ASTM D6060-96(2009)
(Practice)Standard Practice for Sampling of Process Vents With a Portable Gas Chromatograph
Standard Practice for Sampling of Process Vents With a Portable Gas Chromatograph
SIGNIFICANCE AND USE
This practice has been widely used to obtain mass balance data for process scrubbers, to determine the efficiency of VOC emission control equipment, and to obtain data to support air permit applications.
This practice will have applications to the MACT Rule and may have applications to Compliance Assurance Monitoring verification required by the 1990 Clean Air Act Title III Amendments.
This practice, when used with Test Methods D3464 or D3154 or on-line process flow meter data, can be used to calculate detailed emission rate profiles for VOCs from process vents.
This practice provides nearly real time results that can detect process changes or upsets that may be missed using conventional sorbent tube or integrated gas sampling bag sampling.
SCOPE
1.1 This practice describes a method for direct sampling and analysis of process vents for volatile organic compound (VOC) vapors and permanent gases using a portable gas chromatograph (GC).
1.2 This practice is applicable to analysis of permanent gases such as oxygen (O2), carbon dioxide (CO2) and nitrogen (N2), as well as vapors from organic compounds with boiling points up to 125°C.
1.3 The detection limits obtained will depend on the portable gas chromatograph and detector used. Detectors available include thermal conductivity, photoionization, argon ionization, and electron capture. For instruments equipped with thermal conductivity detectors, typical detection limits are one to two parts per million by volume (ppm(v)) with an applicable concentration range to high percent by volume levels. For instruments with photoionization detectors detection limit of one to ten parts per billion by volume (ppb(v)) are obtainable with a concentration range from 1000 to 2000 ppm(v). The argon ionization detector has an achievable detection limit of one (ppb(v)), while the electron capture detector has an achievable detection limit of one part per trillion by volume (ppt(v)) for chlorinated compounds.
1.4 The applicability of this practice should be evaluated for each VOC by determining stability, reproducibility, and linearity.
1.5 The appropriate concentration range must also be determined for each VOC, as the range will depend on the vapor pressure of the particular VOC.
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. Refer to Section 8 on Hazards for additional safety precautions.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D6060 − 96 (Reapproved 2009)
Standard Practice for
Sampling of Process Vents with a Portable Gas
Chromatograph
This standard is issued under the fixed designation D6060; 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 1.7 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 Thispracticedescribesamethodfordirectsamplingand
ization established in the Decision on Principles for the
analysisofprocessventsforvolatileorganiccompound(VOC)
Development of International Standards, Guides and Recom-
vapors and permanent gases using a portable gas chromato-
mendations issued by the World Trade Organization Technical
graph (GC).
Barriers to Trade (TBT) Committee.
1.2 This practice is applicable to analysis of permanent
gases such as oxygen (O ), carbon dioxide (CO ) and nitrogen
2. Referenced Documents
2 2
(N ), as well as vapors from organic compounds with boiling
2.1 ASTM Standards:
points up to 125°C.
D1356Terminology Relating to Sampling and Analysis of
1.3 The detection limits obtained will depend on the por-
Atmospheres
tablegaschromatographanddetectorused.Detectorsavailable
D3154Test Method for Average Velocity in a Duct (Pitot
include thermal conductivity, photoionization, argon
Tube Method)
ionization,andelectroncapture.Forinstrumentsequippedwith D3464Test Method forAverage Velocity in a Duct Using a
thermal conductivity detectors, typical detection limits are one
Thermal Anemometer
totwopartspermillionbyvolume(ppm(v))withanapplicable E355PracticeforGasChromatographyTermsandRelation-
concentration range to high percent by volume levels. For
ships
instruments with photoionization detectors detection limit of
2.2 Other Document:
one to ten parts per billion by volume (ppb(v)) are obtainable
NFPA496 Standard for Purged and Pressurized Enclosures
with a concentration range from 1000 to 2000 ppm(v). The
for Electrical Equipment
argon ionization detector has an achievable detection limit of
one (ppb(v)), while the electron capture detector has an 3. Terminology
achievable detection limit of one part per trillion by volume
3.1 Definitions—For the definition of terms used in this
(ppt(v)) for chlorinated compounds.
practice, refer to Terminology D1356 and Practice E355.
3.2 Definitions of Terms Specific to This Standard:
1.4 Theapplicabilityofthispracticeshouldbeevaluatedfor
3.2.1 portable—refers to gas chromatograph with internal
eachVOC by determining stability, reproducibility, and linear-
battery,internalsamplepump,andinternal/rechargeablecarrier
ity.
gas supply cylinder.
1.5 The appropriate concentration range must also be deter-
mined for each VOC, as the range will depend on the vapor
4. Summary of Practice
pressure of the particular VOC.
4.1 One end of a sampling line (typically 6 mm ( ⁄4 in.)
1.6 This standard does not purport to address all of the
outside diameter TFE-fluorocarbon tubing) is connected to a
safety concerns, if any, associated with its use. It is the
tee in a process vent and the other end to a condensation trap
responsibility of the user of this standard to establish appro-
(see6.1),whichisconnectedtoagassamplingbulb.Theoutlet
priate safety and health practices and determine the applica-
of the gas sampling bulb is connected to a sampling pump set
bility of regulatory limitations prior to use. Refer to Section 8
at a flow rate of 0.5 to 2 L/min. The sample line from the
on Hazards for additional safety precautions.
1 2
This test method is under the jurisdiction of ASTM Committee D22 on Air For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Quality and is the direct responsibility of Subcommittee D22.03 on Ambient contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Atmospheres and Source Emissions. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Oct. 1, 2009. Published December 2009. Originally the ASTM website.
approved in 1996. Last previous edition approved in 2001 as D6060–96 (2001). Available from National Fire Protection Association (NFPA), 1 Batterymarch
DOI: 10.1520/D6060-96R09. Park, Quincy, MA 02169-7471, http://www.nfpa.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6060 − 96 (2009)
portablegaschromatographisinsertedthroughtheseptumport toprotecttheportablegaschromatographifliquidsarepresent
ofthegassamplingbulb.Atuserselectedintervals,theinternal or occur during process upset.
pump of the portable gas chromatograph is activated and
6.2 Interferences sometimes result from analytes having
process vapors drawn through the injection valve of the gas
similar retention times during gas chromatography.
chromatograph and analyzed.
6.3 General approaches which can be followed to resolve
such interferences are given below:
5. Significance and Use
6.3.1 Change the type of column, length of column, or
5.1 This practice has been widely used to obtain mass
operating conditions.
balance data for process scrubbers, to determine the efficiency
6.3.2 Analyze using a nonpolar methyl silicone column
of VOC emission control equipment, and to obtain data to
which separates according to boiling point of the compounds
support air permit applications.
and a polar column whose separations are influenced by the
5.2 This practice will have applications to the MACT Rule
polarity of the compounds.
and may have applications to ComplianceAssurance Monitor-
6.3.3 Use a mass spectrometer to verify the identity of
ing verification required by the 1990 Clean Air Act Title III
peaks.
Amendments.
7. Apparatus
5.3 This practice, when used with Test Methods D3464 or
D3154 or on-line process flow meter data, can be used to 7.1 A schematic drawing of a typical sampling setup is
calculatedetailedemissionrateprofilesforVOCsfromprocess
shown in Fig. 1. The laptop computer may be physically
vents. located near the gas chromatograph as shown in Fig. 1,or
located remotely. In addition, some portable gas chromato-
5.4 This practice provides nearly real time results that can
graphs have an integral computer. Use a short piece of 1.5 mm
detect process changes or upsets that may be missed using
( ⁄16 in.) outside diameter by 1 mm (0.04 in.) inside diameter
conventional sorbent tube or integrated gas sampling bag
stainless steel tubing as the sampling probe line from the gas
sampling.
sampling bulb to the GC inlet.
6. Interferences
6.1 Water or liquid in the process line will plug the sample
Thecolumnsinmostportablegaschromatographsareeasilyinterchanged.One
lineofthegaschromatograph,sincetheinjectionvalveofmost
manufacturer has an instrument that simultaneously injects onto two user selected
portable GCs is not heated. The condensation trap is designed column modules.
FIG. 1 Schematic of Process Sampling Equipment
D6060 − 96 (2009)
7.2 Portable Gas Chromatograph (GC), with a thermal pected concentrations of each component in the testing of the
conductivity, photoionization, argon ionization, electron cap- process vent, if known.
ture or appropriate detector, internal/rechargeable carrier gas 9.3.1 Connect the gas sampling bag to the inlet or the
supply, and internal sampling pump. calibration port of the GC and initiate the analysis. Perform at
7.2.1 Portable gas chromatographs are typically equipped least triplicate injections of each standard.
with particulate filters which should be replaced periodically. 9.3.2 The quantitative response of a GC detector may be
determinedbythemeasurementofthepeakheightorpeakarea
7.3 Data Logger, device used for automated storage of
using the Data System or electronic integrator.
output from a flow measurement device.
9.3.3 Following the standard analyze a gas sampling bag
7.4 Gas Sampling Bulb, 125 mLcapacity with septum port.
containing air only (blank). If carryover is >1% increase the
sampling period (internal GC pump time). Typical sampling
7.5 Personal Sampling Pump.
periods are 20 to 45 s, however, this parameter must be
7.6 Gas-Tight Syringe, 1, 10, 100, 500 mLcapacity or other
optimized for each VOC analyzed.
convenient sizes for preparing standards.
7.7 Microlitre Syringes, 10, 25, 50, 100 µL or other conve- 10. Procedure
nient sizes for preparing standards.
10.1 Preparation of the Gas Chromatograph:
7.8 Gas Sampling Bags, for preparation of gas standards. 10.1.1 Fill the internal carrier gas reservoir as described by
Bags constructed of various polymer films, such as polyvi- the manufacturer.
nylidene fluoride, fluorinated ethylenepropylene, 10.1.2 Select a carrier gas flow or column pressure and
(tetrafluoroethylene)-fluorocarbon, polyvinylidene chloride, column temperature compatible with the column selected for
polyethylene and mixed polymer multilayers, with a variety of the separation.
fittings and capacities (typically 1 to 200 L) are available. 10.1.3 Calibrate the chromatographic column to determine
the relative retention times and response of the various
7.9 ThermalAnemometer,VaneAnemometer,MassFlowme-
compounds of interest.
ter or Pitot Tube, for measurement of vent velocity.
10.2 Preparation of the Sampling Train:
7.10 Condensation Trap, Filtering Flask, 250 or 500 mL
10.2.1 Assemble the sampling train as shown in Fig. 1.
polypropylene fitted with a stopper.
Stainless steel or glass may be substituted for the TFE-
7.11 TFE-Fluorocarbon Tubing, 6mm( ⁄4 in.) outside
fluorocarbon t
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