Some standard content:
Chemical test standard of the Ministry of Chemical Industry of the People's Republic of China
HG 3-957-84
Replaces HG3--957-76
This reagent is emerald green crystals, which will weather slightly in dry air and will deliquesce immediately in humid air. Molecular formula: Ni(NO)2·6H2O
Molecular weight: 290.80 (according to the international atomic weight in 1979) 1 Technical requirements
Ni(NO,)2·6H,O content not less than:
Superior purity
Analytical purity, chemical purity
Maximum impurity content (indicators in percentage): 1.2
Water insoluble matter
Chloride (CI)
Sulfate (S),)
Ammonium salt (NH)
Sodium (Na)
Magnesium (Mg)
Potassium (K)
Calcium (Ca)
Iron (Fe)
Cobalt (Co)
Copper (Cu)
Zinc (Zn)
(Cd)
Lead (Pb)
Test method
The standard solution, impurity standard solution, preparation and product required for the determination shall be prepared in accordance with the provisions of GB601-77 "Preparation Method of Chemical Reagent Standard Solution", GJ3602--77 "Preparation Method of Chemical Reagent Impurity Standard Solution" and GB603-77 "Preparation Method of Chemical Reagent Preparation and Product".
Preparation:
Promulgated by the Ministry of Chemical Industry of the People's Republic of China on January 4, 1984 and implemented on May 1, 1984
HG 3-957-84
2.1Ni（N()3）2·6Hz Content determination: Weigh 0.5g sample and weigh to 0.0002g. Dissolve in 70ml water, add 10ml ammonia-ammonium chloride buffer solution A (pH 10) and 0.2g ammonium violaceum mixed indicator, shake well. Titrate with 0.05mol disodium ethylenediaminetetraacetic acid standard solution until the solution turns blue purple.
Ni(NO,)2·6H,()% content (X) is calculated according to the following formula: XV.CX0.2908 ×100
Where: V----Amount of disodium ethylenediaminetetraacetic acid standard solution, ml; (——Molar concentration of disodium ethylenediaminetetraacetic acid standard solution, mol; G--Sample weight·g;
0.2908---Number of grams of Ni(NO,)·6H per milligram molecule. 2.2 Impurity determination: The sample must be weighed to 0.01g. 2.2.1 Water insoluble matter: Weigh 25g sample, dissolve in 100ml water, heat to boiling, filter with constant weight No. 4 glass filter, wash the filter residue with hot water until the washing liquid is colorless, and dry at 105~～110C to constant weight. The weight of the filter residue shall not be greater than: superior grade pure, analytical pure,
chemical pure
2.50mg.
2.2.2 Chloride: Weigh 1g sample, dissolve in 20ml water (filter if necessary) and dilute to 25ml, add 2ml5N nitric acid and 1ml0.1N silver nitrate, shake well, let stand for 10min, and the turbidity shall not be greater than the standard. The standard is to take 25ml of nickel nitrate solution without chloride and the following amount of chloride impurity standard solution: superior grade pure, analytical pure,
chemical pure
dilute to 28ml, and let stand for 10min with the same volume of sample solution for turbidity comparison. -0.01mgCl;
·0.05mgCl.
Note: Preparation of nickel nitrate solution without chloride - weigh 5g sample, dissolve in 100ml water, add 10ml5N nitric acid and 5ml0.1N silver nitrate, dilute to 125ml, shake well, let stand for 12~18h, filter. 2.2.3 Sulfate: weigh 0.5g sample, add 10ml water and 10ml6N hydrochloric acid, evaporate to dryness, dissolve the residue in 10ml water (filter if necessary), add 5ml95% ethanol, 1ml3N hydrochloric acid, add 3ml25% barium chloride solution under continuous shaking, dilute to 25ml, shake well, let stand for 10min. The turbidity shall not be greater than the standard. The standard is to take 10ml of sulfate-free nickel nitrate solution and the following amount of sulfate impurity standard solution: superior grade, analytical pure
chemical pure
...0.025mgSO.;
...0. 050mgSO4.
Add 3ml95% ethanol, 0.6ml3N hydrochloric acid, add 2ml25% chlorine solution under continuous shaking, dilute to 25ml, shake well, and place it with the sample solution for 10min turbidity.
Note: Preparation of sulfate-free nickel nitrate solution: weigh 2.5g sample and dissolve it in 25ml hydrochloric acid. Evaporate it on a water bath, dissolve the residue in 20ml water, add 10ml95% ethanol, 2ml3N hydrochloric acid, add 5ml25% barium fluoride solution under continuous shaking, dilute to 50ml, shake well, place it for 12-18h, and filter.
2.2.4 Ammonium salt: Weigh 0.1g sample, dissolve in ammonia-free water, pour into branch distillation bottle, dilute to 70ml with ammonia-free water, add 20ml 10% ammonia-free sodium hydroxide solution, heat and distill out 50ml liquid, collect in a 100ml colorimetric tube filled with 50ml water. Add 2ml Nessler's reagent, shake the hook, the yellow color should not be darker than the standard. The standard is to take 0.05mgNH. impurity standard solution and dilute to 70ml, and treat it in the same way as the same volume of sample solution. 2.2.5 Sodium: atomic absorption spectrophotometry. Instrument conditions
Light source: sodium hollow cathode lamp;
Wavelength: 589.0nm;
Flame: acetylene-air.
HG 3---957-84
Determination method: weigh 1g sample, dissolve in water, dilute to 100ml, take 20ml, a total of four portions. Determine according to the provisions of Chapter 2, Article 2, Item (2) of HG31013-76 "General Rules for Atomic Absorption Spectrophotometry of Chemical Reagents". 2.2.6 Magnesium: Atomic absorption spectrophotometry. Instrument conditions
Light source: magnesium hollow cathode lamp;
Wavelength: 285.2nm;
Flame: acetylene-air.
Determination method: weigh 1g sample, dissolve in water, dilute to 100ml, take 10ml, a total of four portions. Determine according to the provisions of Chapter 2, Article 2, Item (2) of HG3-1013-76.
2.2.7 Potassium: Atomic absorption spectrophotometry. Instrument conditions
Light source: potassium hollow cathode lamp;
Wavelength: 766.4nm;
Flame: acetylene-air.
Determination method: Weigh 5g sample, dissolve in water, dilute to 100ml, take 8ml, a total of four portions. Determine according to the provisions of Article 2, Section 2, Chapter 2 of HG3-1013-76 (2).
2.2.8 Calcium: atomic absorption spectrophotometry. Instrument conditions
Light source: calcium hollow cathode lamp;
Wavelength: 422.7nm;
Flame: acetylene-air.
Determination method: Weigh 10g sample, dissolve in water, dilute to 100ml, take 20ml, a total of four portions. Determine according to the provisions of Article 2, Section 2, Chapter 2 of HG3-1013-76 (2).
2.2.9 Iron: Weigh 1g sample, dissolve in 60ml water, add 0.5ml 5N nitric acid, boil for 2min, cool, dilute to 85ml, add 1ml hydrochloric acid, 5ml 25% ammonium thiocyanate solution, shake well, extract with 10ml isoamyl alcohol, the red color of the organic layer shall not be darker than the standard. The standard is to take 25ml iron-free nickel nitrate solution and the following amount of iron impurity standard solution: superior grade, analytical grade...
chemical pure···
dilute to 60ml and treat in the same way as the same volume of sample solution. 0.005mgFe:
-0.01mgFe.
Note: Preparation of nickel nitrate solution without iron: weigh 3g sample, dissolve in 60ml water, add 1.5ml 5N nitric acid and 3g ammonium chloride, boil for 2min. Add 10% ammonia water until the solution is alkaline, filter, neutralize the filtrate with 4N sulfuric acid to pH 4-5, and dilute to 75ml. 2.2.10 Cobalt: atomic absorption spectrophotometry. Instrument conditions
Light source: cobalt hollow cathode lamp:
Wavelength: 240.7nm;
Flame: acetylene-air.
Determination method: weigh 10g sample, dissolve in water, dilute to 100ml, take 20ml (4ml for chemically pure), a total of four portions. Determine according to the provisions of Article 2, Section (2) of Chapter 2 of HG31013-76. 2.2.11 Copper:
2.2.12 Lead:
Anodic stripping voltammetry.
Instrument:
HG 3-957--84
According to the provisions of 4 in GB391483 "Chemical reagents
! General rules for anodic stripping voltammetry". Chemical reagents:
According to the provisions of 5 in GB3914--83.
Determination conditions:
Pre-electrolysis potential: -0.9V;
Scanning potential range: -0.9V～-0.1V; Dissolution peak potential: copper: -0.2V;
Lead: -0.5V.
Determination process: Weigh 0.5g sample, dissolve in 50ml0.1N hydrochloric acid, take 5ml (1ml for chemically pure) and place it in the electrolytic cell, add 0.1N hydrochloric acid supporting electrolyte solution to 40ml. According to the provisions of 6.1 of GB3914-83: Start with "nitrogen is passed through for a certain period of time". If necessary, correct the blank.
Calculation: According to the provisions of 6.2 of GB3914-83. 2.2.13 Zinc: Atomic absorption spectrophotometry. Instrument conditions
Light source: zinc hollow cathode lamp,
Wavelength: 213.9nm;
Flame: acetylene-air.
Determination method: Weigh 15g sample, dissolve in water, dilute to 100ml, take 10ml (chemically pure 4ml), a total of four portions. Determine according to the provisions of HG3-1013-76 Chapter 2, Article 2, Item (2). 2.2.14 Cadmium: Atomic absorption spectrophotometry. Instrument conditions
Light source: cadmium hollow cathode lamp;
Wavelength: 228.8nm;
Flame: acetylene-air.
Determination method: Weigh 10g sample, dissolve in water, dilute to 100ml. Take 20ml, four portions. Determine according to the provisions of Article 2, Section 2, Chapter 2, HG3-1013-76.
3 Inspection rules
Sampling and acceptance shall be carried out in accordance with the provisions of GB619--77 "Chemical Reagent Sampling and Acceptance Rules". 4 Packaging and markingbzxz.net
4.1 Packaging
According to HG3-119---83 "Chemical Reagents
Inner packaging form: G-3.Gz-3;
Outer packaging form: W-1;
Packing unit: Class 4.
4.2 Marking
According to the provisions of HG3~119-83.
Packaging and Marking》.
Additional Notes:
HG3—957-84
This standard was proposed by Tianjin Chemical Industry Bureau and managed by Beijing Chemical Reagent General Factory. This standard was drafted by Tianjin Chemical Reagent Factory No. 3. The main drafters of this standard are Chen Yuwen and Yang Hongjian. 885
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.