LABORATORY MANUAL

7PE4-21: Gas Testing Lab

B.Tech. V Year – VII Semester

Department of Petroleum Engineering

ENGINEERING COLLEGE BARMER

BIKANER TECHNICAL UNIVERSITY

(2021)
 ii
ENGINEERING COLLEGE BARMER

N.H. 68, Jaisalmer Road

Barmer (Rajasthan) – 344001

DEPARTMENT OF PETROLEUM ENGINEERING

Program: Bachelor of Technology (B. Tech)

VISION OF DEPARTMENT

To develop motivated engineers, academicians and entrepreneurs in the field of

Petroleum Engineering.

MISION OF DEPARTMENT

• To pursue excellence in all areas of civil engineering keeping pace with the latest
developments.
• To promote and provide a dynamic learning environment that emphasis real time
problem solving skills, teamwork, communication and leadership skills.
• To develop globally competent students with strong foundations, able to adapt to
changing technology.

2
 iv
SYLLABUS

List of experiments

1. Determination of compositions of Gas with Gas Chromatography.

2. Determination of Reid Vapour Pressure.
3. Determination of % reserve of gas.
4. Determination of Gas gravity.
5. CO2 detection.

3
 v
MANDATORY INSTRUCTIONS

1. Students should report to the labs concerned as per the timetable.

2. Record should be updated from time to time and the previous experiment must be signed by
the faculty in charge concerned before attending the lab.
3. Students who turn up late to the labs will in no case be permitted to perform the experiment
scheduled for the day.
4. After completion of the experiment, certification of the staff in-charge concerned in the
observation book is necessary.
5. Students should bring a notebook of about 100 pages and should enter the
readings/observations/results into the notebook while performing the experiment.
6. The record of observations along with the detailed experimental procedure of the experiment
performed in the immediate previous session should be submitted and certified by the staff
member in-charge.
7. Not more than FIVE students in a group are permitted to perform the experiment on a set up.
8. The group-wise division made in the beginning should be adhered to, and no mix up of
student among different groups will be permitted later.
9. The components required pertaining to the experiment should be collected from Lab- in-
charge after duly filling in the requisition form.
10. When the experiment is completed, students should disconnect the setup made by them, and
should return all the components/instruments taken for the purpose.
11. Any damage of the equipment or burnout of components will be viewed seriously either by
putting penalty or by dismissing the total group of students from the lab for the
semester/year.
12. Students should be present in the labs for the total scheduled duration.
13. Students are expected to prepare thoroughly to perform the experiment before coming to
Laboratory.
14. Procedure sheets/data sheets provided to the students groups should be maintained neatly
and are to be returned after the experiment.
15. DRESS CODE:
• Formal dress and safety shoes.
• Wearing of jeans is strictly prohibited.

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 vi

CONTENTS

S. No. Description Page No.

1. Vision and Mission of Department ii
2. Preface iii
3. Syllabus iv
4. Mandatory Instructions v
5. 6
Experiment No. 1. Determination of compositions of Gas with
Gas Chromatography.
6. 11
Experiment No. 2: Determination of Reid Vapour Pressure.
7. 13
Experiment No. 3: Determination of % reserve of gas.
8. 14
Experiment No. 4: Determination of Gas gravity.
9. 16
Experiment No. 5: CO2 detection.

5
 Experiment No. 1
Determination of compositions of Gas with Gas Chromatography
AIM:
The aim of this unit is to study determination of compositions of Gas with Gas
Chromatography

OBJECTIVES:
After completing this unit students should be able to:
• determine the composition of any gaseous mixture with Gas Chromatography.

APPARATUS:
1. Chromatograph
2. Carrier Gas
3. Drier
4. Integrator
5. Vacuum gauge

THEORY:
Components to be determined in a gaseous sample are physically separated by gas
chromatography and compared to calibration data obtained under identical operating
conditions. A fixed volume of sample in the gaseous phase is isolated in a suitable inlet
sample system and entered onto the column. The inert components, nitrogen and oxygen,
are analyzed on an adsorption column. This analysis detects any air contamination that
could be introduced in field and/or laboratory sampling. Failure to detect air
contamination will result in erroneous data being used to calculate the properties of
natural gas from compositional data. Carbon dioxide in natural gas is difficult to
determine accurately on the silicone 200-500 column due to inadequate resolution of the
minor component (carbon dioxide) from the major component (methane). Results are
acceptable if the carbon dioxide in the reference standard matches closely the carbon
dioxide in the unknown sample (within 20% in the 0.01 to 10% range). For this reason,
an alternate column system for determining carbon dioxide is included in the main body
of this method. Samples containing less than 10% carbon dioxide can be analyzed on

6
either column system by calibrating with a reference standard or the pure component that
approximates the carbon dioxide expected in the unknown gas. The components
nitrogen/air, methane, carbon dioxide and ethane through n-pentane are eluted on
forward flow of carrier gas through the partition column. The numerous heavy
components of natural gas are grouped into a single peak using a precut column which is
backflushed to elute the hexanes and heavier as the first peak in the chromatogram. This
recommended approach to the hexanes and heavier separation has two distinct
advantages: (1) better precision of measuring the peak area, and (2) a reduction in
analysis time over the non-precut (single) column approach. The chromatograms are
interpreted by comparing the areas of the components eluted in the forward position with
the areas taken from response curves obtained using pure
components, or from areas of corresponding peaks in the selected reference standard.
The hexanes and heavier components may be interpreted by comparing the total area
under the reverse flow peak with the corresponding area in a reference standard (whose
hexanes and heavier composition closely resembles that of the hexanes and heavier
composition of the sample being analyzed) or by comparing the total area under the
reverse flow peak with the areas of the pentane peaks in the sample.

PROCEDURE:

The full range analysis of a gaseous sample requires first a run on an adsorption column
to determine oxygen and nitrogen; second, a run on a partition column to determine
methane, carbon dioxide, ethane and heavier hydrocarbons. If carbon dioxide content is
critical in the unknown samples and does not closely match the carbon dioxide in the
reference standard, a third run must be made using a porous polymer column. If helium
and/or hydrogen are to be determined, a fourth run is needed using an adsorption column
with nitrogen or argon as the carrier gas. These runs are independent and may be made
in any order, or may be made separately to obtain less than the full range analysis.
1. Connect columns to the column switching/sampling valve and mount the valve in
the chromatograph oven so that it can be actuated manually or automatically.
Adjust the instrument conditions to the optimum for the selected column
arrangement.
2. Samples must be equilibrated in the laboratory at 20-50°F above the source
temperature of the field sampling. The higher the temperature the shorter the

7
 equilibration time (approximately two hours for small sample containers of 300
ml or less). This analysis method assumes field sampling methods have removed
entrained liquids.
3. Connect the sample outlet valve to the sample entry system via a phosphorous
pentoxide or magnesium perchlorate tube (unless gas samples are known to be
moisture free, a dryer, should be used). This dryer and the transport line must be
maintained at the same elevated temperature (20-S0°F) above the highest
expected field sampling temperature. Sample connections to the sample entry
system of the chromatograph should be accomplished by using metal, teflon,
nylon or some other non-absorbing materials. Rubber and plastic tubing (Tygon)
should be avoided since both materials readily absorb hydrocarbons.
4. Evacuate sample entry system, including sample loop, back to valve on sample
cylinder to 1 mm of mercury absolute. Close valve to vacuum source and
carefully meter gas from sample cylinder until sample loop is filled to the same
predetermined partial pressure as used for the reference standard. Operate
chromatograph sample valve to place sample onto column. The evacuation
method of sample entry at the chromatograph is preferred if hexanes and heavier
concentration exceeds 0.3 mol%.
5. If samples are known to contain a relatively small amount of hexanes and
heavier, the purge technique is satisfactory. In using this technique, open the
sample cylinder outlet valve and carefully purge the sample through the entry
system, including the sample loop. Pass outlet from the sample loop through a
tube extended just below the surface of water held in a beaker or other suitable
container. to indicate the rate of sample flow. Adjust the flow to one or two
bubbles per second. Flush for three minutes or more. Close sample cylinder
outlet valve. Remove bubble tube from water, operate chromatograph sample
valve to place sample onto column.

8
 FIG.: NG ANALYSIS USING GAS CHROMATOGRAPH

RESULTS:

9
The results are obtained in form of the above chromatograph and the peak values are to
be calculated based on the table below.

VIVA QUESTIONS:
1. What is Chromatography and what is its importance?
2. How does Gas Chromatography help in presence of a particular gas?
3. What is the composition of Natural Gas?
4. What are the non-hydrocarbons present in Natural Gas?

10
 Experiment No. 2
Determination of Reid Vapour Pressure.
AIM:
To determine the "Reid Vapor Pressure of the given sample and for the determination of
vapor pressure of volatile non viscous petroleum products.

APPARATUS:
• Gasoline chamber
• Air chamber
• Pressure Gauge
• Cooling bath
• Water bath
• Thermometer

THEORY:
Vapor pressure is defined as the pressure exerted by the vapor of the liquid on the walls
of the closed container.
The temperature at which the vapor pressure of liquid equals 1 (one) atmospheric
pressure is designated as boiling point of liquid. In case of motor sprit, higher vapor
pressure will lead to vapor lock of engine. Vapor pressure is an important physical
property. It is used in the consideration of storage and transportation.

PROCEDURE:
1. Vapor pressure of all volatile fractions is measured by testing the apparatus at
(38+0.1) ◦C.
2. The apparatus consists of two chambers. The lower chamber is in the form of,
cylindrical bomb for holding the test sample.
3. Above this, there is an air chamber which is a hollow cylindrical space, designed
to possess four times the bomb volume.
4. The top portion is filled with Bourdon Gauge for pressure indication.
5. For the test, the bomb is first filled with the sample upto the brim and
immediately the valve is closed and connected to the air chamber.

11
 6. The apparatus is now immersed in a water bath kept at the mentioned
temperature. The maximum pressure indicated by the gauge is counted as the
Reid Vapour Pressure of the sample.
7. LPG, Gasoline, Naphtha, Jet Fuels are tested like this. It is found that true vapor
pressure in most cases is higher than indicated RVP, and the variation for
different fractions is different.
8. Maximum difference is indicated in case of crude oils. Relative Expressions
‘True Vapor Pressure to RVP’ is also sometimes indicated and for gasoline it is
in the range of 1.03 to 1.45, while for crude’s it goes up to 10.

RESULT
The Reid Vapor Pressure of the given sample is found to be …………………...

VIVA QUESTIONS
1. Define Vapor Pressure.
2. Define Partial pressure.
3. What are the different Laws of Partial Pressures?
4. Describe relation between Partial pressure and Mole Fraction.

12
 Experiment No. 3
Determination of percentage reserve of gas.
AIM:
The aim of this unit is to study and measure the percentage reserve of gas.

OBJECTIVES:
After completing this unit students should be able to perform volumetric analysis and
measure the percentage reserve of gas.

THEORY:
Volumetric estimates of OGIP are based on a geological model that geometrically
describes the volume of hydrocarbons in the reservoir. However, due mainly to gas
evolving from the oil as pressure and temperature are decreased, oil at the surface
occupies less space than it does in the subsurface. Conversely, gas at the surface
occupies more space than it does in the subsurface because of expansion. This
necessitates correcting subsurface volumes to standard units of volume measured at
surface conditions.

ESTIMATION OF ORIGINAL GAS IN PLACE

OGIP= (7758*A*H*∅*Sgi)/Bgi

7758 = conversion factor from acre-ft to bbl

A = area of reservoir (acres) from map data
h = height or thickness of pay zone (ft) from log
ø = porosity (decimal) from log and/or core data
SgI = Initial Gas Saturation
Bgi = formation volume factor for gas at initial conditions (reservoir bbl/STB)

RESULT:
OGIP is calculated and found to be ………………...MMSCF.

13
 Experiment No. 4
Determination of Gas gravity.
AIM:
The aim of this unit is to determine specific gravity of a given gas sample.

OBJECTIVES:
The objective is to determine the specific gravity of a particular gas sample having a
mixture of components with varying compositions.

THEORY:
One of the main gas properties that are frequently of interest to engineers is the
apparent molecular weight. If yi represents the mole fraction of the component in a gas
mixture, the apparent molecular weight is defined mathematically by the following
equation.

𝑀𝑎 = ∑ 𝑦𝑖 ∗ 𝑀𝑖

Where, Ma = apparent molecular weight of a gas mixture

Mi = molecular weight of the component in the mixture
yi = mole fraction of component in in the mixture.
The density of an ideal gas mixture is calculated by simply replacing the molecular
weight of the pure component with the apparent molecular weight of the gas mixture to
give:
𝑃 ∗ 𝑀𝑎
𝜌𝑔 =
𝑧∗𝑅∗𝑇

The specific gravity is defined as the ratio of the gas density to that of the air. Both
densities are measured or expressed at the same pressure and temperature. Commonly,
the standard pressure Psc and standard temperature Tsc are used in defining the gas
specific gravity.
𝑀𝑤𝑎
𝛾𝑔 =
28.97
PROCEDURE:
1. Starting by Gas sample at 60 ◦F & 14.7 psia.
2. Use the oven to heat the sample until reach certain temperature.
3. Use Jog mode then increase the volume of the Gas sample.

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 4. Record the new Temperature, Pressure, and Volume.
5. Calculate Z factor
6. Use GC to obtain mole friction.
7. Calculate Gas gravity & density use the above formulas.

RESULTS
The Density and Specific Gravity of the given sample is ……………..

VIVA QUESTIONS
1. What is Gas Gravity?
2. Mathematically describe Gas Gravity.
3. What is Apparent Molecular Weight?
4. Define Apparent Molecular weight mathematically.

15
 Experiment No.-5
CO2 detection

AIM: To study the CO2 detection process experimentally.

OBJECTIVE:
After completing this unit students should be able to determine the composition of C02
in any gaseous mixture with Gas Chromatography.

APPARATUS:

1. Chromatograph
2. Carrier Gas
3. Drier
4. Integrator
5. Vacuum gauge

THEORY:

Components to be determined in a gaseous sample are physically separated by gas

chromatography and compared to calibration data obtained under identical operating
conditions. A fixed volume of sample in the gaseous phase is isolated in a suitable inlet
sample system and entered onto the column. The inert components, nitrogen and oxygen,
are analyzed on an adsorption column. This analysis detects any air contamination that
could be introduced in field and/or laboratory sampling. Failure to detect air
contamination will result in erroneous data being used to calculate the properties of
natural gas from compositional data. Carbon dioxide in natural gas is difficult to
determine accurately on the silicone 200-500 column due to inadequate resolution of the
minor component (carbon dioxide) from the major component (methane). Results are
acceptable if the carbon dioxide in the reference standard matches closely the carbon
dioxide in the unknown sample (within 20% in the 0.01 to 10% range). For this reason,
an alternate column system for determining carbon dioxide is included in the main body
of this method. Samples containing less than 10% carbon dioxide can be analyzed on
either column system by calibrating with a reference standard or the pure component that
approximates the carbon dioxide expected in the unknown gas. The components

16
nitrogen/air, methane, carbon dioxide and ethane through n-pentane are eluted on
forward flow of carrier gas through the partition column. The numerous heavy
components of natural gas are grouped into a single peak using a precut column which is
backflushed to elute the hexanes and heavier as the first peak in the chromatogram. This
recommended approach to the hexanes and heavier separation has two distinct
advantages: (1) better precision of measuring the peak area, and (2) a reduction in
analysis time over the non-precut (single) column approach. The chromatograms are
interpreted by comparing the areas of the components eluted in the forward position with
the areas taken from response curves obtained using pure

components, or from areas of corresponding peaks in the selected reference standard.

The hexanes and heavier components may be interpreted by comparing the total area

under the reverse flow peak with the corresponding area in a reference standard (whose
hexanes and heavier composition closely resembles that of the hexanes and heavier
composition of the sample being analyzed) or by comparing the total area under the
reverse flow peak with the areas of the pentane peaks in the sample.

PROCEDURE:

The full range analysis of a gaseous sample requires first a run on an adsorption column
to determine oxygen and nitrogen; second, a run on a partition column to determine
methane, carbon dioxide, ethane and heavier hydrocarbons. If carbon dioxide content is
critical in the unknown samples and does not closely match the carbon dioxide in the
reference standard, a third run must be made using a porous polymer column. If helium
and/or hydrogen are to be determined, a fourth run is needed using an adsorption column
with nitrogen or argon as the carrier gas. These runs are independent and may be made
in any order, or may be made separately to obtain less than the full range analysis.

1. Connect columns to the column switching/sampling valve and mount the valve in
the chromatograph oven so that it can be actuated manually or automatically.
Adjust the instrument conditions to the optimum for the selected column
arrangement.
2. Samples must be equilibrated in the laboratory at 20-50°F above the source
temperature of the field sampling. The higher the temperature the shorter the

17
 equilibration time (approximately two hours for small sample containers of 300
ml or less). This analysis method assumes field sampling methods have removed
entrained liquids.
3. Connect the sample outlet valve to the sample entry system via a phosphorous
pentoxide or magnesium perchlorate tube (unless gas samples are known to be
moisture free, a dryer, should be used). This dryer and the transport line must be
maintained at the same elevated temperature (20-S0°F) above the highest
expected field sampling temperature. Sample connections to the sample entry
system of the chromatograph should be accomplished by using metal, teflon,
nylon or some other non-absorbing materials. Rubber and plastic tubing (Tygon)
should be avoided since both materials readily absorb hydrocarbons.
4. Evacuate sample entry system, including sample loop, back to valve on sample
cylinder to 1 mm of mercury absolute. Close valve to vacuum source and
carefully meter gas from sample cylinder until sample loop is filled to the same
predetermined partial pressure as used for the reference standard. Operate
chromatograph sample valve to place sample onto column. The evacuation
method of sample entry at the chromatograph is preferred if hexanes and heavier
concentration exceeds 0.3 mol%.
5. If samples are known to contain a relatively small amount of hexanes and
heavier, the purge technique is satisfactory. In using this technique, open the
sample cylinder outlet valve and carefully purge the sample through the entry
system, including the sample loop. Pass outlet from the sample loop through a
tube extended just below the surface of water held in a beaker or other suitable
container. to indicate the rate of sample flow. Adjust the flow to one or two
bubbles per second. Flush for three minutes or more. Close sample cylinder
outlet valve. Remove bubble tube from water, operate chromatograph sample
valve to place sample onto column.

18
FIG.: CO2 in NG ANALYSIS USING GAS CHROMATOGRAPH

Fig.: CO2 presence in NG

19
The results are obtained in form of the above chromatograph and the peak values are to
be calculated based on the table below.

Occasionally the analysis of extremely light hydrocarbon systems such as residue gases
may yield peaks in the propane and heavier components that are too small to measure
accurately. In this case, it is satisfactory to use a sample volume up to 3 ml, depending
on the individual basic sensitivity of the Chromatograph, for the determination of the
components that are too small to be obtained by regular method. A sample similar in size
to the reference standard should also be charged to the chromatograph and the peak areas
of the ethane and heavier components measured. Make calculations of the ethane and
heavier components in the same manner as outlined for the routine procedure. If a
separation between inerts and methane is not necessary, methane and lighter may be
expressed as the difference between 100% and the sum of the rest of the components
(valid for all OPA sampling methods except "Helium Pop").

VIVA QUESTIONS:

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1. What is the importance of CO2 detection in Oil and Gas Industry?
2. What are the different CO2 measuring techniques in lab conditions?
3. Why is it necessary to remove CO2 from crude oil?

21