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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

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.
GB/T 26524-2011
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 71.060.50
G 12
Refined Nickel Sulfates
???????????????
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 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 ??m ~ 15 ??m.
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 (LaCl3???6H2O); 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 manuf...

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