ASTM D6561-20
(Test Method)Standard Test Method for Determination of Aerosol Monomeric and Oligomeric Hexamethylene Diisocyanate (HDl) in Air with (Methoxy-2–phenyl-1) Piperazine (MOPIP) in the Workplace
Standard Test Method for Determination of Aerosol Monomeric and Oligomeric Hexamethylene Diisocyanate (HDl) in Air with (Methoxy-2–phenyl-1) Piperazine (MOPIP) in the Workplace
SIGNIFICANCE AND USE
5.1 HDI is mostly used in the preparation of paints. The use of isocyanates and their industrial needs have been in constant growth.
5.2 Diisocyanates and polyisocyanates are irritants to skin, eyes, and mucous membranes. They are recognized to cause respiratory allergic sensitization, asthmatic bronchitis, and acute respiratory intoxication (3-6).
5.3 The American Conference of Governmental Industrial Hygienists (ACGIH) has adopted a threshold limit value–time weighted average (TLV-TWA) of 0.005 ppm (V) or 0.034 mg/m3 for monomeric HDI (7). The Occupational Safety & Health Administration of the U.S. Department of Labor (OSHA) has not listed a permissible exposure limit (PEL) for HDI (8).
5.4 In any case, there are not separate exposure standards for vapor and aerosol. Therefore, in comparing the results for isocyanate against a standard, results from the two fractions should be combined to give a single total value.
5.5 Due to its low LOD and low required volume (15 L), this test method is well suited for monitoring of respiratory and other problems related to diisocyanates and polyisocyanates. Its short sampling times are compatible with the duration of many industrial processes, and its low detection limit with the concentrations often found in the working area.
SCOPE
1.1 This test method covers the determination of aerosol hexamethylene diisocyanate (HDI) in air samples collected from workplace and ambient atmospheres. The method described in this test method collects separate fractions. One fraction will be dominated by vapor, and the other fraction will be dominated by aerosol. The results obtained from the analysis of the separate fractions do not necessarily represent the true partition of the measured HDI physical phases, and should only be considered a representation of the general trend in the physical phase partition within samples. The analyses of the two fractions are different, and are provided in separate, linked, standards to avoid confusion. This test method is principally used to determine short term exposure (15 min) of HDI in workplace environments for personal monitoring or in ambient air. The analysis of the vapor fraction is performed separately, as described in Test Method D6562.
1.2 Differential air sampling is performed with a segregating device. The aerosol fraction is collected on a polytetrafluoroethylene (PTFE) filter.
1.3 The analysis of the aerosol fraction is performed by using a high performance liquid chromatograph (HPLC) equipped with an ultraviolet (UV) detector. An ultra high performance liquid chromatograph (UPLC) can also be used, provided that its performance is equivalent to what is stated in this standard. The range of application of the test method has been validated from 0.052 to 1.04 μg of monomeric HDI/mL, which corresponds, based on a 15 L air sample, to concentrations from 0.004 to 0.070 mg/m3 of HDI. Those concentrations correspond to a range of aerosol phase concentrations from 0.5 ppb (V) to 10 ppb (V) and cover the established threshold limit valve (TLV) value of 5 ppb (V).
1.4 The quantification limit for the monomeric HDI is 0.041 μg per mL, which corresponds to 0.003 mg/m3 for a 15 L sampled air volume. This value is equivalent to ten times the standard deviation obtained from ten measurements carried out on a standard solution in contact with the PTFE filter whose concentration of 0.1 μg/mL is close to the expected detection limit.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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. See Section 9 for additional hazards.
1.7 This intern...
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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: D6561 − 20
Standard Test Method for
Determination of Aerosol Monomeric and Oligomeric
Hexamethylene Diisocyanate (HDl) in Air with (Methoxy-
1
2–phenyl-1) Piperazine (MOPIP) in the Workplace
This standard is issued under the fixed designation D6561; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope sampled air volume. This value is equivalent to ten times the
standarddeviationobtainedfromtenmeasurementscarriedout
1.1 This test method covers the determination of aerosol
on a standard solution in contact with the PTFE filter whose
hexamethylene diisocyanate (HDI) in air samples collected
concentration of 0.1 µg/mL is close to the expected detection
from workplace and ambient atmospheres. The method de-
limit.
scribed in this test method collects separate fractions. One
fractionwillbedominatedbyvapor,andtheotherfractionwill 1.5 The values stated in SI units are to be regarded as
be dominated by aerosol. The results obtained from the standard. No other units of measurement are included in this
analysis of the separate fractions do not necessarily represent standard.
the true partition of the measured HDI physical phases, and
1.6 This standard does not purport to address all of the
shouldonlybeconsideredarepresentationofthegeneraltrend
safety concerns, if any, associated with its use. It is the
in the physical phase partition within samples.The analyses of
responsibility of the user of this standard to establish appro-
the two fractions are different, and are provided in separate,
priate safety, health, and environmental practices and deter-
linked, standards to avoid confusion. This test method is
mine the applicability of regulatory limitations prior to use.
principally used to determine short term exposure (15 min) of
See Section 9 for additional hazards.
HDI in workplace environments for personal monitoring or in
1.7 This international standard was developed in accor-
ambient air. The analysis of the vapor fraction is performed
dance with internationally recognized principles on standard-
separately, as described in Test Method D6562.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
1.2 Differential air sampling is performed with a segregat-
mendations issued by the World Trade Organization Technical
ing device.The aerosol fraction is collected on a polytetrafluo-
Barriers to Trade (TBT) Committee.
roethylene (PTFE) filter.
1.3 The analysis of the aerosol fraction is performed by
2. Referenced Documents
using a high performance liquid chromatograph (HPLC)
2
2.1 ASTM Standards:
equipped with an ultraviolet (UV) detector. An ultra high
D1193Specification for Reagent Water
performance liquid chromatograph (UPLC) can also be used,
D1356Terminology Relating to Sampling and Analysis of
provided that its performance is equivalent to what is stated in
Atmospheres
this standard. The range of application of the test method has
D1357Practice for Planning the Sampling of the Ambient
been validated from 0.052 to 1.04 µg of monomeric HDI/mL,
Atmosphere
which corresponds, based on a 15 L air sample, to concentra-
3
D4840Guide for Sample Chain-of-Custody Procedures
tionsfrom0.004to0.070mg/m ofHDI.Thoseconcentrations
D5337Practice for Flow RateAdjustment of Personal Sam-
correspondtoarangeofaerosolphaseconcentrationsfrom0.5
pling Pumps
ppb(V)to10ppb(V)andcovertheestablishedthresholdlimit
D6562Test Method for Determination of Gaseous Hexam-
valve (TLV) value of 5 ppb (V).
ethylene Diisocyanate (HDI) in Air with 9-(N-
1.4 ThequantificationlimitforthemonomericHDIis0.041
3 methylaminomethyl)Anthracene Method (MAMA) in the
µg per mL, which corresponds to 0.003 mg/m fora15L
Workplace
1
This test method is under the jurisdiction of ASTM Committee D22 on Air
Quality and is the direct responsibility of Subcommittee D22.04 on WorkplaceAir
2
Quality. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved March 1, 2020. Published May 2020. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2000. Last previous edition approved in 2016 as D6561–06 (2016). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D6561-20. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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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.
Designation: D6561 − 06 (Reapproved 2016) D6561 − 20
Standard Test Method for
Determination of Aerosol Monomeric and Oligomeric
Hexamethylene Diisocyanate (HDl) in Air with (Methoxy-
1
2–phenyl-1) Piperazine (MOPIP) in the Workplace
This standard is issued under the fixed designation D6561; 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
1.1 This test method covers the determination of aerosol hexamethylene diisocyanate (HDI) in air samples collected from
workplace and ambient atmospheres. The method described in this test method collects separate fractions. One fraction will be
dominated by vapor, and the other fraction will be dominated by aerosol. It is not known at the present time whether this represents
a perfect separation of vapor and aerosol, and in any case, there are not separate exposure standards for vapor and aerosol.
Therefore, in comparing the results for isocyanate against a standard, results from the two fractions should be combined to give
a single total value. The reason for splitting the sample into two fractions is to increase analytic sensitivity for the vapor fraction
and also to give the hygienist or ventilation engineer some information concerning the likely state of the isocyanate species. The
results obtained from the analysis of the separate fractions do not necessarily represent the true partition of the measured HDI
physical phases, and should only be considered a representation of the general trend in the physical phase partition within samples.
The analyses of the two fractions are different, and are provided in separate, linked, standards to avoid confusion. This test method
is principally used to determine short term exposure (15 min) of HDI in workplace environments for personal monitoring or in
ambient air. The analysis of the vapor fraction is performed separately, as described in Test Method D6562.
1.2 Differential air sampling is performed with a segregating device. The aerosol fraction is collected on a polytetrafluoroeth-
ylene (PTFE) filter.
1.3 Immediately after sampling, the PTFE filter is transferred into a jar containing a (methoxy-2 phenyl-1) piperazine (MOPIP)
solution in toluene.
1.3 The analysis of the aerosol fraction is performed by using a high performance liquid chromatograph (HPLC) equipped with
an ultraviolet (UV) detector. An ultra high performance liquid chromatograph (UPLC) can also be used, provided that its
performance is equivalent to what is stated in this standard. The range of application of the test method has been validated from
0.052 to 1.04 μg of monomeric HDI/mL, which corresponds, based on a 15 L air sample, to concentrations from 0.004 to 0.070
3
mg/m of HDI. Those concentrations correspond to a range of aerosol phase concentrations from 0.5 ppb (V) to 10 ppb (V) and
cover the established threshold limit valve (TLV) value of 5 ppb (V).
3
1.4 The quantification limit for the monomeric HDI is 0.041 μg per mL, which corresponds to 0.003 mg/m for a 15 L sampled
air volume. This value is equivalent to ten times the standard deviation obtained from ten measurements carried out on a standard
solution in contact with the PTFE filter whose concentration of 0.1 μg/mL is close to the expected detection limit.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. See Section 9 for additional hazards.
1.7 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.
1
This test method is under the jurisdiction of ASTM Committee D22 on Air Quality and is the direct responsibility of Subcommittee D22.04 on Workplace Air Quality.
Current edition approved Nov. 1, 2016March 1, 2020. Published November 2016May 2020. Originally approved
...
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