Some standard content:
GB 7816—1998 | To be revised.
The main differences between this standard and IOCT8986-1982 are: 11OC8986--1982 is divided into three levels: high-quality products and first-class products. 21CT8986-1982 sets four indicators. Three indicators are set according to user requirements, and there is no slag content indicator. The main differences between this standard and the original national standard are: 1. The indicators are divided into high-quality products and first-class products
2. The analysis method of arsenic content is the same as that of GB. /T7686-1987 "General Method for Determination of Arsenic Content in Chemical Products" National Standard.
3 Cylinder packaging has been canceled since the date of implementation. GB78161987.
Appendix A of this standard is a reminder.
This standard is drafted by the Ministry of Chemical Industry of the People's Republic of China. Units: Tianjin Chemical Industry Research Institute of the Ministry of Chemical Industry, Nanjing Chemical Industry Group Co., Ltd. Phosphate Fertilizer Plant, Yunnan Kunyang Phosphate Fertilizer Plant, Sanmenxia Chemical Plant, Guizhou Jinsha Yellow Phosphorus Plant, Hubei Xingfa Chemical Industry Group Co., Ltd., Guizhou Qiannan Prefecture Phosphate Ding Factory. The main drafters of this standard are: Yang Chengyin, Gong Ronglin, Li Jie, Guo Zhimin, Zhao Lianfang, Huang Huining, Lu Meixiang, and Li Guangming. This standard was first released in June 1987.
This standard was entrusted to the Ministry of Chemical Industry for inorganic salts. The responsible unit for product standardization technology is responsible for interpretation. 101
1 Scope
National Standard of the People's Republic of China
Industry
Yellow
Phosphorus
Yellow phosphorus for industrial useGB7816
—1998
Replaces GB7816—1987
This standard specifies the requirements, test methods, inspection rules, marking, and packaging of industrial yellow phosphorus , transportation, storage and safety. This standard applies to industrial yellow phosphorus produced by electric furnace method using phosphate rock as raw material. This product is mainly used to produce red phosphorus, phosphorus sulfide, phosphorus chloride and phosphoric acid.
Molecular formula: P or P
Relative molecular mass: 30.97 or 123.9 (according to the 1995 international relative atomic mass) 2 Reference standards
The provisions contained in the following standards are adopted in this standard The references in this standard constitute provisions of this standard. When this standard is published, the versions indicated are valid. All standards are subject to revision, and parties using this standard should explore the possibility of using the latest version of the following standards. |tt||GB191—1990
Dangerous goods packaging mark
Packaging, storage and transportation pictorial mark
GB/T 325—1991
GB/T 602—1988| |tt||GB/T 603--1988
GB/T 1250—1989
GB/T 6678---1986
GB/T 6682 --. 1992|| tt | Preparation of preparations and products used in the test method (neqISO6353-1:1982) Expression method and judgment method of limit values ??General principles for sampling of chemical products
Analytical laboratory water specifications and test methods (egvISO) 3696:1987) Chemical products General method for determination of arsenic content (eqyIS02590:1973) Industrial yellow phosphorus should comply with the requirements of Table 1
item
appearance
yellow phosphorus content, %
in extraction| |tt||In carbon disulfide
Insoluble matter content, %
In benzene
In carbon disulfide
Country
Table 1 requirements||tt ||refers to
high-quality products
paraffin, light yellow to slightly yellowish green
99.90
99.90
0.10
0.10|| tt||State Bureau of Quality and Technical Supervision approved 102 on October 19, 1998bzxZ.net
standard
first-class product
stone fin-shaped, yellow-green to brown-green
99.50| |tt||0.50
Implemented on 1999-04-01
4 test methods
GB 7816—1998
When required, it refers to analytically pure reagents and grade three water specified in GB/T6682. The standard titration solutions, impurity standard solutions, preparations and products used in the test shall be prepared in accordance with the provisions of GB/T602 and GB/T603 unless other requirements are specified.
Warning: The reagents such as yellow phosphorus and benzene used in the test are poisonous and should be handled with caution. 4.1 The appearance of the sample is determined visually,
4.2 Preparation of the sample: Use the device in Figure 1 to prepare the sample. Wear rubber gloves and place the sample cup containing yellow phosphorus into a water bath (see Figure 1) and heat it to about 70°C to melt the yellow phosphorus. Use a glass sampling tube with an inner diameter of 5mm or 6mm, insert it into the sample cup, stir slowly, and extract the required amount of yellow phosphorus. Seal the upper end of the sampling tube with your fingers, slowly lift the sampling tube up to the water layer (note: do not leave the bottom of the sampling tube out of the water), and inject the yellow phosphorus in the tube into the porcelain glass that has been placed in the water bath in advance. Take out the porcelain crucible containing the sample from the water bath and place it in cold water to cool. After the yellow phosphorus solidifies, take it out with tweezers and store it in a jar filled with water for later use.
1 sampling tube; 2·Water bath: 3-sample cup; 4 yellow phosphorus layer; 5-~hot water; 6---porcelain pot (15mL) Figure 1 sample preparation device
4.3 Determination of yellow phosphorus content
4.3.1 The yellow phosphorus content (X,) expressed as mass percentage is calculated according to formula (1): X = 100 - Xs
Where: X-benzene Insoluble matter content shall be determined according to the provisions of Article 4.4. 4.3.2 The yellow phosphorus content (X,) expressed as a mass percentage is calculated according to the formula (2: X, = 100 Determination as specified in Article 4.5. 4.4 Determination of benzene insoluble content
Safety tips: This test operation should be carried out in a fume hood. 4.4.1 Method summary
Dissolve the yellow phosphorus sample in In benzene, calculate the content of benzene-insoluble matter by filtering, drying and weighing.
4.4.2.2 Absolute ethanol. ||4.4.3 Instruments and equipment
4.4.3.1 Glass sand pot: pore size is 5~~15μm. 4.4.3.2 Electric oven: The temperature can be controlled at 105~~110℃. | | tt | | t | The moisture attached to the surface is dehydrated in a 50mL 103
GB 7816-7998
cup filled with ethanol. Take it out with tweezers, dry it with filter paper and quickly put it into a weighing container filled with water. Weigh the glass sand baked to a constant weight at 105-110°C to the vacuum filter bottle, add 25ml to the glass sand crucible, and heat to boiling temperature on a constant temperature water bath. of benzene, quickly use filter paper to absorb the moisture attached to the surface of the weighed yellow phosphorus sample and place it in a glass sand pot. After a while, turn on the vacuum pump to suck out part of the benzene solution and stop the suction filtration (yellow phosphorus sample). The phosphorus sample must be immersed in benzene). Then add boiling benzene, dissolve and filter. Repeat this process until all the yellow phosphorus is dissolved and the filtrate evaporates on the filter paper without white smoke. After all the benzene has evaporated, put the good glass sand crucible in an oven at 105~~110℃ and bake it to constant weight. 4.4.5 Expression of analysis results
Benzene expressed as mass percentage. The insoluble matter content (X) is calculated according to formula (3): :m,—
The mass of the glass sand crucible and the residue after drying, g: rm2
The mass of the weighing bottle containing water,;
m3
m.|| tt||The mass of the weighing bottle containing water and the yellow phosphorus sample, g. 4.4.6 The allowable difference
shall be the arithmetic mean of the parallel measurement results as the measurement result, and the absolute difference of the parallel measurement results shall not be greater than 0.02%. 4.5 Determination of carbon disulfide insoluble content
Safety tips: This test operation should be carried out in a fume hood. 4.5.1 Method summary
Dissolve the yellow phosphorus sample in carbon disulfide, filter, dry and weigh, and calculate the content of carbon disulfide insoluble matter. 4.5.2 Reagents and materials
4.5.2.1 Carbon disulfide.
4.5.2.2 Anhydrous ethanol.
4.5.3 Instruments and equipment
4.5.3.1 Glass sand crucible: pore diameter is 5~~15μm. 4.5.3.2 Electric oven: The temperature can be controlled at 105~110C. ·(3)
4.5.4 Analysis steps
Use tweezers to pick up about 35g of the sample, quickly use filter paper to absorb the moisture attached to the surface of the sample, and place it in a 50ml beaker containing ethanol. Dehydration. Take it out with tweezers, blot it dry with filter paper and quickly put it into a weighed weighing bottle filled with water for weighing, accurate to 0.01%. Connect the glass sand crucible that has been baked to constant weight at 105 to 110°C to the vacuum filter bottle. Add 15ml of carbon disulfide to the glass sand crucible, and quickly use filter paper to absorb the moisture attached to the surface of the weighed yellow phosphorus sample. Place it in a glass sand crucible. After the yellow phosphorus is dissolved, turn on the vacuum pump for suction filtration. Stop filtering when the liquid layer is nearly dry. Then add 5 pieces of 1 carbon disulfide, dissolve and filter with suction. Repeat this operation until all the yellow phosphorus is dissolved and filtered, and the filtrate is dropped on the filter paper until no white smoke is emitted after evaporation. Place the washed glass sand crucible at room temperature. After all the carbon disulfide has evaporated, place it in an oven at 105-110C and bake until it reaches constant weight. 4.5.5 Expression of analysis results
The carbon disulfide insoluble content (X,) expressed as mass percentage is calculated according to formula (4): tt||In the formula: mi——The mass of the glass sand crucible·g; m2~-The mass of the glass sand crucible and the residue after drying, m. The mass of the weighing bottle filled with water.
m4 ——The mass of the weighing bottle containing water and the yellow phosphorus sample, g. 4.5.6 Allowable difference
104
GB7816-1998
The arithmetic mean of the parallel measurement results is taken as the measurement result, and the absolute difference of the parallel measurement results is not greater than 0.02%. 5 Inspection rules
5.1 All items specified in this standard are factory inspection items. 5.2 Each batch of products shall not exceed 100t.
5.3 Determine the number of sampling units according to the provisions of 6.6 of GB/T6678--1986. Each steel drum is a packaging unit. When packaging in tanks, take samples from each tank. When sampling, heat and melt the yellow phosphorus in the steel drum or tank, open the cone valve of the sampler (shown in Figure 2), insert it vertically into the bottom of the material layer, close the cone valve, stay for a moment, lift the sampler, and The sample in the tube is placed in a sample cup filled with hot water (the sample cup can be a sugar porcelain cup with a capacity of 1000 mL). The sample cup is placed in a metal bucket filled with hot water. The sampling volume should not be less than 500g. A label should be attached to the sample cup containing yellow phosphorus, indicating the manufacturer's name, product name, grade, batch number, sampling date and name of the sampler, and the words "toxic" and "spontaneous combustion".
5.4 Industrial yellow phosphorus 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 each batch of products is in compliance with the requirements of this standard.
If one indicator in the inspection result does not meet the requirements of this standard, samples should be taken from the packaging with twice the number of sampling units for re-inspection. If the re-inspection result even if only one indicator does not meet the requirements of this standard, The entire batch of products is deemed to be unqualified. 5.5 Use the rounded value comparison method specified in 5.2 of GB1250-1989 to determine whether the test results meet the standards. Handle
Compression spring
Gland
Lifting shaft
Circular tube
Conical valve
Figure 2 Yellow phosphorus sampler structure| |tt||105
6 Marking, packaging, transportation, storage
GB 7816—1998
6.1 Industrial yellow phosphorus packaging bags and barrels should have firm and clear markings, including: Manufacturer's name, address, product name, trademark, grade, net content, batch number or production date and this standard number, as well as the "Spontaneous Combustion Materials" mark in Figure 7, the "Drugs" mark in Figure 11 and GB191-1990 specified in GB190-1990 Mark 3\Up" mark (iron drum packaging) and Mark 1\Handle with care" specified in 6.2 Each batch of industrial yellow phosphorus shipped from the factory should be accompanied by a quality certificate, including: manufacturer name, factory address, and product. Name, trademark, grade, net content, batch number or production date, proof that product quality complies with this standard and this standard number. 6.3 Industrial yellow phosphorus is filled with liquid in closed steel drums or tanks, and its performance and inspection are used. The method should comply with the relevant regulations of GB/T325. The net content of each barrel of the product is 2000kg. Before and after the yellow phosphorus is canned, there should be a layer of water on it, with a thickness of not less than 5cm, and a free space. It should account for more than 5% of the total volume. 6.4 Industrial yellow phosphorus should be transported in accordance with the requirements of the "Dangerous Goods Transport Regulations". 6.5 Industrial yellow phosphorus should be stored in packaging containers with water, and the containers should be sealed and the yellow phosphorus should be immersed. In water. 7 Safety requirements
7.1 The benzene and carbon disulfide solution after measuring yellow phosphorus should be burned. The burning site should be more than 1km away from residential buildings, public buildings, roads, and farmland crops. The burning site should be dug into a ditch. The torch used for ignition is tied to a 3-4m long pole. 7.2 In order to recover the solvent, the organic solution containing phosphorus is treated with a saturated copper sulfate solution under vigorous stirring until the phosphorus in the organic phase disappears. Precipitate into non-hazardous compounds, separate the organic layer, filter and perform distillation and purification.
7.3 Every staff member who comes into contact with yellow phosphorus must know first aid in case of poisoning. Method. When acute yellow phosphorus poisoning occurs, gastric lavage should be performed repeatedly with 0.2% potassium permanganate solution or 1% copper sulfate solution until the smell of yellow phosphorus in the washing water disappears. Milk, fat and other foods should not be given to the poisoned person. , because these foods dissolve yellow phosphorus, causing yellow phosphorus to penetrate into the body. When the skin is burned by yellow phosphorus, the burned area should be washed immediately with plenty of water, and then the yellow phosphorus should be carefully removed with a wooden scraper under water. Then let the yellow phosphorus enter the wound. When removing yellow phosphorus, do it in a dark place and completely avoid light. If you use chemical methods to remove phosphorus, use 0.2% potassium permanganate solution to clean the burned area.
If it is in the eyes, flush it with plenty of water immediately and send it to the hospital for treatment. Clothes burned by yellow phosphorus must be doused with water and taken off when water is poured or taken off in the water in the bathtub. Otherwise, the yellow phosphorus may penetrate. clothes and burn the skin.
In any case of yellow phosphorus contamination, it must be sent to a medical department for treatment. 106
GB 7816-1998
Appendix A
(prompted appendix)
Determination of arsenic
This determination method is equivalent to the national standard GB/T7686 1987 "General method for determination of arsenic content in chemical products". When the user has requirements for arsenic content, this method shall be used to measure it, and its index parameters shall be agreed upon by both supply and demand parties. A1 method summary
See Chapter 2 of GB/T7686-1987.
A2 reagents and materials
See Chapter 3 of GB/T7686--1987.
A3 instruments and equipment
See Chapter 4 of GB/T7686.-1987.
A4 analysis steps
Preparation of A4.1 test solution
Weigh 2~3g yellow phosphorus sample, accurate to 0.01g. Place the sample in 250 ml of porcelain blood with a handle containing 70 ml (7+5) nitric acid solution, cover it with a watch glass, and place it on a hot water bath to slowly heat. The degree of reaction between the sample and nitric acid increases as the temperature increases. When the reaction is too violent, remove the porcelain blood from the water bath and place it in cold water to cool it if necessary; otherwise, place it on the water bath to heat it. Control the intensity of the reaction to prevent the smaller particles of the liquid yellow phosphorus sample from floating on the surface of the nitric acid solution, and to prevent the yellow phosphorus from contacting the air and burning. Do not remove the surface during the dissolution of yellow phosphorus
After all the yellow phosphorus has been oxidized into phosphoric acid, lift the watch glass and rinse the surface blood with a small amount of water. Pour 30 mL (1+2) sulfuric acid solution into the porcelain dish, place it on the electric stove and slowly evaporate until white smoke of sulfur trioxide appears. Remove the porcelain dish and cool it. Transfer all the solution into 250mL.In a volumetric flask, dilute to volume with water.
A4.2 Preparation of blank test solution
While preparing the test solution, except that no test material is added, other operations and the amount of reagents added are treated in the same manner as the test solution. A4.3 The drawing of the standard curve
shall be operated according to the provisions of 5.3 of GB/T7686-1987. A4.4 Measurement
Use a pipette to transfer 5ml of the test solution and blank solution, place them in arsine generating bottles, add 10mL (1 + 2) hydrochloric acid solution to each, and add water until the volume is about 40mL . Then start the operation according to 5.4 of GB/T7686-1987 "Add 2 mL potassium iodide solution..." and measure the absorbance of the test solution and blank test solution. A4.5 Expression of analysis results
Expressed in mass percentage Arsenic (As) content (X) is calculated according to the following formula: |(ms-m:) ×
250
Where: m!\...—The mass of arsenic in the blank test solution is found from the standard curve, g; the test solution is found from the standard curve The mass of arsenic in the solution, g; mz
The mass of the weighing bottle containing water, name;
ma
m.-Weighing bottle containing water and yellow phosphorus Mass of sample·g. 107
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