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UDC667.622.2
National Standard of the People's Republic of China
GB/T3184-93
Published on December 30, 1993
Leadchromeyellow
National Technical Supervision Bureau
Implemented on October 1, 1994
National Standard of the People's Republic of China
Lead chrome yellow
GB/T3184-93
Replaces GB3184-82
This standard refers to and adopts the international standard ISO3711-1990 "Lead chromate and lead molybdate chromate pigments for paints". 1 Subject content and scope of application
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of lead chrome yellow pigments. This standard applies to lead chrome yellow pigments composed of lead chromate, lead sulfate or basic lead chromate. The product is mainly used in coating, plastic, rubber and ink industries, not suitable for food packaging and toys. 2 Reference standards
Preparation of standard solution for titration analysis (volume analysis) of chemical reagents. GB1250
GB1710
GB1715
GB1717
GB1864
Method for expressing and determining limit values Method for determining light fastness of pigments
Method for determining residue on sieves of pigments
Determination of pH value of aqueous suspension of pigments
Comparison of pigment colors
GB 5211.1
GB5211.13
GB5211.15
GB5211.19
GB6682
GB9285
GB9287
3Product Classification
Determination of water-soluble pigments Cold extraction method
Determination of volatile pigments at 105℃
Determination of pH value of aqueous pigment extracts Determination of oil absorption of pigments Determination of relative tinting strength and diluted color of coloring pigments Analysis of laboratory water Specifications and test methods Sampling of raw materials for paints and varnishes Comparison of easy dispersibility of pigments Oscillation method Visual comparison method According to the different shades of product color, it is divided into five types: lemon chrome yellow, light chrome yellow, medium chrome yellow, dark chrome yellow and orange chrome yellow. Each variety is divided into two grades: first-class product and qualified product.
4 Technical requirements
Lead chrome yellow pigments should meet the technical requirements listed in Table 1. Approved by the State Bureau of Technical Supervision on December 30, 1993, and implemented on October 1, 1994
Color (compared with standard sample)
Color after dilution (compared with standard sample)
Relative tinting strength (compared with standard sample), %
Volatile matter at 105℃, % (m/m)
Water-soluble matter, % (m/m)
Acidity and alkalinity of water extract, mL
pH value of water suspension
Oil absorption, g/100g
Sieve residue (45μm sieve), % (m /m）Easy to disperse, μm
Lightfastness, grade
Total lead content (in terms of Pb), % (m/m)
Lemon chrome yellow
First-class qualified product
Light chrome yellow
Second-class qualified product
Medium chrome yellow
Second-class qualified product
Note: When the hue of the "color" item is the same, the sample is brighter than the standard sample, and the color difference is "slightly" grade, which can be used as a first-class product. 5 Test method
Dark chrome yellow
First-class product
Qualified product
All reagents used should be analytically pure reagents, and the third-grade water specified in GB6682 or water of corresponding purity should be used. 5.1 Color comparison
Carry out in accordance with the provisions of GB1864, and the sample size is 1g. 2
Orange chrome yellow
First-class product
Qualified product
First addition
Refined linseed oil
Second addition
Refined linseed oil
Lemon chrome yellow
5.2 Determination of color and relative tinting strength after dilution GB/T3184-93
Table 2 Addition amount of refined linseed oil
Light chrome yellow
Medium chrome yellow
Dark chrome yellow
Orange chrome yellow
According to the provisions of GB5211.19, for the preparation of pigment dispersion, 3.0g pigment and 1.5g paint base are taken, and the grinding number of the pigment dispersion is 200 turns; for the preparation of diluted color paste, 3.0g white paste and 0.36g pigment dispersion are taken. 5.3 Determination of volatile matter at 105℃
Perform according to the provisions of GB5211.3.
5.4 Determination of water-soluble matter
Perform according to the provisions of GB5211.1, with a sample size of 20g. 5.5 Determination of pH value of water extract
Perform according to the provisions of 3.2.1 indicator method in GB5211.13. 5.6 Determination of pH value of water suspension
Perform according to the provisions of GB1717.
5.7 Determination of oil absorption
Perform according to the provisions of GB5211.15, with a sample size of 5g. 5.8 Determination of sieve residue
Perform according to the provisions of Method A in GB1715.
5.9 Determination of easy dispersibility
Perform according to the provisions of GB9287. Alkyd resin: dry alkyd resin formed by polycondensation of pentaerythritol-phthalic anhydride modified by soybean oil and cattail oil, solid content 53%~57%, viscosity (S) 200~400 Lemon chrome yellow, medium chrome yellow, dark chrome yellow and orange chrome yellow: pigment relative density 5.0, grinding concentration 60% (m/m); light chrome yellow: pigment relative density 4.0, grinding concentration 50% (m/m). The result is expressed as the fineness of the pigment after grinding for 30 minutes. 5.10 Determination of light resistance
Carry out according to the provisions of GB1710.
5.11 Determination of total lead content
5.11.1 Principle
Dissolve the sample in hydrochloric acid, lead precipitates in the form of lead sulfide, determine the lead precipitated in lead sulfate by weight method, and then extract with ammonium acetate.
5.11.2 Reagents
5.11.2.1 Ammonium acetate (GB1292).
5.11.2.2 Tartaric acid (GB1294).
5.11.2.3 Hydrochloric acid (GB622): pl.18 g/mL. 5.11.2.4 Sulfuric acid (GB625): pl.84 g/mL. 5 Ethanol (GB679): 95% V/V).
5.11.2.6 Ammonia water (GB631): p0.88 g/mL. 5.11.2.7 Hydrogen sulfide: Prepared with hydrochloric acid and sodium sulfide or iron sulfide. 5.11.2.8
3 Nitric acid/bromine reagent: Nitric acid solution saturated with bromine (dilution 1+3). 3
GB/T3184—93
5.11.2.9 Sulfuric acid (GB625) solution: dilute 1+20. 5.11.2.10 Sodium sulfide (GB905): 50g/L solution (freshly prepared). 5.11.2.11 Ammonium acetate (GB1292) saturated solution. 5.11.3 Apparatus
5.11.3.1 Sintered (porous) glass crucible (pore size 10～16μm). 5.11.3.2 Drying oven: capable of maintaining a temperature of 150±2℃. 5.11.4 Operating steps
5.11.4.1 Sample
Weigh about 0.5g of sample, accurate to 0.0001g. 5.11.4.2 Determination
Put the sample in a 600mL beaker, add 100mL water, 15mL hydrochloric acid (5.11.2.3) and 2mL ethanol (5.11.2.5), cover the beaker and heat to boiling, slowly boiling until all aldehyde odors are removed. Dilute to 200mL with hot water, filter the solution with slow filter paper while hot, and wash the filter paper and residue with hot water until a few drops of filtrate meet sodium sulfide solution (5.11.2.10) and no color is shown. Combine the filtrate and washing solution.
Slowly add ammonia solution (5.11.2.6) while stirring until a non-disappearing soft precipitate is formed, then add 0.5g tartaric acid (5.11.2.2) and hydrochloric acid (5.11.2.3) until the pH value of the solution is between 1 and 2. At room temperature (23 ± 2°C), pass hydrogen sulfide (5.11.2.7) into the solution to saturate it, dilute the solution to 400mL, and then pass hydrogen sulfide to saturate it. Let the lead sulfide precipitate, preferably overnight. Use slow suction to extract the supernatant through the sintered crucible. Wash the precipitate once with saturated hydrogen sulfide water by decantation, and use a jet of hydrogen sulfide water to move the precipitate to the crucible with the help of a glass rod with a rubber head. Wash the precipitate in the crucible with hydrogen sulfide water 5 times, and discard the filtrate and washing liquid. Treat the lead sulfide precipitate in the sintered glass crucible with nitric acid/bromine reagent (5.11.2.8) to dissolve it in the original beaker, rinse it with hot water, collect the washing liquid in the same beaker, cover the beaker, heat it in a fume hood, and filter it with another sintered glass. Rinse the beaker, cover and crucible with hot water 5 times, and move the filtrate and washing liquid to another 600mL beaker. Cool the solution, add 15 mL of sulfuric acid (5.11.2.4), and evaporate the solution carefully until the thick white smoke disappears. Cool the beaker and the material, rinse the inner wall of the beaker with water, and evaporate the material again until smoke appears. Cool the beaker again, add 250 mL of water and 100 mL of ethanol (5.11.2.5), and leave all overnight. Draw out the supernatant through another sintered glass crucible with constant weight, wash the precipitate once by decantation with a mixture of equal parts of ethanol and dilute sulfuric acid (5.11.2.9), and spray a stream of the same washing liquid, and move the precipitate into the glass with the help of a glass rod with a rubber head. Wash the precipitate with ethanol until the washing liquid is neutral. Then put the crucible into a 150°C oven and heat until constant weight. Cool in a desiccator and weigh.
Fill the container with crystallized ammonium acetate (5.11.2.1) and pour 50 mL of boiling ammonium acetate solution (5.11.2.11) through it. Rinse with hot water until a few drops of filtrate do not show any color reaction when they meet the sodium sulfide solution. Dry, cool and weigh again according to the above method. 5.11.5 Expression of results
Total lead content 1, expressed as mass percentage of Pb, calculated according to formula (1): 1 = m × 0.6832 × 100
Where: mo - mass of the sample, g;
m1 - mass of the residue (PbSO), g. This mass is the difference between the two weighings before and after extraction with ammonium acetate; 0.6832 - coefficient for converting PbSO to Pb. 5.11.6 Allowable difference
The difference between two parallel determinations shall not be greater than 1.0%. 5.12 Determination of lead chromate content
5.12.1 Principle
The sample is dissolved in hydrochloric acid-sodium chloride solution. Chromium (V) is reduced to chromium (III) with potassium iodide, and the precipitated iodine is titrated with sodium thiosulfate using water-soluble starch as an indicator.
5.12.2 Reagents
GB/T3184-93
5.12.2.1 Hydrochloric acid-sodium chloride mixture: Add 1000mL of saturated sodium chloride solution to 150mL of distilled water and 100mL of hydrochloric acid. 5.12.2.2 Standard sodium thiosulfate titration solution: c(Na2S20s)=0.1mol/L. 5.12.2.3 Hydrochloric acid (GB622): pl.18g/mL. 5.12.2.4 Potassium iodide (GB1272).
5.12.2.5 Soluble starch: 5g/L aqueous solution. 5.12.3 Operation steps
5.12.3.1 Sample
Weigh about 0.3~0.5g of sample, accurate to 0.0001g. 5.12.3.2 Determination
Put the sample in an iodine volumetric flask, add 50mL of hydrochloric acid-sodium chloride solution (5.12.2.1), heat to dissolve, then dilute to 150~200mL, add 2g of potassium iodide (5.12.2.4) and 10mL of concentrated hydrochloric acid (5.12.2.3) after cooling, place in a dark place for 5~10min, then titrate with sodium thiosulfate standard titration solution (5.12.2.2) until the solution turns yellow-green, add 3mL of starch indicator, and continue titrating until it turns bright green, which is the end point. 5.12.4 Expression of results
The content of lead chromate a2, expressed as mass percentage, is calculated according to formula (2): V.×0.1077×100
Wherein: V—the volume of sodium thiosulfate standard titration solution consumed in titration, mL, c—the actual concentration of sodium thiosulfate standard titration solution, mol/L, m2—the mass of the sample, g;
(2)
0.1077——the mass of lead chromate in grams equivalent to 1.00mL sodium thiosulfate standard titration solution Cc(Na2S20:)=1.000mol/LJ.
5.12.5 Allowable difference
The difference between two parallel determinations shall not exceed 0.2%. 6 Inspection rules
6.1 Lead chrome yellow products shall be inspected by the inspection department of the manufacturer in accordance with the provisions of this standard before leaving the factory. The manufacturer shall ensure that all products leaving the factory meet the technical requirements of this standard. Each batch of products leaving the factory shall be accompanied by a certificate of product grade. 6.2 All technical requirements listed in this standard are type inspection items, among which color, color after dilution, relative tinting strength, volatile matter at 105℃, lead chromate content, water-soluble matter, pH value of water extract, pH value of water suspension, oil absorption and sieve residue are ten items for factory inspection. Under normal production conditions, type inspection shall be carried out at least once every six months. 6.3 Sampling method: in accordance with the relevant provisions of GB9285. 6.4 The receiving department has the right to inspect the product in accordance with the provisions of the product standard. If the quality is found to be inconsistent with the provisions of this standard, the supply and demand parties shall jointly take double samples for re-inspection in accordance with the provisions of Article 6.3. If it still does not meet the provisions of this standard, the product is unqualified. 6.5 When a dispute arises between the supply and demand parties over product quality, the product quality supervision and inspection agency shall conduct arbitration. 6.6 The judgment of the test results in this standard shall be carried out according to the rounded value comparison method in GB1250. 7 Marking, packaging, transportation, storage
7.1 Marking
The product packaging bag shall be printed with firm and clear markings, including the manufacturer's name, product name, registered trademark, standard code, quality grade, production batch number, net weight, production date and the specified "wet-afraid" mark. 7.2 Packaging
GB/T3184-93
The product is packaged in plastic woven bags or iron drums, lined with kraft paper or plastic bags. 7.3 Transportation
The transportation and loading and unloading should be light to prevent packaging contamination and damage. The product should be protected from rain and sunlight during transportation. 7.4 Storage
Products should be stored in ventilated and dry places according to grade, classification and batches. It is strictly forbidden to contact with items that may react with the product, and attention should be paid to moisture-proof. 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 was drafted by Shanghai Chrome Yellow Pigment Factory. The main drafters of this standard are Shen Weijiang and Zhao Rong.6 Allowable difference
The difference between two parallel determinations shall not be greater than 1.0%. 5.12 Determination of lead chromate content
5.12.1 Principle
The sample is dissolved in hydrochloric acid-sodium chloride solution. Chromium (V) is reduced to chromium (III) with potassium iodide, and the precipitated iodine is titrated with sodium thiosulfate using water-soluble starch as an indicator.
5.12.2 Reagentswww.bzxz.net
GB/T3184-93
5.12.2.1 Hydrochloric acid-sodium chloride mixture: Add 1000mL of saturated sodium chloride solution to 150mL of distilled water and 100mL of hydrochloric acid. 5.12.2.2 Standard titration solution of sodium thiosulfate: c(Na2S20s)=0.1mol/L. 5.12.2.3 Hydrochloric acid (GB622): pl.18g/mL. 5.12.2.4 Potassium iodide (GB1272).
5.12.2.5 Soluble starch: 5g/L aqueous solution. 5.12.3 Operating steps
5.12.3.1 Sample
Weigh about 0.3~0.5g of sample, accurate to 0.0001g. 5.12.3.2 Determination
Put the sample in an iodine volumetric flask, add 50mL of hydrochloric acid-sodium chloride solution (5.12.2.1), heat to dissolve, then dilute to 150~200mL, cool, add 2g of potassium iodide (5.12.2.4) and 10mL of concentrated hydrochloric acid (5.12.2.3), place in a dark place for 5~10min, then titrate with sodium thiosulfate standard titration solution (5.12.2.2) until the solution turns yellow-green, add 3mL of starch indicator, and continue titrating until it turns bright green, which is the end point. 5.12.4 Expression of results
The content of lead chromate a2, expressed as mass percentage, is calculated according to formula (2): V.×0.1077×100
Wherein: V—the volume of sodium thiosulfate standard titration solution consumed in titration, mL, c—the actual concentration of sodium thiosulfate standard titration solution, mol/L, m2—the mass of the sample, g;
(2)
0.1077——the mass of lead chromate in grams equivalent to 1.00mL sodium thiosulfate standard titration solution Cc(Na2S20:)=1.000mol/LJ.
5.12.5 Allowable difference
The difference between two parallel determinations shall not exceed 0.2%. 6 Inspection rules
6.1 Lead chrome yellow products shall be inspected by the inspection department of the manufacturer in accordance with the provisions of this standard before leaving the factory. The manufacturer shall ensure that all products leaving the factory meet the technical requirements of this standard. Each batch of products leaving the factory shall be accompanied by a certificate of product grade. 6.2 All technical requirements listed in this standard are type inspection items, among which color, color after dilution, relative tinting strength, volatile matter at 105℃, lead chromate content, water-soluble matter, pH value of water extract, pH value of water suspension, oil absorption and sieve residue are ten items for factory inspection. Under normal production conditions, type inspection shall be carried out at least once every six months. 6.3 Sampling method: in accordance with the relevant provisions of GB9285. 6.4 The receiving department has the right to inspect the product in accordance with the provisions of the product standard. If the quality is found to be inconsistent with the provisions of this standard, the supply and demand parties shall jointly take double samples for re-inspection in accordance with the provisions of Article 6.3. If it still does not meet the provisions of this standard, the product is unqualified. 6.5 When a dispute arises between the supply and demand parties over product quality, the product quality supervision and inspection agency shall conduct arbitration. 6.6 The judgment of the test results in this standard shall be carried out according to the rounded value comparison method in GB1250. 7 Marking, packaging, transportation, storage
7.1 Marking
The product packaging bag shall be printed with firm and clear markings, including the manufacturer's name, product name, registered trademark, standard code, quality grade, production batch number, net weight, production date and the specified "wet-afraid" mark. 7.2 Packaging
GB/T3184-93
The product is packaged in plastic woven bags or iron drums, lined with kraft paper or plastic bags. 7.3 Transportation
The transportation and loading and unloading should be light to prevent packaging contamination and damage. The product should be protected from rain and sunlight during transportation. 7.4 Storage
Products should be stored in ventilated and dry places according to grade, classification and batches. It is strictly forbidden to contact with items that may react with the product, and attention should be paid to moisture-proof. 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 was drafted by Shanghai Chrome Yellow Pigment Factory. The main drafters of this standard are Shen Weijiang and Zhao Rong.6 Allowable difference
The difference between two parallel determinations shall not be greater than 1.0%. 5.12 Determination of lead chromate content
5.12.1 Principle
The sample is dissolved in hydrochloric acid-sodium chloride solution. Chromium (V) is reduced to chromium (III) with potassium iodide, and the precipitated iodine is titrated with sodium thiosulfate using water-soluble starch as an indicator.
5.12.2 Reagents
GB/T3184-93
5.12.2.1 Hydrochloric acid-sodium chloride mixture: Add 1000mL of saturated sodium chloride solution to 150mL of distilled water and 100mL of hydrochloric acid. 5.12.2.2 Standard titration solution of sodium thiosulfate: c(Na2S20s)=0.1mol/L. 5.12.2.3 Hydrochloric acid (GB622): pl.18g/mL. 5.12.2.4 Potassium iodide (GB1272).
5.12.2.5 Soluble starch: 5g/L aqueous solution. 5.12.3 Operating steps
5.12.3.1 Sample
Weigh about 0.3~0.5g of sample, accurate to 0.0001g. 5.12.3.2 Determination
Put the sample in an iodine volumetric flask, add 50mL of hydrochloric acid-sodium chloride solution (5.12.2.1), heat to dissolve, then dilute to 150~200mL, cool, add 2g of potassium iodide (5.12.2.4) and 10mL of concentrated hydrochloric acid (5.12.2.3), place in a dark place for 5~10min, then titrate with sodium thiosulfate standard titration solution (5.12.2.2) until the solution turns yellow-green, add 3mL of starch indicator, and continue titrating until it turns bright green, which is the end point. 5.12.4 Expression of results
The content of lead chromate a2, expressed as mass percentage, is calculated according to formula (2): V.×0.1077×100
Wherein: V—the volume of sodium thiosulfate standard titration solution consumed in titration, mL, c—the actual concentration of sodium thiosulfate standard titration solution, mol/L, m2—the mass of the sample, g;
(2)
0.1077——the mass of lead chromate in grams equivalent to 1.00mL sodium thiosulfate standard titration solution Cc(Na2S20:)=1.000mol/LJ.
5.12.5 Allowable difference
The difference between two parallel determinations shall not exceed 0.2%. 6 Inspection rules
6.1 Lead chrome yellow products shall be inspected by the inspection department of the manufacturer in accordance with the provisions of this standard before leaving the factory. The manufacturer shall ensure that all products leaving the factory meet the technical requirements of this standard. Each batch of products leaving the factory shall be accompanied by a certificate of product grade. 6.2 All technical requirements listed in this standard are type inspection items, among which color, color after dilution, relative tinting strength, volatile matter at 105℃, lead chromate content, water-soluble matter, pH value of water extract, pH value of water suspension, oil absorption and sieve residue are ten items for factory inspection. Under normal production conditions, type inspection shall be carried out at least once every six months. 6.3 Sampling method: in accordance with the relevant provisions of GB9285. 6.4 The receiving department has the right to inspect the product in accordance with the provisions of the product standard. If the quality is found to be inconsistent with the provisions of this standard, the supply and demand parties shall jointly take double samples for re-inspection in accordance with the provisions of Article 6.3. If it still does not meet the provisions of this standard, the product is unqualified. 6.5 When a dispute arises between the supply and demand parties over product quality, the product quality supervision and inspection agency shall conduct arbitration. 6.6 The judgment of the test results in this standard shall be carried out according to the rounded value comparison method in GB1250. 7 Marking, packaging, transportation, storage
7.1 Marking
The product packaging bag shall be printed with firm and clear markings, including the manufacturer's name, product name, registered trademark, standard code, quality grade, production batch number, net weight, production date and the specified "wet-afraid" mark. 7.2 Packaging
GB/T3184-93
The product is packaged in plastic woven bags or iron drums, lined with kraft paper or plastic bags. 7.3 Transportation
The transportation and loading and unloading should be light to prevent packaging contamination and damage. The product should be protected from rain and sunlight during transportation. 7.4 Storage
Products should be stored in ventilated and dry places according to grade, classification and batches. It is strictly forbidden to contact with items that may react with the product, and attention should be paid to moisture-proof. 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 was drafted by Shanghai Chrome Yellow Pigment Factory. The main drafters of this standard are Shen Weijiang and Zhao Rong.4 Storage
Products should be stored in ventilated and dry places according to grade, classification and batches. It is strictly forbidden to contact with items that may react with the product, and attention should be paid to moisture-proof. 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 was drafted by Shanghai Chrome Yellow Pigment Factory. The main drafters of this standard are Shen Weijiang and Zhao Rong.4 Storage
The product should be stored in a ventilated and dry place according to grade, classification and batch. It is strictly forbidden to contact with items that may react with the product, and attention should be paid to moisture-proof. 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 was drafted by Shanghai Chrome Yellow Pigment Factory. The main drafters of this standard are Shen Weijiang and Zhao Rong.
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