ASTM D8142-23

Standard Test Method for Determining Chemical Emissions from Spray Polyurethane Foam (SPF) Insulation using Micro-Scale Environmental Test Chambers

SIGNIFICANCE AND USE
6.1 SPF insulation is applied and formed onsite, which creates unique challenges for measuring product emissions. This test method provides a way to measure post-application chemical emissions from SPF insulation.  
6.2 This test method can be used to identify compounds that emit from SPF insulation products, and the emission factors may be used to compare emissions at the specified sampling times and test conditions.  
6.3 Emission data may be used in product development, manufacturing quality control and comparison of field samples.  
6.4 This test method is used to determine chemical emissions from freshly applied SPF insulation samples. The utility of this test method for investigation of odors in building scale environments has not been demonstrated at this time.
SCOPE
1.1 This test method is used to identify and to measure the emissions of volatile organic compounds (VOCs) emitted from samples of cured spray polyurethane foam (SPF) insulation using micro-scale environmental test chambers combined with specific air sampling and analytical methods for VOCs.  
1.2 Specimens prepared from product samples are maintained at specified conditions of temperature, humidity, airflow rate, and elapsed time in micro-scale chambers that are described in Practice D7706. Air samples are collected periodically at the chamber exhaust at the flow rate of the micro-scale chambers.  
1.2.1 Samples for formaldehyde and other low-molecular weight carbonyl compounds are collected on treated silica gel cartridges and are analyzed by high performance liquid chromatography (HPLC) as described in Test Method D5197 and ISO 16000-3.  
1.2.2 Samples for other VOCs are collected on multi-sorbent samplers and are analyzed by thermal-desorption gas chromatography / mass spectrometry (TD-GC/MS) as described in U.S. EPA Compendium Method TO-17 and ISO 16000-6.  
1.3 This test method is intended specifically for SPF insulation products. Compatible product types include two component, high pressure and two-component, low pressure formulations of open-cell and closed-cell SPF insulation.  
1.4 VOCs that can be sampled and analyzed by this test method generally include organic blowing agents such as 1,1,1,3,3-pentafluoropropane, formaldehyde and other carbonyl compounds, residual solvents, and some amine catalysts. Emissions of some organic flame retardants can be measured after 24 h with this method, such as tris (chloroisopropyl) phosphate (TCPP).  
1.5 This test method does not cover the sampling and analysis of methylene diphenyl diisocyanate (MDI) or other isocyanates.  
1.6 Area-specific and mass-specific emission rates are quantified at the elapsed times and chamber conditions as specified in 13.2 and 13.3 of this test method.  
1.7 This test method is used to identify emitted compounds and to estimate their emission factors at specific times. The emission factors are based on specified conditions, therefore, use of the data to predict emissions in other environments may not be appropriate and is beyond the scope of this test method. The results may not be representative of other test conditions or comparable with other test methods.  
1.8 This test method is primarily intended for freshly applied, SPF insulation samples that are sprayed and packaged as described in Practice D7859. The measurement of emissions during spray application and within the first hour following application is outside of the scope of this test method.  
1.9 This test method can also be used to measure the emissions from SPF insulation samples that are collected from building sites where the insulation has already been applied. Potential uses of such measurements include investigations of odor complaints after product application. However, the specific details of odor investigations and other indoor air quality (IAQ) investigations are outside of the scope of this test method.  
1.10 The values stated in SI units are to be regarde...

General Information

• Status: Published
• Publication Date: 31-Aug-2023
• ICS: 13.040.01 - Air quality in general
• Technical Committee: D22 - Air Quality
• Drafting Committee: D22.05 - Indoor Air

Relations

• Replaces: ASTM D8142-17e1 - Standard Test Method for Determining Chemical Emissions from Spray Polyurethane Foam (SPF) Insulation using Micro-Scale Environmental Test Chambers
• Effective Date: 01-Sep-2023
• Refers: ASTM D7706-17(2023) - Standard Practice for Rapid Screening of VOC Emissions from Products Using Micro-Scale Chambers
• Effective Date: 01-Sep-2023
• Refers: ASTM D7706-17 - Standard Practice for Rapid Screening of VOC Emissions from Products Using Micro-Scale Chambers
• Effective Date: 01-May-2017
• Referred By: ASTM D8141-22 - Standard Guide for Selecting Volatile Organic Compounds (VOCs) and Semi-Volatile Organic Compounds (SVOCs) Emission Testing Methods to Determine Emission Parameters for Modeling of Indoor Environments
• Effective Date: 01-Sep-2023
• Referred By: ASTM D7859-19 - Standard Practice for Spraying, Sampling, Packaging, and Test Specimen Preparation of Spray Polyurethane Foam (SPF) Insulation for Testing of Emissions Using Environmental Chambers
• Effective Date: 01-Sep-2023
• Referred By: ASTM D8345-21 - Standard Test Method for Determination of an Emission Parameter for Phthalate Esters and Other Non-Phthalate Plasticizers from Planar Polyvinyl Chloride Indoor Materials for Use in Mass Transfer Modeling Calculations
• Effective Date: 01-Sep-2023
• Referred By: ASTM D8445-22a - Standard Practice for Measuring Chemical Emissions from Spray Polyurethane Foam (SPF) Insulation Samples in a Large-scale Ventilated Enclosure
• Effective Date: 01-Sep-2023

Overview

ASTM D8142-23 is an internationally recognized standard test method developed by ASTM for determining chemical emissions from spray polyurethane foam (SPF) insulation using micro-scale environmental test chambers. This method specifically targets the identification and quantification of volatile organic compounds (VOCs) released from cured SPF insulation. By maintaining precise environmental conditions within micro-scale chambers, the method provides reliable emission data essential for product development, quality control, and comparative analysis of both laboratory-prepared and field-collected samples.

Key Topics

• Chemical Emission Measurement: The standard details the procedures for measuring post-application chemical emissions, primarily VOCs, from SPF insulation.
• Use of Micro-Scale Environmental Test Chambers: Specimens are conditioned at controlled temperature, humidity, and airflow rates in chambers following ASTM Practice D7706 guidelines.
• Sampling and Analytical Techniques:
  • Formaldehyde and carbonyl compounds are sampled with silica gel cartridges and analyzed using HPLC, following ASTM D5197 and ISO 16000-3.
  • Other VOCs are sampled on multi-sorbent tubes and analyzed via thermal desorption GC/MS, guided by EPA Method TO-17 and ISO 16000-6.
• SPF Products Covered: Two-component, high-pressure and low-pressure open-cell and closed-cell formulations are within scope.
• Limitations: The method is not intended for methylene diphenyl diisocyanate (MDI) or other isocyanates and does not cover emissions during spray application or within the first hour post-application. Predicting emissions outside the tested conditions is not within the standard's scope.

Applications

ASTM D8142-23 serves several critical roles for professionals in the building materials, indoor air quality, and SPF manufacturing sectors:

• Product Development: Facilitates the identification of chemical compounds emitted from different SPF insulation formulations, assisting manufacturers in optimizing product formulations for reduced emissions.
• Quality Control: Enables ongoing monitoring and comparison of emissions from production samples, ensuring consistency with regulatory or internal standards.
• Field Sample Assessment: Useful for analyzing emissions from in-situ SPF insulation samples collected from completed buildings, such as in investigations following odor complaints. However, the standard does not detail specific procedures for broader indoor air quality assessments or odor investigations.
• Regulatory Compliance: Provides third-party verification capabilities for meeting specification requirements related to indoor environmental quality.
• Comparative Studies: Allows measurement of emission factors for comparison among products or over different curing times and test environments, supporting transparent product labeling and declarations.

Related Standards

• ASTM D1356: Terminology Relating to Sampling and Analysis of Atmospheres.
• ASTM D5116: Guide for Small-Scale Environmental Chamber Determinations of Organic Emissions from Indoor Materials/Products.
• ASTM D5197: Determination of Formaldehyde and Other Carbonyl Compounds in Air (Active Sampler Methodology).
• ASTM D6196: Choosing Sorbents, Sampling Parameters, and Thermal Desorption Analytical Conditions for Monitoring Volatile Organic Chemicals.
• ASTM D7706: Rapid Screening of VOC Emissions from Products Using Micro-Scale Chambers.
• ASTM D7859: Spraying, Sampling, Packaging, and Test Specimen Preparation of SPF Insulation for Emissions Testing.
• ISO 16000-3/6: International standards for determination of formaldehyde and VOCs in indoor and test chamber air.
• U.S. EPA Method TO-17: Determination of VOCs in ambient air via active sampling and thermal desorption.

Practical Value

Complying with ASTM D8142-23 gives organizations a science-based, standardized method to assess the environmental impact of spray polyurethane foam insulation. This supports healthier indoor environments by enabling the identification and reduction of harmful VOC emissions from building products. The test method is relied upon by manufacturers, researchers, and regulators for trustworthy emission assessments, improving the transparency and safety of modern insulation products.

Keywords: ASTM D8142-23, chemical emissions, spray polyurethane foam insulation, SPF, volatile organic compounds, VOCs, micro-scale environmental test chambers, indoor air quality, product testing, building materials, emission factors, quality control.

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: D8142 − 23
Standard Test Method for
Determining Chemical Emissions from Spray Polyurethane
Foam (SPF) Insulation using Micro-Scale Environmental
Test Chambers
This standard is issued under the fixed designation D8142; 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 1.5 This test method does not cover the sampling and
analysis of methylene diphenyl diisocyanate (MDI) or other
1.1 This test method is used to identify and to measure the
isocyanates.
emissions of volatile organic compounds (VOCs) emitted from
1.6 Area-specific and mass-specific emission rates are quan-
samples of cured spray polyurethane foam (SPF) insulation
tified at the elapsed times and chamber conditions as specified
using micro-scale environmental test chambers combined with
in 13.2 and 13.3 of this test method.
specific air sampling and analytical methods for VOCs.
1.7 This test method is used to identify emitted compounds
1.2 Specimens prepared from product samples are main-
and to estimate their emission factors at specific times. The
tained at specified conditions of temperature, humidity, airflow
emission factors are based on specified conditions, therefore,
rate, and elapsed time in micro-scale chambers that are
use of the data to predict emissions in other environments may
described in Practice D7706. Air samples are collected peri-
not be appropriate and is beyond the scope of this test method.
odically at the chamber exhaust at the flow rate of the
The results may not be representative of other test conditions or
micro-scale chambers.
comparable with other test methods.
1.2.1 Samples for formaldehyde and other low-molecular
1.8 This test method is primarily intended for freshly
weight carbonyl compounds are collected on treated silica gel
applied, SPF insulation samples that are sprayed and packaged
cartridges and are analyzed by high performance liquid chro-
as described in Practice D7859. The measurement of emissions
matography (HPLC) as described in Test Method D5197 and
during spray application and within the first hour following
ISO 16000-3.
application is outside of the scope of this test method.
1.2.2 Samples for other VOCs are collected on multi-
sorbent samplers and are analyzed by thermal-desorption gas 1.9 This test method can also be used to measure the
emissions from SPF insulation samples that are collected from
chromatography / mass spectrometry (TD-GC/MS) as de-
scribed in U.S. EPA Compendium Method TO-17 and ISO building sites where the insulation has already been applied.
Potential uses of such measurements include investigations of
16000-6.
odor complaints after product application. However, the spe-
1.3 This test method is intended specifically for SPF insu-
cific details of odor investigations and other indoor air quality
lation products. Compatible product types include two
(IAQ) investigations are outside of the scope of this test
component, high pressure and two-component, low pressure
method.
formulations of open-cell and closed-cell SPF insulation.
1.10 The values stated in SI units are to be regarded as
1.4 VOCs that can be sampled and analyzed by this test
standard. No other units of measurement are included in this
method generally include organic blowing agents such as
standard.
1,1,1,3,3-pentafluoropropane, formaldehyde and other carbo-
1.11 This standard does not purport to address all of the
nyl compounds, residual solvents, and some amine catalysts.
safety concerns, if any, associated with its use. It is the
Emissions of some organic flame retardants can be measured
responsibility of the user of this standard to establish appro-
after 24 h with this method, such as tris (chloroisopropyl)
priate safety, health, and environmental practices and deter-
phosphate (TCPP).
mine the applicability of regulatory limitations prior to use.
1.12 This international standard was developed in accor-
dance with internationally recognized principles on standard-
This test method is under the jurisdiction of ASTM Committee D22 on Air
ization established in the Decision on Principles for the
Quality and is the direct responsibility of Subcommittee D22.05 on Indoor Air.
Development of International Standards, Guides and Recom-
Current edition approved Sept. 1, 2023. Published October 2023. Originally
ɛ1
mendations issued by the World Trade Organization Technical
approved in 2017. Last previous edition approved in 2017 as D8142 – 17 . DOI:
10.1520/D8142-23. Barriers to Trade (TBT) Committee.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D8142 − 23
2. Referenced Documents U.S. EPA Method 325B Volatile Organic Compounds from
2 Fugitive and Area Sources: Sampler Preparation and
2.1 ASTM Standards:
Analysis, Air Emission Measurement Center (EMC) (Sep-
D1356 Terminology Relating to Sampling and Analysis of
tember 29, 2015)
Atmospheres
D1622/D1622M Test Method for Apparent Density of Rigid
3. Terminology
Cellular Plastics
3.1 Definitions—For definitions and terms commonly used
D5116 Guide for Small-Scale Environmental Chamber De-
for sampling and analysis of atmospheres, refer to Terminology
terminations of Organic Emissions from Indoor Materials/
D1356. For definitions and terms commonly used when testing
Products
materials and products for VOC emissions, refer to Guide
D5197 Test Method for Determination of Formaldehyde and
D5116. For definition of micro-scale test chamber, refer to
Other Carbonyl Compounds in Air (Active Sampler Meth-
Practice D7706.
odology)
D5337 Practice for Setting and Verifying the Flow Rate of
3.2 Definitions of Terms Specific to This Standard:
Personal Sampling Pumps
3.2.1 area specific flow rate, n—the ratio of the airflow rate
D6196 Practice for Choosing Sorbents, Sampling Param-
into the chamber in m /h and the projected surface area of the
eters and Thermal Desorption Analytical Conditions for
test specimen exposed to air in m with units of m/h.
Monitoring Volatile Organic Chemicals in Air
3.2.2 closed-cell SPF insulation, n—SPF insulation that
D7706 Practice for Rapid Screening of VOC Emissions
contains cells or voids that are not interconnected.
from Products Using Micro-Scale Chambers
3.2.2.1 Discussion—Closed-cell SPF insulation typically
D7859 Practice for Spraying, Sampling, Packaging, and Test
3 3
has a density between 24 kg ⁄m to 32 kg ⁄m when fully cured.
Specimen Preparation of Spray Polyurethane Foam (SPF)
3.2.3 open-cell SPF insulation, n—SPF insulation that con-
Insulation for Testing of Emissions Using Environmental
tains cells or voids that are largely interconnected.
Chambers
3.2.3.1 Discussion—Open-cell SPF insulation typically has
2.2 ISO Standards:
3 3
a density between 6.4 kg ⁄m to 9.6 kg ⁄m when fully cured.
ISO 16000-3 Indoor Air—Part 3: Determination of Formal-
dehyde and Other Carbonyl Compounds in Indoor Air and
4. Principles
Test Chamber Air—Active Sampling Method
4.1 Micro-scale test chambers are used for measuring emis-
ISO 16000-6 Indoor Air—Part 6: Determination of Volatile
sions of VOCs including formaldehyde and other carbonyl
Organic Compounds in Indoor and Test Chamber Air by
compounds from materials and products.
Active Sampling on Tenax TA Sorbent, Thermal
Desorption, and Gas Chromatography Using MS or MS-
4.2 Wall adsorption effects of reactive compounds and
FID
SVOCs are minimized by reducing the exposed inner surface
of the chamber by fitting the SPF samples directly into the
2.3 Government Agency Methods:
40 CFR Appendix B to Part 136 Definition and Procedure micro-scale chamber with minimal headspace. Passivated
treatment of the interior surfaces also contributes to reduced
for the Determination of the Method Detection Limit-
Revision 1.11 sorption effects.
California Department of Public Health Standard Method for
4.3 Micro-scale chambers are used for measuring area-
the Testing and Evaluation of Volatile Organic Chemical
specific emissions from the surface of SPF insulation or
Emissions from Indoor Sources Using Environmental
mass-specific emissions from the mass of the sample.
Chambers, CDPH/EHLB/Standard Method V.1.2 (January
2017)
5. Summary of Test Method
U.S. EPA Compendium Method TO-17 Determination of
5.1 A micro-scale chamber is used to measure VOC emis-
Volatile Organic Compounds in Ambient Air Using Active
sions from SPF insulation samples. A representative test
Sampling Onto Sorbent Tubes, Compendium of Methods
specimen is prepared from the sample and is placed directly
for the Determination of Toxic Organic Compounds in
into a micro-scale chamber. Air samples are collected from the
Ambient Air, Second Edition (January 1999)
chamber exhaust at specified elapsed times.
5.2 Clean dry air is supplied to a micro-scale chamber and
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
passes over the exposed surface of the test specimen before
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
reaching the exhaust port. The airflow rate and the temperature
Standards volume information, refer to the standard’s Document Summary page on
within the micro-scale chamber are controlled. As the air
the ASTM website.
passes over the test specimen, emitted compounds are swept
Available from International Organization for Standardization (ISO), ISO
Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier,
away from the sample’s surface.
Geneva, Switzerland, http://www.iso.org.
5.3 The standard temperature for the test method is 35 °C 6
Available from U.S. Government Printing Office, Superintendent of
Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
1 °C. Emission rates of organic compounds from building
www.access.gpo.gov.
materials and sorption and desorption of organic compounds
Available from United States Environmental Protection Agency (EPA), William
from interior surfaces are sensitive to temperature. Operation
Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,
http://www.epa.gov. of the micro-scale chamber at the specified temperature (above
D8142 − 23
ambient) enhances the emission rates of some compounds and 7.1.3 The prepared SPF insulation specimen must fit into
may improve the quantitative recovery of some less volatile the chamber body such that the back surface and edges of the
compounds. specimen are not directly exposed to the stream of air. An
example micro-scale chamber to measure emissions of SPF
5.4 The area-specific flow rate specified for this test method
insulation is shown in Fig. X1.1.
is 0.95 m ⁄h 6 0.05 m ⁄h. The maximum airflow rate for the
micro-scale chamber shall not exceed 150 mL/min, and the
7.2 Construction:
airflow rate shall not exceed the maximum flow rate for the
7.2.1 The micro-scale chamber body and associated lid shall
sampling media.
be constructed of polished stainless steel with an inert coating
by passivation using a process (typically patented) that diffuses
5.5 Gas samples are collected onto media cartridges or tubes
amorphous silicon material into the surface of the stainless
at the exhaust port of the micro-scale chamber at various
steel.
elapsed times throughout the test. The entire gas flow exiting
the chamber passes through the cartridge or tube. The sampling 7.2.2 The gasket or O-ring used to seal the lid to its body
flow rate is equivalent to the airflow rate of the micro-scale shall be low absorbing and low emitting at the operating
chamber. temperature so it does not contribute significantly to back-
5.5.1 Formaldehyde and other carbonyl compounds are ground VOC concentrations. Gaskets and O-rings composed of
sampled onto chemically treated cartridges (DNPH) and ana- fluoropolymer elastomer are suitable for this application. The
lyzed as described in Test Method D5197 and ISO 16000-3. apparatus shall facilitate disassembly for loading samples and
The sampling flow rate may be less than specified in the for cleaning.
analytical methods.
7.3 Temperature and Heating Requirements:
5.5.2 Emissions of other VOCs and SVOCs are collected
7.3.1 Verify the interior temperature of each micro-scale
onto sorbent tubes and analyzed by thermal desorption – gas
chamber with a traceable device, for example with a National
chromatography (GC) with mass spectrometry (MS) to identify
Institute of Standards and Technology (NIST) traceable certifi-
and quantify compounds as described in ISO 16000-6 (Annex
cate. The device used to measure temperature shall have an
D) and U.S. EPA Compendium Method TO-17.
accuracy of at least 61 °C between 30 °C and 40 °C. Various
micro-scale chamber designs may require different temperature
6. Significance and Use
measuring devices or techniques.
6.1 SPF insulation is applied and formed onsite, which
7.3.2 Measure the temperature of each individual micro-
creates unique challenges for measuring product emissions.
scale chamber prior to first use and within 90 days of
This test method provides a way to measure post-application
subsequent use with the water-fill procedure below.
chemical emissions from SPF insulation.
7.3.2.1 Remove each micro-scale chamber from the system
6.2 This test method can be used to identify compounds that
and fill each micro-scale chamber with distilled or deionized
emit from SPF insulation products, and the emission factors
water to between 50 % and 75 % of the chamber volume. Place
may be used to compare emissions at the specified sampling
the water containing micro-scale chambers in the system and
times and test conditions.
set the system to the prescribed test temperature of 35 °C.
Insert the temperature device through the sampling port so that
6.3 Emission data may be used in product development,
it is immersed in the water and the sensor does not touch the
manufacturing quality control and comparison of field samples.
chamber walls or bottom of the chamber. The airflow through
6.4 This test method is used to determine chemical emis-
the chamber shall be set as described in 7.4.3. Allow the
sions from freshly applied SPF insulation samples. The utility
micro-scale chambers to equilibrate for at least 90 min.
of this test method for investigation of odors in building scale
Determine the average temperature from each micro-scale
environments has not been demonstrated at this time.
chamber from at least five data points evenly spaced over a
time that is equal to or greater than period of the heating
7. Apparatus
frequency for the chamber. Record the average micro-scale
chamber temperature and standard deviation to the nearest
7.1 General Description:
0.1 °C. If the average temperature of any micro-scale chamber
7.1.1 Micro-scale chambers are described in Practice
is not between 34.0 °C and 36.0 °C, the temperature control
D7706. The micro-scale chamber test apparatus comprises one
shall be rectified prior to conducting any tests.
or more micro-scale chambers, a means of controlling the
micro-scale chamber(s) at 35 °C 6 1 °C, a regulated clean air
7.3.3 Additionally, prior to each use of 24 or more hours,
supply system and gas sampling capabilities. measure the temperature of each micro-scale chamber with
7.1.2 The micro-scale chamber suitable for SPF insulation either the water-fill procedure (7.3.2.1) or by placing a mea-
emissions testing is cylindrical in shape to accommodate an suring device in the air space of the chamber (7.3.3.1) or taping
O-ring or gasket seal with an internal diameter of 6 cm to the device to the bottom of the chamber (7.3.3.2). The average
10 cm and a depth of at least 3.5 cm. The chamber shall be of the chosen temperature measurement technique shall be
capable of achieving an area specific flow rate of 0.95 m ⁄h 6 demonstrated to agree with 61 °C of the average of the most
0.5 m ⁄h at a flow rate not exceeding 150 mL/min. All of the air recent water-fill measurement. The heating and cooling cycle
exiting the chamber outlet passes onto the sampling media in some micro-scale chamber designs can result in 1 °C to 2 °C
cartridge or tube during sampling events. cycles (at 35 °C). The averaging time should be three times the
D8142 − 23
period of the heating frequency for the chamber. Allow the GC/MS are described in Practice D6196, U.S. EPA Compen-
chamber to equilibrate prior to measurement (up to 20 min). dium Method TO-17, ISO 16000-6 (Annex D).
7.3.3.1 Devices in air should be placed at a consistent depth
8.1.2 Thermal desorption tubes are packed with more than
in the chamber to get reliable values. Micro-scale chamber’s air one sorbent to cover the wide volatility range for this method.
temperature can be vertically stratified in air up to 2 °C.
Multi-sorbent tubes are packed in order of increasing sorbent
7.3.3.2 The ability of temperature devices taped to or strength to facilitate quantitative retention and desorption of
touching the bottom of the chamber to represent the water
VOCs over a wide volatility range. The higher molecular
determined values is dependent upon the chamber design. weight compounds are captured on the front, weaker sorbent;
Micro-scale chamber’s wall temperature can be horizontally
the more volatile compounds are retained farther into the
stratified up to 0.6 °C. packing on a stronger sorbent. The sample tube is marked to
7.3.4 The apparatus may provide for heating of chamber
designate the proper flow path during sampling. Due to the
bodies in some cases as high as 250 °C for facilitating chamber wide range of volatility of compounds two multi-sorbent tubes
cleaning.
are specified:
8.1.2.1 Multi-sorbent Tube A, for VOCs and SVOCs—
7.4 Air Supply Requirements:
Quartz Wool backed up a weak porous polymer further backed
7.4.1 Ultra-zero grade air is used as the carrier gas through
up by a strong strength graphitized carbon black. See Practice
the micro-scale chamber. The air is dry and not humidified.
D6196, Table X1.1, Tabulated Summary of Sorbent Types,
7.4.2 The apparatus includes a means of supplying clean dry
Examples, Features, and Applications for further detail on
air to the chambers. Either electronic or mechanical flow
these sorbents.
controllers are used. The flow rate is controlled with an
8.1.2.2 Multi-sorbent Tube B, for Very Volatile Organic
accuracy of 62 % and a precision of 63 % of the reading.
Compounds (VVOCs) such as Blowing Agents—Weak porous
7.4.3 A constant inlet airflow rate is maintained to achieve
polymer backed up a medium strength graphitized carbon
an area specific flow rate between 0.9 m ⁄h and 1 m ⁄h. Micro-
black further backed up by a carbon molecular sieve. See
scale chambers with a 6.4 cm diameter are operated at
Practice D6196, Table X1.1, Tabulated Summary of Sorbent
50 mL ⁄min and those with a 9.2 cm diameter are operated at
Types, Examples, Features, and Applications for further detail
100 mL ⁄min. For other chamber sizes, do not exceed a flow
on these sorbents.
rate of 150 mL/min, and calculate the area specific flow rate as
follows:
NOTE 1—Not all blowing agents, such as 1,1,1,2-tetraflouroethane, used
in low-pressure SPF insulation systems, can be determined with this test
R 5 ~Q · 0.00006! ⁄A (1)
method.
where:
8.1.3 Follow Practice D6196 for selection of sorbent tubes
R = area specific flow rate, m/h,
if alternative tubes are required to recover specific compounds
Q = flow rate of micro-scale chamber, mL/min,
not listed in this standard.
A = specimen’s horizontally projected surface area
8.1.4 Tubes are conditioned before initial use as specified by
(13.1), m , and
the tube supplier or as described below.
0.00006 = a constant to convert mL/min to m /h.
8.1.4.1 For multi-sorbent Tube A, under a flow of
7.4.4 During operation, the micro-scale chamber should be
50 mL ⁄min to 100 mL ⁄min of pure inert gas (helium or
leak free. The procedure for determining this differs for
nitrogen) condition the sorbent tubes as follows: 2 h at 320 °C,
micro-scale chambers arranged to measure multiple samples in
followed by a further 30 min at 335 °C. Recondition the tubes
parallel to that of a serially operated micro-scale chamber
after each use for 30 min at 335 °C.
which analyzes one sample at a time. For a parallel-operated
8.1.4.2 For multi-sorbent Tube B, under a flow of
micro-scale chamber with a common gas source for all
50 mL ⁄min to 100 mL ⁄min of pure inert gas (helium or
chambers, the airflow rate of each chamber is measured and if
nitrogen) condition the sorbent tubes as follows: 1 h at 100 °C,
all the flows are all within 5 % of each other this indicates a
followed by 1 h at 200 °C, followed by 1 h at 300 °C, followed
leak free system. If one or more of the chambers shows
by 30 min at 335 °C. Recondition the tubes after each use for
anomalously low flow result this indicates a leak. For a serially
15 min at 100 °C, followed by 15 min at 200 °C, followed by
operated micro-scale chamber the cell is considered sufficiently
15 min at 300 °C, followed by 15 min 335 °C.
leak-free if the outlet airflow rate is within 95 % of the inlet
8.1.5 Each tube is indelibly etched with a unique identifi-
airflow rate. The airflow rate can be measured as described in
cation number and optional bar code. The numbers of the tubes
Practice D5337.
selected are recorded and batched according to date of packing
and number of thermal cycles. Sorbent tubes are sealed with
8. Reagents and Materials
long-term storage caps until the start of sample collection and
8.1 Gas Sampling Devices: are resealed with the same caps immediately after sample
collection unless they are to be analyzed immediately.
8.1.1 Sorbent Tubes for Active Sampling—Sorbent tubes are
commercially available either pre-packed by the manufacturer 8.1.6 Sorbent Tube End Caps for Storage—Blank and
or empty. Different suppliers provide different size tubes and sampled tubes are sealed with metal screw-cap compression
packing lengths. The most commonly used tubes for thermal fittings with combined (one-piece) PTFE ferrules for storage
desorption are 8.9 cm long and 6.4 mm O.D. stainless steel. and transportation. If alternate fittings/storage systems are
Appropriate sorbents for analysis by thermal desorption used, the laboratory shall determine that they meet storage and
D8142 − 23
transportation stability requirements. To check that storage example of instrument conditions for measuring SPF emis-
caps have been fitted correctly, check the length of the capped sions.
tube to make sure the seals are seated as far down the tube as 8.4.2 Calibration Solution Loading Rig—Consists of an
possible and check that the caps cannot be pulled off the tubes unheated injector port with a controlled carrier gas (nitrogen)
by hand using reasonable force. supply and a sorbent tube connection point. Heated tube
injectors shall not be used to avoid potential losses of flame
8.2 For formaldehyde and other carbonyl compounds, use
retardants and reactive amine compounds. The sampling end of
cartridges or tubes containing silica gel treated with 2,4-
a packed sorbent tube is connected to the unit and the carrier
dinitrophenylhydrazine (DNPH) as described in Test Method
gas flow is set to between 50 mL ⁄min and 100 mL/min. Carrier
D5197. Use adapters if necessary to obtain a seal on the
gas sweeps through the injection port and passes through the
micro-scale chamber exhaust.
sorbent tube to vent. The calibration standard (liquid or gas) is
8.3 Cutting Tools and Accessories:
introduced through the injector septum using a standard GC
8.3.1 Circular foam coring tool, described in Practice
syringe. Liquid standard solutions vaporize in the flow of gas
D7859. The tool shall be clean, constructed of steel to cut SPF
allowing analytes to reach the sorbent bed in the gas phase.
insulation samples to fit tightly into micro-scale chambers.
8.5 Reference Standards for Thermal Desorption GC/MS:
8.3.2 Knife or saw, clean, and free of cutting oils and other
8.5.1 Purity of Reagents—Reagent grade chemicals shall be
organic contaminants.
used in all tests. It is intended that all reagents conform to the
8.3.3 Shim rings, clean, constructed of PTFE, stainless
specifications of the Committee on Analytical Reagents of the
steel, or other inert material, which may be required to seal off
American Chemical Society where such specifications are
edges of open-cell SPF specimens so they fit tightly into the
available. Other grades may be used, provided it is first
micro-scale chambers.
ascertained that the reagent is of sufficiently high purity to
8.3.4 Spacers, clean, constructed of PTFE, stainless steel, or
permit its use without lessening the accuracy of the determi-
other inert material to elevate the specimen to the specified
nation.
height in the micro-scale chamber.
8.5.2 Reference Target Compounds—High purity com-
8.4 Thermal Desorption GC/MS:
pounds of interest can be sourced from commercial vendors.
8.4.1 The instrumentation for thermal desorption GC/MS is
described in Practice D6196 (thermal desorption), U.S. EPA
Compendium Method TO-17 and U.S. EPA Method 325B, ISO
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington,
16000-6 or use equivalent GC/MS technology. Operate the MS
DC. For suggestions on the testing of reagents not listed by the American Chemical
in full scan mode. The analytical column and transfer line shall
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
be amine-compatible and optimized for the analysis of the
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
target compounds specified in Table 1. See Table X1.1 for an copeial Convention, Inc. (USPC), Rockville, MD.
TABLE 1 Example List of Target Compounds
NOTE 1—TD = Thermal desorption tube (8.1.2),
DNPH = 2,4-dinitrophenylhydrazine tube (8.2), and
The primary quantitation ion for each compound is in parentheses.
GC/MS Primary and Secondary
Compound CAS # Sample Media
Ions
1,1,1,4,4,4-Hexafluoro-2-butene 692-49-9 TD (95), 69, 145
Trans-1-chloro-3,3,3-trifluoropropene 102687-65-0 TD (95), 69, 130
1,1,1,3,3-Pentafluoropropane (HFC-245fa) 460-73-1 TD (64), 69, 134
Trimethylamine 75-50-3 TD (58), 59, 42
1,1-Dichloroethene 75-35-4 TD (61), 96, 98
trans-1,2-Dichloroethene (TDCE) 156-60-5 TD (61), 96, 98
1,2-Dichloropropane 78-87-5 TD (63), 62, 76
1,4-Dioxane 123-91-1 TD (88), 58, 57
2-Ethyl-4-methyl-1,3-dioxolane 4359-46-0 TD (87), 59, 72
Chlorobenzene 108-90-7 TD (112), 77, 114
2-Butoxyethanol 111-76-2 TD (57), 87, 45
1,4-Dichlorobenzene 106-46-7 TD (146), 148, 111
Triethylenediamine (TEDA) 280-57-9 TD (58), 55, 112
1,2-Dichlorobenzene 95-50-1 TD (146), 148, 111
Bis(2-chloroisopropyl) ether 108-60-1 TD (45), 121, 77
Bis[2-(N,N-dimethylamino)ethyl] ether (BDMAEE) 3033-62-3 TD (58), 71, 42
Triethyl phosphate (TEP) 78-40-0 TD (99), 127, 155
Pentamethyldiethylenetriamine (PMDTA) 3030-47-5 TD (72), 58, 115
1,2-Dimethylimidazole 1739-84-0 TD (96), 54, 95
4-(1,1-Dimethylpropyl) phenol 80-46-6 TD (135), 107, 164
Tris(1-chloro-2-propyl) phosphate (TCPP) 13674-84-5 TD (99), 125, 157
Propionaldehyde 123-38-6 DNPH –
Formaldehyde 50-00-0 DNPH –
Acetaldehyde 75-07-0 DNPH –
D8142 − 23
Alternatively, components from raw materials of the SPF 8.5.6 Transfer the stock standard solution into a bottle with
insulation formulation are sourced directly from the SPF a PTFE-lined screw-cap. Store, with minimal headspace and
insulation manufacturer or raw material supplier if the primary protected from light, at –10 °C to –20 °C. Return standards to
chemical content is known. When compound purity is assayed the freezer as soon as the analyst has completed mixing or
to be 96 % or greater, the weight may be used without diluting the standards to prevent evaporation of the solution.
correction to calculate the concentration of the stock standard. 8.5.7 Calibration Solutions—Following guidance given in
The target compounds of interest are determined from specific Practice D6196, dilute the stock standards such that a 0.5 μL to
VOCs and SVOCs that are known to be present or emit from 2 μL injection, by means of the calibration solution loading rig
the SPF formulation. An example list of target compounds introduces 20 ng to 2000 ng of each compound, or an alterna-
derived from a variety of SPF insulation samples is shown in tive mass range if more appropriate to the samples being
Table 1. analyzed.
8.5.8 Internal Standards—Internal standards shall be used
NOTE 2—Toluene equivalents can be used to estimate non-target
as described in U.S. EPA Compendium Method TO-17 or U.S.
compounds, as described in California Department of Public Health
EPA Method 325B. Gas-phase standards must be obtained in
Standard Method for the Testing and Evaluation of Volatile Organic
pressurized cylinders containing vendor certified gas concen-
Chemical Emissions from Indoor Sources Using Environmental
Chambers, CDPH/EHLB/Standard Method V.1.2.
trations accurate to 65 %. The concentration shall be such that
the masses of internal standard components introduced are
8.5.3 Dilution Solvent—Purge-and-trap grade methanol is
similar to those of the target compounds of this method.
used as the solvent to prepare calibration standards. It shall be
Alternatively, liquid solutions containing the internal standards
of chromatographic quality and free from compounds co-
can be loaded onto TD tubes prior to analysis as described in
eluting with the compound or compounds of interest. Alterna-
9.1.2. See Table X1.1 for an example of internal standards used
tive dilution solvents, for example, ethyl acetate or cyclo-
for measuring SPF emissions.
hexane can be used, particularly if there is a possibility of
reaction or chromatographic co-elution with methanol.
8.6 Reagents and materials for the analysis of formaldehyde
and other carbonyl compounds are described in Test Method
8.5.4 Stock Standard Solutions—Prepare stock standard so-
lutions in dilution solvent using assayed liquids or gases, as D5197.
appropriate at 2000 ng/μL or appropriate concentration. Place
8.7 Analytical Balance and Containers:
about 9 mL of methanol in a 10 mL tared ground-glass-
8.7.1 Class A volumetric flasks for preparing standard
stoppered volumetric flask. Allow the flask to stand, un-
solutions, as needed.
stoppered, for about 10 min or until all the dilution solvent
8.7.2 Analytical balance, readable and accurate to the near-
wetted surfaces have dried. Weigh the flask to the nearest
est 0.1 mg.
0.0001 g. Add the assayed reference material, as described
below.
9. Calibration and Standardization
8.5.4.1 Liquids—Using a syringe or pipette, immediately
9.1 Thermal desorption GC/MS standard calibration curves
add one or more drops (0.02 g for 2000 ng/μL) of the reference
are required for each compound of interest comprising at least
material to the flask; then reweigh. The liquid shall fall directly
five points covering an applicable range and with a factor of at
into the dilution solvent without contacting the neck of the
least 20 between the lowest and the highest level standard. At
flask. Very volatile organic liquids (for example 1,1,1,3,3-
least six points are used for quadratic fit calibration curves. The
pentafluoropropane) are placed in a freezer at –10 °C to –20 °C
standard concentrations distribution shall not be greater than
prior to preparation.
five times the concentration of the next lower standard (for
8.5.4.2 Gases—Solution Containing Approximately
example; 20 ng, 50 ng, 100 ng, 200 ng, 500 ng, 1000 ng,
1 mg ⁄mL of Gas Components—For gases, prepare a low level
2000 ng). Prepare loaded tubes by injecting aliquots of stan-
calibration solution as follows. Obtain pure gas at atmospheric
dard solutions onto clean sorbent tubes as follows:
pressure by filling a small plastic gas bag from a gas cylinder.
9.1.1 Fit the sampling end of the clean sorbent tube into the
Fill a 1 mL gas-tight syringe with 1 mL of the pure gas and
calibration solution loading rig (see 8.4.2) with a 50 mL ⁄min to
close the valve of the syringe. Using a 2 mL septum vial, add
100 mL/min flow rate of inert purge gas and inject 0.5 μL to
2 mL solvent and close with the septum cap. Insert the tip of
2 μL aliquot of an appropriate standard solution through the
the syringe needle through the septum cap into the solvent.
septum for 1 min to 5 min. Reproducible and quantitative
Open the valve and withdraw the plunger slightly to allow the
transfer of higher boiling compounds in liquid standards is
solvent to enter the syringe. The action of the gas dissolving
facilitated if the injection unit allows the tip of the syringe to
creates a vacuum, and the syringe fills with solvent. Return the
just touch the sorbent retaining gauze or quartz wool inside the
solution to the flask. Flush the syringe twice with the solution
tube. If calibration tubes are to be prepared using multiple
and return the washings to the flask. Calculate the mass of gas
standards, introduce those containing the least volatile com-
added using the gas laws, that is, 1 mol of gas at STP occupies
pounds of interest first and the most volatile compounds of
22.4 L.
interest (typically the gas phase standards) last. See Practice
8.5.5 Reweigh, dilute to volume, stopper, and then mix by D6196, 8.5, for further information on loading TD sorbent
inverting the flask several times. Calculate the concentration in tubes.
mg/L from the net gain in weight. The concentration in mg/L 9.1.2 If a liquid solution is used to load internal standards,
is equivalent to ng/μL. with 50 mL/min to 100 mL/min flow rate of inert purge gas,
D8142 − 23
inject 1 μL of the internal standard solution though the septum site by a trained applicator using professional spraying equip-
of the calibration loading rig for 1 min to 5 min, and then ment under defined conditions. Spray samples to a minimum
disconnect the tube and seal it using long-term storage caps. thickness specified in Practice D7859.
9.1.3 Use the GC/MS data acquisition software to plot
11.2 Practice D7859 describes standardized procedures for
relative response factors for each compound. Use the average
the preparation, spraying, packaging, and shipping of SPF
of response factors for each compound if the relative standard
insulation product samples to be tested for their emissions. In
deviation is ≤15 % or use a linear fit if the R value is ≥0.995,
addition, the density of the sample can be determined as
otherwise, a quadratic fit calibration curve shall be used.
described in Test Method D1622/D1622M.
NOTE 3—Some reactive compounds such as amine catalysts used in
11.3 To evaluate emissions from SPF insulation that already
SPF insulation may be non-linear. Use of a linear regression of the
has been applied in a building, samples can be collected onsite.
standard responses does not eliminate the possibility of large systematic
With a clean knife or saw, cut out a representative section of
errors if the intercept value is large relative to the quantity being
measured. Non-linearity can be evaluated using statistical software or
material being careful not to damage the surface of the product.
tested for lack of fit by examining the residuals described in the Analytical
Collect the entire applied thickness with minimum dimensions
Methods Committee technical brief cited in the bibliography.
of 30 cm by 30 cm. In the situation where it is not feasible to
9.1.4 Repeat multi-level calibration whenever the single-
collect the entire thickness or a 30 cm by 30 cm sample, collect
level calibration check falls outside the specified range speci-
the maximum thickness possible with dimensions of
fied in 15.7.
minimally, 10 cm by 10 cm. Upon collection, immediately,
9.1.5 TCPP and its isomers elute as three peaks in the
wrap the sample in clean aluminum foil and place the sample
GC/MS chromatogram. In this case, integrate the sum of the
into a layered polyethylene terephthalate (PET) food storage
areas of the target ion from all three observed peaks and report
bag as described in Practice D7859.
as TCPP, total isomers. Manual integration may be necessary to
11.4 Ship the samples in an insulated secondary container
integrate the sum of areas from all three isomers.
by means of overnight delivery as described in Practice D7859.
9.2 Prepare reference standards and calibration curves for
11.5 Upon receipt at the laboratory, note any damage to the
formaldehyde and other carbonyl compounds as described in
shipping container or to the layered PET storage bag. If the
Test Method D5197.
storage bag has been compromised, resampling is necessary;
9.3 Care must be taken to ensure that the calibration
otherwise, if the sample cannot be re-sprayed or re-collected,
standards do not break through the sorbent material, or
qualify the emissions data.
overload the column or detector. The process of thermally
11.6 Prior to testing, the sample is stored in its original
desorbing sorbent tubes can be carried out split or splitless.
unopened layered PET bag at typical indoor conditions as
Table X1.1 in the appendix gives suggested split conditions;
described in Practice D7859. During storage in the bag, protect
however the analyst may need to adjust the split flow (or lack
the sample from chemical contamination and from exposure to
thereof) to accommodate the sensitivity needed or the capacity
temperatures in excess of 25 °C. Do not refrigerate or place the
of the column, the detector or both.
sample in a freezer. Document the storage conditions (for
10. Preparation of Apparatus example, storage location and temperature).
10.1 Cleaning Procedure:
11.7 Prepare the specimens and begin the chamber test
10.1.1 Remove the gaskets or O-rings and clean the cham-
within 48 h or sooner of spraying or sample collection to
ber components using a dilute alkaline detergent followed by
minimize potential losses of VOCs as described in Practice
three separate rinses with distilled water. Alternately, clean the
D7859.
chamber components with methanol. Avoid abrasive cleaners
or cleaners that have a high pH. Dry thoroughly.
12. Specimen Preparation and Chamber Operation
10.1.2 If the apparatus is designed to accommodate elevated
12.1 Open the PET layered bag and prepare the specimen
temperature, the chamber can be cleaned without disassembly.
for chamber testing within 20 min as specified in Practice
Rinse the chamber with methanol, and then raise the chamber
D7859. Prepare duplicate specimens from each sample.
temperature to 150 °C or higher if necessary with elevated flow
of clean dry air sufficiently long to reduce background artifacts 12.2 Using a fabricated circular steel coring tool described
to acceptable levels at normal operating conditions. in Practice D7859, cut the specimen so that it fits tightly into
the chamber body to minimize gaps between the specimen and
10.2 Chamber Background Measurement:
chamber wall. Open-cell SPF may require the use of cylindri-
10.2.1 Measure background levels of each chamber prior to
cal shim rings to reduce gaps.
testing each set of samples. Background measurements are
performed under normal operating conditions but without a
12.3 Collect specimens from the substrate material in a
specimen in the chamber and evaluated for contamination as
random fashion, but avoid taking specimens that are less than
described in 15.5.
3 cm from the edge of the sample block. For open cell SPF
insulation, trim ≤5 mm from the top surface top of the
11. Preparation of Samples and Sample Collection
specimen, which will provide a smoother surface and mimic
11.1 SPF insulation samples are sprayed and prepared for trimming in the field to align with wall studs or other structural
testing in a controlled spray booth or a field product installation elements. Do not trim the surface skin from closed-cell SPF
D8142 − 23
insulation unless specified by the sample submitter. Record if the safe sampling volumes with TD tubes for each compound
the specimen surface is trimmed or not. under the test conditions. At the end of the sampling period,
disconnect the sorbent tube from the outlet of the chamber.
12.4 If necessary, cut the bottom from the specimen so that
Seal the sorbent tube using appropriate fittings.
the specimen height is approximately 30 mm and the head-
12.11.3 If a liquid solution is used to load internal standards,
space from the surface of the specimen to the bottom surface of
inject 1 uL of internal standard solution onto each TD tube
the chamber lid is 5 mm 6 2 mm so that the chamber lids do
using the loading rig as described in 9.1.2. Seal the sorbent
not touch the surface of the specimens. Use spacers to elevate
tube using appropriate fittings.
the sample to the proper height in the micro-scale chamber if
12.11.4 Immediately after sampling the TD sorbent tubes,
the specimen is not thick enough to fill the chamber to the
sample with DNPH cartridges up to a total elapsed time of 20 h
height needed to achieve the required headspace distance.
in order to achieve adequate detection limits for formaldehyde
12.5 Weigh the SPF specimen to the nearest milligram and
and other carbonyl compounds.
record the mass.
12.12 Store and transport batches of sealed TD sorbent
12.6 Carefully, insert the specimen into the chamber cavity
tubes in clean, airtight, non-outgassing containers such as
with the outer surface side facing up; place the O-ring or gasket
uncoated paint cans. TD sorbent tubes do not require refriger-
on the micro-scale chamber. Photograph the specimens prior to
ated transport or storage. However, if refrigerated conditions
closing and sealing the chamber lid.
are used, for example during extended storage periods
(>7 days), retighten the tube seals once the tubes have reached
12.7 Turn on the air supply and adjust the flow rate to
the storage temperature. Allow the tubes to re-equilibrate with
achieve an area specific flow rate between 0.9 m/h and 1.0 m/h.
room temperature before seals are removed immediately prior
This can be done by adjusting the flow rate to 50 mL/min for
to analysis. This prevents humidity from the laboratory air
micro-scale chambers with an inner diameter of 6.4 cm, or
condensing inside the cold tube and interfering in the subse-
adjusting the flow rate to 100 mL/min for micro-scale cham-
quent analysis. Analyze the samples as soon as possible, but no
bers with an inner diameter of 9.2 cm. Other sized micro-scale
later than 30 days after collection. See Practice D6196.
chambers can be used, but the flow rate shall not exceed
150 mL ⁄min.
12.13 Seal the DNPH cartridges and store in the refrigerator
12.8 Record the date and time the test is initiated, t . Check as described in Test Method D5197. Analyze within 30 days
after collection.
the airflow rate at the chamber exhaust as described in Practice
D5337. Record the flow rates. Maintain the supply of air to the
12.14 Option A—Collect another set of samples at 24 h
micro-scale chamber continuously for the entire duration of the
elapsed time following 12.11.1 to 12.11.3.
test (all of the time that the specimen is in the micro-scale
12.15 Option B—In order to evaluate the emissions from 2 h
chamber).
to 168 h or to monitor emissions from semivolatile organic
12.9 Operate the micro-scale chamber at 35 °C 6 1 °C
flame retardants such as TCPP, collect additional sample sets at
throughout the duration of the test. Record the instrument
24 h, 48 h, 72 h, and 168 h following steps 12.11.1 to 12.11.4.
displayed operating temperature each time a sample is col-
12.16 After the last sample has been collected, open the
lected.
chamber lid and photograph the specimens in the chamber
12.10 Begin collecting emissions samples after 2 h from t .
body. Note any specimen shrinking that may have occurred
NOTE 4—TCPP and other semi-volatile compounds may take much
during the test period.
longer than 2 h to reach a quasi-steady state; therefore, emission
measurements of these compounds should only be used for informative
12.17 Analyze the TD tubes for target and non-target
purposes at 2 h. For example, these values can be used to determine how
compounds by thermal desorption GC/MS with the conditions
long to collect emission samples
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D8142 − 17 D8142 − 23
Standard Test Method for
Determining Chemical Emissions from Spray Polyurethane
Foam (SPF) Insulation using Micro-Scale Environmental
Test Chambers
This standard is issued under the fixed designation D8142; 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.
ε NOTE—Editorially added research report information to Section 16 and Appendix X1 in February 2020.
1. Scope
1.1 This test method is used to identify and to measure the emissions of volatile organic compounds (VOCs) emitted from samples
of cured spray polyurethane foam (SPF) insulation using micro-scale environmental test chambers combined with specific air
sampling and analytical methods for VOCs.
1.2 Specimens prepared from product samples are maintained at specified conditions of temperature, humidity, airflow rate, and
elapsed time in micro-scale chambers that are described in Practice D7706. Air samples are collected periodically at the chamber
exhaust at the flow rate of the micro-scale chambers.
1.2.1 Samples for formaldehyde and other low-molecular weight carbonyl compounds are collected on treated silica gel cartridges
and are analyzed by high performance liquid chromatography (HPLC) as described in Test Method D5197 and ISO 16000-3.
1.2.2 Samples for other VOCs are collected on multi-sorbent samplers and are analyzed by thermal-desorption gas chromatog-
raphy / mass spectrometry (TD-GC/MS) as described in U.S. EPA Compendium Method TO-17 and ISO 16000-6.
1.3 This test method is intended specifically for SPF insulation products. Compatible product types include two component, high
pressure and two-component, low pressure formulations of open-cell and closed-cell SPF insulation.
1.4 VOCs that can be sampled and analyzed by this test method generally include organic blowing agents such as
1,1,1,3,3-pentafluoropropane, formaldehyde and other carbonyl compounds, residual solvents, and some amine catalysts.
Emissions of some organic flame retardants can be measured after 24 h with this method, such as tris (chloroisopropyl) phosphate
(TCPP).
1.5 This test method does not cover the sampling and analysis of methylene diphenyl diisocyanate (MDI) or other isocyanates.
1.6 Area-specific and mass-specific emission rates are quantified at the elapsed times and chamber conditions as specified in 13.2
and 13.3 of this test method.
1.7 This test method is used to identify emitted compounds and to estimate their emission factors at specific times. The emission
This test method is under the jurisdiction of ASTM Committee D22 on Air Quality and is the direct responsibility of Subcommittee D22.05 on Indoor Air.
Current edition approved Oct. 1, 2017Sept. 1, 2023. Published October 2017October 2023. Originally approved in 2017. Last previous edition approved in 2017 as
ɛ1
D8142 – 17 . DOI: 10.1520/D8142-17E01.10.1520/D8142-23.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D8142 − 23
factors are based on specified conditions, therefore, use of the data to predict emissions in other environments may not be
appropriate and is beyond the scope of this test method. The results may not be representative of other test conditions or
comparable with other test methods.
1.8 This test method is primarily intended for freshly applied, SPF insulation samples that are sprayed and packaged as described
in Practice D7859. The measurement of emissions during spray application and within the first hour following application is
outside of the scope of this test method.
1.9 This test method can also be used to measure the emissions from SPF insulation samples that are collected from building sites
where the insulation has already been applied. Potential uses of such measurements include investigations of odor complaints after
product application. However, the specific details of odor investigations and other indoor air quality (IAQ) investigations are
outside of the scope of this test method.
1.10 The values stated in SI units are to be regarded as standard. No other units of measure are used.measurement are included
in this standard.
1.11 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.
1.12 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.
2. Referenced Documents
2.1 ASTM Standards:
D1356 Terminology Relating to Sampling and Analysis of Atmospheres
D1622/D1622M Test Method for Apparent Density of Rigid Cellular Plastics
D5116 Guide for Small-Scale Environmental Chamber Determinations of Organic Emissions from Indoor Materials/Products
D5197 Test Method for Determination of Formaldehyde and Other Carbonyl Compounds in Air (Active Sampler Methodology)
D5337 Practice for Setting and Verifying the Flow Rate of Personal Sampling Pumps
D6196 Practice for Choosing Sorbents, Sampling Parameters and Thermal Desorption Analytical Conditions for Monitoring
Volatile Organic Chemicals in Air
D7706 Practice for Rapid Screening of VOC Emissions from Products Using Micro-Scale Chambers
D7859 Practice for Spraying, Sampling, Packaging, and Test Specimen Preparation of Spray Polyurethane Foam (SPF)
Insulation for Testing of Emissions Using Environmental Chambers
2.2 ISO Standards:
ISO 16000-3 Indoor Air—Part 3: Determination of Formaldehyde and Other Carbonyl Compounds in Indoor Air and Test
Chamber Air—Active Sampling Method
ISO 16000-6 Indoor Air—Part 6: Determination of Volatile Organic Compounds in Indoor and Test Chamber Air by Active
Sampling on Tenax TA Sorbent, Thermal Desorption, and Gas Chromatography Using MS or MS-FID
2.3 Government Agency Methods:
40 CFR Appendix B to Part 136 Definition and Procedure for the Determination of the Method Detection Limit-Revision 1.11
California Department of Public Health Standard Method for the Testing and Evaluation of Volatile Organic Chemical Emissions
from Indoor Sources Using Environmental Chambers, CDPH/EHLB/Standard Method V.1.2 (January 2017)
U.S. EPA Compendium Method TO-17 Determination of Volatile Organic Compounds in Ambient Air Using Active Sampling
Onto Sorbent Tubes, Compendium of Methods for the Determination of Toxic Organic Compounds in Ambient Air, Second
Edition (January 1999)
U.S. EPA Method 325B Volatile Organic Compounds from Fugitive and Area Sources: Sampler Preparation and Analysis, Air
Emission Measurement Center (EMC) (September 29, 2015)
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from International Organization for Standardization (ISO), ISO Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva,
Switzerland, http://www.iso.org.
Available from U.S. Government Printing Office, Superintendent of Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://www.access.gpo.gov.
Available from United States Environmental Protection Agency (EPA), William Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,
http://www.epa.gov.
D8142 − 23
3. Terminology
3.1 Definitions—For definitions and terms commonly used for sampling and analysis of atmospheres, refer to Terminology D1356.
For definitions and terms commonly used when testing materials and products for VOC emissions, refer to Guide D5116. For
definition of micro-scale test chamber, refer to Practice D7706.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 area specific flow rate, n—the ratio of the airflow rate into the chamber in m /h and the projected surface area of the test
specimen exposed to air in m with units of m/h.
3.2.2 closed-cell SPF insulation, n—SPF insulation that contains cells or voids that are not interconnected.
3.2.2.1 Discussion—
3 3
Closed-cell SPF insulation typically has a density between 2424 kg ⁄m to 32 32 kg kg/m⁄m when fully cured.
3.2.3 open-cell SPF insulation, n—SPF insulation that contains cells or voids that are largely interconnected.
3.2.3.1 Discussion—
3 3
Open-cell SPF insulation typically has a density between 6.46.4 kg ⁄m to 9.6 9.6 kg kg/m⁄m when fully cured.
4. Principles
4.1 Micro-scale test chambers are used for measuring emissions of VOCs including formaldehyde and other carbonyl compounds
from materials and products.
4.2 Wall adsorption effects of reactive compounds and SVOCs are minimized by reducing the exposed inner surface of the
chamber by fitting the SPF samples directly into the micro-scale chamber with minimal headspace. Passivated treatment of the
interior surfaces also contributes to reduced sorption effects.
4.3 Micro-scale chambers are used for measuring area-specific emissions from the surface of SPF insulation or mass-specific
emissions from the mass of the sample.
5. Summary of Test Method
5.1 A micro-scale chamber is used to measure VOC emissions from SPF insulation samples. A representative test specimen is
prepared from the sample and is placed directly into a micro-scale chamber. Air samples are collected from the chamber exhaust
at specified elapsed times.
5.2 Clean dry air is supplied to a micro-scale chamber and passes over the exposed surface of the test specimen before reaching
the exhaust port. The airflow rate and the temperature within the micro-scale chamber are controlled. As the air passes over the
test specimen, emitted compounds are swept away from the sample’s surface.
5.3 The standard temperature for the test method is 35 6 1 °C. 35 °C 6 1 °C. Emission rates of organic compounds from building
materials and sorption and desorption of organic compounds from interior surfaces are sensitive to temperature. Operation of the
micro-scale chamber at the specified temperature (above ambient) enhances the emission rates of some compounds and may
improve the quantitative recovery of some less volatile compounds.
5.4 The area-specific flow rate specified for this test method is 0.950.95 m ⁄h 6 0.050.05 m m/h. ⁄h. The maximum airflow rate
for the micro-scale chamber shall not exceed 150 mL/min, and the airflow rate shall not exceed the maximum flow rate for the
sampling media.
5.5 Gas samples are collected onto media cartridges or tubes at the exhaust port of the micro-scale chamber at various elapsed
times throughout the test. The entire gas flow exiting the chamber passes through the cartridge or tube. The sampling flow rate is
equivalent to the airflow rate of the micro-scale chamber.
5.5.1 Formaldehyde and other carbonyl compounds are sampled onto chemically treated cartridges (DNPH) and analyzed as
described in Test Method D5197 and ISO 16000-3. The sampling flow rate may be less than specified in the analytical methods.
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5.5.2 Emissions of other VOCs and SVOCs are collected onto sorbent tubes and analyzed by thermal desorption – gas
chromatography (GC) with mass spectrometry (MS) to identify and quantify compounds as described in ISO 16000-6 (Annex D)
and U.S. EPA Compendium Method TO-17.
6. Significance and Use
6.1 SPF insulation is applied and formed onsite, which creates unique challenges for measuring product emissions. This test
method provides a way to measure post-application chemical emissions from SPF insulation.
6.2 This test method can be used to identify compounds that emit from SPF insulation products, and the emission factors may be
used to compare emissions at the specified sampling times and test conditions.
6.3 Emission data may be used in product development, manufacturing quality control and comparison of field samples.
6.4 This test method is used to determine chemical emissions from freshly applied SPF insulation samples. The utility of this test
method for investigation of odors in building scale environments has not been demonstrated at this time.
7. Apparatus
7.1 General Description:
7.1.1 Micro-scale chambers are described in Practice D7706. The micro-scale chamber test apparatus comprises one or more
micro-scale chambers, a means of controlling the micro-scale chamber(s) at 35 6 1 °C, 35 °C 6 1 °C, a regulated clean air supply
system and gas sampling capabilities.
7.1.2 The micro-scale chamber suitable for SPF insulation emissions testing is cylindrical in shape to accommodate an O-ring or
gasket seal with an internal diameter of 6 to 10 cm 6 cm to 10 cm and a depth of at least 3.5 cm. 3.5 cm. The chamber shall be
capable of achieving an area specific flow rate of 0.950.95 m ⁄h 6 0.50.5 m m/h ⁄h at a flow rate not exceeding 150 mL/min. All
of the air exiting the chamber outlet passes onto the sampling media cartridge or tube during sampling events.
7.1.3 The prepared SPF insulation specimen must fit into the chamber body such that the back surface and edges of the specimen
are not directly exposed to the stream of air. An example micro-scale chamber to measure emissions of SPF insulation is shown
in Fig. X1.1.
7.2 Construction:
7.2.1 The micro-scale chamber body and associated lid shall be constructed of polished stainless steel with an inert coating by
passivation using a process (typically patented) that diffuses amorphous silicon material into the surface of the stainless steel.
7.2.2 The gasket or O-ring used to seal the lid to its body shall be low absorbing and low emitting at the operating temperature
so it does not contribute significantly to background VOC concentrations. Gaskets and O-rings composed of fluoropolymer
elastomer are suitable for this application. The apparatus shall facilitate disassembly for loading samples and for cleaning.
7.3 Temperature and Heating Requirements:
7.3.1 Verify the interior temperature of each micro-scale chamber with a traceable device, for example with a National Institute
of Standards and Technology (NIST) traceable certificate. The device used to measure temperature shall have an accuracy of at
least 61 °C between 30 °C and 40 °C. Various micro-scale chamber designs may require different temperature measuring devices
or techniques.
7.3.2 Measure the temperature of each individual micro-scale chamber prior to first use and within 90 days of subsequent use with
the water-fill procedure below.
7.3.2.1 Remove each micro-scale chamber from the system and fill each micro-scale chamber with distilled or deionized water
to between 50 % and 75 % of the chamber volume. Place the water containing micro-scale chambers in the system and set the
system to the prescribed test temperature of 35 °C. Insert the temperature device through the sampling port so that it is immersed
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in the water and the sensor does not touch the chamber walls or bottom of the chamber. The airflow through the chamber shall
be set as described in 7.4.3. Allow the micro-scale chambers to equilibrate for at least 90 min. Determine the average temperature
from each micro-scale chamber from at least five data points evenly spaced over a time that is equal to or greater than period of
the heating frequency for the chamber. Record the average micro-scale chamber temperature and standard deviation to the nearest
0.1 °C. 0.1 °C. If the average temperature of any micro-scale chamber is not between 34.0 °C and 36.0 °C, the temperature control
shall be rectified prior to conducting any tests.
7.3.3 Additionally, prior to each use of 24 or more hours, measure the temperature of each micro-scale chamber with either the
water-fill procedure (7.3.2.1) or by placing a measuring device in the air space of the chamber (7.3.3.1) or taping the device to the
bottom of the chamber (7.3.3.2). The average of the chosen temperature measurement technique shall be demonstrated to agree
with 61 °C of the average of the most recent water-fill measurement. The heating and cooling cycle in some micro-scale chamber
designs can result in 1 °C to 2 °C cycles (at 35 °C). The averaging time should be three times the period of the heating frequency
for the chamber. Allow the chamber to equilibrate prior to measurement (up to 20 min).
7.3.3.1 Devices in air should be placed at a consistent depth in the chamber to get reliable values. Micro-scale chamber’s air
temperature can be vertically stratified in air up to 2 °C.
7.3.3.2 The ability of temperature devices taped to or touching the bottom of the chamber to represent the water determined values
is dependent upon the chamber design. Micro-scale chamber’s wall temperature can be horizontally stratified up to 0.6 °C.
7.3.4 The apparatus may provide for heating of chamber bodies in some cases as high as 250 °C for facilitating chamber cleaning.
7.4 Air Supply Requirements:
7.4.1 Ultra-zero grade air is used as the carrier gas through the micro-scale chamber. The air is dry and not humidified.
7.4.2 The apparatus includes a means of supplying clean dry air to the chambers. Either electronic or mechanical flow controllers
are used. The flow rate is controlled with an accuracy of 62 % and a precision of 63 % of the reading.
7.4.3 A constant inlet airflow rate is maintained to achieve an area specific flow rate between 0.90.9 m ⁄h and 11 m m/hr. ⁄h.
Micro-scale chambers with a 6.4 cm diameter are operated at 5050 mL mL/min ⁄min and those with a 9.2 cm diameter are operated
at 100100 mL mL/min. ⁄min. For other chamber sizes, do not exceed a flow rate of 150 mL/min, and calculate the area specific
flow rate as follows:
R 5 ~Q · 0.00006!⁄A (1)
where:
R = area specific flow rate, m/h,
Q = flow rate of micro-scale chamber, mL/min,
A = specimen’s horizontally projected surface area (13.1), m , and
0.00006 = a constant to convert mL/min to m /h.
7.4.4 During operation, the micro-scale chamber should be leak free. The procedure for determining this differs for micro-scale
chambers arranged to measure multiple samples in parallel to that of a serially operated micro-scale chamber which analyzes one
sample at a time. For a parallel-operated micro-scale chamber with a common gas source for all chambers, the airflow rate of each
chamber is measured and if all the flows are all within 5 % of each other this indicates a leak free system. If one or more of the
chambers shows anomalously low flow result this indicates a leak. For a serially operated micro-scale chamber the cell is
considered sufficiently leak-free if the outlet airflow rate is within 95 % of the inlet airflow rate. The airflow rate can be measured
as described in Practice D5337.
8. Reagents and Materials
8.1 Gas Sampling Devices:
8.1.1 Sorbent Tubes for Active Sampling—Sorbent tubes are commercially available either pre-packed by the manufacturer or
empty. Different suppliers provide different size tubes and packing lengths. The most commonly used tubes for thermal desorption
are 8.9 cm long and 6.4 mm O.D. stainless steel. Appropriate sorbents for analysis by thermal desorption GC/MS are described
in Practice D6196, U.S. EPA Compendium Method TO-17, ISO 16000-6 (Annex D).
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8.1.2 Thermal desorption tubes are packed with more than one sorbent to cover the wide volatility range for this method.
Multi-sorbent tubes are packed in order of increasing sorbent strength to facilitate quantitative retention and desorption of VOCs
over a wide volatility range. The higher molecular weight compounds are captured on the front, weaker sorbent; the more volatile
compounds are retained farther into the packing on a stronger sorbent. The sample tube is marked to designate the proper flow path
during sampling. Due to the wide range of volatility of compounds two multi-sorbent tubes are specified:
8.1.2.1 Multi-sorbent Tube A, for VOCs and SVOCs—Quartz Wool backed up a weak porous polymer further backed up by a
strong strength graphitized carbon black. See Practice D6196, Table X1.1, Tabulated Summary of Sorbent Types, Examples,
Features, and Applications for further detail on these sorbents.
8.1.2.2 Multi-sorbent Tube B, for very volatile organic compoundsVery Volatile Organic Compounds (VVOCs) such as blowing
agents—Blowing Agents—Weak porous polymer backed up a medium strength graphitized carbon black further backed up by a
carbon molecular sieve. See Practice D6196, Table X1.1, Tabulated Summary of Sorbent Types, Examples, Features, and
Applications for further detail on these sorbents.
NOTE 1—Not all blowing agents, such as 1,1,1,2-tetraflouroethane, used in low-pressure SPF insulation systems, can be determined with this test method.
8.1.3 Follow Practice D6196 for selection of sorbent tubes if alternative tubes are required to recover specific compounds not
listed in this standard.
8.1.4 Tubes are conditioned before initial use as specified by the tube supplier or as described below.
8.1.4.1 For multi-sorbent Tube A, under a flow of 50-10050 mL mL/min ⁄min to 100 mL ⁄min of pure inert gas (helium or
nitrogen) condition the sorbent tubes as follows: 2 hoursh at 320 °C, followed by a further 30 minutesmin at 335 °C. Recondition
the tubes after each use for 30 minutesmin at 335 °C.
8.1.4.2 For multi-sorbent Tube B, under a flow of 50–10050 mL mL/min ⁄min to 100 mL ⁄min of pure inert gas (helium or
nitrogen) condition the sorbent tubes as follows: 1 hourh at 100 °C, followed by 1 hourh at 200 °C, followed by 1 hourh at 300
°C, followed by 30 minutesmin at 335 °C. Recondition the tubes after each use for 15 minutes at 100 C, min at 100 °C, followed
by 15 minutesmin at 200 °C, followed by 15 minutesmin at 300 °C, followed by 15 minutesmin 335 °C.
8.1.5 Each tube is indelibly etched with a unique identification number and optional bar code. The numbers of the tubes selected
are recorded and batched according to date of packing and number of thermal cycles. Sorbent tubes are sealed with long-term
storage caps until the start of sample collection and are resealed with the same caps immediately after sample collection unless
they are to be analyzed immediately.
8.1.6 Sorbent Tube End Caps for Storage—Blank and sampled tubes are sealed with metal screw-cap compression fittings with
combined (one-piece) PTFE ferrules for storage and transportation. If alternate fittings/storage systems are used, the laboratory
shall determine that they meet storage and transportation stability requirements. To check that storage caps have been fitted
correctly, check the length of the capped tube to make sure the seals are seated as far down the tube as possible and check that
the caps cannot be pulled off the tubes by hand using reasonable force.
8.2 For formaldehyde and other carbonyl compounds, use cartridges or tubes containing silica gel treated with 2,4-
dinitrophenylhydrazine (DNPH) as described in Test Method D5197. Use adapters if necessary to obtain a seal on the micro-scale
chamber exhaust.
8.3 Cutting Tools and Accessories:
8.3.1 Circular foam coring tool, described in Practice D7859. The tool shall be clean, constructed of steel to cut SPF insulation
samples to fit tightly into micro-scale chambers.
8.3.2 Knife or saw, clean, and free of cutting oils and other organic contaminants.
8.3.3 Shim rings, clean, constructed of PTFE, stainless steel, or other inert material, which may be required to seal off edges of
open-cell SPF specimens so they fit tightly into the micro-scale chambers.
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8.3.4 Spacers, clean, constructed of PTFE, stainless steel, or other inert material to elevate the specimen to the specified height
in the micro-scale chamber.
8.4 Thermal Desorption GC/MS:
8.4.1 The instrumentation for thermal desorption GC/MS is described in Practice D6196 (thermal desorption), U.S. EPA
Compendium Method TO-17 and U.S. EPA Method 325B, ISO 16000-6 or use equivalent GC/MS technology. Operate the MS in
full scan mode. The analytical column and transfer line shall be amine-compatible and optimized for the analysis of the target
compounds specified in Table 1. See Table X1.1 for an example of instrument conditions for measuring SPF emissions.
8.4.2 Calibration Solution Loading Rig—Consists of an unheated injector port with a controlled carrier gas (nitrogen) supply and
a sorbent tube connection point. Heated tube injectors shall not be used to avoid potential losses of flame retardants and reactive
amine compounds. The sampling end of a packed sorbent tube is connected to the unit and the carrier gas flow is set to between
5050 mL ⁄min and 100 mL/min. Carrier gas sweeps through the injection port and passes through the sorbent tube to vent. The
calibration standard (liquid or gas) is introduced through the injector septum using a standard GC syringe. Liquid standard
solutions vaporize in the flow of gas allowing analytes to reach the sorbent bed in the gas phase.
8.5 Reference Standards for Thermal Desorption GC/MS:
8.5.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. It is intended that all reagents conform to the
specifications of the Committee on Analytical Reagents of the American Chemical Society where such specifications are available.
Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without
lessening the accuracy of the determination.
8.5.2 Reference Target Compounds—High purity compounds of interest can be sourced from commercial vendors. Alternatively,
components from raw materials of the SPF insulation formulation are sourced directly from the SPF insulation manufacturer or
TABLE 1 Example List of Target Compounds
NOTE 1—TD = Thermal desorption tube (8.1.2),
DNPH = 2,4-dinitrophenylhydrazine tube (8.2), and
The primary quantitation ion for each compound is in parentheses.
GC/MS Primary and Secondary
Compound CAS # Sample Media
Ions
1,1,1,4,4,4-Hexafluoro-2-butene 692-49-9 TD (95), 69, 145
Trans-1-chloro-3,3,3-trifluoropropene 102687-65-0 TD (95), 69, 130
1,1,1,3,3-Pentafluoropropane (HFC-245fa) 460-73-1 TD (64), 69, 134
Trimethylamine 75-50-3 TD (58), 59, 42
1,1-Dichloroethene 75-35-4 TD (61), 96, 98
3-Chloro-1-propene (Allyl Chloride) 107-05-1 TD (41), 76, 78
trans-1,2-Dichloroethene (TDCE) 156-60-5 TD (61), 96, 98
1,2-Dichloropropane 78-87-5 TD (63), 62, 76
1,4-Dioxane 123-91-1 TD (88), 58, 57
2-Ethyl-4-methyl-1,3-dioxolane 4359-46-0 TD (87), 59, 72
Chlorobenzene 108-90-7 TD (112), 77, 114
2-Butoxyethanol 111-76-2 TD (57), 87, 45
1,4-Dichlorobenzene 106-46-7 TD (146), 148, 111
Triethylenediamine (TEDA) 280-57-9 TD (58), 55, 112
1,2-Dichlorobenzene 95-50-1 TD (146), 148, 111
Bis(2-chloroisopropyl) ether 108-60-1 TD (45), 121, 77
Bis[2-(N,N-dimethylamino)ethyl] ether (BDMAEE) 3033-62-3 TD (58), 71, 42
Triethyl phosphate (TEP) 78-40-0 TD (99), 127, 155
Pentamethyldiethylenetriamine (PMDTA) 3030-47-5 TD (72), 58, 115
1,2-Dimethylimidazole 1739-84-0 TD (96), 54, 95
4-(1,1-Dimethylpropyl) phenol 80-46-6 TD (135), 107, 164
Tris(1-chloro-2-propyl) phosphate (TCPP) 13674-84-5 TD (99), 125, 157
Propionaldehyde 123-38-6 DNPH –
Formaldehyde 50-00-0 DNPH –
Acetaldehyde 75-07-0 DNPH –
ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference Materials, American Chemical Society, Washington, DC. For
suggestions on the testing of reagents not listed by the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and
the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D8142 − 23
raw material supplier if the primary chemical content is known. When compound purity is assayed to be 96 % or greater, the weight
may be used without correction to calculate the concentration of the stock standard. The target compounds of interest are
determined from specific VOCs and SVOCs that are known to be present or emit from the SPF formulation. An example list of
target compounds derived from a variety of SPF insulation samples is shown in Table 1.
NOTE 2—Toluene equivalents can be used to estimate non-target compounds, as described in California Department of Public Health Standard Method
for the Testing and Evaluation of Volatile Organic Chemical Emissions from Indoor Sources Using Environmental Chambers, CDPH/EHLB/Standard
Method V.1.2.
8.5.3 Dilution Solvent—Purge-and-trap grade methanol is used as the solvent to prepare calibration standards. It shall be of
chromatographic quality and free from compounds co-eluting with the compound or compounds of interest. Alternative dilution
solvents, for example, ethyl acetate or cyclohexane can be used, particularly if there is a possibility of reaction or chromatographic
co-elution with methanol.
8.5.4 Stock Standard Solutions—Prepare stock standard solutions in dilution solvent using assayed liquids or gases, as appropriate
at 2000 ng/μL or appropriate concentration. Place about 9 mL of methanol in a 10-mL10 mL tared ground-glass-stoppered
volumetric flask. Allow the flask to stand, un-stoppered, for about 10 minutesmin or until all the dilution solvent wetted surfaces
have dried. Weigh the flask to the nearest 0.0001 g. Add the assayed reference material, as described below.
8.5.4.1 Liquids—Using a syringe or pipette, immediately add one or more drops (0.02 g for 2000 ng/μL) of the reference material
to the flask; then reweigh. The liquid shall fall directly into the dilution solvent without contacting the neck of the flask. Very
volatile organic liquids (for example 1,1,1,3,3-pentafluoropropane) are placed in a freezer at –10°C to –20°C–10 °C to –20 °C prior
to preparation.
8.5.4.2 Gases—Solution Containing Approximately 11 mg mg/mL ⁄mL of Gas Components—For gases, prepare a low level
calibration solution as follows. Obtain pure gas at atmospheric pressure by filling a small plastic gas bag from a gas cylinder. Fill
a 1-mL1 mL gas-tight syringe with 1 mL of the pure gas and close the valve of the syringe. Using a 2-mL2 mL septum vial, add
2-mL2 mL solvent and close with the septum cap. Insert the tip of the syringe needle through the septum cap into the solvent. Open
the valve and withdraw the plunger slightly to allow the solvent to enter the syringe. The action of the gas dissolving creates a
vacuum, and the syringe fills with solvent. Return the solution to the flask. Flush the syringe twice with the solution and return
the washings to the flask. Calculate the mass of gas added using the gas laws, that is, 1 mol of gas at STP occupies 22.4 L.
8.5.5 Reweigh, dilute to volume, stopper, and then mix by inverting the flask several times. Calculate the concentration in mg/L
from the net gain in weight. The concentration in mg/L is equivalent to ng/μL.
8.5.6 Transfer the stock standard solution into a bottle with a PTFE-lined screw-cap. Store, with minimal headspace and protected
from light, at –10–10 °C to –20 °C. Return standards to the freezer as soon as the analyst has completed mixing or diluting the
standards to prevent evaporation of the solution.
8.5.7 Calibration Solutions—Following guidance given in Practice D6196, dilute the stock standards such that a 0.5 to 2-μL0.5 μL
to 2 μL injection, by means of the calibration solution loading rig introduces 2020 ng to 2000 ng of each compound, or an
alternative mass range if more appropriate to the samples being analyzed.
8.5.8 Internal Standards—Internal standards shall be used as described in U.S. EPA Compendium Method TO-17 or U.S. EPA
Method 325B. Gas-phase standards must be obtained in pressurized cylinders containing vendor certified gas concentrations
accurate to 65 %. The concentration shall be such that the masses of internal standard components introduced are similar to those
of the target compounds of this method. Alternatively, liquid solutions containing the internal standards can be loaded onto TD
tubes prior to analysis as described in 9.1.2. See Table X1.1 for an example of internal standards used for measuring SPF emissions.
8.6 Reagents and materials for the analysis of formaldehyde and other carbonyl compounds are described in Test Method D5197.
8.7 Analytical Balance and Containers:
8.7.1 Class A volumetric flasks for preparing standard solutions, as needed.
8.7.2 Analytical balance, readable and accurate to the nearest 0.1 mg.
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9. Calibration and Standardization
9.1 Thermal desorption GC/MS standard calibration curves are required for each compound of interest comprising at least five
points covering an applicable range and with a factor of at least 20 between the lowest and the highest level standard. At least six
points are used for quadratic fit calibration curves. The standard concentrations distribution shall not be greater than five times the
concentration of the next lower standard (for example; 20, 50, 100, 200, 500, 1000, 2000 ng). 20 ng, 50 ng, 100 ng, 200 ng, 500 ng,
1000 ng, 2000 ng). Prepare loaded tubes by injecting aliquots of standard solutions onto clean sorbent tubes as follows:
9.1.1 Fit the sampling end of the clean sorbent tube into the calibration solution loading rig (see 8.4.2) with a 50–10050 mL ⁄min
to 100 mL/min flow rate of inert purge gas and inject 0.5 to 2-μL0.5 μL to 2 μL aliquot of an appropriate standard solution through
the septum for 11 min to 5 minutes.min. Reproducible and quantitative transfer of higher boiling compounds in liquid standards
is facilitated if the injection unit allows the tip of the syringe to just touch the sorbent retaining gauze or quartz wool inside the
tube. If calibration tubes are to be prepared using multiple standards, introduce those containing the least volatile compounds of
interest first and the most volatile compounds of interest (typically the gas phase standards) last. See Practice D6196, 8.5, for
further information on loading TD sorbent tubes.
9.1.2 If a liquid solution is used to load internal standards, with 50–100 mL/min 50 mL/min to 100 mL/min flow rate of inert
purge gas, inject 1 μL of the internal standard solution though the septum of the calibration loading rig for 11 min to 5 minutes,min,
and then disconnect the tube and seal it using long-term storage caps.
9.1.3 Use the GC/MS data acquisition software to plot relative response factors for each compound. Use the average of response
factors for each compound if the relative standard deviation is ≤15 % or use a linear fit if the R value is ≥0.995, otherwise, a
quadratic fit calibration curve shall be used.
NOTE 3—Some reactive compounds such as amine catalysts used in SPF insulation may be non-linear. Use of a linear regression of the standard responses
does not eliminate the possibility of large systematic errors if the intercept value is large relative to the quantity being measured. Non-linearity can be
evaluated using statistical software or tested for lack of fit by examining the residuals described in the Analytical Methods Committee technical brief cited
in the bibliography.
9.1.4 Repeat multi-level calibration whenever the single-level calibration check falls outside the specified range specified in 15.7.
9.1.5 TCPP and its isomers elute as three peaks in the GC/MS chromatogram. In this case, integrate the sum of the areas of the
target ion from all three observed peaks and report as TCPP, total isomers. Manual integration may be necessary to integrate the
sum of areas from all three isomers.
9.2 Prepare reference standards and calibration curves for formaldehyde and other carbonyl compounds as described in Test
Method D5197.
9.3 Care must be taken to ensure that the calibration standards do not break through the sorbent material, or overload the column
or detector. The process of thermally desorbing sorbent tubes can be carried out split or splitless. Table X1.1 in the appendix gives
suggested split conditions; however the analyst may need to adjust the split flow (or lack thereof) to accommodate the sensitivity
needed or the capacity of the column, the detector or both.
10. Preparation of Apparatus
10.1 Cleaning Procedure:
10.1.1 Remove the gaskets or O-rings and clean the chamber components using a dilute alkaline detergent followed by three
separate rinses with distilled water. Alternately, clean the chamber components with methanol. Avoid abrasive cleaners or cleaners
that have a high pH. Dry thoroughly.
10.1.2 If the apparatus is designed to accommodate elevated temperature, the chamber can be cleaned without disassembly. Rinse
the chamber with methanol, and then raise the chamber temperature to 150 ºC°C or higher if necessary with elevated flow of clean
dry air sufficiently long to reduce background artifacts to acceptable levels at normal operating conditions.
10.2 Chamber Background Measurement:
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10.2.1 Measure background levels of each chamber prior to testing each set of samples. Background measurements are performed
under normal operating conditions but without a specimen in the chamber and evaluated for contamination as described in 15.5.
11. Preparation of Samples and Sample Collection
11.1 SPF insulation samples are sprayed and prepared for testing in a controlled spray booth or a field product installation site by
a trained applicator using professional spraying equipment under defined conditions. Spray samples to a minimum thickness
specified in Practice D7859.
11.2 Practice D7859 describes standardized procedures for the preparation, spraying, packaging, and shipping of SPF insulation
product samples to be tested for their emissions. In addition, the density of the sample can be determined as described in Test
Method D1622/D1622M.
11.3 To evaluate emissions from SPF insulation that already has been applied in a building, samples can be collected onsite. With
a clean knife or saw, cut out a representative section of material being careful not to damage the surface of the product. Collect
the entire applied thickness with minimum dimensions of 30 ×30 cm by 30 cm. In the situation where it is not feasible to collect
the entire thickness or a 30 × 30-cm30 cm by 30 cm sample, collect the maximum thickness possible with dimensions of
minimally, 10 ×10 cm by 10 cm. Upon collection, immediately, wrap the sample in clean aluminum foil and place the sample into
a layered polyethylene terephthalate (PET) food storage bag as described in Practice D7859.
11.4 Ship the samples in an insulated secondary container by means of overnight delivery as described in Practice D7859.
11.5 Upon receipt at the laboratory, note any damage to the shipping container or to the layered PET storage bag. If the storage
bag has been compromised, resampling is necessary; otherwise, if the sample cannot be re-sprayed or re-collected, qualify the
emissions data.
11.6 Prior to testing, the sample is stored in its original unopened layered PET bag at typical indoor conditions as described in
Practice D7859. During storage in the bag, protect the sample from chemical contamination and from exposure to temperatures
in excess of 25 °C. 25 °C. Do not refrigerate or place the sample in a freezer. Document the storage conditions (for example,
storage location and temperature).
11.7 Prepare the specimens and begin the chamber test within 48 h or sooner of spraying or sample collection to minimize
potential losses of VOCs as described in Practice D7859.
12. Specimen Preparation and Chamber Operation
12.1 Open the PET layered bag and prepare the specimen for chamber testing within 20 min as specified in Practice D7859.
Prepare duplicate specimens from each sample.
12.2 Using a fabricated circular steel coring tool described in Practice D7859, cut the specimen so that it fits tightly into the
chamber body to minimize gaps between the specimen and chamber wall. Open-cell SPF may require the use of cylindrical shim
rings to reduce gaps.
12.3 Collect specimens from the substrate material in a random fashion, but avoid taking specimens that are less than 3 cm from
the edge of the sample block. For open cell SPF insulation, trim ≤5 mm from the top surface top of the specimen, which will
provide a smoother surface and mimic trimming in the field to align with wall studs or other structural elements. Do not trim the
surface skin from closed-cell SPF insulation unless specified by the sample submitter. Record if the specimen surface is trimmed
or not.
12.4 If necessary, cut the bottom from the specimen so that the specimen height is approximately 30 mm and the headspace from
the surface of the specimen to the bottom surface of the chamber lid is 55 mm 6 2 mm so that the chamber lids do not touch the
surface of the specimens. Use spacers to elevate the sample to the proper height in the micro-scale chamber if the specimen is not
thick enough to fill the chamber to the height needed to achieve the required headspace distance.
D8142 − 23
12.5 Weigh the SPF specimen to the nearest milligram and record the mass.
12.6 Carefully, insert the specimen into the chamber cavity with the outer surface side facing up; place the O-ring or gasket on
the micro-scale chamber. Photograph the specimens prior to closing and sealing the chamber lid.
12.7 Turn on the air supply and adjust the flow rate to achieve an area specific flow rate between 0.9 m/h and 1.0 m/hr.m/h. This
can be done by adjusting the flow rate to 50 mL/min for micro-scale chambers with an inner diameter of 6.4 cm, or adjusting the
flow rate to 100 mL/min for micro-scale chambers with an inner diameter of 9.2 cm. Other sized micro-scale chambers can be used,
but the flow rate shall not exceed 150 150 mL mL/min.⁄min.
12.8 Record the date and time the test is initiated, t . Check the airflow rate at the chamber exhaust as described in Practice D5337.
Record the flow rates. Maintain the supply of air to the micro-scale chamber continuously for the entire duration of the test (all
of the time that the specimen is in the micro-scale chamber).
12.9 Operate the micro-scale chamber at 35 6 1 °C 35 °C 6 1 °C throughout the duration of the test. Record the instrument
displayed operating temperature each time a sample is collected.
12.10 Begin collecting emissions samples after 2 h from t .
NOTE 4—TCPP and other semi-volatile compounds may take much longer than 2 h to reach a quasi-steady state; therefore, emission measurements of
these compounds should only be used for informative purposes at 2 h. For example, these values can be used to determine how long to collect emission
samples from the micro-scale chambers.
12.11 Collecting Organic Vapors from the Exhaust Gas of the Emission Chambers:
12.11.1 To initiate collection of an air sample from the micro-scale chamber, connect a clean media cartridge or tube to the outlet
port of the chamber using an appropriate O-ring to achieve a leak-free seal. No sampling pump is necessary as flow exhausts out
of the chamber sampling port directly into the inlet of a connected media cartridge or tube. Once the media is connected, the gas
sampling is initiated. Re-check the airflow rate at the exhaust of the media cartridge and verify the system is leak free (7.4.4). For
each sample, record the date and time that sampling is initiated. Also record the airflow rate and the time duration of gas sample
collection.
12.11.2 Thermal desorption (TD) sorbent tubes can be collected over times ranging from a few minutes up to 2.5 h depending on
the expected emissions. Be careful not to exceed the safe sampling volumes with TD tubes for each compound under the test
conditions. At the end of the sampling period, disconnect the sorbent tube from the outlet of the chamber. Seal the sorbent tube
using appropriate fittings.
12.11.3 If a liquid solution is used to load
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