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Record number: 2765-1999
HG/T 3583-1999
This standard is formulated based on enterprise standards, domestic production levels and user requirements. This standard has six indicators: phosphorus pentoxide content, calcium oxide content, moisture, pH value, hydrochloric acid insoluble content, and particle size. The analytical methods of this standard are: the determination of phosphorus pentoxide content is carried out by the quinoline phosphomolybdic acid weight method, the determination of calcium oxide is carried out by the EDTA volumetric method, the moisture content is determined by the general method for determining the moisture content in chemical products by the weight method, the pH value is determined according to GB/T9724 "General Rules for Determination of pH Value", the hydrochloric acid insoluble content is determined by the weight method, and the particle size is determined by the test sieve screening method with an aperture of 38um. This standard was proposed by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the inorganic salt product standardization technical centralized unit of the Ministry of Chemical Industry. The drafting units of this standard are: Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Sichuan Mianzhu Chemical General Plant, and Chengdu Chemical Research and Design Institute. The main drafters of this standard are Jiang Junhua, Li Xizhong, Yang Changlin and Yang Chao. This standard is entrusted to the Ministry of Chemical Industry's inorganic salt product standardization technical unit for interpretation. 1064
1 Scope
Chemical Industry Standard of the People's Republic of China
Active calcium phosphate
Activated calcium phosphafe
HG/T 3583—1999
This standard specifies the requirements, sampling, test methods, and marking, packaging, transportation and storage of active calcium phosphate. This standard applies to powdered active calcium phosphate synthesized by the phosphoric acid method. This product is mainly used as a dispersant for suspension polymerization in organic synthesis, as well as ceramics, biomaterials, fluorescent materials, etc. Molecular formula: Approximately Caio (Po.). (OH)2 Reference 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 parties using this standard should explore the possibility of using the latest version of the following standards. GB191—1990 Packaging, storage and transportation pictorial mark
GB/T 601—1988
GB/T 602—-1988
GB/T 603—1988
GB/T 1250-1989
GB/T 6284.--1986
GB/T 66 78-1986
GB/T 6682--1992
GB/T 8946 -1988
GB/T 8947-1988
GB/T 9724-1988
3 Requirements
Chemical reagents titration analysis (volume analysis) preparation of standard solutions for chemical reagents impurity determination preparation of standard solutions (negISO6353-1: 1982) Chemical reagents test methods for preparations and products used in preparation (neqISO6353-1: 1982) Limit value expression and determination method General method for determination of water content in chemical products Gravimetric method
Chemical product sampling general rules
Analytical laboratory water specifications and test methods (eqv1SO3696: 1987) Plastic woven bags
Composite plastic woven bags
Chemical reagents pH determination general rules
3.1 Appearance: Powdered active calcium phosphate is white amorphous powder. 3.2 Powdered active calcium phosphate should meet the requirements of Table 1. Table 1 Requirements
Phosphorus pentoxide content (as PzO,)/%Calcium oxide content (as Ca)/%
Water content! %
pH value (10g/L solution)
Content of hydrochloric acid insoluble matter/%
Particle size (through 38μm aperture sieve)/%
Approved by the State Administration of Petroleum and Chemical Industry on April 20, 1999
38.0~41.7
50.0~~53.5
Implementation on April 1, 2000
Test method
HG/T 3583—1999
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 solution, impurity standard solution, preparation and product required in the test shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603 unless otherwise specified.
Safety Tips: When using some strong acids in the test operation of this standard, be careful to avoid splashing on the skin. When using volatile acids, it should be carried out in a fume hood.
4.1 Determination of phosphorus pentoxide content
4.1.1 Method Summary
In an acidic medium, all phosphates in the test solution react with the added precipitant quinoline molybdate to form phosphomolybdic acid quinoline precipitate. The phosphorus pentoxide content is calculated by filtering, drying and weighing. 4.1.2 Reagents and Materials
4.1.2.1 Nitric acid solution: 1+1;
4.1.2.2 Quinoline molybdate solution.
Preparation:
Solution I: weigh 70g sodium molybdate and dissolve it in 150mL water; Solution II: weigh 60g citric acid and dissolve it in 150ml water and 85ml concentrated nitric acid; Solution III: slowly add Solution I to Solution II under constant stirring; Solution IV: add 35ml concentrated nitric acid and 5ml quinoline to 100mL water; add Solution V to Solution III, mix well and place for 24h to filter, add 280mL acetone to the filtrate, dilute to 1000mL with water, mix well, and store in a polyethylene bottle. 4.1.3 Instruments and equipment
4.1.3.1 Glass sand crucible: pore size is 5μm~15μm; 4.1.3.2 Electric oven: temperature can be controlled at 180℃±5℃. 4.1.4 Analysis steps
4.1.4.1 Preparation of test solution
Weigh about 0.5g of sample (accurate to 0.0002g), place in a 100ml beaker, moisten with a small amount of water, add 5mL nitric acid solution and 50mL water, dissolve and transfer to a 250mL volumetric flask, dilute with water to the scale, and shake well. This solution is test solution A, which is used to determine the content of phosphorus pentoxide and calcium oxide.
4.1.4.2 Preparation of reagent blank solution
Except for not adding sample, the amount of other reagents added is exactly the same as the preparation of test solution. And the same treatment is carried out at the same time as the sample. 4.1.4.3 Determination
Use a pipette to transfer 25 mL of the test solution and reagent blank solution into a 300 mL beaker, add 10 mL of nitric acid solution, dilute with water to 100 mL, heat to a slight boil for 15 min, add 50 mL of quinoline solution while hot, cover with a watch glass, keep warm in a water bath at (75 ± 5) °C for 15 min (add quinoline solution, do not stir during the warming to avoid the formation of lumps), then cool to room temperature, stir 3~~4 times during the cooling process, filter with a glass sand crucible that has been pre-heated at (180 ± 5) °C, first filter the upper clear liquid, wash the precipitate with water 5~6 times by pouring method, each time with about 20 mL of water. Finally, transfer the precipitate to a glass sand crucible for filtration, and then wash the precipitate with water 4 times. Place the glass sand crucible and the precipitate in an electric oven, dry at (180 ± 5) °C for 45 min, take out and cool slightly, place in a desiccator to cool to room temperature, and weigh. 4.1.5 Expression of analysis results
The content of phosphorus pentoxide (in terms of P,O2) expressed as mass fraction X is calculated according to formula (1): Xi = 0.032 07×(ml=ma)×100=25
m×250
Wherein: mi——mass of quinoline phosphomolybdate precipitate generated in the test solution, g; 32.07×(ml-m2)
mass of quinoline phosphomolybdate precipitate generated in the blank test solution, g; m2
·(1)
m-mass of the sample, g;
HG/T 3583--1999
0.03207: coefficient for converting quinoline phosphomolybdate into phosphorus pentoxide. 4.1.6 Allowable difference
Take the arithmetic mean of the results of parallel determinations as the determination result. The absolute difference between the parallel determination results shall not exceed 0.2%. 4.2 Determination of calcium oxide
4.2.1 Method summary
Add an excess of disodium ethylenediaminetetraacetic acid (EDTA) standard titration solution to the test solution to complex with calcium ions, use chrome black T as an indicator, and use zinc standard titration solution to titrate the excess disodium ethylenediaminetetraacetic acid (EDTA). 4.2.2 Reagents and materials
4.2.2.1 Magnesium chloride.
4.2.2.2 Nitric acid solution: 1+3.
4.2.2.3 Ammonia water. Www.bzxZ.net
Ammonia water: 1+1.
Ammonia-ammonium chloride buffer solution A: pH~10.4.2.2.5
4.2. 2. 6
Standard titration solution of disodium ethylenediaminetetraacetate (EDTA): c(EDTA) is about 0.02 mol/L. Standard titration solution of disodium ethylenediaminetetraacetate (EDTA): c(EDTA) is about 0.05 mol/L. 4. 2. 2.7
4.2.2.8 Chrome black T solid indicator: 1% (mass fraction). Grind Chrome black T and sodium chloride in a mortar at a ratio of 1:99 and mix thoroughly. Store in a bottle with a ground stopper. 4.2.2.9 Standard titration solution of zinc oxide: c(ZnCl2) is about 0.1 mol/L. 4.2.3 Analysis steps
4.2.3.1 Preparation of ammonia-ammonium chloride Mg-EDTA buffer solution Weigh 0.25g magnesium chloride (accurate to 0.0002g) and place it in a 100mL beaker. Dissolve it in water and transfer it all to a 100ml volumetric flask. Dilute it to the mark with water and shake it well. This solution is solution B. Use a dry pipette to transfer 50mL solution B to a 250mL conical flask, add 5ml ammonia-ammonium chloride buffer solution A and a small amount of chrome black T indicator, and titrate with 0.02mol/L disodium ethylenediaminetetraacetic acid standard titration solution until the solution changes from purple-red to pure blue. Record the volume of 0.02mol/L disodium ethylenediaminetetraacetic acid standard titration solution consumed. Take another 0.02mol/L disodium ethylenediaminetetraacetic acid standard titration solution with the same consumption as above, add it to the remaining solution B, shake it and set aside (i.e. Mg-EDTA solution).
Weigh 20g of ammonium chloride (accurate to 0.01g), place it in a 300mL beaker, add 200mL of water to dissolve it, then add 100mL of ammonia water, and then add all of the above Mg-EDTA solution. After mixing, transfer all to a 1000mL volumetric flask, dilute with water to the scale, and shake well. This solution is ammonia-ammonium chloride Mg-EDTA buffer solution C. 4.2.3.2 Determination
Use a pipette to transfer 25 mL of test solution A (4.1.4.1) into a 250 mL conical flask. Use 1+1 ammonia water to adjust the test solution until a slight precipitate is precipitated. Then use 1+3 nitric acid to adjust the solution until the precipitate is just dissolved. Accurately add 30 mL of 0.05 mol/L disodium ethylenediaminetetraacetic acid standard titration solution, then add 10 mL of ammonia-ammonium chloride Mg-EDTA buffer solution (i.e., solution C) and a small amount of chrome black T indicator. Use 0.05 mol/L zinc oxide standard titration solution to titrate until the solution changes from pure blue to purple, which is the end point. 4.2.3.3 Expression of analysis results
The calcium oxide content (calculated as CaO) expressed as mass percentage (X2) is calculated according to formula (2): X - (ViG - Vec)X 0.056 08 × 100 56.08 ×(Vc1 - Vec)25
m×250
Wherein: Vi---*--the volume of 0.05 mol/L disodium ethylenediaminetetraacetic acid standard titration solution added in the titration, mL; V,--the volume of 0.05 mol/L zinc oxide standard titration solution consumed in the titration, mL;)-0.05 mol/L actual concentration of disodium ethylenediaminetetraacetic acid standard titration solution, moi/L;.(2)
HG/T 3583—1999
-0.05mol/1. Actual concentration of zinc oxide standard titration solution.mol/I.; mass of sample, g;
0.05608—-mass of calcium oxide (CaO) expressed in grams equivalent to 1.00ml disodium ethylenediaminetetraacetic acid standard titration solution [c (EDTA) = 1.000mol/1, g.
4.2.3.4 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%. 4.3 Determination of moisture
Carry out in accordance with the provisions of GB/T6284.
4.4 Determination of pH
4.4.1 Summary of method
Same as Chapter 3 of GB/T9724—88.
4.4.2 Instruments and equipment
Same as Chapter 5 of GB/T9724-88.
4.4.3 Reagents and materials
Water without carbon dioxide.
4.4.4 Analysis steps
Weigh 1g of sample (accurate to 0.01g), place in a 150ml beaker, add 100mL of water without carbon dioxide, stir for 15min, let stand, take the clear liquid and measure according to Chapter 6 of GB/T9724-1988. 4.5 Determination of hydrochloric acid insoluble matter
4.5.1 Summary of method
Dissolve the sample in hydrochloric acid, filter with a glass sand crucible, wash, dry, weigh, and calculate the insoluble matter content. 4.5.2 Reagents and materials
4.5.2.1 Silver nitrate solution: c (AgNO.) is about 0.1 mol/L; 4.5.2.2 Hydrochloric acid solution: 1+1.
4.5.3 Instruments and equipment
4.5.3.1 Glass sand crucible: filter plate pore size 5μm15μm; 4.5.3.2 Constant temperature water bath;
4.5.3.3 General laboratory instruments and equipment. 4.5.4 Analysis steps
Weigh about 1g of sample (accurate to 0.0002g), place it in a 200mL beaker, add a small amount of water to moisten it, add 20mL of hydrochloric acid solution to dissolve it, cover it with a watch glass, steam it in a water bath until it is almost dry, and add 20mL of water to dissolve it. Filter with a glass crucible that has been dried to constant weight at 105℃～110℃, and wash the residue with hot water until the filtrate does not contain chloride ions (check with silver nitrate solution). Dry at 105℃～110℃ to constant weight. 4.5.5 Expression of analysis results
The hydrochloric acid insoluble content (X,) expressed as mass fraction is calculated according to formula (3): Xg = m2=m>
Where: mi---mass of glass crucible, g; m2---mass of glass crucible and hydrochloric acid insoluble matter, g; m——mass of sample, g.
4.5.6 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 0.03%. 4.6 Determination of particle size
4.6.1 Summary of method
HG/T3583—1999
The percentage of the mass of the sample after passing through a test sieve with a certain aperture to the mass of the sample. 4.6.2 Reagents and materials
95% ethanol.
4.6.3 Instruments and equipment
Test sieve: in accordance with GB/T6003:-1985 "Test sieve" R40/3 series Φ50mm×50mm/38μm. 4.6.4 Analysis steps
Weigh about 5g of sample (accurate to 0.01g), place it in a sieve that has been wetted with 95% volume fraction ethanol after constant weight, wet the sample with ethanol, hold the upper end of the sieve, immerse the sieve in water, and gently scrub it with a medium wool pen until there are no white particles in the water. Rinse twice with water and once with ethanol. Place in an oven at 105℃～110℃ and dry to constant weight. 4.6.5 Expression of analysis results
Particle size (X.) expressed as mass fraction is calculated according to formula (4): X = m-(m=ma)×100
Wherein, m. mass of the sample, g;
mt—mass of the test sieve and residue, g; mass of the test sieve, g.
4.6.6 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 Inspection rules
5.1 All items specified in this standard are factory inspection items. 5.2 Each batch of products shall not exceed 10t.
5.3 Determine the number of sampling units according to the provisions of 6.6 of GB/T6678--1986. Each plastic woven bag is a packaging unit. When sampling, insert the sampler obliquely from the top of the packaging bag to three-quarters of the depth of the material layer to take a sample. Take out no less than 50g of sample from each selected packaging unit, mix the sample thoroughly, reduce it to about 500g by quartering, and immediately put it into two clean, dry wide bottles and seal them. Stick labels on the bottles, indicating the manufacturer's name, product name, batch number, sampling date and name of the sampler. One bottle is used as an experimental sample and the other is kept for three months for future reference.
5.4 Industrial active calcium phosphate 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 leaving the factory meets the requirements of this standard. If any indicator in the inspection results does not meet the requirements of this standard, re-sampling shall be carried out from twice the amount of packaging units for re-inspection. Even if only one indicator in the re-inspection results does not meet the requirements of this standard, the entire batch of products shall be unqualified. 5.5 According to 5.2. The rounded value comparison method specified in the regulations shall be used to determine whether the test results meet the standards. 6. Marking, packaging, transportation and storage
6.1 The packaging bag of active calcium phosphate should have firm and clear markings, including the manufacturer's name, address, product name, trademark, net weight, this standard number, and the "wet-afraid" mark specified in GB191. 6.2 Each batch of products leaving the factory should be accompanied by a quality certificate. The content includes the manufacturer's name, address, product name, trademark, net content, batch number or production date, proof that the product quality meets this standard and this standard number. 6.3 Active calcium phosphate is packaged in polypropylene woven bags lined with plastic bags. The inner packaging uses polyethylene plastic film bags with a thickness of not less than 0.08mm. The outer packaging uses polypropylene woven bags. Its performance and inspection methods should comply with the relevant provisions of GB/T8946. The net content of each bag of this product is 10kg or 20kg.
6.4 When packaging, put the active calcium phosphate into the inner bag, exhaust the remaining air in the bag, tie the inner bag with vinyl rope or other rope of equivalent quality, fold the outer bag 1069
HG/T35831999
at a distance of not less than 30mm from the edge of the bag, and sew the outer bag with vinyl thread or other thread of equivalent quality at a distance of not less than 15mm from the edge of the bag. The stitches are neat and the stitch length is uniform. There is no leakage or skipping. 6.5 Active calcium phosphate should be covered during transportation to prevent sun exposure, rain, and packaging damage. 6.6 Active calcium phosphate should be stored in a ventilated and dry warehouse to prevent sun exposure and moisture. 1070
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