GB/T 7816: Evolution and historical versions
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Yellow phosphorus for industrial use
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Yellow phosphorus for industrial use
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[GB/T 7816-1998] Yellow phosphorus for industrial use
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Technical yellow phosphorus
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Basic data | Standard ID | GB/T 7816-2025 (GB/T7816-2025) | | Description (Translated English) | Yellow phosphorus for industrial use | | Sector / Industry | National Standard (Recommended) | | Date of Implementation | 2026-03-01 | | Older Standard (superseded by this standard) | GB/T 7816-2018 | GB/T 7816-2018: Yellow phosphorus for industrial use---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Yellow phosphorus for industrial use
ICS 71.060.10
G13
National Standards of People's Republic of China
Replace GB/T 7816-1998
Industrial Yellow Phosphorus
2018-02-06 released
2018-09-01 Implementation
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
Issued by China National Standardization Management Committee
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB/T 7816-1998 "Industrial Yellow Phosphorus", compared with GB/T 7816-1998, except for editorial modifications, the main technologies
The changes are as follows.
--- Added arsenic index items and parameters and test methods (see Chapter 4 and 5.7);
--- Remove the original standard "spontaneously ignitable substances" "drugs" and "careful handling" signs, add "prone to spontaneous combustion substances" "toxic substances" and "prohibited substances"
"Stop Rolling" sign (see 7.1,.1998 edition 6.1);
--- Deleted the determination of arsenic in Appendix A of the original standard (Appendix A in.1998 edition);
--- Added Appendix A disposal method of benzene and carbon disulfide filtrate (see Appendix A).
This standard was proposed by the China Petroleum and Chemical Industry Federation.
This standard is under the jurisdiction of the National Chemical Standardization Technical Committee Inorganic Chemical Sub-Technical Committee (SAC/TC63/SC1).
The main drafters of this standard. CNOOC Tianjin Chemical Research and Design Institute Co., Ltd., Hubei Xingfa Chemical Group Co., Ltd.
The main drafters of this standard. Wang Yan, Wang Xiangsen, Xiong Ping, Wan Jinzhu, Yang Zhengyong.
The previous versions of the standard replaced by this standard are as follows.
--- GB 7816-1987, GB/T 7816-1998.
Industrial Yellow Phosphorus
Warning --- According to the provisions of Chapter 6 of GB 12268-2012, this product is classified as a substance of category 4 4.2 and spontaneous combustion and category 6 6.1
This toxic substance should be handled with care. The samples and some reagents used in the test methods of this standard are toxic, flammable or corrosive
Sex, it must be carefully operated in a fume hood. If it splashes on the skin, it should be rinsed with water immediately. Easy to spontaneous use
It is strictly prohibited to use open flame for heating.
1 Scope
This standard specifies the requirements, test methods, inspection rules, signs, labels, packaging, transportation, storage and safety of industrial yellow phosphorus.
This standard applies to industrial yellow phosphorus. Mainly used in the manufacture of red phosphorus, phosphoric acid, phosphorus compounds and phosphates.
2 Normative references
The following documents are essential for the application of this document. For dated references, only the dated version applies to this article
Pieces. For the cited documents without date, the latest version (including all amendments) applies to this document.
GB 190-2009 Dangerous Goods Packaging Mark
GB/T 191-2008 Graphic symbol for packaging, storage and transportation
GB/T 6678 General Rules for Sampling of Chemical Products
GB/T 6682-2008 Specification and test method for analyzing laboratory water
GB/T 7686-2016 General method for determination of arsenic content in chemical products
GB/T 8170 Numerical Rounding Rules and Representation and Judgment of Limit Values
GB 12268-2012 Name table of dangerous goods
GB 12463-2009 General technical conditions for transport packaging of dangerous goods
GB 16473 yellow phosphorus packaging
GB 19358 Yellow Phosphorus Packaging Safety Specification Use Appraisal
HG/T 3696.2 Preparation of standard solutions, preparations and products for chemical analysis of inorganic chemical products. Part 2. Standard solution of impurities
Preparation of liquid
HG/T 3696.3 Preparation of standard solutions, preparations and products for chemical analysis of inorganic chemical products. Part 3. Preparations and products
Preparation
3 Molecular formula, relative molecular mass
Molecular formula. P or P4.
Relative molecular mass. 30.97 or 123.9 (according to.2016 international relative atomic mass).
4 requirements
The detection of industrial yellow phosphorus according to the test method specified in this standard shall comply with the provisions of Table 1.
Table 1
project
index
First-class products
Appearance paraffin-like, light yellow to slightly yellow-green paraffin-like, yellow-green to brown-green
Yellow phosphorus (P) w /% ≥
99.90 99.50 in benzene
99.90 in carbon disulfide-
Insoluble matter w /% ≤
0.10 0.50 in benzene
0.10-in carbon disulfide
Arsenic (As) w /% ≤ 0.01 0.02
5 Test methods
5.1 General provisions
The reagents and water used in this standard refer to analytical reagents and tertiary water specified in GB/T 6682-2008 when no other requirements are indicated.
The standard titration solutions, preparations and products of impurities used in the test, if no other requirements are noted, are in accordance with HG/T 3696.2, HG/T 3696.3
Stipulated preparation.
5.2 Visual inspection
Under natural light conditions, visually determine the appearance of the sample in the sample cup.
5.3 Preparation of samples
Samples were prepared using the device of Figure 1.
Put on rubber gloves, put the sample cup containing yellow phosphorus into the bathtub, and heat to about 70 ℃ to melt the yellow phosphorus. With an inner diameter of 5mm
Or a 6mm glass sampling tube, insert it into the sample cup, and after slowly stirring, extract the required amount of yellow phosphorus. Seal the upper end of the sampling tube with your finger and slowly
Place the sampling tube in the water layer (note. the bottom end of the sampling tube should not leave the water surface), and inject the yellow phosphorus in the tube into the porcelain crucible previously placed in the water bath.
Remove the porcelain crucible containing the sample from the water bath and cool it in cold water. After the yellow phosphorus solidifies, remove it with tweezers and store it in a wide mouth filled with water
In the bottle, spare.
Explanation.
1 --- Sampling tube;
2 --- water bathtub;
3 --- sample cup;
4 --- Yellow phosphorous layer;
5 --- hot water;
6 --- Porcelain crucible (15mL).
Figure 1 Sample preparation device
5.4 Calculation of yellow phosphorus content
5.4.1 The content of yellow phosphorus is calculated by the mass fraction w1 of phosphorus (P), and calculated according to formula (1)
w1 = 100% -w3 (1)
In the formula.
w3 --- The content of benzene insoluble matter is determined according to the provisions of 5.5.
5.4.2 The content of yellow phosphorus is calculated by the mass fraction w2 of phosphorus (P), and calculated according to formula (2)
w2 = 100% -w4 (2)
In the formula.
w4 --- The content of carbon disulfide insoluble matter is determined according to the provisions of 5.6.
5.5 Determination of benzene insoluble content
5.5.1 Principle
Dissolve the yellow phosphorus sample in benzene, calculate the content of benzene insoluble matter by suction filtration, drying and weighing.
5.5.2 Reagents or materials
5.5.2.1 Benzene.
5.5.2.2 Absolute ethanol.
5.5.3 Instruments
5.5.3.1 Glass sand crucible. The filter plate pore size is 5μm ~ 15μm.
5.5.3.2 Electric heating constant temperature oven. the temperature can be controlled at 105 ℃ ~ 110 ℃.
5.5.3.3 Constant temperature water bath.
5.5.4 Test procedure
Take about 3g ~ 5g sample (5.3) with tweezers, quickly absorb the water attached to the surface of the sample with filter paper, and place it in 50mL of ethanol
Dehydrate in the beaker. 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
g. Connect the glass sand crucible baked at 105 ℃ ~ 110 ℃ to a constant quality to the vacuum suction flask, add 25mL to the glass sand crucible
Heated to boiling benzene on a constant temperature water bath, quickly absorb the water attached to the surface of the weighed yellow phosphorus sample with filter paper and place it in a glass sand crucible, slightly
After a while, connect the vacuum pump with suction and buffer device for suction filtration. Aspirate part of the benzene filtrate (see Appendix A for filtrate treatment), stop pumping
Filter (yellow phosphorus sample must be immersed in benzene). Then add to the boiling benzene, dissolve and filter with suction. Repeat this operation until the yellow phosphorus is completely dissolved and filtered
Clean, until the filter droplets evaporate on the filter paper without emitting white smoke. Place the washed glass sand crucible at room temperature.
105 ℃ ~ 110 ℃ electric heating constant temperature drying oven, baked to constant quality (accurate to 0.0001g).
5.5.5 Test data processing
The content of benzene insolubles is calculated based on the mass fraction w3, calculated according to formula (3).
w3 =
m2-m1
m4-m3 ×
100% (3)
In the formula.
m1 --- The value of the mass of the glass sand crucible in grams (g);
m2 --- The value of the mass of glass sand crucible and insoluble matter after drying, the unit is gram (g);
m3 --- The value of the mass of the weighing bottle filled with water, the unit is gram (g);
m4 --- The numerical value of the weight of the weighing bottle and sample with water in grams (g).
The arithmetic mean of the parallel determination results is taken as the measurement result, and the absolute difference between the two parallel determination results is not more than 0.02%.
5.6 Determination of insoluble content of carbon disulfide
5.6.1 Principle
Dissolve the yellow phosphorus sample in carbon disulfide, calculate the content of carbon disulfide insoluble matter by suction filtration, drying and weighing.
5.6.2 Reagents or materials
5.6.2.1 Carbon disulfide.
5.6.2.2 Absolute ethanol.
5.6.3 Equipment
5.6.3.1 Glass sand crucible. The filter plate pore size is 5μm ~ 15μm.
5.6.3.2 Electric constant temperature drying oven. the temperature can be controlled at 105 ℃ ~ 110 ℃.
5.6.4 Test procedure
Take about 3g ~ 5g sample with tweezers, quickly absorb the water attached to the surface of the sample with filter paper, and place it in a 50mL beaker containing ethanol
Medium 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 0.01g. will
Connect the glass sand crucible baked to constant quality at 105 ℃ ~ 110 ℃ to the vacuum suction flask, add 15mL disulfide to the glass sand crucible
Carbon, quickly absorb the moisture attached to the surface of the weighed yellow phosphorus sample with filter paper and place it in a glass sand crucible.After the yellow phosphorus is dissolved, turn on the
The vacuum pump of the adsorption and buffer device performs suction filtration (see Appendix A for filtrate). Stop suction filtration when the liquid layer is nearly dry. Add 5mL
Carbon sulfide, filtered after suction. Repeat this operation until the yellow phosphorus is completely dissolved and filtered, with the filter droplets on the filter paper, and no white smoke after volatilization.
stop. Place the washed glass sand crucible at room temperature. After all the carbon disulfide volatilizes, place it in an electric thermostatic drying oven at 105 ℃ ~ 110 ℃
Medium, bake to constant quality (accurate to 0.0001g).
5.6.5 Test data processing
The content of insoluble matter in carbon disulfide is calculated by mass fraction w4, and calculated according to formula (4).
w4 =
m2-m1
m4-m3 ×
100% (4)
In the formula.
m1 --- The value of the mass of the glass sand crucible in grams (g);
m2 --- The value of the mass of glass sand crucible and insoluble matter after drying, the unit is gram (g);
m3 --- The value of the mass of the weighing bottle filled with water, the unit is gram (g);
m4 --- The numerical value of the weight of the weighing bottle and sample with water in grams (g).
The arithmetic mean of the parallel determination results is taken as the measurement result, and the absolute difference between the two parallel determination results is not more than 0.02%.
5.7 Determination of arsenic content
5.7.1 Principle
See 3.1 of GB/T 7686-2016.
5.7.2 Reagents or materials
See 3.3 of GB/T 7686-2016.
5.7.3 Equipment
See 3.4 of GB/T 7686-2016.
5.7.4 Test procedure
5.7.4.1 Preparation of test solution
Take about 2g ~ 3g sample with tweezers, quickly absorb the water attached to the surface of the sample with filter paper, and place it in a 50mL beaker containing ethanol
Medium 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 0.01g. will
The sample was placed in a 250mL porcelain dish with a handle containing 70mL nitric acid solution (75), covered with a watch glass, and slowly heated on a hot water bath. test
The degree of reaction between the sample and nitric acid increases with the temperature. When the reaction is violent, remove the porcelain from the water bath and place it in cold water if necessary
However; vice versa and then placed on a water bath and heated. Control the severity of the reaction so that the smaller particles of the sample do not float on the surface of the nitric acid solution and avoid yellow phosphorus
Burning in contact with air, the watch glass should not be removed during the dissolution of yellow phosphorus.
When all yellow phosphorus is oxidized to phosphoric acid, lift the watch glass and rinse the watch glass with a small amount of water. Add 30mL of sulfuric acid to the porcelain dish
Liquid (1 2), slowly evaporate on the electric furnace until white smoke of sulfur trioxide emerges, remove the porcelain dish, and cool. Move all the solution into 100mL
In a volumetric flask, dilute to the mark with water.
5.7.4.2 Preparation of blank test solution
While preparing the test solution, except that no sample is added, the other operations and the amount of reagents added are the same as the preparation of the test solution.
5.7.4.3 Drawing of working curve
Operate according to the provisions of 3.5.3 in GB/T 7686-2016.
5.7.4.4 Determination
Pipette 5mL test solution of superior product (10mL test solution of first-class product) and blank test solution, and place them in arsenide
Add 10mL hydrochloric acid solution (12) to the generated bottle and add water to make the volume about 40mL. Then press 3.5.4.1 of GB/T 7686-2016
Start from "Add 2mL potassium iodide solution", and determine the test solution and blank according to 3.5.3.2 of GB/T 7686-2016
The absorbance of the test solution.
5.7.5 Processing of test data
The arsenic content is calculated based on the mass fraction w5 of arsenic (As) and calculated according to formula (5).
w5 =
m2-m1
(m4-m3) × (V/100) ×
100% (5)
In the formula.
m1 --- The value of the mass of arsenic in the blank test solution isolated from the working curve, the unit is gram (g);
m2 --- The value of the mass of arsenic in the test solution found from the working curve, the unit is gram (g);
m3 --- The value of the mass of the weighing bottle filled with water, the unit is gram (g);
m4 --- The value of the mass of the weighing bottle filled with water and the yellow phosphorus sample in grams (g);
V --- Pipette the volume of the test solution in milliliters (mL).
The arithmetic mean of the parallel determination results is taken as the measurement result, and the absolute difference between the two parallel determination results is not more than 0.0005%.
6 Inspection rules
6.1 The index items listed in the requirements of this standard are all factory inspection items and should be inspected batch by batch.
6.2 The production enterprises use the same materials, basically the same production conditions, continuous production or the same grade of industrial yellow phosphorus produced by the same team is
One batch, each batch of products does not exceed 100t.
6.3 Determine the number of sampling units according to the regulations in GB/T 6678. Each steel drum is a packaging unit. When packing in tanks, from each tank
Sampling in the tank. When sampling, heat and melt the yellow phosphorus in the steel drum or tank, open the conical valve of the sampler (shown in Figure 2), and insert it vertically to the bottom
unit. Close the conical valve, stop for a while and lift the sampler, put the sample in the tube into the sample cup containing hot water (the available volume of the sample cup is 1L
Enamel cup), the sample cup is placed in a metal bucket filled with hot water, the sampling volume should not be less than 500g. Put a label on the sample cup, indicating the production
Plant name, product name, grade, batch number, sampling date and sampler's name, and indicate the words "substance liable to spontaneous combustion" and "toxic substance".
The unit is mm
Figure 2 Sampler
6.4 Inspection results If the indicators do not meet the requirements of this standard, re-sampling should be performed from twice the amount of packaging for re-inspection.
When an indicator does not meet the requirements of this standard, the entire batch of products is unqualified.
6.5 Use the rounding value comparison method specified in GB/T 8170 to determine whether the inspection result meets the standard.
7 Signs and labels
7.1 There should be a firm and clear mark on the industrial yellow phosphorus packaging container, including. manufacturer name, factory address, product name, grade, net content, batch
No. or production date, the number of this standard and the signs of "prone to spontaneous combustion" and "toxic substances" specified in GB 190-2009 and
GB/T 191-2008 stipulates the "upward" and "prohibited rollover" signs.
7.2 Each batch of industrial yellow phosphorus leaving the factory shall be accompanied by a quality certificate, which includes. the name of the manufacturer, the site, the name of the product, the grade, the net content, the batch
No. or date of production, certification of product quality in accordance with this standard and serial number of this standard.
8 Packaging, transportation and storage
8.1 The packaging category of industrial yellow phosphorus product packaging shall comply with the provisions of Table 1 in GB 12268-2012, and the limited quality of the packaging shall comply with
The requirements of Appendix A in GB 12463-2009. When rail transportation is used, its packaging shall also comply with
Regulations. The packaging of industrial yellow phosphorus should meet the requirements of GB 19358 and GB 16473.
8.2 The transportation of industrial yellow phosphorus shall comply with the provisions of the "Interim Regulations on the Management of the Transportation of Railway Dangerous Goods" and the "Rules of Transportation of Dangerous Goods on Motor Vehicles". transport
There should be coverings in the process to prevent sun exposure and rain. Prevent violent impact. Prevent packaging damage. Prohibited with oxidants, blowing agents, halogens, gold
It belongs to powder mixed transportation. Handle with care when loading and unloading. Do not impact the drum. It should not be turned upside down.
8.3 Industrial yellow phosphorus is a substance prone to spontaneous combustion and toxic substances, and should be stored in a cool, ventilated warehouse. Keep away from fire and heat. Should not interact with oxygen
Chemical agent, foaming agent, halogen and metal powder are stored in the same warehouse.
Appendix A
(Informative appendix)
Disposal of benzene and carbon disulfide filtrate
A.1 In order to recover the solvent, the organic solution dissolved in phosphorus is treated with saturated copper sulfate solution under vigorous stirring until the
Until the smoke disappears. At this time, the phosphorus becomes a non-hazardous compound and precipitates. The organic layer is separated, filtered and purified by distillation. This operation
Should be carried out in a fume hood.
A.2 The benzene and carbon disulfide solution after the determination of yellow phosphorus is burned under the supervision of a qualified unit or professional department. burning
The site should be far away from residential houses, public buildings, roads, farmland crops more than 1km. The burning site should be dug into a ditch. Tied torch
On a stalk 3m ~ 4m long.
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