HG/T 2364-1992 Determination of viscosity of dilute solutions of poly(alkylene terephthalate)
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Chemical Industry Standard of the People's Republic of China
HG/T 2364-92
ISO1628/5--86
Polyalkylene terephthalate dilute solution
Determination of viscosity number
Published on 1992-10-07
Ministry of Chemical Industry of the People's Republic of China
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Implementation on 1993-05-01| |tt||Chemical Industry Standard of the People's Republic of China
Polyalkylene terephthalate dilute solution
Determination of viscosity
HG/T2364-92
ISO1628/5-86
This standard is equivalent to the international standard ISO1628/5-1986 "Plastics-Determination of viscosity and intrinsic viscosity Part 5: Polyalkylene terephthalate".
1 Subject content and scope of application
This standard specifies the method for determining the viscosity and intrinsic viscosity of dilute solutions of polyethylene terephthalate, polybutylene terephthalate and their copolymers.
Polyethylene terephthalate uses a mixed solvent of phenol and 1,2-dichlorobenzene in a mass ratio of one to one. The rest of the polymers use meta-cresol solvent
2 Reference standards
GB1632 Standards for determining the viscosity and intrinsic viscosity of dilute polymer solutions Standardization guidelines and general conditions GB11995 Method for determining ash content in poly(terephthalate) 3 Principle
Measure the flow time of the solvent and the resin solution with a concentration of 0.005 g/mL at 25°C in a conventional manner, and calculate the viscosity from the flow time value and the solution concentration. In this method, the density difference and kinetic energy correction are very small and are not considered. 4 Reagents
Warning: The solvents used are toxic. Avoid contact with the skin and inhalation of their vapors. Mixed solvent of phenol and 1,2-dichlorobenzene: Weigh one part of phenol and dissolve it in one part of 1,2-dichlorobenzene (m/m). Weighing accuracy 4.1
Not more than 1%.
4.2 Meta-cresol: This reagent should meet the following specifications: Clear and colorless appearance;
The meta-cresol content is not less than 99% (m/m); the o-cresol content is not more than 0.3% (m/m); the water content is not more than 0.13% (m/m);
The purity of the reagent can be analyzed by gas chromatography. In order to make the reagent purity meet the requirements, meta-cresol needs to be distilled. This operation should be carried out under reduced pressure distillation under the protection of ammonia to prevent oxidation.
4.3 Storage of solvents: Solvents should be stored away from light, such as in brown glass bottles. The flow time of the used solvent should be measured at least once a day (see 7.3). If the solvent flow time differs from the initial flow time by more than 1%, the solvent should be replaced. 5 Instruments
5.1 Pulverizer: Pulverize the sample into particles with a diameter of about 0.5 mm. Approved by the Ministry of Chemical Industry of the People's Republic of China on October 7, 19921
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5.2 Volumetric flask: with ground glass stopper, 100 mL.5.3 Conical flask: with ground glass stopper, 150 mL.5.4 Burette: graduation is 0. 1mL.
HG/T2364—92
5.5 Steam bath: or other device that can heat the contents of the conical flask to 90~100℃, 5.6 Oil bath: can be heated to 135~145 or other device that can heat the contents of the conical flask to 135~145℃ 5.7 Magnetic stirrer: or other device that can continuously stir the contents in the conical flask with a stopper 5.8 Constant temperature bath: control the temperature at 25±0.05t. 5.9 Viscometer: air-liquid column Ubbelohde type. The main dimensions are shown in the figure on page 5. , any other viscometer that can get the same result can be used. This type of viscometer must be used in case of dispute. 5.10 Stainless steel screen, fused glass filter funnel with nominal pore size of 63~90um or micropore diameter of 40~100um, 5.11 Analytical balance: sensitivity 0.1mg.
5.12 Stopwatch: accurate to 0.1s.
6 Test sample
6.1 Solvent selection
Polyethylene terephthalate uses a mixed solvent of phenol and 1,2-dichlorobenzene (4.1); polybutylene terephthalate and the copolymer of polyethylene terephthalate and butylene terephthalate use meta-cresol (4.2) solvent.
6.2 Determination of inorganic matter or other additives in the sample If the content of inorganic matter or other additives in the sample exceeds 0.5% (m/m), the method in 6.3 should be considered when preparing the test solution. 6.2.1 Determination of inorganic matter content
If the sample contains inorganic materials, such as fillers or glass fiber piles, their content should be determined in accordance with GB11995. 6.2.2 Determination of other additives content
If the sample contains additives such as polyolefins or flame retardants, they should be determined by appropriate methods and the method used should be reported. 6.3 Preparation of test solution
Use one of the following methods
6.3.1 Method A
Weigh a sample ml. The weighing range is determined according to formula (1) (accurate to 0.2 mg). In grams: 0.5
T- [(w, +w,)/100]±0.01
Where: w——the content of inorganic matter in the sample determined according to 6.2.1, expressed in mass percentage; w——the content of other additives in the sample determined according to 6.2.2, expressed in mass percentage. Correction is necessary only when the content of inorganic matter and additives exceeds 0.5% (m/m) respectively. (1)
Transfer the sample to a volumetric flask (5.2), add 60 mL of solvent, cover the flask with a stopper and heat it on a steam bath (5.5), stirring from time to time until the polymer is completely dissolved (polymer degradation will not occur on a steam bath, and continuous stirring with a magnetic stirrer (5.7) can accelerate dissolution).
Highly crystalline polyethylene terephthalate samples (e.g., post-condensation molded slices, whose crystallinity can reach about 65%) do not dissolve on a steam bath even if stirred continuously. To dissolve a highly crystalline sample, it should be finely ground in a pulverizer (5.1) and heated in a 135-145°C oil bath (5.6) with continuous stirring to dissolve. At the above temperature, the polymer will undergo some degradation. The heating time should not exceed 30 min.
After dissolution, cool the volumetric flask and its contents to 25±2°C, add solvent at the same temperature to bring the volume to the 100 mL mark, and mix thoroughly. If magnetic stirring is used during dissolution, the removed stirring rod should be cleaned with this solvent, and all the washing liquid should be put into the volumetric flask. Standard Technology Quick Network wm.b2soao.ca Various standards industry information and science competition download HG/T2364-92
Calculate the polymer solution concentration p (g/mL) according to formula (2); .0
Wherein, w—same as formula (1);
wo—same as formula (1);
-mass of sample, g.
Note: Usually, the actual concentration of the test solution will be slightly higher than 0.005g/mL, but within the stated range, since the relative increase in viscosity is still linearly related to the concentration, the effect on viscosity can be ignored. 6.3.2 Method B
Weigh a sample mz, with a mass of about 0.4~0.6g (accurate to 0.2mg). Transfer the sample to a conical flask (5.3) and use a burette (5.4) to add a volume (mL) of solvent equal to the formula (3), accurate to 0.1mL. w.+w.
Wherein w—same as formula (1);
(3))
w. —-same as formula (1).
Only when the content of inorganic matter and additives exceeds 0.5% (m/m) respectively, w and w are needed to correct the temperature of the added solvent, which should be 25±2℃.
After stoppering the conical flask; heat the conical flask on a steam bath or, if necessary, on an oil bath according to the procedures and precautions described in 6.3.1 to dissolve the polymer, and cool to room temperature after dissolution. 7 Analysis Steps
7.1 Cleaning of Viscometer
Warning: Chromic acid solution and other similar cleaning fluids are toxic chemicals. Avoid contact with skin and inhalation of their vapors. Clean the viscometer before use if there are inconsistent readings and after a period of normal use (5.9). When cleaning, fill the viscometer with cleaning fluid and soak it for at least 12 hours. The cleaning fluid can be a chromic acid solution prepared with equal volumes of concentrated sulfuric acid and saturated potassium dichromate solution. After soaking, discard the cleaning fluid and clean the viscometer with distilled water first, then with a volatile solvent (such as freshly distilled acetone), and then dry it with a filtered slow air flow.
After the measurement, empty the viscometer of liquid, wash it with solvent and then with freshly distilled acetone or similar volatile solvent, and then dry it with air flow as above. www.bzxz.net
If the next solution to be tested is a polymer of the same type and has a similar viscosity, the viscometer can be emptied of the solution, washed with the solution to be tested, and then filled with the solution to be tested. 7.2 Preparation
When using a mixed solvent of phenol and 1,2-dichlorobenzene, a No. 1 C type viscometer can be selected. When using m-cresol as solvent, a No. 2 viscometer can be used.
The test solution is passed through a screen or a fused glass filter funnel (5.10) into the viscometer L tube (see Figure on page 5). The volume of liquid in the viscometer should be such that the liquid level is between the two markings after discharge. This operation should be done away from the constant temperature bath to avoid overflow and contamination of the constant temperature bath.
Install the viscometer in the constant overflow bath, ensure that the tube N is vertical and the upper mark E is at least 30mm below the bath surface. It takes at least 15min for the viscometer to reach the constant temperature bath temperature (25±0.05℃). 7.3 Flow time measurement
Close the M tube, suck air into the N tube or press air into the L tube, so that the liquid level reaches about 5mm above the E line. Close the N tube, keep the liquid level at 3
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, open the M tube, let the liquid flow out from the lower end of the capillary, when there is no liquid at the end of the capillary and the lower end of the M tube, open the N tube, and measure the time required for the lowest point of the liquid meniscus to reach the upper edge of the mark F from the upper edge of the mark E, which is the flow time (accurate to 0.2s). For polymer solutions containing a small amount of finely dispersed pigments such as carbon black, it may be necessary to observe the top end of the meniscus. The above pipeline can be opened and closed with a stopcock connected to one end of the tube or a clamp of a latex tube. Without emptying and refilling the test liquid, the flow time is immediately repeated until the difference between two consecutive measurement times is within 0.25%. Take the average of the two flow times as the flow time of the test liquid. Use the same viscometer and the same method to determine the average flow time of the solvent. For each set of tests, it is sufficient to measure the average flow time of the solvent only once, but the flow time of the solvent used must be measured at least once a day. If the difference between the average flow time of two consecutive measurements is greater than 0.4s, the viscometer should be cleaned.
8 Calculation of analysis results
Calculate the viscosity number (mL/g) according to formula (4):
Where: test solution flow time, s;
to——solvent flow time, s;
Polymer test solution concentration, g/mL
(4)
When the solution is prepared by method A, calculate the concentration p according to 6.3.1. When the solution is prepared by method B, the concentration p is equal to 0.005g/mL. For each sample viscosity number, at least two measurements are performed. A new solution shall be prepared each time until the difference between two consecutive measured values is no more than 3%. The average value of the two measurements shall be reported, rounded to 1, as the viscosity of the sample. 9 Test report
The test report shall include the following items:
Indicate the reference to this industry standard;
Complete identification of the sample
If the sample contains more than 0.5% (m/m) additives, the method used to determine the additives shall be stated: c
d. If the viscometer used is different from the No. 1 C type and No. 2 Ubbelohde type viscometer specified in this standard, the specifications of the viscometer used shall be stated;
The viscosity number obtained,
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Viscometer diagram
1—Graduate mark with a volume of 4±0.2mL; 2—When using a mixed solvent of phenol and 1,2-difluorobenzene, the inner diameter of the capillary is 0.73mm±2%; when using m-cresol, the inner diameter of the capillary is 1.03mm±2%; 3—Liquid filling mark standard Jiewang ww.bazoso.cm Various standards industry information competitive offline Additional notes:
HG/T2364—92
This standard was proposed by the Science and Technology Bureau of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Chemical Method Branch of the National Technical Committee for Plastics Standardization. This standard was drafted by Hangzhou Tape Factory, and the main drafters of this standard were Shuai Jinfang and Zhang Hongan. Standard Exchange Search Network m.baecao.cm Various Standards Industry Data Competitive Download People's Republic of China
Chemical Industry Standards
Polyalkylene terephthalate dilute solution
Determination of viscosity
HG/T2364-92
ISO1628/5-86
Editor Chemical Industry Standards Editorial Department
(Standardization Research Institute of Ministry of Chemical Industry)
Postal Code: 100013
Printing Chemical Industry Standardization Research Institute
Copyright reserved. No reproduction allowed
Format 880×12301/16 Printing Sheet Word Count 10000 First Edition July 1993
First Printing July 1993
Print Count 1500
Standard Exchange Search Network wm.baecao.cm Various Standards Industry Data Competitive Download 9cm Various types of standard industry materials are competitively charged for offline additional notes:
HG/T2364-92
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China, and is under the jurisdiction of the Chemical Method Branch of the National Plastics Standardization Technical Committee. This standard is drafted by Hangzhou Magnetic Tape Factory, and the main drafters of this standard are Shuai Jinfang and Zhang Hongan. Standard Exchange Search Network m.baecao.cm Various Standards Industry Data Competitive Download People's Republic of China
Chemical Industry Standards
Polyalkylene terephthalate dilute solution
Determination of viscosity
HG/T2364-92
ISO1628/5-86
Editor Chemical Industry Standards Editorial Department
(Standardization Research Institute of Ministry of Chemical Industry)
Postal Code: 100013
Printing Chemical Industry Standardization Research Institute
Copyright reserved. No reproduction allowed
Format 880×12301/16 Printing Sheet Word Count 10000 First Edition July 1993
First Printing July 1993
Print Count 1500
Standard Exchange Search Network wm.baecao.cm Various Standards Industry Data Competitive Download 9cm Various types of standard industry materials are competitively charged for offline additional notes:
HG/T2364-92
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China, and is under the jurisdiction of the Chemical Method Branch of the National Plastics Standardization Technical Committee. This standard is drafted by Hangzhou Magnetic Tape Factory, and the main drafters of this standard are Shuai Jinfang and Zhang Hongan. Standard Exchange Search Network m.baecao.cm Various Standards Industry Data Competitive Download People's Republic of China
Chemical Industry Standards
Polyalkylene terephthalate dilute solution
Determination of viscosity
HG/T2364-92
ISO1628/5-86
Editor Chemical Industry Standards Editorial Department
(Standardization Research Institute of Ministry of Chemical Industry)
Postal Code: 100013
Printing Chemical Industry Standardization Research Institute
Copyright reserved. No reproduction allowed
Format 880×12301/16 Printing Sheet Word Count 10000 First Edition July 1993
First Printing July 1993
Print Count 1500
Standard Exchange Search Network wm.baecao.cm Various Standards Industry Data Competitive Download 9
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