ASTM D2124-99(2011)
(Test Method)Standard Test Method for Analysis of Components in Poly(Vinyl Chloride) Compounds Using an Infrared Spectrophotometric Technique (Withdrawn 2020)
Standard Test Method for Analysis of Components in Poly(Vinyl Chloride) Compounds Using an Infrared Spectrophotometric Technique (Withdrawn 2020)
SIGNIFICANCE AND USE
PVC compounds are used in a wide variety of products and hence they are formulated to provide a wide range of physical properties. The physical properties required in a compound depend upon the product in which it is used. These properties are largely determined by the type, quantity, and quality of the compounding ingredients. The analytical test method described below makes use of infrared spectrophotometry for the qualitative or quantitative determination, or both, of many of these ingredients in PVC compounds. This test method may be used for a variety of applications including process control, raw material acceptance, product evaluation, and determination of changes in composition resulting from environmental testing.
This test method is directly applicable only to those components listed in the appendix and to those components which are known to be similar in chemical composition and in solubility characteristics to the chemicals listed in the appendix.
SCOPE
1.1 This test method provides for the identification of certain resins, plasticizers, stabilizers, and fillers in poly(vinyl chloride) (PVC) compounds by an infrared spectrophotometric technique. In many cases, individual components may be measured quantitatively. Complementary procedures, such as chromatographic and other separations, will be necessary to separate specific components and extend the applications of this test method. Other instrumental test methods, such as optical emission or X-ray spectroscopic methods, may yield complementary information which may allow more complete or, in some cases, easier measurement of the components. The resin components covered in this test method are listed in the appendix.
1.2 PVC formulations are too varied to be covered adequately by a single test method. Using the following test method, many compounds may be separated into resins, plasticizers, stabilizers, and fillers. A number of components can be quantitatively measured. Many more can be identified and their concentrations estimated. By the use of prepared standards, one may determine the usefulness and accuracy of the test method for specific PVC formulations. This test method is applicable for the resin components listed in the appendix and for other components having similar chemical compositions and solubility characteristics. This test method can lead to error in cases where the nature of the components is not known.
1.3 The values stated in SI units are to be regarded as the standard. The values in brackets are given for information only.
1.4 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.
Note 1—There is no known ISO equivalent to this standard.
WITHDRAWN RATIONALE
This test method provides for the identification of certain resins, plasticizers, stabilizers, and fillers in poly(vinyl chloride) (PVC) compounds by an infrared spectrophotometric technique. In many cases, individual components may be measured quantitatively. Complementary procedures, such as chromatographic and other separations, will be necessary to separate specific components and extend the applications of this test method. Other instrumental test methods, such as optical emission or X-ray spectroscopic methods, may yield complementary information which may allow more complete or, in some cases, easier measurement of the components. The resin components covered in this test method are listed in the appendix.
Formerly under the jurisdiction of Committee D20 on Plastics, this test method was withdrawn in July 2020 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D2124 − 99 (Reapproved 2011)
Standard Test Method for
Analysis of Components in Poly(Vinyl Chloride) Compounds
Using an Infrared Spectrophotometric Technique
This standard is issued under the fixed designation D2124; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 This test method provides for the identification of 2.1 ASTM Standards:
certain resins, plasticizers, stabilizers, and fillers in poly(vinyl E131Terminology Relating to Molecular Spectroscopy
chloride)(PVC)compoundsbyaninfraredspectrophotometric E168Practices for General Techniques of Infrared Quanti-
technique. In many cases, individual components may be tative Analysis
measured quantitatively. Complementary procedures, such as E177Practice for Use of the Terms Precision and Bias in
chromatographic and other separations, will be necessary to ASTM Test Methods
separate specific components and extend the applications of E275PracticeforDescribingandMeasuringPerformanceof
this test method. Other instrumental test methods, such as Ultraviolet and Visible Spectrophotometers
optical emission or X-ray spectroscopic methods, may yield
3. Terminology
complementary information which may allow more complete
or, in some cases, easier measurement of the components. The
3.1 Definitions:
resin components covered in this test method are listed in the
3.1.1 For definitions related to the material on infrared
appendix.
spectroscopy, refer to Terminology E131.
1.2 PVC formulations are too varied to be covered ad-
4. Summary of Test Method
equately by a single test method. Using the following test
4.1 The PVC compound is solvent-extracted in order to
method, many compounds may be separated into resins,
plasticizers, stabilizers, and fillers. A number of components separate the plasticizer from the compound. The resin is
dissolved from the remaining compound and the inorganic
can be quantitatively measured. Many more can be identified
and their concentrations estimated. By the use of prepared fillers and stabilizers separated by centrifuging. By this
standards, one may determine the usefulness and accuracy of technique, the compound is separated into (1) plasticizers, (2)
the test method for specific PVC formulations. This test resin, and (3) inorganic stabilizers and fillers. Each may be
method is applicable for the resin components listed in the individually analyzed by an infrared technique to identify and
appendix and for other components having similar chemical measure the components.
compositions and solubility characteristics. This test method
5. Significance and Use
can lead to error in cases where the nature of the components
is not known.
5.1 PVC compounds are used in a wide variety of products
and hence they are formulated to provide a wide range of
1.3 The values stated in SI units are to be regarded as the
physical properties. The physical properties required in a
standard.Thevaluesinbracketsaregivenforinformationonly.
compound depend upon the product in which it is used. These
1.4 This standard does not purport to address all of the
properties are largely determined by the type, quantity, and
safety concerns, if any, associated with its use. It is the
quality of the compounding ingredients. The analytical test
responsibility of the user of this standard to establish appro-
methoddescribedbelowmakesuseofinfraredspectrophotom-
priate safety and health practices and determine the applica-
etryforthequalitativeorquantitativedetermination,orboth,of
bility of regulatory limitations prior to use.
many of these ingredients in PVC compounds. This test
NOTE 1—There is no known ISO equivalent to this standard.
method may be used for a variety of applications including
process control, raw material acceptance, product evaluation,
ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods
(Section D20.70.08). For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Feb. 1, 2011. Published March 2011. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1962. Last previous edition approved in 2004 as D2124-99(2004). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D2124-99R11. the ASTM website.
*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
D2124 − 99 (2011)
and determination of changes in composition resulting from sufficiently high purity to permit its use without lessening the
environmental testing. accuracy of the determination.
5.2 This test method is directly applicable only to those 7.2 Alumina, absorption.
components listed in the appendix and to those components
7.3 Carbon Disulfide (CS ).
which are known to be similar in chemical composition and in
7.4 Ether, anhydrous.
solubility characteristics to the chemicals listed in the appen-
dix.
7.5 Potassium Bromide, (KBr) infrared quality.
7.6 Tetrachloroethane, technical.
6. Apparatus
7.7 Tetrahydrofuran (stabilized with 0.1% hydroquinone).
6.1 Initial Sample Preparation—Use any of the following
apparatus,dependingonshapeandsizeofsample,forreducing
8. Component Separations
solid samples to small particle sizes:
8.1 Initial Sample Preparation—Any test method that will
6.1.1 Pencil Sharpenerorgraterandacoldboxorcontainer
increase the surface area of a sample sufficiently to permit
capable of maintaining at least the temperature of solid carbon
complete plasticizer extraction in a reasonable time is satisfac-
dioxide.
tory. PVC compounds as received are usually in the form of
6.1.2 Grinding Wheel, coarse.
powders, granules, slabs, or offshaped pieces. Powders may be
6.1.3 Microtome.
useddirectly.Thinsheets,0.02to0.05-mmthick,moldedfrom
6.1.4 Grinding or Cutting Mills,commercial,forexample,a
individualgranulesmaybeused.Granulesmaybepressedinto
Wiley mill (for samples larger than 1 g).
slabs. Slabs or appropriately shaped pieces may be treated by
6.2 Soxhlet Extraction Apparatus:
one of the following techniques:
6.2.1 For0.5and1.0-gsamples,useanextractionapparatus
8.1.1 Buffing on a coarse grinding wheel,
with a 150-mL flask and a 27 by 100-mm thimble.
8.1.2 Cooling the sample with solid carbon dioxide and
6.2.2 For 0.2-g samples, use an extraction apparatus with a
grinding the brittle sample in a clean pencil sharpener or on a
30-mL flask and a 10 by 50-mm thimble.
grater or clean file, or
6.3 Mold and Press for KBr Pellets—A mold assembly 8.1.3 Shavingthinslicesfromthesamplewithamicrotome.
capable of pelletizing a 12.7-mm ( ⁄2-in.) minimum diameter
8.2 Plasticizer Extraction—Weigh to 60.2 mg approxi-
pellet under vacuum and a press capable of exerting pressures
mately1goffine particle size sample into a 27 by 100-mm
ofatleast140MPa(20000psi)arerequiredtopressclearKBr
paper extraction thimble. Place the thimble in a jacketed
pellets.
Soxhlet apparatus fitted with a tared 150-mLflask, and extract
6.4 Infrared Spectrophotometer—The spectral region from with 120 mLof ethyl ether for6h(Note 2). Remove the tared
−1
4000 to 650 cm (2.5 to 15 µm) is used. Refer to Practice 150-mL flask, containing the ethyl ether and the extracted
E275,withparticularemphasisonSections5and14relatingto plasticizer,fromthejacketedSoxhletapparatusandgentlyheat
resolution and spectral slit width measurements. An ultimate to boil off the ethyl ether. Place the flask in an evacuated
3 −1 −1
resolving power (1) of at least 1.5 cm at 850 cm (0.02 µm desiccator for a minimum of1hto remove the last traces of
at 12 µm) is satisfactory. The suitability of the instrument ethyl ether. Weigh to 60.2 mg the flask containing the
should be proven in the user’s laboratory. Demountable cells, extracted plasticizers. Calculate the percentage of plasticizers
1.0-mmliquidcells,andaKBrpelletholderaretheaccessories in the PVC sample as follows:
used.
weightofextractedplasticizers 3100
plasticizers,% 5
weightofPVCsample
6.5 Infrared Spectrophotometer, Fourier Transform (FT-IR),
capable of attaining a 4 wave number resolution.
8.2.1 Keep the plasticizers for infrared identification or
determination (8.4).
7. Reagents
NOTE 2—Organometallic or organic stabilizer, if present, may partially
7.1 Purity of Reagents—Reagent grade chemicals shall be
or wholly separate from either the plasticizer or resin components and
used in all tests. Unless otherwise indicated, it is intended that
should be considered when examining these compounds.
all reagents shall conform to the specifications of the Commit-
8.3 Separation of Stabilizers and Fillers—Empty the resin,
tee onAnalytical Reagents of theAmerican Chemical Society,
stabilizers, and fillers remaining in the extraction thimble into
where such specifications are available. Other grades may be
a 50-mL beaker.Add 20 mL of tetrachloroethane and heat the
used, provided it is first ascertained that the reagent is of
sample gently until the resin has dissolved. Wash the contents
of the beaker quantitatively into a tared 50-mLcentrifuge tube
with 20 mL of tetrahydrofuran (which has been previously
Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof
passed through a 150 by 12.7-mm (6 by ⁄2-in.) diameter
this test method.
alumina absorption column to remove hydroquinone), swirl to
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
mix, and centrifuge for 30 min. Decant the resin solution and
listed by the American Chemical Society, see Analar Standards for Laboratory
reserveforinfraredanalysis.Washtheresidueremaininginthe
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
tared centrifuge tube with 20 mL of tetrahydrofuran and
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. centrifugeagainfor30min.Decantthesolutioncontainingthe
D2124 − 99 (2011)
−1
remainingresin.Repeattheoperation.Drythetaredcentrifuge µm) are useful. Dioctyl phthalate bands at 1725 cm (5.80
−1 −1
tube containing the stabilizer and filler in an oven at 110°C for µm), 1270 cm (7.87 µm), and 1121 cm (8.92 µm), and
−1
1 h, cool, weigh, and calculate the percentage of inorganic tricresylphosphatebandat1191cm (8.4µm)aresatisfactory.
stabilizer and filler as follows: The dioctyl phthalate band chosen will depend, in part, on
secondary plasticizer interferences. Choice of bands for other
inorganicstabilizerandfiller,%
plasticizersislefttothediscretionoftheuser.Attheanalytical
weightofstabilizerandfiller 3100
band frequency (wavelength) chosen, absorbances for the
weightofPVCsample
sample spectrum (A + A ) and the blank spectrum (A ) are
s b b
measured. Net absorbance due to sample component A is
8.3.1 Keep the stabilizer and filler for infrared analysis.
s
Usually carbon black and color pigments are included in this (A + A)− A .
s b b
9.3.3 Prepare plasticizer standards by dissolving the pure
portion.
plasticizers of interest in CS to give a series of standard
8.4 Resin—Calculate the percentage of resin by difference
solutions covering the 3.0 to 0.5-mg/mL range for each
(100 minus the total percent of plasticizers, stabilizers, and
plasticizer. Run these standard plasticizer solutions under
fillers).
conditions identical to those under which the samples are run
to obtain the net absorbances of the components at a series of
9. Infrared Analysis of Extracted Plasticizers
concentrations. Plot Beer’s law curves of net absorbances
9.1 The extracted plasticizers may be run on the infrared
versus concentrations in milligrams per millilitre for each
spectrophotometer as liquid films for identification or in CS
component. All quantitative manipulations shall be in accor-
solution for quantitative determinations.
dance with Practices E168.
9.3.4 Use the net absorbance of a specific plasticizer in
9.2 Identification of Plasticizers—MostplasticizersforPVC
conjunctionwiththeappropriateBeer’slawcurvetodetermine
compounds are liquid at room temperature. A few secondary
the concentration in milligrams per millilitre.
plasticizers may be solid but would be suspended or dissolved
9.3.5 Calculate the percentage of plasticizer in the PVC
inprimaryplasticizers.AdemountablecellwithNaClwindows
compound as follows:
and a 0.025-mm spacer usually suffices to give a strong
−1
plasticizer spectrum (1). Scan the spectrum from 4000 cm to specificplasticizer, % 5 ~AB/3W! 3100
−1
650 cm (2.5 to 15 µm). By reference to a collection of
where:
plasticizer spectra the plasticizers in the sample may be
A = concentration of plasticizer, mg/mL,
identified (2, 3, 4, 5, 6, 7, 8).With experience, rough estimates
B = total weight of extracted plasticizers, mg, and
of concentrations may be made to enable preparation of
W = weight of PVC sample, mg.
matching standards for quantitative analysis.
9.3 Quantitative Analysis of Plasticizers—The variety of 10. Direct Infrared Determination of Plasticizers
plasticizers and their possible combinations in PVC com-
10.1 The use of this procedure usually presupposes that a
pounds is extensive. It is impossible to specify a single
complete formulation analysis is not required and that the
procedure that determines quantitatively all plasticizers with
plasticizers to be determined are known.
equal precision and bias.The following procedure is useful for
10.2 Weigh 0.25 g (60.25 mg) of fine particle size sample
a number of plasticizers and their combinations, particularly if
into a 10 by 50-mm extraction thimble. Place the thimble in a
either dioctyl phthalate or tricresyl phosphate is the primary
microSoxhletextractionapparatus.Extractfor6hwith20mL
plasticizer. The user should decide whether the efficiency,
ofCS .TransfertheCS containingtheextractedplasticizersto
2 2
precision,andbiasoftheprocedureissatisfactoryforaspecific
a25-mLvolumetricflask,dilutetothemarkwithCS ,andmix
combination of plasticizers to be analyzed.
thoroughly. Run this solution on the infrared spectrophotom-
9.3.1 Weigh60 60.2mgofextractedplasticizer(from8.2)
eter. Instrumental conditions and techniques, preparation of
into a 25-mL Erlenmeyer flask equipped with a glass stopper;
standards, and Beer’s law curves are the same as those
add 20.00 mL of CS to dissolve the plasticizers. Take care to
specified in 9.2.
avoid loss of solvent by keep
...
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