Some standard content:
ICS87.060.10
Chemical Industry Standard of the People's Republic of China
HG/T3007—1999
Barium metaborate for paints
Issued on 1999-06-16
Implemented on 2000-06-01
State Administration of Petroleum and Chemical Industry
W.bzsoso.cOIHG/T3007—1999
This standard is revised from the chemical industry standard HG/T3007-1988 "Barium metaborate for paints", and some changes have been made in the technical content.
The main difference between this standard and HG/T3007—1988 is that the barium oxide index is changed from the original 54%~61% to 56%~61%. The boron trioxide index was changed from the original 21% to 28% to 22% to 28%. The oil absorption index was changed from the original no more than 30g/100g to (20~35)g/100g. The pH value index of the water suspension was changed from the original 9~10.5 to 9.0~10.5. This standard will replace HG/T3007-1988 from the date of implementation. This standard was proposed by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China, and this standard is under the jurisdiction of the National Technical Committee for Standardization of Paints and Pigments. The main drafting units of this standard are: Tianjin Dongfeng Chemical Plant, Changzhou Paint Chemical Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are: Wang Naiyue, Peng Huamin, Zheng Wenjuan, Jin Liandi. This standard was first issued in 1977 and revised in 1988. I
W.bzsoso.cOm1Scope
Chemical Industry Standard of the People's Republic of China
Barium metaborate for paints
Barium metaborate for paints
HG/T3007—1999
Replaces HG/T3007—1988
This standard specifies the requirements, sampling, test methods, inspection rules, as well as marking, packaging, transportation and storage of barium metaborate for paints. This standard applies to barium metaborate synthesized from barium sulfide aqueous solution and borax aqueous solution and modified with sodium silicate. The product is mainly used in the paint industry.
Its composition is Ba(BO2)2nH2O.
2Cited Standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard was published, the versions shown were all valid. All standards will be revised. Parties using this standard should explore the possibility of using the latest version of the following standards. GB/T601—1988 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T1250—1989 Methods for expressing and determining limit values GB/T1717—1986 Determination of pH value of aqueous suspension of pigments (eqvISO787-9:1981) GB/T5211.3—1985 Determination of volatile matter of pigments at 105°C (eqvISO787-2:1981) GB/T5211.15—1988 Determination of oil absorption of pigments (eqvI ISO787-5:1980) GB/T5211.18—1988 Determination of pigment sieve residue - Water method - Manual operation (neqISO787-7:1981) GB/T6682—1992 Specifications and test methods for water used in analytical laboratories GB9285—1988 Sampling of raw materials for paints and varnishes (eqvISO842:1984) HG/T2457—1993 General rules for inspection, marking, packaging, transportation and storage of pigment products 3 Requirements
The products shall comply with the requirements of Table 1.
Requirements of Table 1
Oxide, % (mass fraction)
Boron trioxide, % (mass fraction)
Silicon dioxide, % (mass fraction)
Water soluble matter, g/100mL
pH value of aqueous suspension
Sieve residue (45μm sieve hole), % (mass fraction)Oil absorption, %/100g
Volatile matter, % (mass fraction)
Indicators approved by the State Administration of Petroleum and Chemical Industry on June 16, 1999
Implementation on June 1, 2000
W.bzsoso.cOI4 Sampling
HG/T3007—1999
Take representative samples of the test product in accordance with the provisions of GB9285. 5 Test method
All reagents used should be analytically pure reagents; use grade 3 water or water of corresponding purity specified in GB/T6682. 5.1 Determination of barium oxide content
5.1.1 Principle
Dissolve the barium metaborate sample with a quantitative acid to generate barium chloride and boric acid, and titrate the excess acid with a sodium hydroxide standard titration solution to determine the barium oxide content.
5.1.2 Reagents and solutions
5.1.2.1 Standard sodium hydroxide titration solution: c(NaOH)=0.5mol/L, prepared and calibrated according to GB/T601. 5.1.2.2 Standard hydrochloric acid solution: c(HC1)=0.5mol/L, prepared according to GB/T601. 5.1.2.3 Mixed indicator: weigh 0.12g methyl red indicator and 0.08g methylene blue indicator, dissolve in ethanol, and dilute to 100mL with ethanol.
5.1.3 Test steps
Weigh 1.5g of metaboric acid lock sample (accurate to 0.1mg), put it into a 500mL conical flask, add 100mL of water and 30.00mL of hydrochloric acid standard solution (5.1.2.2), and boil it slightly at low temperature for 10min. After cooling, add 2 drops of mixed indicator (5.1.2.3) and titrate with sodium hydroxide standard titration solution (5.1.2.1) to the green end point. At the same time, do a blank test.
5.1.4 Expression of results
The content of barium oxide expressed as mass percentage (X) is calculated according to formula (1): X×0. 0765100
Wherein: Vo-
the volume of sodium hydroxide standard titration solution consumed by blank, mL; V——the volume of sodium hydroxide standard titration solution consumed by sample titration, mL; the actual concentration of sodium hydroxide standard titration solution, mol/Lc
the mass of sample, g,
·(1)
the mass of barium oxide expressed in grams equivalent to 1.00mL sodium hydroxide standard titration solution [c(Na0H)=1.000mol/L].
5.1.5 Allowable difference
The difference between two results of parallel determination shall not exceed 0.5%. 5.2 Determination of Boron Trioxide Content
5.2.1 Principle
In the solution where the barium oxide is titrated to the endpoint, the boric acid in the solution is strengthened with mannitol, and then titrated with a standard sodium hydroxide solution to determine the content of boron trioxide. 5.2.2 Reagents and Solutions
5.2.2.1 Standard sodium hydroxide solution: c(NaOH)=0.5mol/L, prepared and calibrated according to GB/T601. 5.2.2.2 Phenol ethanol solution indicator: 10g/L. 5.2.2.3 Mannitol.
5.2.3 Test Procedure
In the solution where the barium oxide is titrated to the endpoint, add 20 drops of phenolphthalein indicator (5.2.2.2) and about 25g of mannitol (5.2.2.3), and titrate with a standard sodium hydroxide solution (5.2.2.1). When near the end point, add another 25g of mannitol (5.2.2.3). Continue titrating until the color is 2
Wbzsoso, cOnHG/T3007—1999
The pink color after the first addition of mannitol and shaking the hook is the end point. 5.2.4 Expression of results
The content of boron trioxide expressed as mass percentage (X2) is calculated according to formula (2): V21 × 0. 034 81 X 100
Wherein: V2—volume of sodium hydroxide standard titration solution consumed by the titrated sample, mL; Cr
-actual concentration of sodium hydroxide standard titration solution, mol/L; Same as in formula (1): m13
++.+..+.+....(2)
0.03481——mass of boron trioxide expressed in grams equivalent to 1.00mL sodium hydroxide standard titration solution [c(Na0H)=1.000mol/L].
5.2.5 Allowable difference
The difference between two results of parallel determination shall not exceed 0.2%. 5.3 Determination of silicon dioxide content
5.3.1 Principle
After barium metaborate is dissolved in acid, in the presence of an appropriate amount of fluoride ions, silicate can generate potassium fluorosilicate precipitation. Potassium fluorosilicate is then hydrolyzed into hydrofluoric acid, which is titrated with a standard sodium hydroxide solution to determine the silicon dioxide content. 5.3.2 Reagents and solutions
5.3.2.1 Hydrochloric acid.
5.3.2.2 Hydrochloric acid solution: 1+1.
5.3.2.3 Nitric acid.
5.3.2.4 Potassium chloride.
5.3.2.5 Phenolphthalein ethanol solution indicator: 10g/L. 5.3.2.6 Anhydrous ethanol.
5.3.2.7 Qualitative filter paper.
5.3.2.8 Potassium fluoride solution: 200g/L.
Weigh 40g potassium fluoride and put it in a plastic cup, add 150mL water, and add 25mL each of hydrochloric acid (5.3.2.1) and nitric acid (5.3.2.3). Add potassium chloride to saturate it, let it stand for 30 minutes, and filter it with a plastic funnel. 5.3.2.9 Washing solution.
Dissolve 50g potassium chloride in 500mL water, then add 500mL ethanol (5.3.2.6) to prepare a 50g/L mixed washing solution of potassium chloride and ethanol (the suitable storage temperature is below 25℃). 5.3.2.10 Paper pulp.
Tear ordinary filter paper into small pieces (about 1cm2), and soak them in washing solution (5.3.2.9). 5.3.2.11 Standard titration solution of sodium hydroxide: c(NaOH)=0.1mol/L Prepare and calibrate according to GB/T601. 5.3.3 Test steps
Weigh 0.2g (accurate to 0.2mg) of barium metaborate sample, place it in a 300mL plastic cup, add about 1mL water to soak it, and then add 20mL boiling hydrochloric acid (5.3.2.2). After the sample is dissolved, add 12 mL of hydrochloric acid (5.3.2.1), 5 mL of nitric acid (5.3.2.3), and potassium chloride (5.3.2.4) to saturate it. Cool to below 25°C, stir continuously with a plastic stick, slowly add 5 mL of potassium fluoride solution (5.3.2.8), and stir for 1 minute. Let it stand for a while, add about 6 pieces of pulp (5.3.2.10), and filter with a plastic funnel [the filter paper should be moistened with washing liquid (5.3.2.9) before filtering]. After all the precipitate is transferred to the funnel, wash it 3 times with washing liquid below 25°C. Immediately put the filter paper and the precipitate into the original plastic cup, add 10 mL of washing liquid and 20 drops of phenol indicator (5.3.2.5), and then neutralize with sodium hydroxide solution until it is light pink and does not fade within 1 minute, then add 200 mL of fully boiled water, and quickly titrate with sodium hydroxide standard titration solution (5.3.2.11). The color of the titration endpoint is the color after neutralization.
Do a blank test at the same time.
HG/T3007—1999
1 Neutralization can be done with 0.1mol/L sodium hydroxide solution or 30% alkali solution. Neutralization should be completed within 15min. 2 When titrating with sodium hydroxide standard titration solution, the temperature of the dripping liquid should be kept above 80℃. 3 When potassium fluorosilicate precipitation is generated, the added potassium amide should be supersaturated, otherwise the result will be low. However, it is also necessary to avoid too much potassium amide to avoid the formation of cryolite (KsAIF) precipitation, which will make the result high.
4 When washing with washing liquid, the number of washing times should not be too many, generally three times is appropriate, so as not to cause potassium fluorosilicate hydrolysis, which will make the result low. In addition, filtering, washing, neutralization and other operations should be rapid, especially in summer when the room temperature is high, the operation should be more rapid. If potassium chloride is too supersaturated during precipitation, it is necessary to use the tilting method to wash repeatedly during filtration until the solid potassium chloride is completely dissolved. Otherwise, the acid will not be easy to wash out, causing the result to be biased high. The presence of more potassium salt will also make the color of the titration endpoint not obvious.
5.3.4 Expression of results
The silicon dioxide content (X) expressed as mass percentage is calculated according to formula (3): -V) .×0. 015 02×100
Wherein: Vo
The volume of sodium hydroxide standard titration solution consumed in the titration blank, mL; V3—The volume of sodium hydroxide standard titration solution consumed in the titration sample, mL; C2
The actual concentration of sodium hydroxide standard titration solution, mol/Lm2——Sample mass, g;
·(3)
0.01502—The mass of silicon dioxide in grams equivalent to 1.00mL of sodium hydroxide standard titration solution [c(Na0H)=1.000mol/L].
5.3.5 Allowable difference
The difference between two results of parallel determination shall not exceed 0.2%. 5.4 Determination of water-soluble contentbzxZ.net
5.4.1 Reagents and solutions
Distilled water: 25℃, pH value 6~7.
5.4.2 Instruments and equipment
5.4.2.1 Single-scale volumetric flask: 250mL. 5.4.2.2 Qualitative filter paper.
5.4.2.3 Beaker: 150mL.
5.4.2.4 Oven: (105±2)℃.
5.4.2.5 Desiccator: with effective desiccant inside. 5.4.2.6 Pipette: 100mL.
5.4.3 Test steps
Weigh 5g of barium metaborate sample (accurate to 0.01g) and place it in a volumetric flask (5.4.2.1), and accurately add 200mL of water (5.4.1). Shake for 30min. Filter into a dry conical flask. Use a pipette (5.4.2.6) to absorb 100mL of this solution, transfer it into a beaker (5.4.2.3) with a constant mass, and heat it on an electric stove at low temperature to evaporate it to near dryness. Place it in a (105±2)℃ oven (5.4.2.4) for 2h, take it out and place it in a desiccator (5.4.2.5), cool it to room temperature, and weigh it. Note: Since the determination result of water-soluble content is affected by the test temperature, when arbitration is required, the test should be carried out at (23±2)℃. 5.4.4 Expression of results
The water-soluble content (X) expressed in g/100mL is calculated according to formula (4): X4=G1-G2
Wherein: G1—
Total mass of the residue and beaker, g;
Mass of the empty beaker, g.
5.4.5 Permissible difference
The difference between two results of parallel determination shall not exceed 0.01g/100mL. 4
(4)
W.bzsoso,cOn5.5 Determination of pH value of aqueous suspension
HG/T3007—1999
Perform according to the provisions of GB/T1717. Sample size 3g. 5.6 Determination of sieve residue
Perform according to the provisions of GB/T5211.18. Sample weight 10g, add 300mL water, and add 20mL of 20g/L sodium pyrophosphate dispersant, place on a magnetic stirrer and stir for 30min. 5.7 Determination of oil absorption
According to the provisions of GB/T5211.15. Sample weight 10g. 5.8 Determination of volatile matter
According to the provisions of GB/T5211.3. Sample weight 10g. Heating temperature is (90±2)℃, and baked in an oven for 2h. 6 Inspection rules
6.1 According to the provisions of Chapter 3 of HG/T2457-1993. All the requirements listed in this standard are both type inspection items and factory inspection items.
6.2 The determination of the inspection results in this standard shall be carried out in accordance with the provisions of 5.2 of GB/T1250-1989. 7 Marking, packaging, transportation and storage
7.1 Marking
According to the provisions of Chapter 4 of HG/T2457-1993. And add the quality certification mark. 7.2 Packaging
According to the provisions of Chapter 5 of HG/T2457-1993. The product should be packed in plastic woven bags lined with plastic bags. The net content of each bag is 25kg or 50kg.
7.3 Transportation and storage
According to the provisions of Chapter 6 of HG/T2457-1993. The product should be purchased and stored in a dry and ventilated place. The unopened product can be effectively stored for ten months from the date of production.
Wbzsoso，cO10 Paper pulp.
Tear into small pieces (about 1cm2) with ordinary filter paper, and soak with detergent (5.3.2.9). 5.3.2.11 Standard sodium hydroxide titration solution: c(NaOH)=0.1mol/L Prepare and calibrate according to GB/T601. 5.3.3 Test steps
Weigh 0.2g (accurate to 0.2mg) of barium metaborate sample, place it in a 300mL plastic cup, add about 1mL of water to soak it, and then add 20mL of boiling hydrochloric acid (5.3.2.2). After the sample is dissolved, add 12mL of hydrochloric acid (5.3.2.1), 5mL of nitric acid (5.3.2.3), and potassium chloride (5.3.2.4) to saturate it. Cool to below 25℃, stir continuously with a plastic stick, slowly add 5mL potassium fluoride solution (5.3.2.8), stir for 1min, let stand for a while, add about 6 pieces of pulp (5.3.2.10), and filter with a plastic funnel [the filter paper should be moistened with washing liquid (5.3.2.9) before filtering]. After all the precipitate is transferred to the funnel, wash it 3 times with washing liquid below 25℃. Immediately put the filter paper and the precipitate into the original plastic cup, add 10mL washing liquid and 20 drops of phenol indicator (5.3.2.5), and then neutralize with sodium hydroxide solution until the light pink color does not fade within 1min, then add 200mL of fully boiled water, and quickly titrate with sodium hydroxide standard titration solution (5.3.2.11). The color at the end point of titration is the color after neutralization.
At the same time, do a blank test.
HG/T3007—1999
1 Neutralization can be done with 0.1mol/L sodium hydroxide solution or 30% alkali solution. Neutralization should be completed within 15min. 2 When titrating with sodium hydroxide standard titration solution, the temperature of the dripping liquid should be kept above 80℃. 3 When potassium fluorosilicate precipitation is generated, the added potassium amide should be supersaturated, otherwise the result will be low. However, it is also necessary to avoid too much potassium amide to avoid the formation of cryolite (KsAIF) precipitation, which will make the result high.
4 When washing with detergent, the number of washing times should not be too many, generally three times is appropriate, so as not to cause potassium fluorosilicate hydrolysis and make the result low. In addition, filtering, washing, neutralization and other operations should be rapid, especially in summer when the room temperature is high, the operation should be more rapid. If potassium chloride is too supersaturated during precipitation, it is necessary to use the tilting method to wash repeatedly during filtration until the solid potassium chloride is completely dissolved. Otherwise, the acid will not be easy to wash out, causing the result to be biased high. The presence of more potassium salt will also make the color of the titration endpoint not obvious.
5.3.4 Expression of results
The silicon dioxide content (X) expressed as mass percentage is calculated according to formula (3): -V) .×0. 015 02×100
Wherein: Vo
The volume of sodium hydroxide standard titration solution consumed in the titration blank, mL; V3—The volume of sodium hydroxide standard titration solution consumed in the titration sample, mL; C2
The actual concentration of sodium hydroxide standard titration solution, mol/Lm2——Sample mass, g;
·(3)
0.01502—The mass of silicon dioxide in grams equivalent to 1.00mL of sodium hydroxide standard titration solution [c(Na0H)=1.000mol/L].
5.3.5 Allowable difference
The difference between two results of parallel determination shall not exceed 0.2%. 5.4 Determination of water-soluble content
5.4.1 Reagents and solutions
Distilled water: 25℃, pH value 6~7.
5.4.2 Instruments and equipment
5.4.2.1 Single-scale volumetric flask: 250mL. 5.4.2.2 Qualitative filter paper.
5.4.2.3 Beaker: 150mL.
5.4.2.4 Oven: (105±2)℃.
5.4.2.5 Desiccator: with effective desiccant inside. 5.4.2.6 Pipette: 100mL.
5.4.3 Test steps
Weigh 5g of barium metaborate sample (accurate to 0.01g) and place it in a volumetric flask (5.4.2.1), and accurately add 200mL of water (5.4.1). Shake for 30 minutes. Filter into a dry conical flask. Use a pipette (5.4.2.6) to absorb 100mL of this solution, transfer it into a beaker (5.4.2.3) with a constant mass, and heat it on an electric stove at low temperature to evaporate it to near dryness. Place it in a (105±2)℃ oven (5.4.2.4) for 2 hours, take it out and place it in a desiccator (5.4.2.5), cool it to room temperature, and weigh it. Note: Since the determination result of water-soluble content is affected by the test temperature, when arbitration is required, the test should be carried out at (23±2)℃. 5.4.4 Expression of results
The water-soluble content (X) expressed in g/100mL is calculated according to formula (4): X4=G1-G2
Wherein: G1—
Total mass of the residue and beaker, g;
Mass of the empty beaker, g.
5.4.5 Permissible difference
The difference between two results of parallel determination shall not exceed 0.01g/100mL. 4
(4)
W.bzsoso,cOn5.5 Determination of pH value of aqueous suspension
HG/T3007—1999
Perform according to the provisions of GB/T1717. Sample size 3g. 5.6 Determination of sieve residue
Perform according to the provisions of GB/T5211.18. Sample weight 10g, add 300mL water, and add 20mL of 20g/L sodium pyrophosphate dispersant, place on a magnetic stirrer and stir for 30min. 5.7 Determination of oil absorption
According to the provisions of GB/T5211.15. Sample weight 10g. 5.8 Determination of volatile matter
According to the provisions of GB/T5211.3. Sample weight 10g. Heating temperature is (90±2)℃, and baked in an oven for 2h. 6 Inspection rules
6.1 According to the provisions of Chapter 3 of HG/T2457-1993. All the requirements listed in this standard are both type inspection items and factory inspection items.
6.2 The determination of the inspection results in this standard shall be carried out in accordance with the provisions of 5.2 of GB/T1250-1989. 7 Marking, packaging, transportation and storage
7.1 Marking
According to the provisions of Chapter 4 of HG/T2457-1993. And add the quality certification mark. 7.2 Packaging
According to the provisions of Chapter 5 of HG/T2457-1993. The product should be packed in plastic woven bags lined with plastic bags. The net content of each bag is 25kg or 50kg.
7.3 Transportation and storage
According to the provisions of Chapter 6 of HG/T2457-1993. The product should be purchased and stored in a dry and ventilated place. The unopened product can be effectively stored for ten months from the date of production.
Wbzsoso，cO10 Paper pulp.
Tear into small pieces (about 1cm2) with ordinary filter paper, and soak with detergent (5.3.2.9). 5.3.2.11 Standard sodium hydroxide titration solution: c(NaOH)=0.1mol/L Prepare and calibrate according to GB/T601. 5.3.3 Test steps
Weigh 0.2g (accurate to 0.2mg) of barium metaborate sample, place it in a 300mL plastic cup, add about 1mL of water to soak it, and then add 20mL of boiling hydrochloric acid (5.3.2.2). After the sample is dissolved, add 12mL of hydrochloric acid (5.3.2.1), 5mL of nitric acid (5.3.2.3), and potassium chloride (5.3.2.4) to saturate it. Cool to below 25℃, stir continuously with a plastic stick, slowly add 5mL potassium fluoride solution (5.3.2.8), stir for 1min, let stand for a while, add about 6 pieces of pulp (5.3.2.10), and filter with a plastic funnel [the filter paper should be moistened with washing liquid (5.3.2.9) before filtering]. After all the precipitate is transferred to the funnel, wash it 3 times with washing liquid below 25℃. Immediately put the filter paper and the precipitate into the original plastic cup, add 10mL washing liquid and 20 drops of phenol indicator (5.3.2.5), and then neutralize with sodium hydroxide solution until the light pink color does not fade within 1min, then add 200mL of fully boiled water, and quickly titrate with sodium hydroxide standard titration solution (5.3.2.11). The color at the end point of titration is the color after neutralization.
At the same time, do a blank test.
HG/T3007—1999
1 Neutralization can be done with 0.1mol/L sodium hydroxide solution or 30% alkali solution. Neutralization should be completed within 15min. 2 When titrating with sodium hydroxide standard titration solution, the temperature of the dripping liquid should be kept above 80℃. 3 When potassium fluorosilicate precipitation is generated, the added potassium amide should be supersaturated, otherwise the result will be low. However, it is also necessary to avoid too much potassium amide to avoid the formation of cryolite (KsAIF) precipitation, which will make the result high.
4 When washing with detergent, the number of washing times should not be too many, generally three times is appropriate, so as not to cause potassium fluorosilicate hydrolysis and make the result low. In addition, filtering, washing, neutralization and other operations should be rapid, especially in summer when the room temperature is high, the operation should be more rapid. If potassium chloride is too supersaturated during precipitation, it is necessary to use the tilting method to wash repeatedly during filtration until the solid potassium chloride is completely dissolved. Otherwise, the acid will not be easy to wash out, causing the result to be biased high. The presence of more potassium salt will also make the color of the titration endpoint not obvious.
5.3.4 Expression of results
The silicon dioxide content (X) expressed as mass percentage is calculated according to formula (3): -V) .×0. 015 02×100
Wherein: Vo
The volume of sodium hydroxide standard titration solution consumed in the titration blank, mL; V3—The volume of sodium hydroxide standard titration solution consumed in the titration sample, mL; C2
The actual concentration of sodium hydroxide standard titration solution, mol/Lm2——Sample mass, g;
·(3)
0.01502—The mass of silicon dioxide in grams equivalent to 1.00mL of sodium hydroxide standard titration solution [c(Na0H)=1.000mol/L].
5.3.5 Allowable difference
The difference between two results of parallel determination shall not exceed 0.2%. 5.4 Determination of water-soluble content
5.4.1 Reagents and solutions
Distilled water: 25℃, pH value 6~7.
5.4.2 Instruments and equipment
5.4.2.1 Single-scale volumetric flask: 250mL. 5.4.2.2 Qualitative filter paper.
5.4.2.3 Beaker: 150mL.
5.4.2.4 Oven: (105±2)℃.
5.4.2.5 Desiccator: with effective desiccant inside. 5.4.2.6 Pipette: 100mL.
5.4.3 Test steps
Weigh 5g of barium metaborate sample (accurate to 0.01g) and place it in a volumetric flask (5.4.2.1), and accurately add 200mL of water (5.4.1). Shake for 30 minutes. Filter into a dry conical flask. Use a pipette (5.4.2.6) to absorb 100mL of this solution, transfer it into a beaker (5.4.2.3) with a constant mass, and heat it on an electric stove at low temperature to evaporate it to near dryness. Place it in a (105±2)℃ oven (5.4.2.4) for 2 hours, take it out and place it in a desiccator (5.4.2.5), cool it to room temperature, and weigh it. Note: Since the determination result of water-soluble content is affected by the test temperature, when arbitration is required, the test should be carried out at (23±2)℃. 5.4.4 Expression of results
The water-soluble content (X) expressed in g/100mL is calculated according to formula (4): X4=G1-G2
Wherein: G1—
Total mass of the residue and beaker, g;
Mass of the empty beaker, g.
5.4.5 Permissible difference
The difference between two results of parallel determination shall not exceed 0.01g/100mL. 4
(4)
W.bzsoso,cOn5.5 Determination of pH value of aqueous suspension
HG/T3007—1999
Perform according to the provisions of GB/T1717. Sample size 3g. 5.6 Determination of sieve residue
Perform according to the provisions of GB/T5211.18. Sample weight 10g, add 300mL water, and add 20mL of 20g/L sodium pyrophosphate dispersant, place on a magnetic stirrer and stir for 30min. 5.7 Determination of oil absorption
According to the provisions of GB/T5211.15. Sample weight 10g. 5.8 Determination of volatile matter
According to the provisions of GB/T5211.3. Sample weight 10g. Heating temperature is (90±2)℃, and baked in an oven for 2h. 6 Inspection rules
6.1 According to the provisions of Chapter 3 of HG/T2457-1993. All the requirements listed in this standard are both type inspection items and factory inspection items.
6.2 The determination of the inspection results in this standard shall be carried out in accordance with the provisions of 5.2 of GB/T1250-1989. 7 Marking, packaging, transportation and storage
7.1 Marking
According to the provisions of Chapter 4 of HG/T2457-1993. And add the quality certification mark. 7.2 Packaging
According to the provisions of Chapter 5 of HG/T2457-1993. The product should be packed in plastic woven bags lined with plastic bags. The net content of each bag is 25kg or 50kg.
7.3 Transportation and storage
According to the provisions of Chapter 6 of HG/T2457-1993. The product should be purchased and stored in a dry and ventilated place. The unopened product can be effectively stored for ten months from the date of production.
Wbzsoso，cO1mol/L sodium hydroxide solution or 30% alkali solution can be used. Neutralization should be completed within 15min. 2 When titrating with sodium hydroxide standard titration solution, the temperature of the droplet should be kept above 80℃. 3 When potassium fluorosilicate precipitation is generated, the potassium amide added should be supersaturated, otherwise the result will be low. However, it is also necessary to avoid too much potassium amide to avoid the formation of cryolite (KsAIF) precipitation, which will make the result high.
4 When washing with washing liquid, the number of washings should not be too many, generally three times is appropriate, so as not to cause potassium fluorosilicate hydrolysis and make the result low. In addition, filtration, washing, neutralization and other operations should be rapid, especially in summer when the room temperature is high, the operation should be more rapid. If potassium chloride is too supersaturated during precipitation, it is necessary to use the tilting method to wash repeatedly until the solid potassium chloride is completely dissolved during filtration, otherwise the acid is not easy to wash, resulting in a high result. The presence of more potassium salts also makes the color of the titration end point unclear.
5.3.4 Expression of results
The silicon dioxide content (X) expressed as mass percentage is calculated according to formula (3): -V) .×0. 015 02×100
Wherein: Vo
The volume of sodium hydroxide standard titration solution consumed in the titration blank, mL; V3—The volume of sodium hydroxide standard titration solution consumed in the titration sample, mL; C2
The actual concentration of sodium hydroxide standard titration solution, mol/Lm2——Sample mass, g;
·(3)
0.01502—The mass of silicon dioxide in grams equivalent to 1.00mL of sodium hydroxide standard titration solution [c(Na0H)=1.000mol/L].
5.3.5 Allowable difference
The difference between two results of parallel determination shall not exceed 0.2%. 5.4 Determination of water-soluble content
5.4.1 Reagents and solutions
Distilled water: 25℃, pH value 6~7.
5.4.2 Instruments and equipment
5.4.2.1 Single-scale volumetric flask: 250mL. 5.4.2.2 Qualitative filter paper.
5.4.2.3 Beaker: 150mL.
5.4.2.4 Oven: (105±2)℃.
5.4.2.5 Desiccator: with effective desiccant inside. 5.4.2.6 Pipette: 100mL.
5.4.3 Test steps
Weigh 5g of barium metaborate sample (accurate to 0.01g) and place it in a volumetric flask (5.4.2.1), and accurately add 200mL of water (5.4.1). Shake for 30min. Filter into a dry conical flask. Use a pipette (5.4.2.6) to absorb 100mL of this solution, transfer it into a beaker (5.4.2.3) with a constant mass, and heat it on an electric stove at low temperature to evaporate it to near dryness. Place it in a (105±2)℃ oven (5.4.2.4) for 2h, take it out and place it in a desiccator (5.4.2.5), cool it to room temperature, and weigh it. Note: Since the determination result of water-soluble content is affected by the test temperature, when arbitration is required, the test should be carried out at (23±2)℃. 5.4.4 Expression of results
The water-soluble content (X) expressed in g/100mL is calculated according to formula (4): X4=G1-G2
Wherein: G1—
Total mass of the residue and beaker, g;
Mass of the empty beaker, g.
5.4.5 Permissible difference
The difference between two results of parallel determination shall not exceed 0.01g/100mL. 4
(4)
W.bzsoso,cOn5.5 Determination of pH value of aqueous suspension
HG/T3007—1999
Perform according to the provisions of GB/T1717. Sample size 3g. 5.6 Determination of sieve residue
Perform according to the provisions of GB/T5211.18. Sample weight 10g, add 300mL water, and add 20mL of 20g/L sodium pyrophosphate dispersant, place on a magnetic stirrer and stir for 30min. 5.7 Determination of oil absorption
According to the provisions of GB/T5211.15. Sample weight 10g. 5.8 Determination of volatile matter
According to the provisions of GB/T5211.3. Sample weight 10g. Heating temperature is (90±2)℃, and baked in an oven for 2h. 6 Inspection rules
6.1 According to the provisions of Chapter 3 of HG/T2457-1993. All the requirements listed in this standard are both type inspection items and factory inspection items.
6.2 The determination of the inspection results in this standard shall be carried out in accordance with the provisions of 5.2 of GB/T1250-1989. 7 Marking, packaging, transportation and storage
7.1 Marking
According to the provisions of Chapter 4 of HG/T2457-1993. And add the quality certification mark. 7.2 Packaging
According to the provisions of Chapter 5 of HG/T2457-1993. The product should be packed in plastic woven bags lined with plastic bags. The net content of each bag is 25kg or 50kg.
7.3 Transportation and storage
According to the provisions of Chapter 6 of HG/T2457-1993. The product should be purchased and stored in a dry and ventilated place. The unopened product can be effectively stored for ten months from the date of production.
Wbzsoso，cO1mol/L sodium hydroxide solution or 30% alkali solution can be used. Neutralization should be completed within 15min. 2 When titrating with sodium hydroxide standard titration solution, the temperature of the droplet should be kept above 80℃. 3 When potassium fluorosilicate precipitation is generated, the potassium amide added should be supersaturated, otherwise the result will be low. However, it is also necessary to avoid too much potassium amide to avoid the formation of cryolite (KsAIF) precipitation, which will make the result high.
4 When washing with washing liquid, the number of washings should not be too many, generally three times is appropriate, so as not to cause potassium fluorosilicate hydrolysis and make the result low. In addition, filtration, washing, neutralization and other operations should be rapid, especially in summer when the room temperature is high, the operation should be more rapid. If potassium chloride is too supersaturated during precipitation, it is necessary to use the tilting method to wash repeatedly until the solid potassium chloride is completely dissolved during filtration, otherwise the acid is not easy to wash, resulting in a high result. The presence of more potassium salts also makes the color of the titration end point unclear.
5.3.4 Expression of results
The silicon dioxide content (X) expressed as mass percentage is calculated according to formula (3): -V) .×0. 015 02×100
Wherein: Vo
The volume of sodium hydroxide standard titration solution consumed in the titration blank, mL; V3—The volume of sodium hydroxide standard titration solution consumed in the titration sample, mL; C2
The actual concentration of sodium hydroxide standard titration solution, mol/Lm2——Sample mass, g;
·(3)
0.01502—The mass of silicon dioxide in grams equivalent to 1.00mL of sodium hydroxide standard titration solution [c(Na0H)=1.000mol/L].
5.3.5 Allowable difference
The difference between two results of parallel determination shall not exceed 0.2%. 5.4 Determination of water-soluble content
5.4.1 Reagents and solutions
Distilled water: 25℃, pH value 6~7.
5.4.2 Instruments and equipment
5.4.2.1 Single-scale volumetric flask: 250mL. 5.4.2.2 Qualitative filter paper.
5.4.2.3 Beaker: 150mL.
5.4.2.4 Oven: (105±2)℃.
5.4.2.5 Desiccator: with effective desiccant inside. 5.4.2.6 Pipette: 100mL.
5.4.3 Test steps
Weigh 5g of barium metaborate sample (accurate to 0.01g) and place it in a volumetric flask (5.4.2.1), and accurately add 200mL of water (5.4.1). Shake for 30 minutes. Filter into a dry conical flask. Use a pipette (5.4.2.6) to absorb 100mL of this solution, transfer it into a beaker (5.4.2.3) with a constant mass, and heat it on an electric stove at low temperature to evaporate it to near dryness. Place it in a (105±2)℃ oven (5.4.2.4) for 2 hours, take it out and place it in a desiccator (5.4.2.5), cool it to room temperature, and weigh it. Note: Since the determination result of water-soluble content is affected by the test temperature, when arbitration is required, the test should be carried out at (23±2)℃. 5.4.4 Expression of results
The water-soluble content (X) expressed in g/100mL is calculated according to formula (4): X4=G1-G2
Wherein: G1—
Total mass of the residue and beaker, g;
Mass of the empty beaker, g.
5.4.5 Permissible difference
The difference between two results of parallel determination shall not exceed 0.01g/100mL. 4
(4)
W.bzsoso,cOn5.5 Determination of pH value of aqueous suspension
HG/T3007—1999
Perform according to the provisions of GB/T1717. Sample size 3g. 5.6 Determination of sieve residue
Perform according to the provisions of GB/T5211.18. Sample weight 10g, add 300mL water, and add 20mL of 20g/L sodium pyrophosphate dispersant, place on a magnetic stirrer and stir for 30min. 5.7 Determination of oil absorption
According to the provisions of GB/T5211.15. Sample weight 10g. 5.8 Determination of volatile matter
According to the provisions of GB/T5211.3. Sample weight 10g. Heating temperature is (90±2)℃, and baked in an oven for 2h. 6 Inspection rules
6.1 According to the provisions of Chapter 3 of HG/T2457-1993. All the requirements listed in this standard are both type inspection items and factory inspection items.
6.2 The determination of the inspection results in this standard shall be carried out in accordance with the provisions of 5.2 of GB/T1250-1989. 7 Marking, packaging, transportation and storage
7.1 Marking
According to the provisions of Chapter 4 of HG/T2457-1993. And add the quality certification mark. 7.2 Packaging
According to the provisions of Chapter 5 of HG/T2457-1993. The product should be packed in plastic woven bags lined with plastic bags. The net content of each bag is 25kg or 50kg.
7.3 Transportation and storage
According to the provisions of Chapter 6 of HG/T2457-1993. The product should be purchased and stored in a dry and ventilated place. The unopened product can be effectively stored for ten months from the date of production.
Wbzsoso，cO15. Sample size: 10 g. 5.8 Determination of volatile matter
Perform according to the provisions of GB/T5211.3. Sample size: 10 g. Heating temperature: (90 ± 2) °C, bake in oven for 2 hours. 6 Inspection rules
6.1 Perform according to the provisions of Chapter 3 of HG/T2457-1993. All the requirements listed in this standard are both type inspection items and factory inspection items.
6.2 The determination of the inspection results in this standard shall be carried out in accordance with the provisions of 5.2 of GB/T1250-1989. 7 Marking, packaging, transportation and purchase and storage
7.1 Marking
Perform according to the provisions of Chapter 4 of HG/T2457-1993. And add quality certification mark. 7.2 Packaging
Perform according to the provisions of Chapter 5 of HG/T2457-1993. The product should be packed in plastic woven bags lined with plastic bags. The net content of each bag is 25kg or 50kg.
7.3 Transportation and storage
According to the provisions of Chapter 6 of HG/T2457-1993. The product should be stored in a dry and ventilated place. The product can be effectively stored for ten months if it is not opened from the date of production.
Wbzsoso，cO15. Sample size: 10 g. 5.8 Determination of volatile matter
Perform according to the provisions of GB/T5211.3. Sample size: 10 g. Heating temperature: (90 ± 2) °C, bake in oven for 2 hours. 6 Inspection rules
6.1 Perform according to the provisions of Chapter 3 of HG/T2457-1993. All the requirements listed in this standard are both type inspection items and factory inspection items.
6.2 The determination of the inspection results in this standard shall be carried out in accordance with the provisions of 5.2 of GB/T1250-1989. 7 Marking, packaging, transportation and purchase and storage
7.1 Marking
Perform according to the provisions of Chapter 4 of HG/T2457-1993. And add quality certification mark. 7.2 Packaging
Perform according to the provisions of Chapter 5 of HG/T2457-1993. The product should be packed in plastic woven bags lined with plastic bags. The net content of each bag is 25kg or 50kg.
7.3 Transportation and storage
According to the provisions of Chapter 6 of HG/T2457-1993. The product should be stored in a dry and ventilated place. The product can be effectively stored for ten months if it is not opened from the date of production.
Wbzsoso，cO
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