GB/T 5211.11-1986 Determination of water-soluble sulfate, chloride and nitrate of pigments

This standard specifies the general test method for the determination of soluble sulfate, chloride and nitrate in water of pigment samples. This standard adopts the international standard ISO 787/13-1973 "General test methods for pigments and extenders - Part 13: Determination of water-soluble sulfate, chloride and nitrate". GB/T 5211.11-1986 Determination of water-soluble sulfate, chloride and nitrate in pigments GB/T5211.11-1986 Standard download decompression password: www.bzxz.net

UDC667.622:543.06
National Standard of the People's Republic of China
GB 5211.11—86
Determination of water-soluble sulfates chlorides and
nitrates of pigments
Published on August 26, 1986
National Bureau of Standards
Implemented on August 1, 1987
National Standard of the People's Republic of China
Determination of water-soluble sulfates chlorides and
nitrates of pigments Pigments
UDC667.622：543
GB5211.11—86
This standard specifies the general test method for determining the soluble sulfate, chloride and nitrate in water of pigment samples. This standard adopts the international standard ISO787/13-1973 "General test methods for pigments and extenders - Part 13: Determination of water-soluble sulfate, chloride and nitrate". Note: When this general method is applicable to a specified pigment or extender, it is only necessary to include the clauses of this standard in the product standard of the pigment or extender, and indicate the changes required due to the characteristics of the product. Only when this general method is not applicable to a specific product, a special method should be specified for determination. 1 Reagents
The reagents used are all analytically pure, using distilled water or water with a purity equivalent to distilled water. 1.1 Hydrochloric acid, 11 solution. www.bzxz.net
1.2 Standard silver nitrate solution, 0.01 mol/L, 1.3 Ammonium chloride solution, 17.2 mg/L.
1.4 Sodium hydroxide solution, 200 g/L.
1.5 Barium chloride solution, 50 g/L.
1.6 Potassium chromate solution, 50 g/L.
1.7 Devarda alloy powder. 1.8 Nessler reagent, prepared according to method 1.8.1 or 1.8.2. 1.8.1 Dissolve 5 g potassium iodide in 3.5 mL water, add cold saturated mercuric chloride (HgCl2) solution dropwise, stir until a light red precipitate is formed, continue stirring, add 40 mL potassium hydroxide (500 g/L), dilute to 100 mL with water, mix well, let stand, decant the supernatant, and store in a dark place.
1.8.2 Dissolve 3.5g potassium iodide and 1.25g mercuric chloride (HgC12) in 80mL water, add cold saturated mercuric chloride solution, shake until a reddish precipitate appears, then add 12g sodium hydroxide, shake until dissolved, finally add a little saturated mercuric chloride solution and dilute to 100mL with water, shake from time to time for several days, then let it stand, and take the upper clear liquid for testing. 2 Instruments
In addition to conventional laboratory instruments, the following instruments are also required. 2.1 Glass filter (pore size 4~16um).
2.2 Distillation equipment.
2.3 Nessler colorimetric tube, capacity 50mL. 3 Determination of sulfate
3.1 Test steps
Take 50 mL of the clear solution obtained according to GB5211.1-85 "Determination of water-soluble pigment matter by cold extraction method" or GB5211.2-85 "Determination of water-soluble pigment matter by National Bureau of Standards, issued on August 26, 1986
Implementation on August 1, 1987
GB5211.11-86
hot extraction method", put it into a 250 mL beaker, add 1 mL of hydrochloric acid (1.1) to acidify, boil, add 10 mL of barium chloride solution (1.5) dropwise while stirring continuously, and let the solution stand overnight. Filter with a glass filter (2.1) that has been weighed at 150±5℃ in advance, wash the precipitate until there is no chloride, transfer it to an oven at 150±5℃ and dry it for 1h, transfer it to a desiccator and cool it to room temperature, weigh it, and weigh it to 1mg until it reaches constant weight. 3.2 Result Expression
Calculate the water-soluble sulfate content according to formula (1) and express it as the mass percentage of SO: 206Xml
-the mass of barium sulfate precipitate, g,
wherein: m
-the mass of the pigment used to determine the water-soluble matter, g. The calculation result is retained to two decimal places. 4 Determination of chloride
4.1 Test steps
Pipette 50mL of the clear solution obtained according to GB5211.1-85 or GB5211.2-85, add 1mL of potassium chromate solution (1.6) to a 250mL conical flask, and slowly titrate with standard silver nitrate solution (1.2) under sufficient shaking until a light reddish brown color is generated and does not disappear. For a blank test, add 1mL of potassium chromate solution to 50mL of water and titrate with standard silver nitrate solution until the color is consistent with the previous titration.
Note: The endpoint can also be determined by potentiometric titration. 4.2 Result expression
Calculate the water-soluble chloride content according to formula (2) and express it as the mass percentage of CI-: Vi-V
Where: V. —The volume of 0.01mol/L silver nitrate solution consumed in the blank test, mL; V1 —The volume of 0.01mol/L silver nitrate standard solution consumed by the test sample, mL, —The mass of the pigment used to determine the water-soluble matter, 8. m
The calculation result is retained to two decimal places. 5 Determination of nitrate
5.1 Test steps
Put 50mL of the clear solution obtained according to GB5211.1-85 or GB5211.2-85 into a distillation flask (2.2), dilute with water to about 150mL, add 3g of DeVarda alloy powder (1.7) and 30mL of sodium hydroxide solution (1.4), immediately close the distillation equipment, and put 4mL of hydrochloric acid (1.1) and 30mL of water into the receiving flask. Heat with a low fire to start the reduction reaction, and let the reaction proceed gently for about 0.5h, and continue to distill out about 70mL of liquid. During this process, the receiving flask must be kept cool with water. Transfer the distillate to a 250mL volumetric flask, add water to dilute to the mark, and mix. Pipette 5mL of the solution into a Nessler colorimetric tube (2.3), dilute to 50mL with water, add 1mL of Nessler reagent (1.8) and mix, then color the test solution. Use a burette to add different volumes of ammonium chloride solution (1.3) to several Nessler colorimetric tubes, prepare a standard series in the same way as the test solution color development process, and obtain a standard solution with the same color as the test solution. Take 50mL of water for a blank test.
5.2 Result expression
Calculate the water-soluble nitrate content according to formula (3), expressed as the mass percentage of NO:: 0.5×-V.
GB5211.11—86
Where: V. - Volume of ammonium chloride solution required for a blank test, mL; V1——Volume of ammonium chloride solution required for the sample, mL; m——Mass of pigment used to determine the water-soluble matter, 8. The calculation result shall be retained to two decimal places. 6 Test report
The test report shall at least include the following contents: type and name of the test pigment;
test results;
differences from the operation specified in this test;
method for obtaining the extract used in the test, whether it is hot extraction or cold extraction; e.
test date.
Additional notes:
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China and is under the jurisdiction of the National Technical Committee for Standardization of Paints and Pigments. This standard was drafted by the 16th Working Group of the Technical Committee for Standardization of Pigment Testing Methods. The main drafters of this standard are Huang Shengwei and Chen Baochi. 3
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