ASTM D2195-00
(Test Method)Standard Test Methods for Pentaerythritol
Standard Test Methods for Pentaerythritol
SCOPE
1.1 These test methods cover the testing of pentaerythritol for use in the manufacture of alkyd resins and other synthetic resins.
1.2 The test procedures appear in the following sections: Section Sulfate ash 5 to 10 Moisture 11 to 16 Hydroxyl 17 to 22 Assay (by dibenzal) 23 to 29 Assay (by gas chromatography) 30 to 41 Phthalate ester color 42 to 49
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 34.
1.4 For hazard information and guidance, see the supplier's Material Safety Data Sheet.
General Information
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Standards Content (Sample)
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Designation:D2195–00
Standard Test Methods for
Pentaerythritol
This standard is issued under the fixed designation D 2195; 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 * E 180 Practice for Determining the Precision Data of
ASTM Methods for Analysis and Testing of Industrial
1.1 These test methods cover the testing of pentaerythritol
Chemicals
for use in the manufacture of alkyd resins and other synthetic
E 200 Practice for Preparation, Standardization, and Stor-
resins.
age of Standard Solutions for Chemical Analysis
1.2 The test procedures appear in the following sections:
E 203 TestMethodforWaterUsingVolumetricKarlFischer
Section
Titration
Sulfate ash 5 to 10
E 222 Test Methods for Hydroxyl Groups by Acetic Anhy-
Moisture 11 to 16
dride Acetylation
Hydroxyl 17 to 22
E 260 Practice for Packed Column Gas Chromatography
Assay (by dibenzal) 23 to 29
Assay (by gas chromatography) 30 to 41
Phthalate ester color 42 to 49
3. Significance and Use
1.3 This standard does not purport to address all of the 3.1 These test methods provide a measurement of sulfate,
safety concerns, if any, associated with its use. It is the
ash, moisture (water), hydroxyl content, assay by dibenzal and
responsibility of the user of this standard to establish appro- gas chromatography, and phthalate ester color of pentaerythri-
priate safety and health practices and determine the applica-
tol. The results of these measurements can be used for
bility of regulatory limitations prior to use. For specific hazard specification acceptance.
statements, see Section 34.
4. Purity of Reagents
1.4 For hazard information and guidance, see the supplier’s
Material Safety Data Sheet. 4.1 Reagent grade chemicals shall be used in all tests.
Unless otherwise indicated, it is intended that all reagents shall
2. Referenced Documents
conform to the specifications of the Committee on Analytical
2.1 ASTM Standards: Reagents of the American Chemical Society, where such
2 10
D 1193 Specification for Reagent Water specifications are available. Other grades may be used,
D 1209 Test Method for Color of Clear Liquids (Platinum- provided it is first ascertained that the reagent is of sufficiently
Cobalt Scale) high purity to permit its use without lessening the accuracy of
D 1615 Test Methods for Glycerol, Ethylene Glycol, and the determination.
Pentaerythritol in Alkyd Resins 4.2 Unless otherwise indicated, references to water shall be
D 1728 Test Method for Phthalate Ester Color of High- understood to mean Type IV of reagent water conforming to
Gravity Glycerin Specification D 1193.
D 2593 Test Method for Butadiene Purity and Hydrocarbon
6 SULFATE ASH
Impurities by Gas Chromatography
E 1 Specification for ASTM Thermometers
5. Summary of Test Method
5.1 Theorganicmatterisburnedoff,theresiduetreatedwith
sulfuric acid, ignited, and the ash weighed.
ThesetestmethodsareunderthejurisdictionofASTMCommitteeD-1onPaint
and Related Coatings, Materials, and Applications and are the direct responsibility
of Subcommittee D01.35 on Solvents, Plasticizers, and Chemicals Intermediates.
Current edition approved Jan. 10, 2000. Published March 2000. Originally Annual Book of ASTM Standards, Vol 15.05.
published as D 2195 – 63 T. Last previous edition D 2195 – 95. Annual Book of ASTM Standards, Vol 14.02.
2 10
Annual Book of ASTM Standards, Vol 11.01. Reagent Chemicals, American Chemical Society Specifications, American
Annual Book of ASTM Standards, Vol 06.04. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Annual Book of ASTM Standards, Vol 06.03. listed by the American Chemical Society, see Analar Standards for Laboratory
Discontinued, see 1991 Annual Book of ASTM Standards, Vol 06.03. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Annual Book of ASTM Standards, Vol 05.01. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Annual Book of ASTM Standards, Vol 14.03. MD.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D2195
6. Apparatus 12. Preparation of Sample
6.1 Crucible or Dish—Asilica, quartz, or platinum crucible 12.1 Grind a 25-g portion of the sample in a mortar and
or dish having a capacity of 50 to 60 mL. pestle, to pass a 40-mesh sieve, and use portions for the
6.2 Bunsen Burner. subsequent tests.
6.3 Electric Muffle Furnace, maintained at 600 6 25°C.
13. Apparatus
7. Reagents and Materials 13.1 Weighing Dish, aluminum, 70 by 30 mm, with cover.
13.2 Oven, gravity convection, maintained at 105 6 2°C.
7.1 Sulfuric Acid (1 + 1)—Carefully mix 1 volume of con-
centrated sulfuric acid (H SO , sp gr 1.84) with 1 volume of
2 4
14. Procedure
water.
14.1 Dry the aluminum dish at 105° C. Cool in a dessicator
and store until ready for use.
8. Procedure
14.2 Weigh, to 0.1 mg, a 5-g portion of the ground sample
8.1 Preignite the crucible or dish at 600°C, transfer to a
into a tared-aluminum dish, and place in the 105 6 2°C oven
desiccator, and when cool, weigh to 0.1 mg. Place approxi-
for 3 h. Remove, cover, cool in a desiccator, and weigh.
mately 20 g of the sample in the crucible or dish and weigh to
0.1 mg. Heat gently with a gas flame and ignite the specimen, 15. Calculation
allowing it to burn completely. Cool somewhat, and then
15.1 Calculate the percent of moisture content, M,as
moisten the residue with 10 to 20 drops of H SO (1 + 1).
2 4
follows:
Cautiously ignite until the carbon is completely consumed.
M 5 @~A 2 B!/W# 3 100 (2)
Finally, ignite in the muffle furnace at 600°C (dark red heat) to
constant weight, cool, and weigh to 0.1 mg.
where:
A 5 weight of dish + specimen before heating, g,
9. Calculation
B 5 weight of dish + specimen after heating, g, and
W 5 sample used, g.
9.1 Calculate the percent of sulfate ash, A, to three decimal
15.2 Duplicate determinations that agree within 0.15 % are
places as follows:
acceptable for averaging.
A 5 ~R/S! 3 100 (1)
16. Precision and Bias
where:
16.1 Precision—The following criteria should be used for
R 5 residue, g, and
S 5 sample used, g. judging the acceptability of results at the 95 % confidence
9.2 Duplicate determinations that agree within 0.005 % are level:
16.1.1 Repeatability—Two results, each the mean of dupli-
acceptable for averaging.
cate determinations, obtained by the same analyst should be
consideredsuspectiftheydifferbymorethan0.20 %,absolute.
10. Precision and Bias
16.1.2 Reproducibility—Two results, each the mean of du-
10.1 Precision—The following criteria should be used for
plicate determinations, obtained by analysts in different labo-
judging the acceptability of results at the 95 % confidence
ratories should be considered suspect if they differ by more
level:
than 0.30 % absolute.
10.1.1 Repeatability—Two results, each the mean of dupli-
cate determinations, obtained by the same analyst should be
NOTE 2—The above precision estimates are based on an interlaboratory
study involving seven laboratories using three samples with one analyst
considered suspect if they differ by more than 0.008 %,
performing duplicate runs on each of two days. The mean level of the
absolute.
moisture content of the samples studied was 0.3 %.
10.1.2 Reproducibility—Two results, each the mean of du-
plicate determinations, obtained by analysts in different labo- 16.2 Bias—Bias cannot be determined because there is no
ratories should be considered suspect if they differ by more available material having an accepted reference value.
than 0.008 %, absolute.
HYDROXYL CONTENT
NOTE 1—The above precision estimates are based on an interlaboratory
study involving seven laboratories using three samples with one analyst
17. Summary of Test Method
performing duplicate runs on each of two days. The average level of the
17.1 The hydroxyl content is determined in accordance with
ash content of the samples studied was 0.01%.
Test Methods E 222.
10.2 Bias—Bias cannot be determined because there is no
available material having an accepted reference value. 18. Apparatus
18.1 Flasks, Erlenmeyer, 300-mLwith standard-taper 24/40
MOISTURE
joint.
18.2 Condenser, 400-mm, standard-taper 24/40 joint with
11. Summary of Test Method
cooling extending into the joint, drip tip.
11.1 The loss in weight on heating at 105°C for3his 18.3 Hot Plates, with variable resistance for temperature
determined. control.
D2195
18.4 Buret, calibrated, 100-mL, with a 50 or 75-mL reser- 21. Calculation
voir on top of a lower portion calibrated in 0.1-mLdivisions.A
21.1 Calculate the percent of hydroxyl content, H,as
TFE-fluorocarbon resin stopcock is suitable for this purpose.
follows:
19. Reagents and Materials H 5 @~B 2 V! N 3 17.01# / @S 3 1000# 3 100 (4)
19.1 Acetic Anhydride.
where:
19.2 Acetylation Reagents—Mix 105 mL of acetic anhy-
V 5 NaOH solution required for titration of the specimen,
dride with 1 L of pyridine (see 19.4). The reagent shall be
mL,
freshly prepared each day, and used and kept in a dark bottle.
B 5 NaOH solution required for titration of the reagent
It should not be used if darker than a pale yellow color.
blank, mL,
19.3 Phenolphthalein Indicator Solution (1 g/100 mL)—
N 5 normality of the NaOH solution used, and
Dissolve1gofphenolphthaleinin100mLofaqueouspyridine
S 5 specimen used, g.
solution (1 + 1).
21.2 Duplicate determinations that agree within 0.3 % are
19.4 Pyridine, containing 0.30 to 0.45 % water. Determine
acceptable for averaging.
the water content of the pyridine using Test Method E 203 and
add the required amount of water. Calculate the volume of
22. Precision and Bias
water to add in millilitres per litre of pyridine, V, as follows:
22.1 Precision—The following criteria should be used for
V 5 4.0 2 9A (3)
judging the acceptability of results at the 95 % confidence
level:
where A 5 water in pyridine, %.
22.1.1 Repeatability—Two results, each the mean of dupli-
19.5 Sodium Hydroxide, Standard Solution (0.5 N)—
cate determinations, obtained by the same analyst should be
Prepare and standardize in accordance with Practice E 200.
considered suspect if they differ by more than 0.8 %, absolute.
Apply temperature corrections to the volumes of titrant so that
22.1.2 Reproducibility—Two results, each the mean of du-
the normality is for concentration at 20°C.
plicate determinations, obtained by analysts in different labo-
20. Procedure
ratories should be considered suspect if they differ by more
20.1 Weigh a 0.30 to 0.33-g portion of the ground sample than 1.2 %, absolute.
into a small glass-stoppered weighing bottle. Dry for3hat
NOTE 5—The above precision estimates are based on an interlaboratory
105°C. Weigh accurately, transfer the portion to a 250-mL
study involving seven laboratories using three samples with one analyst
Erlenmeyer flask with ground joint, and reweigh the bottle to
performing duplicate runs on each of two days. The mean level of the
obtain the specimen weight by difference. hydroxyl value of the samples studied was 48%.
20.2 Pipet 25 mL of the acetylation reagent into the flask
22.2 Bias—Bias cannot be determined because there is no
using a uniform drainage time for all aliquots. Connect the
available material having an accepted reference value.
flask to the condenser (Note 3), sealing the joint with 1 or 2
drops of pyridine, and place on a hot plate; if necessary, swirl
ASSAY (BY DIBENZAL)
the flask to dissolve the specimen. Heat at reflux for 30 min,
regulating the heat so that the vapors condense in the con-
23. Scope and Application
denser.
23.1 This test method covers the determination of the
NOTE 3—If the surrounding atmosphere is humid, connect the con- monopentaerythritol content of pentaerythritol (PE) by the
denser to a drying trap containing a mixture of No. 2 mesh calcium
dibenzalmethod.Itisapplicabletomaterialcontaining75 %or
chloride and indicating anhydrous calcium sulfate.
more monopentaerythritol. Normal amounts of dipentaerythri-
tol do not interfere. Tripentaerythritol, etc, interferes due to its
20.3 Allow the flask to cool somewhat, then rinse the
condenser with 25 mL of water. Remove the condenser and insolubility in the reaction mixture. Refer to Test Methods
D 1615.
rinse the joint of the condenser and the flask with water,
collecting the rinsing in the flask.
24. Summary of Test Method
20.4 Cool the flask in an ice-water bath so that the contents
arebelow20°C,add0.5to1.0mLofphenolphthaleinindicator
24.1 A weighed specimen is dissolved in water, a methanol
solution,andtitrateslowlywiththe0.5 NNaOHsolutiontothe
solution of benzaldehyde is added, followed by hydrochloric
first permanent, faint pink end point. The solution must be
acid, and the mixture cooled to 0°C. The pentaerythritol-
swirled or magnetically stirred during the titration, and the
dibenzal precipitate is filtered, dried, and weighed.Asolubility
solution must be vigorously swirled as the end point is
correction factor is added to the weight of precipitate found.
approached. Read the volume of the titrant to 0.02 mL (Note
4). Record the temperature of the 0.5 N NaOH solution. 25. Apparatus
25.1 Crucibles, filtering, fritted-glass, medium-porosity.
NOTE 4—If the volume of 0.5 N NaOH solution required for the
specimen is less than 80 % of that required for the blank, the specimen 25.2 Stirring Rods, about 70 mm long, preferably having
was too large and the analysis must be repeated with a smaller specimen
one flat end.
weight.
25.3 Vacuum Pump or Water Aspirator— It is convenient to
20.5 Perform a blank determination in parallel by the same have at least two outlets, in order to make duplicate filtrations
procedure, omitting only the addition of the specimen. simultaneously.
D2195
26. Reagents and Materials
43.59 5 (mol weight PE / mol weight PE-
dibenzal) 3 100.
26.1 Benzaldehyde, N.F. grade, 98 % minimum purity. This
material is easily oxidized by air. If it is to be used over a long 28.2 Duplicate determinations that agree within 0.3 % are
acceptable for averaging.
period, transfer the contents of a 0.5-kg bottle to a number of
22-mL capacity screw-cap vials.
29. Precision and Bias
26.2 Benzaldehyde-Methanol Reagent— Add 20 mL of
benzaldehyde to 100 mL of methanol. Prepare fresh for each
29.1 Precision—The following criteria should be used for
series of determinations.
judging the acceptability of results at the 95 % confide
...
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