ASTM D6060-96(2001)

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 D 3464 or D 3154 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.

General Information

• Status: Historical
• Publication Date: 09-Dec-1996
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: D22 - Air Quality
• Drafting Committee: D22.03 - Ambient Atmospheres and Source Emissions

Relations

• Replaces: ASTM D6060-96 - Standard Practice for Sampling of Process Vents With a Portable Gas Chromatograph
• Effective Date: 10-Dec-1996
• Replaced By: ASTM D6060-96(2009) - Standard Practice for Sampling of Process Vents With a Portable Gas Chromatograph
• Effective Date: 01-Oct-2009

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information.
Designation:D6060–96 (Reapproved 2001)
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 2. Referenced Documents
1.1 Thispracticedescribesamethodfordirectsamplingand 2.1 ASTM Standards:
analysisofprocessventsforvolatileorganiccompound(VOC) D1356 Terminology Relating to Sampling and Analysis of
vapors and permanent gases using a portable gas chromato- Atmospheres
graph (GC). D3464 Test Method forAverageVelocity in a Duct Using a
1.2 This practice is applicable to analysis of permanent Thermal Anemometer
gases such as oxygen (O ), carbon dioxide (CO ) and nitrogen D3154 Test Method for Average Velocity in a Duct (Pitot
2 2
(N ), as well as vapors from organic compounds with boiling Tube Method)
points up to 125°C. E355 Practice for Gas Chromatography Terms and Rela-
1.3 The detection limits obtained will depend on the por- tionships
tablegaschromatographanddetectorused.Detectorsavailable 2.2 Other Document:
include thermal conductivity, photoionization, argon ioniza- NFPA496 Standard for Purged and Pressurized Enclosures
tion, and electron capture. For instruments equipped with for Electrical Equipment
thermal conductivity detectors, typical detection limits are one
3. Terminology
totwopartspermillionbyvolume(ppm(v))withanapplicable
concentration range to high percent by volume levels. For 3.1 Definitions—For the definition of terms used in this
practice, refer to Terminology D1356 and Practice E355.
instruments with photoionization detectors detection limit of
one to ten parts per billion by volume (ppb(v)) are obtainable 3.2 Definitions of Terms Specific to This Standard:
3.2.1 portable—refers to gas chromatograph with internal
with a concentration range from 1000 to 2000 ppm(v). The
battery,internalsamplepump,andinternal/rechargeablecarrier
argon ionization detector has an achievable detection limit of
one (ppb(v)), while the electron capture detector has an gas supply cylinder.
achievable detection limit of one part per trillion by volume
4. Summary of Practice
(ppt(v)) for chlorinated compounds.
4.1 One end of a sampling line (typically 6 mm ( ⁄4 in.)
1.4 Theapplicabilityofthispracticeshouldbeevaluatedfor
outside diameter TFE-fluorocarbon tubing) is connected to a
eachVOC by determining stability, reproducibility, and linear-
tee in a process vent and the other end to a condensation trap
ity.
(see6.1),whichisconnectedtoagassamplingbulb.Theoutlet
1.5 The appropriate concentration range must also be deter-
of the gas sampling bulb is connected to a sampling pump set
mined for each VOC, as the range will depend on the vapor
at a flow rate of 0.5 to 2 L/min. The sample line from the
pressure of the particular VOC.
portablegaschromatographisinsertedthroughtheseptumport
1.6 This standard does not purport to address all of the
ofthegassamplingbulb.Atuserselectedintervals,theinternal
safety concerns, if any, associated with its use. It is the
pump of the portable gas chromatograph is activated and
responsibility of the user of this standard to establish appro-
process vapors drawn through the injection valve of the gas
priate safety and health practices and determine the applica-
chromatograph and analyzed.
bility of regulatory limitations prior to use. Refer to Section 8
on Hazards for additional safety precautions.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This test method is under the jurisdiction of ASTM Committee D22 on contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Sampling andAnalysis ofAtmospheres and is the direct responsibility of Subcom- Standards volume information, refer to the standard’s Document Summary page on
mittee D22.03 on Ambient Atmospheres and Source Emissions. the ASTM website.
Current edition approved December, 10, 1996. Published February 1997. DOI: Available from National Fire ProtectionAssn., 1 Batterymarch Park, P.O. Box
10.1520/D6060-96R01. 9101, Quincy, MA 02269-9101.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6060–96 (2001)
FIG. 1 Schematic of Process Sampling Equipment
5. Significance and Use 6.3.2 Analyze using a nonpolar methyl silicone column
which separates according to boiling point of the compounds
5.1 This practice has been widely used to obtain mass
and a polar column whose separations are influenced by the
balance data for process scrubbers, to determine the efficiency
polarity of the compounds.
of VOC emission control equipment, and to obtain data to
6.3.3 Use a mass spectrometer to verify the identity of
support air permit applications.
peaks.
5.2 This practice will have applications to the MACT Rule
and may have applications to ComplianceAssurance Monitor-
7. Apparatus
ing verification required by the 1990 Clean Air Act Title III
7.1 A schematic drawing of a typical sampling setup is
Amendments.
shown in Fig. 1. The laptop computer may be physically
5.3 This practice, when used with Test Methods D3464 or
located near the gas chromatograph as shown in Fig. 1,or
D3154 or on-line process flow meter data, can be used to
located remotely. In addition, some portable gas chromato-
calculatedetailedemissionrateprofilesforVOCsfromprocess
graphs have an integral computer. Use a short piece of 1.5 mm
vents.
( ⁄16 in.) outside diameter by 1 mm (0.04 in.) inside diameter
5.4 This practice provides nearly real time results that can
stainless steel tubing as the sampling probe line from the gas
detect process changes or upsets that may be missed using
sampling bulb to the GC inlet.
conventional sorbent tube or integrated gas sampling bag
7.2 Portable Gas Chromatograph (GC), with a thermal
sampling.
conductivity, photoionization, argon ionization, electron cap-
6. Interferences ture or appropriate detector, internal/rechargeable carrier gas
supply, and internal sampling pump.
6.1 Water or liquid in the process line will plug the sample
7.2.1 Portable gas chromatographs are typically equipped
lineofthegaschromatograph,sincetheinjectionvalveofmost
with particulate filters which should be replaced periodically.
portable GCs is not heated. The condensation trap is designed
7.3 Data Logger, device used for automated storage of
toprotecttheportablegaschromatographifliquidsarepresent
output from a flow measurement device.
or occur during process upset.
7.4 Gas Sampling Bulb, 125 mLcapacity with septum port.
6.2 Interferences sometimes result from analytes having
7.5 Personal Sampling Pump.
similar retention times during gas chromatography.
6.3 General approaches which can be followed to resolve
such interferences are given below:
Thecolumnsinmostportablegaschromatographsareeasilyinterchanged.One
6.3.1 Change the type of column, length of column, or
manufacturer has an instrument that simultaneously injects onto two user selected
operating conditions. column modules.
D6060–96 (2001)
7.6 Gas-Tight Syringe, 1, 10, 100, 500 mLcapacity or other periods are 20 to 45 s, however, this parameter must be
convenient sizes for preparing standards. optimized for each VOC analyzed.
7.7 Microlitre Syringes, 10, 25, 50, 100 µL or other conve-
10. Procedure
nient sizes for preparing standards.
7.8 Gas Sampling Bags, for preparation of gas standards.
10.1 Preparation of the Gas Chromatograph:
Bags constructed of various polymer films, such as polyvi-
10.1.1 Fill the internal carrier gas reservoir as described by
nylidene fluoride, fluorinated ethylenepropylene,
the manufacturer.
(tetrafluoroethylene)-fluorocarbon, polyvinylidene chloride,
10.1.2 Select a carrier gas flow or column pressure and
polyethylene and mixed polymer multilayers, with a variety of
column temperature compatible with the column selected for
fittings and capacities (typically 1 to 200 L) are available.
the separation.
7.9 ThermalAnemometer,VaneAnemometer,MassFlowme-
10.1.3 Calibrate the chromatographic column to determine
ter or Pitot Tube, for measurement of vent velocity.
the relative retention times and response of the various
7.10 Condensation Trap, Filtering Flask, 250 or 500 mL
compounds of interest.
polypropylene fitted with a stopper.
10.2 Preparation of the Sampling Train:
7.11 TFE-Fluorocarbon Tubing, 6 mm ( ⁄4 in.) outside
10.2.1 Assemble the sampling train as shown in Fig. 1.
diameter by 5 mm ( ⁄16 in.) inside diameter.
Stainless steel or glass may be substituted for the TFE-
7.12 Data System, an integral or external computer used for
fluorocarbon transfer line.
control of operation of a portable gas chromatograph, data
10.2.2 For process vents containing high concentrations of
reduction, and storage of results.
higher boiling (>125°C) low vapor pressure (<2 kPa) VOCS a
heated transfer line may be necessary. A portable GC with a
8. Hazards
heated injector is also required.
8.1 See NFPA496 for use of electrical equipment in areas 10.2.3 Recheck the calibration after assembly of the sam-
classified as hazardous by Article 500 of NFPA 70, National plingtrainbyconnectinganappropriatestandardtotheinletof
Electrical Code. A purged and pressurized enclosure is re- the sample line. If results
...