ASTM D6562-12
(Test Method)Standard Test Method for Determination of Gaseous Hexamethylene Diisocyanate (HDI) in Air with 9-(N-methylaminomethyl) Anthracene Method (MAMA) in the Workplace
Standard Test Method for Determination of Gaseous Hexamethylene Diisocyanate (HDI) in Air with 9-(N-methylaminomethyl) Anthracene Method (MAMA) in the Workplace
SIGNIFICANCE AND USE
HDI is mostly used in the preparation of paints. For the last ten years, the use of isocyanates and their industrial needs have been in constant growth.
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 (4-7).
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 (8). The Occupational Safety & Health Administration of the U.S. Department of Labor (OSHA) has not listed a permissible exposure limit (PEL) for HDI (9).
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 gaseous 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 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 aerosol fraction is performed separately, as described in Test Method D6561.
1.2 Differential air sampling is performed with a segregating device. The vapor fraction is collected on a glass fiber filter (GFF) impregnated with 9-(N-methylaminomethyl) anthracene (MAMA).
1.3 The analysis of the gaseous fraction is performed with a high performance liquid chromatograph (HPLC) equipped with ultraviolet (UV) and fluorescence detectors.
1.4 The range of application of this test method, using UV and fluorescence detectors both connected in serial, has been validated from 0.006 to 1.12 μg of monomeric HDI/2.0 mL of desorption solution, which corresponds to concentrations equivalent to 0.0004 to 0.075 mg/m3 of HDI based on a 15-L air sample. Those concentrations correspond to a range of vapor phase concentrations from 0.06 ppb(V) to 11 ppb(V) and cover the established threshold limit value (TLV) value of 5 ppb(V).
1.5 The quantification limit for the monomeric HDI, using the UV detection, has been established as 0.012 μg/2 mL of desorption solution and as 0.008 μg/2 mL, using the fluorescence detector. These limits correspond to 0.0008 mg/m3 and 0.0005 mg/m3 respectively for an air sampled volume of 15 L. These values are equal to ten times the standard deviation (SD) obtained from ten measurements carried out on a standard solution in contact with the GFF, whose concentration of 0.02 μg/2 mL is close to the expected detection limit.
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 and health practices and determine the applicability of regu...
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Designation: D6562 − 12
Standard Test Method for
Determination of Gaseous Hexamethylene Diisocyanate
(HDI) in Air with 9-(N-methylaminomethyl) Anthracene
1
Method (MAMA) in the Workplace
This standard is issued under the fixed designation D6562; 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 1.4 The range of application of this test method, using UV
and fluorescence detectors both connected in serial, has been
1.1 This test method covers the determination of gaseous
validated from 0.006 to 1.12 µg of monomeric HDI/2.0 mL of
hexamethylene diisocyanate (HDI) in air samples collected
desorption solution, which corresponds to concentrations
from workplace and ambient atmospheres. The method de-
3
equivalent to 0.0004 to 0.075 mg/m of HDI based on a 15-L
scribed in this test method collects separate fractions. One
air sample. Those concentrations correspond to a range of
fraction will be dominated by vapor, and the other fraction will
vapor phase concentrations from 0.06 ppb(V) to 11 ppb(V) and
be dominated by aerosol. It is not known at the present time
cover the established threshold limit value (TLV) value of 5
whether this represents a perfect separation of vapor and
ppb(V).
aerosol, and in any case, there are not separate exposure
1.5 The quantification limit for the monomeric HDI, using
standards for vapor and aerosol. Therefore, in comparing the
the UV detection, has been established as 0.012 µg/2 mL of
results for isocyanate against a standard, results from the two
desorption solution and as 0.008 µg/2 mL, using the fluores-
fractions should be combined to give a single total value. The
3
cence detector. These limits correspond to 0.0008 mg/m and
reason for splitting the sample into two fractions is to increase
3
0.0005 mg/m respectively for an air sampled volume of 15 L.
analytic sensitivity for the vapor fraction and also to give the
These values are equal to ten times the standard deviation (SD)
hygienist or ventilation engineer some information concerning
obtained from ten measurements carried out on a standard
the likely state of the isocyanate species. The analyses of the
solution in contact with the GFF, whose concentration of 0.02
twofractionsaredifferent,andareprovidedinseparate,linked,
µg/2 mL is close to the expected detection limit.
standards to avoid confusion. This test method is principally
used to determine short term exposure (15 min) of HDI in
1.6 This standard does not purport to address all of the
workplace environments for personal monitoring or in ambient
safety concerns, if any, associated with its use. It is the
air.Theanalysisoftheaerosolfractionisperformedseparately,
responsibility of the user of this standard to establish appro-
as described in Test Method D6561.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. See Section 9 for
1.2 Differential air sampling is performed with a segregat-
2
additional hazards.
ing device. The vapor fraction is collected on a glass fiber
filter (GFF) impregnated with 9-(N-methylaminomethyl) an-
2. Referenced Documents
thracene (MAMA).
3
2.1 ASTM Standards:
1.3 The analysis of the gaseous fraction is performed with a
D1193 Specification for Reagent Water
high performance liquid chromatograph (HPLC) equipped
D1356 Terminology Relating to Sampling and Analysis of
with ultraviolet (UV) and fluorescence detectors.
Atmospheres
D1357 Practice for Planning the Sampling of the Ambient
Atmosphere
1
This test method is under the jurisdiction of ASTM Committee D22 on Air D5337 Practice for Flow RateAdjustment of Personal Sam-
Qualityand is the direct responsibility of Subcommittee D22.04 on Workplace Air
pling Pumps
Quality.
D6561 Test Method for Determination of Aerosol Mono-
Current edition approved April 1, 2012. Published May 2012. Originally
mericandOligomericHexamethyleneDiisocyanate(HDl)
approved in 2000. Last previous edition approved in 2011 as D6562 – 06 (2011).
DOI: 10.1520/D6562-12.
2
The sampling device for isocyanates is covered by a patent held by Jacques
3
Lesage et al, IRSST, 505 De Maisonneuve Blvd. West, Montreal, Quebec, Canada. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
If you are aware of an alternative to this patented item, please provide this contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
information to ASTM Headquarters. Your comments will receive careful consider- Standards volume information, refer to the standard’s Document Summary page on
1
ation at a meeting of the responsible technical committee, whi
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D6562–06 (Reapproved 2011) Designation:D6562–12
Standard Test Method for
Determination of Gaseous Hexamethylene Diisocyanate
(HDI) in Air with 9-(N-methylaminomethyl) Anthracene
1
Method (MAMA) in the Workplace
This standard is issued under the fixed designation D6562; 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 gaseous 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
dominatedbyvapor,andtheotherfractionwillbedominatedbyaerosol.Itisnotknownatthepresenttimewhetherthisrepresents
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
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 aerosol fraction is performed separately, as described in Test Method D6561.
2
1.2 Differentialairsamplingisperformedwithasegregatingdevice. Thevaporfractioniscollectedonaglassfiberfilter(GFF)
impregnated with 9-(N-methylaminomethyl) anthracene (MAMA).
1.3 The analysis of the gaseous fraction is performed with a high performance liquid chromatograph (HPLC) equipped with
ultraviolet (UV) and fluorescence detectors.
1.4 The range of application of this test method, using UV and fluorescence detectors both connected in serial, has been
validated from 0.006 to 1.12 µg of monomeric HDI/2.0 mLof desorption solution, which corresponds to concentrations equivalent
3
to 0.0004 to 0.075 mg/m of HDI based on a 15-L air sample. Those concentrations correspond to a range of vapor phase
concentrations from 0.06 ppb(V) to 11 ppb(V) and cover the established threshold limit value (TLV) value of 5 ppb(V).
1.5 The quantification limit for the monomeric HDI, using the UV detection, has been established as 0.012 µg/2 mL of
3
desorption solution and as 0.008 µg/2 mL, using the fluorescence detector. These limits correspond to 0.0008 mg/m and 0.0005
3
mg/m respectively for an air sampled volume of 15 L. These values are equal to ten times the standard deviation (SD) obtained
from ten measurements carried out on a standard solution in contact with the GFF, whose concentration of 0.02 µg/2 mL is close
to the expected detection limit.
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 and health practices and determine the applicability of regulatory
limitations prior to use. See Section 9 for additional hazards.
2. Referenced Documents
3
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D1356 Terminology Relating to Sampling and Analysis of Atmospheres
D1357 Practice for Planning the Sampling of the Ambient Atmosphere
D5337 Practice for Flow Rate Adjustment of Personal Sampling Pumps
D6561 Test Method for Determination ofAerosol Monomeric and Oligomeric Hexamethylene Diisocyanate (HDl) inAir with
(Methoxy-2phenyl-1) Piperazine (MOPIP) in the 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 Workplace Air Quality.
Current edition approved Oct.April 1, 2011.2012. Published October 2011.May 2012. Originally approved in 2000. Last previous edition approved in 20062011 as
D6562 - 06(2011). DOI: 10.1520/D6562-06R11.10.1520/D6562-12.
2
The sampling device for isocyanates is covered by a patent held by Jacques Lesage et al, IRSST, 505 De Maisonneuve Blvd. West, Montreal, Quebec, Canada.Ifyou
are aware of an alternative to this patented item, p
...
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