Some standard content:
Chemical Industry Standard of the People's Republic of China
Tribasic Lead Sulfate
1 Subject and Remote Application Model
HG 2240-82
This standard specifies the technical requirements, test methods, inspection and measurement, marking, packaging, transportation and storage of tribasic lead sulfate products.
This standard applies to powdered tribasic lead sulfate directly produced by the yellow lead flotation method with sulfuric acid. This product is mainly used as a heat stabilizer for chloroform.
Molecular formula. 3Pb0·PbSO,*H,0
Molecular weight: 990.87 (according to the International Atomic Energy Agency in 1987) 2 Standards
Chemical reagent titration analysis (volume analysis) standard solution preparation GB603
Chemical reagent test method preparation of preparations and products GB6682 Laboratory water specifications
3 Technical requirements
3.1 Appearance, superior and first-class products are white powder, qualified products are white or slightly yellow powder, without obvious organic impurities. 3.2 Technical indicators: Tribasic lead hydroxide should meet the requirements of Table 1. Table 1
Lead content (in terms of PbO), %
Sulfur trioxide (SOs), weak
Heating loss, %
Sieve residue (754m sieve), 9
Test method
Superior quality
B8,0~80,0
7,5~B,6
First quality
88.0~90.0
7,5~8,5
Qualified quality
B7,50,5
The standard titration solutions, preparations and products used in this standard shall be prepared in accordance with the provisions of GB601 and GB603 unless otherwise specified.
The experimental materials in this standard shall comply with the specifications of Grade 3 water in GB6682. Approved by the Ministry of Chemical Industry of the People's Republic of China on September 1, 1892 and implemented on July 1, 1993
4.1 Determination of lead content (in terms of FbO)
4.1.1 Principle of the method
HG 2340--92
After the sample is incubated with ethyl ammonium, it is placed in a medium with H=66 and the lead is titrated with disodium ethylenediaminetetraacetic acid (EDTA) standard titration solution using xylenol orange as an indicator. 4.1.2 Reagents and materials
4.1.2.1 Ethyl ammonium: 300g/L solution.
4.1.2.2 EDTA standard titration solution: (EDTA) = 0.04mol/L4.1.2.3 Xylenol as an indicator: 2g/L. 4.1,8 Analysis steps
Weigh 0.3 g of the sample (accurate to 00001 g) and place it in a 250 mL conical flask, add 15 mL of acetic acid, heat and decompose. After cooling, add 50 mL of water, add 3 to 5 drops of dimethyl orange, and titrate with EDTA standard until the solution changes from red to bright yellow, which is the end point.
4.1.4 Expression of results
Lead content is expressed as the mass percentage of lead monoxide (Pbo), calculated according to formula (1): X± -.*0.2232~ +100..
where c is the actual liquid concentration of EDTA standard titration solution, mol/L, the amount of EDTA standard filtration solution,
the area of the sample, B
0.2232 is the mass of lead monoxide expressed in grams equivalent to 1.00ml EDTA standard titration solution [c(EDTA)=1.000mol/L].
4.1.5 It is allowed that the difference between the results of two parallel determinations shall not exceed 0.4%, and the arithmetic mean shall be taken as the determination result. 4.2 Determination of the amount of sulfur dioxide
4.2.1 Reagents and materials
4.2.1.1 Nitrilotriacetic acid, 20g/L solution. Weigh 20g of nitrilotriacetic acid and dissolve it in an appropriate amount of water without carbon dioxide. Add 3-4 drops of neutral red-methylene blue as a combined indicator and add 8% sodium hydroxide to dissolve the nitrilotriacetic acid. Then adjust the solution to a blue color with 0.1mol/L sodium hydroxide solution and the pH value to about 6.B7.0 (or adjust the pH directly with an acidometer). Then dilute to 1000ml for use. The pH value of the nitrilotriacetic acid solution should be checked once a month. 4.2.1.2 Standard hydrochloric acid titration solution: c (HC1) = 0.1mol/L. 4.2.1.3 Oxycresol green and dimethyl red mixed indicator, 3 parts of 10g/L nitrilotriacetic green ethanol solution and 1 part of 20g/L methyl red ethanol solution are mixed evenly.
4.2.1.1 Neutral red-methylene blue mixed indicator: Mix 1 part of 10g/L neutral red alcohol solution and 1 part of 10g/L methylene blue beta solution.
4.2.2 Analysis steps
Weigh 0.5ml of the sample (accuracy 0.0001g), place it in a 250ml conical flask, and use a small amount of this to dehumidify the sample. Add 30ml of nitrotriacetic acid bath, heat and decompose. After cooling, add 46 drops of cresol green-methyl red mixed indicator, and titrate with 0.1ml/L salt 1146
HG 2840--92
standard difficult titration solution until the solution changes from yellow to purple, which is the end point. At the same time, perform a blank test. 4.2.8 Expression of results
The content of sulfur trifluoride (SO4) is expressed as mass percentage X, and is calculated according to formula (2): Ya
wherein, X is the lead content,
c*(V1 -V2) ×0.2232×100
is the actual concentration of the hydrochloric acid standard titration solution, mol/LV—→the amount of hydrochloric acid standard titration solution consumed by the sample, mlV. The amount of hydrochloric acid standard titration solution consumed by the blank, ml, m is the mass of the sample, 8
X0,3587 -...
0.2232 is the mass of the oxidant in grams equivalent to 1.00 ml of the hydrochloric acid standard titration solution (Cc(HC1)=1.000 mol/L),
is the conversion constant for lead trioxide and lead monoxide. 4.2.4 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.2%, and the arithmetic mean shall be taken as the determination result. 4.8 Determination of heating loss
4.8.1 Instruments and equipment bzxz.net
4.8.1.1 Weighing bottle: 450×30
4.8.1.2 Oven: sensitivity is ±2℃. 4.8.t. Dryer, with appropriate desiccant (gelatin). 4.3.2 Analysis steps
Weigh 10g of sample (accurate to 0.0001z), dry it in advance at 105~110℃ into a weighing bottle of Henghui, move it into the oven, and open the bottle cap. Make the sample surface to be tested in the weighing bottle and the mercury ball of the oven thermometer at the same level, and the vertical distance shall not exceed 100mm. Keep the temperature at 105-110℃ for 2 hours, put the bottle on the weighing plate, take out the weighing plate bottle, place it in a desiccator, cool it to room temperature (not less than 30 minutes), and weigh it. 4.8.3 Expression of results
The heating mass is expressed as a percentage of mass, and Xa is calculated according to formula (3): a. ×100.
Where m is the mass of the weighing bottle and the sample before drying, and the mass of the weighing bottle and the sample after drying, and the heating mass is the mass of the sample, 8.
4.3.4 The allowable error
The difference between the results of two parallel determinations shall not exceed 0.08%, and the arithmetic mean is the determination result. 4.4 Determination of residual matter
4.4.1 Instruments and equipment
4.4.1.1 Test sieve: Φ76×25/0.075. ()
HG 2340--92
4.4.1.2 Soft brush: bristle length is about 30mm, width is about 30mml. ). 4.1.3 Drying, sensitivity is ±2℃. ,4,1.4 Desiccator, with appropriate desiccant (such as silica gel) inside. 4.4,2 Analysis steps
Weigh 50g sample (accurate to 0.01g), cover it in a 240ml grid, add water to mix, then pour it into the test sieve, carefully rinse it with a self-cleaning and soft brush, so that all the sample that can pass through the sieve can pass through the sieve. After rinsing, place the sieve residue together with the test sieve in an oven, dry it at 105-110℃ for 1h, take it out and place it in a dryer, cool it to room temperature (not less than 30min), then put all the sieve residue into a constant weight surface and weigh it. 4.4.8 Expression of the result
The residue on sieve is expressed as a mass percentage X. It is calculated according to formula (4): X,=-- ×100..
Where n, is the mass of the residue on sieve after drying, and n is the mass of the sample, B.
Instrument inspection regulations
5.1 Tribasic lead sulfate shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that each batch of products shipped from the factory meets the technical requirements specified in this standard.
5.2 The user may accept the received tribasic lead sulfate according to the provisions of this standard. .$ Tribasic lead sulfate products are produced daily as one batch. 5,When sampling, determine the number of sampling units according to Table 2
The number of single dead units of the total material
50~64
82~101
102~155
The minimum number of sampling units
, 5 Sampling method: Insert a U-shaped gold tube sampling probe from top to bottom into 2/3 of the material, turn it three times and carefully withdraw the probe, pour the sample in the probe into a dry and clean container, mix the sample evenly, divide it into two bottles, tighten the bottle caps, paste labels, and indicate the manufacturer name, product name, batch number, sampling date and sampler. One of the bottles is inspected by the quality inspection department, and the other is stored for six months for reference. The sample volume of each bottle should be at least three times the required plate for testing. 5. If the inspection result does not meet the requirements of this standard, samples should be taken from the packaging of the batch for inspection. If one of the indicators still does not meet the requirements of this standard, the whole batch of products cannot be accepted. 5.1 When the supply and demand parties have objections to the quality of the products, arbitration can be carried out in accordance with this standard. The arbitration institution shall be selected by both parties through consultation. 1148
Reference Marking, Packaging, Transportation, Storage
HG2340-92
6.1 Packaging of lead tribasic sulfate: plastic woven plastic film bag. The name of the manufacturer, product name, standard, grade, net weight and production date should be marked on the bag. Each batch of packaged products should be accompanied by a product certificate, which includes: manufacturer name, product name, batch number, technical indicators and this standard number. Each bag has a net weight of 25kg. 6.2 Prevent damage during transportation, and the packaging line shall not be damaged. 6. Tribasic lead sulfide should be stored in a dry and well-ventilated place. It should not be piled up in the open air to prevent moisture. The storage period is half a year.
This standard is 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 Shanxi Chemical Research Institute. This standard was drafted by the State-owned Yizhou Additive Factory of Wenzhou Plastic Additives Industrial Group Co., Ltd. The main drafters of this standard are Chen Zhenzhen, Lin Xuejin, Li Junqing, and the former Ministry of Chemical Industry issued standard HG2-1053-77 "Tribasic Lead Sulfate" from the date of implementation of this standard.
Tribasic Lead Sulfate Industry Standard (HG2340-92) Explanation This standard applies to powdery tribasic lead sulfide synthesized directly by adding sulfuric acid to the yellow lead flotation method. The product is white or gray powder, with a density of 7.1, a refractive index of 2.1, a sweet and toxic taste, easy to absorb moisture, no flammability and corrosion, does not fall into water, can dissolve in hot ammonium acetate solution, loses crystal water above 200°C, and will discolor and decompose when exposed to sunlight when humid. It should be stored and transported in a moisture-proof manner and must not be piled in the open air. It has excellent heat resistance and electrical insulation. The product is suitable for opaque high-temperature processed ethylene hard pipes, plate products, injection molded products, artificial leather and other relatively hard products, and can also be used as a pigment for coatings. Generally, the maximum concentration is 8%. Process route:
Dai Dan→
(Wu Hua Guo)
Reaction or:
HAcHso,Ho
He Qi→washing and drying
2PhO+ 2HAc-Pb(OH), + Pb(Ac)2Pb(OH) - Pb(Ae), + 2H,SO,-2PbSO, + 2HAc2PbSO,+BPbO+H,0-+2(3PbO.PbSo,H20J crushing
Manufacturers include Beijing Chemical Plant No. 8, Tianjin Red Star Chemical Plant, Dandong Zhen'an District Langtou Commune Chemical Plant, Dandong.1149
HG 2840—$2
Zhen'an Chemical Factory, Jiangsu Huaiyin County Chemical Factory, Lijing Jinling Chemical Factory, Zhejiang Wenyan Shuguang Chemical Factory, Lanzhou Dianliao Chemical Factory, Jiaxing Chemical Factory No. 2, Wuhu Smelting Comprehensive Factory, Bengbu Xinxing Chemical Factory, Jinan Xiaohe Chemical Factory, Qingdao Chengyang Chemical Factory, Xiangtan Zhijin Chemical Factory, Guangdong Chao'an Plastic Material Factory, Guangxi Wuzhou Xumin Chemical Factory, Chongqing Changjiang Chemical Factory, Xi'an Taqu Light Chemical Company Xingguang Chemical Factory, Yaozhou Wangliao Additive General Factory, Fuzhou Chemical Raw Materials Factory, Shenyang Additive Factory, etc. The output, calculated based on the five factories that won the Ministry of Quality Products in 1989, is 5,000 tons/year. Among them, some products of Shenyang Additive Factory and Nan'ai Jinfu Chemical Factory are exported to seven countries in Southeast Asia, including Pakistan, Japan, and Bangladesh. This standard refers to the standards of Japan Pinqi Company. The superior products are based on the technical indicators of the Ministry of Quality Products in 1989, reaching the advanced level abroad, and the first-class products are based on the technical indicators of the Ministry of Quality Products in 1989, reaching the advanced level abroad, and the first-class products are based on the technical indicators of the Erben Pinchuan Company. Technical standards, reaching the general level of foreign countries. The test methods of lead oxide content and mercury trioxide content have been compared by many manufacturers and users, and this standard method, which is based on the original standard, has been selected. It is considered to be superior to the method of Japan's Shinagawa Company.
Technical conditions for high-quality products of tribasic lead thioaldehyde (1989) Item
Total lead content (chemical lead), %
Blue sulfur oxide, response
Heating loss (1051 10%℃、1h), %
Sieve product (200m),
In 1989, it won the title of Quality Product Enterprise of Tri-base Research and Development Department, Shenfu Additive Factory
Haijin Chemical Factory.
Lanjing Jinling Chemical Factory
Self-colored powder, no bright and evil impurities.
29.0±1,0
Chongqing Changjiang Chemical Factory
Zhouzhou Plastic Additive Factory
Xiangtan City1149
HG 2840—$2
Zhen'an Chemical Factory, Jiangsu Huaiyin County Chemical Factory, Lijing Jinling Chemical Factory, Zhejiang Wenyan Shuguang Chemical Factory, Lanzhou Dianliao Chemical Factory, Jiaxing Chemical Factory No. 2, Wuhu Smelting Comprehensive Factory, Bengbu Xinxing Chemical Factory, Jinan Xiaohe Chemical Factory, Qingdao Chengyang Chemical Factory, Xiangtan Zhijin Chemical Factory, Guangdong Chao'an Plastic Material Factory, Guangxi Wuzhou Xumin Chemical Factory, Chongqing Changjiang Chemical Factory, Xi'an Taqu Light Chemical Company Xingguang Chemical Factory, Yaozhou Wangliao Additive Factory, Fuzhou Chemical Raw Materials Factory, Shenyang Additive Factory, etc. The output, based on the five factories that won the Ministry of Quality Products in 1989, is 5,000 tons/year. Among them, some products of Shenyang Additive Factory and Nan'ai Jinfu Chemical Factory are exported to seven countries in Southeast Asia, including Pakistan, Japan, and Bangladesh. This standard refers to the standards of Japan's leading product company. The superior products are in accordance with the technical indicators of the Ministry of Quality Products in 1989, reaching the advanced level abroad. The first-class products are in accordance with the technical standards of Japan's Shinagawa Company, reaching the general level abroad. The test methods of lead oxide content and mercury trioxide content have been compared by many manufacturers and users, and this standard method, which is improved on the basis of the original Ministry's standards, has been selected. It is considered to be superior to the method of Japan's Shinagawa Company.
Technical conditions for high-quality products of tribasic lead thioaldehyde (1989) Item
Total lead content (chemical lead), %
Blue sulfur oxide, response
Heating loss (105110%℃, 1h), %, %
Sieve material (200m),
Won the title of the Ministry of Quality Products Enterprise of Tribasic Lead in 1989, Shenfu Auxiliary Agent Factory
Haijin Chemical Factory.
Lanjing Jinling Chemical Factory
Self-colored powder, no dark and evil impurities.
29.0±1,0
Chongqing Changjiang Chemical Factory
Zhouzhou Plastic Additives Factory
Xiangtan City1149
HG 2840—$2
Zhen'an Chemical Factory, Jiangsu Huaiyin County Chemical Factory, Lijing Jinling Chemical Factory, Zhejiang Wenyan Shuguang Chemical Factory, Lanzhou Dianliao Chemical Factory, Jiaxing Chemical Factory No. 2, Wuhu Smelting Comprehensive Factory, Bengbu Xinxing Chemical Factory, Jinan Xiaohe Chemical Factory, Qingdao Chengyang Chemical Factory, Xiangtan Zhijin Chemical Factory, Guangdong Chao'an Plastic Material Factory, Guangxi Wuzhou Xumin Chemical Factory, Chongqing Changjiang Chemical Factory, Xi'an Taqu Light Chemical Company Xingguang Chemical Factory, Yaozhou Wangliao Additive Factory, Fuzhou Chemical Raw Materials Factory, Shenyang Additive Factory, etc. The output, based on the five factories that won the Ministry of Quality Products in 1989, is 5,000 tons/year. Among them, some products of Shenyang Additive Factory and Nan'ai Jinfu Chemical Factory are exported to seven countries in Southeast Asia, including Pakistan, Japan, and Bangladesh. This standard refers to the standards of Japan's leading product company. The superior products are in accordance with the technical indicators of the Ministry of Quality Products in 1989, reaching the advanced level abroad. The first-class products are in accordance with the technical standards of Japan's Shinagawa Company, reaching the general level abroad. The test methods of lead oxide content and mercury trioxide content have been compared by many manufacturers and users, and this standard method, which is improved on the basis of the original Ministry's standards, has been selected. It is considered to be superior to the method of Japan's Shinagawa Company.
Technical conditions for high-quality products of tribasic lead thioaldehyde (1989) Item
Total lead content (chemical lead), %
Blue sulfur oxide, response
Heating loss (105110%℃, 1h), %, %
Sieve material (200m),
Won the title of the Ministry of Quality Products Enterprise of Tribasic Lead in 1989, Shenfu Auxiliary Agent Factory
Haijin Chemical Factory.
Lanjing Jinling Chemical Factory
Self-colored powder, no dark and evil impurities.
29.0±1,0
Chongqing Changjiang Chemical Factory
Zhouzhou Plastic Additives Factory
Xiangtan City
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