Some standard content:
National Standard of the People's Republic of China
Zinc Oxide
(Indirect Method)
Zinc Oxide (Indirect Method)Subject Content and Scope of Application
GB/T 3185-92
Replaces GB318582
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of zinc oxide prepared by the indirect method. This standard is applicable to zinc oxide used in industries such as coatings, rubber, medicine, chemical industry and light industry. Molecular formula: ZnO
Relative molecular mass: 81.39 (1987 international atomic weight) 2 Reference standardsWww.bzxZ.net
Chemical reagents
Preparation of standard solutions for titration analysis (volume analysis) GB603 Chemical reagents
GB 1715
GB 1864
Preparation of preparations and products used in test methods Determination of pigment sieve residue
Comparison of pigment colors
GB 5211.2
GB 5211. 3
GB 5211. 15
GB 5211. 16
GB 6682
GB 9285
Determination of water-soluble matter in pigments by hot extraction method
Determination of volatile matter in pigments at 105°C
Determination of oil absorption of pigments
Comparison of tinting power of white pigments
Specifications of water for laboratories
Raw materials for paints and varnishes
General rules for flame atomic absorption spectrometry for chemical reagents GB9723
3 Product classification
It is divided into two categories according to different uses, and each category is divided into the following grades: a.
BA01-05 (Type I) for rubber, superior grade, first grade, qualified product; b. BA01-05 (Type I) for coatings, superior grade, first grade, qualified product. 4 Technical requirements
The technical indicators of zinc oxide shall meet the requirements of the following table: Approved by the State Bureau of Technical Supervision on June 9, 1992 146
Implemented on June 1, 1993
Zinc oxide (in dry product), %
Metallic matter (in Zn), %
Lead oxide (in Pb), %
Manganese oxide (in Mn), %
Copper oxide (in Cu), %
Hydrochloric acid insoluble matter, %
Ignition loss, %
Sieve residue (45 μm mesh), %
Water-soluble matter, %
105C volatile matter, %
Oil absorption, g/100g
Color\(compared with standard sample)
Color-reducing power\(compared with standard sample), %
GB/T 3185-92
BA01-05(Type 1)
Superior grade
First grade
Note: 1) Type 1 "color" and "color-reducing power" standard samples provided by: Lanzhou Chemical Raw Materials Factory. 5 Test methods
Qualified products
BA01-05(Type)
Superior grade
First grade
Qualified products
The reagents used in this standard are analytically pure reagents unless otherwise specified. This standard uses grade 3 water or water of corresponding purity specified in GB6682.
5.1 Determination of zinc oxide content
5.1.1 Principle
Dissolve the sample in hydrochloric acid, neutralize it, and titrate the zinc oxide content with EDTA standard titration solution. 5.1.2 Reagents and materials
5.1.2.1 Hydrochloric acid (GB622): high-grade pure, diluted 1+1. 5.1.2.2 Ammonia water (GB631): high-grade pure. 5.1.2.3 Ammonia water (GB631): high-grade pure, diluted 1+-1. 5.1.2.4 Buffer solution (pH=10).
Weigh 54g ammonium chloride (GB658) and dissolve it in 200mL water, add 350mL ammonia water (5.1.2.2), and then continue to dilute with water to 1 000mlc
5.1.2.5 Chrome black T indicator: 5g/L, prepared according to GB603. Disodium ethylenediaminetetraacetic acid (EDTA) standard titration solution: C(EDTA)=0.05mol/L, prepared according to GB601 and standard 5.1.2.6
5.1.3 Instruments and equipment
5.1.3.1 Balance: sensitivity 0.0001g.
5.1.3.2 Conical flask: 500mL.
5.1.3.3 Electric furnace.
5.1.4 Analysis steps
GB/T 3185-92
5.1.4.1 Sample
Weigh 0.13~0.15g of the sample that has been dried in advance (105±1C) to an accuracy of 0.0001g. 5.1.4.2 Determination
Put the sample in a 500ml conical flask, add a small amount of water to moisten it, add 3mL of hydrochloric acid (5.1.2.1), heat to dissolve, add water to 200ml, neutralize with ammonia water (5.1.2.3) to pH7~8 (zinc hydroxide precipitation is generated), then add 10ml of buffer solution (5.1.2.4) and 5 drops of chrome black T indicator (5.1.2.5), and titrate with EDTA standard titration solution (5.1.2.6) until the solution changes from purple to blue, which is the end point.
5.1.5 Result Expression
The zinc oxide content (X,) is expressed as mass percentage and is calculated according to formula (1): X 0. 081 39 × C. V
× 100
Wherein: X,—the percentage of zinc oxide, expressed as mass percentage; the molar concentration of CEDTA standard titration solution, mol/L; V-the amount of EDTA standard titration solution, mI.; (1)
m——the mass of the sample, g;
0.08139-—the mass of zinc oxide in grams equivalent to 1.00 mL of C (EDTA) standard titration solution [C (EDTA) 1.000 mol/L].
Take the average of two determinations and keep two decimal places. 5.1.6 Permissible Difference
The relative error of two parallel determinations shall not be greater than 0.1%. 5.2 Determination of metal content (in terms of Zn) 5.2.1 Principle
Qualitative test: Dissolve the sample in hydrochloric acid and observe its dissolution process. Quantitative test: Dissolve the sample in iodine standard solution and hydrochloric acid, cool, and titrate zinc with sodium thiosulfate standard titration solution. 5.2.2 Reagents and materials
5.2.2.1 Hydrochloric acid (GB622): high-grade pure, diluted 1+1. 5.2.2.2 Hydrochloric acid (GB622): high-grade pure, diluted 1+3. 5.2.2.3 Iodine standard solution: C (No. Iz) = 0.05 mol/L, prepared according to GB601. 5.2.2.4 Sodium thiosulfate standard titration solution: C (Na2S, O.) = 0.05 mol/L, prepared and calibrated according to GB601. 5.2.2.5 Starch solution: 5 g/L, prepared according to GB603. 5.2.3 Instruments and equipment
5.2.3.1 Balance: sensitivity 0.1g.
5.2.3.2 Beaker: 400ml.
5.2.3.3 Iodine volumetric flask: 500mL.
5.2.3.4 Pipette: 25mL.
5.2.4 Analysis steps
5.2.4.1 Sample
Weigh 30g and 10g of the sample, accurate to 0.1g. 5.2.4.2 Determination
Qualitative test: Place 30g of the sample in a 400mL beaker, moisten it with a little basic water, add 200ml of hydrochloric acid (5.2.2.1) to stir and observe the dissolution of zinc oxide. During the dissolution process, if no black dot-like metal objects or metal-containing objects that emit hydrogen bubbles are found, a quantitative test is required. GB/T 3185-92
Quantitative test: Place 10g of the sample in a 500mL iodine volumetric bottle with a glass ball, moisten it with water, add 25mL of the iodine standard solution (5.2.2.3) with a pipette, shake to mix, cover the bottle stopper and seal it with water, place it in a dark place for 1h, shake it from time to time, then slowly add 90mL of hydrochloric acid (5.2.2.2), cover the bottle stopper tightly, and immediately cool it to room temperature with running water. After the zinc oxide is completely dissolved, rinse the bottle stopper and bottle wall with distilled water, and immediately titrate with sodium thiosulfate standard titration solution (5.2.2.4). When the solution turns light blue, add 1~2ml of starch solution (5.2.2.5), and continue to titrate until the blue disappears as the end point. At the same time, perform a blank test. 5.2.5 Result Expression
The content (X) of metal in terms of zinc (Zn) is expressed as mass percentage and is calculated according to formula (2): 0.032 69 ×C (Vo-VI) × 100X, =
Where: X. -- The percentage content of the metal in terms of zinc, expressed as mass percentage; C -- The molar concentration of the sodium thiosulfate standard titration solution, mol/L; V -- The amount of sodium thiosulfate standard titration solution used for the blank test, mL; V1 -- The amount of sodium thiosulfate standard titration solution used for the titration sample, mL; m -- The mass of the sample, g;
(2)
0.03269 -- The mass of zinc in grams equivalent to 1.00 mL of sodium thiosulfate standard titration solution [C(Na2S,O,) = 1.000 mol/L].
5.3 Determination of lead oxide (in terms of Pb) content
Determine according to the following method A (oxidation-reduction method) or method B (atomic absorption spectrometry). 5.3.1 Method A - Redox Method
5.3.1.1 Reagents and Materials
5.3.1.1.1 Nitric Acid (GB626): Superior Grade, Diluted 1+1. 5.3.1.1.2 Sodium Hydroxide Solution (GB629): Superior Grade, 100g/L, Prepared According to GB603. 5.3.1.1.3 Methyl Orange Indicator: 1g/L, Prepared According to GB603. 5.3.1.1.4 Glacial Acetic Acid Solution (GB676): 2% (V/V), Prepared According to GB603. 5.3.1.1.5 Glacial Acetic Acid Solution (GB676): 12% (V/V), Prepared According to GB603. 5.3.1.1.6 Potassium Chromate Solution: 50g/1., Prepared According to GB603. 5.3.7.7.7 Silver nitrate solution (GB670): 10g/1, prepared according to GB603. 5.3.1.1.8 Hydrochloric acid (GB622): high-grade pure, diluted 1+1. 5.3.1.1.9 Saturated sodium chloride solution (GB1266). Hydrochloric acid-sodium fluoride mixed solution
5. 3. 1. 1. 10
Take 100mL of saturated sodium chloride solution (5.3.1.1.9), add 30mL of hydrochloric acid (5.3.1.1.8) and mix. 5.3.1.1.11 Potassium iodide (GB1272).
5.3.1.1.12 Standard sodium thiosulfate titration solution: C(Na2S,),）)=0.01mol/L, prepared and calibrated according to GB601. 5.3.1.1.13 Starch solution: 5g/1, prepared according to GB603. 5.3.1.2 Instruments and equipment
5.3.1.2.1 Balance: sensitivity 0.1g.
5.3.1.2.2 Beaker: 300mL.
5.3.1.2.3 Ground-mouth conical flask: 300ml. 5.3.1.2.4 Electric furnace.
5.3.1.3 Analysis steps
5.3.1.3.1 Sample
Weigh 10g of sample, accurate to 0.1g.
5.3.1.3.2 Determination
GB/T3185-—92
Place the sample in a 300ml beaker, first moisten it with a small amount of water, add 40mL of nitric acid (5.3.1.1.1), dissolve it, then add sodium hydroxide solution (5.3.1.1.2) to neutralize it until a white suspended precipitate is formed, add 2 drops of methyl orange indicator (5.3.1.1.3), then add sodium hydroxide solution (5.3.1.1.2) to neutralize it until the methyl orange changes from red to orange-yellow (pH - 5), then add glacial acetic acid solution (5.3.1.1.5) to acidify to pH = 3.5 (using 0.5~~5.5 precision pH test paper for comparison), gradually add 5 ml of potassium chromate solution (5.3.1.1.6) while stirring, heat and boil for 5 minutes, cool, filter after the lead chromate condenses, and rinse the precipitate on the filter paper with 30 ml of glacial acetic acid solution (5.3.1.1.4) until the filtrate is no longer yellow, and then wash with water until there is no chromate ion [test with silver nitrate solution (5.3.1.1.7) until there is no red precipitate). Use 50mL of hot hydrochloric acid-sodium chloride mixture (5.3.1.1.10) to dissolve the precipitate in a 300mL ground-mouth conical flask. Wash the filter paper with hot water and then with cold water until there is no chromate ion. Then add 0.5g of potassium iodide (5.3.1.1.11) and place in a dark place for 15min. Titrate with sodium thiosulfate standard titration solution (5.3.1.1.12) until it turns light yellow. Then add 2-3mL of starch solution (5.3.1.1.13) and continue titrating until the blue color disappears. 5.3.1.4 Expression of results
Lead oxide contains (X) in terms of lead (Pb) and is expressed as mass percentage, calculated according to formula (3): X: 0.069 06 ×CV
The percentage content of lead oxide as lead, expressed as mass percentage; where: X.—
C--the molar concentration of sodium thiosulfate standard titration solution, mol/L; V—.the amount of sodium thiosulfate standard titration solution used, mL; the mass of the sample, g;
s—-the mass of 0.069 06-
lead expressed in grams equivalent to 1.00mL sodium thiosulfate standard titration solution [C(NazS2O3)=1.000mol/L].
5.3.2B method—atomic absorption spectrometry
Perform according to the provisions of GB9723, and take 5g of sample. 5.4 Determination of manganese oxide (as Mn) content The content is determined according to the following method A (oxidation-reduction method) or method B (atomic absorption spectrometry). 5.4.1 Method A - Redox Method
5.4.1.1 Reagents and Materials
5.4.1.1.1 Nitric Acid (GB626): Premium Grade, Diluted 1+3. 5.4.1.1.2 Sulfuric Acid (GB625): Premium Grade. 5.4.1.1.3 Phosphoric Acid (GB1282): Premium Grade. 5.4.1.1.4 Potassium Periodate: Premium Grade.
5.4.1.1.5 Manganese Standard Solution (A)
Accurately weigh 0.2749g of anhydrous manganese sulfate (premium grade) burned to constant weight at 400-500℃ and place it in a beaker, add 100ml of water to dissolve it, transfer it into a 1000ml brown volumetric flask and dilute to the mark, shake it. This solution contains 0.1mg of manganese per ml. Manganese standard solution (B)
Pipette 25mL of manganese standard solution (A), add it to a 250mL brown volumetric flask, dilute to the mark with water, and shake well. This solution contains 0.01mg of manganese per milliliter. This solution must be prepared on the same day. Note: Manganese standard solution is prepared with double distilled water. 5.4.1.2 Instruments and equipment
5.4.1.2.1 Balance: 0.1g.
5.4.1.2.2 Beaker: 100ml.
5.4.1.2.3 Colorimetric tube: 50mL.
5.4.1.2.4 Electric furnace.
5.4.1.3 Analysis steps
5.4.1.3.1 Sample
Weigh 5g of sample, accurate to 0.1g.
5.4.1.3.2 Determination
GB/T 3185--92
Put the sample in a beaker, add 25mL of nitric acid (5.4.1.1.1) to dissolve it, then add 5mL of sulfuric acid (5.4.1.1.2) and 5mL of phosphoric acid (5.4.1.1.3), then boil it for 5min, add 0.5g of potassium periodate (5.4.1.1.4) after cooling, then boil it for 5~~10min, quickly cool it and transfer it into a 50mL colorimetric tube, dilute it to the scale with water for colorimetric use. Also take the manganese standard solution [5.4.1.1.5 (B)] and treat it in the same way as the sample, then perform colorimetric analysis. When the color of the sample is not darker than the standard, it is qualified. Manganese standard solution is drawn in the following quantities:
Superior quality: draw manganese standard solution [5.4.1.1.5 (B)> 0.5mL (equivalent to manganese content 0.0001%). -Qualified quality: draw manganese standard solution [5.4.1.1.5 (B) 0.5mL (equivalent to manganese content 0.0001%). Qualified quality: draw manganese standard solution [5.4.1.1.5 (B)] 1.5mL (equivalent to manganese content 0.0003%). 5.4.2 Method B - Atomic absorption spectrometry
Perform according to the provisions of GB9723, and take 5g of sample. 5.5 Determination of copper oxide (Cu) content
Perform determination according to the following method A (oxidation-reduction method) or method B (atomic absorption spectrometry). 5.5.1 Method A - Redox Method
5.5.1.1 Reagents and Materials
5.5.1.1.1 Nitric Acid (GB626): Premium Grade, Diluted 1+1. 5.5.1.1.2 Ammonia Water (GB631): Premium Grade, Diluted 1+1. 5.5.1.1.3 Chloroform (GB682).
5.5.1.1.4 Phenol anhydride ethanol solution: 10g/1. 5.5.1.1.5 Metallic copper: 99.95%.
5.5.1.1.6 Sodium diethyldithiocarbamate (copper reagent) solution: 1g/L. Accurately weigh 0.1g of copper reagent and dissolve it in 100mL of double distilled water. Prepare it when needed. 5.5.1.1.7 Triammonium citrate: 200g/L. Purification method: Take 100ml of 20% ammonium citrate solution and put it into a 250ml separatory funnel, add 2 drops of phenolphthalein (5.5.1.1.4), neutralize with 1:1 ammonium hydroxide until it turns red, then add 6 drops in excess, add 10mL of copper reagent (5.5.1.1.6), add 25ml of chloroform (5.5.1.1.3), cover the bottle stopper and shake for 1min, then separate and remove the organic solvent layer, add 10ml of chloroform. Repeat the extraction until the organic solvent layer is colorless, and finally separate and remove the organic solvent layer. Put the ammonium citrate solution into a reagent bottle for later use. 5.5.1.1.8 Copper standard solution (A)
Accurately weigh 0.1000g of metallic copper (5.5.1.1.5), put it into a 200ml beaker, add 10ml of nitric acid (5.5.1.1.1) to dissolve, heat to drive off nitrogen oxides, remove and cool, wash into a 1000ml volumetric flask, dilute to scale with water, and shake well. This solution contains 0.1mg of copper per milliliter.
Copper standard solution (B)
Put 5mL of copper standard solution (A) into a 500mL volumetric flask, dilute to scale with water, and shake well. This solution contains 0.001mg of copper per milliliter.
5.5.1.2 Instruments and equipment
5.5.1.2.1 Balance: sensitivity 0.1g.
5.5.1.2.2 Beaker; 100ml.
5.5.1.2.3 Separating funnel: 250mL.
5.5.1.2.4 Colorimetric tube: 50ml.
5.5.1.2.5 Electric furnace.
5.5.1.3 Analysis steps
5.5.1.3.1 Sample
Weigh 2g of sample, accurate to 0.1g.
5.5.1.3.2 Determination
GB/T 3185-92
Place the sample in a beaker, moisten it with a small amount of water, add 10mL of nitric acid (5.5.1.1.1) to dissolve it, heat and evaporate it to about 5ml.. Cool it. Wash it into a 250mL separating funnel with a volume of about 30mL, add 40ml of triammonium citrate (5.5.1.1.7), add 2 drops of phenolphthalein (5.5.1.1.4), and then add ammonia water (5.5.1.1.2) to neutralize it until it turns red and add 6 drops of excess, add 10ml of copper reagent (5.5.1.1.6), accurately add 5mlL of dichloromethane (5.5.1.1.3), cover the bottle stopper, shake it for 1min, and after the organic solvent layer is separated, transfer the organic solvent layer into a 50ml colorimetric tube for colorimetry. Draw copper standard solution [5.5.1.1.8 (B)] and treat it in the same way as the sample, then compare the color with the sample. When the color of the sample is not darker than the standard, it is qualified.
Draw copper standard solution in the following quantities;
Superior quality: draw copper standard solution C5.5.1.1.8 (B)) 4mL (equivalent to copper content 0.0002%). -Qualified quality: draw copper standard solution [5.5.1.1.8 (B) 8mL (equivalent to copper content 0.0004%). Qualified quality: draw copper standard solution [5.5.1.1.8 (B) 10ml. (equivalent to copper content 0.0005%). 5.5.2B method - atomic absorption spectrometry
Perform according to the provisions of GB9723, and take 5g of sample. 5.6 Determination of hydrochloric acid insoluble matter
5.6.1 Reagents and materials
5.6.1.1 Hydrochloric acid (GB622): high-grade pure, diluted 1+1. 5.6.1.2 Silver nitrate (GB670): 10g/L, prepared according to GB603. 5.6.2 Instruments and equipment
5.6.2.1 Balance: sensitivity 0.1g, 0.0001g. Beaker 300ml.
5.6.2.3 Crucible.
5.6.2.4 Electric furnace.
5.6.2.5 Filter paper: quantitative filter paper.
5.6.2.6 Dryer.
5.6.2.7 High-temperature furnace: 800C.
5.6.3 Analysis steps
5.6.3.1 Sample
Weigh 30 g of sample with an accuracy of 0.1 g.
5.6.3.2 Determination
Put the sample in a beaker, moisten it with a small amount of water, add 200mL of hydrochloric acid (5.6.1.1), heat and dissolve, filter with quantitative filter paper, wash the residue with water until there is no chloride ion (test with silver nitrate solution (5.6.1.2), it should not be turbid), transfer the filter paper to a crucible with constant weight, after the filter paper is completely carbonized, transfer it to a high-temperature furnace, burn it at 800C for 30min, take out the crucible, transfer it to a desiccator, cool it to room temperature and weigh it to constant weight.
5.6.4 Expression of results
The content of hydrochloric acid insoluble matter (X) is expressed as mass percentage and calculated according to formula (4): 152
GB/T 3185--92
Wherein: X—the percentage of hydrochloric acid insoluble matter, expressed as mass percentage; m—
-the total mass of the crucible and the hydrochloric acid insoluble matter, g; mo—the mass of the crucible, g;
m—the mass of the sample, g.
5.7 Determination of loss on ignition
5.7.1 Instruments and equipment
5.7.1.1 Balance: sensitivity 0.0001g.
5.7.1.2 Crucible blocking
5.7..1.3 High temperature furnace: 800~~850℃. 5.7.1.4 Dryer
5.7.2 Analysis steps
5.7.2.1 Sample
Weigh 2~~3g of the sample that has been dried in advance (105~110℃) to the nearest 0.0002g. (4)
5.7.2.2 Determination
Put the sample in a crucible with constant weight and burn it in a high-temperature furnace at 800~850℃ for 2h, then take it out and move it to a dryer, cool it to room temperature and weigh it (accurate to 0.0002g) until constant weight. 5.7.3 Expression of results
Loss on ignition (X) is expressed in mass percentage According to formula (5), calculate: mo-mi
The percentage of loss on ignition is expressed as mass percentage; where: X,
m. ———The mass of the sample and the crucible before ignition, g; m
The mass of the sample and the crucible after ignition, g;
m—The mass of the sample in g.
5.8 Determination of sieve residue
According to method A of GB1715.
5.9 Determination of water-soluble matter
According to the provisions of GB5211.2.
5.10 Determination of volatile matter at 105°C
Perform in accordance with the provisions of GB5211.3.
5.11 Determination of oil absorption
Perform in accordance with the provisions of GB5211.15. Sample weight 10g. (5)
5.12 Comparison of color
Perform in accordance with the provisions of GB1864. Sample weight 2g, add 0.7mL of refined linseed oil for the first time, grind for 200 turns (50×4), then add 0.7ml and grind for 25 turns.
5.13 Comparison of color-reducing power
Perform in accordance with the provisions of GB5211.16.
6 Inspection rules
6.1 Zinc oxide products shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that the quality of all zinc oxide products shipped out of the factory meets the technical requirements of this standard. Each batch of zinc oxide shipped out of the factory shall be accompanied by a product certificate. 6.2 Each batch of products shall be inspected item by item according to the test methods specified in this standard. 6.3 Sampling method: in accordance with the relevant provisions of GB9285. 6.4 The user has the right to inspect the received products according to the technical requirements and test methods specified in this standard. If the inspection results do not meet the requirements of this standard, double sampling shall be carried out from the original batch number according to the provisions of 6.3 for re-inspection. If the re-inspection results still do not meet the requirements of this standard, the entire batch of products shall be unqualified.
6.5 If both parties disagree with the re-inspection results and need to conduct arbitration, the arbitration institution shall be selected by agreement between the two parties. 7 Marking, packaging, transportation, storage
7.1 Marking
The packaging should be clearly marked, including the manufacturer's name, product name, trademark, standard number, production batch number, model, grade and net weight, and accompanied by a quality certificate.
7.2 Packaging
Zinc oxide is packed in plastic woven bags lined with plastic film or waterproof paper bags, with a net weight of 25kg or 50kg per bag. 7.3 Transportation
When transporting and loading, it is required to load and unload lightly, and collision and rupture should be prevented. It should be carried out in accordance with relevant transportation regulations. 7.4 Storage
Zinc oxide should be stored in a dry and ventilated place. It is strictly forbidden to contact with acidic and alkaline items. According to the above storage conditions, the effective storage period of unopened zinc oxide is half a year from the date of production. After the expiration of the period, it should be inspected according to the provisions of this standard. If it meets the requirements of this standard, it can continue to be used. Additional remarks:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the National Technical Committee for Standardization of Paints and Pigments. This standard is drafted by the Shanghai Coatings Research Institute. The main drafters of this standard are Yang Fen and Shui Liqin. This standard refers to JIS K1410-1962 (confirmed in 1983) "Zinc Oxide" and JIS K5102-1965 (confirmed in 1978) "Zinc Oxide (Pigment)".
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