ASTM F1884-04(2023)

Standard Test Methods for Determining Residual Solvents in Packaging Materials

SIGNIFICANCE AND USE
5.1 This test method is intended to measure volatile organic compounds that are emitted from packaging materials under high-temperature conditions.  
5.2 This test method may be useful in assisting in the development and manufacture of packaging materials having minimal retained packaging ink/adhesive solvents.  
5.3 Modification of this procedure by utilizing appropriate qualitative GC detection devices such as a mass spectrometer in place of the flame ionization detector may provide identification of volatile organics of unknown identity.
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 F151.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 31-Mar-2023
• ICS: 55.040 - Packaging materials and accessories
• Technical Committee: F02 - Primary Barrier Packaging
• Drafting Committee: F02.15 - Chemical/Safety Properties

Relations

• Refers: ASTM E260-96(2019) - Standard Practice for Packed Column Gas Chromatography
• Effective Date: 01-Sep-2019
• Refers: ASTM E177-14 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2014
• Refers: ASTM E177-13 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2013
• Refers: ASTM E691-13 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-May-2013
• Refers: ASTM E691-11 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2011
• Refers: ASTM E260-96(2011) - Standard Practice for Packed Column Gas Chromatography
• Effective Date: 01-Nov-2011
• Refers: ASTM E177-10 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2010
• Refers: ASTM E691-08 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Oct-2008
• Refers: ASTM E177-08 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Oct-2008
• Refers: ASTM E177-06b - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 15-Nov-2006
• Refers: ASTM E177-06a - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2006
• Refers: ASTM E260-96(2006) - Standard Practice for Packed Column Gas Chromatography
• Effective Date: 01-Mar-2006
• Refers: ASTM E691-05 - Standard Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• Effective Date: 01-Nov-2005
• Refers: ASTM E177-04 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004
• Refers: ASTM E177-04e1 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-Nov-2004

Overview

ASTM F1884-04(2023) - Standard Test Methods for Determining Residual Solvents in Packaging Materials provides procedures for quantifying volatile organic compounds (VOCs) retained in packaging materials. The standard is issued by ASTM International and is intended as a reliable method for measuring solvents that can be emitted from packaging, particularly under elevated temperatures. It focuses on improving packaging safety by helping manufacturers control residual solvent levels in inks, adhesives, and other components, ensuring compliance with industry regulations and consumer safety expectations.

Residual solvents can impact the overall performance and safety of packaging materials, especially those used in food, pharmaceutical, and consumer goods industries. By applying the ASTM F1884-04(2023) standard, organizations can detect, quantify, and identify retained solvents, promoting best practices in packaging material development and manufacturing.

Key Topics

• Measurement of Residual Solvents: The standard outlines methods to determine the amount of volatile organic compounds released when packaging is exposed to high temperatures.
• Quantitative and Qualitative Analysis: Procedures are provided for both identifying and quantifying known volatile compounds retained in packaging. Gas chromatography is the principal analytical technique, with optional enhancements such as mass spectrometry or infrared spectroscopy for compound identification.
• Method Sensitivity & Reproducibility: Users are advised to validate sensitivity and reproducibility for each type of solvent and substrate, referencing ASTM Practice E260 for guidance.
• Sample Handling & Preparation: The document stresses the importance of representative sampling, proper vial cleaning, and blank determinations to minimize contamination or solvent loss.
• Calibration and Calculation: Establishing calibration curves and using internal standards are recommended for quantitation. Results are typically reported as milligrams of solvent per ream of packaging material.
• Safety Considerations: The standard requires that users establish appropriate safety, health, and environmental practices due to the handling of hazardous solvents.

Applications

ASTM F1884-04(2023) is applicable to a range of packaging sectors where controlling residual solvent content is vital, including:

• Food Packaging: Ensuring that retained solvents in inks, adhesives, or coatings do not migrate into food products, maintaining food safety and regulatory compliance.
• Pharmaceutical Packaging: Verifying low levels of residual solvents helps safeguard sensitive pharmaceutical products and comply with stringent industry standards.
• Flexible Packaging Manufacturing: Facilitates conformance to client specifications and supports process optimization by monitoring solvent retention.
• Quality Control Laboratories: Provides reproducible methods for routine monitoring of VOC content in raw materials and finished packaging.
• Packaging Development: Assists R&D and engineering teams in selecting and qualifying new materials with minimal solvent retention for improved product safety and environmental impact.

The methods can be adapted for both known and unknown volatile organics, allowing for use in investigative situations such as the identification of off-odors or unexpected VOCs.

Related Standards

Implementing ASTM F1884-04(2023) often involves reference to additional standards, including:

• ASTM E260 - Practice for Packed Column Gas Chromatography
• ASTM E177 - Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• ASTM E691 - Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
• ASTM F151 - Test Method for Residual Solvents in Flexible Barrier Materials (now withdrawn, but provided as a comparison in F1884)
• ISO and Regulatory Guidance: The methods complement international guidelines regarding volatile organic compounds and packaging safety.

Summary

ASTM F1884-04(2023) is an essential standard for the quantitative and qualitative determination of residual solvents in packaging materials. Its correct application improves packaging quality, safety, and regulatory compliance, benefiting producers, quality assurance teams, and end users in industries where low residual solvent levels are critical. Incorporation of modern analytical techniques ensures adaptability with evolving industry requirements.

Keywords: ASTM F1884, residual solvents, packaging materials, headspace analysis, retained solvent, volatile organic compounds, gas chromatography, packaging safety, VOC detection.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: F1884 − 04 (Reapproved 2023)
Standard Test Methods for
Determining Residual Solvents in Packaging Materials
This standard is issued under the fixed designation F1884; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 1.9 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This test method covers determination of the amount of
ization established in the Decision on Principles for the
residual solvents released from within a packaging material
Development of International Standards, Guides and Recom-
contained in a sealed vial under a given set of time and
mendations issued by the World Trade Organization Technical
temperature conditions and is a recommended alternative for
Barriers to Trade (TBT) Committee.
Test Method F151.
1.2 This test method covers a procedure for quantitating
2. Referenced Documents
volatile compounds whose identity has been established and
2.1 ASTM Standards:
which are retained in packaging materials.
E177 Practice for Use of the Terms Precision and Bias in
1.3 The analyst should determine the sensitivity and repro-
ASTM Test Methods
ducibility of the method by carrying out appropriate studies on
E260 Practice for Packed Column Gas Chromatography
the solvents of interest. The analyst is referred to Practice E260
E691 Practice for Conducting an Interlaboratory Study to
for guidance.
Determine the Precision of a Test Method
1.4 For purposes of verifying the identity of or identifying F151 Test Method for Residual Solvents in Flexible Barrier
Materials (Withdrawn 2004)
unknown volatile compounds the analyst is encouraged to
incorporate techniques such as gas chromatography/mass
spectroscopy, gas chromatography/infrared spectroscopy or 3. Terminology
other suitable techniques in conjunction with this test method.
3.1 Definitions:
2 2 6 2
1.5 Sensitivity of this test method in the determination of 3.1.1 ream, n—3000 ft = 278.7 m = 27.87×10 cm .
the concentration of a given retained solvent must be deter-
3.1.2 retained solvents, n—those chemical species, which
mined on a case by case basis due to the variation in the
are retained by packaging material and can be detected in the
substrate/solvent interaction between different types of
headspace of sealed sample vials under conditions of elevated
samples.
temperature.
1.6 This test method does not address the determination of
total retained solvents in a packaging material. Techniques 4. Summary of Test Method
such as multiple headspace extraction can be employed to this
4.1 Retained volatile organic solvents are determined by
end. The analyst is referred to the manual supplied with the
subjecting the packaging material to elevated temperatures in a
GC-Autosampling system for guidance.
headspace sampling system with subsequent gas chromatogra-
1.7 The values stated in SI units are to be regarded as the phy of the headspace and detection using a suitable detection
device such as a flame ionization detector (FID).
standard.
1.8 This standard does not purport to address all of the
4.2 Volatile components can then be quantified by compari-
safety concerns, if any, associated with its use. It is the son with standards of known concentration.
responsibility of the user of this standard to establish appro-
4.3 Qualitative analysis may be carried out on a gas chro-
priate safety, health, and environmental practices and deter-
matograph (GC) coupled to an appropriate detector capable of
mine the applicability of regulatory limitations prior to use.
1 2
This test method is under the jurisdiction of ASTM Committee F02 on Primary For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Barrier Packaging and is the direct responsibility of Subcommittee F02.15 on contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Chemical/Safety Properties. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved April 1, 2023. Published April 2023. Originally the ASTM website.
approved in 1998. Last previous edition approved in 2018 as F1884 – 04 (2018). The last approved version of this historical standard is referenced on
DOI: 10.1520/F1884-04R23. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1884 − 04 (2023)
compound detection / identification, such as a mass spectrom- 7.2.1 An example of a working standard is listed below. The
eter or infrared detector. standard used will vary based on the solvents present in the
sample to be tested. The quantities shown in the table will
5. Significance and Use
result in roughly equivalent size peaks due to differences in
detector response. If the solvents are mixed neat, adding 1 μL
5.1 This test method is intended to measure volatile organic
compounds that are emitted from packaging materials under per gram of material in the headspace vial provides a good
starting point for calibration.
high-temperature conditions.
7.2.2 If desired, water may be used as the diluent for the
5.2 This test method may be useful in assisting in the
standard. The solvents are diluted in 1 L of water, typically
development and manufacture of packaging materials having
2 mL of the resulting solution is added per gram of sample in
minimal retained packaging ink/adhesive solvents.
the headspace vial for calibration. 2 mL of 20 μl ⁄L of
5.3 Modification of this procedure by utilizing appropriate
4-heptanone containing solution in water can be used as an
qualitative GC detection devices such as a mass spectrometer
internal standard.
in place of the flame ionization detector may provide identifi-
NOTE 1—Water will change the partition coefficient between the sample
cation of volatile organics of unknown identity.
and retained solvents.
Solvent μL/L μg/mL
6. Interferences
6.1 Gas Chromatography—Because of the potentially large
Methanol 120 94.96
Ethanol 80 63.14
number of chemical species that can be analyzed using this
2-Propanol 60 47.13
methodology, not all species will be resolved from one another
n-Propanol 60 48.21
on a particular GC column under a given set of conditions. Methylethyl ketone 40 32.20
Ethylacetate 40 36.08
Techniques available to the analyst to verify the identity of
2-Propylacetate 20 17.08
chemical species being quantitated include retention time
Benzene 10 8.76
comparisons using alternate GC conditions or using an alter- Methylisobutylketone 20 16.02
Toluene 10 8.70
nate GC column. Good judgment in the interpretation of
Heptanone 20 16.42
chromatographic results is always important. Refer to Practice
7.3 Vials, 20 mL. To ensure against extraneous peaks in the
E260 for guidance.
gas chromatographic traces, wash vials thoroughly and dry in
6.2 Apparatus—Because this method is designed for detect-
a 125 °C air oven for a minimum of 4 h before using.
ing trace quantities of organic compounds, contaminants can
7.4 Vial Crimp Caps.
lead to misinterpretation of results. Preparing apparatus prop-
erly and carrying out blank determinations is essential to 7.5 Septa, Teflon/Silicone. To ensure that the septa are free
minimize this possibility. of volatiles, condition the septa in a vacuum oven at 130 °C for
16 h.
TEST METHOD A
4,5
7.6 Crimping Tool for Vials.
4,6
7. Apparatus and Reagents
7.7 Syringe—2 mL gas tight with valve. Store syringe in
90 °C oven between uses.
7.1 Gas chromatograph equipped as follows:
4,7
7.1.1 FID Detector, compatible with capillary columns.
7.8 4-Heptanone.
7.1.2 Injector, split/split-less compatible with capillary col-
7.9 For Manual Injection Only—Hot air oven and heat
umns.
resistant gloves.
7.1.3 Column, DB-5, 30m, 0.25 mm ID, 1 μm film
thickness, Cat. No. 122–5033, or 0.32 mm, Cat. No.
4 8. Instrument Setup
123–5033. A short piece of deactivated fused silica column
8.1 Set up the gas chromatographic system per the manu-
may be placed between the injector and the column to serve as
facturer’s recommendations and as follows:
a guard column.
8.1.1 Injector Temperature—250 °C.
7.1.4 Peak Area Integration System, compatible with GC
system in use. Alternately, a chart recorder and hand integra- 8.1.2 Detector Temperature—250 °C.
8.1.3 Column Temperature:
tion can be used.
7.1.5 Auto sampler is recommended. 8.1.3.1 Initial 40 °C for 4 min.
8.1.3.2 Program—Adjust temperature program to give a
7.2 Standard Solutions, consisting of the organic solvent
retention window of at least 15 min to ensure optimum
mixture of interest, at concentrations that simulate the expected
separation of solvents.
retention levels. 4-Heptanone may be added to the solutions for
use as an internal standard as described in Practice E260.
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 Cat. No. 33280, Supelco Inc., Bellefonte, PA 16823.
is J. and W. Scientific, Cat. No. 122-5033 and Cat. No. 123-5033. If you are aware The sole source of supply of the apparatus known to the committee at this time
of alternative suppliers, please provide this information to ASTM Headquarters. is Cat. No. 050034, Alltech, 2051 Waukegan Rd., Deerfield, IL 60015.
Your comments will receive careful consideration at a meeting of the responsible The sole source of supply of the apparatus known to the committee at this time
technical committee, which you may attend. is Cat. No. 10, 174-5, Aldrich, 940 W. St. Paul Ave., Milwaukee, WI 53233.
F1884 − 04 (2023)
8.1.4 Attenuation or sensitivity, or both, set to give a 10.2 Samples should be taken and handled in such a way as
detector response of 40 % or more of full scale on the recorder to minimize loss of solvent from the sample between the time
or integrator of the expected internal standard and standard the sample is taken, cut and loaded into the sample vial. Taking
sample response. See Practice E260 for guidance. samples at press side, cutting and loading into vials immedi-
ately is the preferred method. Alternately, full web samples can
8.2 Set up autosampler, if used, to heat vials for 20 min at
be collected at press side and placed in a sealed container
90 °C before autoinjection.
(samples can also be wrapped tightly in foil) for transport to the
lab for cutting and loading into vials.
9. Calibration Procedure
10.3 When taking samples from roll stock, discard the first
9.1 Standard Curve:
8 to 10 layers before taking samples from the next 30 to 40
9.1.1 Prepare blanks by heating a sample of the packaging
layers to ensure that the samples are representative of the entire
material of interest (enough sample can be prepared at one time
roll.
for several analysis runs) in a vacuum oven at 90 °C for 24 h.
Remove the blanks and store in a closed container. Blanks
10.4 When possible, samples should have 100 % ink cov-
should be cut to the same relative size as the sample prior to
erage in the area selected for testing. Selecting an area with
heating in the vacuum oven.
100 % ink coverage will ensure that the testing will elucidate a
9.1.2 To prepare a calibration standard place a blank (cut to
worst case. Using a sample area with representative ink
appropriate size) in the 20 mL headspace vial and add the
coverage may also be considered.
appropriate amount of standard solvent mix to the vial.
10.5 The sample size is dictated by the thickness of the
Immediately cap and crimp the vial with the Teflon side of the
sample and the ease of filling the vial. The sample size will
septum toward the vial. It is suggested that blanks be fortified
2 2
vary from 5 in. to 50 in. Typically, the vial will be less than
at five different concentrations along with an unfortified blank
20 % full by volume. Alternately the ratio of the weight of the
be prepared for calibration. See Practice E260 for guidance.
sample in grams to the volume of the vial in millilitres should
9.2 Manual Injection:
not exceed 1 to 10. In the case of a 20 mL sample vial, the
9.2.1 If using a syringe and hot air oven, heat each vial for
weight of the sample should not exceed 2 g.
20 min at 90 °C. Ensure that the syringe is heated to at least
10.6 The preferred method of cutting samples is the use of
90 °C before taking headspace samples from the vials for
a punch press or die.
injection into the chromatograph.
10.7 Add the appropriate amount of internal standard (if
NOTE 2—When handling the hot syringe be sure that hands are
used) to the vial.
adequately protected. Fill the gas tight syringe with 1 mL of air, close
valve and insert the needle through the septum into the preheated vial.
1 10.8 Immediately cap and crimp the vial with the Teflon
Open valve, inject the air into vial. Draw ⁄2 mL of gas from vial into
side of the septa toward the vial.
syringe, inject back into vial. Repeat 2 times. Draw exactly 1 mL of gas
into syringe and close valve. Insert needle into injector of GC and inject.
NOTE 3—Consistent technique from injection to injection of standards
11. Procedure
and sample is required. This step should take no more than 30 s.
11.1 Manual Injection:
9.3 Automated Injection—The recommended method of in-
11.1.1 For those using the syringe, place the sample (vial) in
jecting the headspace gas into the GC is use of an automated
a forced air oven at 90 °C for 20 min.
headspace sampling system where the vials are heated to 90 °C
for 20 min and then the headspace of each vial is automatically
NOTE 6—Longer heating times may be used if it is deemed necessary to
injected onto the GC column.
ensure that the solvent in the headspace of the vial has totally equilibrated
with the sample.
9.4 Repeat the procedure for all five calibration standards
NOTE 7—When handling the hot syringe be sure that hands are
and the blank.
adequately protected. Fill the preheated gas-tight syringe with 1 mL of air,
close valve and insert the needle through the septum into the above
9.5 Construct a standard calibration curve from the data
conditioned vial. Open valve, inject the air into vial. Draw ⁄2 mL of gas
obtained using standard techniques as defined in Practice E260.
from vial into syringe, inject back into vial. Repeat 2 times. Draw exactly
1 mL of gas into syringe and close valve. Insert needle into injector of GC
NOTE 4—Longer heating times may be used if it is deemed necessary to
and inject.
ensure that the solvent in the headspace of the vial has totally equilibrated
with the sample. NOTE 8—Consistent technique from injection to injection of standards
and sample is required. This step should take no more than 30 s.
10. Sampling
11.2 Automated Injection:
10.1 Samples should be taken in such a manner as to 11.2.1 The recommended method of injecting the headspace
represent the entire web. The analyst should cut several layers
gas into the GC is use of an automated headspace sampling
deep into a roll of packaging material, discarding the outer system where the vials are heated to 90 °C for 20 min and then
layers, to ensure the sampling is representative of the entire
the headspace of the vial is automatically injected onto the GC
roll. Samples should be taken from the left, center and right column.
side of the web.
NOTE 9—Longer heating times may be used if it is deemed necessary to
NOTE 5—Consideration should also be given when sampling rolls ensure that the solvent in the headspace of the vial has totally equilibrated
within a production lot to ensure uniformity within the production run. with the sample.
F1884 − 04 (2023)
11.3 Chromatograph the sample under the same conditions of three sub-samples taken from a given packaging material to
used for establishment of the standard curve. represent the right, center and left side of the printed film roll.
Laboratories were instructed to analyze each sub-sample in
11.4 Run a blank and one calibration standard along with
triplicate. Five laboratories reported data.
each sample set to ensure system integrity.
14.2 Each sample contained seven analytes, however be-
11.5 Sample sets should contain a minimum of three repli-
cause of the differences in testing equipment only four of the
cates per sample.
analytes were reported by all five labs. The bulk samples were
12. Calculation
prepared by one laboratory and placed in sealed aluminum foil
pouches to minimize loss of solvents. The individual test
12.1 Calculate the amounts of retained solvents as follows:
specimens were prepared at the laboratory conducting the
12.1.1 Measure the area of the analyte peak and compare to
testing. Data reported consists of the average of three indi-
the area with that from the standard curve and determine the
vidual determinations on each sub-sample.
concentration of the analyte in mg/ream of retained solvent.
Normalize the analyte peak area with that of the internal
TEST METHOD B
standard peak area if the internal standard method is used
before calculating the retained solvent concentration.
15. Apparatus
NOTE 10—The above methodologies are described in Practice E260.
15.1 Container, rigid, capable of being sealed vacuum-tight.
12.2 Add each of the analyte concentrations together to The volume of this container s
...