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2720

Anaerobic Sludge Digester Gas Analysis

Approved by Standard Methods Committee, 2009. Editorial revisions, 2021.

2720  A. Introduction

Gas produced during the anaerobic decomposition of wastes


contains methane (CH4) and carbon dioxide (CO2) as the major
components with minor quantities of hydrogen (H2), hydrogen
sulfide (H2S), nitrogen (N2), and oxygen (O2). It is saturated with
water vapor. Common practice is to analyze the gases produced
to estimate their fuel value and to check on the treatment process.
The relative proportions of CO2, CH4, and N2 are normally of
most concern and the easiest to determine because of the rela-
tively high percentages of these gases.

1. Selection of Method

Two procedures are described for gas analysis, the volumetric


method (B), and the gas chromatographic method (C). The volu-
metric analysis is suitable for the determination of CO2, H2, CH4,
and O2. Nitrogen is estimated indirectly by difference. Although
the method is time-consuming, the equipment is relatively simple.
Because no calibration is needed before use, the procedure is par-
ticularly appropriate when analyses are conducted infrequently.
The principal advantage of gas chromatography is speed.
Commercial equipment is designed specifically for isothermal
or temperature-programmed gas analysis and permits the routine
separation and measurement of CO2, N2, O2, and CH4 in less than
15 to 20 min. The requirements for a recorder, pressure-regulated
bottles of carrier gas, and certified standard gas mixtures for cal-
ibration raise costs to the point where infrequent analyses by this
Figure 2720:1. Gas collection apparatus.
method may be uneconomical. The advantages of this system are
freedom from the cumulative errors found in sequential volumet- the tube. If the gas supply is limited, fill the gas sampling bulb
ric measurements, adaptability to other gas component analyses, (tube) with an acidic salt solution.9 Then completely displace the
adaptability to intermittent on-line sampling and analysis, and the acidic salt solution in the gas sampling bulb (tube) with the sam-
use of samples of 1 mL or less.1-8 ple gas. Because the acidic salt solution absorbs gases to some
extent, fill the gas sampling bulb completely with the gas and seal
2. Sample Collection off from any contact with displacement fluid during temporary
storage. When transferring gas to the gas-analyzing apparatus, do
When the source of gas is some distance from the apparatus not transfer any fluid.
used for analysis, collect samples in sealed containers and bring
to the instrument. Displacement collectors are the most suitable References
containers. Glass sampling bulbs (or tubes) with 3-way glass or
PTFE stopcocks at each end, as indicated in Figure 2720:1, are 1. Grune WN, Chueh CF. Sludge gas analyses using gas chromatogra-
particularly useful. These also are available with centrally located phy. Water Sewage Works. 1962;109:468–473.
ports provided with septa for syringe transfer of samples. Replace 2. Grune WN, Chueh CF. Sludge gas analyses using gas chromatogra-
septa periodically to prevent contamination by atmospheric phy. Water Sewage Works. 1963;110:43–48.
gases. Connect one end of collector to gas source and vent the 3. Grune WN, Chueh CF. Sludge gas analyses using gas chromatogra-
3-way stopcock to the atmosphere. Clear the line of air by pass- phy. Water Sewage Works. 1963;111:77–81.
ing 10 to 15 volumes of gas through the vent and open the stop- 4. Grune WN, Chueh CF. Sludge gas analyses using gas chromatogra-
phy. Water Sewage Works. 1963;112:102–107.
cock to admit the sample. If large quantities of gas are available,
5. Grune WN, Chueh CF. Sludge gas analyses using gas chromatogra-
sweep the air away by passing 10 to 15 volumes of gas through phy. Water Sewage Works. 1963;113:127–129.

https://doi.org/10.2105/SMWW.2882.036 1
2720 ANAEROBIC SLUDGE DIGESTER GAS ANALYSIS - B. Volumetric Method

6. Grune WN, Chueh CF. Sludge gas analyses using gas chromatogra- 8. Grune WN, Chueh CF. Sludge gas analyses using gas chromatogra-
phy. Water Sewage Works. 1963;114:171–174. phy. Water Sewage Works. 1963;116:254–256.
7. Grune WN, Chueh CF. Sludge gas analyses using gas chromatogra- 9. Chin KK, Wong KK. Thermophilic anaerobic digestion of palm oil
phy. Water Sewage Works. 1963;115:220–224. mill effluent. Water Res. 1983;17(9):993–995.

2720  B. Volumetric Method

1. General Discussion c. Oxygen gas: Use approximately 100 mL for each gas sample
analyzed.
a. Principle: This method may be used for the analysis either d. Displacement liquid (acidic salt solution): Dissolve 200 g
of digester gas or of methane in water (see Section 6211 Meth- Na2SO4 in 800 mL reagent water; add 30 mL conc H2SO4. Add
ane). A measured volume of gas is passed first through a solution a few drops of methyl orange indicator. When color fades, replace
of potassium hydroxide (KOH) to remove CO2, next through a solution.
solution of alkaline pyrogallol to remove O2, and then over heated
cupric oxide, which removes H2 by oxidation to water. After each 4. Procedure
of the above steps, the volume of gas remaining is measured; the
decrease that results is a measure of the relative percentage of vol- a. Sample introduction: Transfer 5 to 10 mL gas sample into
ume of each component in the mixture. Finally, CH4 is determined the gas buret through a capillary-tube connection to the collector.
by conversion to CO2 and H2O in a slow-combustion pipet or a Expel this sample to the atmosphere to purge the system. Transfer
catalytic oxidation assembly. The volume of CO2 formed during up to 100 mL gas sample to the buret. Bring the sample in the
combustion is measured to determine the fraction of methane orig- buret to atmospheric or reference pressure by adjusting the level-
inally present. Nitrogen is estimated by assuming that it represents ing bulb. Measure the volume accurately and record as V1.
the only gas remaining and equals the difference between 100% b. Carbon dioxide absorption: Remove CO2 from the sample
and the sum of the measured percentages of the other components. by passing it through the CO2-absorption pipet charged with the
When only CO2 is measured, report only CO2. No valid KOH solution. Pass the gas back and forth until the sample vol-
assumptions may be made about the remaining gases present ume remains constant. Before opening the stopcocks between
without making a complete analysis. the buret and any absorption pipet, make sure that the gas in the
Follow the equipment manufacturers’ recommendations with buret is under a slight positive pressure to prevent the reagent
respect to oxidation procedures. in the pipet from contaminating the stopcock or manifold. After
Caution: Do not attempt any slow-combustion procedure absorption of CO2, transfer the sample to the buret and measure
on digester gas because of the high probability of exceeding the volume. Record as V2.
the explosive 5% by volume concentration of CH4. c. Oxygen absorption: Remove O2 by passing the sample
b. Quality control (QC): The QC practices considered to be an through an O2-absorption pipet charged with alkaline pyrogallol
integral part of each method are summarized in Tables 2020:1 reagent until the sample volume remains constant. Measure the
and 2020:2. volume and record as V3 . For digester gas samples, continue as
directed in paragraph d below. For CH4 in water, store the gas in
2. Apparatus the CO2 pipet and proceed to paragraph e below.
d. Hydrogen oxidation: Remove H2 by passing the sample
Orsat-type gas-analysis apparatus, consisting of at least: through the CuO assembly maintained at a temperature in the
• a water-jacketed gas buret with leveling bulb; range 290 to 300 °C. When a constant volume has been obtained,
• a CO2-absorption pipet; transfer the sample back to the buret, cool, and measure the vol-
• an O2-absorption pipet; ume. Record as V4.
• a cupric oxide-hydrogen oxidation assembly; Waste to the atmosphere all but 20 to 25 mL of the remaining
• a shielded catalytic CH4-oxidation assembly or slow-com- gas. Measure the volume and record as V5. Store temporarily in
bustion pipet assembly; and the CO2- absorption pipet.
• a leveling bulb. With the slow-combustion pipet use a controlled e. Methane oxidation: Purge the inlet connections to the buret
source of current to heat the platinum filament electrically. with O2 by drawing 5 to 10 mL into the buret and expelling to the
Preferably use mercury as the displacement fluid; alternatively atmosphere. Oxidize CH4 either by the catalytic oxidation pro-
use aqueous Na2SO4-H2SO4 solution for sample collection. Use cess for digester gas and gas phase of water samples or by the
any commercially available gas analyzer having these units. slow-combustion process for the gas phase of water samples.
1) Catalytic oxidation process—For the catalytic oxidation of
3. Reagents digester gas and gas phase of water samples, transfer 65 to 70 mL
O2 to the buret and record this volume as V6. Pass O2 into the
a. Potassium hydroxide solution: Dissolve 500 g KOH in dis- CO2-absorption pipet so that it will mix with the sample stored
tilled water and dilute to 1 L. there. Return this mixture to the buret and measure the volume.
b. Alkaline pyrogallol reagent: Dissolve 30 g pyrogallol (also Record as V7. This volume should closely approximate V5 plus V6.
called pyrogallic acid) in reagent water and make up to 100 mL. Pass the O2-sample mixture through the catalytic oxidation assem-
Add 500 mL KOH solution. bly, which should be heated in accordance with the manufacturer’s

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2720 ANAEROBIC SLUDGE DIGESTER GAS ANALYSIS - C. Gas Chromatographic Method

directions. Keep the rate of gas passage less than 30 mL/min. b. Alternatively, calculate CH4 by either of the 2 following
After the first pass, transfer the mixture back and forth through the equations:
assembly between the buret and the reservoir at a rate not faster
than 60 mL/min until a constant volume is obtained. Record as V8. V ×(V6 + V10 − V9 )× 100
2) Slow-combustion process—For the slow combustion of the % CH 4 = 4
2 × V1 × V5
gas phase of water samples, transfer 35 to 40 mL O2 to the buret and
record the volume as V6. Transfer the O2 to the slow-combustion V ×(V7 − V9 )× 100
% CH 4 = 4
pipet and then transfer the sample from the CO2-absorption pipet 2 × V1 × V5
to the buret. Heat the platinum coil in the combustion pipet to
yellow heat while controlling the temperature by adjusting the Results from the calculations for CH4 by the 3 equations
current. Reduce the pressure of O2 in the pipet to somewhat less should be in reasonable agreement. If not, repeat the analysis after
than atmospheric pressure by means of the leveling bulb attached checking the apparatus for the sources of error, such as leaking
to the pipet. Pass the sample into the slow-combustion pipet at stopcocks or connections. Other combustible gases, such as eth-
rate of approximately 10 mL/min. After the first pass, transfer ane, butane, or pentane, will cause a lack of agreement among the
the sample and O2 mixture back and forth between the pipet and calculations; however, the possibility that digester gas contains a
buret several times at a faster rate, allowing the mercury in the significant amount of any of these is remote.
pipet to rise to a point just below heated coil. Collect the sample
in the combustion pipet, turn off the coil, and cool the pipet and
6. Precision and Bias
sample to room temperature with a jet of compressed air. Transfer
the sample to the buret and measure the volume. Record as V8.
A gas buret measures gas volume with a precision of 0.05 mL
f. Measurement of carbon dioxide produced: Determine the
and a probable accuracy of 0.1 mL. With the large fractions of
amount of CO2 formed in the reaction by passing the sample
CO2 and CH4 normally present in digester gas, the overall error
through the CO2-absorption pipet until the volume remains constant.
for their determination can be made less than 1%. The error in
Record the volume as V9. Check the accuracy of determination by
the determination of O2 and H2, however, can be considerable
absorbing residual O2 from the sample. After this absorption,
because of the small concentrations normally present. For a con-
record the final volume as V10.
centration as low as 1%, an error as large as 20% can be expected.
When N2 is present in a similar low-volume percentage, the error
5. Calculation in its determination would be even greater, because errors in each
of the other determinations would be reflected in the calculation
a. CH4 and H2 usually are the only combustible gases present for N2.
in sludge digester gas. When this is the case, determine the per-
centage by volume of each gas as follows:
Bibliography

(V1 − V2 )×100 Yant WF, Berger LB. Sampling of mine gases and the use of the Bureau
% CO2 =
V1 of Mines portable Orsat apparatus in their analysis; Miner’s Circ. No.
(V2 − V3 )×100 34. Washington DC: U.S. Bureau of Mines, 1936.
% O2 = Mullen PW. Modern gas analysis. New York (NY): Interscience Publish-
V1 ers; 1955.
(V3 − V4 )×100
% H2 =
V1
V ×(V8 − V9 )×100
% CH 2 = 4
V1 ×V5
% N 2 = 100 − (% CO2 + % O2 + % H 2 + % CH 4 )

2720 C. Gas Chromatographic Method

1. General Discussion controllers, injector and column temperature setting dials, TCD
current controller, attenuator, carrier-gas pressure gauge, injec-
See Section 6010 C for discussions of gas chromatography. tion port, signal output, and power switch. Some columns require
The quality control practices considered to be an integral part temperature programming while others are isothermal. Preferably
of each method are summarized in Tables 2020:1 and 2020:2. use a unit with a gas sampling loop and valve that allow automatic
injection of a constant sample volume.
2. Apparatus b. Sample introduction apparatus: An instrument equipped with
gas-sampling valves is designed to permit the automatic injection
a. Gas chromatograph: Use any instrument system equipped of a specific sample volume into the chromatograph. If such an
with a thermal conductivity detector (TCD), carrier-gas flow instrument is not available, introduce samples with a 2-mL syringe

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2720 ANAEROBIC SLUDGE DIGESTER GAS ANALYSIS - C. Gas Chromatographic Method

fitted with a 27-gauge hypodermic needle. Reduce the escape of an 8.5% hydrogen–91.5% helium carrier gas mixture.7 To detect
gas by greasing the plunger lightly with mineral oil or preferably trace quantities of hydrogen use argon or nitrogen as carrier gas.1
by using a special gas-tight syringe. One-step separation of oxy- b. Calibration gases: Use samples of CH4, CO2, and N2 of
gen, nitrogen, methane, and carbon dioxide may be accomplished known purity, or gas mixtures of certified composition, for cali-
in concentric columns (column within a column) under isothermal bration. Also use samples of O2, H2, and H2S of known purity if
conditions at room temperature instead of performing 2 column these gases are to be measured. Preferably use custom-made gas
analyses. These concentric columns permit the simultaneous use mixtures to closely approximate digester gas composition.
of 2 different packings for the analysis of gas samples. c. Displacement liquids: See 2720 B.3d.
c. Chromatographic column: Select the column on the basis
of manufacturer’s recommendations. Report the column and 4. Procedure
packing specifications and conditions of analyses with results.
Note: Gas chromatographic methods are extremely sensitive to a. Preparation of gas chromatograph: Open the main valve of
the materials used. The use of trade names in Standard Methods the carrier-gas cylinder and adjust the carrier-gas flow rate to rec-
does not preclude the use of other existing or as-yet-undeveloped ommended values. To obtain accurate flow measurements, con-
products that give demonstrably equivalent results. Commercially nect a soap-film flow meter to the TCD vent. Turn the power on.
available columns (and gases they separate) include: Turn on oven heaters, if used, and the detector current and adjust
Silica gel and activated alumina: to desired values.
• Silica gel: H2, air (O2 + N2), CO, CH4, C2H6. Set the injection port and column temperatures as specified for the
• Activated alumina: air (O2 + N2), CH4, C2H6, C3H8. column being used. Set the TCD current. Turn on the recorder or data
Molecular sieves (zeolites): processor. Check that the injector or detector temperature has risen
• Molecular sieve 5A: H2, (O2 − Ar), N2, CH4, CO. to the appropriate level and confirm that the column temperature is
• Molecular sieve 13X: O2, N2, CH4, CO. stabilized. Set the range and attenuation at appropriate positions.
Porous polymers: The instrument is ready for use when the recorder yields a stable
• Chromosorb 102: air (H2, O2, N2, CO), CH4, CO2. base line. Silica gel and molecular sieve columns gradually lose
Porapak Q: (air–CO), CO2. activity because of adsorbed moisture or materials permanently
• HayeSep Q: H2, air (O2 + N2), CH4, CO2, C2H6, H2S. adsorbed at room temperature. If insufficient separations occur,
Carbon molecular sieves: reactivate by heating or repacking.
• Carbosphere: O2, N2, CO, CH4, CO2, C2H6 (these gases b. Calibration: For accurate results, prepare a calibration curve
can be eluted isothermally at various temperatures or by tem- for each gas to be measured because different gas components
perature programming). do not give equivalent detector responses on either a weight or a
• Carbosieve S-II: H2, air (O2 + N2), CO, CH4, CO2, C2H6 molar basis. Calibrate with synthetic mixtures or with pure gases.
(temperature programming required). 1) Synthetic mixtures—Use purchased gas mixtures of certified
A 2-column system usually is required. A molecular sieve composition or prepare in the laboratory. Inject a standard volume
column separates H2, O2, N2, CO, and CH4 isothermally, but of each mixture into the gas chromatograph and note the response
because CO2 is adsorbed by the molecular sieve, a second column for each gas. Compute the detector response, either as area under
is needed to complete the analysis. A commonly used 2-column a peak or as height of peak, after correcting for attenuation. Read
system uses a Chromosorb 102 column and a Molecular Sieve peak heights accurately and correlate with the concentration of
5A or 13X column to separate H2, O2, N2, CH4, and CO2 iso- the component in the sample. Reproduce the operating parameters
thermally.1,2 exactly from one analysis to the next. If sufficient reproducibility
A single-column procedure can be used; however, it requires cannot be obtained by this procedure, use peak areas for calibra-
temperature programming. Columns packed with special porous tion. Preferably use peak areas when peaks are not symmetrical.
spherical or granular packing materials effect separation with Prepare a calibration curve by plotting either peak area or peak
sharp, well-resolved peaks.3 With temperature programming, height against volume or mole percent for each component.
columns packed with Chromosorb 102,2 Carbosphere,4 and Car- Computer applications are available to generate calibration
bosieve3 separate the gases listed. Commercial equipment specif- tables for certified gas mixtures.
ically designed for such operations is available.2,4–6 2) Pure gases—Introduce pure gases into the chromatograph
d. Integrator/recorder: Use a 10-mV full-span strip chart individually with a syringe. Inject sample volumes of 0.25, 0.5,
recorder with the gas chromatograph. When minor components 1.0 mL, etc., and plot detector response, corrected for attenuation,
such as H2 and H2S are to be detected, a 1-mV full-span recorder against gas volume.
is preferable. When the analysis system yields a linear detector response with
Integrators that can easily detect very minute quantities of increasing gas component concentration from zero to the range of
gases are available. Computerized data-processing systems are interest, run standard mixtures along with samples. If the same sam-
available to record and manipulate the chromatographic signals. ple size is used, calculate the gas concentration by direct proportions.
c. Sample analysis: If samples are to be injected with a syringe,
3. Reagents equip the sample collection container with a port closed by a rub-
ber or silicone septum. To take a sample for analysis, expel the air
a. Carrier gases: Preferably use helium for separating digester from the barrel of the syringe by depressing the plunger and force
gases. It is impossible to detect less than 1% hydrogen when the needle through the septum. Withdraw the plunger to take the
helium is used as the carrier gas.1 Obtain linear TCD responses for gas volume desired, pull the needle from the collection container,
molar concentrations of hydrogen between 0 and 60% by using and inject the sample rapidly into the chromatograph.

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2720 ANAEROBIC SLUDGE DIGESTER GAS ANALYSIS - C. Gas Chromatographic Method

When samples are to be injected through a gas-sampling valve, The saturation water vapor pressure can be found in common
connect the sample collection container to the inlet tube. Let the handbooks. The correction factor 1 is usually small and is
1- Pv
gas flow from the collection tube through the valve to purge the often neglected by analysts.
dead air space and fill the sample tube. Typically, about 15 mL are
sufficient to clear the lines and to provide a sample of 1 to 2 mL. 6. Precision and Bias
Transfer the sample from the loop into the carrier gas stream by
following the manufacturer’s instructions. Bring the samples to Precision and bias depend on the instrument, the column, oper-
atmospheric pressure before injection. ating conditions, gas concentrations, and techniques of operation.
When calibration curves have been prepared with a synthetic The upper control limits for replicate analyses of a high-methane-
gas mixture of certified composition, use the same sample vol- content standard gas mixture (65.01% methane, 29.95% carbon
ume as that used during calibration. When calibration curves are dioxide, 0.99% oxygen, and 4.05% nitrogen) by a single oper-
prepared by the procedure using varying volumes of pure gases, ator were as follows: 65.21% for methane, 30.36% for carbon
inject any convenient gas sample volume up to about 2 mL. dioxide, 1.03% for oxygen, and 4.15% for nitrogen. The lower
Inject the sample and standard gases in sequence to permit control limits for this same standard gas mixture were: 64.67%
calculation of unknown gas concentration in volume (or mole) for methane, 29.88% for carbon dioxide, 0.85% for oxygen, and
percent by direct comparison of sample and standard gas peak 3.85% for nitrogen. The observed relative standard deviations
heights or areas. For more accurate analysis, make duplicate or (RSD) were: 0.14% for methane, 0.26% for carbon dioxide, 3.2%
triplicate injections of sample and standard gases. for oxygen, and 1.25% for nitrogen.
In a similar analysis of another standard gas mixture (55%
5. Calculation methane, 35% carbon dioxide, 10% diatomic gases—2% hydro-
gen, 6% nitrogen, 2% oxygen), typical upper control limits for
a. When calibration curves have been prepared with synthetic precision of duplicate determinations were: 55.21% for methane,
mixtures and the volume of the sample analyzed is the same as 35.39% for carbon dioxide, and 10.26% for the diatomic gases.
that used in calibration, read the volume percent of each compo- The lower control limits for this standard gas mixture were:
nent directly from the calibration curve after the detector response 54.78% for methane, 34.62% for carbon dioxide, and 9.73% for
for that component is computed. the diatomic gases. The observed RSDs for this analysis were:
b. When calibration curves are prepared with varying volumes 0.13% for methane, 0.36% for carbon dioxide, and 0.88% for the
of pure gases, calculate the percentage of each gas in the mixture diatomic gases.
as follows: A low-methane-content standard gas mixture (35.70% meth-
ane, 47.70% carbon dioxide, 3.07% oxygen, 8.16% nitrogen, and
A 5.37% hydrogen) was analyzed as above yielding upper control
Volume % = × 100 limits as follows: 34.4% for methane, 49.46% for carbon dioxide,
B
3.07% for oxygen, and 8.2% for nitrogen. The lower control lim-
its were: 34.18% for methane, 49.11% for carbon dioxide, 2.83%
where:
for oxygen, and 7.98% for nitrogen. The observed RSDs were:
A = partial volume of component (read from calibration curve), and 0.11% for methane, 0.16% for carbon dioxide, 1.37% for oxygen,
B = volume sample injected. and 0.46% for nitrogen.
With digester gas the sum of the percent CH4, CO2, and N2
c. Where standard mixtures are run with samples and instru-
should approximate 100%. If it does not, suspect errors in col-
ment response is linear from zero to the concentration range of
lection, handling, storage, and injection of gas, or in instrumental
interest:
operation or calibration.

C References
Volume % = volume % (std)
D
1. Isothermal and temperature programmed analyses of permanent
where: gases and light hydrocarbons; GC Bulletin 760F. Bellefonte (PA):
Supelco, Inc.; 1983.
C = recorder value of sample, and
2. Mindrup R. The analysis of gases and light hydrocarbons by gas
D = recorder value of standard. chromatography. J Chromatogr Sci. 1978;16:380–389.
d. Digester gases usually are saturated with water vapor that is 3. Analyzing mixtures of permanent gases and light (C1–C3) hydro-
not a digestion product. Therefore, apply corrections to calculate carbons on a single GC column; GC Bulletin 712F. Bellefonte (PA):
Supelco, Inc.; 1983.
the dry volume percent of each digester gas component as follows:
4. Chromatography; Catalog No. 200. Deerfield (IL): Alltech Associ-
ates, Inc.; 1989.
volume%as above 5. Column selection for gas and light hydrocarbon analysis; GC Bulle-
Dry volume % = tin 786C. Bellefonte (PA): Supelco, Inc.; 1983.
1 − Pv
6. Supelco Chromatography Products; Catalog 27. Bellefonte (PA):
Supelco, Inc.; 1989.
where: 7. Purcell JE, Ettre LS. Analysis of hydrogen with thermal conductivity
detectors. J Gas Chromatogr. 19653(2):69–71.
Pv = saturated water vapor pressure at room temperature and pres-
sure, decimal %.

https://doi.org/10.2105/SMWW.2882.036 5
2720 ANAEROBIC SLUDGE DIGESTER GAS ANALYSIS - C. Gas Chromatographic Method

Bibliography Burgett C, Green L, Bonelli E. Chromatographic methods in gas analysis.


Avondale (PA): Hewlett-Packard Inc.; 1977.
Leibrand RJ. Atlas of gas analyses by gas chromatography. J Gas Chro- Thompson B. Fundamentals of gas analysis by gas chromatography. Palo
matogr. 1967;5(10):518–524. Alto (CA): Varian Associates, Inc.; 1977.
Jeffrey PG, Kipping PJ. Gas analysis by gas chromatography, 2nd ed.
Elmsford (NY): Pergamon Press Inc.; 1972.

Published Online: August 27, 2018


Revised: December 16, 2021
https://doi.org/10.2105/SMWW.2882.036 6

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