ASTM D3421-75

Recommended Practice for Extraction and Determination of Plasticizer Mixtures from Vinyl Chloride Plastics (Withdrawn 1987)

General Information

• Status: Withdrawn
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

Standards Content (Sample)

q~l~ Designation: D 3421 - 75
Standard Recommended' Practice for
EXTRACTION' AND DETERMINATION OF PLASTICIZER.
o • • •
MIXTURES FROM VINYL CHLORIDE PLASTICSl
This Standard is issueil"under.the fixed designation D 3421: the number immediatel);" followiilg the designation indicates
the year of original adoption or. in the case or revision. the year of last revision. ~'number in parentheses indicates the
year of last 'reapproval. "
1. Scope these .may be .used with paper thimbles",or
5
with gIass shells. TheWiley-Richards'on'ap­
1.1 This recommended pr~ctice covers
paratus (Method D 494) {s useful and gives
the isolation and determination of the mono­
.shortened extraction times due to.full iinmer­
meric and polymeric constituents, of plasti­
,sion of the saJIlple holder in solvent vapors;
cizer D)i~tun~s used in, pply(vinyl chloride)
this type of apparatus must be'modifi~,~, to
compositions; it pr9vides' means for the analy­
eliminate contact between solvent vapors and
sis of compositions containing dioctyl phthal­
metal parts. All-glass extractors having an
ate with one or more homogeneous polyester
outer jacket permitting solvent vapors ,to sur-
plasticizers, and may be e~tended to analysis
6
round the barrel are available. '
of plasticizer mixtures containing simple
phthalate esters other than diQctyl phthalate.
s. Reagents
NOTE I-The values stated in SI units are to be
5.1 Carbqn ,Tetrachloride, ACS, reagent
regarded as the standard.
grade.
2. Appiicable Documents
5.2 Chloroform. ACS, reagent grade.
2. I ASTM Standards: NOTE 2: Caution-Both carbon tetrachloride
and chloroform are highly toxic ,and should be
D494Test for Acetone Extraction of Phe­
. han:dled.withe~tfeme "care, preferably within an
2
nolic Molded or Laminated Products •
efficient hood; inhalation of vapors is to be
E 260 Recommended Practice for General avoided." .".;' .,
Gas Chromatography P;ocedu~es3
5.3 M~thanol, ACS,reagent grade .
• , .' •••• " I'
3. SigItificance
6. Sample Preparation
3;1 Separation and identification of the
6.1 Grind'the sample in a Wiley polymer
components used in thermoplastics com­
mill to ZQ-mesh particle size. If a Wiley mill is
pounds is, often required in efforts to relate
unavailable, 5 by 5-mm squares cut from
performance properties to constitution, and
sheeting of 0.6 to 2-mm thickness give'satis­
in the design of fabrication control, proce-
factory results.
dures.,: ' :; ,
, 3.2 The" method obviates ,difficulties
I This recommended practice is' under the jurisdiction
caused by incomplete reprecipitation of high
of ASTM Committee 0-20 on Plastics. and is the direct
polymeric material from compositions com­ responsibility of Subcommittee D20.70 on Analytical
Methods. ,. , " , ' .
pletely dissolved in solvents such as tetrahy­
.Current editiori approved June 30. 191.5. Published Au-
drofuran. gust 1975. .'
. •Annual Book ofASTM Standards. Part 35.
, aAnnual Book ofASTM Standards. ,Part 42.
4. Apparatus,
• For example. Scientific Glass Apparatus Co. Catalog
No. JR-5700A. Sargent S-31247A.
4.1 For small samples (approximately (g),
5 Sargent 5-31709. 31710.
4
seniimicro Soxhlet extractors are adequate; • Scientific Glass Apparatus Catalog No. JM-5120.

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03421
6.2 When sufficient material is available, ate-Into a 100-011 volumetric flask contain­
the preferred sample weight is approximately ing approximately 50 ml ofchloroform, weigh
5 g. 1.5 g of dioctyl phthalate of known purity and
1.5 g of dibutyl phthalate of known purity.
7. Procedure
(Make all weighings to the nearest 0.0001 g.)
7.1 Place 1to 5 g of the prepared sample in Dilute to volume with chloroform and mix
a preweighed (to ± 0.0001 g) paper thimble or, thorol;lghly. Obtain a chromatogram of this
glass/ceramic extractor cup, and weigh the' " ~olution using the pafameters ~yen in 7.5.1.
assembly to ± O.OOOlg. Place the assembly'in
Calibration factor for dioctyl phthalate .
'" ·=(A) (B) (C)/(D) (E) (G)
the extractor barreL' ;"'., .',
7.2 Attach a condeD'~er to the' ext~~tor '
where:
barrel~d extract the sampl~16 h with a 2+1
A = weight of dioctylphthalate, g,
(by volume) 'mixture of carbon tetrachloride
B = purity of the dioctyl phthalate"
and methanol.
C = area under the dibutyl phthalate peak,
7.3 Cool the extract and filter through a
D = weight of dibutyl phthalate, g,
'fluted paper'into a tared flask, rinsing the
E = purity of dibutyl phthalate, and'
paper with small portions of the solvent mix-
G = area under dioctyl phthalate' peak.
" ,
ture. '
9. Calculation
7.4 Evaporate the solvent to constant re­
sidual weight on a steam bath; weigh the
9.1 Calculate the percent total plasticizing
residue to the nearest 0.0001 g.
additives, TPA;' as follows:
7.5 Determine the dioctyl phthalate con­
TPA, % = [RfS(A -: C)] x 100
tent by gas chromatography (see Recom­
where:
mended Practice E 260).
R weight of residue,
7.5.1 A general description of conditions
S = weight of sample,
appropriate for determi
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