ASTM D2163-91(1996)
(Test Method)Standard Test Method for Analysis of Liquefied Petroleum (LP) Gases and Propene Concentrates by Gas Chromatography (Withdrawn 2005)
Standard Test Method for Analysis of Liquefied Petroleum (LP) Gases and Propene Concentrates by Gas Chromatography (Withdrawn 2005)
SCOPE
1.1 This test method covers the determination of the composition of liquefied petroleum (LP) gases. It is applicable to analysis of propane, propene, and butane in all concentration ranges 0.1% and above.
1.2 This standard does not purport to address all of the safety problems, 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.>
1.3 The values stated in SI units are to be regarded as standard.
WITHDRAWN RATIONALE
This test method covers the determination of the composition of liquefied petroleum (LP) gases. It is applicable to analysis of propane, propene, and butane in all concentration ranges 0.1 % and above.
Formerly under the jurisdiction of Committee D02 on Petroleum Products and Lubricants, this test method was withdrawn in January 2005 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
AnAmerican National Standard
Designation: D 2163 – 91 (Reapproved 1996)
Designation: 264/72(85)
Standard Test Method for
Analysis of Liquefied Petroleum (LP) Gases and
Propene Concentrates by Gas Chromatography
This standard is issued under the fixed designation D 2163; 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 ing components separated under identical operating conditions
from a reference standard mixture of known composition or
1.1 This test method covers the determination of the com-
from use of pure hydrocarbons. The chromatogram of the
position of liquefied petroleum (LP) gases. It is applicable to
sample is interpreted by comparing peak heights or areas with
analysis of propane, propene, and butane in all concentration
those obtained on the reference standard mixture of pure
ranges 0.1 % and above.
hydrocarbons.
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Significance and Use
responsibility of the user of this standard to establish appro-
5.1 Thecomponentdistributionofliquefiedpetroleumgases
priate safety and health practices and determine the applica-
and propene concentrates is often required as a specification
bility of regulatory limitations prior to use.
analysis for end-use sale of this material. Its wide use as
1.3 The values stated in SI units are to be regarded as
chemical feedstocks or as fuel, require precise compositional
standard.
data to ensure uniform quality of the desired reaction products.
2. Referenced Documents 5.2 The component distribution data of liquefied petroleum
gases and propene concentrates can be used to calculate
2.1 ASTM Standards:
physicalpropertiessuchasrelativedensity,vaporpressure,and
D 2421 Practice for Interconversion of Analysis of C and
motor octane (see Practice D 2598). Precision and accuracy of
Lighter Hydrocarbons to Gas-Volume, Liquid-Volume, or
2 compositional data are extremely important when these data
Weight Basis
are used to calculate various properties of these petroleum
D 2598 Practice for Calculation of Certain Physical Prop-
products.
erties of Liquified Petroleum (LP) Gases from Composi-
tional Analysis
6. Gas Chromatograph System
D 3700 PracticeforContainingHydrocarbonFluidSamples
3 6.1 Detector—The detector shall be a thermal conductivity
Using a Floating Piston Cylinder
type or its equivalent in sensitivity and stability. The system
3. Terminology shall be capable of detecting 0.1 % concentration of any
component of interest. For calculation techniques utilizing a
3.1 Definitions:
recorder, the signal for the concentration shall be at least 5
3.1.1 propene concentrate—concentrate containing more
chart divisions above the noise level ona0to100 scale chart.
than 50 % propene.
Noise level must be restricted to a maximum of 1 chart
4. Summary of Test Method
division. When electronic integration is employed the signal
for 0.1 % concentration must be at least twice the noise level.
4.1 Components in a sample of LP gas are physically
6.2 Recorder—A strip-chart recorder and integrator with a
separatedbygaschromatographyandcomparedtocorrespond-
full-scalerangeof10mVorlessshallberequired.Amaximum
full-scale balance time of 2 s and a minimum chart speed of ⁄2
This test method is under the jurisdiction of ASTM Committee D-2 on
in. (12.7 mm)/min shall be required.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
6.3 Attenuator—A multistep attenuator for the detector
D02.D0.03 on C4 Test Methods Liquefied Petroleum Gas.
Current edition approved Oct. 15, 1991. Published December 1991. Originally output signal shall be necessary to maintain maximum peaks
published as D 2163 – 63. Last previous edition D 2163 – 87.
within the recorder chart range. The attenuator system must be
Annual Book of ASTM Standards, Vol 05.01.
3 accurate to 0.5 % in any position.
Annual Book of ASTM Standards, Vol 05.02.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959, United States.
D 2163 – 91 (1996)
FIG. 1 Illustration of A/B Ratio FIG. 2 Illustration of A/B Ratio for Small-Component Peak
6.4 Sample Inlet System—Provision shall be made to intro-
by more than 10 % if the peak height method of calculation is
duce up to 0.50 mLof the sample.The sample volume must be
used. On propene concentrates, the calibration standard mix-
repeatable such that successive runs agree within 1 mm or 1 %
tures shall not differ from that of like component in the sample
(whichever is larger) on each component peak height.
to be analyzed by more than 5 %. Typical composition ranges
6.5 Temperature Control—The analyzer columns shall be
of suitable calibration standard mixtures are given in Table 1.
maintained at a temperature constant to 0.3°C during the
NOTE 1—Test Method D 2421 may be used whenever a need exists for
course of the sample and corresponding reference standard
such translations.
runs.
6.6 Carrier Gas—The instrument shall be equipped with
8. Procedure
suitable facilities to provide a flow of carrier gas through the
8.1 Apparatus Preparation—Mount the column suitable for
analyzer column at a flow rate that is constant to 1.0 %
the analysis desired (see Appendix X1) in the chromatograph
throughout the analysis.
and adjust the conditions to optimum for the column selected
6.7 Columns—Any column may be used provided all com-
(Table 2). Allow sufficient time for the instrument to reach
ponent peaks for compounds present in concentration of more
equilibrium as indicated by a stable base line.
than5 %areresolvedsothattheratio A/Bshallnotbelessthan
8.1.1 The test method allows the user a wide latitude in
0.8, Fig. 1
choice of instrumentation to make the analysis, and most
commercial instrumentation easily meets the requirements
where:
defined in the test method. However, only by strict adherence
A = depth of the valley on either side of peak B, and
to the calibration procedures outlined in the method can
B = height above the baseline of the smaller of any two
reproducibility between instruments expect to be achieved.
adjacent peaks (see Fig. 1).
8.1.2 Proper maintenance of instrumentation is critical to
For compounds present in concentrations of 5 % or less, the
continued satisfactory performance of this analysis. Clean
ratio of A/B shall not be less than 0.4. In case the small-
sample containers, clean sample inlet systems and clean
component peak is adjacent to a large one, it may be necessary
detectors are mandatory to achieve the precision and accuracy
to construct the baseline of the small peak tangent to the curve
capabilities of this method.
as shown in Fig. 2.
NOTE 2—Warning: Samples and reference mixtures are extremely
7. Calibration Standard
flammable. Keep away from heat, sparks, and flames. Use with adequate
ventilation. Cylinders must by supported at all times. Hydrocarbon vapors
7.1 Pure components or calibration standard mixtures may
that may be vented must be controlled to assure compliance with
be used for calibration. If pure components are used, identical
applicable safety and environmental regulations. Vapor reduces oxygen
volumes of each component are injected into the chromato-
available for breathing. Liquid causes cold burns.
graph and relative area response factors are determined. These
8.2 Preparation and Introduction of Sample—Attach the
factors are valid for a given instrument and operating condi-
cylinder containing the gas mixture to the sampling valve of
tions and should be redetermined periodically. If pure compo-
the chromatograph so that a liquid phase sample is withdrawn.
nents are used for calibration, the calculation should be made
Adjust the flow rate from the sample cylinder so that complete
in mole percent and converted to liquid volume percent (Note
vaporization of the liquid occurs at the cylinder valve. (An
1). Factors repeatable to within 1 % are required. The concen-
alternative technique is to trap a sample of only liquid phase in
tration of each component in the calibration standard mixtures
a short section of tubing, and then permit the entire sample to
shall be known to within 0.1 %.The concentration of the major
vaporize into an evacuated container). Adjust the ratio of the
component in the calibration standard mixture shall not differ
two volumes so that a gage pressure of 69 to 138 kPa (10 to 20
from that of the like component in the sample to be analyzed
psi) is obtained in the final container. Then use this sample for
the analysis. Flush the sample loop for 1 to 2 min at a flow rate
of 5 to 10 mL/min before introducing the sample into the
Suitable reference standard mixtures of pure hydrocarbons are available from
Scott Specialty Gases, Inc., Plumsteadville, PA. carrier gas stream.
D 2
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