ASTM D1945-14 Análisis de Gas Por Cromat

Designation: D1945 − 14
Standard Test Method for

Analysis of Natural Gas by Gas Chromatography1
This standard is issued under the fixed designation D1945; 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* composition of the sample is calculated by comparing either

1.1 This test method covers the determination of the chemi- the peak heights, or the peak areas, or both, with the corre-
cal composition of natural gases and similar gaseous mixtures sponding values obtained with the reference standard.
within the range of composition shown in Table 1. This test
4. Significance and Use
method may be abbreviated for the analysis of lean natural
gases containing negligible amounts of hexanes and higher 4.1 This test method is of significance for providing data for
hydrocarbons, or for the determination of one or more calculating physical properties of the sample, such as heating
components, as required. value and relative density, or for monitoring the concentrations
of one or more of the components in a mixture.
1.2 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 5. Apparatus
standard.
5.1 Detector—The detector shall be a thermal-conductivity
1.3 This standard does not purport to address all of the type, or its equivalent in sensitivity and stability. The thermal
safety concerns, if any, associated with its use. It is the conductivity detector must be sufficiently sensitive to produce
responsibility of the user of this standard to establish appro- a signal of at least 0.5 mV for 1 mol % n-butane in a 0.25-mL
priate safety and health practices and determine the applica- sample.
bility of regulatory limitations prior to use.
5.2 Recording Instruments—Either strip-chart recorders or
2. Referenced Documents electronic integrators, or both, are used to display the separated
components. Although a strip-chart recorder is not required
2.1 ASTM Standards:2
when using electronic integration, it is highly desirable for
D2597 Test Method for Analysis of Demethanized Hydro-
evaluation of instrument performance.
carbon Liquid Mixtures Containing Nitrogen and Carbon
5.2.1 The recorder shall be a strip-chart recorder with a
Dioxide by Gas Chromatography
full-range scale of 5 mV or less (1 mV preferred). The width of
E260 Practice for Packed Column Gas Chromatography
the chart shall be not less than 150 mm. A maximum pen
3. Summary of Test Method response time of 2 s (1 s preferred) and a minimum chart speed
of 10 mm/min shall be required. Faster speeds up to 100
3.1 Components in a representative sample are physically mm/min are desirable if the chromatogram is to be interpreted
separated by gas chromatography (GC) and compared to using manual methods to obtain areas.
calibration data obtained under identical operating conditions 5.2.2 Electronic or Computing Integrators—Proof of sepa-
from a reference standard mixture of known composition. The ration and response equivalent to that for a recorder is required
numerous heavy-end components of a sample can be grouped for displays other than by chart recorder. Baseline tracking
into irregular peaks by reversing the direction of the carrier gas with tangent skim peak detection is recommended.
through the column at such time as to group the heavy ends
either as C5 and heavier, C6 and heavier, or C7 and heavier. The 5.3 Attenuator—If the chromatogram is to be interpreted
using manual methods, an attenuator must be used with the
detector output signal to maintain maximum peaks within the
1
This test method is under the jurisdiction of ASTM Committee D03 on Gaseous recorder chart range. The attenuator must be accurate to within
Fuels and is the direct responsibility of Subcommittee D03.07 on Analysis of 0.5 % between the attenuator range steps.
Chemical Composition of Gaseous Fuels.
Current edition approved Nov. 1, 2014. Published November 2014. Originally 5.4 Sample Inlet System:
approved in 1962. Last previous edition approved in 2010 as D1945-96(2010). DOI: 5.4.1 The sample inlet system shall be constructed of
10.1520/D1945-14.
2
materials that are inert and nonadsorptive with respect to the
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
components in the sample. The preferred material of construc-
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on tion is stainless steel. Copper, brass, and other copper-bearing
the ASTM website. alloys are unacceptable. The sample inlet system from the
*A Summary of Changes section appears at the end of this standard

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D1945 − 14
TABLE 1 Natural Gas Components and Range of 5.5.1 Isothermal—When isothermal operation is used,
Composition Covered maintain the analyzer columns at a temperature constant to
Component Mol % 0.3 °C during the course of the sample run and corresponding
Helium 0.01 to 10 reference run.
Hydrogen 0.01 to 10
Oxygen 0.01 to 20 5.5.2 Temperature Programming—Temperature program-
Nitrogen 0.01 to 100 ming may be used, as feasible. The oven temperature shall not
Carbon dioxide 0.01 to 20
Methane 0.01 to 100
exceed the recommended temperature limit for the materials in
Ethane 0.01 to 100 the column.
Hydrogen sulfide 0.3 to 30
Propane 0.01 to 100 5.6 Detector Temperature Control—Maintain the detector
Isobutane 0.01 to 10 temperature at a temperature constant to 0.3 °C during the
n-Butane 0.01 to 10
Neopentane 0.01 to 2 course of the sample run and the corresponding reference run.
Isopentane 0.01 to 2 The detector temperature shall be equal to or greater than the
n-Pentane 0.01 to 2 maximum column temperature.
Hexane isomers 0.01 to 2
Heptanes+ 0.01 to 1 5.7 Carrier Gas Controls—The instrument shall be
equipped with suitable facilities to provide a flow of carrier gas
through the analyzer and detector at a flow rate that is constant
to 1 % throughout the analysis of the sample and the reference
standard. The purity of the carrier gas may be improved by
cylinder valve to the GC column inlet must be maintained at a
flowing the carrier gas through selective filters prior to its entry
temperature constant to 61 °C.
into the chromatograph.
5.4.2 Provision must be made to introduce into the carrier
gas ahead of the analyzing column a gas-phase sample that has 5.8 Columns:
been entrapped in a fixed volume loop or tubular section. The 5.8.1 The columns shall be constructed of materials that are
fixed loop or section shall be so constructed that the total inert and nonadsorptive with respect to the components in the
volume, including dead space, shall not normally exceed sample. The preferred material of construction is stainless
0.5mL at 100 kPa. If increased accuracy of the hexanes and steel. Copper and copper-bearing alloys are unacceptable.
heavier portions of the analysis is required, a larger sample size 5.8.2 An adsorption-type column and a partition-type col-
may be used (see Test Method D2597). The sample volume umn may be used to make the analysis.
must be reproducible such that successive runs agree within
1 % on each component. A flowing sample inlet system is NOTE 2—See Practice E260.
acceptable as long as viscosity effects are accounted for.
5.8.2.1 Adsorption Column—This column must completely
NOTE 1—The sample size limitation of 0.5 mL or smaller is selected separate oxygen, nitrogen, and methane. A 13X molecular
relative to linearity of detector response, and efficiency of column sieve 80/100 mesh is recommended for direct injection. A 5A
separation. Larger samples may be used to determine low-quantity
components to increase measurement accuracy.
column can be used if a pre-cut column is present to remove
interfering hydrocarbons. If a recorder is used, the recorder pen
5.4.3 An optional manifold arrangement for entering must return to the baseline between each successive peak. The
vacuum samples is shown in Fig. 1. resolution (R) must be 1.5 or greater as calculated in the
5.5 Column Temperature Control: following equation:
FIG. 1 Suggested Manifold Arrangement for Entering Vacuum Samples

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D1945 − 14
x2 2 x1 5.11 Vacuum Gauge—Any type of vacuum gauge may be
R ~ 1,2 ! 5 3 2, (1)
y 2 1y 1 used which has a resolution of 0.14 kPa or better and covers the
range of 0 to 120 kPa or larger.
where x1, x2 are the retention times and y1, y2 are the peak
widths. Fig. 2 illustrates the calculation for resolution. Fig. 3 is 5.12 Vacuum Pump—Must have the capability of producing
a chromatogram obtained with an adsorption column. a vacuum of 0.14 kPa absolute or less.
5.8.2.2 Partition Column—This column must separate eth-
ane through pentanes and carbon dioxide. If a recorder is used, 6. Preparation of Apparatus
the recorder pen must return to the base line between each peak 6.1 Linearity Check—To establish linearity of response for
for propane and succeeding peaks, and to base line within 2 % the thermal conductivity detector, it is necessary to complete
of full-scale deflection for components eluted ahead of the following procedure:
propane, with measurements being at the attenuation of the 6.1.1 The major component of interest (methane for natural
peak. Separation of carbon dioxide must be sufficient so that a gas) is charged to the chromatograph by way of the fixed-size
0.25-mL sample containing 0.1-mol % carbon dioxide will sample loop at partial pressure increments of 13 kPa from 13
produce a clearly measurable response. The resolution (R) to 100 kPa or the prevailing atmospheric pressure.
must be 1.5 or greater as calculated in the above equation. The 6.1.2 The integrated peak responses for the area generated at
separation should be completed within 40 min, including each of the pressure increments are plotted versus their partial
reversal of flow after n-pentane to yield a group response for pressure (see Fig. 9).
hexanes and heavier components. Figs. 4-6 are examples of 6.1.3 The plotted results should yield a straight line. A
chromatograms obtained on some of the suitable partition perfectly linear response would display a straight line at a 45°
columns. angle using the logarithmic values.
5.8.3 General—Other column packing materials that pro- 6.1.4 Any curved line indicates the fixed volume sample
vide satisfactory separation of components of interest may be loop is too large. A smaller loop size should replace the fixed
used (see Fig. 7). In multicolumn applications, it is preferred to volume loop and 6.1.1 through 6.1.4 should be repeated (see
use front-end backflush of the heavy ends. Fig. 9).
NOTE 3—The chromatograms in Figs. 3-8 are only illustrations of 6.1.5 The linearity over the range of interest must be known
typical separations. The operating conditions, including columns, are also for each component. It is useful to construct a table noting the
typical and are subject to optimization by competent personnel. response factor deviation in changing concentration. (See
5.9 Drier—Unless water is known not to interfere in the Table 2 and Table 3).
analysis, a drier must be provided in the sample entering 6.1.6 It should be noted that nitrogen, methane, and ethane
system, ahead of the sample valve. The drier must remove exhibit less than 1 % compressibility at atmospheric pressure.
moisture without removing selective components to be deter- Other natural gas components do exhibit a significant com-
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mined in the analysis. pressibility at pressures less than atmospheric.

6.1.7 Most components that have vapor pressures of less
NOTE 4—See A2.2 for preparation of a suitable drier. than 100 kPa cannot be used as a pure gas for a linearity study
5.10 Valves—Valves or sample splitters, or both, are re- because they will not exhibit sufficient vapor pressure for a
quired to permit switching, backflushing, or for simultaneous vacuum gauge reading to 100 kPa. For these components, a
analysis. mixture with nitrogen or methane can be used to establish a
FIG. 2 Calculation for Resolution

D1945 − 14
FIG. 3 Separation Column for Oxygen, Nitrogen, and Methane (See Annex A2)
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FIG. 4 Chromatogram of Natural Gas (BMEE Column) (See Annex A2)
partial pressure that can extend the total pressure to 100 kPa. where:
Using Table 4 for vapor pressures at 38 °C, calculate the B = blend pressure, max, kPa;
maximum pressure to which a given component can be blended V = vapor pressure, kPa;
with nitrogen as follows: i = mol %;
B 5 ~ 100 3 V ! /i (2) P = partial pressure, kPa; and
M = vacuum gauge pressure, kPa.
P 5 ~ i 3 M ! /100 (3)

D1945 − 14
FIG. 5 Chromatogram of Natural Gas (Silicone 200/500 Column) (See Annex A2)
FIG. 6 Chromatogram of Natural Gas (See Annex A2)
6.2 Procedure for Linearity Check: 6.2.2 Carefully open the needle valve to admit the pure
6.2.1 Connect the pure-component source to the sample- component up to 13 kPa of partial pressure.
entry system. Evacuate the sample-entry system and observe 6.2.3 Record the exact partial pressure and actuate the
the vacuum gauge for leaks. (See Fig. 1 for a suggested sample valve to place the sample onto the column. Record the
manifold arrangement.) The sample-entry system must be peak area of the pure component.
vacuum tight.
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D1945 − 14
FIG. 7 Chromatogram of Natural Gas (Multi-Column Application) (See Annex A2)

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FIG. 8 Separation of Helium and Hydrogen
6.2.4 Repeat 6.2.3 for 26, 39, 52, 65, 78, and 91 kPa on the 6.2.6 An alternative method is to obtain a blend of all the
vacuum gauge, recording the peak area obtained for sample components and charge the sample loop at partial pressure over
analysis at each of these pressures. the range of interest. If a gas blender is available, the mixture
6.2.5 Plot the area data (x axis) versus the partial pressures can be diluted with methane thereby giving response curves for
(y axis) on a linear graph as shown in Fig. 9. all the components. (Warning—If it is not possible to obtain

D1945 − 14
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FIG. 9 Linearity of Detector Response
TABLE 2 Linearity Evaluation of Methane TABLE 3 Linearity Evaluation for Nitrogen

S/B diff = (low mole % − high mole %) ⁄ low mole % × 100 S/B diff = (low mole % − high mole %) ⁄ low mole % × 100
S/B diff., % on low S/B diff., % on low
B area S mole % S/B mole % ⁄ area B area S mole % S/B mole % ⁄ area
value value
223 119 392 51 2.2858e-07 5 879 836 1 1.7007e-07
242 610 272 56 2.3082e-07 −0.98 29 137 066 5 1.7160e-07 −0.89
261 785 320 61 2.3302e-07 −0.95 57 452 364 10 1.7046e-07 −1.43
280 494 912 66 2.3530e-07 −0.98 84 953 192 15 1.7657e-07 −1.44
299 145 504 71 2.3734e-07 −0.87 111 491 232 20 1.7939e-07 −1.60
317 987 328 76 2.3900e-07 −0.70 137 268 784 25 1.8212e-07 −1.53
336 489 056 81 2.4072e-07 −0.72 162 852 288 30 1.8422e-07 −1.15
351 120 721 85 2.4208e-07 −0.57 187 232 496 35 1.8693e-07 −1.48
information on the linearity of the available gas chromatograph

detector for all of the test gas components, then as a minimum contain known percents of the components, except oxygen
requirement the linearity data must be obtained for any gas (Note 5), that are to be determined in the unknown sample. All
component that exceeds a concentration of 5 mol%. Chromato- components in the reference standard must be homogenous in
graphs are not truly linear over wide concentration ranges and the vapor state at the time of use. The concentration of a
linearity should be established over the range of interest.) component in the reference standard gas should not be less than
one half nor more than twice the concentration of the corre-
7. Reference Standards sponding component in the test gas.
7.1 Moisture-free gas mixtures of known composition are NOTE 5—Unless the reference standard is stored in a container that has
required for comparison with the test sample. They must been tested and proved for inertness to oxygen, it is preferable to calibrate

D1945 − 14
TABLE 4 Vapor Pressure at 38 °CA 8.2.2 Connections from the sample container to the sample
Component kPa absolute inlet of the instrument should be made with stainless steel or
Nitrogen >34 500 with short pieces of TFE-fluorocarbon. Copper, vinyl, or
Methane >34 500
Carbon dioxide >5 520
rubber connections are not acceptable. Heated lines may be
Ethane >5 520 necessary for high hydrocarbon content samples.
Hydrogen sulfide 2 720
Propane 1 300
8.3 Sample Introduction—The size of the sample introduced
Isobutane 501 to the chromatographic columns shall not exceed 0.5 mL. (This
n-Butane 356 small sample size is necessary to obtain a linear detector
Isopentane 141
n-Pentane 108 response for methane.) Sufficient accuracy can be obtained for
n-Hexane 34.2 the determination of all but the minor constituents by the use of
n-Heptane 11.2 this sample size. When increased response is required for the
A
The most recent data for the vapor pressures listed are available from the determination of components present in concentrations not
Thermodynamics Research Center, Texas A&M University System, College
Station, TX 77843.
exceeding 5 mol %, it is permissible to use sample and
reference standard volumes not exceeding 5 mL. (Avoid
introduction of liquids into the sample system.)
for oxygen by an alternative method. 8.3.1 Purging Method—Open the outlet valve of the sample
cylinder and purge the sample through the inlet system and
7.2 Preparation—A reference standard may be prepared by
sample loop or tube. The amount of purging required must be
blending pure components. Diluted dry air is a suitable
established and verified for each instrument. The sample loop
standard for oxygen and nitrogen (see 8.5.1).3,4
pressure should be near atmospheric. Close the cylinder valve
8. Procedure and allow the pressure of the sample in the loop or tube to
stabilize. Then immediately inject the contents of the loop or
8.1 Instrument Preparation—Place the proper column(s) in
tube into the chromatographic column to avoid infiltration of
operation as needed for the desired run (as described in either
contaminants.
8.4, 8.5, or 8.6). Adjust the operating conditions and allow the
8.3.2 Water Displacement—If the sample was obtained by
chromatograph to stabilize.
water displacement, then water displacement may be used to
8.1.1 For hexanes and higher, heat the sample loop.
purge and fill the sample loop or tube. (Warning—Some
NOTE 6—Most modern chromatographs have valve ovens that can be components, such as carbon dioxide, hydrogen sulfide, and
temperature controlled. It is strongly recommended in the absence of hexanes and higher hydrocarbons, may be partially or com-
valve ovens to mount the gas sampling valve in the chromatograph oven
pletely removed by the water.)
and operate at the column temperature.
8.3.3 Evacuation Method—Evacuate the charging system,
8.1.2 After the instrument has apparently stabilized, make including the sample loop, and the sample line back to the
check runs on the reference standard to establish instrument valve on the sample cylinder, to less than 0.1 kPa absolute
repeatability. Two consecutive checks must agree within the pressure. Close the valve to the vacuum source and carefully
repeatability limits for the mol % amount present of each meter the fuel-gas sample from the sample cylinder until the
component. Either the average of the two consecutive checks, sample loop is filled to the desired pressure, as indicated on the
or the latest check agreeing within the repeatability limits of vacuum gauge (see Fig. 1). Inject the sample into the chro-
the previous check on each component may be used as the matograph.
reference standard for all subsequent runs until there is a
change in instrument operating conditions. Daily calibrations 8.4 Partition Column Run for Ethane and Heavier Hydro-
are recommended. carbons and Carbon Dioxide—This run is made using either
helium or hydrogen as the carrier gas; if other than a thermal
8.2 Sample Preparation—If desired, hydrogen sulfide may conductivity detector is used, select a suitable carrier gas for
be removed by at least two methods (see Annex A2.3). that detector. Select a sample size in accordance with 8.1. Enter
8.2.1 Preparation and Introduction of Sample—Samples the sample, and backflush heavy components when appropri-
must be equilibrated in the laboratory at 10 to 30 °C above the ate. Obtain a corresponding response on the reference standard.
source temperature of the field sampling. The higher the 8.4.1 Methane may also be determined on this column if the
temperature the shorter the equilibration time (approximately column will separate the methane from nitrogen and oxygen
2 h for small sample containers of 300 mL or less). This (such as with silicone 200/500 as shown in Fig. 5), and the
analysis method assumes field sampling methods have re- sample size does not exceed 0.5 mL.
moved entrained liquids. If the hydrocarbon dewpoint of the
8.5 Adsorption Column Run for Oxygen, Nitrogen, and
sample is known to be lower than the lowest temperature to
Methane—Make this run using helium or hydrogen as the
which the sample has been exposed, it is not necessary to heat
carrier gas. The sample size must not exceed 0.5 mL for the
the sample.
determination of methane. Enter the sample and obtain a
response through methane (Note 5). Likewise, obtain a re-
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3
A suitable reference standard is available from Scott Specialty Gases Inc., sponse on the reference standard for nitrogen and methane.
Plumsteadville, PA.
4
A ten-component reference standard traceable to the National Institute of
Obtain a response on dry air for nitrogen and oxygen, if
Standards and Technology (NIST) is available from Institute of Gas Technology desired. The air must be either entered at an accurately
(IGT), 3424 S. State St., Chicago, IL 60616. measured reduced pressure, or from a helium-diluted mixture.

D1945 − 14
8.5.1 A mixture containing approximately 1 % of oxygen 9.2.2 Hexanes and Heavier Components—Measure the ar-
can be prepared by pressurizing a container of dry air at eas of the hexanes portion and the heptanes and heavier portion
atmospheric pressure to 2 MPa with pure helium. This pressure of the reverse-flow peak (see Annex A1, Fig. A1.1, and X3.6).
need not be measured precisely, as the concentration of Also measure the areas of both pentane peaks on the sample
nitrogen in the mixture thus prepared must be determined by chromatogram, and adjust all measured areas to the same
comparison to nitrogen in the reference standard. The percent attenuation basis.
nitrogen is multiplied by 0.268 to obtain the mole percent of 9.2.3 Calculate corrected areas of the reverse flow peaks as
oxygen or by 0.280 to obtain the mole percent total of oxygen follows:
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and argon. Do not rely on oxygen standards that have been Corrected C 6 area 5 72/86 3 measured C 6 area (6)
prepared for more than a few days. It is permissible to use a
response factor for oxygen that is relative to a stable constitu- Corrected C 7 and heavier area (7)
ent. 5 72/A 3 measured C 7 and heavier area
8.6 Adsorption Column Run for Helium and Hydrogen—
where A = average molecular weight of the C7 and heavier
Make this run using either nitrogen or argon as the carrier gas.
fraction.
Enter a 1 to 5 mL sample and record the response for helium,
followed by hydrogen, which will be just ahead of oxygen NOTE 7—The value of 98 is usually sufficiently accurate for use as the
(Note 5). Obtain a corresponding response on a reference C7 and heavier fraction average molecular weight; the small amount of C8
and heavier present is usually offset by the lighter methyl cyclopentane
standard containing suitable concentrations of helium and
and cyclohexane that occur in this fraction. A more accurate value for the
hydrogen (see Fig. 8). molecular weight of C7 and heavier can be obtained as described in Annex
A1.3.
9. Calculation 9.2.4 Calculate the concentration of the two fractions in the
9.1 The number of significant digits retained for the quan- sample as follows:
titative value of each component shall be such that accuracy is Mol % C6 5 ~ corrected C 6 area! (8)
neither sacrificed or exaggerated. The expressed numerical
value of any component in the sample should not be presumed 3 ~ mol % iC 5 1nC 5 ! / ~ iC 5 1nC 5 area! .
to be more accurate than the corresponding certified value of Mol % C 7 1 5 ~ corrected C 7 area! (9)
that component in the calibration standard.
3 ~ mol % i C 5 1nC 5 ! / ~ iC 5 1nC 5 area! .
9.2 External Standard Method:
9.2.1 Pentanes and Lighter Components—Measure the 9.2.4.1 If the mole percent of iC5 + nC5 has been deter-
height of each component peak for pentanes and lighter, mined by a separate run with a smaller sized sample, this value
convert to the same attenuation for corresponding components need not be redetermined.
in the sample and reference standard, and calculate the con- 9.2.5 The entire reverse flow area may be calculated in this
centration of each component in the sample as follows: manner as C6 and heavier, or as C5 and heavier should the
C 5 S 3 ~ A/B ! (4) carrier gas reversal be made after n-butane. The measured area
should be corrected by using the average molecular weights of
where: the entire reverse-flow components for the value of A. The
C = component concentration in the sample, mol %; mole percent and area of the iC5 and nC5 reverse flow peak of
A = peak height of component in the sample, mm; an identically sized sample of reference standard (free of C6
B = peak height of component in the standard, mm; and and heavier) shall then be used for calculating the final mole
S = component concentration in the reference standard, percent value.
mol %. 9.2.6 Normalize the mole percent values by multiplying
9.2.1.1 If air has been run at reduced pressure for oxygen or each value by 100 and dividing by the sum of the original
nitrogen calibration, or both, correct the equation for pressure values. The sum of the original values should not differ from
as follows: 100.0 % by more than 1.0 %.
9.2.7 See sample calculations in Appendix X2.
C 5 S 3 ~ A/B ! 3 ~ P a /P b ! (5)
where: 10. Precision

Pa = pressure at which air is run and 10.1 Precision—The precision of this test method, as deter-
Pb = true barometric pressure during the run, with both mined by the statistical examination of the interlaboratory test
pressures being expressed in the same units. results, for gas samples of pipeline quality 38 MJ/m3 is as
9.2.1.2 Use composition values of 78.1 % nitrogen and follows:
21.9 % oxygen for dry air, because argon elutes with oxygen 10.1.1 Repeatability—The difference between two succes-
on a molecular sieves column under the normal conditions of sive results obtained by the same operator with the same
this test method. apparatus under constant operating conditions on identical test

D1945 − 14
materials should be considered suspect if they differ by more 11. Keywords
than the following amounts: 11.1 gas analysis; gas chromatography; natural gas compo-
Component, mol % Repeatability sition
0 to 0.09 0.01
0.1 to 0.9 0.04
1.0 to 4.9 0.07
5.0 to 10 0.08
Over 10 0.10
10.1.2 Reproducibility—The difference between two results
obtained by different operators in different laboratories on
identical test materials should be considered suspect if they
differ by more than the following amounts:
Component, mol % Reproducibility
0 to 0.09 0.02
0.1 to 0.9 0.07
1.0 to 4.9 0.10
5.0 to 10 0.12
Over 10 0.15
ANNEXES
(Mandatory Information)
A1. SUPPLEMENTARY PROCEDURES
A1.1 Analysis for Only Propane and Heavier Components A1.2.2 Enter a 1 to 5 mL sample into the partition column
A1.1.1 This determination can be made in 10 to 15 min run and reverse the carrier gas flow after n-pentane is separated.
time by using column conditions to separate propane, Obtain a corresponding chromatogram of the reference stan-
isobutane, n-butane, isopentane, n-pentane, hexanes, and dard. Measure the peak heights of ethane through n-pentane
heptanes, and heavier, but disregarding separation on ethane and the areas of the pentane peaks of the standard. Make
and lighter. calculations on ethane and heavier components in the same
manner as for the complete analysis method. Methane and
A1.1.2 Use a 5 m bis-(2(2-methoxyethoxy) ethyl)ether
lighter may be expressed as the difference between 100 and the
(BMEE) column at about 30 °C, or a suitable length of another
sum of the determined components.
partition column that will separate propane through n-pentane
in about 5 min. Enter a 1 to 5 mL sample into the column and A1.3 Special Analysis to Determine Hexanes and Heavier
reverse the carrier gas flow after n-pentane is separated. Obtain Components
a corresponding chromatogram on the reference standard,
which can be accomplished in about 5 min run time, as there is A1.3.1 A short partition column can be used advantageously
no need to reverse the flow on the reference standard. Make to separate heavy-end components and obtain a more detailed
calculations in the same manner as for the complete analysis breakdown on composition of the reverse-flow fractions. This
method. information provides quality data and a basis for calculating
physical properties such as molecular weight on these frac-
A1.1.3 A determination of propane, isobutane, n-butane, tions.
and pentanes and heavier can be made in about 5 min run time
by reversing the carrier-gas flow after n-butane. However, it is A1.3.2 Fig. A1.1 is a chromatogram that shows components
necessary to know the average molecular weight of the that are separated by a 2 m BMEE column in 20 min. To make
pentanes and heavier components. this determination, enter a 5 mL sample into the short column
and reverse the carrier gas after the separation of n-heptane.
A1.2 Single-Run Analysis for Ethane and Heavier Compo- Measure areas of all peaks eluted after n-pentane. Correct each
nents peak area to the mol basis by dividing each peak area by the
A1.2.1 In many cases, a single partition run using a sample molecular weight of the component. A value of 120 may be
size in the order of 1 to 5 mL will be adequate for determining used for the molecular weight of the octanes and heavier
all components except methane, which cannot be determined reverse-flow peak. Calculate the mole percent of the hexanes
accurately using this size sample with peak height and heavier components by adding the corrected areas and
measurements, because of its high concentration. dividing to make the total 100 %.
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10
Order Number: 02085540
D1945 − 14
FIG. A1.1 Composition of Hexanes and Heavier Fraction
A2. PREPARATION OF COLUMNS AND DRIER
A2.1 Preparation of Columns—See Practice E260. sulfate in the line upstream of both the chromatograph and
drying tube. This procedure will remove small amounts of
A2.2 Preparation of Drier—Fill a 10 mm diameter by 100 hydrogen sulfide while having but minimal effect on the carbon
mm length glass tube with granular phosphorus pentoxide or dioxide in the sample.
magnesium perchlorate, observing all proper safety precau-
tions. Mount as required to dry the sample. Replace the drying A2.4 Column Arrangement—For analyses in which
agent after about one half of the material has become spent. hexanes and heavier components are to be determined, Fig.
A2.1 shows an arrangement whereby columns can be quickly
A2.3 Removal of Hydrogen Sulfide:
and easily changed by the turn of a selector valve. Two
A2.3.1 For samples containing more than about 300 ppm by columns are necessary to determine all of the components
mass hydrogen sulfide, remove the hydrogen sulfide by con- covered in this test method. However, short and long partition
necting a tube of sodium hydrate absorbent (Ascarite) ahead of columns provide the flexibility of three partition column
the sample container during sampling, or ahead of the drying lengths, by using them either singly or in series. The connec-
tube when entering the sample into the chromatograph. This tion between V1 and V2 in Fig. A2.1 should be as short as
procedure also removes carbon dioxide, and the results ob- possible (20 mm is practical) to minimize dead space between
tained will be on the acid-gas free basis. the columns when used in series. If all columns are chosen to
A2.3.2 Hydrogen sulfide may also be removed by connect- operate at the same temperature, then stabilization time be-
ing a tube of pumice that has been impregnated with cupric tween changing columns will be minimized.
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D1945 − 14
FIG. A2.1 Column Arrangement
APPENDIXES
(Nonmandatory Information)
X1. REFERENCE STANDARD MIXTURE
X1.1 Preparation dioxide. The pure components should be 99+ % pure. Methane
X1.1.1 Gas mixtures of the following typical compositions should be in a 1 L cylinder at 10 MPa) pressure. Run a
will suffice for use as reference standards for most analytical chromatogram of each component to check on its given
requirements (Note X1.1): composition.
Lean Gas, mol Rich Gas, mol
X1.1.2.2 Evacuate the 20 L cylinder for several hours.
Component Evacuate 100 mL Cylinder A, and obtain its true weight.
% %
Connect Cylinder A to a cylinder of pure n-pentane with a
Helium 1.0 0.5
metal connection of calculated length to contain approximately
--```````,`,,`,`,`,,`,,-`-``,```,,,`---
Hydrogen 3.0 0.5
Nitrogen 4.0 0.5 the amount of n-pentane to be added. Flush the connection with
Methane (maximum) 85 74 the n-pentane by loosening the fitting at the valve on Cylinder
Ethane 6.0 10
Carbon dioxide 1.0 1.0 A. Tighten the fitting. Close the n-pentane cylinder valve and
Propane 4.0 7.0 open Cylinder A valve to admit the n-pentane from the
Isobutane 2.0 3.0
n-Butane 2.0 3.0
connection and then close the valve on Cylinder A. Disconnect
Neopentane 0.5 1.0 and weigh Cylinder A to obtain the weight of n-pentane added.
Isopentane 0.5 1.0 X1.1.2.3 Similarly, add isopentane, n-butane, isobutane,
n-Pentane 0.5 1.0
Hexanes+ 0.1 0.2 propane, ethane, and carbon dioxide, in that order, as desired,
in the reference standard. Weigh Cylinder A after each addition
NOTE X1.1—If the mixture is stored under pressure, take care to ensure
that the partial pressure of any component does not exceed its vapor to obtain the weight of the component added. Connect Cylinder
pressure at the temperature and pressure at which the sample is stored and A to the evacuated 20 L cylinder with as short a clean,
used. The lean mixture has a cricondentherm at 15.6 °C and the rich small-diameter connector as possible. Open the valve on the 20
mixture has a cricondentherm at 37.8 °C. L cylinder, then open the valve on Cylinder A. This will result
X1.1.2 A useful method for preparation of a reference in the transfer of nearly all of the contents of Cylinder A into
standard by weight is as follows:3 the 20 L cylinder. Close the cylinder valves, disconnect, and
X1.1.2.1 Obtain the following equipment and material: weigh Cylinder A to determine the weight of mixture that was
Cylinder, 20 L not transferred to the 20 L cylinder.
Pressure Cylinders, two 100 mL (A and B) X1.1.2.4 Evacuate and weigh 100 mL Cylinder B. Then fill
Balance, 2000 g capacity, sensitivity of 10 mg. Cylinder B with helium and hydrogen respectively to the
Pure Components, methane through n-pentane, and carbon pressures required to provide the desired concentrations of

12
D1945 − 14
these components in the final blend. (Helium and hydrogen are where:
prepared and measured separately from the other components C = component concentration, mol;
to prevent their pressures, while in the 100-mL cylinder, from A = peak height of component in blend;
causing condensation of the higher hydrocarbons.) Weigh B = peak height of pure component;
Cylinder B after each addition to obtain the weight of the Pa = pressure at which blend is run, kPa;
component added. Connect Cylinder B to the 20 L cylinder Pb = pressure at which component is run, kPa; and
with as short a clean, small-diameter connector as possible. Vf = volume fraction of pure component.
Open the valve on the 20 L cylinder, then open the valve on NOTE X1.3—Vf = 1.000 if the calibration component is free of impu-
rities.
Cylinder B, which will result in the transfer of nearly all of the
contents of Cylinder B into the 20 L cylinder. Close the X1.2.5.3 Normalize values to 100.0 %.
cylinder valves, disconnect, and weigh Cylinder B to obtain the
weight of the mixture that was not transferred to the 20 L X1.3 Calibration using Relative Molar Response Values
cylinder. X1.3.1 Relative response ratios can be derived from linear-
X1.1.2.5 Weigh a 1 L cylinder containing pure methane at ity data and used for calculating response factors. This elimi-
about 10 MPa pressure. Transfer the methane to the 20 L nates the need for a multicomponent standard for daily
--```````,`,,`,`,`,,`,,-`-``,```,,,`---
cylinder until the pressure equalizes. Weigh the 1 L cylinder to calibration. The test method can be used on any gas chromato-
determine the weight of methane transferred. graph using a thermal conductivity or thermistor detector.
X1.1.2.6 Thoroughly mix the contents of the 20 L cylinder X1.3.2 Obtain a blend that brackets the expected concen-
by heating at the bottom by a convenient means such as hot tration the instrument will be analyzing. The major component
water or a heat lamp, and leaving the cylinder in a vertical (methane) is used as the balance gas and may fall below the
position for at least 6 h. expected concentration. This component is present in the daily
X1.1.2.7 Use the weights and purities of all components calibration standard and linearity is assured from previous
added to calculate the weight composition of the mixture. tests.
Convert the weight percent to mole percent. X1.3.3 Inject the sample at reduced pressures using the
apparatus in Fig. 1 or using a mechanical gas blender. Obtain
X1.2 Calibration with Pure Components repeatable peak areas or height at 90, 75, 60, 45, 30, and 15 %
X1.2.1 Use helium carrier gas to admit a sample volume of of absolute pressure. For 100 kPa, the pressures used are 90
0.25 to 0.5 mL into the adsorption column, providing methane kPa, 75 kPa, 60 kPa, 45 kPa, 30 kPa, 15 kPa.
at 50 kPa and nitrogen at 10 kPa absolute pressure. Run a X1.3.4 Plot the area or height (attenuated at the same height
sample of the standard mixture at 70 kPa pressure and obtain as the reference component) versus concentration and calculate
peaks for methane and nitrogen. the slope of the line by the least squares method. Given the
NOTE X1.2—Each run made throughout this procedure should be
equation of the line as Y = a0 + a1 X where Y represents the
repeated to ensure that peak heights are reproducible after correction for area or height points and X the concentration points. The line
pressure differences to within 1 mm or 1 % of the mean value. All peaks is assumed to intersect through the origin and a0 = 0. The slope
should be recorded at an instrument attenuation that gives the maximum a1 can be calculated by:
measurable peak height.
X1.2.2 Change the carrier gas to argon or nitrogen and, after a1 5 ( XY (X1.2)
the base line has stabilized, enter a sample of pure helium at
~( Y!2
7 kPa absolute pressure, recording the peak at an attenuation X1.3.5 Ratio the slopes of the referenced components (i) to
that allows maximum peak height. Run a sample of the mixture the slopes of the reference components (r) present in the daily
at 70 kPa absolute pressure and obtain the helium peak. calibration standard. This gives the Relative Molar Response
factor (RMRi) for component (i). The reference component
X1.2.3 Switch to the partition column with helium carrier must be present in the same instrumental sequence (except
gas, and run the gas mixture at 70 kPa absolute pressure. Then Hexanes+) as the referenced components. For instance, pro-
admit samples of pure ethane and propane at 10 kPa absolute pane can be the reference component for the butanes and
pressure, and butanes, pentanes, and carbon dioxide at 5 kPa pentanes if propane is separated on the same column in the
absolute pressure. same sequence as the butanes and pentanes. Ethane can be the
X1.2.4 Run the gas mixture at 70 kPa absolute pressure. reference component for carbon dioxide if it elutes in the same
sequence as carbon dioxide. The hexanes + peak can be refer-
X1.2.5 Calculate the composition of the prepared gas mix- enced to propane or calculated as mentioned in the body of the
ture as follows: standard.
X1.2.5.1 Correct peak heights of all pure components and
X1.3.6 For daily calibration, a four-component standard is
the respective components in the blend to the same attenuation
used containing nitrogen, methane, ethane, and propane. The
(Note X1.2).
fewer components eliminates dew point problems, reactivity, is
X1.2.5.2 Calculate the concentration of each component as more accurate and can be blended at a higher pressure. The
follows: referenced components’ response factors are calculated from
C 5 ~ 100V f !~ A/B !~ P b /P a ! (X1.1) the current reference factor and the Relative Molar Response

13
D1945 − 14
TABLE X1.1 Least Square Calculation for Slope of Iso-Butane Mole %
Response Factor ~ R ! 5 , (X1.3)
Area Mole % Area
2
Y X XY Y
Mole % ~ i ! /Area~ i !
984 515 1 984 515 9.693e + 11 Relative Molar Response ~ RMRi ! 5 (X1.4)
900 410 0.9 810 369 8.107e + 11 Mole % ~ r ! /Area~ r !
758 917 0.75 569 187.75 5.670e + 11
611 488 0.6 366 892.8 3.739e + 11
R iC4 5 RMRic4 3 R C 3 (X1.5)
466 037 0.45 209 716.65 2.172e + 11
314 649 0.3 94 394.7 9.900e + 10 X1.3.7 Periodic checks of the RMR relationship is recom-
159 303 0.15 23 895.45 2.538e + 10 mended. The relationship is independent of temperature,
sample size, and carrier gas flow rate. If changes occur in these
--```````,`,,`,`,`,,`,,-`-``,```,,,`---
sum = 4 195 319 4.15 3 058 971.35 3.071 452e + 12
operating conditions, all of the components will be affected
2
slope = ^XY/^Y 9.9594e-07 equally and the calculated response factors will shift accord-
ingly. See Table X1.1 and Fig. X1.1 and Table X1.2.
factor. Following is a description of the basic calculations, an
example of deriving a Relative Molar Response factor (Fig.
X1.1), and a table showing how response factors are calculated
(Table X1.2).
FIG. X1.1 Example of Deriving a Relative Molar Response Factor

14
D1945 − 14
TABLE X1.2 Calculation of Response Factors Using Relative Molar Response Values
Mole % in Response of Response Factor Relative MolarA Response Factor
Reference Reference From Reference Response from of Referenced
Component
Standard Standard Standard Slopei/Ki Components
S B S/B,K RMRi (RMRi)x(Ki)
Nitrogen 5.08 2 685 885 1.8914E-6
Methane 82.15 36 642 384 2.2419E-6
Ethane 8.75 6 328 524 1.3826E-6
Propane 4.02 3 552 767 1.1315E-6
Carbon dioxide 1.116 07c2 1.5429E-6
Isobutane 0.729 58c3 9.9594E-7
n-Butane 0.693 10c3 9.1142E-7
Neopentane 0.682 71c3 8.9776E-7
Isopentane 0.638 74c3 8.3994E-7
n-Pentane 0.600 41c3 7.8953E-7
Hexanes+ 0.547 62c3 7.2012E-7
A
The Relative Molar Response is a constant that is calculated by dividing the slope of the referenced component by the component that is present in the reference standard.
For example:
RMRic4 5 s slopeic4 d / s Kc 3 d 5 9.9594E 2 7 1.1315E 2 6 5 0.729 58
--```````,`,,`,`,`,,`,,-`-``,```,,,`---
X2. SAMPLE CALCULATIONS (SEE SECTION 9)
TABLE X2.1 Sample Calculations

Mol % in
Response of Reference Response Percent
Component Reference Response for Sample,A A Normalized, %
Standard, B Factor, S/B C = (S × A) ⁄ B
Standard, S
Helium 0.50 41.1 0.0122 12.6 0.154 0.15
Hydrogen 0.74 90.2 0.0082 1.5 0.012 0.01
Oxygen 0.27 35.5 0.0076 2.1 0.016 0.02
Nitrogen 4.89 77.8 0.0629 75.6 4.755 4.75
Methane 70.27 76.4 0.9198 90.4 83.150 83.07
Ethane 9.07 96.5 0.0940 79.0 7.426 7.42
Carbon dioxide 0.98 57.5 0.0170 21.2 0.360 0.36
Propane 6.65 55.2 0.1205 20.6 2.482 2.48
Isobutane 2.88 73.2 0.0393 11.0 0.432 0.43
n-Butane 2.87 60.3 0.0476 15.0 0.714 0.71
Neopentane 0.59 10.4 0.0567 0.1 0.006 0.01
Isopentane 0.87 96.0 0.0091 24.0 0.218 0.22
n-Pentane 0.86 86.8 0.0099 20.5 0.203 0.20
Hexanes+B 72.1C 0.166D 0.17
100.094 % 100.00 %
A
The response for a constituent in the sample has been corrected to the same attenuation as for that constituent in the reference standard.
B
Average molecular weight of C6 + = 92.
C
Corrected C6 response = (original response of 92.1) × (72 ⁄ 92) = 72.1.
D
Mol % C6 + = (0.218 + 0.203) × (72.1) ⁄ (96.0 + 86.8) = 0.166.
% iC5 % nC5 Areas iC + nC5

15
D1945 − 14
X3. PRECAUTIONS FOR AVOIDING COMMON CAUSES OF ERRORS
X3.1 Hexane and Heavier Content Change X3.5.3 Be sure that the inlet drier is in good condition.
X3.1.1 The amounts of heavy-end compounds in natural gas Moisture on the column will enlarge the reverse flow peak.
are easily changed during handling and entering of samples to X3.5.4 Be sure the column is clean by occasionally giving it
give seriously erroneous low or high values. Concentration of several hours’ sweep of carrier gas in reverse flow direction. A
these components has been observed to occur in a number of level baseline should be quickly attained in either flow direc-
cases because of collection of heavier components in the tion if the column is clean.
sample loop during purging of the system. The surface effect of X3.5.5 When the reverse flow valve is turned, there is a
small diameter tubing acts as a separating column and must not reversal of pressure conditions at the column ends that upsets
be used in the sampling and entering system when components the carrier gas flow. This flow should quickly return to the same
heavier than pentanes are to be determined. An accumulation flow rate and the baseline level out. If it does not, the cause
of oily film in the sampling system greatly aggravates this may be a leak in the carrier gas system, faulty flow regulator,
problem. Also, the richer the gas, the worse the problem. or an unbalanced condition of the column or plumbing.
Periodically, check C6 and heavier repeatability of the appara-
tus by making several check runs on the same sample. It is X3.6 Reference Standard
helpful to retain a sample containing some hexanes and heavier X3.6.1 Maintain the reference standard at +15 °C or a
for periodic checking. When enlargement of the heavy end temperature that is above the hydrocarbon dew point. If the
peaks is noted, thoroughly clean the sampling valve and loop reference standard should be exposed to lower temperatures,
with acetone. This trouble has been experienced with some heat at the bottom for several hours before removing a sample.
inlet systems even when clean and with the specified sample If in doubt about the composition, check the n-pentane and
loop size. This contamination can be minimized by such isopentane values with pure components by the procedure
techniques as purging with inert gas, heating the sample loop, prescribed in Annex A2.
using a vacuum system, or other such effective means.
--```````,`,,`,`,`,,`,,-`-``,```,,,`---
X3.7 Measurements
X3.2 Acid Gas Content Change
X3.7.1 The baseline and tops of peaks should be plainly
X3.2.1 The carbon dioxide and hydrogen sulfide contents of visible for making peak height measurements. Do not use a
gas are easily altered during sampling and handling. If samples fixed zero line as the baseline, but use the actual observed
containing carbon dioxide or hydrogen sulfide, or both, are to baseline. On high sensitivity, this baseline may drift slightly
be taken, use completely dry sample cylinders, connections, without harm and it need not frequently be moved back to zero.
and lines, as moisture will selectively absorb appreciable A strip-chart recorder with an offset zero is desirable. The area
amounts of the acid gases. If hydrogen is present, use of reverse flow peak may be measured by planimeter or
aluminum, stainless steel, or other materials inert to hydrogen geometric construction. The reverse flow area, and the pen-
sulfide for the cylinder, valves, lines, and connections. tanes peaks used for comparison, should be measured by the
X3.3 Sample Dew Point same method. That is, use either geometric construction or
planimeter, but do not intermix. When a planimeter is used,
X3.3.1 Nonrepresentative samples frequently occur because carefully make several tracings and use the average. Check this
of condensation of liquid. Maintain all samples above the average by a second group of tracings.
hydrocarbon dew point. If cooled below this, heat 10 °C or
more above the dew point for several hours before using. If the X3.8 Miscellaneous
dew point is unknown, heat above the sampling temperature. X3.8.1 Moisture in the carrier gas that would cause trouble
X3.4 Sample Inlet System on the reverse flow may be safeguarded against by installing a
cartridge of molecular sieves ahead of the instrument. Usually
X3.4.1 Do not use rubber or plastic that may preferentially 1 m of 6 mm tubing packed with 30- to 60-mesh molecular
adsorb sample components. Keep the system short and the sieves is adequate, if changed with each cylinder of carrier gas.
drier small to minimize the purging required.
X3.8.2 Check the carrier gas flow system periodically for
X3.5 Sample Size Repeatability leaks with soap or leak detector solution.
X3.5.1 Varying back pressures on the sample loop may X3.8.3 Use electrical contact cleaner on the attenuator if
impair sample size repeatability. noisy contacts are indicated.
X3.5.2 Make it a practice to make all reverse flow determi- X3.8.4 Peaks with square tops with omission of small peaks
nations in the same carrier gas flow direction. All single-peak can be caused by a sluggish recorder. If this condition cannot
determinations and corresponding reference runs will then be be remedied by adjustment of the gain, check the electronics in
made in the same carrier gas flow direction. the recorder.

16
D1945 − 14
SUMMARY OF CHANGES
Committee D03 as identified the location of selected changes to this standard since the last issue
(D1945–96(2010)) that may impact the use of this standard.
(1) Subsection 5.11 was rewritten to allow the use of any (3) References to pressure in mm Hg have been removed and
vacuum gauge, including mercury manometers. replaced with the SI unit Pascal.
(2) Fig. 1 replaced. (4) All non-SI units removed.
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.
This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
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--```````,`,,`,`,`,,`,,-`-``,```,,,`---

17

ASTM D1945-14 Análisis de Gas Por Cromat

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Designation: D1945 − 14

Standard Test Method for

1. Scope* composition of the sample is calculated by comparing either

*A Summary of Changes section appears at the end of this standard

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FIG. 1 Suggested Manifold Arrangement for Entering Vacuum Samples

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mined in the analysis. pressibility at pressures less than atmospheric.

FIG. 2 Calculation for Resolution

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FIG. 4 Chromatogram of Natural Gas (BMEE Column) (See Annex A2)

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FIG. 6 Chromatogram of Natural Gas (See Annex A2)

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FIG. 7 Chromatogram of Natural Gas (Multi-Column Application) (See Annex A2)

FIG. 8 Separation of Helium and Hydrogen

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FIG. 9 Linearity of Detector Response

TABLE 2 Linearity Evaluation of Methane TABLE 3 Linearity Evaluation for Nitrogen

information on the linearity of the available gas chromatograph

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where: 10. Precision

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A1. SUPPLEMENTARY PROCEDURES

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FIG. A1.1 Composition of Hexanes and Heavier Fraction

A2. PREPARATION OF COLUMNS AND DRIER

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FIG. A2.1 Column Arrangement

X1. REFERENCE STANDARD MIXTURE

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FIG. X1.1 Example of Deriving a Relative Molar Response Factor

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X2. SAMPLE CALCULATIONS (SEE SECTION 9)

TABLE X2.1 Sample Calculations

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X3. PRECAUTIONS FOR AVOIDING COMMON CAUSES OF ERRORS

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