.
6.11.4 Analytical procedures
In four 100 mL volumetric flasks, use a transfer pipette to respectively add 0 mL, 1.00
mL, 2.00 mL and 3.00 mL of calcium standard solution. Respectively add 20 mL of test
solution A (6.6.4.1), 2 mL of hydrochloride acid solution and 2 mL of lanthanum chloride
solution; use water to dilute to the scale; shake it well. On the atomic absorption
spectrophotometer, use calcium hollow cathode lamp as the light source, use air-
acetylene flame, at a wavelength of 422.7 nm, determine the absorbance of the above-
mentioned solutions. Take the mass of calcium as the x-coordinate; take the
6.15.1.2 Reagents
6.15.1.2.1 Hydrochloric acid solution: 1 + 99.
6.15.1.2.2 Stannous chloride hydrochloric acid solution: 100 g/L.
Weigh 25 g of stannous chloride, dissolve it in 50 mL of hot concentrated hydrochloric
acid. After cooling it down, transfer it to a 250 mL volumetric flask. Use water to dilute
to the scale; shake it well.
6.15.1.2.3 Mercury standard solution stock solution: 1 mL of solution contains 0.1 mg
of mercury (Hg).
Use a transfer pipette to transfer-take 10 mL of mercury standard solution (prepared in
accordance with HG/T 3696.2), place it in a 100 mL volumetric flask. Use water to
dilute to the scale; shake it well.
6.15.1.2.4 Mercury standard solution: 1 mL of solution contains 0.001 mg of mercury
(Hg).
Use a transfer pipette to transfer-take 1 mL of mercury standard stock solution, place
it in a 100 mL volumetric flask; dilute to the scale; shake it well. This solution shall be
prepared before usage.
6.15.1.3 Instruments
6.15.1.3.1 Atomic absorption spectrophotometer: equipped with low-pressure mercury
lamp or hollow cathode lamp.
6.15.1.3.2 Quick response recorder.
6.15.1.4 Analytical procedures
6.15.1.4.1 Drawing of working curve
Take four 100 mL volumetric flasks. Use a transfer pipette to respectively add 0 mL,
2.00 mL, 4.00 mL and 6.00 mL of mercury standard solution. Use water to dilute to the
scale; shake it well. Respectively add 1 mL of stannous chloride hydrochloric acid
solution; immediately and tightly close the reduction bottle. Inlet the carrier gas. From
the highest point displayed by the instrument reading, determine its absorption value.
Successively suck the working curve solution into the hydride generator (or equivalent
device), at a wavelength of 253.7 nm, use water for zero adjustment; determine its
absorbance. Subtract the absorbance of the reagent’s blank solution from the
absorbance of different working curve solutions. Take the mass (mg) of mercury in
different solutions as the x-coordinate; take the corresponding absorbance as the y-
coordinate; draw a working curve.
(Cr).
Preparation: use a transfer pipette to transfer-take 1 mL of chromium standard solution
(prepared in accordance with HG/T 3969.2), place it in a 100 mL volumetric flask. Use
water to dilute to the scale; after shaking it well, transfer-take 20 mL and place into a
100 mL volumetric flask. Use water to dilute to the scale; shake it well. This solution
shall be prepared before usage.
6.16.3 Instruments
6.16.3.1 Conical separating funnel: 125 mL.
6.16.3.2 Spectrophotometer: equipped with 1 cm absorption cell.
6.16.4 Analytical procedures
6.16.4.1 Determination of test solution
Weigh-take around 0.5 g of sample, accurate to 0.01 g. Place it in a 250 mL beaker;
add 40 mL of water to dissolve it. Dropwise add potassium permanganate solution,
until the solution maintains purple-red; carefully boil it for 3 min. After cooling it down,
add 2 mL of urea solution, then, evenly stir it. Dropwise add sodium nitrite solution,
until the purple color of the potassium permanganate solution just fades. Continue to
heat it up and boil it for 1 min ~ 2 min. After cooling it down, add water to around 30
mL. Completely transfer the solution to a separating funnel; add 0.5 mL of sulfuric acid
solution, 0.5 mL of phosphoric acid and 2.0 mL of diphenylcarbazide solution. Shake it
well, then, add 10 mL of isoamyl alcohol; shake it for 2 min. Use a 1 cm cuvette, at a
wavelength of 545 nm, determine the absorbance of the organic phase.
6.16.4.2 Determination of blank test solution
Except that no sample is added, the amount of added reagent is exactly the same as
the amount in the preparation of the test solution. Process it at the same time and in
the same way as the sample.
6.16.4.3 Drawing of working curve
In a group of 125 mL separating funnels, add 0 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00
mL and 10.00 mL of chromium standard solution. Then, respectively add 0.5 mL of
sulfuric acid solution, 0.5 mL of phosphoric acid solution and 2.0 mL of
diphenylcarbazide solution. Add 50 mL of water. Shake it well, then, add 10 mL of
isoamyl alcohol; shake it for 2 min. Use a 1 cm cuvette, at a wavelength of 545 nm,
determine the absorbance of the organic phase. Take the mass (mg) of chromium as
the x-coordinate; take the corresponding absorbance as the y-coordinate; draw a
working curve. In accordance with the working curve, find out the mass (mg) of
chromium in the test solution and the blank test solution.
7.3 In accordance with the stipulations of GB/T 6678, determine the number of
sampling units. During the sampling, vertically insert the sampler, from the top of the
packaging bag, to 3/4 depth of the material layer for sampling. The sample taken from
each bag shall be not less than 50 g. Mix the sample taken; use the quartering method
to divide it into around 500 g. Pack in two dry and clean jars or plastic bags; seal them
and affix a label, indicating: the name of manufacturer, the name of product, category,
batch No., date of sampling and the name of the sampler. One jar (bag) shall be used
for inspection, the other jar (bag) shall kept for further reference. The storage time is
determined by the manufacturer in accordance with the actual situation.
7.4 In the inspection result, when there are indicators that do not meet the requirements
of this Standard, sampling shall be re-conducted from twice the amount of packaging
for re-inspection. Even if only one indicator in the re-inspection result does not meet
the requirements of this Standard, the entire batch of products shall be determined as
disqualified.
7.5 Adopt GB/T 8170 Rules of Rounding off for Numerical Values & Expression and
Judgement of Limiting Values to inspect whether the result complies with the Standard.
8 Marking and Labeling
8.1 On the packaging of refined nickel sulfates, there shall be a firm and clear mark,
which includes: the name and address of manufacturer, name of product, category, net
content, batch No. or date of production, serial No. of this Standard and the “keep away
from rain” marking specified in GB/T 191-2008.
8.2 Each batch of exit-factory refined nickel sulfates shall be attached with a quality
certificate, which includes: the name and address of manufacturer, name of product,
category, net content, batch No. or date of production, and serial No. of this Standard.
9 Packaging, Transportation and Storage
9.1 Refined nickel sulfates shall adopt double-layer packaging. The inner packaging
shall adopt polyethylene plastic film bag; the inner bag shall be artificially tied with
vinylon rope or other ropes with equivalent quality, or, be sealed by other equivalent
modes. The outer packaging shall adopt plastic woven bag; the outer bag shall be
firmly seamed with vinylon rope or other ropes with equivalent quality. Or, align the
inner and outer bag mouths, fold the seams; use vinylon rope or other ropes with
equivalent quality to secure the seams. The net content of each bag is 25 kg.
9.2 During the transportation process, refined nickel sulfates shall be covered, so as
to prevent the products from the sun, the rain and moisture.
9.3 Refined nickel sulfates shall be stored in a dry warehouse, so as to prevent the
......
| Standard ID | GB/T 26524-2023 (GB/T26524-2023) | | Description (Translated English) | Refined nickel sulfates | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | G12 | | Classification of International Standard | 71.060.50 | | Word Count Estimation | 18,140 | | Date of Issue | 2023-09-07 | | Date of Implementation | 2024-04-01 | | Older Standard (superseded by this standard) | GB/T 26524-2011 | | Drafting Organization | Jinchuan Group Nickel Salt Co., Ltd., GEM Co., Ltd., Quzhou Huayou Cobalt New Materials Co., Ltd., Fuan Qingmei Energy Materials Co., Ltd., Guangxi Yinyi New Materials Co., Ltd., Guangxi Zhongwei New Energy Technology Co., Ltd., CNOOC Tianjin Chemical Research Design Institute Co., Ltd., Guangdong Bangpu Recycling Technology Co., Ltd., Jiangxi Nuclear Industry New Materials Co., Ltd. | | Administrative Organization | National Chemical Standardization Technical Committee (SAC/TC 63) | | Proposing organization | China Petroleum and Chemical Industry Federation | | Issuing agency(ies) | State Administration for Market Regulation, National Standardization Administration |
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