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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 Plastics1
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 Meter8

1.1 These test methods cover sampling and testing of liquid E 1 Specification for ASTM Thermometers9
plasticizers used in compounding of plastics. Acid number, E 203 Test Method for Water Using Karl Fischer Reagent10
ester content, specific gravity, color, refractive index, and water
3. Terminology
content are determined.
1.2 The values stated in SI units are to be regarded as the 3.1 Definitions—Definitions are in accordance with Termi-
standard. The values given in parentheses are for information nology D 883 and Terminology D 1600, unless otherwise
only. indicated.
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
responsibility of the user of this standard to establish appro- 4.1 These test methods may be used in establishing and
priate safety and health practices and determine the applica- confirming quality control standards for liquid plasticizers used
bility of regulatory limitations prior to use. Specific hazards in the compounding of plastics.
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 Materials2 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)3 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 Displacement4 composite sample taken shall be not less than 2 L (1⁄2 gal) and
D 883 Terminology Relating to Plastics4 should consist of small samples of not more than 1 L (1 qt)
D 1193 Specification for Reagent Water5 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,
Plastics4 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 Liquids6 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 Chromatography7 bomb will fill on the way down.
D 4052 Test Method for Density and Relative Density of 6.3 From Barrels and Drums—At least 5 % of the packages
in any shipment shall be represented in the sample. The
1
These methods are under the jurisdiction of ASTM Committee D-20 on Plastics purchaser may increase the percentage of packages to be
and are the direct responsibility of Subcommittee D20.15 on Thermoplastics sampled at his discretion; in the case of plasticizers that are
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
published as D 1045 – 49 T. Last previous edition D 1045 – 86 (1990)e1.
analyzed, if desired. A portion shall be withdrawn from near
This edition contains changes in Section 1 to include an ISO equivalency the center of each package sampled by means of a “thief” or
statement. other sampling device and composited. The composite sample
2
Annual Book of ASTM Standards, Vol 04.03. thus obtained shall be not less than 1 L (1 qt) and shall consist
3
Annual Book of ASTM Standards, Vol 05.01.
4
Annual Book of ASTM Standards, Vol 08.01.
5
Annual Book of ASTM Standards, Vol 11.01. 8
6 Annual Book of ASTM Standards, Vol 05.03.
Annual Book of ASTM Standards, Vol 10.03. 9
7 Annual Book of ASTM Standards, Vol 14.03.
Annual Book of ASTM Standards, Vol 08.02. 10
Annual Book of ASTM Standards, Vol 15.05.

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 D 1045
of equal portions of not less than 250 mL (1⁄2 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:
7.1 Purity of Reagents—Reagent-grade chemicals shall be A 5 NaOH or KOH solution required for titration of the
used in all tests. Unless otherwise indicated, it is intended that sample, mL,
all reagents shall conform to the specifications of the Commit- B 5 NaOH or KOH solution required for titration of the
tee on Analytical Reagents of the American Chemical Society, blank, mL,
where such specifications are available.11 Other grades may be N 5 normality of the NaOH or KOH solution, and
used, provided it is first ascertained that the reagent is of C 5 sample used, g.
sufficiently high purity to permit its use without lessening the 11.2 If desired, in the case of esters, the results may be
accuracy of the determination. expressed as a percentage by weight of the appropriate acid, by
7.2 Unless otherwise indicated, references to water shall be using the proper factor in the equation in 11.1.
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 about 2 g of the 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
S. Bureau of Alcohol, Tobacco, and Firearms. a constant delivery pipet or buret, add 50 mL of 0.5 N KOH
9.2 Alkali, Standard Solution ( 0.01 N)—Prepare and stan- solution. Connect to a water-cooled condenser with ground-
dardize a 0.01 N aqueous solution of sodium hydroxide glass joint and reflux for a period of 1 to 4 h, depending on the
(NaOH) or a 0.01 N alcoholic solution of potassium hydroxide ester being tested, or until saponification is complete.
(KOH). 13.2 After the apparatus has cooled, wash down the con-
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.
10. Procedure 14. Calculation
10.1 Weigh 25 g of the sample into a 125-mL Erlenmeyer 14.1 Calculate the ester content, expressed in milligrams of
flask and dissolve in 50 mL of alcohol. If the sample is not KOH per gram of sample, as follows:
completely soluble in alcohol, use 50 mL of a mixture of equal Ester content 5 @~D 2 E!N 3 56.1#/G 2 F (2)
parts of alcohol and acetone. With certain samples it may be
necessary first to add 25 mL of acetone, warm to effect where:
solution, and then add 25 mL of alcohol. D 5 HCl required for titration of the blank, mL,
E 5 HCl required for titration of the sample, mL,
10.2 Add a few drops of bromthymol blue indicator solution
F 5 correction for acidity of sample (Section 11),
and titrate with 0.01 N NaOH or KOH solution. If the titration N 5 normality of the HCl, and
exceeds 10 mL, repeat the determination using 0.1 N NaOH or G 5 sample used, g.
KOH solution. 14.2 If desired, the results may be expressed as a percentage
10.3 Blank—Make a blank titration on 50 mL of the solvent of the appropriate ester by weight, by using the proper factor in
used to dissolve the sample. the equation in 14.1.
11. Calculation ESTER CONTENT—GAS CHROMATOGRAPHY
11.1 Calculate the acid number, expressed as milligrams of 15. Procedure
15.1 The ester content may be determined using Practice
11
Reagent Chemicals, American Chemical Society Specifications, American D 3465.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory SPECIFIC GRAVITY
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia 16. Selection of Test Method
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD. 16.1 Specific gravity may be determined using a hydrometer

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 D 1045
(Test Method D 287), Westphal balance, pycnometer (Section compare with the standards by holding side by side and looking
17) or Digital Density Meter (Test Method D 4052). Extremely down through the columns of liquid at a matte white surface
viscous samples may be tested by Test Methods D 792 or Test illuminated by northern daylight.
Method D 70.
22. Apparatus
17. Procedure Using Pycnometer 22.1 Refractometer—An Abbé refractometer with scale
17.1 Determine the weight capacity of the pycnometer with graduated directly in terms of refractive index of the D line of
water at 23 6 1°C. Fill this standardized pycnometer with a sodium at a temperature of 23°C.
portion of the sample that has been cooled to approximately 22.2 Water Supply—A water supply, the temperature of
20°C. Insert the thermometer or capillary tube, taking care to which may be varied.
avoid introduction of air bubbles. Set the pycnometer in a
constant-temperature water bath maintained at 23 6 1°C (73.4 REFRACTIVE INDEX
6 1.8°F) for a period of at least 30 min. Remove the droplet of 23. Procedure
sample from the overflow capillary and cover with the glass
cap. Clean the outside of the pycnometer and weigh. 23.1 The refractive index may be measured using the
appropriate routine or precision method from Test Method
18. Calculation D 1807 or the method given in Sections 22 and 24.
18.1 Calculate the specific gravity as follows:
24. Procedure
Specific gravity at 23/23°C 5 A/B (3)
24.1 Place the refractometer in front of a suitable source of
where: light (either daylight or electric light), insert the thermometer,
A 5 grams of sample used, and and adjust the circulation of water so as to bring the prisms to
B 5 water capacity of pycnometer in grams. the desired temperature (usually 23°C (73.4°F)). Clean with
alcohol and wipe dry. Spread a drop of the liquid to be tested
COLOR upon the lower prism and clamp the prisms together. Adjust the
19. Application mirror so that the light enters the telescope. Focus the eyepiece
on the cross-hairs and the reading lens of the scale. Upon
19.1 Useful comparisons between the color of relatively
moving the prism arm, a position can now be found where the
light colored plasticizers and platinum-cobalt standards may be
lower part of the field is dark and the upper part light. In
made for colors in the range from 0 to 200, as defined in
general, the borderline will be colored. Correct by turning the
Section 20.
milled head on the right of the telescope so that a sharp black
20. Preparation of Color Standards12 and white edge is obtained. Move the prism arm until this black
20.1 Dissolve 1.245 g of potassium chloroplatinate (K2 edge just crosses the intersection of the cross-hairs. Read the
PtCl6), containing 0.5 g of platinum, and 1 g of crystallized refractive index from the scale, estimating the fourth decimal
cobaltous chloride (CoCl2 ·6H2 O), containing about 0.248 g of place.
cobalt, in water containing 100 mL of HCl (sp gr 1.19). Dilute 24.2 The accuracy of the instrument may be checked by a
to 1 L with water to prepare a solution having a color of 500. small test plate of known refractive index, which is supplied
This solution, already prepared, may be purchased from with the refractometer. Attach this test plate to the upper prism
laboratory supply houses. with a liquid of high refractive index (usually monobro-
20.2 To prepare standards having colors of 5, 10, 15, etc., monaphthalene). Errors may be corrected by means of a small
dilute 0.5, 1.0, 1.5 mL, etc., of the solution described in 20.1 adjusting screw.
with water to 50 mL in standard Nessler tubes. If 100-mL WATER CONTENT
standard Nessler tubes are used, dilute 1.0, 2.0, 3.0 mL, etc., to
100 mL with water to obtain colors of 5, 10, 15, etc. Protect the 25. Procedure
tubes from evaporation and from dust when not in use. If 25.1 The water content may be measured using Test Method
desired, commercially available platinum-cobalt standards in E 203.
Nessler tubes or colored glass disks with proper spectral
transmission may be used, provided they are first checked 26. Precision and Bias
against standards prepared from K2 PtCl6 and CoCl2 ·6H2 O as 26.1 Precision and bias statements are an integral part of
described above. referenced test procedures used in this test method. These
21. Procedure statements are to be considered applicable to test results
obtained by use of this test method.
21.1 Fill a 50 or 100-mL Nessler tube with the sample and 26.2 Attempts to develop precision and bias statements for
Acid Number, Ester Content-Titrimetric, Specific Gravity-
12
The preparation of these platinum-cobalt color standards was originally Pycnometer, Color, and Refractive Index by the procedure in
described by Hazen, A., American Chemical Journal, Vol 14, 1892, 300. The Section 22 have not been successful. For this reason, data on
description given in these methods is substantially identical with that given in the
Standard Methods for the Examination of Water and Sewage. Am. Public Health
precision and bias cannot be given. Anyone wishing to partici-
Assn., Ninth Edition, p. 14. A description of these standards is also given by Scott, pate in the development of precision and bias data should
W. W., Standard Methods of Chemical Analyses. Fifth Edition, Vol 2, p. 2048. contact the ASTM headquarters.

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 D 1045
27. Keywords
27.1 plasticizer; plasticizer acid number; plasticizer color;
plasticizer ester content; plasticizer refractive index; sampling;
test methods

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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views known to the ASTM Committee on Standards, 100 Barr Harbor Drive, West Conshohocken, PA 19428.

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