GB/T 3401-2007 PDF English
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Determination of the viscosity of Poly (vinyl chloride) resins in dilute solution using capillary viscometers
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| GB/T 3401-1999 | English | 359 |
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Determination of viscosity number of PVC resins in dilute solution
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Determination of viscosity number of PVC resins in dilute solution
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GB/T 3401-2007: Determination of the viscosity of Poly (vinyl chloride) resins in dilute solution using capillary viscometers
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GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 83.080.20
G 32
Replacing GB/T 3401-1999
Determination of the viscosity of Poly (vinyl chloride)
resins in dilute solution using capillary viscometers
(ISO 1628-2.1998, Determination of the viscosity of Polymers in dilute solution
using capillary viscometers - Part 2. Poly (vinyl chloride) resins, MOD)
Issued on: AUGUST 13, 2007
Implemented on: FEBRUARY 1, 2008
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of the PRC;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 Terms and definitions ... 6
4 Principle ... 7
5 Materials ... 7
6 Apparatus ... 7
7 Sampling ... 8
8 Number of determinations ... 8
9 Procedure ... 8
10 Expression of results ... 11
11 Precision ... 13
12 Test report ... 13
Appendix A (Informative) Comparison between the chapter-clause number of
this Standard and the chapter-clause number of ISO 1628-2.1998 ... 23
Appendix B (Informative) Technical differences between this Standard and ISO
1628-2.1998 and their causes ... 25
Appendix C (Informative) Determination of the kinematic viscosity of
cyclohexanone ... 27
Appendix D (Informative) Solution preparation by conical flask method ... 29
Appendix E (Informative) Cleaning of apparatus ... 31
Foreword
This Standard modifies and adopts ISO 1628-2.1998 “Determination of the
viscosity of Polymers in dilute solution using capillary viscometers - Part 2. Poly
(vinyl chloride) resins” (English edition) (confirmed on October 3, 2003).
This Standard was redrafted in accordance with ISO 1628-2.1998. The table
for comparison between the chapter-clause number of this Standard and the
chapter-clause number of ISO 1628-2.1998 is listed in Appendix A.
Considering China’s national conditions, in the adoption of ISO 1628-2.1998,
this Standard has made some changes. The technical differences have been
incorporated into the text and identified by vertical single lines in the margins of
the clauses they refer to. A table for these technical differences and their causes
is given in Appendix B for reference.
For ease of use, the following editorial changes have been made to this
Standard.
a) The word “this part of ISO 1628” is replaced by the word “this Standard”;
b) REPLACE the comma “,” as a decimal point with a decimal point “.”;
c) DELETE the foreword of the international standard.
This Standard replaces GB/T 3401-1999 “Determination of viscosity number of
PVC resins in dilute solution”.
The main technical differences between this Standard and GB/T 3401-1999 are.
- MODIFY the standard’s name;
- MODIFY the requirement for the volatile-matter content of sample (Chapter
7 of 1999 edition; Chapter 1 of this edition);
- ADD the definition of K-value (3.2 of this edition);
- ADD test method A for sample weight of 0.250 g (9.1.1 of this edition);
- DELETE “Method 2” (8.1.2 of 1999 edition);
- MODIFY the range of sampling quantity (8.1.1 of 1999 edition; 9.1.2 of this
edition);
- MODIFY the range of control temperature of temperature-regulated bath
(8.2 of 1999 edition; 9.2 of this edition);
- MODIFY the relative deviation requirement for parallel determination
(Chapter 9 of 1999 edition; 10.1 of this edition);
- ADD the calculation of K-value (10.2 of this edition);
- ADD the chapter “Precision” (Chapter 11 of this edition);
- ADD Table 3 “Conversion of viscosity ratio (VR) to reduced viscosity (I) and
K-value”;
- CHANGE “Calculation method of cyclohexanone dosage in the preparation
of 0.005 g/mL solution by conical flask method” to Appendix D “Solution
preparation by conical flask method” (Appendix A of 1999 edition; Appendix
D of this edition);
- ADD Appendix A “Comparison between the chapter-clause number of this
Standard and the chapter-clause number of ISO 1628-2.1998”;
- ADD Appendix B “Technical differences between this Standard and ISO
1628-2.1998 and their causes”;
- CHANGE “Determination of the kinematic viscosity of cyclohexanone” to
Appendix C (Appendix B of 1999 edition; Appendix C of this edition);
- ADD Appendix E “Cleaning of apparatus”.
Appendix A, Appendix B, Appendix C, Appendix D, and Appendix E of this
Standard are informative appendixes.
This Standard was proposed by China Petroleum and Chemical Industry
Federation.
This Standard shall be under the jurisdiction of Branch of PVC Resin Products,
National Technical Committee 15 on Plastic of Standardization Administration
of China (SAC/TC 15/SC 7).
Drafting organizations of this Standard. Jinxi Research Institute of Chemical
Industry, Fujian Southeast Electrochemical Co., Ltd..
Main drafters of this Standard. Hao Jing, Sun Lijuan, Zhao Min, Chen Peiyun.
This Standard was first issued in 1982 and first revised in 1999.
Attention is drawn to the possibility that some of the elements of this Standard
may be the subject of patent rights. The issuing authority of this Standard shall
not be held responsible for identifying any or all such patent rights.
Determination of the viscosity of Poly (vinyl chloride)
resins in dilute solution using capillary viscometers
1 Scope
This Standard specifies conditions for the determination of the reduced
viscosity (also known as viscosity) and K-value of PVC resins. It is applicable
to resins in powder form which consist of homopolymers of the monomer vinyl
chloride and copolymers, terpolymers, etc., of vinyl chloride with one or more
other monomers, but where vinyl chloride is the main constituent. The resins
may contain small amounts of unpolymerized substances (e.g. emulsifying or
suspending agents, catalyst residues, etc.) and other substances added during
the course of the polymerization. This Standard is not applicable, however, to
resins having a volatile-matter content in excess of 0.5%, when determined in
accordance with GB/T 2914. In addition to this, it is not applicable to resins
which are not entirely soluble in cyclohexanone.
The reduced viscosity and K-value of a particular resin are related to its
molecular mass, but the relationship varies depending on the concentration and
type(s) of other monomer(s) present. Hence homopolymers and copolymers
having the same reduced viscosity or K-value may not have the same molecular
mass.
The values determined for reduced viscosity and K-value, for a particular
sample of PVC resin, are influenced differently by the concentration of the
solution chosen for the determination. Hence the use of the procedures
described in this Standard will only give values for reduced viscosity and K-
value that are comparable when the concentrations of the solutions used are
identical.
2 Normative references
The clauses in the following documents, by reference in this Standard,
constitute the clauses of this Standard. For the dated references, the
subsequent amendments (not including errata content) or revisions do not
apply to this Standard. However, parties which have reached an agreement
according to this Standard are encouraged to study whether the latest edition
of these documents can be used. For the undated references, the latest edition
is applicable to this Standard.
GB/T 2914-1999 Plastics - Homopolymer and copolymer resins of vinyl
chloride - Determination of volatile matter (including water) (idt ISO
1269.1980)
3 Terms and definitions
The following terms and definitions apply to this Standard.
3.1 Reduced viscosity (also known as viscosity)
The ratio of the viscosity ratio increment to the polymer concentration c in the
solution.
If the solution concentration is low, the viscosity ratio η/η0 can be given by the
efflux time ratio t/t0, then the reduced viscosity can be expressed as.
The dimension of reduced viscosity is L3M-1.
The unit of reduced viscosity is m3/kg.
In practical applications, it is more convenient to use its 1/1000 (10-3m3/kg), that
is, mL/g. The so-called viscosity number refers to the reduced viscosity
(viscosity number) of this empirical unit.
The reduced viscosity is usually measured at a low concentration (less than 5
kg/m3, i.e., 0.005 g/mL) unless the concentration is increased for a polymer
having a low molecular mass.
3.2 K-value
A constant which is independent of the concentration of polymer solution and is
unique to the polymer sample, which is a measure of average degree of
polymerization.
Where.
9.1.1 Method A
WEIGH (0.250±0.005)g of resin, accurate to 0.0001 g; and TRANSFER it
quantitatively to the 50 mL volumetric flask (6.2.1). ADD about 40 mL of
cyclohexanone to the flask, swirling the flask by hand to prevent coagulation or
the formation of lumps. Continue dissolution by agitating for 1 h between
(80~85)°C using the agitator (6.4). CHECK visually that dissolution is complete.
If gelatinized particles are still visible, START again with a new portion of the
resin. COOL the solution to (25±1)°C and make up to the mark with
cyclohexanone at the same temperature. MIX the solution thoroughly by
shaking.
9.1.2 Method B
WEIGH (0.125±0.0025)g of resin, accurate to 0.0001 g; and TRANSFER it
quantitatively to the 25 mL volumetric flask (6.2.2). ADD about 20 mL of
cyclohexanone to the flask, swirling the flask by hand to prevent coagulation or
the formation of lumps. Continue dissolution by agitating for 1 h between
(80~85)°C using the agitator (6.4). CHECK visually that dissolution is complete.
If gelatinized particles are still visible, START again with a new portion of the
resin. COOL the solution to (25±1)°C and make up to the mark with
cyclohexanone at the same temperature. MIX the solution thoroughly by
shaking.
9.1.3 Alternative methods
In addition to preparing the solution according to the above two methods,
alternative methods for the preparation of the solution may be used, for example
the addition of a measured volume of solvent to a measured mass of test portion,
provided that the values obtained for the reduced viscosity and K-value can be
shown to be equivalent to those obtained with the method of solution
preparation described above. Such alternative methods of solution preparation
will require the amounts of solvent and test portion taken to be determined by
experiment, and may also require compensation for loss of solvent by
evaporation during the dissolution process (Appendix D gives the method of
solution preparation by conical flask).
9.2 Determination of efflux times
9.2.1 Determination of efflux times of solvent
9.2.1.1 The temperature of the temperature-regulated bath (6.6) shall be set
such that the temperature which is measured by the thermometer (6.7) lies in
the range (25±0.5)°C. The measured temperature shall be stable to ±0.05 °C
around the temperature at which the temperature-regulated bath has been set.
9.2.1.2 On the viscometer tube M and tube N, CONNECT the latex tube; and
PLACE the viscometer vertically in the temperature-regulated bath, so that the
liquid level exceeds the viscometer D ball by about 20 mm.
9.2.1.3 USE the filter funnel (6.3) to filter approximately 15 mL of cyclohexanone
into the viscometer through the L tube, at constant temperature for about 10
min.
9.2.1.4 When the temperature is balanced, CLOSE the M tube, SUCK the N
tube or PRESSURIZE on the L tube, so that the solvent, through the capillary,
slowly enters the C ball. When the liquid level rises to about 5 mm above the E-
line, STOP sucking or pressurizing. OPEN the M tube; and MEASURE the efflux
time of the liquid through the E-line to the F-line.
9.2.1.5 The efflux time first read is discarded, and it is repeatedly measured
three times. The arithmetic mean thereof is taken as the efflux time t0 of the
solvent. Efflux times with the control solvent cyclohexanone shall remain
constant to within 0.2 s for a given viscometer. If the difference between the two
successive average efflux times measured of the solvent is greater than 0.4 s,
the viscometer shall be cleaned (SEE Appendix E).
9.2.2 Determination of efflux times of solution
9.2.2.1 ASPIRATE the above solvent; USE the filter funnel (6.3) to filter
approximately 10 mL of solution into the viscometer through the L tube, so that
the solution is washed three times through the C ball and then the solution is
aspirated. Then, FILTER about 15 mL of the solution through the L tube into the
viscometer, at constant temperature for about 10 min.
9.2.2.2 According to 9.2.1.4, DETERMINE efflux times of the solution.
9.2.2.3 DISCARD the first efflux time reading. REPEAT the measurement of the
efflux time until two successive measurements differ by less than 0.25%. The
arithmetic mean thereof is taken as the efflux time t of the solution.
Note. The above is a manual procedure. Proprietary equipment is available which will
organize the charging of the viscometer with solution and solvent and measure the
respective efflux times automatically. The use of such equipment is included in the
scope of this Standard provided that all the procedures and verification checks
described above are followed by the automated procedure.
10 Expression of results
10.1 Reduced viscosity
Appendix A
(Informative)
Comparison between the chapter-clause number of this Standard and
the chapter-clause number of ISO 1628-2.1998
Table A.1 gives the comparison between the chapter-clause number of this
Standard and the chapter-clause number of ISO 1628-2.1998.
Table A.1 -- Comparison between the chapter-clause number of this
Standard and the chapter-clause number of ISO 1628-2.1998
Chapter-clause number of this Standard Corresponding chapter-clause number of the international standard
1 Paragraphs 1, 2, and 3 of 1
3.1 -
3.2 -
5 5.1
Figure 1 -
6.2.1 6.2
6.2.2 -
- Paragraph 1 of 9.1
9.1 Paragraphs 7 and 2 of 9.1
9.1.1 Paragraph 3 of 9.1
- Paragraphs 4 and 5 of 9.1
9.1.2 -
9.1.3 Paragraph 6 of 9.1
9.2.1 -
- Paragraph 1 of 9.2
9.2.1.1 Paragraph 2 of 9.2
9.2.1.2 -
9.2.1.3 -
9.2.1.4 -
9.2.1.5 Part content of paragraph 4 of 9.2
Appendix B
(Informative)
Technical differences between this Standard and ISO 1628-2.1998 and
their causes
Table B.1 gives the technical differences between this Standard and ISO 1628-
2.1998 and their causes.
Table B.1 -- Technical differences between this Standard and ISO 1628-
2.1998 and their causes
Chapter-
clause
number of
this
Standard
Technical differences Causes
Cover
MODIFY the standard’s name. The current national standard number does
not correspond to the various parts of ISO
1628. This revision still uses the former
standard number and cannot correspond to
the international standard name.
1 DELETE paragraphs 4 and 5 of Chapter 1 of ISO 1628-2.1998.
Does not meet the provisions of GB/T 1.1 for
the content of scope.
CITE Chinese standards which
adopt international standards.
DELETE other standards cited.
To adapt to China’s national conditions.
Other standards cited have not been
translated into Chinese national standards. To
facilitate standard application, the reference
content is added to the corresponding position
in the text.
The content for which ISO 1628-
2.1998 cites ISO 1628-1 is listed
as 3.1 and 3.2.
MAKE standard applications more convenient.
5 CHANGE 5.1 of ISO 1628-2.1998 to a paragraph.
Does not match China’s national standard
format.
6.1
ADD the specific content of the
referenced part in 6.1 of ISO
1628-2.1998.
ADD Figure 1.
MAKE standard applications more convenient.
MAKE standard applications more convenient.
Appendix C
(Informative)
Determination of the kinematic viscosity of cyclohexanone
C.1 Materials
C.1.1 Cyclohexanone, SEE Chapter 5.
C.1.2 Standard liquid of viscosity. The kinematic viscosity is similar to that of
cyclohexanone, such as GBW 13601.
C.2 Apparatus
SEE Chapter 6 for other apparatus.
Ubbelohde viscometer, model 1. The capillary diameter is 0.58 mm, with a
relative error of ±2%. The dimensions of other parts are shown in Figure 1.
C.3 Determination of the kinematic viscosity of cyclohexanone
C.3.1 Calibration of the coefficient of Ubbelohde viscometer
In a (20±0.05)°C constant temperature water bath, USE the model 1 Ubbelohde
viscometer to measure the efflux time t0 of the standard liquid of viscosity. The
coefficient of the Ubbelohde viscometer is calculated by the equation (C.1).
Where.
c - The coefficient of the Ubbelohde viscometer, in square meters per square
second (m2/s2);
ν0 - The kinematic viscosity of the standard liquid of viscosity, in square meters
per second (m2/s);
t0 - The efflux time of the standard liquid of viscosity, in seconds (s).
C.3.2 Determination of the kinematic viscosity of solvent cyclohexanone
In a (25±0.05)°C constant temperature water bath, USE the model 1 Ubbelohde
viscometer to measure the efflux time t1 of solvent cyclohexanone. The
kinematic viscosity of solvent cyclohexanone is calculated by the equation (C.2).
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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