University Of Zakho

College of Engineering
Petroleum Engineering Department
Petroleum Engineering II
Fourth Stage 2020-2021

Sampling & Analysis in

Oil and Gas industry

Prepared By: Ali Hussain Waheed

Aza M.Ali Abdulkareem
Nizar Ali

Supervised By: Mr. Barham S. Mahmood

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 List of Contents:
1. Introduction 3

2. Sampling 3

.3 Methods of Sampling 3

3.1 Bottom-hole Sampling 4

3.2 Wellhead sampling 6

3.3 Surfaces or separator sampling 6

4. Methods of Sampling Advantages 8

5. PVT-Analysis 9

6. Differential Liberation Test 10

6.1 Instrument (Equipment) used 10

6.2 Procedure 11

7. Conclusion 12

8. References 12

List Of Figures:
Figure 1 Separator sampling procedure .................................................................... 4
Figure 2 Wellhead sampling procedure ..................................................................... 4
Figure 3 Bottom-hole sampling procedure ............................................................... 4
Figure 4 inside of bottom-hole sampler device ........................................................ 5
Figure 5 well-head sampling process .......................................................................... 6
Figure 6 surface sampling process ............................................................................... 7
Figure 7: Differential Liberation Test ...................................................................... 10
Figure 8: Schematic of PV cell and associated equipment ................................ 11
Figure 9: Differential liberation experimental diagram. ................................... 11

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1. Introduction

Oil and gas samples are collected to analyze the properties of extracted fluids in
reservoirs, production tubing, and pipeline transport. The following are the main
PVT (pressure-volume-temperature) properties of a reservoir fluid that must be
calculated:

• Original reservoir composition(s)

• Oil and gas viscosities
• Oil and gas densities
• Saturation pressure at reservoir temperature
• Liquid (NGL/condensate) content of reservoir gas
• Gas solubility in reservoir oil
• Equilibrium phase compositions
• Shrinkage (volume) factors of oil and gas from reservoir to surface
conditions

As a result, we must recognize that the primary goal of sampling is to obtain

"representative" samples of the fluid or fluids present in the reservoir under
initial conditions. To ensure that the fluids evaluated are representative of the
field, the accuracy of the samples obtained is critical.

2. Sampling

The quality to be assigned to laboratory findings is determined by whether the

sample examined is indicative of the well contents or, at the very least, of the
well's drainage area. To minimize errors created by variations in relative
movement of oil & gas after solution gas has been liberated, samples should be
taken early in the reservoir's life.

3. Methods of Sampling

To gather reservoir fluids, a variety of sampling methods can be used, including:

• Separator sampling
• Bottom-hole sampling
• Wellhead sampling

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 Figure 1: Separator sampling procedure

Figure 2: Wellhead sampling procedure

Figure 3: Bottom-hole sampling procedure

Bottom-hole Sampling

Bottom-hole containers are lowered into the wellbore on a wireline to sample

under-saturated oils. The conventional subsurface approach entails lowering a
sampling unit, often referred to as a "bottomhole sampler," to a predetermined
depth down the well. Bottomhole samplers can be used in cased-hole or open-
hole wells, and they can also be run in tubing. A pressure-tight portion of the
sampler traps a sample of the fluid in the wellbore at that depth. The sampler is
taken to the surface, where it is repressured and returned to a single-phase state
before being moved to an appropriate pressure vessel for transport to the
laboratory.

If the well is running at a low rate, a bottom-hole sample is obtained. At least two
(and ideally three) BH samples with the same bubble point pressure should be
collected to ensure representative samples.

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 Figure 4: inside of bottom-hole sampler device

The flowing bottom-hole pressure should still be greater than the reservoir oil's
projected bubble-point pressure. When a well is shut down, bottom-hole oil
samples may be collected. The flowing bottom-hole pressure should be greater
than the bubble-point pressure prior to shut-in. The following is a standard
bottom-hole sampling procedure:

• Install sample container in the production tubing

• Make pressure gradient measurements going into the hole
• Position sampler at the specified depth
• Produce the well at a low, stable rate (following conditioning)
• Sample during the flow test (dynamic sample) or after shutting in the well
(static sample)

Subsurface samples can only be representative of well contents where the

pressure at the point of sampling is above or equal to the saturation pressure. In
this situation, a Bottom-hole sampler is lowered into the well and held opposite
the producing layer for a relatively long time. If this condition is not met, a surface
sample should be taken. Since the device goes two phases during transition to the
sample chamber, even at temperatures similar to the saturation pressure, there is
a high probability of sample integrity being lost.

At least two (preferably three) BH samples should have the same bubble-point
pressure at ambient temperature, within 3 to 4 percent, to ensure that
representative samples have been collected.

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 Wellhead sampling

This method will provide the simplest and most accurate results if the fluid is in
a single-phase state at the wellhead temperature and pressure. As a consequence,
if the oil formed at the wellhead is single phase, a sample may be taken upstream
to the choke. There are a variety of wellhead sampling techniques that can be
used:

• Fill a membrane sampler by displacing the backpressure fluid (ethylene glycol).

• Fill a piston cylinder sampler.

• Fill an open cylinder containing mercury (sometimes not allowed offshore)

If the temperature is above the wax appearance limit, effective wellhead samples
should be very reliable (WAP). Wellhead samples are usually only obtained from
high-pressure, deep wells that are severely under-saturated. For asphaltene study,
wellhead (or bottom-hole) samples are desired. Dry gas and a reservoir that is
extremely undersaturated.

Figure 5 well-head sampling process

Surfaces or separator sampling

Gas condensates and saturated oils are sampled using separators. Separator
samples are also collected for large-scale gas injection analyses, and also some
special studies such as asphaltene precipitation, wax (paraffin) stage, emulsions,
hydrates, and corrosion analysis. The approach focuses on sampling the gas and
oil separately as they exit the primary separator. (Figure 6). The samples should
be taken simultaneously, filling the sample containers at a constant rate of about
1 liter/minute. The 20-liter gas bottles are first emptied. By displacing ethylene
glycol, a piston cylinder, or a mercury-filled tube, the separator oil

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(approximately 600 cm3) can be collected in a membrane bottle (not allowed
offshore).

A good rule of thumb is that collecting a collection of separator samples takes

approximately half an hour. Valid separator sampling criteria include the
following:

• Stable separator pressure and temperature, liquid level, and flow rates.
Excessive carryover (due to high rates) should be avoided.
• Critical flow through the choke, requiring that separator pressure is less
than 1/2 of the wellhead flowing pressure.

This criterion is also impossible to achieve, and it isn't necessarily necessary if

separator conditions are stable. During the sampling, the rates of separator gas
and separator oil are measured to assess the ratio in which the separator samples
can be recombined. The recombined mixture can produce a fluid that closely
resembles the well stream that entered the separator.

To determine if a reliable sample was collected, a basic test may be performed in

the field at the well site. The sample cylinder is pressurized in this test either with
a piston cell or with mercury as the displacing solvent. Mercury was once the
most commonly used pressure transfer and volume shift solvent, but its use is
reducing due to toxic and other issues. From the relation between injection
pressure and volume of mercury injected, the following properties are derived:

1. the pressure existing within the sampler when it is received at the surface.
2. the compressibility of the material within the sampler.
3. the bubble-point pressure of the contents of the sampler.
4. The samples should be taken simultaneously, filling the sample containers
at a constant rate.
5. Then we recombine gas and oil separator samples and make some slight
adjustment.

Figure 6 surface sampling process

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To decide the exact ratio in which the samples can be recombined, a minor change
must be made. This is due to the fact that, as seen in (fig. 1), the oil sample is
obtained at separator pressure and temperature, while the gas oil ratio is
determined compared to the storage tank barrel, resulting in the necessary
recombination ratio.

Dimensionally, the measured gas oil ratio must be multiplied by the shrinkage
factor from separator to stock tank conditions. This factor is typically calculated
in the lab as the first step of a PVT examination of a surface recombination sample
by putting a small volume of the oil sample in a cell with the required separator
conditions and discharging it (flash expansion) to a second cell with field stock
tank conditions.

4. Methods of Sampling Advantages

Table 1: Methods of Sampling Advantages

Bottom-hole Recombination Wellhead

Relatively easy,
Collects the desired convenient and less
Easy
sample directly expensive compared to
subsurface sampling
Avoids the potential for
Can maintain full
getting the subsurface Cheaper
pressure on sample
sampling tool
Avoids the need for No need for truly single-
Some advantages of
flow rate metering phase at the sampling
recombination
devices point
Could be done when
Avoids use of surface highly under-saturated at
Large amount
separators wellhead conditions or
for dry gasses

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5. PVT-Analysis

PVT-Analysis of a reservoir fluid comprises the determination of:

a) the correlation between pressure and volume at reservoir temperature.

b) various physical constants that enter into reservoir engineering
calculations, such as viscosity, density, compressibility etc.…
c) the effect of separator pressure and temperature on oil formation volume
factor, gas/oil ratio etc.…
d) the chemical composition of the most volatile components.

The apparatus required for PVT analysis consists of:

a) apparatus for the transfer and the recombination of separator oil and gas
samples;
b) apparatus for measuring gas-volumes and for performing separator tests;
c) the PV cell and displacement pumps and dispensing cell;
d) high pressure viscometer;
e) gas chromatograph.

There are four main PVT tests for oil systems plus associated compositional
analysis:

1. the flash vaporization (for detecting bubble point pressure)

2. the differential test.
3. the separator tests.
4. viscosity measurements
5. compositional measurements.

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6. Differential Liberation Test

The differential liberation expansion (DLE) experiment is aimed to estimate an

oil reservoir's depletion mechanism and thus provide appropriate PVT data for
estimating reservoir performance. The following are some of the most important
findings from the differential liberation experiment:

• Density of the remaining oil as a function of pressure.

• The shrinkage in the oil volume as a function of pressure.
• Amount of gas in solution as a function of pressure.
• Properties of the evolved gas including the composition of the liberated
gas, the gas specific gravity, and the gas compressibility factor.

The test is carried at reservoir temperature in order to assess the volumetric and
compositional changes in the oils during the primary processing period (pressure
depletion). The solution gas that is released from an oil sample after a decrease
in pressure is continually separated from contact with the oil until maintaining
equilibrium with the liquid form in the differential liberation process.

The composition of the total hydrocarbon system varies throughout this form of
liberation. The test is performed on reservoir oil samples and entails loading a
liquid sample into a visual PVT cell at the bubble-point pressure and reservoir
temperature.

Figure 7: Differential Liberation Test

Instrument (Equipment) used

This experiment was carried out using the PV cell (see fig. 8). The fluid is charged
into the PV cell after recombining the oil and gas in the correct proportions. The
PV cell is held at a constant temperature during the tests, the measured reservoir
temperature. A positive displacement mercury pump regulates the cell pressure,
which is measured with a precision pressure scale. The plunger movement is

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calibrated in terms of the amount of mercury injected or removed from the PV
cell, allowing for precise measurement of volume variations in the cell

Figure 8: Schematic of PV cell and associated equipment

Procedure

The reservoir fluid sample is equilibrated in a windowed PVT cell at its bubble
point pressure and reservoir temperature. The pressure inside the cell is reduced
by increasing its volume. Since the cell pressure is now less than bubble point
pressure, a gas phase will form. The gas is equilibrated with the liquid in the cell
by agitation. Once equilibrium has been established between the fluid phases, the
gas is completely displaced from the cell at constant pressure by slowly reducing
the volume of the cell. The volume and specific gravity of the gas expelled from
the cell is measured. The volume of liquid left in the cell is also measured. This
represents Stage 1, as illustrated in Figure (9). The procedure used in Stage 1 is
repeated for the next pressure level at Stage 2, as illustrated in Figure (9). These
stages are repeated until atmospheric pressure is reached as the final stage with
the cell still at reservoir temperature. The temperature of the cell is further
reduced to 60 F to determine residual oil volume from differential liberation.
This is the volume of liquid remaining in the cell at 60 F. And the final oil is
cooled, where the resulting "residual" oil volume and specific gravity are
measured (or calculated) at 15.5 C. Residual oil composition may also be
reported.

Figure 9: Differential liberation experimental diagram.

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7. Conclusion

Many of our advanced oil analysis instruments, procedures, and diagnostic

methods are useless until the oil sample accurately represents the state of the oil
in use inside the unit. An effective oil analysis software is built on the basis of
proper sampling procedures. Time and resources are lost if poor sampling
methods are used, and erroneous results can be drawn based on flawed evidence.
Both conditions erode the oil analysis program's perceived worth and confidence.
The three main application areas of PVT data: to provide data for reservoir
calculations, to provide physical property data for well flow calculations and for
surface facility design.

8. References

1) Dandekar, A.Y., 2013. Petroleum reservoir rock and fluid properties.

CRC press.
2) Ahmed, T., 2013. Equations of state and PVT analysis. Elsevier.
3) Dake, L.P., 1983. Fundamentals of reservoir engineering. Elsevier.
4) Ahmed, T., 2006. Reservoir Engineering Handbook. Elsevier.
5) Department of Petroleum Engineering, Heriot-Watt University chapter
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6) Sampling Petroleum Reservoir Fluids - API RECOMMENDED
PRACTICE 44 SECOND EDITION, APRIL 2003- API Publishing
Services, 1220 L Street, N.W., Washington, D.C. 20005
7) Fluid Sampling & Laboratory Data Chapter 3 / Curtis H. Whitson.

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