HG/T 2776-1996 Industrial ultrafine calcium carbonate and ultrafine activated calcium carbonate
Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2776—1996
Industrial Ultrafine Calcium Carbonate and
Industrial Ultrafine Activated Calcium Carbonate
Published on January 24, 1996
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1997
WHG/T2776—1996
In this standard, the superior ultrafine activated calcium carbonate is equivalent to the specifications of well-known foreign companies. The main technical differences are as follows: 1 This standard includes industrial ultrafine calcium carbonate and industrial ultrafine activated calcium carbonate. 2 This standard divides industrial ultrafine calcium carbonate into two grades. Industrial ultrafine activated calcium carbonate is divided into three grades. According to my country's national conditions and user requirements, hydrochloric acid insoluble matter replaces silicon dioxide, and iron replaces iron-aluminum oxide. 3
In terms of test methods, this standard adopts the standard methods of similar products in my country: the determination of calcium oxide and magnesium oxide content adopts the classic EDTA complexometric titration method. The determination of hydrochloric acid insoluble matter, volatile matter at 105℃, pH value, whiteness and oil absorption adopts the methods specified in HG/T2226-91 "Industrial precipitated calcium carbonate" and HG/T2567-94 "Industrial active precipitated calcium carbonate". The determination of specific surface area adopts the method specified in GB/T2922-82 "Method for determination of specific surface area of chromatographic carriers of chemical reagents". The determination of density adopts the method specified in GB/T4472-84 "General rules for determination of density and relative density of chemical products". The determination of iron adopts GB/T3049-86 "General method for determination of iron content in chemical products - o-phenanthroline spectrophotometry". The determination of loss on ignition adopts the classic method. This standard is 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. The drafting units of this standard are: Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Zhejiang Linghua Enterprise Group Co., Ltd., Guangdong Guangping Chemical Industry Co., Ltd., Sichuan Chongqing Songshan Chemical Plant, Shandong Zibo Huaxin Chemical Co., Ltd. The main drafters of this standard are: Yao Jinjuan, Shen Huifang, Wu Hanyuan, Mi Chuantao, Pu Chaoyu. I
W.1 Scope
Chemical Industry Standard of the People's Republic of China
Industrial Ultrafine Calcium Carbonate and
Industrial Ultrafine Activated Calcium Carbonate
HG/T2776—1996
This standard specifies the requirements, sampling, test methods, marking, packaging, transportation and storage of industrial ultrafine calcium carbonate and industrial ultrafine activated calcium carbonate.
This standard applies to industrial ultrafine calcium carbonate produced by precipitation method using limestone as raw material and industrial ultrafine activated calcium carbonate produced by precipitation method using limestone as raw material and surface treated with activators and specially processed. This product is mainly used as filler for plastics, rubber, etc.
Molecular formula: Industrial ultrafine calcium carbonate: Ca2COsRelative molecular weight: Industrial ultrafine calcium carbonate: 100.09 (according to the 1991 international relative atomic mass). 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and the parties using this standard should explore the possibility of using the latest versions of the following standards. GB191-90 Pictorial marking for packaging, storage and transportation
GB/T601-88 Preparation of standard solution for titration analysis (volume analysis) of chemical reagents GB/T602-88 Preparation of standard solution for determination of impurities of chemical reagents (neqISO6353/1:1982) GB/T603-88 Preparation of preparations and products used in test methods for chemical reagents (neqISO6353/1:1982) GB/T1250-89 Method for expressing and determining limit values GB/T2922-82 Method for determining specific surface area of chromatographic carriers for chemical reagents GB/T3049-86 General method for determination of iron content in chemical products - o-phenanthroline spectrophotometric method (neqIS O6685:1982)
General rules for determination of density and relative density of chemical products GB/T4472—841
GB/T6678—86
6 General rules for sampling of chemical products
GB/T6682—92
GB/T8946—88
GB/T2226—91
Specifications and test methods for water used in analytical laboratories (eqvISO3696:1987)Plastic woven bags
Industrial precipitated calcium carbonate
4 Industrial activated precipitated calcium carbonate
GB/T2567—94
3 Requirements
3.1 Appearance: white powder.
3.2 Industrial ultrafine activated calcium carbonate and industrial ultrafine calcium carbonate shall meet the requirements of Table 1: Approved by the Ministry of Chemical Industry of the People's Republic of China on January 24, 1996 and implemented on January 1, 1997
W.bzsoso.coI Item
Calcium oxide (CaO) content, %
Magnesium oxide (MgO) content, %
Hydrochloric acid insoluble matter content, %
Iron (Fe ) content, %
Volatile matter content at 105℃, %
pH (100g/L suspension)
Whiteness, degree
Specific surface area, m/g
Density, g/cm2
Average particle size, um
Oil absorption, mL/100g
Loss on ignition, %
4 Sampling
4.1 Each batch of products shall not exceed 60t.
HG/T2776—1996
Requirements in Table 1
Industrial ultrafine activated calcium carbonate
Superior quality
First quality
8.5—10.0
43.0—45.5
Qualified quality
8.5—11.0
Industrial ultrafine calcium carbonate
First quality
Qualified quality
8.5—10.0
2.55—2.65
4.2 Determine the number of sampling units in accordance with the provisions of 6.6 of GB/T6678. When sampling, insert the sampler obliquely from the top of the packaging bag to 3/4 of the material layer depth to take a sample. After mixing the sample, divide it into about 500g according to the quartering method, and pack it into two clean and dry wide-mouth bottles with stoppers and seal them. Paste labels on the bottles, indicating: manufacturer name, product name, category, batch number, sampling date and name of the sampler. One bottle is used as a laboratory sample, and the other bottle is kept for three months for reference. 4.3 If one of the test results does not meet the requirements of this standard, re-sample from twice the amount of packaging for verification. If even one of the verification results does not meet the requirements of this standard, the entire batch of products will be unqualified. 5 Test methods
5.1 All twelve index items specified in this standard are type test items, of which calcium oxide content, magnesium oxide content, hydrochloric acid insoluble content, iron content, volatile matter content at 105℃, pH, whiteness, oil absorption, and ignition loss are routine test items and should be tested batch by batch. Under normal production conditions, type tests shall be conducted at least once every three months. 5.2 The rounded value comparison method specified in GB/T12505.2 shall be used to determine whether the test results meet the standard. 5.3 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 solutions, impurity standard solutions, preparations and products used in the test, unless otherwise specified, shall be prepared in accordance with the provisions of 2
W.HG/T2776-1996
GB/T601, GB/T602 and GB/T603. 5.4 Determination of calcium oxide content
5.4.1 Summary of the method
A small amount of trivalent iron, trivalent aluminum and divalent manganese ions shall be masked with triethanolamine. At a pH of 12.5, calcium reagent carboxylate sodium salt shall be used as an indicator and calcium ions shall be titrated with disodium ethylenediaminetetraacetic acid standard titration solution. 5.4.2 Reagents and materials
5.4.2.195% ethanol;
5.4.2.2 Hydrochloric acid solution: 1+1;
5.4.2.3 Sodium hydroxide solution: 100g/L
Triethanolamine solution: 1+3;
Standard titration solution of disodium ethylenediaminetetraacetate (EDTA): C(C1oHiuOgN2Na2) about 0.02mol/L5.4.2.5
5.4.2.6 Calcium reagent carboxylic acid sodium salt [1-(2-hydroxy-4-sulfonyl-1-naphthylazo)-2-hydroxy-3-naphthoic acid): 1% (m/m) solid indicator;
Grind the calcium reagent carboxylic acid sodium salt indicator and sodium chloride in a mortar in a ratio of 1+99 and mix thoroughly, and store in a wide-mouth bottle with a ground-mouth stopper.
5.4.3 Analysis steps
Weigh about 0.6g of the sample (accurate to 0.0002g) dried at 105℃ to constant weight is placed in a 250mL beaker. A small amount of ethanol is added to the ultrafine active calcium carbonate to moisten the sample, and a small amount of water is added to the ultrafine calcium carbonate to moisten the sample. Cover the surface blood and drip hydrochloric acid solution until the sample is completely dissolved. Add 50mL of water, transfer all into a 250mL volumetric flask, dilute to the scale with water, shake well, and obtain test solution A. This solution is used to determine the content of calcium oxide and magnesium oxide.
Use a pipette to transfer 25mL of test solution A, place it in a 250mL conical flask, add 30mL of water and 5mL of triethanolamine solution, and add sodium hydroxide solution dropwise while shaking. When the solution just becomes turbid, add a small amount of calcium reagent sodium carboxylate indicator, and continue to drip sodium hydroxide solution until the test solution changes from blue to wine red, with an excess of 0.5mL, and titrate with disodium ethylenediaminetetraacetic acid standard titration solution until the solution changes from wine red to pure blue. Perform a blank test at the same time. 5.4.4 Expression of analysis results
Calcium oxide (CaO) content X expressed as mass percentage is calculated according to formula (1): _(Vi-Vo): cX0. 056 08×
56.08(Vi-Vo).c
Wherein: c——actual concentration of disodium ethylenediaminetetraacetic acid standard titration solution, mol/L; V1——volume of disodium ethylenediaminetetraacetic acid standard titration solution consumed in titration, mL; V.——volume of disodium ethylenediaminetetraacetic acid standard titration solution consumed in blank titration, mL; m——mass of sample, g;
0.05608——mass of calcium oxide in grams equivalent to 1.00mL disodium ethylenediaminetetraacetic acid standard titration solution c(C1oH1uO:N2Na2)=1.000mol/L).
5.4.5 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.2%. 5.5 Determination of magnesium oxide content
5.5.1 Summary of method
W.bzsosO.cOHG/T2776—1996
A small amount of trivalent iron, trivalent aluminum and divalent manganese ions shall be masked with triethanolamine. When the pH is 10, chrome black T is used as an indicator and the total amount of calcium and magnesium is titrated with disodium ethylenediaminetetraacetic acid standard titration solution. The calcium content is subtracted from it to calculate the magnesium oxide content. 5.5.2 Reagents and materials
5.5.2.1 Triethanolamine solution: 1+3;
5.5.2.2 Ammonia-ammonium chloride buffer solution A: pH~10; 5.5.2.3 Disodium ethylenediaminetetraacetic acid (EDTA) standard titration solution c (CioHuOgN2Na2), about 0.02 mol/L; 5.5.2.4 Eriochrome black T solid indicator: 1% (m/m); 5.5.3 Analysis steps
Use a pipette to transfer 25 mL of test solution A (5.4.3) into a 250 mL conical flask, add 50 mL of water, 5 mL of triethanolamine solution, 10 mL of buffer solution and a small amount of chromium black T indicator, and titrate with disodium ethylenediaminetetraacetic acid standard titration solution until the solution changes from purple-red to pure blue.
5.5.4 Expression of analysis results
The magnesium oxide (Mgo) content X2 expressed as mass percentage is calculated according to formula (2): X2
(V2-V)cX0.04030
40. 3 (V2-V1)-c.
Wherein: c-
-actual concentration of disodium ethylenediaminetetraacetic acid standard titration solution, mol/L; V1--volume of disodium ethylenediaminetetraacetic acid standard titration solution consumed in titrating calcium in 5.4.3, mL; V2--volume of disodium ethylenediaminetetraacetic acid standard titration solution consumed in titration, mL; -mass of the sample weighed in 5.4.3, g;
0.04030--mass of magnesium oxide expressed in grams equivalent to 1.00mL disodium ethylenediaminetetraacetic acid standard titration solution [c (CioH1uOsN2Na2) = 1.000mol/L).
5.5.5 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 0.05%. 5.6 Determination of hydrochloric acid insoluble matter
Industrial ultrafine calcium carbonate shall be determined according to 4.4 of HG/T2226. Industrial ultrafine activated calcium carbonate shall be determined according to 4.4 of HG/T2567. 5.7 Determination of iron content
5.7.1 Method summary
According to Chapter 2 of GB/T3049.
5.7.2 Reagents and materials
According to Chapter 3 of GB/T3049 and 95% ethanol.
5.7.3 Instruments and equipment
According to Chapter 4 of GB/T3049.
5.7.4 Analysis steps
5.7.4.1 Drawing of working curve
According to 5.3 of GB/T3049, use a 1cm absorption cell and the corresponding iron standard solution to draw the working curve. 5.7.4.2 Preparation of test solution
Weigh about 2g of sample (accurate to 0.01g), place in a 250mL beaker, add 2mL of ethanol to moisten the sample, drop 4
WHG/T2776—1996
9mL of 1+1 hydrochloric acid solution 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 mark, and shake well.
5.7.4.3 Preparation of blank test solution
Except for not adding the sample, the amount of other reagents added is exactly the same as that of the test solution, and the same treatment is carried out at the same time as the sample. 5.7.4.4 DeterminationbZxz.net
Use a pipette to transfer 25mL of the test solution and blank test solution, and place them in 100mL beakers respectively. The following operations shall be in accordance with GB/T30495.4, starting from "add water to 60mL if necessary" to "measure the absorbance of the test solution and reagent blank solution".
5.7.5 Expression of analysis results
Same as 4.6.5 of HG/T2226.
5.7.6 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference between two parallel determinations shall not exceed 0.01%. 5.8 Determination of volatile matter content at 105℃
Determine in accordance with HG/T22264.3.
5.9 Determination of pH value
Industrial ultrafine calcium carbonate shall be determined in accordance with HG/T22264.2; industrial ultrafine activated calcium carbonate shall be determined in accordance with HG/T25674.2. 5.10 Determination of whiteness
Determine according to HG/T22264.9.
5.11 Determination of specific surface area
Weigh about 3g of sample (accurate to 0.01g), and determine according to the method specified in GB/T2922. 5.12 Determination of density
Use a 50mL specific gravity bottle, weigh about 10g of sample (accurate to 0.0002g), use ethanol as the determination medium, and determine according to GB/T44722.2.2.
5.13 Determination of average particle size
Take a calcium carbonate sample, use water as a solvent, disperse it with an ultrasonic oscillator, place it on the sample stage of an electron microscope, and take an electron microscope picture with a camera at a certain magnification. Under the photo, measure the particle size of no less than 20 particles along a certain direction. Average particle size X: calculated according to formula (3):
Wherein: a——the sum of particle diameters, um; N——magnification of electron microscope;
n——the number of particles measured.
5.14 Determination of oil absorption
5.14.1 Reagents and materials
Refined linseed oil: acid value is 5.0~7.0mgKOH/g; 5.14.2 Instruments and equipment
5.14.2.1 Spatula: length 178mm, width 7~8mm, 5.14.2.2 Glass plate or glazed porcelain plate: 20cm×20cm. 5.14.3 Analysis steps
(3)
Weigh about 5g of sample (accurate to 0.01g), place it on a glass plate or glazed porcelain plate, and add refined linseed oil with a burette. During the addition, use a spatula to continuously stir and grind. At first, the sample is dispersed, and then gradually forms a mass until it is completely wetted by the refined linseed oil. The end point is when a whole mass is formed. Record the volume of the added refined linseed oil. 5.14.4 Expression of analysis results
The oil absorption value X, expressed as the volume (mL) of refined linseed oil absorbed by every 100g of calcium carbonate, is calculated according to formula (4): V
Where: V is the volume of a drop of refined linseed oil, mL; m is the mass of the sample, g.
5.14.5 Allowable difference
.(4)
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference between two parallel determinations shall not exceed 1.0mL/100g. 5.15 Determination of loss on ignition
5.15.1 Analysis steps
Weigh about 0.5g of sample (accurate to 0.0002g), place it in a porcelain crucible that has been ignited to constant weight at 800-900℃, and ignite it at 800-900℃ to constant weight.
5.15.2 Expression of analysis results
The loss on ignition X expressed as a mass percentage is calculated according to formula (5): Xg=m=mz×100
Where: m1—mass of sample before ignition, g; m2—mass of crucible and sample after ignition, g; -mass of sample, g.
5.15.3 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.1%. 6 Marking, packaging, transportation, purchase and storage
(5)
6.1 The packaging of industrial ultrafine calcium carbonate and industrial ultrafine activated calcium carbonate shall be firmly and clearly marked, including: manufacturer name, factory 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 Each batch of industrial ultrafine calcium carbonate and industrial ultrafine activated calcium carbonate shipped from the factory shall be accompanied by a quality certificate. The contents include: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, proof that the product quality complies with this standard and this standard number.
6.3 Industrial ultrafine calcium carbonate and industrial ultrafine activated calcium carbonate are packaged in two ways. 6.3.1 Plastic woven bag packaging: The inner packaging adopts polyethylene plastic film bags with a thickness of 0.03-0.05mm; the outer packaging adopts plastic woven bags, and its performance and inspection methods shall comply with the provisions of Type A of GB/T8946. The net weight of each bag is 25kg. 6.3.2 Double-layer kraft paper bag packaging, its performance and inspection methods shall comply with relevant regulations. The net weight of each bag is 25kg. 6.4 When industrial ultrafine calcium carbonate and industrial ultrafine activated calcium carbonate are packaged in plastic woven bags, 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 opening is sewed with vinyl thread or other threads of equivalent quality at a distance of not less than 15mm from the bag edge. When kraft paper bags are used for packaging, the edges should be folded at 30mm from the bag edge, and the opening should be sewed 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. No leaking or jumpering.
6.5 Industrial ultrafine calcium carbonate and industrial ultrafine activated calcium carbonate should be covered during transportation to prevent rain and moisture. They must not be mixed with acids.
HG/T 2776—1996
Industrial ultrafine calcium carbonate and industrial ultrafine activated calcium carbonate should be stored in a dry and cool place to prevent rain and moisture. They must not be mixed with acids. 6.6
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