ASTM D1045-95

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
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Designation: D 1045 – 95 An American National Standard
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Methods for
Sampling and Testing Plasticizers Used in Plastics
This standard is issued under the fixed designation D 1045; 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 Liquids by Digital Density Meter
E 1 Specification for ASTM Thermometers
1.1 These test methods cover sampling and testing of liquid
E 203 Test Method for Water Using Karl Fischer Reagent
plasticizers used in compounding of plastics. Acid number,
ester content, specific gravity, color, refractive index, and water
3. Terminology
content are determined.
3.1 Definitions—Definitions are in accordance with Termi-
1.2 The values stated in SI units are to be regarded as the
nology D 883 and Terminology D 1600, unless otherwise
standard. The values given in parentheses are for information
indicated.
only.
1.3 This standard does not purport to address all of the
4. Significance and Use
safety concerns, if any, associated with its use. It is the
4.1 These test methods may be used in establishing and
responsibility of the user of this standard to establish appro-
confirming quality control standards for liquid plasticizers used
priate safety and health practices and determine the applica-
in the compounding of plastics.
bility of regulatory limitations prior to use. Specific hazards
information is given in Section 5.
5. Hazards
NOTE 1—There is no similar or equivalent ISO standard.
5.1 Chemical Hazard of Reagents—Some of the chemicals
used in this test method may be hazardous. Accepted labora-
2. Referenced Documents
tory safety procedures must be followed. See suppliers’ mate-
2.1 ASTM Standards:
rial safety data sheets for further information.
D 70 Test Method for Specific Gravity of Semi-Solid Bitu-
minous Materials 6. Sampling
D 287 Test Method for API Gravity of Crude Petroleum and
6.1 The method of sampling specified in 6.2 or 6.3 shall be
Petroleum Products (Hydrometer Method)
used, according to the special conditions that exist.
D 792 Test Methods for Specific Gravity (Relative Density)
6.2 From Loaded Tank Car or Other Large Vessel—The
and Density of Plastics by Displacement 1
composite sample taken shall be not less than 2 L ( ⁄2 gal) and
D 883 Terminology Relating to Plastics
should consist of small samples of not more than 1 L (1 qt)
D 1193 Specification for Reagent Water
each, taken from near the top and bottom by means of a metal
D 1600 Terminology for Abbreviated Terms Relating to
or glass container with removable stopper or top. This device,
Plastics
attached to a suitable pole, shall be lowered to the desired
D 1807 Test Methods for Refractive Index and Specific
depth, when the stopper or top shall be removed and the
Optical Dispersion of Electrical Insulating Liquids
container allowed to fill. A bomb sampler attached to a chain is
D 3465 Practice for Purity of Monomeric Plasticizers by
convenient to use; the opening should be adjusted so that the
Gas Chromatography
bomb will fill on the way down.
D 4052 Test Method for Density and Relative Density of
6.3 From Barrels and Drums—At least5%ofthe packages
in any shipment shall be represented in the sample. The
1 purchaser may increase the percentage of packages to be
These methods are under the jurisdiction of ASTM Committee D-20 on Plastics
sampled at his discretion; in the case of plasticizers that are
and are the direct responsibility of Subcommittee D20.15 on Thermoplastics
Materials (Section D20.15.11 on Plasticizers).
purchased in small quantity, each package may be sampled and
Current edition approved March 15, 1995. Published May 1995. Originally
analyzed, if desired. A portion shall be withdrawn from near
e1
published as D 1045 – 49 T. Last previous edition D 1045 – 86 (1990) .
the center of each package sampled by means of a “thief” or
This edition contains changes in Section 1 to include an ISO equivalency
statement. other sampling device and composited. The composite sample
Annual Book of ASTM Standards, Vol 04.03.
thus obtained shall be not less than 1 L (1 qt) and shall consist
Annual Book of ASTM Standards, Vol 05.01.
Annual Book of ASTM Standards, Vol 08.01.
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 05.03.
Annual Book of ASTM Standards, Vol 10.03.
Annual Book of ASTM Standards, Vol 14.03.
Annual Book of ASTM Standards, Vol 08.02.
Annual Book of ASTM Standards, Vol 15.05.
D 1045
of equal portions of not less than 250 mL ( ⁄2 pt) from each KOH per gram of sample, as follows:
package sampled.
Acid number 5 A 2 B!N3 56.1 /C (1)
@~ #
7. Purity of Reagents
where:
A 5 NaOH or KOH solution required for titration of the
7.1 Purity of Reagents—Reagent-grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that sample, mL,
B 5 NaOH or KOH solution required for titration of the
all reagents shall conform to the specifications of the Commit-
blank, mL,
tee on Analytical Reagents of the American Chemical Society,
N 5 normality of the NaOH or KOH solution, and
where such specifications are available. Other grades may be
C 5 sample used, g.
used, provided it is first ascertained that the reagent is of
11.2 If desired, in the case of esters, the results may be
sufficiently high purity to permit its use without lessening the
expressed as a percentage by weight of the appropriate acid, by
accuracy of the determination.
using the proper factor in the equation in 11.1.
7.2 Unless otherwise indicated, references to water shall be
understood to mean reagent water conforming to Specification
ESTER CONTENT—TITRIMETRIC
D 1193.
12. Reagents
ACID NUMBER
12.1 Bromthymol Blue Indicator Solution.
12.2 Hydrochloric Acid, Standard (0.5 N)Prepare and stan-
8. Thermometers
dardize a 0.5 N aqueous solution of hydrochloric acid (HCI).
8.1 All temperature measurements shall be made with
12.3 Potassium Hydroxide, Standard Solution (0.5 N)—
ASTM thermometers of suitable range, accurate to within
Prepare and standardize a 0.5 N alcoholic solution of potassium
0.1°C and conforming to the requirements prescribed in
hydroxide (KOH).
Specification E 1.
13. Procedure
9. Reagents
13.1 Weigh accurately about2gofthe sample into a
9.1 Alcohol—Denatured alcohol, Formula No. 3A of the U. 250-mL Erlenmeyer flask with ground-glass joint. By means of
a constant delivery pipet or buret, add 50 mL of 0.5 N KOH
S. Bureau of Alcohol, Tobacco, and Firearms.
9.2 Alkali, Standard Solution ( 0.01 N)—Prepare and stan- solution. Connect to a water-cooled condenser with ground-
glass joint and reflux for a period of 1 to 4 h, depending on the
dardize a 0.01 N aqueous solution of sodium hydroxide
(NaOH) or a 0.01 N alcoholic solution of potassium hydroxide ester being tested, or until saponification is complete.
13.2 After the apparatus has cooled, wash down the con-
(KOH).
9.3 Alkali, Standard Solution (0.1 N)—Prepare and stan- denser with water and disconnect. Add a few drops of
dardize a 0.1 N aqueous solution of sodium hydroxide (NaOH) bromthymol blue indicator solution to contents of the flask and
or a 0.1 N alcoholic solution of potassium hydroxide (KOH). titrate with 0.5 N HCl.
9.4 Acetone. 13.3 Blank—Run a blank, containing 50 mL of the 0.5 N
9.5 Bromthymol Blue Indicator Solution. KOH solution, along with the sample.
14. Calculation
10. Procedure
14.1 Calculate the ester content, expressed in milligrams of
10.1 Weigh 25 g of the sample into a 125-mL Erlenmeyer
KOH per gram of sample, as follows:
flask and dissolve in 50 mL of alcohol. If the sample is not
completely soluble in alcohol, use 50 m
...