Designation: D 3030 – 95 An American National Standard

Standard Test Method for

Volatile Matter (Including Water) of Vinyl Chloride Resins1
This standard is issued under the fixed designation D 3030; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope mass loss defines quantitatively the volatile matter present in

1.1 This test method covers the quantitative determination the sample.
of the volatile matter (including water) present in vinyl 5. Significance and Use
chloride resins.
1.2 The values stated in SI units are to be regarded as the 5.1 The quantity of volatile components in a vinyl chloride
standard. resin can be established by this test method. This test method
1.3 This standard does not purport to address all of the does not identify the components.
safety concerns, if any, associated with its use. It is the 6. Apparatus
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 6.1 Oven—A forced-ventilation oven conforming to the
bility of regulatory limitations prior to use. requirements for Type IIA in Specification E 145. The oven
should be capable of maintaining a temperature of 110 6 1°C
NOTE 1—This test method and ISO 1269–1980 are identical in all when the damper is half open and the vent is wide open.
technical details. 6.1.1 The oven shall be equipped with a calibrated ASTM
2. Referenced Documents thermometer and the proper stem correction shall be applied to
the temperature measurement.
2.1 ASTM Standards: 6.1.2 The oven temperature shall be controlled by an
D 618 Practice for Conditioning Plastics and Electrical accurate, reliable thermoregulator, maintaining the set point
Insulating Materials for Testing2 within 60.5°C or better.
D 883 Terminology Relating to Plastics2 6.1.3 The inside of the oven shall be free of contamination
D 1600 Terminology for Abbreviated Terms Relating to or surface deposits. Stainless steel oven liners should be used
Plastics2 to reduce corrosion due to continued exposure to decomposi-
E 145 Specification for Gravity-Convection and Forced- tion gases.
Ventilation Ovens3 6.2 Sample Container—A weighing vessel of low shape
2.2 ISO Standard: design in glass, aluminum, or stainless steel of sufficient size to
ISO 1269–1980 Homopolymer and Copolymer Resins of hold a 10-g resin sample. An aluminum weighing dish, 57 mm
Vinyl Chloride—Determination of Volatile Matter Includ- in diameter and 18 mm in depth, is suitable.
ing Water4 6.3 Balance—A weighing balance with a precision to within
3. Terminology 0.001 g.
3.1 Definitions: Definitions are in accordance with Defini- 7. Preparation of Apparatus
tions D 883 and Terminology D 1600, unless otherwise indi- 7.1 Maintain the oven at the temperature of the test for at
cated. least 1 h prior to insertion of the specimens.
4. Summary of Test Method 7.2 Prior to test operation, verify the uniformity of tempera-
ture within the oven according to Specification E 145. The
4.1 This test method consists of heating at 110°C a known
airflow in the oven should be greater than 0.3 m3 /min (10 ft3
quantity of powdered resin to constant mass. The calculated
/min).
1
NOTE 2—The temperature uniformity can also be verified by placing 5
This test method is under the jurisdiction of ASTM Committee D-20 on Plastics or more portions of the same resin sample in the oven, distributed over the
and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials
test area, following Section 8. Calculate the percent of volatile loss
(Section D20.15.08).
Current edition approved April 15, 1995. Published June 1995. Originally (Section 9). If the differences in the volatile loss of the samples exceed the
published as D 3030 – 72. Last previous edition D 3030 – 84 (1990)e1. test reproducibility, the temperature in the oven is not uniform and must
This edition includes the addition of an ISO equivalency statement (Note 1). be corrected before proceeding with the test.
2
Annual Book of ASTM Standards, Vol 08.01.
3
Annual Book of ASTM Standards, Vol 14.02. 8. Procedure
4
Available from American National Standards Institute, 11 W. 42nd St., 13th
Floor, New York, NY 10036.
8.1 Dry the weighing vessel in the oven at 110 6 1°C for 30

Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.

1
 D 3030
min and cool to room temperature in a desiccator. Tare the 10.1.1 The arithmetic average of the determinations to the
weighing vessel to the nearest 0.001 g. nearest 0.01 mass %.
8.2 Spread approximately 10 g of sample resin evenly over
the bottom of the weighing vessel and weigh to the nearest 11. Precision and Bias 5

0.001 g. Record the sample mass.

8.3 Place the resin-filled weighing dish in the oven con- 11.1 The following should be used for judging the accept-
trolled at 110 6 1°C and close the oven. ability of results (95 % confidence limits):
8.4 After 1 h, remove the weighing dish, cool to room 11.2 Reproducibility—The average of two determinations
temperature in a desiccator, and weigh to the nearest 0.001 g. reported by one laboratory should be considered suspect if it
Return the weighing dish to the oven and heat for an additional differs from that of another laboratory by more than 22 %
15 min, cool to room temperature in the desiccator, and relative.
re-weigh. Constant mass is reached when the successive 11.3 Repeatability—The average of two determinations ob-
weighing differs by 0.001 g or less; if the mass variation is tained on two separate days at the same laboratory on the same
greater than 0.001, continue the 15 min heating-weighing cycle sample should be considered suspect if it differs by more than
until constant mass is obtained. 4.4 % relative.
NOTE 3—Prompt weighing after removal of the dish from desiccator 11.4 Bias—No justifiable statement of bias can be made for
will improve accuracy. this test method, since the true value of the property cannot be
8.5 Test a minimum of two samples, and average the results. established by an accepted referee method.
9. Calculation NOTE 4—Other techniques of volatile determinations may be substi-
9.1 For each determination calculate the mass percent of tuted at the option of the purchaser and seller, such as the use of a
semi-automatic moisture tester or a procedure employing an infrared lamp
volatile matter present as follows:
as a heating source. With such methods, the temperature of the heated
@~M 2 M8!/M# 3 100 sample must be maintained at 1106 1°C.

where: 12. Keywords

M and M8 5 respectively, the mass before and after heating
of the resin determined at room temperature (a 12.1 moisture content; test method; vinyl chloride resins;
temperature in the range from 20 to 30°C (68 volatile matter
to 85°F), as defined in Methods D 618).

10. Report 5
Round-robin data for this test method may be obtained from ASTM Headquar-
10.1 Report the following information: ters. Request RR: D-20-1025.

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