ASTM F1884-98
(Test Method)Standard Test Method for Determining Residual Solvents in Packaging Materials
Standard Test Method for Determining Residual Solvents in Packaging Materials
SCOPE
1.1 This test method covers determination of the amount of residual solvents released from within a packaging material contained in a sealed vial under a given set of time and temperature conditions and is a recommended alternative for Test Method F 151.
1.2 This test method covers a procedure for quantitating volatile compounds whose identity has been established and which are retained in packaging materials.
1.3 The analyst should determine the sensitivity and reproducibility of the method by carrying out appropriate studies on the solvents of interest. The analyst is referred to Practice E260 for guidance.
1.4 For purposes of verifying the identity of or identifying unknown volatile compounds the analyst is encouraged to incorporate techniques such as gas chromatography/mass spectroscopy, gas chromatography/infrared spectroscopy or other suitable techniques in conjunction with this test method.
1.5 Sensitivity of this test method in the determination of the concentration of a given retained solvent must be determined on a case by case basis due to the variation in the substrate/solvent interaction between different types of samples.
1.6 This test method does not address the determination of total retained solvents in a packaging material. Techniques such as multiple headspace extraction can be employed to this end. The analyst is referred to the manual supplied with the GC-Autosampling system for guidance.
1.7 The values stated in SI units are to be regarded as the standard.
1.8 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.
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Designation: F 1884 – 98
Standard Test Method for
Determining Residual Solvents in Packaging Materials
This standard is issued under the fixed designation F 1884; 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 177 Practice for Use of the Terms Precision and Bias in
ASTM Test Methods
1.1 This test method covers determination of the amount of
E 260 Practice for Gas Chromatographic Procedures
residual solvents released from within a packaging material
E 691 Practice for Conducting an Interlaboratory Study to
contained in a sealed vial under a given set of time and
Determine the Precision of a Test Method
temperature conditions and is a recommended alternative for
F 151 Test Method for Residual Solvents in Flexible Barrier
Test Method F 151.
Materials
1.2 This test method covers a procedure for quantitating
volatile compounds whose identity has been established and
3. Terminology
which are retained in packaging materials.
3.1 Definitions:
1.3 The analyst should determine the sensitivity and repro-
2 2 6 2
3.1.1 ream—3000 ft = 278.7 m = 27.87310 cm .
ducibility of the method by carrying out appropriate studies on
3.1.2 retained solvents—those chemical species, which are
the solvents of interest. The analyst is referred to Practice
retained by packaging material and can be detected in the
E 260 for guidance.
headspace of sealed sample vials under conditions of elevated
1.4 For purposes of verifying the identity of or identifying
temperature.
unknown volatile compounds the analyst is encouraged to
incorporate techniques such as gas chromatography/mass spec-
4. Summary of Test Method
troscopy, gas chromatography/infrared spectroscopy or other
4.1 Retained volatile organic solvents are determined by
suitable techniques in conjunction with this test method.
subjecting the packaging material to elevated temperatures in a
1.5 Sensitivity of this test method in the determination of
headspace sampling system with subsequent gas chromatogra-
the concentration of a given retained solvent must be deter-
phy of the headspace and detection using a suitable detection
mined on a case by case basis due to the variation in the
device such as a flame ionization detector (FID).
substrate/solvent interaction between different types of
4.2 Volatile components can then be quantified by compari-
samples.
son with standards of known concentration.
1.6 This test method does not address the determination of
4.3 Qualitative analysis may be carried out on a gas chro-
total retained solvents in a packaging material. Techniques
matograph (GC) coupled to an appropriate detector capable of
such as multiple headspace extraction can be employed to this
compound detection / identification, such as a mass spectrom-
end. The analyst is referred to the manual supplied with the
eter or infrared detector.
GC-Autosampling system for guidance.
1.7 The values stated in SI units are to be regarded as the
5. Significance and Use
standard.
5.1 This test method is intended to measure volatile organic
1.8 This standard does not purport to address all of the
compounds that are emitted from packaging materials under
safety concerns, if any, associated with its use. It is the
high-temperature conditions.
responsibility of the user of this standard to establish appro-
5.2 This test method may be useful in assisting in the
priate safety and health practices and determine the applica-
development and manufacture of packaging materials having
bility of regulatory limitations prior to use.
minimal retained packaging ink/adhesive solvents.
5.3 Modification of this procedure by utilizing appropriate
2. Referenced Documents
qualitative GC detection devices such as a mass spectrometer
2.1 ASTM Standards:
in place of the flame ionization detector may provide identifi-
cation of volatile organics of unknown identity.
This test method is under the jurisdiction of ASTM Committee F-2 on Flexible
Barrier Materials and is the direct responsibility of Subcommittee F02.30 on Test
Methods. Annual Book of ASTM Standards, Vol 14.02.
Current edition approved May 10, 1998. Published March 1999. Annual Book of ASTM Standards, Vol 15.09.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
F1884–98
6. Interferences
Methanol 120 94.96
Ethanol 80 63.14
6.1 Gas Chromatography—Because of the potentially large
2-Propanol 60 47.13
number of chemical species that can be analyzed using this
n-Propanol 60 48.21
Methylethyl ketone 40 32.20
methodology, not all species will be resolved from one another
Ethylacetate 40 36.08
on a particular GC column under a given set of conditions.
2-Propylacetate 20 17.08
Techniques available to the analyst to verify the identity of Benzene 10 8.76
Methylisobutylketone 20 16.02
chemical species being quantitated include retention time
Toluene 10 8.70
comparisons using alternate GC conditions or using an alter-
Heptanone 20 16.42
nate GC column. Good judgment in the interpretation of
7.3 Vials,20mL. To ensure against extraneous peaks in the
chromatographic results is always important. Refer to Practice
gas chromatographic traces, wash vials thoroughly and dry in
E 260 for guidance.
a 125°C air oven for a minimum of 4 h before using.
6.2 Apparatus—Because this method is designed for detect-
7.4 Vial Crimp Caps.
ing trace quantities of organic compounds, contaminants can
7.5 Septa, Teflon/Silicone. To ensure that the septa are free
lead to misinterpretation of results. Preparing apparatus prop-
of volatiles, condition the septa in a vacuum oven at 130°C for
erly and carrying out blank determinations is essential to
16 h.
minimize this possibility.
7.6 Crimping Tool for Vials.
7.7 Syringe—2 mL gas tight with valve. Store syringe in
7. Apparatus and Reagents
90°C oven between uses.
7.1 Gas chromatograph equipped as follows:
7.8 4-Heptanone.
7.1.1 FID Detector, compatible with capillary columns.
7.9 For Manual Injection Only—Hot air oven and heat
7.1.2 Injector, split/split-less compatible with capillary col-
resistant gloves.
umns.
7.1.3 Column, DB-5, 30m, 0.25 mm ID, 1 μm film thick- 8. Instrument Setup
ness, Cat. No. 122–5033, or 0.32 mm, Cat. No. 123–5033. A
8.1 Set up the gas chromatographic system per the manu-
short piece of deactivated fused silica column may be placed
facturer’s recommendations and as follows:
between the injector and the column to serve as a guard
8.1.1 Injector Temperature—250°C.
column.
8.1.2 Detector Temperature—250°C.
7.1.4 Peak Area Integration System, compatible with GC
8.1.3 Column Temperature:
system in use. Alternately, a chart recorder and hand integra-
8.1.3.1 Initial 40°C for 4 min.
tion can be used.
8.1.3.2 Program—Adjust temperature program to give a
7.1.5 Auto sampler is recommended.
retention window of at least 15 min to ensure optimum
7.2 Standard Solutions, consisting of the organic solvent
separation of solvents.
mixture of interest, at concentrations that simulate the expected
8.1.4 Attenuation or sensitivity, or both, set to give a
retention levels. 4-Heptanone may be added to the solutions for
detector response of 40 % or more of full scale on the recorder
use as an internal standard as described in Practice E 260.
or integrator of the expected internal standard and standard
7.2.1 An example of a working standard is listed below. The
sample response. See Practice E 260 for guidance.
standard used will vary based on the solvents present in the
sample to be tested. The quantities shown in the table will
result in roughly equivalent size peaks due to differences in Cat. No. 6676601, available from Shamrock Glass Co., 220 N. Delaware Ave.,
Seaford, DE or Cat. No. 237-502 Chemical Research Supplies, PO Box 888,
detector response. If the solvents are mixed neat, adding 1 μL
Addison, IL 60101, or equivalent, have been found suitable for this purpose.
per gram of material in the headspace vial provides a good
Cat. No. 778704, available from Shamrock Glass Co., 220 N. Delaware Ave.,
starting point for calibration.
Seaford, DE or Cat. No. 07675-20625, available from Hewlett Packard Computer
Supplies Operation, PO Box 62124, San Francisco, CA 94162, or equivalent, have
7.2.2 If desired, water may be used as the diluent for the
been found suitable for this purpose.
standard. The solvents are diluted in 1 L of water, typically 2
Cat. No. 778183A, available from Shamrock Glass Co., 220 N. Delaware Ave.,
mL of the resulting solution is added per gram of sample in the
Seaford, DE or Cat. No. 5080-8726, available from Hewlett Packard Computer
headspace vial for calibration. 2 mL of 20 μl/L of 4-heptanone Supplies Operation, PO Box 62124, San Francisco, CA 94162, or equivalent, have
been found suitable for this purpose.
containing solution in water can be used as an internal
The sole source of supply of the apparatus known to the committee at this time
standard.
is Cat. No. 33280, Supelco Inc., Bellefonte, PA 16823. If you are aware of
alternative suppliers, please provide this information to ASTM Headquarters. Your
NOTE 1—Water will change the partition coefficient between the sample
comments will receive careful consideration at a meeting of the responsible
and retained solvents.
technical committee, which you may attend
Solvent μL/L μg/mL
The sole source of supply of the apparatus known to the committee at this time
is Cat. No. 050034, Alltech, 2051 Waukegan Rd., Deerfield, IL 60015. If you are
aware of alternative suppliers, please provide this information to ASTM Headquar-
ters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend.
4 10
The sole source of supply of the apparatus known to the committee at this time The sole source of supply of the apparatus known to the committee at this time
is J. and W. Scientific, Cat. No. 122-5033 and Cat. No. 123-5033. If you are aware is Cat. No. 10, 174-5, Aldrich, 940 W. St. Paul Ave., Milwaukee, WI 53233. If you
of alternative suppliers, please provide this information to ASTM Headquarters. aware of
...
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