GB/T 5761-1993 Suspension process general purpose polyvinyl chloride resin
Some standard content:
National Standard of the People's Republic of China
Suspension polyvinyl chloride resins of general purpose
1 Subject content and scope of application
GB/T 5761-93
Replaces GB5761-86
This standard specifies the model, technical requirements, test methods, inspection rules and marking, packaging, storage and transportation of suspension polyvinyl chloride resins.
This standard applies to general-purpose polyvinyl chloride resins produced by the suspension process. 2 Reference standards
GB1.3 Guidelines for standardization work Provisions for the preparation of product standards GB 2913
GB 2914
GB2915
GB2916
GB2917
GB3400
GR3401
GB 3402
GB4611
GB 4615
GB6679
GB9348
GB 9349
3Product categories
Test method for whiteness of plastics
Test method for volatile matter (including water) of polyvinyl fluoride resinsTest method for conductivity of aqueous extract of polyvinyl chloride resinsTest method for dry sieving of polyvinyl chloride resins
Test method for thermal stability of polyvinyl chlorideCongo red method and PH methodDetermination of plasticizer absorption of general-purpose polyvinyl fluoride resins at room temperatureDetermination of viscosity of dilute solution of polyvinyl fluoride resinsName of polyvinyl homopolymer and copolymer resins
Test method for "fish eye" of general-purpose polyvinyl chloride resinsDetermination method for residual vinyl chloride monomer content in polyvinyl chloride resinsSolid chemicals General rules for product sampling
Determination of impurities and foreign particles in polyvinyl chloride resins Determination of thermal stability of polyethylene homopolymers, copolymers and compositions Color change method Suspension method The product model of general-purpose polyvinyl chloride resins consists of four items specified in GB3402, namely, product name, polymerization method and symbols for use, and viscosity classification number (see Table 1): Approved by the State Bureau of Technical Supervision on January 6, 1993 and implemented on October 1, 1993
Classification number n
Viscosity number, ml./g
4 Technical requirements
4.1 Appearance: white powder.
156~144
143~136
Physical and chemical properties shall meet the requirements of Table 2.
GB/T 5761-93
Viscosity classification
135~127
126~119
Viscosity classification
Application classification
Polymerization method
Product name
118~107
106~96
86~73
GB/T5761—93
(99~69)
Superior product
(09~29)
108096
(9~99)
96~901
Superior product
[0001~001
(99~89)
201811
Superior product
(69~02)
000090
Superior product
Superior product
Superior product
%(ot0.09)
.8/Tu*
5 Test method
5.1 Appearance evaluation
Visual observation.
5.2 Determination of viscosity number (or K value and degree of polymerization) 5.2.1 Determination of viscosity number
Perform according to GB3401.
5.2.2 Determination of K value
GB/T 5761—93
According to GB3401. K value is calculated as follows: K 10° ×(1 lg//1)+V1+(3 + 300/c +2. 251g./): igr./)150+3c
Where: t. ——arithmetic mean of the three flow-through times of the solution, s; arithmetic mean of the three flow-through times of the solvent, s; te
Ct——concentration of the solution, g/100mL.
The test result is the arithmetic mean of the two parallel results, rounded to an integer. 5.2.3 Determination of average degree of polymerization
According to Appendix A.
5.3 Determination of apparent density
According to Appendix A of GB3402.
5.4 Determination of plasticizer absorption
Perform according to GB3400.
5.5 Determination of volatile matter (including water) content shall be carried out according to GB2914. The heating time in the oven at 110±2℃ is 1h, and the result is calculated according to the weight loss in 1h. 5.6 Determination of sieve residue
Perform according to GB2916.
5.7 Determination of "fish eye" number
Perform according to GB4611.
5.8 Determination of conductivity of water extract
Perform according to GB2915.
5.9 Determination of impurity particle number
Perform according to GB9348.
5.10 Determination of residual vinyl chloride content
Perform according to GB4615.
5.11 Determination of whiteness (160℃, 10min) shall be carried out in accordance with Appendix B.
6 Inspection rules
6.1 Batch
GB/T5761-93
Products obtained from a single batch or products from several batches with the same polymerization conditions are mixed uniformly as a batch. 6.2 Sampling
6.2.1 Random sampling is carried out from the total number of bags in the batch pile according to the number of sampling units specified below. When the total number of bags is less than 500, it is determined according to Table 3; when it is greater than 500, it is determined according to the formula (n) = 3×N (N is the total number of bags), and any decimals are rounded up to integers. Table 3
Total number of bags
11~49
82~101
102~123
124~151
152~181
Number of sampling bags
Total number of bags
182~216
217~254
255~296
297~3 43
344~394
395~450
451~512
Number of sampling bags
6.2.2 During sampling, use a sampling probe (Appendix A and Appendix C of GB6679 or similar probe) to vertically insert from the center of the bag to 3/4 of the depth, and take uniform samples or use a continuous automatic sampler to automatically sample at intervals determined by the number of sampling units on the packaging line. 6.2.3 The sampling volume shall not be less than 2kg. After mixing, divide it into two clean and dry ground-mouth glass bottles (or three-layer plastic bags), seal them tightly, and mark the model, batch number and sampling time. One copy is for testing and the other copy is kept for three months for future reference. 6.3 Inspection before delivery
6.3.1 Before delivery, the product shall be inspected by the technical inspection department of the manufacturer to ensure that each batch of products meets the requirements of this standard. A quality inspection report shall be attached, which includes the manufacturer name, product name, model, batch number, batch size, quality index, grade, production date, and stamped with the inspection seal and the inspection personnel seal. 6.3.2 The viscosity number, apparent density, volatile content, 0.25mm sieve residue, number of impurity particles, number of "fish eyes", residual vinyl chloride content and other indicators in the technical requirements are mandatory inspection items for each batch. Plasticizer absorption, 0.063mm sieve residue, whiteness (160℃, 10min) and conductivity of water extract are random inspection items in the type inspection items. In continuous normal production, it should be ensured that the indicators specified in this standard are met. Random inspection shall be carried out once every quarter. If the random inspection does not meet the standards, each batch shall be inspected until the inspection results of five consecutive batches meet the requirements of the standard. Only then can normal random inspection be carried out. Type inspection shall be carried out in accordance with the provisions of Article 6.6.1 of G31.3.
6.3.3 If any item in the inspection result does not meet the technical requirements of this standard, sampling shall be repeated with double the number of sampling units from the same batch of products, and the re-inspection results shall be used to determine. If it still does not meet the technical requirements of this standard, it is a non-conforming product. 6.4 User acceptancebzxz.net
The user unit has the right to accept the received products in accordance with the provisions of this standard. If it is found that the product does not meet the provisions of this standard, it shall submit handling opinions to the manufacturer within three months from the date of leaving the factory. If there is a dispute, the quality supervision and inspection agency shall conduct arbitration inspection. If the quality of the product is affected by improper storage and transportation management, the storage and transportation unit shall be responsible. 7 Marking, packaging, storage and transportation
7.1. Marking
The packaging bag should be marked with the trademark, product name, product standard number, net weight, model, grade and manufacturer name. 7.2. Packaging
This product is packed in four-layer "kraft" paper bags, polypropylene woven bags or composite bags of "kraft" paper and polypropylene woven fabrics lined with plastic film bags thicker than 0.1mm. The seal should ensure that the product is not contaminated or leaked during normal storage and transportation. The net weight of each bag is 25.0±0.2kg. 7.3. Storage
GB/T5761-93
The product should be stored in a dry and ventilated warehouse, stored separately in batches, and must not be piled in the open air to prevent sunlight and moisture. 7.4. Transportation
The transportation must be carried out by clean and covered transportation vehicles to prevent rain. This product is non-dangerous goods.
A1 Reagent
Nitrobenzene (HG3-963).
A2 Instruments
A2.1 Island viscometer, as shown in Figure A1. D.11
Ball AD, 18
Scale line 1
GB/T 5761 --- 93
Appendix A
Determination of average degree of polymerization
(Supplement)
Upper scale line (D, 3)
B (1.3 ± 0.2mL)
Lower scale line (D, 0.52 ± 0.04)
The lower end of the capillary should have the same curvature as the upper end of the capillary
Figure A1 Ubbelohde viscometer
A2.2 Glycerol (propylene glycol) bath, controllable at 100 ± 2℃. A2.3 Constant temperature water bath, can control 30±0.05℃. A2.4 Portable aspirator, 2.30kPa.
A2.5 Analytical balance, sensitivity 0.1mg.
A2.6 Stopwatch, scale 0.1s.
A3 Operation steps
Preparation of test solution
GB/T 5761—93
A3.1.1 Weigh 200±0.1mg of dried and cooled polyvinyl chloride sample and accurately put it into a 50mL volumetric flask with a glass stopper. A3.1.2 Add about 40mL of nitrobenzene and heat in a glycerol bath maintained at 100±2℃, shaking intermittently to completely dissolve the sample. A3.1.3 Take out the volumetric flask and cool it to room temperature. Then place it in a constant temperature water bath at 30±0.05℃ for 20 minutes, dilute it to the scale with nitrobenzene at the same temperature, filter it with dry filter paper, and use it as the test solution. A3.2 Test
A3.2.1 Place the test solution in viscometer ball A until the liquid level of the solution is between the two scale lines engraved on ball A, so that the solution becomes horizontal between the two scale lines of the ball. A3.2.2 Then immerse the viscometer vertically in a constant temperature water bath, maintain the temperature at 30±0.05℃, and keep ball C below the horizontal plane. A3.2.3 Connect viscometer tubes 2 and 3 to latex tubes. When the test solution reaches 30±0.05℃, close the rubber tube of tube 3, draw the solution through the rubber tube attached to tube 2 and inject it into ball B to the upper scale, then open the ports of tubes 2 and 3. A3.2.4 Immediately use a stopwatch to measure the time required for the liquid level to drop from the upper scale to the lower scale, accurate to 0.1 s. A3.2.5 Repeat the test and take the average value. A3.2.6 Perform the same operation with nitrobenzene without sample for calibration. A4 Calculation
A4.1 Specific viscosity nap
Calculate according to formula (A1):
Where: t is the outflow time of nitrobenzene without sample, s; the outflow time of the test solution, s.
A4.2 Intrinsic viscosity (n)
Calculate according to formula (A2):
Where: n.
Relative viscosity (t2/t);
Specific viscosity;
-solution concentration, g/L.
A4.3 Average degree of polymerization P
Calculate according to formula (A3):
Where:-
B1 Instrument
Intrinsic viscosity.
. Vnep Ing.
P = 500[antilg o.168
Appendix B
Whiteness (160℃, 10min) Test Method
(Supplement)
B1.1 Heat aging test chamber, with rotating disk and blast, the temperature inside the chamber is uniform and can be controlled at 160±2℃. 154
·(A2)
B1.2 Weighing bottle, 975mm×35mm.
B1.3 Pan balance, sensitivity 0.5g.
B2 Test steps
GB/T 576193
2.1 Weigh 9.5~10.5g of resin sample and spread it evenly in the weighing bottle. Then put the weighing bottle with the sample on the turntable outside the test box and fix it with a clip.
B2.2 Heat the test box and adjust it to 160±2℃. Quickly place the turntable in the test box so that the upper plane of the sample bottle is 1cm away from the thermometer. Immediately close the door and start timing to make the turntable rotate. At this time, the temperature of the test box is not lower than 155℃. Continue to heat up to 160±2℃. B2.3 Turn off the power of the test box at 10min±5s, take out the turntable, crush the agglomerated sample with a sample spoon and mix it evenly. B2.4 Determine the whiteness according to the whiteness test method for powder samples specified in GB2913. B2.5 Take the arithmetic average of the two measured values of parallel tests as the result. If the relative deviation is greater than 1%, retest is required. B2.6 When taking or placing the turntable, the arms should be equipped with protective gear to avoid burns. Additional Notes:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Polyvinyl Chloride Resin Product Sub-Technical Committee of the National Plastic Standardization Technical Committee. This standard was drafted by the Jinxi Chemical Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are An Shaohua, Sun Lijuan, Pan Guirong, Du Fengmei, and Chen Yanru. The superior products of this standard refer to the superior product indicators in the Soviet national standard FOCT14332 "Suspension Polyvinyl Chloride Resin". 155At 05°C, close the rubber tube of tube 3, draw the solution through the rubber tube attached to tube 2 and inject it into ball B to the upper scale, then open tubes 2 and 3. A3.2.4 Immediately use a stopwatch to measure the time required for the liquid level to drop from the upper scale to the lower scale, accurate to 0.1 s. A3.2.5 Repeat the test and take the average value. A3.2.6 Perform the same operation with nitrobenzene without sample for calibration. A4 Calculation
A4.1 Specific viscosity nap
Calculate according to formula (A1):
Where: t is the outflow time of nitrobenzene without sample, s; the outflow time of the test solution, s.
A4.2 Intrinsic viscosity (n)
Calculate according to formula (A2):
Where: n.
Relative viscosity (t2/t);
Specific viscosity;
-solution concentration, g/L.
A4.3 Average degree of polymerization P
Calculate according to formula (A3):
Where:-
B1 Instrument
Intrinsic viscosity.
. Vnep Ing.
P = 500[antilg o.168
Appendix B
Whiteness (160℃, 10min) Test Method
(Supplement)
B1.1 Heat aging test chamber, with rotating disk and blast, the temperature inside the chamber is uniform and can be controlled at 160±2℃. 154
·(A2)
B1.2 Weighing bottle, 975mm×35mm.
B1.3 Pan balance, sensitivity 0.5g.
B2 Test steps
GB/T 576193
2.1 Weigh 9.5~10.5g of resin sample and spread it evenly in the weighing bottle. Then put the weighing bottle with the sample on the turntable outside the test box and fix it with a clip.
B2.2 Heat the test box and adjust it to 160±2℃. Quickly place the turntable in the test box so that the upper plane of the sample bottle is 1cm away from the thermometer. Immediately close the door and start timing to make the turntable rotate. At this time, the temperature of the test box is not lower than 155℃. Continue to heat up to 160±2℃. B2.3 Turn off the power of the test box at 10min±5s, take out the turntable, crush the agglomerated sample with a sample spoon and mix it evenly. B2.4 Determine the whiteness according to the whiteness test method for powder samples specified in GB2913. B2.5 Take the arithmetic average of the two measured values of parallel tests as the result. If the relative deviation is greater than 1%, retest is required. B2.6 When taking or placing the turntable, the arms should be equipped with protective gear to avoid burns. Additional Notes:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Polyvinyl Chloride Resin Product Sub-Technical Committee of the National Plastic Standardization Technical Committee. This standard was drafted by the Jinxi Chemical Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are An Shaohua, Sun Lijuan, Pan Guirong, Du Fengmei, and Chen Yanru. The superior products of this standard refer to the superior product indicators in the Soviet national standard FOCT14332 "Suspension Polyvinyl Chloride Resin". 155At 05°C, close the rubber tube of tube 3, draw the solution through the rubber tube attached to tube 2 and inject it into ball B to the upper scale, then open tubes 2 and 3. A3.2.4 Immediately use a stopwatch to measure the time required for the liquid level to drop from the upper scale to the lower scale, accurate to 0.1 s. A3.2.5 Repeat the test and take the average value. A3.2.6 Perform the same operation with nitrobenzene without sample for calibration. A4 Calculation
A4.1 Specific viscosity nap
Calculate according to formula (A1):
Where: t is the outflow time of nitrobenzene without sample,; the outflow time of the test solution, s.
A4.2 Intrinsic viscosity (n)
Calculate according to formula (A2):
Where: n.
Relative viscosity (t2/t);
Specific viscosity;
-solution concentration, g/L.
A4.3 Average degree of polymerization P
Calculate according to formula (A3):
Where:-
B1 Instrument
Intrinsic viscosity.
. Vnep Ing.
P = 500[antilg o.168
Appendix B
Whiteness (160℃, 10min) Test Method
(Supplement)
B1.1 Heat aging test chamber, with rotating disk and blast, the temperature inside the chamber is uniform and can be controlled at 160±2℃. 154
·(A2)
B1.2 Weighing bottle, 975mm×35mm.
B1.3 Pan balance, sensitivity 0.5g.
B2 Test steps
GB/T 576193
2.1 Weigh 9.5~10.5g of resin sample and spread it evenly in the weighing bottle. Then put the weighing bottle with the sample on the turntable outside the test box and fix it with a clip.
B2.2 Heat the test box and adjust it to 160±2℃. Quickly place the turntable in the test box so that the upper plane of the sample bottle is 1cm away from the thermometer. Immediately close the door and start timing to make the turntable rotate. At this time, the temperature of the test box is not lower than 155℃. Continue to heat up to 160±2℃. B2.3 Turn off the power of the test box at 10min±5s, take out the turntable, crush the agglomerated sample with a sample spoon and mix it evenly. B2.4 Determine the whiteness according to the whiteness test method for powder samples specified in GB2913. B2.5 Take the arithmetic average of the two measured values of parallel tests as the result. If the relative deviation is greater than 1%, retest is required. B2.6 When taking or placing the turntable, the arms should be equipped with protective gear to avoid burns. Additional Notes:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Polyvinyl Chloride Resin Product Sub-Technical Committee of the National Plastic Standardization Technical Committee. This standard was drafted by the Jinxi Chemical Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are An Shaohua, Sun Lijuan, Pan Guirong, Du Fengmei, and Chen Yanru. The superior products of this standard refer to the superior product indicators in the Soviet national standard FOCT14332 "Suspension Polyvinyl Chloride Resin". 155
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