ASTM D6060-96

Standard Practice for Sampling of Process Vents With a Portable Gas Chromatograph

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
• Technical Committee: D22 - Air Quality
• Drafting Committee: D22.03 - Ambient Atmospheres and Source Emissions

Relations

• Replaced By: ASTM D6060-96(2001) - Standard Practice for Sampling of Process Vents With a Portable Gas Chromatograph
• Effective Date: 10-Dec-1996

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 6060 – 96
Standard Practice for
Sampling of Process Vents With a Portable Gas
Chromatograph
This standard is issued under the fixed designation D 6060; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope D 1356 Terminology Relating to Sampling and Analysis of
Atmospheres
1.1 This practice describes a method for direct sampling and
D 3464 Test Method for Average Velocity in a Duct Using a
analysis of process vents for volatile organic compound (VOC)
Thermal Anemometer
vapors and permanent gases using a portable gas chromato-
D 3154 Test Method for Average Velocity in a Duct (Pitot
graph (GC).
Tube Method)
1.2 This practice is applicable to analysis of permanent
E 355 Practice for Gas Chromatography Terms and Rela-
gases such as oxygen (O ), carbon dioxide (CO ) and nitrogen
2 2
tionships
(N ), as well as vapors from organic compounds with boiling
2.2 Other Document:
points up to 125°C.
NFPA 496 Standard for Purged and Pressurized Enclosures
1.3 The detection limits obtained will depend on the por-
for Electrical Equipment
table gas chromatograph and detector used. Detectors available
include thermal conductivity, photoionization, argon ioniza-
3. Terminology
tion, and electron capture. For instruments equipped with
3.1 Definitions—For the definition of terms used in this
thermal conductivity detectors, typical detection limits are one
practice, refer to Terminology D 1356 and Practice E 355.
to two parts per million by volume (ppm(v)) with an applicable
3.2 Definitions of Terms Specific to This Standard:
concentration range to high percent by volume levels. For
3.2.1 portable—refers to gas chromatograph with internal
instruments with photoionization detectors detection limit of
battery, internal sample pump, and internal/rechargeable carrier
one to ten parts per billion by volume (ppb(v)) are obtainable
gas supply cylinder.
with a concentration range from 1000 to 2000 ppm(v). The
argon ionization detector has an achievable detection limit of
4. Summary of Practice
one (ppb(v)), while the electron capture detector has an
4.1 One end of a sampling line (typically 6 mm ( ⁄4 in.)
achievable detection limit of one part per trillion by volume
outside diameter TFE-fluorocarbon tubing) is connected to a
(ppt(v)) for chlorinated compounds.
tee in a process vent and the other end to a condensation trap
1.4 The applicability of this practice should be evaluated for
(see 6.1), which is connected to a gas sampling bulb. The outlet
each VOC by determining stability, reproducibility, and linear-
of the gas sampling bulb is connected to a sampling pump set
ity.
at a flow rate of 0.5 to 2 L/min. The sample line from the
1.5 The appropriate concentration range must also be deter-
portable gas chromatograph is inserted through the septum port
mined for each VOC, as the range will depend on the vapor
of the gas sampling bulb. At user selected intervals, the internal
pressure of the particular VOC.
pump of the portable gas chromatograph is activated and
1.6 This standard does not purport to address all of the
process vapors drawn through the injection valve of the gas
safety concerns, if any, associated with its use. It is the
chromatograph and analyzed.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Significance and Use
bility of regulatory limitations prior to use. Refer to Section 8
5.1 This practice has been widely used to obtain mass
on Hazards for additional safety precautions.
balance data for process scrubbers, to determine the efficiency
of VOC emission control equipment, and to obtain data to
2. Referenced Documents
support air permit applications.
2.1 ASTM Standards:
5.2 This practice will have applications to the MACT Rule
1 2
This test method is under the jurisdiction of ASTM Committee D-22 on Annual Book of ASTM Standards, Vol 11.03.
Sampling and Analysis of Atmospheres and is the direct responsibility of Subcom- Annual Book of ASTM Standards, Vol 14.02.
mittee D22.03 on Ambient Atmospheres and Source Emissions. Available from National Fire Protection Assoc., 1 Batterymarch Park, P.O. Box
Current edition approved Dec, 10, 1996. Published February 1997. 9101, Quincy, MA 02269-9101.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 6060
FIG. 1 Schematic of Process Sampling Equipment
and may have applications to Compliance Assurance Monitor- polarity of the compounds.
ing verification required by the 1990 Clean Air Act Title III 6.3.3 Use a mass spectrometer to verify the identity of
Amendments. peaks.
5.3 This practice, when used with Test Methods D 3464 or
7. Apparatus
D 3154 or on-line process flow meter data, can be used to
7.1 A schematic drawing of a typical sampling setup is
calculate detailed emission rate profiles for VOCs from process
shown in Fig. 1. The laptop computer may be physically
vents.
located near the gas chromatograph as shown in Fig. 1, or
5.4 This practice provides nearly real time results that can
located remotely. In addition, some portable gas chromato-
detect process changes or upsets that may be missed using
graphs have an integral computer. Use a short piece of 1.5 mm
conventional sorbent tube or integrated gas sampling bag
( ⁄16 in.) outside diameter by 1 mm (0.04 in.) inside diameter
sampling.
stainless steel tubing as the sampling probe line from the gas
sampling bulb to the GC inlet.
6. Interferences
7.2 Portable Gas Chromatograph (GC), with a thermal
conductivity, photoionization, argon ionization, electron cap-
6.1 Water or liquid in the process line will plug the sample
ture or appropriate detector, internal/rechargable carrier gas
line of the gas chromatograph, since the injection valve of most
supply, and internal sampling pump.
portable GCs is not heated. The condensation trap is designed
7.2.1 Portable gas chromatographs are typically equipped
to protect the portable gas chromatograph if liquids are present
with particulate filters which should be replaced periodically.
or occur during process upset.
7.3 Data Logger, device used for automated storage of
6.2 Interferences sometimes result from analytes having
output from a flow measurement device.
similar retention times during gas chromatography.
7.4 Gas Sampling Bulb, 125 mL capacity with septum port.
6.3 General approaches which can be followed to resolve
7.5 Personal Sampling Pump.
such interferences are given below:
7.6 Gas-Tight Syringe, 1, 10, 100, 500 mL capacity or other
6.3.1 Change the type of column, length of column, or convenient sizes for preparing standards.
operating conditions.
6.3.2 Analyze using a nonpolar methyl silicone column
The columns in most portable gas chromatographs are easily interchanged. One
which separates according to boiling point of the compounds
manufacturer has an instrument that simultaneously injects onto two user selected
and a polar column whose separations are influenced by the column modules.
D 6060
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
7.9 Thermal Anemometer, Vane Anemometer, Mass Flowme-
the relative retention times and response of the various
ter or Pitot Tube, for measurement of vent velocity.
compounds of interest.
7.10 Condensation Trap, Filtering Flask, 250 or 500 mL
10.2 Preparation of the Sampling Train:
polypropylene fitted with a stopper.
10.2.1 Assemble the sampling train as shown in Fig. 1.
7.11 TFE-Fluorocarbon Tubing,6mm( ⁄4 in.) outside
Stainless steel or glass may be substituted for the TFE-
diameter by 5 mm ( ⁄16 in.) inside diameter.
fluorocarbon transfer line.
7.12 Data System, an integral or external computer used for
10.2.2 For process vents containing high concentrations of
control of operation of a portable gas chromatograph, data
higher boiling (>125°C) low vapor pressure (<2 kPa) VOCS a
reduction, and storage of results.
heated transfer line may be necessary. A portable GC with a
heated injector is also required.
8. Hazards
10.2.3 Recheck the calibration after assembly of the sam-
8.1 See NFPA 496 for use of electrical equipment in areas
pling train by connecting an appropriate standard to the inlet of
classified as hazardous by Article 500 of NFPA 70, National
the sample line. If results obtained for the analysis of the
Electrical Code. A purged and pressurized enclosure is re-
standard are not within 15 % relative standard deviation of the
quired.
expected concentration, check the sampling train for
...