Some standard content:
HG/T 2770-1996
This standard is formulated based on the domestic main enterprise standards. And according to the actual production situation and user requirements, it is divided into two levels. The differences between this standard and the existing enterprise standards are as follows: 1 The pH index is stricter than the enterprise standard.
2 Some enterprise standards stipulate solubility indicators. After analysis, this indicator can be reflected by the pH index. Therefore, this industry standard does not stipulate the solubility index.
The test methods all adopt the classic methods that have been verified by many years of use. Appendix A of this standard is the standard appendix.
Appendix B of this standard is the prompt appendix.
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: Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Sichuan Chuanxi Phosphorus Chemical Industry Group Co., Ltd., Sichuan West Chemical Plant, Shandong Zaozhuang Calcium Carbide Plant.
Main drafters of this standard: Yao Jinjuan, Feng Chang, Li Difa, Zhang Fengyun, Zhou Qingzhong618
Chemical Industry Standard of the People's Republic of China
Industrial ammonium polyphosphate
HG/T 2770—1996
This standard specifies the requirements, sampling, test methods, marking, packaging, transportation and storage of industrial ammonium polyphosphate. This standard applies to industrial ammonium polyphosphate produced with urea and phosphoric acid, urea and diammonium phosphate as raw materials. The product is mainly used as a flame retardant additive for coatings, papermaking, plastics, wood and organic building materials. General formula: (NH)n+2P,Oaa+1
2Referenced 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 are subject to revision, and parties using this standard should explore the possibility of using the latest version of the following standards. GB 191-—1990
Picture mark for packaging, storage and transportation
GB/T 601-19881
Preparation of standard solution for titration analysis (volume analysis) of chemical reagentsGB/T 602--1988
GB/T 603-1988
GB/T 1250--1989
GB/T 6003-1985
GB/T 6678—1986
GB/T 6682—1992
GB/T 8946—-1988
3 Requirements
3.1 Appearance: white powder. Www.bzxZ.net
Preparation of standard solution for determination of impurities in chemical reagents (negISO6353-1:1982) Preparation of preparations and products used in test methods for chemical reagents (neqISO6353-1:1982) Methods for expressing and determining limit values Test sieves
General rules for sampling of chemical products
Specifications and test methods for water in analytical laboratories (eqvISO3696:1987)) Plastic woven bags
2 Industrial ammonium polyphosphate shall comply with the requirements of Table 1: 3.2
Requirements of Table 1
Phosphorus pentoxide (P2O.) content/%
Nitrogen (N) content/%
Average degree of polymerization
pH (10 g/L solution)
Fineness (through 150μm sieve)/%
4 Sampling
4.1 Each batch of product shall not exceed 5t.
1996-01-24 Approved by the Ministry of Chemical Industry of the People's Republic of China First-class product
Qualified product
1997-01-01 Implementation
HG/T 2770—1996
4.2 Determine the number of sampling units according to the provisions of (GB/T66786.6. When sampling, insert the sampler obliquely from the top of the packaging bag to 3/4 of the depth of the material layer to take a sample. After mixing the sample, reduce it to no less than 500g according to the quartering method, and pack it into two clean and dry wide-mouth bottles with stoppers and seal them. Stick labels on the bottles, indicating: manufacturer name, product name, grade, batch number, sampling date and name of the sampler. One bottle is used as a laboratory sample, and the other bottle is used to store three 4.3 If any of the test results do not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-verification. If any of the test results do not meet the requirements of this standard, the entire batch of products shall be deemed unqualified. 5 Test method
5.1 The rounded value comparison method specified in 5.2 of GB/T1250 shall be used to determine whether the test results meet the standard. 5.2 The reagents and water used in this standard, unless otherwise specified, refer to analytical pure reagents and water specified in GB/T6682. The standard titration solution, impurity standard solution, preparation and product used in the test, unless otherwise specified, are prepared in accordance with the provisions of (GB/T601, GB/T602, GB/T603). 5.3 Determination of phosphorus pentoxide content
5.3.1 Method summary
In an acidic medium, phosphate reacts with sodium molybdate and quinoline to form quinoline phosphomolybdate precipitate. The phosphorus pentoxide content is calculated by filtering, drying, weighing.
5.3.2 Reagents Materials
5.3.2.1 Nitric acid solution: 1+1;
5.3.2.2 Quinoline molybdate solution;
Preparation method:
a) Weigh 70g sodium molybdate and dissolve it in 150mL water; b) Weigh 60g citric acid and dissolve it in 85ml nitric acid solution and 150mL water; c) Pour solution a into solution b under stirring; d) Add 35mL nitric acid solution and 5mL quinoline to 100mL water; e) Pour solution d into solution c. After standing for 24h, filter with a glass sand crucible, add 280mL acetone, dilute with water to 1000ml, mix well, store in a polyethylene bottle, and store in a dark place. 5.3.3 Instruments and equipment
5.3.3.1 Glass sand: the pore size of the filter plate is 5μm~15μm; 5.3.3.2 Electric oven: the temperature can be controlled at 180℃±5℃. 5.3.4 Analysis steps
Weigh about 0.5g of sample (accurate to 0.0002g), place it in a 150mL beaker, add water to moisten it, add 10mL nitric acid solution, heat it on an electric stove to boiling and keep it for 10min. Remove the beaker, transfer it to a 250mL volumetric flask after cooling, add water to the scale, and shake it. Use a pipette to transfer 10mL of the test solution, place it in a 250mL beaker, add 10mL nitric acid solution and 80mL water, cover the surface blood, and heat it to boiling. Add 50mL of quinoline molybdate solution and continue to heat it to boiling for 1min. Remove the beaker and stir to promote precipitation. After cooling, filter by pouring through a glass sand crucible that has been dried to constant weight at 180±5℃. Wash the precipitate in a beaker 5-6 times, using 20ml of water each time. Finally, transfer all the precipitate to a glass sand crucible and wash it with water 5-6 times. Dry the glass sand and precipitate at 180±5℃ for 45 minutes, take it out and place it in a desiccator to cool, and weigh it. Perform a blank test at the same time. 5.3.5 Expression of analysis results
The content of phosphorus pentoxide (P,Os) X expressed as mass percentage is calculated according to formula (1): X = (mm)X0 032 07 × 100
m×250
80. 18 X (ml - m2)
（1）
Wherein:
HG/T 2770--1996
The mass of quinoline phosphomolybdic acid precipitate generated in the test solution, g; The mass of quinoline phosphomolybdic acid precipitate generated in the blank test solution, g; m
The mass of the sample, g;
0.03207--The coefficient for converting quinoline phosphomolybdic acid into phosphorus pentoxide. 5.3.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.2%. 5.4 Determination of nitrogen content
5.4.1 Summary of the method
Ammonium polyphosphate is depolymerized in sulfuric acid solution to generate ammonium sulfate, and then the ammonium ion content is determined by the formaldehyde method. 5.4.2 Reagents and materials
5.4.2.1 Sulfuric acid solution: 1+1;
5.4.2.2 Sulfuric acid solution: 1+19;
5.4.2.3 Neutral formaldehyde solution: 1+3;
Add 2 drops of phenolic acid indicator solution to the 1+3 solution and titrate with sodium hydroxide standard titration solution until it turns pink. 5.4.2.4 Sodium hydroxide solution: 300g/L
5.4.2.5 Sodium hydroxide standard titration solution: c(NaOH) is about 0.5mol/L; 5.4.2.6 Phenolic acid indicator solution: 10g/L.
5.4.3 Analysis steps
Weigh about 1g of sample (accurate to 0.0002g), place in a 250ml conical flask, moisten with a small amount of water, and add 10mL of sulfuric acid solution (5.4.2.1) Heat until sulfur trioxide smoke is produced. Stop heating, remove and cool to room temperature. Add 30mL of water and 2 drops of phenol anhydride indicator solution, neutralize excess sulfuric acid with sodium hydroxide solution until the solution turns red, add sulfuric acid solution (5.4.2.2) dropwise until the test solution turns colorless, and then add sodium hydroxide standard titration solution dropwise until the test solution turns pink. Add 15mL of neutral formaldehyde solution and titrate with sodium hydroxide standard titration solution until the solution turns pink, which is the end point. 5.4.4 Expression of analysis results
Nitrogen (N) content X2 expressed as mass percentage is calculated according to formula (2): X2 = cVX0. 014 01
Wherein: c-actual concentration of sodium hydroxide standard titration solution, mol/L; V-volume of sodium hydroxide standard titration solution consumed in titration, mL; m
mass of sample, g;
(2)
0.01401——mass of nitrogen expressed in grams equivalent to 1.00mL sodium hydroxide standard titration solution (c(NaOH)=1.000mol/L)
5.4.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.2%. 5.5 Determination of average degree of polymerization
5.5.1 Method summary
The terminal phosphorus content of the sample is determined by potentiometric titration. The ratio of twice the total phosphorus content to the terminal phosphorus content is the average degree of polymerization. 5.5.2 Reagents and materials
5.5.2.1 H-732 ion exchange resin; 5.5.2.2 Hydrochloric acid solution: 1+1;
5.5.2.3. Standard sodium hydroxide titration solution: c(NaOH) is about 0.1 mol/L. 5.5.3 Instruments and equipment
5.5.3.1 Ion exchange column: glass tube with an inner diameter of 10 mm and a length of 400 mm, equipped with a glass stopcock. 621
HG/T 2770—1996
5.5.3.2 pH meter: measuring range pH 0～14, graduation value 0.02pH, 5.5.3.3 calomel electrode.
5.5.3.4 glass electrode.
5.5.4 analysis steps
5.5.4.1 preparation of ion exchange column
fix the ion exchange column on the rack, close the piston, fill the bottom of the column with 1cm thick glass wool, pour about 10ml water to soak. Pour the resin into the column, make the resin bed height 300mm. Soak it with hydrochloric acid solution for later use. Before use, the resin should be treated according to the pre-use treatment process in Appendix A, and then it can be injected.
5.5.4.2 determination of sample
weigh about 0.5g sample (accurate to 0.0002g). Place in a 100mL beaker, add 10ml of water, stir thoroughly, and inject. Use water as the elution solution, control the column flow rate to (5.5~~6.0)mL/min, and wash until the effluent is neutral (pH test paper test). Collect the washing solution in a 250mL volumetric flask, dilute with water to the scale, and shake. Take 100.0mL of the test solution in a 250ml beaker, place the beaker on an electromagnetic stirrer, put in an electromagnetic stirrer, and start the stirrer. Insert the glass electrode (measuring electrode) and the saturated calomel electrode (reference electrode) into the solution and connect it to the pH meter. Adjust the zero point positioning. Adjust the pH to about 3 with sodium hydroxide standard titration solution. Then titrate with sodium hydroxide standard titration solution. Record the total volume and corresponding pH value after adding sodium hydroxide standard titration solution each time. When the pH is in the range of 4-6 and 7-9, only 0.10mL is added each time. Calculate △pH and ApH. Record another pH value after ApH reaches the maximum value. For the record format, please refer to Appendix B. 5.5.5 Expression of analysis results
The volume V of the sodium hydroxide standard titration solution consumed in the titration of the terminal phosphorus is calculated according to formula (3): V = (v. + 0.1×)
) (V + 0.1×)
Where: Vi is the total volume of the sodium hydroxide standard titration solution added before △pH reaches the maximum value when the pH is between 4 and 6, mL; Vi is the total volume of the sodium hydroxide standard titration solution added before ApH reaches the maximum value when the pH is between 7 and 9, mL; b is the last positive value of △pH when the pH is between 4 and 6; b2 is the last positive value of △pH when the pH is between 7 and 9; B1 is the sum of the absolute values of the last positive value and the first negative value of △pH when the pH is between 4 and 6; B2 is the sum of the absolute values of the last positive value and the first negative value of △pH when the pH is between 7 and 9. The average degree of polymerization X is calculated according to formula (4):
X:=vx0.070 97 ×100
m×250
_ 0. 112 8 X Xi m
Wherein: X -——mass percentage of phosphorus pentoxide (P,O,) measured in 5.3, %; V——volume of sodium hydroxide standard titration solution consumed for titrating terminal phosphorus, mL; actual concentration of sodium hydroxide standard titration solution, mol/L; m--—mass of sample, g
0. 070 97-
5.5.6 Allowable difference
(3)
mass of phosphorus pentoxide expressed in grams equivalent to 1.00mL sodium hydroxide standard titration solution Cc(NaOH)=1.000mol/L.
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference between the parallel determination results shall not exceed 1. 5.6 Determination of pH value
5.6.1 Reagents and materials
Water without carbon dioxide.
5.6.2 Instruments and equipment
HG/T 2770—1996
5.6.2.1 pH meter: the measuring range is pH 0~～14, and the graduation value is 0.02pH. 5.6.2.2 Calomel electrode.
5.6.2.3 Glass electrode.
5.6.3 Analysis steps
Weigh 1.00g of sample (accurate to 0.01g), place it in a 150mL beaker, dilute it to 100ml with water without carbon dioxide, place it on an electromagnetic stirrer, and stir it for 5min. Let it stand for 10min, and measure the pH value of the suspension with a pH meter. 5.6.4 Allowable difference
The arithmetic mean of the parallel determination results is taken as the measurement result. The absolute difference of the parallel determination results shall not exceed 0.3 pH units. 5.7 Determination of fineness
5.7.1 Instruments and equipment
5.7.1.1 Test sieve: in accordance with GB/T6003R40/3 series, Φ200mm×50mm/0.15mm, with sieve cover and sieve bottom; 5.7.1.2 No. 11 wool brush.
5.7.2 Analysis steps
Weigh 10g of sample (accurate to 0.01g). Place it in the test sieve and brush the sample lightly with a wool brush until there is no trace of the sample on the black paper under the sieve. Move the sieve residue to a surface dish of known mass and weigh it (accurate to 0.0002g). 5.7.3 Expression of analysis results
Fineness X expressed as mass percentage. Calculate according to formula (5): X
Where: ml—mass of sieve residue, g;
m—mass of test material, g.
5.7.4 Allowable difference
m2ml ×100
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 1.0%. 6 Marking, packaging, transportation, storage
6.1 The packaging of industrial ammonium polyphosphate should have firm and clear markings, including: manufacturer's 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 ammonium polyphosphate shipped from the factory should be accompanied by a quality certificate. The contents include: manufacturer's 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 ammonium polyphosphate is double-packed: the inner packaging is a polyethylene plastic film bag with a thickness of 0.03mm to 0.05mm; the outer packaging is a plastic woven bag, and its performance and inspection methods should comply with the provisions of Type B in GB/T8946. The net weight of each bag of this product is 40kg. 6.4 The inner bag of industrial ammonium polyphosphate packaging is manually 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 edge of the bag, and sewn with vinyl thread or other thread of equivalent quality at a distance of not less than 15mm from the edge of the bag. The stitch length is 7mm~~12mm, the stitches are neat and uniform, and there are no leaks or skipped stitches. 6.5 Industrial ammonium polyphosphate should be covered during transportation to prevent rain and moisture. 6.6 Industrial ammonium polyphosphate should be stored in a cool and dry place to prevent rain and moisture. 6.7 Industrial ammonium polyphosphate is susceptible to moisture. From the date of leaving the factory, the storage period is one year. The presence of loose blocks does not affect the use. 623
HG/T 2770--1996
Appendix A
(Appendix to the standard)
Regeneration of resin
After each sample elution and separation, 200mL.1+1 hydrochloric acid solution is passed through the resin bed and soaked overnight to regenerate the resin. Before use, let 50mL of hydrochloric acid solution flow through the column, close the exchange column piston, fill the column with water, plug the rubber stopper, invert several times to loosen the resin and discharge air bubbles. Fix the column vertically on the rack, wash the resin slowly with water first, and then wash at a flow rate of (5.5~6.0)mL/min until the effluent is neutral (pH test paper test). Keep the liquid level 1cm higher than the resin layer, close the exchange column and set aside. Appendix B
(Suggested Appendix)
Example of the average polymerization degree determination test record format Sodium hydroxide standard
Volume of titration solution/mL
V= (5.40 + 0.1× 0.03+0.04)-(3.50+0.1×0.05+0.16）
= 1.92(mI.)
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