Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2249-91
Iron oxide yellow pigment
Published on November 12, 1991
Ministry of Chemical Industry of the People's Republic of China
Implementation on July 1, 1992
W Chemical Industry Standard of the People's Republic of China
Iron oxide yellow pigment
This standard adopts the international standard ISO1248-1974 "Iron oxide pigment for paint". 1 Subject content and scope of application
HG/T2249-91
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of iron oxide yellow pigment. This standard applies to iron oxide yellow pigment obtained by oxidation of ferrous salt. It is mainly used in coatings, inks, construction and other industries. Molecular formula: Fe20:·H20
Relative molecular mass: 177.71 (according to the international relative atomic mass in 1987) 2 Reference standards
GB1715
GB1717
GB1864
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents Preparation of preparations and products used in test methods of chemical reagents Determination of pigment sieve residue
Determination of pH value of aqueous pigment suspension
Comparison of pigment colors
GB5211.13
GB5211.15
GB5211.19
GB6682
GB9285
3Product model
Determination of water-soluble pigmentsHot extraction method
Determination of volatile pigments at 105°C
Determination of pH value of pigment water extract
Determination of oil absorption of pigments
Determination of relative tinting strength and diluted color of coloring pigmentsLaboratory water specifications
Raw materials for paints and varnishes
HU01—01.
4Technical requirements
The technical indicators of iron oxide yellow shall meet the requirements in the following table. Item
Iron content [expressed as Fe20: (drying at 105℃)], % volatile matter at 105℃, %
Water-soluble matter, %
Approved by the Ministry of Chemical Industry of the People's Republic of China on 1991-11-12>
Visual comparison method
Qualified products
Implemented on 1992-07-01
W.bzsoso, comItem
Sieve residue (45um sieve hole), %
pH of water extract, mL||tt ||pH value of water suspension
Oil absorption g/100g
Lead chromate
Total calcium content (expressed as Cao), %
Color 1).2) (Compared with standard sample)
Relative tinting strength\(Compared with standard sample), %
Presence of organic coloring matter
HG/T2249-91
Approximately ~ slightly
Note: 1) The standard sample provider of "color" and "relative tinting strength" is Hunan Pingtang Iron Oxide Pigment Factory. 2) When the hue of the "color" item is the same, the sample is brighter than the standard sample, and the color difference is "slightly", which can be used as a first-class product. 5 Test method
Qualified products
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 Determination of iron content
5.1.1 Principle of the method
According to the principle of redox reaction, the iron content is titrated with potassium dichromate standard titration solution. 5.1.2 Reagents and materials
5.1.2.1 Hydrochloric acid (GB622): dilute 1+1. 5.1.2.2
Stannic chloride SnCl2 (GB638): 100g/L, weigh 50g stannous chloride (SnCl2) and dissolve it in 300mL hydrochloric acid (GB622), and dilute it to 500mL with water.
Put this clear solution in a sealed bottle and add a small amount of metal tin particles. 5.1.2.3 Mercuric chloride (1) (HG3-1068) saturated solution: 60~100g/L. Mixture of sulfuric acid and phosphoric acid: Mix 150mL sulfuric acid (GB625) and 150mL phosphoric acid (GB1282) in 500mL water, and dilute to 1L.
Barium diphenylamine sulfonate solution: Dissolve 1g barium diphenylamine sulfonate in 100mL sulfuric acid (GB625). Potassium dichromate standard titration solution: c (No.
KCr20z) = 0.1mol/L. Accurately weigh 4.9035g potassium dichromate that has been dried at 150℃ in advance, dissolve in water, and dilute to 1L.
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 Oven: 150±2℃.
5.1.3.4 Electric furnace.
5.1.4 Analysis steps
5.1.4.1 Sample
Weigh 0.3g of the sample that has been dried in advance (105±2℃) to an accuracy of 0.0001g. 5.1.4.2 Determination
W.HG/T2249—91
Put the sample in a 500mL conical flask, add 30mL of hydrochloric acid (5.1.2.1), and heat to completely dissolve it. In order to promote the dissolution of the sample, a few drops of stannous chloride (5.1.2.2) can be added while heating, but be careful not to add too much to cause the solution color to disappear. Continue to heat the above solution to a slight boil, slowly add stannous chloride (5.1.2.2) while shaking until the solution just turns colorless, then add 1-2 drops in excess, cool the flask to room temperature under running water, add 200 mL of cold water to dilute, then add 15 mL of mercuric chloride (I) (5.1.2.3) and shake vigorously to produce a slightly white precipitate. After 1 minute, add 50 mL of sulfuric acid and phosphoric acid mixed solution (5.1.2.4) and 3 drops of diphenylamine barium sulfonate solution (5.1.2.5), slowly titrate with potassium dichromate standard titration solution (5.1.2.6) until the color changes from dark green to purple, which is the end point. The titration should be started no more than 3 minutes after the addition of the mercuric chloride solution. 5.1.5 Result Expression
Expressed as the mass percentage of ferric oxide (Fe2O32) X, calculated according to formula (1): X,·1X0. 079 84×100V·01X7.984m1
Wherein: V1—the volume of potassium dichromate standard titration solution consumed, mL; ci——the actual concentration of potassium dichromate standard titration solution, mol/L; the mass of the sample, g,
0.07984——the mass of ferric oxide equivalent to 1.00mL potassium dichromate standard titration solution cKCr20)=1.000mol/LJ, expressed in grams.
Take the average of two determinations and keep one decimal place. 5.1.6 Permissible Difference
The relative error of two parallel determinations shall not be greater than 0.2%. 5.2 Determination of volatile matter at 105℃
Perform according to the provisions of GB5211.3.
5.3 Determination of water-soluble matter
Perform according to the provisions of GB5211.2. Sample weight is 5g. 5.4 Determination of sieve residue
Perform according to the provisions of Method A in GB1715.
5.5 Determination of pH value of water extract
Perform according to the provisions of 3.2.1 in GB5211.13. 5.6 Determination of pH value of water suspension
Perform according to the provisions of GB1717. Sample weight is 5g. 5.7 Determination of oil absorption
Perform according to the provisions of GB5211.15. Sample weight is 5g. 5.8 Determination of lead chromate
5.8.1 Reagents and materials
5.8.1.1 Nitric acid (GB626) solution: 1+5 solution. 5.8.1.2 Potassium iodide (GB1272) solution: 100g/L. 5.8.2 Instruments and equipment
5.8.2.1 Beaker.
5.8.2.2 Glass funnel.
Filter paper.
5.8.2.4 Balance: sensitivity 0.01g.
Wbzsoso, cOn5.8.3 Analysis steps
5.8.3.1 Sample
Weigh 0.5g of sample, accurate to 0.01g.
5.8.3.2 Determination
HG/T2249—91
Put 0.5g of the sample in a small beaker, add 10mL of cold nitric acid solution (5.8.1.1), stir vigorously, filter, then add 1mL of potassium iodide solution (5.8.1.2) to the filtrate, and observe the color of the filtrate. 5.8.4 Result indication
The presence of yellow crystals indicates the presence of lead chromate. 5.9 Determination of total calcium
5.9.1 Principle of the method
The organic extractant extracts iron, and the total calcium is titrated with potassium permanganate standard titration solution according to the principle of redox reaction. 5.9.2 Reagents and materials
5.9.2.1 Hydrochloric acid (GB622) solution: 1+1 solution. 5.9.2.2 Nitric acid: (GB626)
Methyl isobutyl ketone (HG3-1118): chemically pure. 5.9.2.4
Ammonia water (GB631): does not contain carbon dioxide. 5.9.2.5
Methyl red indicator: 1g/L ethanol solution, prepared according to GB603. 5.9.2.6
Acetic acid (GB676) solution: 99~100%. Ammonium oxalate (HG3-976) saturated solution.
Ammonium oxalate (HG3-976) solution: 1g/L. Sulfuric acid (GB625) solution: 1+4 solution. 5.9.2.9
5.9.2.10 Potassium permanganate standard titration solution: c(KMnO)=0.1mol/L Prepared and calibrated according to GB601. 5.9.3 Instruments and equipment
5.9.3.1 Beaker: 250mL.
5.9.3.2 Volumetric flask: 250mL.
5.9.3.3 Pipette: 100mL.
5.9.3.4 Pear-shaped separating funnel: 250mL. 5.9.3.5 Electric furnace: connected to autotransformer.
5.9.3.6 Balance: sensitivity 0.001g.
5.9.4 Analysis steps
5.9.4.1 Sample
Weigh 10g of sample, accurate to 0.001g.
5.9.4.2 Determination
Put the sample in a beaker, add 100mL of hydrochloric acid solution (5.9.2.1) containing 5mL of nitric acid (5.9.2.2), evaporate to dryness on an electric furnace (5.9.3.5), add 100mL of hydrochloric acid (5.9.2.1) and boil, after cooling, transfer to a 250mL volumetric flask and dilute it to the mark with hydrochloric acid (5.9.2.1), take 100mL of the solution, and evaporate to dryness. Add 60mL of hydrochloric acid (5.9.2.1) to dissolve it. After cooling, use 60mL of methyl isobutyl ketone (5.9.2.3) to extract the iron. If the solution is still colored, distill it for a second time until the solution is colorless. Add 2 drops of methyl red (5.9.2.5) indicator to the above solution, neutralize it with ammonia water (5.9.2.4), and then acidify the solution with a slightly excessive amount of acetic acid (5.9.2.6). Boil the solution and add 50mL of preheated ammonium oxalate solution (5.9.2.7) to continue boiling until the precipitate becomes granular. Let it stand for about 1 hour, filter it, and wash it with dilute ammonium oxalate solution (5.9.2.8) until the filtrate is free of chloride ions. Finally, use a minimum amount of cold water to wash away the ammonium oxalate.
W.HG/T2249—91
Use a glass rod to penetrate the tip of the filter paper and rinse the precipitate into the flask with hot water. Use about 30mL of warm sulfuric acid (5.9.2.9) to wash the filter paper and dilute the solution in the flask to 250mL. Titrate with potassium permanganate standard titration solution (5.9.2.10) at about 75℃ until it turns slightly red. The solution temperature should not be lower than 60℃ at the titration endpoint. 5.9.5 Expression of results
Expressed as the mass percentage of calcium oxide (CaO) X2, calculated according to formula (2): X100_V·c2X7.01
V2 : c2X0. 028 04
Wherein: V2——the volume of potassium permanganate standard titration solution consumed, mL; C2——the actual concentration of potassium permanganate standard titration solution, mol/L; m2——the mass of the sample, 8,
0.02804——the mass of calcium oxide equivalent to 1.00mL potassium permanganate standard titration solution Cc(kMnO,)=1.000mol/L), expressed in grams.
The measurement results shall be rounded to two decimal places.
5.10 Determination of color
Carry out in accordance with the provisions of GB1864. Take 1.0g of sample, add 1.0mL of refined linseed oil for the first time, grind for 200 turns (50X4), then add 0.4mL and grind for 25 turns.
5.11 Determination of relative tinting strength
Perform according to the provisions of GB5211.19. Preparation of pigment dispersion: take 1.0g of pigment and 1.5g of paint base. Preparation of dilute color paste: take 3.0g of white paste and 0.6g of pigment dispersion.
5.12 Determination of the presence of organic coloring matter
5.12.1 Reagents and materials
5.12.1.1 Ethanol (GB678): 95% (V/V). 5.12.1.2 Sodium hydroxide (GB629) solution: 40g/L ethanol solution. 5.12.1.3 Chloroform (GB682).
5.12.2 Apparatus and Equipment
5.12.2.1 Balance: Sensitivity 0.01 g.
5.12.2.2 Beaker.
5.12.2.3 Water bath.
5.12.3 Analysis Procedure
5.12.3.1 Sample
Weigh 2 g of sample (two portions) to the nearest 0.01 g. 5.12.3.2 Determination
Place one portion of the sample in a small beaker, add 25 mL of water, heat to boil, let it clarify, and pour off the supernatant. Add 25 mL of ethanol (5.12.1.1) to the residue (pigment), place in a water bath and boil, and pour off the supernatant as before. Add 25mL of sodium hydroxide solution (5.12.1.2) to the residue (pigment), boil it in a water bath, let it clarify, pour out the supernatant, and observe its color. If the supernatant contains pigment, filter it and observe it again. Put another sample in a small beaker, add 25mL of chloroform (5.12.1.3) and boil it in a water bath, let it clarify, pour out the supernatant, and observe its color. If the supernatant still contains pigment, filter it and observe it again. 5.12.4 Result Expression
If one of the above solutions is colored, it is considered that there is an organic colorant. 5
Wbzsoso，cOnHG/T2249—91
If the solutions are all colorless, there is no organic colorant. 6 Inspection Rules
6.1 The quality inspection department of the manufacturer shall be responsible for the inspection of iron oxide yellow products. The manufacturer shall ensure that the quality of all products shipped meets the technical requirements of this standard. Each batch of yellow iron oxide shipped out of the factory shall be accompanied by a product quality certificate. 6.2 Among the technical indicators of yellow iron oxide products, nine items, namely, iron content, volatile matter at 105℃, water-soluble matter, sieve residue, pH value of water extract, pH value of water suspension, oil absorption, color, and relative tinting strength, shall be used as factory inspection items. Each batch of products shall be inspected item by item according to the test methods specified in this standard.
6.3 Among the technical indicators of yellow iron oxide products, three items, namely, lead chromate, total calcium content, and the presence of organic coloring matter, shall be inspected once every six months according to the test methods specified in this standard.
6.4 Sampling method: in accordance with the relevant provisions of GB9285. 6.5 The quality inspection department shall inspect according to the technical requirements and test methods specified in this standard. If the results do not meet the requirements of this standard, it shall double the sampling from the original batch number according to the provisions of Article 6.4 and re-inspect the items that do not meet the requirements of this standard. If the re-inspection results still do not meet the requirements of this standard, the entire batch of products shall be considered unqualified. 6.6 The user has the right to inspect the product according to the technical requirements and test methods specified in this standard. If the two parties disagree with the inspection results and need to conduct arbitration, the arbitration institution shall be selected by the two parties through consultation. 7 Marking, packaging, transportation, purchase and storage
7.1 Marking
The packaging should be clearly marked, including the manufacturer's name, product name, trademark, production batch number, standard number, grade and net weight, and attached with a quality certificate.
7.2 Packaging
Iron oxide yellow pigment is packaged in plastic woven bags lined with plastic film bags or plastic-coated woven bags, with a net weight of 25kg per bag. 7.3 Transportation
During transportation and loading and unloading, it is required to load and unload gently, and collision and rupture should be prevented. It should be carried out in accordance with relevant transportation regulations. 7.4 Storage
Iron oxide yellow pigment is stored in a dry and ventilated place, and it is strictly forbidden to contact with acidic and alkaline items. According to the above storage conditions, the effective purchase and storage period of unopened pigment is three years.
Additional Notes:
This standard was proposed by the Science and Technology Department of 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 Iron Oxide Pigment Factory. The main drafters of this standard are Lai Shenghua and Yang Baogen. From the date of implementation of this standard, the original national standard GB1862-80 "Iron Oxide Yellow" will be invalid. 6
Free download of various US standard industry materials9 Determination of total calcium content
5.9.1 Principle of the method
The organic extractant extracts iron, and the total calcium content is titrated with potassium permanganate standard titration solution according to the principle of redox reaction. 5.9.2 Reagents and materials
5.9.2.1 Hydrochloric acid (GB622) solution: 1+1 solution. 5.9.2.2 Nitric acid: (GB626)
Methyl isobutyl ketone (HG3-1118): chemically pure. 5.9.2.4
Ammonia water (GB631): does not contain carbon dioxide. 5.9.2.5
Methyl red indicator: 1g/L ethanol solution, prepared according to GB603 regulations. 5.9.2.6
Acetic acid (GB676) solution: 99~100%. Ammonium oxalate (HG3-976) saturated solution.
Ammonium oxalate (HG3-976) solution: 1g/L. Sulfuric acid (GB625) solution: 1+4 solution. 5.9.2.9
5.9.2.10 Potassium permanganate standard titration solution: c(KMnO)=0.1mol/L Prepared and calibrated according to GB601. 5.9.3 Instruments and equipment
5.9.3.1 Beaker: 250mL.
5.9.3.2 Volumetric flask: 250mL.
5.9.3.3 Pipette: 100mL.
5.9.3.4 Pear-shaped separating funnel: 250mL. 5.9.3.5 Electric furnace: connected to autotransformer.
5.9.3.6 Balance: sensitivity 0.001g.
5.9.4 Analysis steps
5.9.4.1 Sample
Weigh 10g of the sample, accurate to 0.001g.
5.9.4.2 Determination
Put the sample in a beaker, add 100mL of hydrochloric acid solution (5.9.2.1) containing 5mL of nitric acid (5.9.2.2), evaporate to dryness on an electric stove (5.9.3.5), add 100mL of hydrochloric acid (5.9.2.1) and boil, after cooling, transfer to a 250mL volumetric flask and dilute it to the mark with hydrochloric acid (5.9.2.1), take 100mL of the solution, and evaporate to dryness. Add 60mL of hydrochloric acid (5.9.2.1) to dissolve it. After cooling, use 60mL of methyl isobutyl ketone (5.9.2.3) to extract the iron. If the solution is still colored, distill it for a second time until the solution is colorless. Add 2 drops of methyl red (5.9.2.5) indicator to the above solution, neutralize it with ammonia water (5.9.2.4), and then acidify the solution with a slightly excessive amount of acetic acid (5.9.2.6). Boil the solution and add 50mL of preheated ammonium oxalate solution (5.9.2.7) to continue boiling until the precipitate becomes granular. Let it stand for about 1 hour, filter it, and wash it with dilute ammonium oxalate solution (5.9.2.8) until the filtrate is free of chloride ions. Finally, use a minimum amount of cold water to wash away the ammonium oxalate.
W.HG/T2249—91
Use a glass rod to penetrate the tip of the filter paper and rinse the precipitate into the flask with hot water. Use about 30mL of warm sulfuric acid (5.9.2.9) to wash the filter paper and dilute the solution in the flask to 250mL. Titrate with potassium permanganate standard titration solution (5.9.2.10) at about 75℃ until it turns slightly red. The solution temperature should not be lower than 60℃ at the titration end point. 5.9.5 Expression of results
Expressed as the mass percentage of calcium oxide (CaO) X2, calculated according to formula (2): X100_V·c2X7.01
V2 : c2X0. 028 04
Wherein: V2——the volume of potassium permanganate standard titration solution consumed, mL; C2——the actual concentration of potassium permanganate standard titration solution, mol/L; m2——the mass of the sample, 8,
0.02804——the mass of calcium oxide equivalent to 1.00mL potassium permanganate standard titration solution Cc(kMnO,)=1.000mol/L), expressed in grams.
The measurement results shall be rounded to two decimal places.
5.10 Determination of color
Carry out in accordance with the provisions of GB1864. Take 1.0g of sample, add 1.0mL of refined linseed oil for the first time, grind for 200 turns (50X4), then add 0.4mL and grind for 25 turns.
5.11 Determination of relative tinting strength
Perform according to the provisions of GB5211.19. Preparation of pigment dispersion: take 1.0g of pigment and 1.5g of paint base. Preparation of dilute color paste: take 3.0g of white paste and 0.6g of pigment dispersion.
5.12 Determination of the presence of organic coloring matter
5.12.1 Reagents and materials
5.12.1.1 Ethanol (GB678): 95% (V/V). 5.12.1.2 Sodium hydroxide (GB629) solution: 40g/L ethanol solution. 5.12.1.3 Chloroform (GB682).
5.12.2 Apparatus and Equipment
5.12.2.1 Balance: Sensitivity 0.01 g.
5.12.2.2 Beaker.
5.12.2.3 Water bath.
5.12.3 Analysis Procedure
5.12.3.1 Sample
Weigh 2 g of sample (two portions) to the nearest 0.01 g. 5.12.3.2 Determination
Place one portion of the sample in a small beaker, add 25 mL of water, heat to boil, let it clarify, and pour off the supernatant. Add 25 mL of ethanol (5.12.1.1) to the residue (pigment), place in a water bath and boil, and pour off the supernatant as before. Add 25mL of sodium hydroxide solution (5.12.1.2) to the residue (pigment), boil it in a water bath, let it clarify, pour out the supernatant, and observe its color. If the supernatant contains pigment, filter it and observe it again. Put another sample in a small beaker, add 25mL of chloroform (5.12.1.3) and boil it in a water bath, let it clarify, pour out the supernatant, and observe its color. If the supernatant still contains pigment, filter it and observe it again. 5.12.4 Result Expression
If one of the above solutions is colored, it is considered that there is organic coloring matter. 5
Wbzsoso，cOnHG/T2249—91
If the solutions are all colorless, there is no organic coloring matter. 6 Inspection Rules
6.1 The quality inspection department of the manufacturer shall be responsible for the inspection of iron oxide yellow products. The manufacturer shall ensure that the quality of all products shipped meets the technical requirements of this standard. Each batch of yellow iron oxide shipped out of the factory shall be accompanied by a product quality certificate. 6.2 Among the technical indicators of yellow iron oxide products, nine items, namely, iron content, volatile matter at 105°C, water-soluble matter, sieve residue, pH value of water extract, pH value of water suspension, oil absorption, color, and relative tinting strength, shall be used as factory inspection items. Each batch of products shall be inspected item by item according to the test methods specified in this standard.
6.3 Among the technical indicators of yellow iron oxide products, three items, namely, lead chromate, total calcium content, and the presence of organic coloring matter, shall be inspected once every six months according to the test methods specified in this standard.
6.4 Sampling method: in accordance with the relevant provisions of GB9285. 6.5 The quality inspection department shall inspect according to the technical requirements and test methods specified in this standard. If the results do not meet the requirements of this standard, it shall double the sampling from the original batch number according to the provisions of Article 6.4 and re-inspect the items that do not meet the requirements of this standard. If the re-inspection results still do not meet the requirements of this standard, the entire batch of products shall be considered unqualified. 6.6 The user has the right to inspect the product according to the technical requirements and test methods specified in this standard. If the two parties disagree with the inspection results and need to conduct arbitration, the arbitration institution shall be selected by the two parties through consultation. 7 Marking, packaging, transportation, purchase and storage
7.1 Marking
The packaging should be clearly marked, including the manufacturer's name, product name, trademark, production batch number, standard number, grade and net weight, and attached with a quality certificate.
7.2 Packaging
Iron oxide yellow pigment is packaged in plastic woven bags lined with plastic film bags or plastic-coated woven bags, with a net weight of 25kg per bag. 7.3 Transportation
During transportation and loading and unloading, it is required to load and unload gently, and collision and rupture should be prevented. It should be carried out in accordance with relevant transportation regulations. 7.4 Storage
Iron oxide yellow pigment is stored in a dry and ventilated place, and it is strictly forbidden to contact with acidic and alkaline items. According to the above storage conditions, the effective purchase and storage period of unopened pigment is three years.
Additional Notes:
This standard was proposed by the Science and Technology Department of 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 Iron Oxide Pigment Factory. The main drafters of this standard are Lai Shenghua and Yang Baogen. From the date of implementation of this standard, the original national standard GB1862-80 "Iron Oxide Yellow" will be invalid. 6
Free download of various US standard industry materials9 Determination of total calcium content
5.9.1 Principle of the method
The organic extractant extracts iron, and the total calcium content is titrated with potassium permanganate standard titration solution according to the principle of redox reaction. 5.9.2 Reagents and materials
5.9.2.1 Hydrochloric acid (GB622) solution: 1+1 solution. 5.9.2.2 Nitric acid: (GB626)
Methyl isobutyl ketone (HG3-1118): chemically pure. 5.9.2.4
Ammonia water (GB631): does not contain carbon dioxide. 5.9.2.5
Methyl red indicator: 1g/L ethanol solution, prepared according to GB603 regulations. 5.9.2.6
Acetic acid (GB676) solution: 99~100%. Ammonium oxalate (HG3-976) saturated solution.
Ammonium oxalate (HG3-976) solution: 1g/L. Sulfuric acid (GB625) solution: 1+4 solution. 5.9.2.9
5.9.2.10 Potassium permanganate standard titration solution: c(KMnO)=0.1mol/L Prepared and calibrated according to GB601. 5.9.3 Instruments and equipment
5.9.3.1 Beaker: 250mL.
5.9.3.2 Volumetric flask: 250mL.
5.9.3.3 Pipette: 100mL.
5.9.3.4 Pear-shaped separating funnel: 250mL. 5.9.3.5 Electric furnace: connected to autotransformer.
5.9.3.6 Balance: sensitivity 0.001g.
5.9.4 Analysis steps
5.9.4.1 Sample
Weigh 10g of the sample, accurate to 0.001g.
5.9.4.2 Determination
Put the sample in a beaker, add 100mL of hydrochloric acid solution (5.9.2.1) containing 5mL of nitric acid (5.9.2.2), evaporate to dryness on an electric stove (5.9.3.5), add 100mL of hydrochloric acid (5.9.2.1) and boil, after cooling, transfer to a 250mL volumetric flask and dilute it to the mark with hydrochloric acid (5.9.2.1), take 100mL of the solution, and evaporate to dryness. Add 60mL of hydrochloric acid (5.9.2.1) to dissolve it. After cooling, use 60mL of methyl isobutyl ketone (5.9.2.3) to extract the iron. If the solution is still colored, distill it for a second time until the solution is colorless. Add 2 drops of methyl red (5.9.2.5) indicator to the above solution, neutralize it with ammonia water (5.9.2.4), and then acidify the solution with a slightly excessive amount of acetic acid (5.9.2.6). Boil the solution and add 50mL of preheated ammonium oxalate solution (5.9.2.7) to continue boiling until the precipitate becomes granular. Let it stand for about 1 hour, filter it, and wash it with dilute ammonium oxalate solution (5.9.2.8) until the filtrate is free of chloride ions. Finally, use a minimum amount of cold water to wash away the ammonium oxalate.
W.HG/T2249—91
Use a glass rod to penetrate the tip of the filter paper and rinse the precipitate into the flask with hot water. Use about 30mL of warm sulfuric acid (5.9.2.9) to wash the filter paper and dilute the solution in the flask to 250mL. Titrate with potassium permanganate standard titration solution (5.9.2.10) at about 75℃ until it turns slightly red. The solution temperature should not be lower than 60℃ at the titration endpoint. 5.9.5 Expression of results
Expressed as the mass percentage of calcium oxide (CaO) X2, calculated according to formula (2): X100_V·c2X7.01
V2 : c2X0. 028 04
Wherein: V2——the volume of potassium permanganate standard titration solution consumed, mL; C2——the actual concentration of potassium permanganate standard titration solution, mol/L; m2——the mass of the sample, 8,
0.02804——the mass of calcium oxide equivalent to 1.00mL potassium permanganate standard titration solution Cc(kMnO,)=1.000mol/L), expressed in grams.
The measurement results shall be rounded to two decimal places.
5.10 Determination of color
Carry out in accordance with the provisions of GB1864. Take 1.0g of sample, add 1.0mL of refined linseed oil for the first time, grind for 200 turns (50X4), then add 0.4mL and grind for 25 turns.
5.11 Determination of relative tinting strength
Perform according to the provisions of GB5211.19. Preparation of pigment dispersion: take 1.0g of pigment and 1.5g of paint base. Preparation of dilute color paste: take 3.0g of white paste and 0.6g of pigment dispersion.
5.12 Determination of the presence of organic coloring matter
5.12.1 Reagents and materials
5.12.1.1 Ethanol (GB678): 95% (V/V). 5.12.1.2 Sodium hydroxide (GB629) solution: 40g/L ethanol solution. 5.12.1.3 Chloroform (GB682).
5.12.2 Apparatus and Equipment
5.12.2.1 Balance: Sensitivity 0.01 g.
5.12.2.2 Beaker.
5.12.2.3 Water bath.
5.12.3 Analysis Procedure
5.12.3.1 Sample
Weigh 2 g of sample (two portions) to the nearest 0.01 g. 5.12.3.2 Determination
Place one portion of the sample in a small beaker, add 25 mL of water, heat to boil, let it clarify, and pour off the supernatant. Add 25 mL of ethanol (5.12.1.1) to the residue (pigment), place in a water bath and boil, and pour off the supernatant as before. Add 25mL of sodium hydroxide solution (5.12.1.2) to the residue (pigment), boil it in a water bath, let it clarify, pour out the supernatant, and observe its color. If the supernatant contains pigment, filter it and observe it again. Put another sample in a small beaker, add 25mL of chloroform (5.12.1.3) and boil it in a water bath, let it clarify, pour out the supernatant, and observe its color. If the supernatant still contains pigment, filter it and observe it again. 5.12.4 Result Expression
If one of the above solutions is colored, it is considered that there is organic coloring matter. 5
Wbzsoso，cOnHG/T2249—91
If the solutions are all colorless, there is no organic coloring matter. 6 Inspection Rules
6.1 The quality inspection department of the manufacturer shall be responsible for the inspection of iron oxide yellow products. The manufacturer shall ensure that the quality of all products shipped meets the technical requirements of this standard. Each batch of yellow iron oxide shipped out of the factory shall be accompanied by a product quality certificate. 6.2 Among the technical indicators of yellow iron oxide products, nine items, namely, iron content, volatile matter at 105°C, water-soluble matter, sieve residue, pH value of water extract, pH value of water suspension, oil absorption, color, and relative tinting strength, shall be used as factory inspection items. Each batch of products shall be inspected item by item according to the test methods specified in this standard.
6.3 Among the technical indicators of yellow iron oxide products, three items, namely, lead chromate, total calcium content, and the presence of organic coloring matter, shall be inspected once every six months according to the test methods specified in this standard.
6.4 Sampling method: in accordance with the relevant provisions of GB9285. 6.5 The quality inspection department shall inspect according to the technical requirements and test methods specified in this standard. If the results do not meet the requirements of this standard, it shall double the sampling from the original batch number according to the provisions of Article 6.4 and re-inspect the items that do not meet the requirements of this standard. If the re-inspection results still do not meet the requirements of this standard, the entire batch of products shall be considered unqualified. 6.6 The user has the right to inspect the product according to the technical requirements and test methods specified in this standard. If the two parties disagree with the inspection results and need to conduct arbitration, the arbitration institution shall be selected by the two parties through consultation. 7 Marking, packaging, transportation, purchase and storage
7.1 Marking
The packaging should be clearly marked, including the manufacturer's name, product name, trademark, production batch number, standard number, grade and net weight, and attached with a quality certificate.
7.2 Packaging
Iron oxide yellow pigment is packaged in plastic woven bags lined with plastic film bags or plastic-coated woven bags, with a net weight of 25kg per bag. 7.3 Transportation
During transportation and loading and unloading, it is required to load and unload gently, and collision and rupture should be prevented. It should be carried out in accordance with relevant transportation regulations. 7.4 Storage
Iron oxide yellow pigment is stored in a dry and ventilated place, and it is strictly forbidden to contact with acidic and alkaline items. According to the above storage conditions, the effective purchase and storage period of unopened pigment is three years.
Additional Notes:
This standard was proposed by the Science and Technology Department of 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 Iron Oxide Pigment Factory. The main drafters of this standard are Lai Shenghua and Yang Baogen. From the date of implementation of this standard, the original national standard GB1862-80 "Iron Oxide Yellow" will be invalid. 6
Free download of various US standard industry materials1 Principle of the method
The organic extractant extracts iron, and according to the principle of redox reaction, the total calcium is titrated with potassium permanganate standard titration solution. 5.9.2 Reagents and materialsbzxz.net
5.9.2.1 Hydrochloric acid (GB622) solution: 1+1 solution. 5.9.2.2 Nitric acid: (GB626)
Methyl isobutyl ketone (HG3-1118): chemically pure. 5.9.2.4
Ammonia water (GB631): does not contain carbon dioxide. 5.9.2.5
Methyl red indicator: 1g/L ethanol solution, prepared according to GB603. 5.9.2.6
Acetic acid (GB676) solution: 99~100%. Ammonium oxalate (HG3-976) saturated solution.
Ammonium oxalate (HG3-976) solution: 1g/L. Sulfuric acid (GB625) solution: 1+4 solution. 5.9.2.9
5.9.2.10 Potassium permanganate standard titration solution: c(KMnO)=0.1mol/L Prepared and calibrated according to GB601. 5.9.3 Instruments and equipment
5.9.3.1 Beaker: 250mL.
5.9.3.2 Volumetric flask: 250mL.
5.9.3.3 Pipette: 100mL.
5.9.3.4 Pear-shaped separating funnel: 250mL. 5.9.3.5 Electric furnace: connected to autotransformer.
5.9.3.6 Balance: sensitivity 0.001g.
5.9.4 Analysis steps
5.9.4.1 Sample
Weigh 10g of the sample, accurate to 0.001g.
5.9.4.2 Determination
Put the sample in a beaker, add 100mL of hydrochloric acid solution (5.9.2.1) containing 5mL of nitric acid (5.9.2.2), evaporate to dryness on an electric stove (5.9.3.5), add 100mL of hydrochloric acid (5.9.2.1) and boil, after cooling, transfer to a 250mL volumetric flask and dilute it to the mark with hydrochloric acid (5.9.2.1), take 100mL of the solution, and evaporate to dryness. Add 60mL of hydrochloric acid (5.9.2.1) to dissolve it. After cooling, use 60mL of methyl isobutyl ketone (5.9.2.3) to extract the iron. If the solution is still colored, distill it for a second time until the solution is colorless. Add 2 drops of methyl red (5.9.2.5) indicator to the above solution, neutralize it with ammonia water (5.9.2.4), and then acidify the solution with a slightly excessive amount of acetic acid (5.9.2.6). Boil the solution and add 50mL of preheated ammonium oxalate solution (5.9.2.7) to continue boiling until the precipitate becomes granular. Let it stand for about 1 hour, filter it, and wash it with dilute ammonium oxalate solution (5.9.2.8) until the filtrate is free of chloride ions. Finally, use a minimum amount of cold water to wash away the ammonium oxalate.
W.HG/T2249—91
Use a glass rod to penetrate the tip of the filter paper and rinse the precipitate into the flask with hot water. Use about 30mL of warm sulfuric acid (5.9.2.9) to wash the filter paper and dilute the solution in the flask to 250mL. Titrate with potassium permanganate standard titration solution (5.9.2.10) at about 75℃ until it turns slightly red. The solution temperature should not be lower than 60℃ at the titration endpoint. 5.9.5 Expression of results
Expressed as the mass percentage of calcium oxide (CaO) X2, calculated according to formula (2): X100_V·c2X7.01
V2 : c2X0. 028 04
Wherein: V2——the volume of potassium permanganate standard titration solution consumed, mL; C2——the actual concentration of potassium permanganate standard titration solution, mol/L; m2——the mass of the sample, 8,
0.02804——the mass of calcium oxide equivalent to 1.00mL potassium permanganate standard titration solution Cc(kMnO,)=1.000mol/L), expressed in grams.
The measurement results shall be rounded to two decimal places.
5.10 Determination of color
Carry out in accordance with the provisions of GB1864. Take 1.0g of sample, add 1.0mL of refined linseed oil for the first time, grind for 200 turns (50X4), then add 0.4mL and grind for 25 turns.
5.11 Determination of relative tinting strength
Perform according to the provisions of GB5211.19. Preparation of pigment dispersion: take 1.0g of pigment and 1.5g of paint base. Preparation of dilute color paste: take 3.0g of white paste and 0.6g of pigment dispersion.
5.12 Determination of the presence of organic coloring matter
5.12.1 Reagents and materials
5.12.1.1 Ethanol (GB678): 95% (V/V). 5.12.1.2 Sodium hydroxide (GB629) solution: 40g/L ethanol solution. 5.12.1.3 Chloroform (GB682).
5.12.2 Apparatus and Equipment
5.12.2.1 Balance: Sensitivity 0.01 g.
5.12.2.2 Beaker.
5.12.2.3 Water bath.
5.12.3 Analysis Procedure
5.12.3.1 Sample
Weigh 2 g of sample (two portions) to the nearest 0.01 g. 5.12.3.2 Determination
Place one portion of the sample in a small beaker, add 25 mL of water, heat to boil, let it clarify, and pour off the supernatant. Add 25 mL of ethanol (5.12.1.1) to the residue (pigment), place in a water bath and boil, and pour off the supernatant as before. Add 25mL of sodium hydroxide solution (5.12.1.2) to the residue (pigment), boil it in a water bath, let it clarify, pour out the supernatant, and observe its color. If the supernatant contains pigment, filter it and observe it again. Put another sample in a small beaker, add 25mL of chloroform (5.12.1.3) and boil it in a water bath, let it clarify, pour out the supernatant, and observe its color. If the supernatant still contains pigment, filter it and observe it again. 5.12.4 Result Expression
If one of the above solutions is colored, it is considered that there is an organic colorant. 5
Wbzsoso，cOnHG/T2249—91
If the solutions are all colorless, there is no organic colorant. 6 Inspection Rules
6.1 The quality inspection department of the manufacturer shall be responsible for the inspection of iron oxide yellow products. The manufacturer shall ensure that the quality of all products shipped meets the technical requirements of this standard. Each batch of yellow iron oxide shipped out of the factory shall be accompanied by a product quality certificate. 6.2 Among the technical indicators of yellow iron oxide products, nine items, namely, iron content, volatile matter at 105℃, water-soluble matter, sieve residue, pH value of water extract, pH value of water suspension, oil absorption, color, and relative tinting strength, shall be used as factory inspection items. Each batch of products shall be inspected item by item according to the test methods specified in this standard.
6.3 Among the technical indicators of yellow iron oxide products, three items, namely, lead chromate, total calcium content, and the presence of organic coloring matter, shall be inspected once every six months according to the test methods specified in this standard.
6.4 Sampling method: in accordance with the relevant provisions of GB9285. 6.5 The quality inspection department shall inspect according to the technical requirements and test methods specified in this standard. If the results do not meet the requirements of this standard, it shall double the sampling from the original batch number according to the provisions of Article 6.4 and re-inspect the items that do not meet the requirements of this standard. If the re-inspection results still do not meet the requirements of this standard, the entire batch of products shall be considered unqualified. 6.6 The user has the right to inspect the product according to the technical requirements and test methods specified in this standard. If the two parties disagree with the inspection results and need to conduct arbitration, the arbitration institution shall be selected by the two parties through consultation. 7 Marking, packaging, transportation, purchase and storage
7.1 Marking
The packaging should be clearly marked, including the manufacturer's name, product name, trademark, production batch number, standard number, grade and net weight, and attached with a quality certificate.
7.2 Packaging
Iron oxide yellow pigment is packaged in plastic woven bags lined with plastic film bags or plastic-coated woven bags, with a net weight of 25kg per bag. 7.3 Transportation
During transportation and loading and unloading, it is required to load and unload gently, and collision and rupture should be prevented. It should be carried out in accordance with relevant transportation regulations. 7.4 Storage
Iron oxide yellow pigment is stored in a dry and ventilated place, and it is strictly forbidden to contact with acidic and alkaline items. According to the above storage conditions, the effective purchase and storage period of unopened pigment is three years.
Additional Notes:
This standard was proposed by the Science and Technology Department of 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 Iron Oxide Pigment Factory. The main drafters of this standard are Lai Shenghua and Yang Baogen. From the date of implementation of this standard, the original national standard GB1862-80 "Iron Oxide Yellow" will be invalid. 6
Free download of various US standard industry materials1 Principle of the method
The organic extractant extracts iron, and according to the principle of redox reaction, the total calcium is titrated with potassium permanganate standard titration solution. 5.9.2 Reagents and materials
5.9.2.1 Hydrochloric acid (GB622) solution: 1+1 solution. 5.9.2.2 Nitric acid: (GB626)
Methyl isobutyl ketone (HG3-1118): chemically pure. 5.9.2.4
Ammonia water (GB631): does not contain carbon dioxide. 5.9.2.5
Methyl red indicator: 1g/L ethanol solution, prepared according to GB603. 5.9.2.6
Acetic acid (GB676) solution: 99~100%. Ammonium oxalate (HG3-976) saturated solution.
Ammonium oxalate (HG3-976) solution: 1g/L. Sulfuric acid (GB625) solution: 1+4 solution. 5.9.2.9
5.9.2.10 Potassium permanganate standard titration solution: c(KMnO)=0.1mol/L Prepared and calibrated according to GB601. 5.9.3 Instruments and equipment
5.9.3.1 Beaker: 250mL.
5.9.3.2 Volumetric flask: 250mL.
5.9.3.3 Pipette: 100mL.
5.9.3.4 Pear-shaped separating funnel: 250mL. 5.9.3.5 Electric furnace: connected to autotransformer.
5.9.3.6 Balance: sensitivity 0.001g.
5.9.4 Analysis steps
5.9.4.1 Sample
Weigh 10g of the sample, accurate to 0.001g.
5.9.4.2 Determination
Put the sample in a beaker, add 100mL of hydrochloric acid solution (5.9.2.1) containing 5mL of nitric acid (5.9.2.2), evaporate to dryness on an electric stove (5.9.3.5), add 100mL of hydrochloric acid (5.9.2.1) and boil, after cooling, transfer to a 250mL volumetric flask and dilute it to the mark with hydrochloric acid (5.9.2.1), take 100mL of the solution, and evaporate to dryness. Add 60mL of hydrochloric acid (5.9.2.1) to dissolve it. After cooling, use 60mL of methyl isobutyl ketone (5.9.2.3) to extract the iron. If the solution is still colored, distill it for a second time until the solution is colorless. Add 2 drops of methyl red (5.9.2.5) indicator to the above solution, neutralize it with ammonia water (5.9.2.4), and then acidify the solution with a slightly excessive amount of acetic acid (5.9.2.6). Boil the solution and add 50mL of preheated ammonium oxalate solution (5.9.2.7) to continue boiling until the precipitate becomes granular. Let it stand for about 1 hour, filter it, and wash it with dilute ammonium oxalate solution (5.9.2.8) until the filtrate is free of chloride ions. Finally, use a minimum amount of cold water to wash away the ammonium oxalate.
W.HG/T2249—91
Use a glass rod to penetrate the tip of the filter paper and rinse the precipitate into the flask with hot water. Use about 30mL of warm sulfuric acid (5.9.2.9) to wash the filter paper and dilute the solution in the flask to 250mL. Titrate with potassium permanganate standard titration solution (5.9.2.10) at about 75℃ until it turns slightly red. The solution temperature should not be lower than 60℃ at the titration endpoint. 5.9.5 Expression of results
Expressed as the mass percentage of calcium oxide (CaO) X2, calculated according to formula (2): X100_V·c2X7.01
V2 : c2X0. 028 04
Wherein: V2——the volume of potassium permanganate standard titration solution consumed, mL; C2——the actual concentration of potassium permanganate standard titration solution, mol/L; m2——the mass of the sample, 8,
0.02804——the mass of calcium oxide equivalent to 1.00mL potassium permanganate standard titration solution Cc(kMnO,)=1.000mol/L), expressed in grams.
The measurement results shall be rounded to two decimal places.
5.10 Determination of color
Carry out in accordance with the provisions of GB1864. Take 1.0g of sample, add 1.0mL of refined linseed oil for the first time, grind for 200 turns (50X4), then add 0.4mL and grind for 25 turns.
5.11 Determination of relative tinting strength
Perform according to the provisions of GB5211.19. Preparation of pigment dispersion: take 1.0g of pigment and 1.5g of paint base. Preparation of dilute color paste: take 3.0g of white paste and 0.6g of pigment dispersion.
5.12 Determination of the presence of organic coloring matter
5.12.1 Reagents and materials
5.12.1.1 Ethanol (GB678): 95% (V/V). 5.12.1.2 Sodium hydroxide (GB629) solution: 40g/L ethanol solution. 5.12.1.3 Chloroform (GB682).
5.12.2 Apparatus and Equipment
5.12.2.1 Balance: Sensitivity 0.01 g.
5.12.2.2 Beaker.
5.12.2.3 Water bath.
5.12.3 Analysis Procedure
5.12.3.1 Sample
Weigh 2 g of sample (two portions) to the nearest 0.01 g. 5.12.3.2 Determination
Place one portion of the sample in a small beaker, add 25 mL of water, heat to boil, let it clarify, and pour off the supernatant. Add 25 mL of ethanol (5.12.1.1) to the residue (pigment), place in a water bath and boil, and pour off the supernatant as before. Add 25mL of sodium hydroxide solution (5.12.1.2) to the residue (pigment), boil it in a water bath, let it clarify, pour out the supernatant, and observe its color. If the supernatant contains pigment, filter it and observe it again. Put another sample in a small beaker, add 25mL of chloroform (5.12.1.3) and boil it in a water bath, let it clarify, pour out the supernatant, and observe its color. If the supernatant still contains pigment, filter it and observe it again. 5.12.4 Result Expression
If one of the above solutions is colored, it is considered that there is an organic colorant. 5
Wbzsoso，cOnHG/T2249—91
If the solutions are all colorless, there is no organic colorant. 6 Inspection Rules
6.1 The quality inspection department of the manufacturer shall be responsible for the inspection of iron oxide yellow products. The manufacturer shall ensure that the quality of all products shipped meets the technical requirements of this standard. Each batch of yellow iron oxide shipped out of the factory shall be accompanied by a product quality certificate. 6.2 Among the technical indicators of yellow iron oxide products, nine items, namely, iron content, volatile matter at 105℃, water-soluble matter, sieve residue, pH value of water extract, pH value of water suspension, oil absorption, color, and relative tinting strength, shall be used as factory inspection items. Each batch of products shall be inspected item by item according to the test methods specified in this standard.
6.3 Among the technical indicators of yellow iron oxide products, three items, namely, lead chromate, total calcium content, and the presence of organic coloring matter, shall be inspected once every six months according to the test methods specified in this standard.
6.4 Sampling method: in accordance with the relevant provisions of GB9285. 6.5 The quality inspection department shall inspect according to the technical requirements and test methods specified in this standard. If the results do not meet the requirements of this standard, it shall double the sampling from the original batch number according to the provisions of Article 6.4 and re-inspect the items that do not meet the requirements of this standard. If the re-inspection results still do not meet the requirements of this standard, the entire batch of products shall be considered unqualified. 6.6 The user has the right to inspect the product according to the technical requirements and test methods specified in this standard. If the two parties disagree with the inspection results and need to conduct arbitration, the arbitration institution shall be selected by the two parties through consultation. 7 Marking, packaging, transportation, purchase and storage
7.1 Marking
The packaging should be clearly marked, including the manufacturer's name, product name, trademark, production batch number, standard number, grade and net weight, and attached with a quality certificate.
7.2 Packaging
Iron oxide yellow pigment is packaged in plastic woven bags lined with plastic film bags or plastic-coated woven bags, with a net weight of 25kg per bag. 7.3 Transportation
During transportation and loading and unloading, it is required to load and unload gently, and collision and rupture should be prevented. It should be carried out in accordance with relevant transportation regulations. 7.4 Storage
Iron oxide yellow pigment is stored in a dry and ventilated place, and it is strictly forbidden to contact with acidic and alkaline items. According to the above storage conditions, the effective purchase and storage period of unopened pigment is three years.
Additional Notes:
This standard was proposed by the Science and Technology Department of 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 Iron Oxide Pigment Factory. The main drafters of this standard are Lai Shenghua and Yang Baogen. From the date of implementation of this standard, the original national standard GB1862-80 "Iron Oxide Yellow" will be invalid. 6
Free download of various US standard industry materials1 Hydrochloric acid (GB622) solution: 1+1 solution. 5.9.2.2 Nitric acid: (GB626)
Methyl isobutyl ketone (HG3-1118): chemically pure. 5.9.2.4
Ammonia water (GB631): does not contain carbon dioxide. 5.9.2.5
Methyl red indicator: 1g/L ethanol solution, prepared according to GB603. 5.9.2.6
Acetic acid (GB676) solution: 99~100%. Ammonium oxalate (HG3-976) saturated solution.
Ammonium oxalate (HG3-976) solution: 1g/L. Sulfuric acid (GB625) solution: 1+4 solution. 5.9.2.9
5.9.2.10 Potassium permanganate standard titration solution: c (KMnO) = 0.1 mol/L Prepare and calibrate according to GB601. 5.9.3 Instruments and equipment
5.9.3.1 Beaker: 250 mL.
5.9.3.2 Volumetric flask: 250 mL.
5.9.3.3 Pipette: 100 mL.
5.9.3.4 Pear-shaped separating funnel: 250 mL. 5.9.3.5 Electric furnace: connected to autotransformer.
5.9.3.6 Balance: sensitivity 0.001 g.
5.9.4 Analysis steps
5.9.4.1 Sample
Weigh 10 g of sample to an accuracy of 0.001 g.
5.9.4.2 Determination
Put the sample in a beaker, add 100mL of hydrochloric acid solution (5.9.2.1) containing 5mL of nitric acid (5.9.2.2), evaporate to dryness on an electric furnace (5.9.3.5), add 100mL of hydrochloric acid (5.9.2.1) and boil, after cooling, transfer to a 250mL volumetric flask and dilute to scale with hydrochloric acid (5.9.2.1), take 100mL of the solution, and evaporate to dryness. Add 60mL of hydrochloric acid (5.9.2.1) to dissolve it, cool it, and extract the iron with 60mL of methyl isobutyl ketone (5.9.2.3). If the solution is still colored, evaporate it a second time until the solution is colorless. Add 2 drops of methyl red (5.9.2.5) indicator to the above solution, neutralize with ammonia water (5.9.2.4), and then acidify the solution with a slightly excess of acetic acid (5.9.2.6). Boil the solution and add 50 mL of preheated ammonium oxalate solution (5.9.2.7) and continue boiling until the precipitate becomes granular. Let it stand for about 1 hour, filter, and wash with dilute ammonium oxalate solution (5.9.2.8) until the filtrate is free of chloride ions. Finally, wash away the ammonium oxalate with a minimum amount of cold water.
W.HG/T2249—91
Use a glass rod to penetrate the tip of the filter paper and rinse the precipitate into the flask with hot water. Use about 30mL of warm sulfuric acid (5.9.2.9) to wash the filter paper and dilute the solution in the flask to 250mL. Titrate with potassium permanganate standard titration solution (5.9.2.10) at about 75℃ until it turns slightly red. The solution temperature should not be lower than 60℃ at the titration endpoint. 5.9.5 Expression of results
Expressed as the mass percentage of calcium oxide (CaO) X2, calculated according to formula (2): X100_V·c2X7.01
V2 : c2X0. 028 04
Wherein: V2——the volume of potassium permanganate standard titration solution consumed, mL; C2——the actual concentration of potassium permanganate standard titration solution, mol/L; m2——the mass of the sample, 8,
0.02804——the mass of calcium oxide equivalent to 1.00mL potassium permanganate standard titration solution Cc(kMnO,)=1.000mol/L), expressed in grams.
The measurement results shall be rounded to two decimal places.
5.10 Determination of color
Carry out in accordance with the provisions of GB1864. Take 1.0g of sample, add 1.0mL of refined linseed oil for the first time, grind for 200 turns (50X4), then add 0.4mL and grind for 25 turns.
5.11 Determination of relative tinting strength
Perform according to the provisions of GB5211.19. Preparation of pigment dispersion: take 1.0g of pigment and 1.5g of paint base. Preparation of dilute color paste: take 3.0g of white paste and 0.6g of pigment dispersion.
5.12 Determination of the presence of organic coloring matter
5.12.1 Reagents and materials
5.12.1.1 Ethanol (GB678): 95% (V/V). 5.12.1.2 Sodium hydroxide (GB629) solution: 40g/L ethanol solution. 5.12.1.3 Chloroform (GB682).
5.12.2 Apparatus and Equipment
5.12.2.1 Balance: Sensitivity 0.01 g.
5.12.2.2 Beaker.
5.12.2.3 Water bath.
5.12.3 Analysis Procedure
5.12.3.1 Sample
Weigh 2 g of sample (two portions) to the nearest 0.01 g. 5.12.3.2 Determination
Place one portion of the sample in a small beaker, add 25 mL of water, heat to boil, let it clarify, and pour off the supernatant. Add 25 mL of ethanol (5.12.1.1) to the residue (pigment), place in a water bath and boil, and pour off the supernatant as before. Add 25mL of sodium hydroxide solution (5.12.1.2) to the residue (pigment), boil it in a water bath, let it clarify, pour out the supernatant, and observe its color. If the supernatant contains pigment, filter it and observe it again. Put another sample in a small beaker, add 25mL of chloroform (5.12.1.3) and boil it in a water bath, let it clarify, pour out the supernatant, and observe its color. If the supernatant still contains pigment, filter it and observe it again. 5.12.4 Result Expression
If one of the above solutions is colored, it is considered that there is an organic colorant. 5
Wbzsoso，cOnHG/T2249—91
If the solutions are all colorless, there is no organic colorant. 6 Inspection Rules
6.1 The quality inspection department of the manufacturer shall be responsible for the inspection of iron oxide yellow products. The manufacturer shall ensure that the quality of all products shipped meets the technical requirements of this standard. Each batch of yellow iron oxide shipped out of the factory shall be accompanied by a product quality certificate. 6.2 Among the technical indicators of yellow iron oxide products, nine items, namely, iron content, volatile matter at 105℃, water-soluble matter, sieve residue, pH value of water extract, pH value of water suspension, oil absorption, color, and relative tinting strength, shall be used as factory inspection items. Each batch of products shall be inspected item by item according to the test methods specified in this standard.
6.3 Among the technical indicators of yellow iron oxide products, three items, namely, lead chromate, total calcium content, and the presence of organic coloring matter, shall be inspected once every six months according to the test methods specified in this standard.
6.4 Sampling method: in accordance with the relevant provisions of GB9285. 6.5 The quality inspection department shall inspect according to the technical requirements and test methods specified in this standard. If the results do not meet the requirements of this standard, it shall double the sampling from the original batch number according to the provisions of Article 6.4 and re-inspect the items that do not meet the requirements of this standard. If the re-inspection results still do not meet the requirements of this standard, the entire batch of products shall be considered unqualified. 6.6 The user has the right to inspect the product according to the technical requirements and test methods specified in this standard. If the two parties disagree with the inspection results and need to conduct arbitration, the arbitration institution shall be selected by the two parties through consultation. 7 Marking, packaging, transportation, purchase and storage
7.1 Marking
The packaging should be clearly marked, including the manufacturer's name, product name, trademark, production batch number, standard number, grade and net weight, and attached with a quality certificate.
7.2 Packaging
Iron oxide yellow pigment is packaged in plastic woven bags lined with plastic film bags or plastic-coated woven bags, with a net weight of 25kg per bag. 7.3 Transportation
During transportation and loading and unloading, it is required to load and unload gently, and collision and rupture should be prevented. It should be carried out in accordance with relevant transportation regulations. 7.4 Storage
Iron oxide yellow pigment is stored in a dry and ventilated place, and it is strictly forbidden to contact with acidic and alkaline items. According to the above storage conditions, the effective purchase and storage period of unopened pigment is three years.
Additional Notes:
This standard was proposed by the Science and Technology Department of 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 Iron Oxide Pigment Factory. The main drafters of this standard are Lai Shenghua and Yang Baogen. From the date of implementation of this standard, the original national standard GB1862-80 "Iron Oxide Yellow" will be invalid. 6
Free download of various US standard industry materials1 Hydrochloric acid (GB622) solution: 1+1 solution. 5.9.2.2 Nitric acid: (GB626)
Methyl isobutyl ketone (HG3-1118): chemically pure. 5.9.2.4
Ammonia water (GB631): does not contain carbon dioxide. 5.9.2.5
Methyl red indicator: 1g/L ethanol solution, prepared according to GB603. 5.9.2.6
Acetic acid (GB676) solution: 99~100%. Ammonium oxalate (HG3-976) saturated solution.
Ammonium oxalate (HG3-976) solution: 1g/L. Sulfuric acid (GB625) solution: 1+4 solution. 5.9.2.9
5.9.2.10 Potassium permanganate standard titration solution: c (KMnO) = 0.1 mol/L Prepare and calibrate according to GB601. 5.9.3 Instruments and equipment
5.9.3.1 Beaker: 250 mL.
5.9.3.2 Volumetric flask: 250 mL.
5.9.3.3 Pipette: 100 mL.
5.9.3.4 Pear-shaped separating funnel: 250 mL. 5.9.3.5 Electric furnace: connected to autotransformer.
5.9.3.6 Balance: sensitivity 0.001 g.
5.9.4 Analysis steps
5.9.4.1 Sample
Weigh 10 g of sample to an accuracy of 0.001 g.
5.9.4.2 Determination
Put the sample in a beaker, add 100mL of hydrochloric acid solution (5.9.2.1) containing 5mL of nitric acid (5.9.2.2), evaporate to dryness on an electric furnace (5.9.3.5), add 100mL of hydrochloric acid (5.9.2.1) and boil, after cooling, transfer to a 250mL volumetric flask and dilute to scale with hydrochloric acid (5.9.2.1), take 100mL of the solution, and evaporate to dryness. Add 60mL of hydrochloric acid (5.9.2.1) to dissolve it, cool it, and extract the iron with 60mL of methyl isobutyl ketone (5.9.2.3). If the solution is still colored, evaporate it a second time until the solution is colorless. Add 2 drops of methyl red (5.9.2.5) indicator to the above solution, neutralize with ammonia water (5.9.2.4), and then acidify the solution with a slightly excess of acetic acid (5.9.2.6). Boil the solution and add 50 mL of preheated ammonium oxalate solution (5.9.2.7) and continue boiling until the precipitate becomes granular. Let it stand for about 1 hour, filter, and wash with dilute ammonium oxalate solution (5.9.2.8) until the filtrate is free of chloride ions. Finally, wash away the ammonium oxalate with a minimum amount of cold water.
W.HG/T2249—91
Use a glass rod to penetrate the tip of the filter paper and rinse the precipitate into the flask with hot water. Use about 30mL of warm sulfuric acid (5.9.2.9) to wash the filter paper and dilute the solution in the flask to 250mL. Titrate with potassium permanganate standard titration solution (5.9.2.10) at about 75℃ until it turns slightly red. The solution temperature should not be lower than 60℃ at the titration end point. 5.9.5 Expression of results
Expressed as the mass percentage of calcium oxide (CaO) X2, calculated according to formula (2)
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