Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2567—94
Industrial Activated Precipitated Calcium Carbonate
Published on February 9, 1994
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1994
WChemical Industry Standard of the People's Republic of China
Industrial Activated Precipitated Calcium Carbonate
Subject Content and Scope of Application
HG/T2567—94
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage of industrial activated precipitated calcium carbonate.
This standard applies to precipitated calcium carbonate produced by precipitation method, using activator or coupling agent for surface activation treatment, and calcium carbonate produced by dry method or wet method. This product is mainly used as filler in industries such as plastics, rubber, and organic resins. Cited standards
Packaging, storage and transportation pictorial symbols
GB/T601
GB/T602
GB/T603
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagentsPreparation of standard solutions for determination of impurities in chemical reagentsPreparation of preparations and products used in test methods for chemical reagentsExpression and determination methods of limit valuesGB1250
GB/T3049
GB/T6678||tt ||GB/T6682
GB8946
GB8947
General method for determination of iron content in chemical products Deoxyphenanthroline spectrophotometry
General rules for sampling of chemical products
Specifications and test methods for water used in analytical laboratories Plastic woven bags
Composite plastic woven bags
HG/T2226
Industrial precipitated calcium carbonate
3 Technical requirements
3.1 Appearance: white powder.
3.2 Industrial active precipitated calcium carbonate shall meet the requirements of the following table. Item
Main content (calculated as CaCOs), %
Volatile matter content at 105℃, %
Content insoluble in hydrochloric acid, %
125um test sieve, %
Sieve residue
45um test sieve, %
Approved by the Ministry of Chemical Industry of the People's Republic of China on February 9, 1994
Qualified products
Implemented on July 1, 1994
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Iron (Fe) content, %
Manganese (Mn) content, %
Whiteness, degree
Oil absorption value, g/100g
Activation degree, %
Test method
HG/T2567-94
First-class product
Qualified product
The reagents and water used in this standard, unless otherwise specified, refer to analytical pure reagents and grade 3 water specified in GB/T6682.
The standard titration solution, impurity standard solution, preparation and products required in the test, unless otherwise specified, shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603.
4.1 Determination of main content
4.1.1 Summary of method
Wet the sample with a small amount of ethanol solution, add an excess of hydrochloric acid standard titration solution, use bromocresol green-methyl red as indicator, and back-titrate with sodium hydroxide standard titration solution.
4.1.2 Reagents and materials
4.1.2.195% ethanol (GB/T679);
4.1.2.2 Hydrochloric acid (GB/T622) standard titration solution: c (HCI) about 1 mol/L; 4.1.2.3 Sodium hydroxide (GB/T629) standard titration solution: c (NaOH) about 0.5 mol/L; 4.1.2.4 Bromocresol green (HG/T3-1220)-methyl red (HG/T3-958) indicator solution. 4.1.3 Analysis steps
Weigh 2-2.2g of the sample (accurate to 0.0002g) that has been dried to constant weight at 105±5℃ in advance, place it in a conical flask, add 2mL of ethanol to moisten the sample, use a pipette to transfer 50mL of hydrochloric acid standard titration solution to dissolve the sample, shake, boil for 2min, and cool; add 10 drops of bromocresol green-methyl red indicator solution, and titrate with sodium hydroxide standard titration solution until the test solution changes from red to green. This is the end point.
4.1.4 Expression of analysis results
The main content (in terms of CacO:) X expressed as mass percentage is calculated according to formula (1): Xi (V) × 0.050 04 ×100
5.004(ciV1 - c2V 2)
Wherein: ci——actual concentration of hydrochloric acid standard titration solution, mol/L; Vi
——volume of hydrochloric acid standard titration solution added, mL; (1)
W.bzsoso.coDHG/T2567-94
c2——actual concentration of sodium hydroxide standard titration solution, mol/L; V2——volume of sodium hydroxide standard titration solution consumed in titration, mL;——mass of sample, g;
0.05004——mass of calcium carbonate expressed in grams equivalent to 1.00mL hydrochloric acid standard titration solution [c (HCI) = 1.000mol/L).
4.1.5 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result, and the absolute difference of the parallel determination results shall not exceed 0.2%. 4.2 Determination of pH value
4.2.1 Reagents and materials
4.2.1.1 Water without carbon dioxide;bzxz.net
4.2.1.2 95% ethanol (GB/T679) neutral solution: use phenolphthalein as indicator and adjust to light pink with sodium hydroxide solution. 4.2.2 Instruments and equipment
4.2.2.1 Acidity meter: measuring range pH 0~14, nominal graduation value 0.02pH; 4.2.2.2 Reference electrode: calomel electrode;
4.2.2.3 Indicator electrode: glass electrode.
4.2.3 Analysis steps
Weigh about 10g of sample (accurate to 0.01g), place in a 150mL beaker, add 5mL ethanol to moisten, add 100mL water (4.2.1.1), stir well, let stand for 10min, and measure the pH value of the suspension with an acidometer. 4.2.4 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result, and the absolute difference of the parallel determination results shall not exceed 0.3pH. 4.3 Determination of volatile matter content at 105℃
Same as Article 4.3 of HG/T2226.
4.4 Determination of hydrochloric acid insoluble matter content
4.4.1 Method summary
Same as Article 4.4.1 of HG/T2226.
4.4.2 Reagents and materials
4.4.2.1 95% ethanol (GB/T679);
The rest is the same as HG/T2226 Section 4.4.2.
4.4.3 Analysis steps
Weigh about 4g of sample (accurate to 0.01g), place it in a beaker, add 4mL of ethanol to moisten it, and the following operations are the same as HG/T2226 Section 4.4.3, starting from "adding 20mL of hydrochloric acid solution" until "burning to constant weight". 4.4.4 Expression of analysis results
The same as HG/T2226 Section 4.4.4.
4.4.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result, and the absolute difference of the parallel determination results shall not exceed 0.03%. 4.5 Determination of sieve residue
4.5.1 Instruments and equipment
4.5.1.1 Test sieve (GB6003): R40/3 series, @200mmX50mm/0.125mm and @200mmX50mm/0.045mm;
4.5.1.2 No. 11 wool brush.
4.5.2 Analysis steps
Weigh about 10g of sample (accurate to 0.01g), transfer it to the test sieve, and lightly brush the sample with a wool brush to pass through the sieve until there is no trace of the sample on the black paper under the sieve. Transfer the sieve residue to a watch glass of known mass and weigh it (accurate to 0.0002g). 3
4.5.3 Table of analysis results The same as Article 4.8.3 of HG/T2226.
4.5.4 Allowable difference
HG/T2567-94
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results is 0.003% for the 125μm test sieve and 0.03% for the 45μm test sieve.
4.6 Determination of iron content
4.6.1 Method summary
Same as Article 2 of GB/T3049.
4.6.2 Reagents and materials
4.6.2.1 Hydrochloric acid (GB/T622) solution: 1+1; 4.6.2.2 Hydrochloric acid (GB/T622) solution: 1+4; 4.6.2.3 95% ethanol (GB/T679);
Others are the same as Article 3 of GB/T3049.
4.6.3 Instruments and equipment
4.6.3.1 Spectrophotometer: with an absorption cell with a thickness of 1 cm. 4.6.4 Analysis steps
4.6.4.1 Drawing of working curve
According to Article 5.3 of GB/T3049, select an absorption cell with a thickness of 1 cm and the corresponding amount of iron standard solution, and draw the working curve.
4.6.4.2 Determination
Weigh 2g of the sample (accurate to 0.01g), place it in a 250mL beaker, add 2mL of ethanol to moisten the sample, add 9mL of hydrochloric acid solution (4.6.2.1) to dissolve the sample, heat and boil for 2min, filter while hot, collect the filtrate and washings in a 250mL volumetric flask after cooling, add water to the scale, and shake well. Use a pipette to transfer 25mL of the test solution into a 100mL beaker, and at the same time take 1mL of hydrochloric acid solution (4.6.2.1) into another beaker as a blank. The following operations are in accordance with Article 5.4 of GB/T3049, starting from "If necessary, add water to 60mL".
4.6.5 Expression of analysis results
Same as Article 4.6.5 of HG/T2226.
4.6.6 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result, and the absolute difference of the parallel determination results shall not exceed 0.01%. 4.7 Determination of manganese content
4.7.1 Method summary
Same as Article 4.7.1 of HG/T2226.
4.7.2 Reagents and materials
4.7.2.1 Nitric acid (GB626) solution: 1+1; the rest is the same as Article 4.7.2 of HG/T2226.
4.7.3 Instruments and equipment
Same as Article 4.7.3 of HG/T2226.
4.7.4 Analysis steps
4.7.4.1 Drawing of working curve
Same as Article 4.7.5 of HG/T2226.
4.7.4.2 Determination
Weigh about 2g of sample (accurate to 0.01g), place it in a 250mL tall beaker, add 7mL of nitric acid solution to dissolve the sample, heat and boil for 2min; filter with medium-speed quantitative filter paper, take 80mL of hot water for 5 times of washing, and collect the filtrate and washing liquid in a 250mL beaker.
HG/T2567—94
Take another 6mL of nitric acid solution in a beaker, adjust it to neutrality with ammonia water, and then add 1mL of nitric acid solution as a blank test solution. Operate the test solution and the blank test solution according to Article 4.7.6 of HG/T2226 at the same time, starting from "according to the provisions of Article 4.7.5" to "find out the manganese content in the sample". 4.7.5 Expression of analysis results
Same as Article 4.7.7 of HG/T2226.
4.7.6 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result, and the absolute difference of the parallel determination results shall not exceed 0.001%. 4.8 Determination of whiteness
Same as Article 4.9 of HG/T2226.
4.9 Determination of oil absorption value
4.9.1 Reagents and materials
Dioctyl phthalate (DOP).
4.9.2 Instruments and equipment
4.9.2.1 Spatula: 178mm long, 7~8mm wide; 4.9.2.2 Glass plate or glazed porcelain plate: 20×20cm; 4.9.2.3 Dropper bottle: 60mL.
4.9.3 Analysis steps
Weigh 5g of sample (accurate to 0.01g), place it on a glass plate or glazed porcelain plate, add DOP with a dropper of known weight containing DOP, and use a spatula to continuously turn and grind. At first, the sample is dispersed, and then gradually forms a mass until it is completely wetted by DOP. The end point is when a whole mass is formed. Weigh the mass of the dropper, accurate to 0.01g. 4.9.4 Expression of analysis results
The oil absorption value X2 expressed as the mass of DOP absorbed by every 100g of active calcium carbonate (g) is calculated according to formula (2): Xz = (m = m2) × 100
Wherein, m1—the mass of the dropper and DOP before adding DOP, g; m2—the mass of the dropper and DOP after adding DOP, g; m——the mass of the sample, g.
4.9.5 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result, and the absolute difference of the parallel determination results shall not exceed 1.0g/100g. 4.10 Determination of activation degree
4.10.1 Summary of method
The surface coating degree of calcium carbonate is determined by utilizing the hydrophobic characteristics of calcium carbonate after surface treatment. 4.10.2 Instruments and equipment
4.10.2.1 Pear-shaped separatory funnel: 250mL; 4.10.2.2 filter: pore size 5~15μm. 4.10.3 Analysis steps
Weigh 5g of sample (accurate to 0.01g), place it in a 250mL separatory funnel, add 200mL of water, shake it back and forth at a speed of 120 times/min for 1min, and gently place it on the funnel stand. Let it stand for 2030min. When the layers are clearly separated, put the precipitated calcium carbonate into a filter that has been dried to constant weight at 105±5℃. Remove water by suction and transfer to a constant temperature box to dry to constant weight at 105±5℃. 4.10.4 Expression of analysis results
Activation degree X expressed as mass percentage: Calculate according to formula (3): 5
WHG/T2567-94
Xs=[1 -mz=m]× 100
Where: m2——mass of crucible and uncoated calcium carbonate after drying, g; m1——mass of crucible, g;
m——mass of sample, g.
4.10.5 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 2%. 5 Inspection rules
5.1 Industrial activated precipitated calcium carbonate shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that all products shipped meet the requirements of this standard. Each batch of products shipped shall be accompanied by a quality certificate. The content includes the manufacturer's name, address, product name, type of activator, grade, net weight, batch number or production date, proof that the product quality meets this standard and the standard number. 5.2 The user has the right to inspect and accept the industrial activated precipitated calcium carbonate received in accordance with the provisions of this standard. 5.3 Each batch of products shall not exceed 40t.
5.4 Determine the number of sampling units in accordance with the provisions of Article 6.6 of GB/T6678. When sampling, insert the sampler vertically from the center of the packaging bag to 3/4 of the depth of the material layer to collect samples. After mixing the collected samples, reduce them to about 500g according to the quartering method, and pack them in two clean and dry wide-mouth bottles with stoppers and seal them. A label is attached to the bottle, indicating the manufacturer's name, product name, grade, batch number, sampling date and the name of the sampler. One bottle is used for inspection and the other is kept for three months for future reference. 5.5 If one of the test results does not meet the requirements of this standard, the sample should be re-tested from twice the amount of packaging. Even if only one of the test results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.6 When the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 5.7 The rounded value comparison method specified in GB1250 shall be used to determine whether the test results meet the standards. 6 Marking, packaging, transportation, storage
6.1 The packaging bag of industrial activated precipitated calcium carbonate should have firm and clear markings, including the manufacturer's name, address, product name, trademark, grade, net weight, batch number or production date, this standard number and the "wet-afraid" mark specified in GB191. 6.2 Industrial activated precipitated calcium carbonate adopts two packaging methods. 6.2.1 Double-layer packaging: The inner packaging is made of polyethylene plastic film bags, with specifications and dimensions: 850~950mm×500~650mm, and a thickness of 0.03~0.05mm; the outer packaging is made of plastic woven bags, with specifications and dimensions: 800~900mm×500~650mm. Its performance and inspection methods should comply with the provisions of GB8946B. The net weight of each bag of this product is 25kg and 40kg. 6.2.2 Single-layer packaging: Use type B composite plastic woven bags specified in GB8947, with specifications and dimensions: 850～950mm×500~650mm, and a thickness of 0.03~0.05mm, its performance and inspection methods shall comply with the provisions of GB8947B. The net weight of each bag of this product is 25kg and 40kg.
6.3 When industrial active precipitated calcium carbonate is double-layered, the inner bag is tied with vinyl rope or other ropes of equivalent quality, or sealed with other equivalent methods; the outer bag is folded at a distance of not less than 30mm from the bag edge, and the mouth is sewn with vinyl thread or other threads of equivalent quality at a distance of not less than 15mm from the bag edge. The stitch length is 7-12mm, the stitches are neat and the stitch length is uniform. There is no leakage and skipping. 6.4 Industrial active precipitated calcium carbonate should be covered during transportation to prevent rain and moisture. It shall not be mixed with acid. 6.5 Industrial active precipitated calcium carbonate should be stored in a cool and dry place to prevent rain, moisture, sunlight and heat. It shall not be mixed with acid. 6
W.bzsoso.coIAdditional Notes:
HG/T2567—94
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Tianjin Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Zhejiang Linghu Chemical Plant, Tangshan Dong Mineral Chemical Plant, Jiangsu Taicang Calcium Carbonate Plant, Chongqing Songshan Chemical Plant and Hubei Huangshi Chemical Plant. The main drafters of this standard are Yao Jinjuan, Shen Huifang, Jiang Bogeng, Tao Pinqiu, Wang Yuanming and Fan Baoxiang. 7
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