Vision Advanced Petroleum Solutions LLC

MEASUREMENT OF ASPHALTENE CONTENT

This work instruction is a mandatory requirement, and forms part of the Approved Integrated Management System.
Alterations are not permitted without the prior approval of the Senior Technical Manager or the relevant Department
Supervisor.

1. PURPOSE
This is the procedure to use as an initial measurement of asphaltene content (measurement of
heptane/pentane).
2. AUTHORITY
This work instruction is written and maintained with the authority of the Senior Technical Manager or the
relevant document owner.
3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this work
instruction.
4. PROCEDURE
4.1. Safety Precautions
- Eye protection and protective clothing must be worn.
- Ensure pipe work is in good condition and the appropriate fittings used.
- Ensure suitable screening devices are used wherever possible.
4.2. Quality Assurance
- Ensure all equipment is in calibration before commencement of work
- Record next calibration date on worksheet.
4.3. Apparatus

4.4. Method
Check to see if the fluid under investigation contains H 2S; if so consult as to the correct safety
measures.

1. Thermally restore the liquid sample to above reservoir temperature for a minimum of 24 hours.
Ensure that during the thermal restoration period the pressure of the sample is maintain in excess
of reservoir pressure.

VAPS-PVT-WI-015/Rev.00/03 May 2015 / Page 1 of 2

Any hard of copy this document will be considered as UNCONTROLLED COPY unless otherwise mentioned on it.
Approved copy of document is available with Management Representative only.
 Vision Advanced Petroleum Solutions LLC

MEASUREMENT OF ASPHALTENE CONTENT

2. Set up the sample as in figure 1. Ensure that the sample can be kept at a temperature above
reservoir temperature.
3. Perform a single phase flash of the sample, where the fluid passes through the filter. Ensure the
pressure is kept above reservoir pressure at all times. Flash enouugh volume to give a sample of
approximately 20g mass of liquid. Label this subsample as filtered flash. Note: The gas does not
need to be collected, but should be vented off or put through a scrubber as appropriate.
4. Set up the sample as in figure 2. Again, ensure that the sample can be kept at a temperature
above reservoir temperature.
5. Perform a single phase flash of the sample, where the fluid does not pass through the filter.
Ensure the pressure is kept above reservoir pressure. Flash enouugh volume to give a sample of
approximately 20g mass of liquid. Label this subsample as non-filtered flash. Note: The gas does
not need to be collected, but should be vented off or put through a scrubber as appropriate.
6. Put both samples in for asphaltene content analysis.
Note: If sample volume is limited, the mass required for analysis can be halved, however the analysis
will be for heptane only.

VAPS-PVT-WI-015/Rev.00/03 May 2015 / Page 2 of 2

Any hard of copy this document will be considered as UNCONTROLLED COPY unless otherwise mentioned on it.
Approved copy of document is available with Management Representative only.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

All experimental work at the VAPS is conducted in accordance with documented procedures and work
instructions. A listing for these is also enclosed in the tender which gives more detailed about the procedure
and methodology

In Summary, the list below is to confirm the experiments which can be performed by VAPS

Black Gas
Reference PVT Analysis
Oil Condensate

G.1 Quality and Validity ✔️ ✔️

G.2 Reporting ✔️ ✔️

Routine Experiments
R.1 Compositional Analysis ✔️ ✔️
R.2 Physical Recombination
R.3 Pseudo-components analysis ✔️ ✔️
Pressure Volume Relation/Constant Mass Expansion
R.4 ✔️ ✔️
(CME) study
R.5 Differential Vaporisation Analysis ✔️ ✔️
R.6 Constant Volume Depletion (CVD) ✔️ ✔️
R.7 Additional Constant Mass Expansion ✔️ ✔️
R.8 Viscosity ✔️ ✔️
R.9 Separator test ✔️ ✔️
R.10 On-site Bubble Point Determination ✔️ ✔️

Specialised Experiments
S.1 Rheology Experiments
S.1.1 Kinemetic Viscosity ✔️ ✔️
S.1.2 Wax ✔️ ✔️
S.1.3 Asphaltanes ✔️ ✔️
S.2 Miscibility Related Experiments
S.2.1 Synthetic Gas Preparation ✔️ ✔️
S.2.2 Solubility Swelling Experiment ✔️ ✔️
S.2.3 Slim Tube Test ✔️ ✔️
S.3 Interfacial Tension Measurements ✔️ ✔️
S.4 Non-Hydrocarbon Analysis ✔️ ✔️
S.5 On Site Gas-Chromatography ✔️ ✔️
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Thermal Experiments
T.1 Thermal PVT Analysis, at T ≤ 150 C
T.1.1 Constant Composition Expansion (CCE) ✔️ ✔️
HP Capillary Viscosity at each Specified Pressure and
T.1.2 ✔️ ✔️
Temperature
T.2 Thermal PVT Analysis, at T > 150 C
T.2.1 Constant Composition Expansion (CCE) ✔️ ✔️
HP Capillary Viscosity at each Specified Pressure and
T.2.2 ✔️ ✔️
Temperature
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

We have reviewed the scope of work requirements in C4 and below our summary of our understanding of the scope of work and referenced to C4
and C5 where the prices would be based on those method statement understanding.

C4 C5
Experiment Method Description
Ref Ref

The objective is to collect separator samples of the gas and liquid from the separator and to report the separator
flow rates of the two phases to obtain the gas-oil ratio (GOR). Some of the biggest errors affecting fluid samples
are related to the measurement of separator-gas and -liquid flow rates, which are crucial for the recombination
process in the laboratory. Good accuracy is often considered to be in the region of 5%, but the figure can be much
worse, for example, if there is carry-over of liquid in the gas exit stream (or carry-under of gas in an oil with
foaming tendencies). In line with current trends in the oil industry, this work is conducted using evacuated
No
Separator Sampling 1.2.1a mercury-free bottles for gases and piston bottles for liquids.
Ref
The requirement that the vessel be evacuated before transported to the sampling point (with possible loss of
vacuum during transport), or that a vacuum pump be provided at the wellsite.
As a minimum VAPS will collect 3 sets of samples i.e. 3 oil and 3 gas samples. However for the case of high GOR or
low CGR it is recommended to collect 2 gas samples for each oil pair sample i.e. 2 sets.
After the preparation of the bottles and pre-sampling operations are completed, Sampling engineer would take oil
sample from the separator slight glass and the gas samples from the gas manifold.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Wellhead sampling involves capturing fluid sample from wellhead downstream sampling point. This sampling
method is advised only when fluid saturation point is known and the wellhead pressure during sampling operation
is well above fluid saturation point. This option is restricted to wells producing dry gas, very-low-GOR oils, and
No some high-pressure/high-temperature reservoir fluids. As a minimum VAPS will collect 3 samples during each
Wellhead sampling 1.2.1b
Ref wellhead sampling operation.
The collection of a fluid sample at the surface from the wellhead itself or from the flowline or upstream side of the
choke manifold, provided that the fluid is still in one-phase condition. The sampled fluid is kept at single phase by
applying pressure compensation after sampling.

Downhole sampling involves capturing reservoir fluid samples at reservoir /downhole conditions. To obtain
accurate compositional and PVT analyses of these samples, the recovered samples must remain in downhole
conditions (i.e. there is no leak in the samples). Company would instruct on the sampling depth, and VAPS shall
connect its sampling tool with uncoated PDS bottles with the third party RIH tool provided by PDO. The well would
then be closed prior to rig in hole and VAPS would set the clock to open the samples after reaching the desired
depth and account for stabilisation time that PDO would advise. Once the tool is in the desired depth, PDO
Down Hole Phase No
1.2.2 operator and/or PDO site representative would arrange the well to be opened and flowed. Once the stabilisation
Sampling Ref
period is over, the clock would trigger the sampling champers to open and the fluid enters the bottles. Once it is
filled, the champer would close, and the wireline company can rig-out of hole. It is very essential that PDO runs
pressure and temperature gauges Simultaneously along with wireline tool to measure the flowing/static reservoir
pressure and temp. It is crucial that the samples should be in single phase, and that PDO needs to run flowing
survey or gradio survey prior to run the downhole sampling tool. As a minimum VAPS will collect 2 samples during
each downhole sampling operation.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Separator Samples Quality No

G.1.1 The separator liquid sample shall be connected to a pump to measure its opening pressure and water content.
& Validity Check Ref

No
Single Phase Quality Check G.1.2 Single phase sample shall be connected to a pump to measure its opening pressure and water content.
Ref
The samples should be restored for 24hrs prior to any experiment by wrapping the heating jacket fully around the
No part of the sample volume in the bottle at a temperature either advised by PDO or based on the sampling
Restoration G.1.3
Ref operation (i.e. Separator liquid samples would be restored at separator temp and separator gas samples would be
restored at separator temp + 10 degree C).

Sub-sample, 35- 50cc is charged to a PVT cell to measure saturation point at high reservoir or separator pressure.
No The pressure is then reduced in steps by controlling the piston movement until it reaches low pressure or relative
Psat determination G.1.4
Ref volume of 2. Duplicate samples should have bubble points within 10 psi each other. Also bubble point at room
temperature for Separator Liquid Samples can be performed on bottle itself if required
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Very small amount of the flashed gas and liquid samples would be run in Gas chromatography (GC) to measure
their compositions. VAPS has four GCs; two for running compositional analysis for gas samples and 2 for liquid
samples. On daily basis, VAPS runs standards on those GC to assess their accuracy while the standards have close
compositions with known mole or weight %. Helium is used as the gas carrier. The results would be reported either
in mole % or weight % for the pure components and pseudo components (plus fractions) for C7 onwards up to
C30+. The Molecular weight of the C30+ is then get calculated using the typical trends of C7 vs MW and adjusted to
the weight% of C30+. Molecular weight data for other components are obtained from CRC Handbook of Chemistry
and Physics, 88th Edition, 2002-2008.
Compositional analysis of If requested by PDO, H2S can be measured using dragger tube and its composition is input while normalising the
No
coated Bottom Hole G.1.5 other components.
Ref
Sample Finally, the reservoir fluid get mathematically recombined using the GOR and oil density obtained from the single
phase flash experiment.
The following are standard reported properties
• Gas and liquid composition to C30+ (and N2, CO2, H2S)
• Density and Molecular Weight for the C6 to C30+
• Mathematically determined recombined reservoir fluid reporting corresponding flashed liquid specific gravity
and gas liquid ratio or liquid gas ratio
• Summary of various plus fraction (C7+, C10+,C12+, C20+, C30+) properties including mass and mole fractions,
Molecular Weights and Densities.

Upon receival of client call out, as per the contract minimum notice period, the job preparation starts. The
Mobilisation/Demobilisation No
1.4.1 sampling bottles (i.e. PDS, GSB and SPS) should have been redressed before sampling job. VAPS shall mobilise 3
Rate Ref
sampling bottles/cylinders for each job which would be collected and delivered to site by the Driver.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Standby Rate for Empty
No
Conventional bottle at well 1.4.2a On-site PDS and GSB standby rates.
Ref
site

Standby Rate for Surface No

1.4.2b On-site Surface sampling kit standby rate.
sampling kit at well site Ref

Standby rate for empty

No
Single-phase bottle at well 1.4.2c On-site SPS standby rates.
Ref
site

Standby Rate for single

No
Phase Sampling Kit at Well 1.4.2d On-site Single phase sampling kit standby rate.
Ref
site

Standby Rate for Open-

hole single phase sampling No
1.4.2e Standby rate for VAPS Open-hole single phase not-coated sampling bottle if VAPS is the wireline provider for PDO
bottle at well site (without Ref
non-reactive coating)

Standby Rate for open-

hole single phase sampling No
1.4.2f Standby rate for VAPS Open-hole single phase coated sampling bottle if VAPS is the wireline provider for PDO
bottle at well site (with Ref
non-reactive coating)
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Retention of bottle with

sample at PVT Laboratory No The samples would be retained beyond the 30 days after submission of interim report in case PDO would like to
1.4.3a
beyond (30) days Ref retain them for future analysis.
submission of report

Daily Rental of
conventional bottle with Daily rental of PDS and GSB bottles with samples beyond 30 days while waiting for PDO to review the report
No
sample at PVT Laboratory 1.4.3b and/or discuss with VAPS regarding the experiments before issuing the interim report or conducting further
Ref
beyond 30 days after the experiments.
submission of report

Daily Rental of single-

phase bottle with sample
No Daily rental of SPS bottles with samples beyond 30 days while waiting for PDO to review the report and/or discuss
at PVT Laboratory beyond 1.4.3c
Ref with VAPS regarding the experiments before issuing the interim report or conducting further experiments.
30 days after submission
of report

Sample Transfer (From If requested by PDO, VAPS shall transfer the oil and gas samples from third party bottles (for instance MDT bottles)
No
Third party Bottle to 1.4.3d to VAPS bottles. VAPS bottle would be connected to the third party bottle and slowly opening the valve of the third
Ref
Contractor Bottle) party bottle to transfer it to VAPS bottle at small rate to ensure smooth transfer.

Coated Open Hole Single When there is requirement for Open Hole single phase sampling, VAPS would arrange to deliver Single Phase
Phase Sampler - Daily Rate No
1.4.3f Modular champer with heating jacket. This bottle would then be connected with PDO wireline provider open hole
for 1 SPMC Set with Ref
Supporting Equipment
tool in order to rig-down to the specified depth by PDO to take the samples.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Run and Sample Recovery
No This involves connecting the Single Phase Modular champer with PDO wireline provider and collecting the sample
Charge - Per coated 1.4.3g
Ref using coated bottle.
Sample
Non-Reactive Single-Phase
Sampling Bottle - No Prior to running the Single Phase Modular champer, the bottles needs to be prepared to ensure that the coating
1.4.3h
Preparation of Sampling Ref material is sufficient to contain the H2S above 10ppm and that new orings are been used to seal it.
Bottle

Shipping and Handling of

No This involves shipping the samples within 7 days to third party labs for any analysis which can not be done in VAPS
Sample Bottles via FEDEX 1.5a
Ref lab in Oman.
(Rush)

Shipping and Handling of

No This involves shipping the samples within 30 days to third party labs for any analysis which can not be done in
Sample Bottles via Regular 1.5b
Ref VAPS lab in Oman using either Regular Airfreight or by sea.
Airfreight

No This involves transportation (collection or delivery) of bottles between VAPS lab in Muscat to/from the
Driver (Round Trip) 1.5c
Ref wellsite/third party labs/PDO labs.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Very small amount of the flashed gas and liquid samples would be run in Gas chromatography (GC) to measure
their compositions. VAPS has four GCs; two for running compositional analysis for gas samples and 2 for liquid
samples. On daily basis, VAPS runs standards on those GC to assess their accuracy while the standards have close
compositions with known mole or weight %. Helium is used as the gas carrier. The results would be reported either
in mole % or weight % for the pure components and pseudo components (plus fractions) for C7 onwards up to
C30+. The Molecular weight of the C30+ is then get calculated using the typical trends of C7 vs MW and adjusted to
the weight% of C30+. Molecular weight data for other components are obtained from CRC Handbook of Chemistry
and Physics, 88th Edition, 2002-2008.
If requested by PDO, H2S can be measured using dragger tube and its composition is input while normalising the
Compositional Analysis- other components.
R.1 R.1.1
Bottom Hole Sample Finally, the reservoir fluid get mathematically recombined using the GOR and oil density obtained from the single
phase flash experiment.
The following are standard reported properties
• Gas and liquid composition to C30+ (and N2, CO2, H2S)
• Density and Molecular Weight for the C6 to C30+
• Mathematically determined recombined reservoir fluid reporting corresponding flashed liquid specific gravity
and gas liquid ratio or liquid gas ratio
• Summary of various plus fraction (C7+, C10+,C12+, C20+, C30+) properties including mass and mole fractions,
Molecular Weights and Densities.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Very small amount of the flashed gas and liquid samples would be run in Gas chromatography (GC) to measure
their compositions. VAPS has four GCs; two for running compositional analysis for gas samples and 2 for liquid
samples. On daily basis, VAPS runs standards on those GC to assess their accuracy while the standards have close
compositions with known mole or weight %. Helium is used as the gas carrier. The results would be reported either
in mole % or weight % for the pure components and pseudo components (plus fractions) for C7 onwards up to
C30+. The Molecular weight of the C30+ is then get calculated using the typical trends of C7 vs MW and adjusted to
the weight% of C30+. Molecular weight data for other components are obtained from CRC Handbook of Chemistry
and Physics, 88th Edition, 2002-2008.
If requested by PDO, H2S can be measured using dragger tube and its composition is input while normalising the
Compositional Analysis-
other components.
Surface Sample (Separator R.1 R1.2a
Finally, the reservoir fluid get mathematically recombined using the GOR and oil density obtained from the single
Samples)
phase flash experiment.
The following are standard reported properties
• Gas and liquid composition to C30+ (and N2, CO2, H2S)
• Density and Molecular Weight for the C6 to C30+
• Mathematically determined recombined reservoir fluid reporting corresponding flashed liquid specific gravity
and gas liquid ratio or liquid gas ratio
• Summary of various plus fraction (C7+, C10+,C12+, C20+, C30+) properties including mass and mole fractions,
Molecular Weights and Densities.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Very small amount of the flashed gas and liquid samples would be run in Gas chromatography (GC) to measure
their compositions. VAPS has four GCs; two for running compositional analysis for gas samples and 2 for liquid
samples. On daily basis, VAPS runs standards on those GC to assess their accuracy while the standards have close
compositions with known mole or weight %. Helium is used as the gas carrier. The results would be reported either
in mole % or weight % for the pure components and pseudo components (plus fractions) for C7 onwards up to
C30+. The Molecular weight of the C30+ is then get calculated using the typical trends of C7 vs MW and adjusted to
the weight% of C30+. Molecular weight data for other components are obtained from CRC Handbook of Chemistry
and Physics, 88th Edition, 2002-2008.
If requested by PDO, H2S can be measured using dragger tube and its composition is input while normalising the
Compositional Analysis-
other components.
Surface Sample (Well head R.1 R1.2b
Finally, the reservoir fluid get mathematically recombined using the GOR and oil density obtained from the single
sample)
phase flash experiment.
The following are standard reported properties
• Gas and liquid composition to C30+ (and N2, CO2, H2S)
• Density and Molecular Weight for the C6 to C30+
• Mathematically determined recombined reservoir fluid reporting corresponding flashed liquid specific gravity
and gas liquid ratio or liquid gas ratio
• Summary of various plus fraction (C7+, C10+,C12+, C20+, C30+) properties including mass and mole fractions,
Molecular Weights and Densities.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Separator samples usually in triplicate are collected whenever it is not possible to collect representative downhole
or wellhead sample. It will be necessary to conduct recombination of separator samples for PVT further analysis.
Physical Recombination-
R.2 R.2.1 Once PDO advises the GOR/CGR for recombination, VAPS would boost the pressure of the gas cylinder (compress
To Specified GOR
the gas) and transfer it to a recombination bottle. Then, it would inject the associated volume of oil in that
cylinder.

Separator samples usually in triplicate are collected whenever it is not possible to collect representative downhole
or wellhead sample. It will be necessary to conduct recombination of separator samples for PVT further analysis.
Once PDO advises the saturation pressure required for recombination, VAPS would calculate the associated
Physical Recombination-
R.2 R.2.2 GOR/CGR required for Recombination and discuss it with PDO. Once PDO approve it, VAPS would boost the
To Specified Psat
pressure of the gas cylinder (compress the gas) and transfer it to a recombination bottle. Then, it would inject the
associated volume of oil in that cylinder. It might be essential (based on PDO request, optional) to carry out
saturation pressure determination to confirm the results.

Pseudo-components When breakdowns of the C7 to C9 components are required, VAPS can measure those in their current GC and
R.3 R.3
analysis report the breakdown for instance Benzene, Toluene.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Oil Samples –
Test involves charging sub-sample 30 to 35 cc to high-pressure cell. Prior to charging the sample into cell, It is
advised to restore the sample to reservoir temperature & stabilized for 24 hours at a pressure 2000 psi above the
reservoir pressure. The density of the single phase oil would be measured using coil with known volume and mass
at constant temp. The sample is expanded in incremental steps, through its bubble point, until it is around three
times its volume at bubble point. In addition to providing a calculation of saturation pressure based on changes in
phase compressibility, for the single-phase region, relative volume, average compressibility and density are
reported at each pressure step. In the two-phase region, relative volume and Y function are reported at each
pressure step. The following are standard reported properties
• Saturation pressure
• Relative volumes
• Single phase compressibility’s
• Single phase fluid densities
Pressure Volume • “Y” functions
Relation/Constant Mass R.4 R.4
Expansion (CME) study Gas Condensate Samples –
This experiment involves charging a subsample 60 to 70cc of reservoir fluid to a high-pressure visual cell. Prior to
charging the sample into cell, It is advised to restore the sample to reservoir temperature & stabilized for 24 hours
at a pressure 2000 psi above the reservoir pressure. The density of the single phase oil would be measured using
coil with known volume and mass at constant temp. The fluid is then expanded in incremental pressure stages to
about three times its volume at reservoir pressure. During this process, the dew- point is calculated (if applicable)
along with quantification of the liquid build-up below the dew point. Relative volumes are provided for each
pressure step, and deviation factor Z for the single phase region. The following are standard reported properties

• Pressure volume relationship for the gas and report the saturation pressure,
• Relative volumes
• Single phase compressibility
• Gas deviation factor Z
• Retrograde liquid deposit at each pressure step.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

This experiment is performed on a sub-sample of 60 to 80 cc of reservoir fluid. The reservoir fluid is expanded in
incremental pressure steps between bubble point and maximum expandable cell pressure or depending on the
GOR of the fluid and the uncertainty of the experiment. After each expansion, all of the evolved gas is removed
from the cell and collected. The collected gas is analysed by Gas Chromatography and its gas gravity and volume at
standard conditions are measured. The resultant shrinkage of liquid remaining in the cell is determined before
proceeding to the next pressure stage.
The following data is reported for each stage during this test; Solution gas-oil ratio, Relative Oil Volume, Relative
Total Volume, Oil Density, Gas Deviation Factor, Gas Expansion Factor and Gas Gravity. Gas viscosity is calculated
Differential Vaporisation using the Lee, Gonzales and Eakin correlation.
R.5 R.5
Analysis Following completion of the final stage gas removal the residual pressurised fluid is flashed to atmospheric
conditions to allow a mass balance and compositional check. The following are standard reported properties

• Report oil volume factor (Bo)

• Solution gas oil ratio (Rs)
• Gas volume factor (Bg)
• Liquid density
• Molecular composition and properties of liberated gas (Z factor, density, and viscosity)
• Composition of residual liquid from differential vaporization to C10+.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

The reservoir gas is depleted in approximately 7 stages from dewpoint pressure to a suitable abandonment /
maximum expandable pressure in PVT system or depending on the CGR of the fluid (not possible for low CGR to
have 7 stages sometimes as the condensate dropout is very small to be measured). The experiment involves
removing gas at a stable pressure until the overall fluid volume is returned to a constant volume reference.
Measurements are made of the volume and composition of produced gas and the retrograde liquid accumulation.
The composition of liquid in place at abandonment is measured as a discreet manner where possible; this provides
a mass balance and overall fluid composition check.
The viscosity of the gas condensate can be measured at reservoir temperature in a series of pressure steps from
Constant Volume Depletion
R.6 R.6 above reservoir pressure to dew point, although in most cases using the Lee, Gonzales and Eakin correlation data
(CVD)
to determine these values is sufficient. The following are standard reported properties
• Composition of produced fluid C12+
• Viscosity, Density and Molecular Weight of produced fluid
• Retrograde liquid deposit (percent liquid drop-out with respect to saturation pressure)
• Moles of produced fluid
• Cumulative liquid Recovery
• Single phase and Two-Phase Z-factors.
• Recoveries of various plus fractions ( C3+, C4+ and C5+)

Additional Constant Mass Similar to Pressure Volume Relation/Constant Mass Expansion (CME) study, however, the temperature is higher or
R.7 R.7
Expansion lower than the reservoir temp. This is essential for accurate phase envelope calculations.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

The viscosity of the reservoir oil is measured using a separate sub-sample at reservoir temperature in a series of
pressure steps from reservoir to atmospheric pressure, using a capillary or EMV viscometer. Once the fluid reaches
Viscosity R.8 R.8
below saturation pressure, the gas is removed and the viscosity of the oil is measured using EMV viscometer. The
gas viscosity is calculated using the Lee, Gonzales and Eakin correlation.

This test is performed by charging small volume of the reservoir fluid to the PVT cell at high pressure. The temp of
the cell is then get reduced to the temperature specified by PDO until it stabilizes. Then, the pressure is reduced to
the pressure specified by PDO until it stabilizes. The gas is removed and analysed. Then, the remaining oil get
flashed to standard conditions/ambient conditions, where the flashed oil and gas get collected and analysed to
provide a mass balance and overall fluid composition check.
Single-Stage Separator This process allows determination of the effect of the separator conditions on phase compositions, solution gas-oil
R.9 R.9.1
Test ratio, formation volume factor, and stock tank oil density. The following are standard reported properties
• Volume factors.
• Shrinkage factors.
• Separator GOR, Stock Tank GOR.
• Separator density, stock tank density & API.
• Separator & tank gas compositions, and compositional analysis of stock Tank Oil.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

This test is performed by charging small volume of the reservoir fluid to the PVT cell at high pressure. The temp of
the cell is then get reduced to the first stage temperature specified by PDO until it stabilizes. Then, the pressure is
reduced to the first stage pressure specified by PDO until it stabilizes. The gas is removed and analysed. Then, the
temp of the cell is then get reduced to the second stage temperature specified by PDO until it stabilizes followed
by the pressure is been reduced to the second stage pressure specified by PDO until it stabilizes. The gas is
removed and analysed. Then, the remaining oil get flashed to standard conditions/ambient conditions, where the
flashed oil and gas get collected and analysed to provide a mass balance and overall fluid composition check.
Three-Stage Separator test R.9 R.9.2
This process allows determination of the effect of the separator conditions on phase compositions, solution gas-oil
ratio, formation volume factor, and stock tank oil density. The following are standard reported properties
• Volume factors.
• Shrinkage factors.
• Separator GOR, Stock Tank GOR.
• Separator density, stock tank density & API.
• Separator & tank gas compositions, and compositional analysis of stock Tank Oil.

Incremental Charge for This involves subjecting a small volume of the reservoir fluid to additional separator stage, where the fluid get
R.9 R.9.2.1
each extra Stage reduced and stabilized to a new temp and pressure and the gas is been removed and analysed.

On-site Bubble Point No This test involves connecting the PDS bottles to a pump where the pressure is reduced in stages and the volume is
R.10
Determination Ref calculated, which would then be plotted to calculate the saturation pressure at ambient condition.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Rheology Experiments-
When there is a request for Rheology Experiments (Wax or Asphaltene) ; Single phase sample shall be connected
Quality Check: Bottom S.1.1 S.1.0a
to a pump to measure its opening pressure and water content.
Hole Sample

Rheology Experiments-
Atmospheric oil samples (or stock tank samples) are heated in a water bath at temp of around 60-80 degree C and
Quality Check: S.1.1 S.1.0b
then, using manual centrifuge, the water content is measured.
Atmospheric

Kinematic viscosity, defined as a fluid’s resistance to flow, is traditionally measured by noting the time taken for a
Rheology Experiments- fluid sample to travel through an orifice in a capillary under the force of gravity. This method is defined by ASTM
S.1.1 S.1.1
Viscosity D445. The time taken is noted and converted into Kinematic Viscosity, reported in Centistoke units (cSt). 1 cSt = 1
mm2/s.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Cloud Point: The test oil is required to be transparent in layers 40mm in thickness (in accordance with ASTM
D2500). The wax crystals typically first form at the lower circumferential wall with the appearance of a whitish or
milky cloud. The cloud point is the temperature at which these crystals first appear. The test sample is first poured
into a test jar to a level approximately half full. A cork carrying the test thermometer is used to close the jar. The
thermometer bulb is positioned to rest at the bottom of the jar. The entire test subject is then placed in a constant
temperature cooling bath on top of a gasket to prevent excessive cooling. At every 1°C, the sample is taken out
and inspected for cloud then quickly replaced. Successively lower temperature cooling baths may be used
Rheology Experiments-
S1.2 S.1.2 depending on the cloud point. Lower temperature cooling bath must have temperature stability not less than 1.5 K
Wax
for this test.
Pour Point: The pour-point temperature is the lowest temperature at which the oil is mobile. This is usually
identified as the stock-tank-oil gelation temperature. The ASTM pour-point test, similar to the ASTM cloud point
tests, involves placing a sample of the fluid in a jar and cooling it in a temperature-controlled bath. At each 3°C
temperature step, the sample is tested by tipping the jar to determine if the oil is still mobile.
Wax content by UOP 46-64 method: Oil sample will be solved in toluene, and Asphaltene will be removed. Remain
will be dissolved in aceton-petroleun naphta and chilled to -17 oC. Wax will be removed/weighted and reported.

A subsample of the reservoir fluid is charged to the PVT cell at higher pressure than reservoir pressure. The
pressure is reduced at constant temperature in stages. During each depressurization of the fluid, a sub-sample is
Rheology Experiments- taken through a 0.5 micro-filter. A UV/Visible absorption technique is used to determine the asphaltene content of
S.1.3 S.1.3
Asphaltanes the sub-samples of stabilized liquid. The asphaltene content is then get plotted vs Pressure and a decrease in the
asphaltene content of the produced liquid demonstrates the deposition. This test can be repeated for various
Temperatures.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Miscibility Related
The composition of the gas would be provided by PDO in mole% or weight%. VAPS would then arrange to create
Experiments- Synthetic S.2.1 S.2.1
600-2000cc of synthetic gas to match the compositions provided by the client.
Gas Preparation

A pre-determined volume of injection gas is added to the reservoir fluid (after it is been charged to the PVT cell
and CCE is completed) and the total sample volume is measured and the increase in sample volume is determined.
The newly created sample is subjected to a CCE experiment, as described above and the saturation pressure and
Miscibility Related
liquid shrinkage data re-measured.
Experiments- Solubility
S.2.2 S.2.2.1
Swelling Experiment with
The composition of each fluid mixture is calculated from the measured reservoir fluid and gas injection
Synthetic Produced Gas
compositions, together with the mole/mole recombination ratio. The composition of the final mixture is measured.
The swelling test consists of several gas injections but it is fairly typical to perform five fluid mixtures and CCE
experiments, culminating in the creation of a gas condensate fluid after the last gas addition.

A pre-determined volume of injection gas is added to the reservoir fluid (after it is been charged to the PVT cell
and CCE is completed) and the total sample volume is measured and the increase in sample volume is determined.
The newly created sample is subjected to a CCE experiment, as described above and the saturation pressure and
Miscibility Related
liquid shrinkage data re-measured.
Experiments- Solubility
S.2.2 S.2.2.2
Swelling Experiment with
The composition of each fluid mixture is calculated from the measured reservoir fluid and gas injection
Company Supplied Gas
compositions, together with the mole/mole recombination ratio. The composition of the final mixture is measured.
The swelling test consists of several gas injections but it is fairly typical to perform five fluid mixtures and CCE
experiments, culminating in the creation of a gas condensate fluid after the last gas addition.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Miscibility Related No After the injection gas is been mixed with the reservoir fluid at a ration specified by the client, small volume of the
S.2.2.3
Experiments- Viscosity Ref mixture get measured in EMV for viscosity.

These experiments involve displacement reservoir fluid in a packed column by injecting injection gas (lean, rich or
CO2 gas). The column can be 40 foot long pre packed with glass beads or Ottawa sands ¼ “ OD length coiled
stainless steel tubing. However, alternative column dimensions and packing materials can be manufactured if
Miscibility Related
required. The porosity & permeability column is measured at the beginning of the each displacement test
Experiments- Slim Tube
S.2.3 S.2.3.1 pressure. Typically, 4 to 6 runs are required to accurately define the minimum miscibility pressure. A plot of
Test Synthetically Supplied
recovered oil volume at 1.0 or 1.2 pore volumes versus test pressure will indicate the minimum miscibility pressure
Gas
of the reservoir fluid, for the selected injection gas composition.
Data is collected throughout the displacement process which includes injected volume, recovered volume, outlet
density and GOR. It is also possible to obtain samples of the produced gas for compositional analysis.

These experiments involve displacement reservoir fluid in a packed column by injecting injection gas (lean, rich or
CO2 gas). The column can be 40 foot long pre packed with glass beads or Ottawa sands ¼ “ OD length coiled
stainless steel tubing. However, alternative column dimensions and packing materials can be manufactured if
Miscibility Related
required. The porosity & permeability column is measured at the beginning of the each displacement test
Experiments- Slim Tube
S.2.3 S.2.3.2 pressure. Typically, 4 to 6 runs are required to accurately define the minimum miscibility pressure. A plot of
Test Company Supplied
recovered oil volume at 1.0 or 1.2 pore volumes versus test pressure will indicate the minimum miscibility pressure
Gas
of the reservoir fluid, for the selected injection gas composition.
Data is collected throughout the displacement process which includes injected volume, recovered volume, outlet
density and GOR. It is also possible to obtain samples of the produced gas for compositional analysis.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Interfacial Tension
S.3 S.3 Contact angle or IFT is measured between the oil and water for core analysis studies.
Measurements
Non-Hydrocarbon No
No Ref This involves collecting the gas samples in plastic bags.
Analysis- Sampling Ref

Non-Hydrocarbon Mercury is toxic and corrosive element which varies in concentration from ng/m3 to mg/m3 in gas from
Analysis- Mercury S.4 S.4.1a Hydrocarbon reservoirs. Element mercury analysed by Sir Galahad Mercury analyser or alternative equipment. It is
Analysis preferable to conduct mercury in site for accurate representation.

Non-Hydrocarbon Radon-222 is radioactive isotope, originates from radium-226, has shelf life of 3.8 days. Analysis is performed on
S.4 S.4.1b
Analysis- Radon Analysis dedicated Radon detector

Non-Hydrocarbon
Sulphur species can be done either by GC-SCD which typically provides the various Sulphur components/elements
Analysis- Sulphur Species S.4 S.4.1c
(up to 30 elements) including H2S and Mercaptans.
Analysis

Non-Hydrocarbon
Analysis- Analysis of Trace
Argon, Helium and Nitrogen are non combustible gases analysed in laboratory in gas chromatography with thermal
Gas Components ( Helium, S.4 S.4.1d
conductivity detector. H2S is analysed using dragger tubes.
Oxygen, Nitrogen, H2S &
Argon)
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Non-Hydrocarbon
Analysis- Condensate
Analysis (Polonium 210,
Polonium i a radioactive isotope analysed by radon or alpha spectrometry method.
Mercury, Iron, Nickel,
S.4 S.4.2 Sulphur content in crude is analysed by an ICP-AAS method.
Vanadium, Radon, Total
Heavy metals (such as Nickel, Vanadium, Iron) are analysed using neutron activation method.
Chlorides, Asphaltanes,
Total Sulphur and Other
Sulphur Components)

Chloride (total halide) was determined by potentiometric titration on a Metrohm 888 Titrando using a Metrohm
Water Analysis - silver titrode and 0.1 M silver nitrate as titrant calibrated with a 1000 mg/L chloride standard. Bromide, iodide and
Components (Alkalinity, thiosulphate correction was applied using the data obtained from ion chromatography.
Chlorides, Sulphate, S.4 S.4.3a A known mass of filtered (0.2 µm) sample was transferred to a separate tared beaker and evaporated to insipient
Barium/Strontium, dryness in an oven set at 70ºC. The oven temperature was then increased to 110ºC and then 140ºC and the sample
Suspended Solids) dried to constant mass. The oven was then set at 180ºC and the sample dried to constant mass before recording a
final mass. The TDS was then calculated from the mass ratio of sample residue to sample taken.

Conductivity was determined with a Multiline P3 pH/Conductivity meter or alternative meter. A potential is
Water Analysis -
S.4 S.4.3b applied between two electrodes with defined areas. The electrodes are immersed in the water sample, and
Conductivity
conductivity is read directly from the instrument. Resistivity is calculated from conductivity.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

The pH was determined by potentiometer measurement using a Multiline Sen Tix 41 combined pH electrode with
integrated temperature probe or alternative equipment. The electrode consists of a glass electrode and a
Water Analysis - pH S.4 S.4.3c reference electrode in a single unit. Hydrogen ion activity is registered via a hydrogen sensor and the signal is
converted to a digital read out by the pH-meter. The temperature at which measurements were made at was
recorded.

Density was measured using an Anton Paar DMA-4500 density meter or alternative device. A fixed volume, u-
shaped glass tube in contact with an oscillator, was filled with the sample. The oscillation-frequency of the
Water Analysis - Density S.4 S.4.3d
undamped glass-tube is mass dependent, thus density of the sample can be determined from the oscillation
frequency.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Chloride (total halide) was determined by potentiometric titration on a Metrohm 888 Titrando using a Metrohm
silver titrode and 0.1 M silver nitrate as titrant calibrated with a 1000.1 mg/L chloride standard. Bromide and
iodide correction was applied using the data obtained from ion chromatography.
The weak acid anions (C1-C5br) and total carbonate species (expressed as bicarbonate) were separated from each
other and any interfering species by ion exclusion chromatography and detected by suppressed conductivity using
the analytical parameters listed below. Quantification was by reference to a series of external standards, taking
Water Analysis - 12 Ion into account any contribution from the blank (deionised water, used for dilutions and standard preparation).
S.4 S.4.3e
Analysis All cations, boron, phosphorus, silicon and Sulphur were determined by ICP–OES using a Perkin Elmer DV4300 ICP-
OES calibrated with certified standard reference materials. Dilutions were prepared using 2% v/v nitric acid in
order to bring the concentrations of the species of interest into the calibration range, and to reduce the
concentration of salt entering the plasma. Cobalt and Yttrium were employed as internal standards.

Total species were determined on an unfiltered aliquot of the non preserved samples after acidification to
redissolve any precipitated species.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Chloride (total halide) was determined by potentiometric titration on a Metrohm 888 Titrando using a Metrohm
silver titrode and 0.1 M silver nitrate as titrant calibrated with a 1000.1 mg/L chloride standard. Bromide and
iodide correction was applied using the data obtained from ion chromatography.
The weak acid anions (C1-C5br) and total carbonate species (expressed as bicarbonate) were separated from each
other and any interfering species by ion exclusion chromatography and detected by suppressed conductivity using
the analytical parameters listed below. Quantification was by reference to a series of external standards, taking
Water Analysis - 20 into account any contribution from the blank (deionised water, used for dilutions and standard preparation).
S.4 S.4.3f
Element Analysis All cations, boron, phosphorus, silicon and sulphur were determined by ICP–OES using a Perkin Elmer DV4300 ICP-
OES calibrated with certified standard reference materials. Dilutions were prepared using 2% v/v nitric acid in
order to bring the concentrations of the species of interest into the calibration range, and to reduce the
concentration of salt entering the plasma. Cobalt and Yttrium were employed as internal standards.

Total species were determined on an unfiltered aliquot of the non preserved samples after acidification to
redissolve any precipitated species.

Water Analysis - Trace

Mobilisation of the Trace elements from Oman PVT lab to site which shall include either the water analysis kit or
Element Testing S.4 S.4.4
the mercury kit.
Equipment Mob

Water Analysis - Trace

Element Testing S.4 S.4.5 Rental of the Trace element kit on site starting from the day of mobilisation from base country.
Equipment Rental
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Water Analysis -
S.4 S.4.6 Daily rental for additional engineer for the Trace element analysis if required.
Additional Specialist Staff

Water Analysis - Water

Analysis - Ionic Polonium i a radioactive isotope analysed by radon or alpha spectrometry method.
composition - Non- S.4 S.4.7 Sulphur content in crude is analysed by an ICP-AAS method.
Preserved Sample Only - Heavy metals (such as Nickel, Vanadium, Iron) are analysed using neutron activation method.
standard suite

Chloride (total halide) was determined by potentiometric titration on a Metrohm 888 Titrando using a Metrohm
Water Analysis - Water silver titrode and 0.1 M silver nitrate as titrant calibrated with a 1000 mg/L chloride standard. Bromide, iodide and
Analysis - bicarbonate / thiosulphate correction was applied using the data obtained from ion chromatography.
carbonate / total alkalinity S.4 S.4.8 A known mass of filtered (0.2 µm) sample was transferred to a separate tared beaker and evaporated to insipient
/ hydroxide by pH titration dryness in an oven set at 70ºC. The oven temperature was then increased to 110ºC and then 140ºC and the sample
with HCl dried to constant mass. The oven was then set at 180ºC and the sample dried to constant mass before recording a
final mass. The TDS was then calculated from the mass ratio of sample residue to sample taken.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Chloride (total halide) was determined by potentiometric titration on a Metrohm 888 Titrando using a Metrohm
silver titrode and 0.1 M silver nitrate as titrant calibrated with a 1000 mg/L chloride standard. Bromide, iodide and
Water Analysis - Water thiosulphate correction was applied using the data obtained from ion chromatography.
Analysis - Oil in water S.4 S.4.9 A known mass of filtered (0.2 µm) sample was transferred to a separate tared beaker and evaporated to insipient
/water effluents dryness in an oven set at 70ºC. The oven temperature was then increased to 110ºC and then 140ºC and the sample
dried to constant mass. The oven was then set at 180ºC and the sample dried to constant mass before recording a
final mass. The TDS was then calculated from the mass ratio of sample residue to sample taken.

On-Site measurements-
S.5 S.5.1a This involves collection of gas samples iso-kinetically.
Iso-Kinetic Sampling

On-Site measurements-
Iso-Kinetic Sampling Kit S.5 S.5.1b This involves mobilisation of the Iso-kinetic equipment from Oman PVT lab to site.
Mobilisation

On-Site measurements-
Iso-Kinetic Sampling Kit S.5 S.5.1c This involves the daily rental of the Iso-Kinetic equipment from the day it mobilise from base country.
Rental

On-Site measurements-
On Site Gas- S.5 S.5.2a Analysis of gas composition onsite using Micro GC.
Chromatography
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

On-Site measurements-
S.5 S.5.2b This involves mobilisation of the equipment set (Micro GC) from Oman PVT lab to site.
GC Mobilisation

On-Site measurements-
S.5 S.5.2c This involves the daily rental of the Micro GC from the day it mobilise from base country.
GC Rental

On-Site measurements-
S.5 S.5.3 Daily rental of the specialist to run the Micro GC while on site.
Additional Specialist Staff

Separator samples usually in triplicate are collected whenever it is not possible to collect representative downhole
or wellhead sample. It will be necessary to conduct recombination of separator samples for PVT further analysis.
Once PDO advises the requirement for Thermal experiments i.e. Temperature > 200 C and the saturation pressure
Thermal Experiments-
required for recombination, VAPS would calculate the associated GOR/CGR required for Recombination and
Physical Recombination To R.2 T.0.1a
discuss it with PDO. Once PDO approve it, VAPS would boost the pressure of the gas cylinder (compress the gas)
Specified GOR
and transfer it to a recombination bottle. Then, it would inject the associated volume of oil in that cylinder. It
might be essential (based on PDO request, optional) to carry out saturation pressure determination to confirm the
results.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Separator samples usually in triplicate are collected whenever it is not possible to collect representative downhole
or wellhead sample. It will be necessary to conduct recombination of separator samples for PVT further analysis.
Once PDO advises the requirement for Thermal experiments i.e. Temperature > 200 C and the saturation pressure
Thermal Experiments-
required for recombination, VAPS would calculate the associated GOR/CGR required for Recombination and
Physical Recombination To R.2 T.0.1b
discuss it with PDO. Once PDO approve it, VAPS would boost the pressure of the gas cylinder (compress the gas)
Specified Psat
and transfer it to a recombination bottle. Then, it would inject the associated volume of oil in that cylinder. It
might be essential (based on PDO request, optional) to carry out saturation pressure determination to confirm the
results.

Thermal Experiments-
Single Stage Equilibrium No This test involves flashing a sub-sample of the oil sample to atmospheric conditions and collecting the gas and oil
T.0.2
Flash of Oil Sample Ref samples while measuring the GOR and the API of the stock tank flashed oil.
(includes GOR, API)
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Upon PDO requirement for Thermal experiments i.e. Temperature > 200 C; Very small amount of the flashed gas
and liquid samples would be run in Gas chromatography (GC) to measure their compositions. VAPS has four GCs;
two for running compositional analysis for gas samples and 2 for liquid samples. On daily basis, VAPS runs
standards on those GC to assess their accuracy while the standards have close compositions with known mole or
weight %. Helium is used as the gas carrier. The results would be reported either in mole % or weight % for the
pure components and pseudo components (plus fractions) for C7 onwards up to C30+. The Molecular weight of the
C30+ is then get calculated using the typical trends of C7 vs MW and adjusted to the weight% of C30+. Molecular
weight data for other components are obtained from CRC Handbook of Chemistry and Physics, 88th Edition, 2002-
2008.
Thermal Experiments-
If requested by PDO, H2S can be measured using dragger tube and its composition is input while normalising the
Compositional Analysis for
R.1 T.0.3 other components.
Recombined Fluid up to C
Finally, the reservoir fluid get mathematically recombined using the GOR and oil density obtained from the single
30+
phase flash experiment.
The following are standard reported properties
• Gas and liquid composition to C30+ (and N2, CO2, H2S)
• Density and Molecular Weight for the C6 to C30+
• Mathematically determined recombined reservoir fluid reporting corresponding flashed liquid specific gravity
and gas liquid ratio or liquid gas ratio
• Summary of various plus fraction (C7+, C10+,C12+, C20+, C30+) properties including mass and mole fractions,
Molecular Weights and Densities.
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Test involves charging sub-sample 30 to 35 cc to high-pressure cell. Prior to charging the sample into cell, It is
advised to restore the sample to reservoir temperature & stabilized for 24 hours at a pressure 2000 psi above the
reservoir pressure. The density of the single phase oil would be measured using coil with known volume and mass
at constant temp. The sample is expanded in incremental steps, through its bubble point, until it is around three
Thermal Experiments-
times its volume at bubble point. In addition to providing a calculation of saturation pressure based on changes in
Constant Composition
phase compressibility, for the single-phase region, relative volume, average compressibility and density are
Expansion (CCE) per each
T.1.1 T.1.1 reported at each pressure step. In the two-phase region, relative volume and Y function are reported at each
Temperature ≤ 150 C with
pressure step. The following are standard reported properties
Liquid Volume
• Saturation pressure
Measurements
• Relative volumes
• Single phase compressibility’s
• Single phase fluid densities
• “Y” functions

Thermal Experiments- HP
The viscosity of the reservoir oil is measured using a separate sub-sample at reservoir temperature in a series of
Capillary Viscosity at each
T.1.2 T.1.2 pressure steps from reservoir to atmospheric pressure, using a capillary or EMV viscometer. Once the fluid reaches
Specified Pressure and
below saturation pressure, the gas is removed and the viscosity of the oil is measured.
Temperature
 Vision Advanced Petroleum Solutions LLC

Method Statement Scope Understanding

Test involves charging sub-sample 30 to 35 cc to high-pressure cell. Prior to charging the sample into cell, It is
advised to restore the sample to reservoir temperature & stabilized for 24 hours at a pressure 2000 psi above the
reservoir pressure. The temperature is been get increased in the cell to the desired temp (typically less than 250
degree C).The density of the single phase oil would be measured using coil with known volume and mass at
Thermal Experiments- constant temp. The sample is expanded in incremental steps, through its bubble point, until it is around three
Constant Composition times its volume at bubble point. In addition to providing a calculation of saturation pressure based on changes in
Expansion (CCE) per each phase compressibility, for the single-phase region, relative volume, average compressibility and density are
T.2.1 T.2.1
Temperature >150 C with reported at each pressure step. In the two-phase region, relative volume and Y function are reported at each
Liquid Volume pressure step. The following are standard reported properties
Measurements • Saturation pressure
• Relative volumes
• Single phase compressibility’s
• Single phase fluid densities
• “Y” functions

Thermal Experiments- HP
The viscosity of the reservoir oil is measured using a separate sub-sample at the desired high temperature in a
Capillary Viscosity at each
T.2.2 T.2.2 series of pressure steps from reservoir to atmospheric pressure, using a capillary or EMV viscometer. Once the
Specified Pressure and
fluid reaches below saturation pressure, the gas is removed and the viscosity of the oil is measured..
Temperature
Fluid Sampling & Analysis
PVT (Pressure, Volume, Temperature) Studies
PVT analysis provides description of thermodynamic properties/behaviour that exists at
reservoir conditions and throughout the production & processing systems. PVT analysis
essential for all reservoirs to describe the relationships that exit between pressure, volume,
temperature and phase composition. Accurate Fluid analysis is key element in the
development of hydrocarbon reservoirs and optimization of surface processing and
transportation facilities. Accurate data is required to construct and tune a significant equation
of state to mathematically model the fluid behaviour at any conditions likely to be
encountered during the life of the field.

This type of analysis is carried out at the vision advanced petroleum solution, Muscat one of
latest and the best equipped facilities available to the oil industries in the Gulf Region.

Applications:

Physical & compositional analysis of all types

Reservoir fluids including

Black oil

Heavy oil

Volatile oil/Critical oil

Gas condensate (Rich/lean)

Dry/ wet gas

Pipeline fluids

Plant fluids

Features: Benefits:

ISO 9000-2000 registered Short turnaround time

In House Laboratory Flexible analysis time

Multiple equipments available Correct characterisation critical fluids

Measurement range 15C to 200 C Traceable QA process

Atmospheric pressure to 15000 psi Sample management

PVT Studies

Services Provided

Sample Transfer from MDT, MPSR & RCI Chambers

Sample restoration and conditioning

Sample validation

Pressured Density

Compositional analysis of pressurised fluids to C36+

Physical Recombination of separator samples for any specified GOR.

Constant mass expansion (P V relationship)

. Measurement of saturation pressure

. Measurement of Liquid shrinkage

. Measurement of Dew point

Reservoir Depletion studies

.Differential Vaporisation

.Constant Volume Depletion (for gas condensate & Volatile fluid)

Reservoir fluid viscosity for black oil & gas condensate

EOR/Multi contact studies

Single stage & multistage separator studies for black oil & gas condensate studies

Flow assurance & production chemistry

Pipeline fluid phase behaviour and contamination studies

Enhanced Oil Recovery (EOR)
Enhanced oil recovery (abbreviated EOR) is the implementation of various techniques for increasing
the amount of crude oil that can be extracted from an oil field. The global average recovery factor for
a typical oilfield is approximately 40%. This result in a large amount of identified oil left behind despite
an existing production infrastructure. Using EOR 40 to 60% oil can be recovered. Prior to launching
into an expensive project to recover additional oil from a reservoir, the process can be simulated in the
laboratory to establish project viability. Knowledge optimum injection pressure & injection gas (Rich, Lean)
is very important to viability of project.

Vaps Enhanced oil recovery analysis uses High

pressure PVT glass windowed cell, gas chromatograms

slime tube apparatus, EMV along with other equipments

are all used to measure physical and compositional

properties.

Studies are designed with client consultation and interim

results are provided so that modification can be during

course of the experiments.

Applications:

Swelling & solubility studies

Slim tube studies

Multi contact studies (back ward & forward contact)

Gas Revaporization studies

Equilibrium contact

Inter Facial Tension

Features: Benefits:

Studies can be fully defined or can be changed Client has complete control over studies

during course of tests based interim results pressure & injection ratios.

Test process is simulated with EOS software before Turn around time reduced

conducting studies.

Enhanced Oil Recovery (EOR)

Technical Specifications:

Services provided

Preparation of injection gases

Preparation live fluid sample from stock tank oil.

Single component Hydrocarbon or Non Hydrocarbon gases or mixture of both

Synthetic gas can be enriched with NGL

Swelling / Solubility studies

Equation of state (EOS) simulation with tuned or untuned data

Gas additions targeted saturation pressure

Gas additions targeted gas/liquid concentrations

Percent of liquid level measurement below saturation pressure

Percent of liquid level measurement below dew point pressure at last gas additions.

Constant mass expansion data to desired level of expansion

Miscibility studies

Equation of State (EOS) simulation with tuned or untuned data

Type of injection gases

Displacement at specified pressure

Determination minimum miscibility pressure

Gas analysis of up to C15

Liquid analysis to C36+

Density measurement displaced oil

Multi contact studies

Backward multi contact studies, original oil is multi contacted with fresh injection gas

Forward multi contact studies,

Equilibrium contact studies, stage pressures as per client request

Condensate or Revaporisation studies

Simulating gas injection into gas reservoir for gas enrichment and recovery intermediate liquid components

from condensed retrograde liquids

Gas injection or production can be performed either constant volume or differential basis.

Detail options available as per solubility / swelling studies

 Down-Hole Sampling

A. Summary of Operations

Downhole sampling involves capturing reservoir fluid samples at reservoir conditions. To

obtain accurate compositional and PVT analyses of these samples, the recovered samples
must remain in downhole conditions. Special chambers compensate for the pressure drop as
the samples are returned to the surface.

B. Sampling Tool

Pressure Compensated Sampler (PCS) non-corrosive

Downhole sampling involves capturing reservoir fluid samples at reservoir

conditions. To obtain accurate compositional and PVT analyses of these samples,
the recovered samples must remain in downhole conditions. Special chambers
compensate for the pressure drop as the samples are returned to the surface.
VAPS PCS is single-phase downhole sampling tool with pressure compensation
system to keep the sample in single phase condition from reservoir to surface.

Technical Specifications: Features:

Length 4.16 m Non corrosive

Weight 38 kg works under high H2S & CO2

Working pressure 1000 bar and high GOR containing well

Working Temperature 180C Positive displacement operation

Sample capacity 540 cc no pressure differential across sampling port

due

Maximum OD 44 mm slow positive displacement of floating system

Material Inconel No recombination required

Test pressure 15000 bar As sample is in single phase at surface,

Design Code ASME VIII no lengthy sample transfer required

Max time delay 84 hours

Certified by DNV

Applications: Benefits:
Single phase reservoir sampling is widely non corrosive design provides almost no loss
 been accepted as industries standards for H2S sample in the sampler

PVT sampling, Asphaltene studies and unlike conventional sampler PCS maintains

Water studies, In addition sampler also single phase all the way to the surface

find applications in gas condensate Fast sample transfer

Field where it is important obtain sample Fast redress of sampler

in single phase.

C. Summary of Operations

Operation Highlights:

• The Bottom hole samples is to be captured from Fahud Natih B (F-668) at flowing
conditions at the optimum minimum choke size. It is highly recommended to run
gradient survey to confirm sampling depth and down hole pressure & temperature.
Note, down hole pressure will be used to prepare and charge up the sampling tools.
• All parties should be in agreement with the selection of the sampling station depth. Thus
the sampling depth needs to be decided based on the pressure gradient survey. This
survey will depict the possible fluid contacts of water, oil and/gas.
• Rig up Slickline and place lubricator above Charismas Tree. Set tool activator
(mechanical clock) to the calculated time required to reach the sampling depth + two
hours to allow tool closure.
• Assemble and connect BHA ( SRSs + Gauge) in tandem to slickline. It is recommended to
run a pressure gauge on slick line with the bottom hole samplers in order to verify the
time of sample collection and the bottom hole pressures while sampling. Downhole
gauge will be provided by third party.
• RIH the bottomohole samplers at static condition and land samplers at the dedicated
and pre-determined sampling station.
• After sample collection POOH the BH Samplers. Confirm tool closure and that the
samples are collected successfully.
 • Heat and condition the samples for one hour.
• Transfer bottomhole samples into shippable sample bottles (SPS)

Recommendation and Comments

All bottles, samplers and analysis equipment will be provided by VAPS and VAPS will also take
care of the labeling and shipment of samples to the Lab in Muscat. See the below bottle
requirement table; this indicates the number of bottles/ containers required.

Table 1:
Sample Bottle Requirements for two BHS ;
All Samples will be shipped to Muscat Lab once labeled on site

item Description Qty Volume Comments

1 Bottomhole Samplers 2 600 ml BHS tools

Bottomhole Samples- Shippable For the collection of pressurized

2 2 600 ml
(SPS) BHS
Fluid Sampling

Sample Transfer Unit for BHS Sampling

VAPS PCS downhole sample transfer unit allows sample transfer and preparation of sampling

tools. Samples can be transferred to either single or two phase positive displacement bottles.

The unit is pneumatically powered to operate the synthetic oil and glycol. The unit is also fitted with

Autoclave universal safety head containing rupture disk. If required unit allows validation to be carried

After transfer to measure bubble point and comparison between samples.

Technical Specifications:

Working pressure 1000 bar

Weight 42 kg

Length 570 mm

Width 340 mm

Height 430 mm

Material Stainless Steels

Test Pressure 1500 bar

Applications:
Designed to use all VAPS downhole tools as wells

As RCI chambers, MDT tools or any well head sample

Transfer or cylinder transfers.

Features: Benefits:
Mercury free operation Fast sample transfer time

Onsite bubble point determination As no recombination required sample

Leak testing sample transfer cylinders & lines transfer can be performed in minimum time

The unit can be easily dissembled and transported with no reduction in sample quality.

By air thus enabling rapid mobilisation worldwide.

 Separator Sampling
A. Summary of Operations

The objective is to collect separate samples of the gas and liquid exiting the separator and to
measure the separate flow rates of the two phases and obtain the gas-oil ratio (GOR). Although the
two phases are never in perfect equilibrium, providing that the two samples are representative of the
separate flows, it is possible to mix the two samples together in the same proportion in which they are
produced t obtain a recombined sample that represents the fluid entering the separator.

This method often used has back up for data that

can be used to validate downhole sample &
wellhead samples or check aleady known reservoir
composition.

For high quality recombination- Vaps use vaccum

displacement method for gas samples & positive
diaplacement method for oil samples.

Issues:

Some of key consideration related to successful separator sampling are

Collection of seprator samples at first stage separator itself

Stable flow rates & low flow rates for minimum 24 hours prior to sampling

Separator capacity is sufficient to allow gas & liquid phase to separate

Calibrated oil & gas flow meters to measure accurate flow rates

No chemical injection during sampling

Well flow should be natural, no injection gas or artificial lift.

Features & Benefits:

Economical

Portable equipments, easy to dissemble & ship by plane

Full control of sampling process

Relatively quick to assemble sampling unit

B. Summary of Operations
Separator Sampling
Three sets of PVT separator samples (3 separator oil samples and 3 separator gas
samples) will be collected at the optimum minimum choke size. Sampling steps are
described below:

1 Open well at the optimum minmum possible choke size and divert flow through separator.
This to ensure that the well is flowing in single phase.

2 Once stable conditions are achieved i.e. the gas rate and FTHP change within 1% in 30 min,
collect 3 sets of separator samples (1 set is: 1 separator oil sample and 1 gas separator
sample).

3 During the sampling period Well test unit should record the GOR, gas rate, oil rate and
water rate every 15 mins.

4 VAPS Sampling engineer should record the flowing rates aligned with the pressures when
collect surface sampling.

5 VAPS sampling engineer should label the surface sampling 1 content : well name, date,
time, FTHP, FTHT and rate

Separator Sampling Procedures:

Liquid surface sample using PDS bottles

• Check Sample Bottle Status Form and Sample Bottle Certificate, Bottle
pressure tested certificate have to be valid.
• Place sample bottle in stand.
• Fit upper and lower manifold in to the sample bottle
• Connect glycol/water pump to the lower manifold
• Flush manifold with glycol/water prior to tightening connection to bottle
• Connect liner between upper manifold and sampling point
• Ensure all valves are closed
• Pressure up liner by opening valve on sampling point
• Purge line through bleed valve
• Proceed to take sample by gently opening lower bleed valve and allowing
sample to displace water into measuring cylinder.
• Maintain separator pressure on gauge at all times to avoid sample flash using
the needle valve at the lower manifold.
• A 600 cc sample should be taken then Secure your sample by closing the
sample port valve at the sample bottle
• Create a 10% gas cap for safe transportation.
• Record the final pressure, the ambient temperature and the end time of
Sampling.
• Close the bottom valve at the sample bottle.
• Bleed down the pressure and disconnect liners and manifolds
Separator Sampling
• Check bottle for leaks, label the bottle and box and complete a surface
sample datasheet.

Gas surface sample using GSB bottles

• Check bottle has been evacuated to less than 1.0 mbar or less than 10
MmHg

• Connect gas manifold to top valve on bottle, with suitable test gauge
• Connect liner between separator gas sampling point and gas manifold.
• Check both GSB valves are closed
• Purge at least five liner volumes of gas through the gas manifold
• Close the bleed valve, the gas manifold gauge should now read separator
pressure.
• Crack open bottle valve GSB V1, avoiding pressure drop on gauge. Record
time for commencing sampling.
• Sampling time for 20 liter cylinder should be 20-30 mins - periodically
check Bottle is filling by cycling GSB V1 again avoiding pressure drops on
gauge.
• When bottle is full close GSB valve.
• Open cylinder top valve and confirm gas manifold gauge pressure rises to
original sampling pressure. (This confirms cylinder is full of gas and did not
plug during sampling).
• Open the GSB to restore separator pressure to bottle.
• Close GSB valve and record the final pressure, ambient temperature and the
time for the completion of sampling
• Close the valves and bleed down liner and gas manifold pressure.
• Check bottle for leaks, label the bottle and box and complete a surface
sample datasheet.

Recommendation and Comments

All bottles, samplers and analysis equipment will be provided by VAPS and VAPS will
also take care of the labeling and shipment of samples to the Lab in Muscat. See the
bottle requirement table on the below table; this indicates the number of bottles/
containers required.
Separator Sampling
Table 1:
Sample Bottle Requirements for three sets of Separator Sampling;
All Samples will be shipped to Muscat Lab once labeled on site

item Description Qty Volume Comments

1 Positive 3 600 ml For the collection of

Displacement pressurized oil
Sampler (PDS) samples from the
separator.

2 Gas Sampling 3 20 liters For the collection of

Bottles (GSB) gas samples from
separator for PVT
studies.
Fluid Sampling
Non-Hydrocarbons & Trace Elements
Trace elements & non-hydrocarbons are always present in natural gas, condensate crude oil present
in the underground reservoir. These are accurately quantified prior filed developments has they
consider has impurities or contamination to the hydrocarbons.

Some of constituents are toxic or poisonous & fractions can dilute over all composition of crude
oil/gas, thereby reducing the calorific valves. Others are corrosive in nature, which requires forces to
use special design and materials to use in upstream processing & transportation systems, while
others are non-combustible, thereby reducing economic value.

The most important non-hydrocarbon constituents in the hydrocarbon fluids are

.Sulphur compounds-largest group of non-hydrocarbons in crude oil

.Non-combustible gases (N2, CO2, Helium, Argon etc)

.Radioactive Components (Radon)

.Mercury

.Organometalllic Compounds (Vanadium, nickel, copper, iron)

.Formation Water

Analysis of hydrocarbons requires special precautions, has some of components have tendency to
adsorb with sampling system. This can lead to reduction in measured concentration. Also radioactive
elements may be affected by delays in the analysis. There for analysis should be performed onsite on
line system or on samples especially collected or preserved for later analysis.
Fluid Sampling
Non-Hydrocarbons & Trace Elements
Vaps experience in onsite gas sampling and analysis

And can perform following analysis

Hydrogen Sulphide (H2)

Natural gases contain hydrogen sulphide from very

Small concentration ppm level to several percentage

According client vaps can offer several field methods

a) Gastec or dragger tubes under line pressure, various tubes are available from 2 ppm to 40%.
A simple & robust method.
b) Potentiometric/Iodometric titration (UOP-212,ASTM 2385), highly recommended for low ppm
level
c) Jerome-H2S analyzer, Handheld instruments works on gold-film principle provides quick
approximate determination H2S in ppm level.
d) Microcoulometric method.

Mercapatans (R-SH)

Mercapatans are known also as thiols, various marcapatans found in the crude oil & odour
contributed by small quantities of these materials led to the name sour crude. Analysis performed with
Gastec/ Drager tubes, potentiometric titration (UOP-212, or ASTM 23850) or microcoulometric
methods.

Carbonyl Sulphide- potentiometric titration (UOP 212)

Carbon Dioxide (CO2)

Carbon Dioxide is a corrosive but stable gas. The content in natural gas can vary from few ppm to
over 90%. Analysis performed by Gastec or Drager tubes, Orsat gas analyser or onsite gas
chromatography.

Radon-222 (Rn)

Radon-222 is radioactive isotope, originates from radium-226, has shelf life of 3.8 days. Analysis is
performed on dedicated Radon detector.

Mercury (Hg)

Mercury is toxic and corrosive element which varies in concentration from ng/m3 to mg/m3 in gas
from Hydrocarbon reservoirs. Element mercury analysed by Sir Galahad Mercury analyser.

Argon (Ar), Helium (He) & Nitrogen (N2)

They are non combustible gases analysed in laboratory in gas chromatography with thermal
conductivity detector

Arsenic (As), Can be absorbed in Charcoal & analysed in onshore

Fluid Sampling
Non-Hydrocarbons & Trace Elements
Oil and Gas condensate Analysis:

Vaps can perform following non-hydrocarbon analysis in oil /condensate:

Water content:

Small amount of water up to 3% are determined by coulometric Karl Fisher titration

Above 3% can be determined by centrifuge BSW

Salt in crude:

Salt in crude is analysed by either chloride titration method or conductivity method based on
IP 265.

Sulphur content:

Sulphur content in crude is analysed by an ICP-AAS method. It’s an important sales

parameter in crude.

Heavy metals: Nickel, Vanadium, Iron, Mercury.

Heavy metals in crudes may poison the catalyst present n refinery process. They should be
quantified before the crude enters refinery. Heavy metals are analysed neutron activation
method.

Polonium-210

Polonium i a radioactive isotope analysed by radon or alpha spectrometry method.

Other analysis commonly performed on crude oil/condensate include but, are not limited to

.asphaltenes

.wax content

.density

.pour point

H2S, Mercaptans & COS by absorption and potentiometric method.

Fluid Sampling and Analysis

Sulphur specification analysis and treatment of sampling equipment for

reduced sulphur species
Sulphur compounds form largest group of nonhydrocarbons in crude oil. Sulphur is present in various
forms and concentration in crude oils. Of all sulphur containing compounds found volatile components
such as Sulphides (RSR/RSSR), mercaptans (thiols-RSH) and thiophenes ( lage molecules
containing 30 or more carbon atoms).

Hydrogen Sulphide is most commonly found in crude oil, mercaptans are next most prevalent
species. Sulphur compounds poison the metallic catalyst used in the refining process. Many
processing facilities specifically aimed at removing these sulphur species. Hence it is very important
to know which species are present and at what concentration. Also there are legal and contractual
limits on the amount of sulphur contained in most products.

Since sulphur species have affinity for surface of steel sampling vessels sampling for pressurised oil
and gases for subsequent determination of these sulphur species can be problematic. A untreated
sample cylinder can adsorb sulphur species (in particular H2S) from the sample during transit and
storage. When these samples are analysed in the laboratory erroneously low values from the volatile
sulphur compounds may be obtained.

For this reason coated sampling cylinders must be used for determination volatile sulphur species or
conditioned prior to sampling. Conditioning can be done by repeated use of the cylinder to sample to
particular well. By repeated using same cylinder, it will neutralise the active site inside cylinder body,
so that it will no longer will adsorbs. However this takes and until equilibrium has been reached, data
obtained from this cylinder will erroneously low.

A faster conditioning can be carried out which involves pacifying metal surfaces of sampling
equipment under carefully controlled laboratory conditions. The process takes several days and
brings active surfaces to the point of neutrality where they no longer adsorb reduced sulphur species
from the sample. This method has advantage over conditioning through repeated sampling.

Which type of cylinder can be used?

The conditioning technique is ideal for stainless steel surface, other material such has titanium, and
aluminium can be treated successfully.

What needs to be treated?

Ideally anything which comes into contact with sample needs to be treated: cylinders, valves,cylinder
heads, pistons, agitation balls, in case downhole sampling tool need to be treated. Equipments can
only be treated if it’s dry & clean

How long conditioning treatment last?

The surface treatment is certified for 60 days provided equipment is stored in order restore the
integrity. Exposure to atmospheric oxygen or moisture can reduce the time over which treatment
remains effective. Dismantled tool must be assembled as soon as practical to protect the coating, but
touching and handling of treated surface should be avoided as far as possible.
Fluid Sampling and Analysis

Sulphur specification analysis and treatment of sampling equipment for

reduced sulphur species
What type of samples can be analysed?

Any hydrocarbon liquids, hydrocarbon gases, aqueous liquid and plant samples. By the nature of
multiphase hydrocarbons, these are typically pressurised samples. Theses samples are degassed
down to room temperature and atmospheric pressure and analysis is carried out oil and gas fraction
separately.

How Sulphur species are determined?

All Sulphur species are determined by gas chromatography with sulphur chemiluminesence detection
(GC-SCD). Gaseous samples & clean condensate samples are injected directly. Sometimes gas
samples are diluted with Helium for accurate measurement of peak area. Black oil & aqueous
samples are introduced using headspace analyser. For sulphur species which are gaseous at room
temperature calibration is carried out certified gas calibration standards. For liquid sulphur species at
room temperature calibration is carried out using standards prepared from pure components.

What sulphur species included in the analysis?

Any of following species can be determined individually or as a suite

Sulphides Mercapatans (Thiols) Thiophenes

Hydrogen Sulphide Methane thiol 1-Methyl-1-Proanethiol

Carbonly Sulphide Ethane thiol 2-Methylthiophene

Dimethyl Sulphide Propane 2-thiol 3-Methylthiophene

Carbon Disulphide Propanethiol Tetrahydothiophene

Ethylmethyl Sulphide Butanethiol 2-Ethylthiophene

Diethyl Sulphide Pentanethiol 2-Propylthiophene

t-Butylmethyl Sulphide Hexanethiol 2-Butylthiophene

Dimethyl Disulphide Heptaethiol 3-Butylthiophene

t-Butylethyl Suphide Octanethiol 1-Benzothiophene

Di-Propyl Sulphide Nonanethiol

Diethyl Disulphide 2-Methyl- 2-Propanethiol

2-Methyl-1-Propanethiol

3-Methyl-1-Butanethiol

2-Methly-1-Butanethiol
Fluid sampling
Water Testing & Analysis:

Main objective of testing formation water and its associated gases is to establish chemical and
physical properties

The first challenge is to obtain representative formation water samples. During drilling and completion
operations zone close to the wellbore is occupied by drilling mud and brine. Therefore first produced
water is mixture of mud/brine and formation water. The challenge is to determine when representative
formation water is o be produced?

Secondly, samples should be analysed as soon as possible because properties sample changes with
time. Changes occur in temperature, pressure, gases evolve, ph changes and precipitations takes
place. These processes have effect important ion as well as some physical properties.

Thirdly sample should be analysed the experience and qualified engineers using accepted standard
methods and reliable instrumentation. Quality control and quality assurance throughout all stages of
test is required.

Producing Formation Wireline Sampling:

Reservoir fluids can be collected without producing well to surface, by the use of wireline formation
samplers (WFS) such has RDT (reservoir description tool) & MDT (modular dynamic tester)

The only limited chemical information may be obtained from these samples due to high level of
contamination (20 to 40%) from mud filtrate or brine from wellbore area.

Also precipitation takes place when mud filtrate mixes with formation water, this cannot be quantified
or corrected. Very often presence of tracer it is possible to correct the mud contamination in the
sample and adjust the analytical results. A full production test required to obtain good characterization
formation water.

Production well Test:

Artificial lift s required due to very high specific gravity of the formation water. Commonly three
techniques are used

Gas Lift

Jet pump

Electrical Pump

Gas lift

Injection gas into production tubing reduces the hydrostatic pressure of the fluid column and thus
eases the flow.

The injection of N2 or natural gas has serious drawbacks. The injection gas has tendency to strip
CO2 and other gas molecules from the water. This will result in change in pH, due to shift in
CO2/HCO2 equilibrium. Downhole samples are used normally used in combination with gas lift to
obtain the water samples which are not affected by injection gas
Fluid sampling
Water Testing & Analysis:

Jet Pump

Jet pump technique is similar gas lift except injection gas is replaced by driving water. The driving
water is pumped down the annulus and into the production tubing through nozzles which will create
upward venturi effect.

The disadvantage of jet pump is that it mixes injection water with formation water. Normally drillwater
used for jet. The produced water at the surface is mixture of driving water and formation water. The
technique must be completed with downhole sampling to obtain sample of formation water. Special
care should be taken to prevent scaling in the pump.

Electrical Pump

The subsurface electrical pump is preferred method with respect to water chemistry. No fluids are
introduced and clean well can be accurately monitored at the surface. This method is robust and well
proven.

Downhole Sampling

The single phase downhole sampling is strongly recommended regardless of which method is used
for produce the well. Single phase sampling ensures that sample is collected, transferred and stored
under pressure. Dissolved gases and other ions that may participate out are kept in solution. Also it
should be noted that once gas comes out from the formation water, it will very difficult to push back.

PVT analysis of the single phase will generate accurate water/gas ratios, formation volume factor and
compositional analysis of evolved gases.

Well Monitoring

During well test or DST (drill stem test) large changes in the properties and behaviour of the produced
fluid are observed. After a period of clean up-production relatively constant level of fluid properties
can signals that clean, representative formation water is produced to surface. There after sampling
program is initiated.

Three different techniques are used alone or in combination to monitor well flow composition in order
to determine when well clean, uncontaminated formation water is produced. These techniques are:

1) Traditional wellsite analysis

2) Ion tracking using Multi Ion Analyzer
3) Tracer techniques

Traditional wellsite analysis

Traditional wellsite analysis include following

1) Chloride 2) Barium/Strontium 3) Sulphate

4) pH 5) Alkalinity 6) Density

7) Conductivity/ resistivity

These determinations are quick to perform and give approximation of water characteristics
Fluid sampling
Water Testing & Analysis:

Ion tracking using the Multi Ion Analyzer

Multi ion analyzer is based on the principle of ion chromatography and it represents breakthrough
water analysis technology. Multi ion analyzer can determine all major ions in the formation water
except bicarbonate and organic acids which are determined separately by titrations. In one sample
injection following ions is determined.

Lithium, Li+ Strontium Sr2+

Sodium, Na+ Barium Ba2+
Potassium, K+ Chloride, Cl-
Calcium, Ca2+ Bromide, Br-
Magnesium, Mg2+ Sulphate SO42-

In addition pH and conductivity is also determined.

Tracer Application

The use of tracer is important tool to verify when the produced water is representative. The tracer will
act has label in the mud which makes it easy to identify. Tracer techniques are used in combination
with multi ion analyzer and it is strongly recommended when sampling is performed with WFS tool.

A number of different tracers are available which include both radioactive and chemical, a common
radioactive is tritiated water, among chemicals tracers are Thyocyante are used brines and water
based mud.
When drilling through water fixed concentration tracer is used and it is monitored, has decreased in
tracer content when formation water is produced.
Prior to offshore water tests it is important that samples are collected of any brine and mud are
involved in the operations. In particular fluids which might come in contact with formation water should
be sampled and analyzed.

Use of Tracer

Action 1
The tracer chemical is added to mud process under controlled conditions to maintain the required
concentrations. The concentration must be measured frequently when drilling through actual zone of
interest.

Action 2
The Multi Ion Analyzer is used to measure the ion concentration of mud filtrate from the pit.

Action 3
The WFS chamber is run in hole and the sampling process is initiated. When WFS tool is returned to
the surface one chamber is opened and sampled. The sample is analysed for tracer, cation, anions,
pH, conductivity, and bicarbonate. From detailed analysis quantitative interpretation of the water
phase and mass balance calculation is performed.

Each of three techniques, traditional wellsite analysis, Multi Ion Analyzer and tracer application can be
used individually. However by performing two or three techniques in parallel, consistency of the
results will provide added confidence as quality of the data.
Fluid sampling
Water Testing & Analysis:

Multivariate Data Analysis (MVDA)

Decision based on variation of concentration only one variable has resulted in erroneous conclusions
when representative formation water is produced.
By considering greater number of variables, i.e. by analysing samples for a greater number of cations
and anions with Multi ion analyzer it is possible to arrive at more reliable decisions. A MVDA computer
program is used to interpret the analytical data to identify the trend.

Sampling and Analysis

When it is decided that well is producing pure formation water, sampling program is initiated, it
consists 3 set of sample and one backup sample. One set consists of
.Raw untreated water (no preservation) .Raw water preserved with nitric acid
. Filtered produced water (no preservation) .Filtered water with acid preservation
.The above filters for solid characterization
. Raw untreated water to be frozen immediately for preservation
.raw water preserved with mercury chloride
Vaps can offer wide range chemical and physical water analysis, listed below most common analysis

In Organic Analysis:
Basic ion composition* Tracer Analysis*
27 element analysis Heavy metal analysis Isotope ratio 87Sr/86Sr
Radioactive isotope analysis Dissolved Iron* Sulphide content*
Dissolved oxygen* Dissolved carbon dioxide*
Organic components Organic Acids Total organic carbon
Aromatics Oil in water*

Physical Properties:
pH* Alkalinity* Density*
Conductivity/resistivity* Temperature*
Turbidity* Suspended solids
Particle count* Particle Size distribution* Particle analysis (SEM/EDX,XRF)
Bacteria (SRB, GAB) Compatibility Test

PVT Analysis:
Gas/water ratio Saturation pressure Formation volume factor
Composition of associated gases pH in water in equilibrium with associated gases
*analysis performed onsite

Scale Prediction

The chemical and reservoir data gathered during water test can serve has useful input for the
computer program for Multiscale. This multiphase PC based program can simulate where there is
mixture of different water types, changes in pressure or changes in temperature and will ultimately
predict the corresponding scale formation characteristics.

The following type of scale are predicted:

Calcite (CaCO3) Siderite (FeCO3) Gypsum (CaCO3+2H20)
Strontium Sulphate (SrSO4) Barium Sulphate (BaSO4)
Halite (NaCl) Marcasite (FeS2)
 Vision Advanced Petroleum Solutions LLC

REMOTE LAB: CHARGING A SAMPLE TO REMOTE LAB SYSTEM

This Work Instruction is a mandatory requirement, and forms part of the Approved Integrated
Management System. Alterations are not permitted without the prior approval of the Fluids Laboratory
Manager or the relevant department senior supervisor.

1. PURPOSE
This is the procedure should be adopted when charging the Remote Lab PVT system with a
pressurised fluid sample.
2. AUTHORITY
This work instruction is written and maintained with the authority of the Fluids Laboratory
Manager or the relevant document owner.
3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this
work instruction.
4. PROCEDURE
4.1. Outline
Before charging, ensure the sample has been restored to reservoir/sampling
temperature and pressure for a minimum of twelve hours.
Connect the water/glycol side of a sample bottle to the ISCO transfer pump and agitate
the sample.
Connect the sample side (above the piston) to the Remote Lab system.
At all times during the transfer the pressurised fluid must be maintained in single-phase
conditions, using the constant pressure facility on the ISCO transfer pump. The volume
of the sample injected is calculated from displacement volume of the ISCO transfer
pump recorded before and after charging.
4.2. Safety Precautions for Handling Liquids and Gases under Pressure
- Eye protection and protective clothing be worn.
- Ensure pipe work is in good condition and that end connectors are compatible.
- Ensure the maximum working pressures of the sample cylinder and pipe work are
not exceeded.
4.3. Quality Assurance
Ensure all equipment is in calibration before commencement of work. Record next
calibration date on the worksheet.
4.4. Apparatus

VAPS-PVT-WI-004/Rev.00/03 May 2015 / Page 1 of 3

Any hard of copy this document will be considered as UNCONTROLLED COPY unless otherwise mentioned on it.
Approved copy of document is available with Management Representative only.
 Vision Advanced Petroleum Solutions LLC

REMOTE LAB: CHARGING A SAMPLE TO REMOTE LAB SYSTEM

Top Valve
Pump Top Valve Remote Lab PVT Cell

Pressure Oil Sample Oil Sample

Gauge

Water/Glycol Pump A Pump B

Pump B: Stop

Pump A: Constant Pressure

Transfer Pump

4.5. Method
1. Restore the required fluid to the required conditions for a minimum of 12 hours.
2. The Remote Lab system can either be charged at ambient temperature, (this makes
access to the system easier, and means any leaks can be spotted easily) or at
reservoir / specified temperature if it needs to be done quickly.
3. The sample bottle is mounted vertically adjacent to the ISCO transfer pump and a
line is connected at the bottom valve of the bottle. The bottom valve is opened and
the cylinder stabilised at charging pressure by extensive agitation. Ensure the ISCO
transfer pump is running in constant pressure.
4. A line is connected from the top of the bottle to the top of the system and flushed
by cracking the line, or evacuated using a three way valve and then filled with the
sample, (when the valve is opened the ISCO transfer pump should hold the pressure
at a constant pre-specified value.) The temperature and volume on the ISCO
transfer pump should now be recorded.
5. The top valve of the Remote Lab system is now opened. A small pressure change
should be observed, and the transfer pump should ‘flow in’ as the sample fills the
dead space. The resulting volume on the ISCO transfer pump should be recorded in
order to calculate the dead space. The pressure displayed on the calibrated druck
gauge should now be recorded as your charge pressure.
6. The Remote Lab system ISCO pumps should now be set to refill at 5 ml/minute. As
the Remote Lab system refills, a pressure change and flowrate should be observed
on the ISCO transfer pump. (If this is not the case and the pressure in the Remote
Lab system drops, stop the Remote Lab system pumps immediately). The refill rate
of the Remote Lab system pumps can be increased gradually to approximately
15mls / minute until the required volume of sample has been charged. At all times
the pressure should be monitored to ensure it does not drop below reservoir /
sampling pressure (i.e. the sample should be kept single phase).
7. The Remote Lab PVT system pumps should now be stopped, and once the transfer
pump stops flowing the pressure and volume recorded, the Remote Lab system
valve and the top valve of the sample container should now be closed.
The volume of the sample transferred to the Remote Lab system will depend on the
test to be conducted and also the volume of the sample available and the GOR
expected.

VAPS-PVT-WI-004/Rev.00/03 May 2015 / Page 2 of 3

Any hard of copy this document will be considered as UNCONTROLLED COPY unless otherwise mentioned on it.
Approved copy of document is available with Management Representative only.
 Vision Advanced Petroleum Solutions LLC

REMOTE LAB: CHARGING A SAMPLE TO REMOTE LAB SYSTEM

Typical volumes are:
(i) Separator/Reservoir flash / pV / Density 80 cc
(ii) Differential Vaporisation 80 cc
(iii) Separator Test 30 cc
(iv) Capillary Viscosity 50 cc
Disconnection
Before disconnecting, a check is made that the top valve of the sample container
and the Remote Lab system valve are both closed. The charging line is carefully
disconnected, and cleaned. On the sample charge sheet the volume of sample
removed is recorded along with, the date and test to be performed. The bottom
valve of the sample (water/glycol side) is closed and the line to the transfer pump is
depressurised by withdrawing the displacement fluid into the transfer pump.
All equipment is thoroughly cleaned and replaced in the racks provided.

VAPS-PVT-WI-004/Rev.00/03 May 2015 / Page 3 of 3

Any hard of copy this document will be considered as UNCONTROLLED COPY unless otherwise mentioned on it.
Approved copy of document is available with Management Representative only.
 Vision Advanced Petroleum Solutions LLC

TRANSFER OF FLUIDS FROM OPEN HOLE SUB-SURFACE SAMPLERS

This work instruction is a mandatory requirement, and forms part of the Approved Integrated Management System.
Alterations are not permitted without the prior approval of the Senior Technical Manager or the relevant
Department Supervisor.

1. PURPOSE
This is the procedure to use when it is necessary to transfer fluids from a sub-surface sampler to a storage
vessel or PVT cell.

2. AUTHORITY
This work instruction is written and maintained with the authority of the Senior Technical Manager or the
relevant document owner.

3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this work
instruction.

4. PROCEDURE
4.1. Outline
The following procedure is for the transfer of pressurised live fluids from down hole chambers to
storage/shipping containers. Typically the down hole chambers encountered will be MDT
(MPSR), RCI and RDT tools.

4.2. Safety Precaution

- Staff should be familiary with all asssociated Risk Assessments and COSHH Risk Assessments
before proceeding.
- Examine sampling sheets for any special hazards and pressure rating of sub-surface
sampler.
- Eye protection and protective clothing to be worn.
- Ensure pipe work is in good condition and that end connectors are compatible, and
threads are in good condition.
- Worn connectors should be handed to the laboratory engineer.
- Ensure suitable screening devices are used where possible.

4.3. Method
Check to see if the fluid under investigation contains H 2S; as to the correct safety measures.
Consult the owner manual or specification prior to using a down hole chamber.
The client should also supply information about the reservoir and sampling processes.
Particularly reservoir pressure and temperature and if the chambers have been taken to excess
pressures by use of a pump or single phase buffers.
On receipt of the down hole chamber remove the blanks and clean the orifices of the valves. It is
not unusual for the valves to be covered with grey/brown drilling mud residue. If this is heated it
can dry out to a concrete like substance which can make opening valves and securing cross over
connectors difficult.
It is normal for the chambers to be heated to reservoir temperatures. However this may be
limited by the chambers specifications, for instances the MPSR chambers can only be heated to
93°C.

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TRANSFER OF FLUIDS FROM OPEN HOLE SUB-SURFACE SAMPLERS

As the fluids are trapped at downhole conditions, returning the temperatures to the reservoir
state should mean that the pressure also return to this point. In this case there is no need to
monitor the pressure during heating. A contact pressure should be taken before heating the
sampler.
The exception to this is if the fluids have been pressured to in excess of reservoir conditions by
the samplers or if a single phase buffer has been introduced subsequent to the sampling process.
In this case the pressure does need to be monitored during heating. Prior to heating a check is
made on the “single phase integrity” by measuring the opening pressure at ambient
temperature.
Once the chamber is at transfer temperature then the opening pressure of the heated sampler is
measured.
Transfer pressure must be either above the reservoir pressure or a saturation event measured
within the chamber. To do otherwise is to risk transfering in two phase and significantly changing
the nature of the fluid.
Contact/opening pressure is measured by attaching a water/glycol transfer pump system to the
bottom of the chamber. With some chambers the internal piston may bottom out which will
require the operator to pump some water/glycol into the chamber and therefore move the
piston off the bottom before measuring the contact pressure.
If the fluid is known to be oil, the chamber can be drained of water contamination prior to
transfer. Invert the chamber and allow to stand for some time. Open the top of the chamber to a
transfer head with a secondary valve with good metering characteristics. Slowly open the
secondary valve and access the nature of the fluid coming out. If it is water continue until all is
removed and oil begins to show. Record the volume of the water drained. If it is thick oil, wait a
further period of time and check again.
Take care that the fluid is not supposed to be a down hole water sample that requires work to be
carried out at pressure. If so the sample should be transferred as described below.
Gas samples should be heated to reservoir temperature and pressured to in excess of the
sampling condition if draining contamination. As water and condensate are both clear liquids it is
difficult to distinguish between them, it is probably better to check for water from the storage
cylinder after transfer.
Once thermal stability at transfer conditions has been achieved the chamber should be
pressured to inexcess to the downhole condition. It is normally sufficient to go to the next but
one thousand psi mark. For example if the reservor pressure is 4700 psia then a reasonable
transfer pressure would be 6000 psia.. The down hole chamber should be throughly agitated to
ensure a homogenous single phase fluid. Bring the chamber into the upright position and
connect to an Expro storage cylinder via a good quality line. Evacuate the line to the top of the
storage cylinder via a three way valve.
The storage cylinder should already be clean, filled with hydraulic fluid below it’s piston and
pressure tested. The dead space on top of it’s piston should be evacuated.
Open the transfer head secondary valve slowly and fill the transfer line while maintaining the
down hole chamber pressure by injecting hydraulic fluid under the piston. Record the transfer
pump reading.
Slowly open the valve on top of the storage cylinder and allow the fluid from the down hole
chamber to fill the dead space. The pressure in the down hole chamber is again maintained at
the transfer condition by inject further hydraulic fluid. At no time during the transfer process
must the pressure be allowed to fall below reservoir/transfer conditions.

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TRANSFER OF FLUIDS FROM OPEN HOLE SUB-SURFACE SAMPLERS

The transfer process is carried out by injecting hydraulic fluid below the piston of the down hole
chamber and pushing the reservoir fluid over into the storage cylinder. The pressure is
maintained at transfer conditions by draining fluid from below the storage cylinder’s piston.
It is normal to transfer all available fluid from the down hole chamber. As it’s piston head hits
the top of the chamber a sudden rise will occur on the pressure gauge of the transfer pump.
When this happens stop the transfer pump and close the drain valve of the storage cylinder.
Record the transfer pump reading.
Record the volume of hydraulic fluid has been drain from beneath the piston of the storage
cylinder. This is volume of fluid available for further test and is therefore of great importance.
Close the valve on top of the storage cylinder. Close the valve on top of the down hole chamber
and the secondary valve of the transfer head. De-pressure the transfer line via the three way
valve and record any observations of gas/oil/water/mud.
De-pressure and empty the down hole chamber. The head space of which will still be full of
reservoir fluid at transfer conditions. This may be enough to push the piston down and remove
all the hydraulic fluid. If the volume of hydraulic fluid does not match the expected volume an air
line can be attached and the piston forced down to eject the remaining hydraulic fluid.
After completing the transfers, the validity of the fluids is determined by measuring the
saturation pressure within the storage/shipping containers.

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SATELLITE LAB: CHARGING A SAMPLE - BLACK OIL SYSTEM

This Work Instruction is a mandatory requirement, and forms part of the Approved Integrated Management System.
Alterations are not permitted without the prior approval of the Senior Technical Manager or the relevant
Department Supervisor.

1. PURPOSE
This is the procedure should be adopted when charging the Satellite Lab PVT black oil system (SLS) with a
pressurised fluid sample.
2. AUTHORITY
This work instruction is written and maintained with the authority of the Senior Technical Manager or the
relevant document owner.
3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this work
instruction.
4. PROCEDURE
4.1. Outline
Before charging, ensure the sample has been restored to reservoir/sampling
temperature and pressure for a minimum of twelve hours.
Connect the water/glycol side of a sample bottle to the ISCO transfer pump and agitate the
sample.
Connect the sample side (above the piston) to the Satellite Lab system.
At all times during the transfer the pressurised fluid must be maintained in single-phase
conditions, using the constant pressure facility on the ISCO transfer pump. The volume of the
sample injected is calculated from displacement volume of the ISCO transfer pump recorded
before and after charging.
4.2. Safety Precautions for Handling Liquids and Gases under Pressure
- Staff should be familiar with all associated Risk Assessments and COSHH Risk Assessments
before proceeding.
- Eye protection and protective clothing be worn. Personal Protective Equipment
- Ensure pipe work is in good condition and that end connectors are compatible.
- Ensure the maximum working pressures of the sample cylinder and pipe work are
not exceeded.
4.3. Quality Assurance
Ensure all equipment is in calibration before commencement of work. Record next calibration
date on the worksheet.

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SATELLITE LAB: CHARGING A SAMPLE - BLACK OIL SYSTEM

4.4.
Apparatus

4.5. Method
Check to see if the fluid under investigation contains H 2S; if so consult as to the correct safety
measures.
1. Restore the required fluid to the required conditions for a minimum of 12 hours.
2. The Satellite Lab Black Oil system (SLS) can either be charged at ambient temperature, (this
makes access to the system easier, and means any leaks can be spotted easily) or at
reservoir / specified temperature if it needs to be done quickly. The charging pressure
should be well in excess of the sampling conditions or if known the saturation pressure
(1000 psi+). The essential point is to always maintain the fluid in single phase during sample
transfer. The Satellite lab black oil system should be clean and evacuated. The line inside the
oven linking the top valve of the RLS to the valve on the side of external oven wall should
also have been cleaned and evacuated. The valves at top of the SLS and the side valve
should be closed after evacuation.
3. The sample bottle is mounted vertically adjacent to the transfer pump. A line connects the
transfer pump to the bottom valve of the sample bottle. Water is purged through this line to
eliminate air contamination. The bottom valve of the sample is opened and the cylinder
stabilised at charging pressure by extensive agitation. Ensure the transfer pump is running in
constant pressure mode set at the charging pressure. Ensure that there is sufficient volume
in the transfer pump to complete the transfer of the required/desired volume of sample into
the SLS.
4. The top of the sample bottle is connected to the SLS through a pressurised line. This will
generally be to the valve on the side of the external wall of the oven. The air contamination
of this line should be removed through evacuation or by purging with live fluid. Filling this
line should be done with care and the pressure in the sample cylinder should be kept close
to charging pressure. Once this line is filled, the side valve should be carefully opened and
the line linking to the top of the SLS filled. Again this should be done carefully to maintain
the pressure in the sample cylinder. Allow the pressure in the sample cylinder and charging

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SATELLITE LAB: CHARGING A SAMPLE - BLACK OIL SYSTEM

lines to stabilise and the transfer pump flow rate reads 0.0000. Once stable, the
temperature and volume of the transfer pump should be recorded.
5. The top valve of the Satellite Lab Black Oil system (SLS) is now opened. A small pressure
change should be observed, and the transfer pump should ‘flow in’ as the sample fills the
dead space. Once stable, the resulting volume on the transfer pump should be recorded in
order to calculate the dead space. The pressure displayed on the calibrated druck gauge
should now be recorded as your charge pressure.
6. The SLS pump A should now be set to refill at 5 ml/minute. As the SLS refills, a pressure
change and flow rate should be observed on the transfer pump If this is not the case and the
pressure in the SLS drops, stop the SLS pumps immediately. This would indicate that fluid is
not being removed from the sample cylinder, possibly due to insufficient available sample. If
unchecked, the SLS refills and reduces the pressure in the SLS, charging lines and sample
cylinder dead space below the transfer pressure. This may cause the fluid to pass into two
phase. If the pumps are synchronised, the refill rate of the SLS pumps can be increased
gradually to approximately 15mls / minute until the required volume of sample has been
charged. At all times the pressure should be monitored to ensure it does not drop below
reservoir / sampling pressure (i.e. the sample should be kept single phase).
An alternative method would be to set the SLS pump A on refill at 5 ml/minute. Once a small
volume has been passed into the SLS, then stop A. Set pump A to work in constant pressure
mode at a setting lower than the transfer pump, but obviously above the
saturation/reservoir pressure. Continue until the required volume has been injected and
then stop. This then prevents the possibility of going into two phase if you run out of
sample. Increase the pressure differential between the transfer pump and the SLS (keeping
both above the saturation/reservoir pressure) until you get a flow rate of around 15ml/min.
7. The SLS system pumps should now be stopped, and once the transfer pump stops flowing
the pressure and volume recorded, the SLS valve and the top valve of the sample container
should now be closed.
8. If no work is to be immediately started then the SLS should be put into constant pressure
mode, this is especially important if the cell has been charged cold and is to be heated to
experimental temperature due to thermal expansion of the sample.
The volume of the sample transferred to the SLS will depend on the test to be conducted
and also the volume of the sample available and the GOR expected.

Typical volumes are:

(i) Separator/Reservoir flash / pV / Density 80 cc
(ii) Differential Vaporisation 80 cc
(iii) Separator Test 30 cc
(iv) Capillary Viscosity 50 cc
Disconnection
Before disconnecting, a check is made that the top valve of the sample container and the
SLS valves are both closed. The charging line is carefully disconnected, and cleaned. On the
sample charge sheet the volume of sample removed is recorded along with, the date and
test to be performed. The bottom valve of the sample (water/glycol side) is closed and the
line to the transfer pump is depressurised by withdrawing the displacement fluid into the
transfer pump.
All equipment is thoroughly cleaned and replaced in the racks provided.

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SATELLITE LAB: MEASUREMENT OF SATURATION PRESSURE IN CONTAINER

This Work Instruction is a mandatory requirement, and forms part of the Approved Integrated Management System.
Alterations are not permitted without the prior approval of the Senior Technical Manager or the relevant
Department Supervisor.

1. PURPOSE
This is the procedure to use when it is necessary to determine the saturation pressure of a fluid contained
in its storage/transportation vessel. This procedure is used as part of the sample validation process.

2. AUTHORITY
This work instruction is written and maintained with the authority of the Senior Technical Manager or the
relevant document owner.
3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this work
instruction.
4. PROCEDURE
4.1. Safety Precaution
- Staff should be familiar with all associated Risk Assessments and COSHH Risk Assessments
before proceeding.
- Examine sampling sheets for any special hazards and pressure rating of bottle.
- Eye protection and protective clothing to be worn. WI/0025 Personal Protective Equipment.
- Ensure pipe work is in good condition and that end connectors are compatible, and
threads are in good condition.
- Ensure operator is familiar with the workings of the particular sample cylinder as
these can vary between supplier.
- Worn connectors should not be used.
4.2 Method
Check to see if the fluid under investigation contains H 2S; if so consult WI/0015 as to the
correct safety measures.
1. Place cylinder in rocker stand and attach water/glycol side to FTU (or ISCO transfer pump),
obtain opening pressure.
2. Ensure that fluid is above sampling pressure and agitate cylinder until the pressure is stable.
3. Once stable note down pressure and remove a known volume of water/glycol from below
the piston. This is done using the ‘refill’ function of the ISCO transfer pump, or the constant
volume unit on the FTU.
4. Agitate once more until stable pressure has been obtained and note pressure.
5. Repeat stage 3 until pV is complete. A minimum of 5 points in the single phase and 5 in the
two-phase region are required.
6. Once plotted the saturation point should become clear from an inflection in the plot.

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SATELLITE LAB: MEASUREMENT OF SATURATION PRESSURE IN CONTAINER

4.3. Apparatus

Sample Bottle

Pressure
Gauge

Fluid transfer unit /

ISCO transfer Pump

Valve

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CRYOGENIC DISTILLATION OF LEAN GASES

This work instruction is a mandatory requirement, and forms part of the Approved Integrated Management System.
Alterations are not permitted without the prior approval of the Fluids Laboratory Manager or the relevant
department senior supervisor.

1. PURPOSE
This is the procedure to use when a detailed description of the heavy components in a lean gas is
required by the customer.
2. AUTHORITY
This work instruction is written and maintained with the authority of the Fluids Laboratory Manager or
the relevant document owner.
3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this work
instruction.
4. PROCEDURE
4.1. Outline
To determine accurate concentrations of heavy components in lean hydrocarbon gases the
heavy components have to be first separated by distillation.
A hydrocarbon gas is condensed in a glass receiver using liquid nitrogen as a cooling agent. The
glass receiver is allowed to warm up and as the gas distils the pressure is regulated using an
automatic valve. The products from the distillation are re-frozen in a pressure vessel; again
using liquid nitrogen as a cooling agent. The quantity of liquid and gas are determined by mass.

4.2. Apparatus
AUTOMATIC CRYOGENIC DISTILLATION
Fill
Valve

Digital
Pressure Soleniod
Indicator Valve

Flow
Restrictor
Glass
Receiver Evacuation
Point
Pressure
Vessel

Dewar
Liquid
Nitrogen

Dewar
Liquid
Nitrogen

Figure 1

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CRYOGENIC DISTILLATION OF LEAN GASES

Figure 2

4.3. Safety Precautions

- Eye protection and protective clothing must be worn.
- Ensure pipe work is in good condition and the appropriate fittings used.
- Wear the appropriate gloves when handling liquid nitrogen.
- Ensure suitable screening devices are used wherever possible.
4.4. Quality Assurance
Ensure all equipment is in calibration before commencement of work. Record next calibration
date on worksheet.

4.5. Preparation
Prior to sampling the gas into the automatic cryogenic distillation, the gas cylinder is heat soaked
at an appropriately high temperature, above either separator or reservoir temperature. Ensure
all pipe work and glassware is clean and if necessary rinse with solvents and dry. Evacuate the
pressure vessel and weigh this and the glass receiver individually on a calibrated balance. Ensure
that the blank for the pressure vessel and the cap for the glass receiver are included in the
respective masses. Connect all the components of the system as given in Figure 1.
Close fill valve and ensuring the solenoid valve is enabled (Figure 2), set the solenoid valve to
“hold open”. Evacuate the system via the evacuation point. The pressure gauge will indicate
when a full vacuum has been achieved. Close the evacuation point and observe any pressure
change. If pressure increases this indicates the system is not holding a vacuum so check all
fittings for leaks and re-evacuate. Connect the inlet port of the fill valve to the sample vessel
using high pressure line.
4.6. System Settings for Operation
There are no definitive settings for this system as each fluid will behave in a slightly different
way. But the following are the recommended settings and if necessary can be adjusted to suit
individual fluids.
4.6.1. Pressure Transducer
To set/observe the settings push the ‘S’ button and the ‘Arrow Up’ button at the same
time. Press the ‘S’ button to scroll though the menu. The pressure transducer is set to
indicate mbar (1 atmosphere is approx. 1000 mbar).

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CRYOGENIC DISTILLATION OF LEAN GASES

Option Description Setting
General controller settings
Pas This is a password and locks the settings so that
they can not be changed (do not change the default) 0
dp Moves the decimal point 1111. mbar
Hie Proportional band for scale 6.00
LoE Scaling factor for scale 1.00
Hi Highest pressure value before gauge goes into error
Mode 1723 mbar
Lo Lowest pressure value before gauge goes into error
Mode 0 mbar

Settings for one gauge

SP1 The opening pressure of the solenoid valve 760 mbar
Hys The difference below SP1 before the solenoid valve
Closes 50 mbar
del Time delay on reaching SP1 before solenoid valve
closes 0 seconds
up or do Whether the solenoid valve opens with
increase/decrease pressure up
nd or ne Unknown what this option gives nd
on or off Whether the above settings for one gauge are activated on
Settings for two gauge
These are the same as above for one gauge but are disable (OFF) as this system only uses one gauge.

4.6.2. Temperature
The temperature controller is for operation with heat tracing on the system manifold.
This requirement is outside normal operation and should be set to the off position.
4.6.3. Alarm System
The two temperature probes are connected to the alarm system and are design to give
an indication of low levels of liquid nitrogen in the dewar flasks. If the system goes into
alarm, a buzzer sounds and the solenoid automatically closes. The closing of the
solenoid valve is not necessarily a safe situation and it is recommended that the alarm
system is disabled. Even in the disabled mode, a red alarm light is activated when
nitrogen levels are becoming low.
4.7. System Operation
Prior to filling with gas, the pressure transducer is set to disabled and the solenoid valve
activated by switching to the run position. The glass receiver is immersed in liquid nitrogen by
raising the lab jack. Regulate the gas flow to the glass receiver by turning the fill valve until the
pressure indicator is showing 600 to 700 mbar. As the glass receiver fills the pressure will
increase. If the pressure reaches approximately 800 mbar, raise the nitrogen level or adjust the
fill valve as this should then reduce the pressure.
Once a suitable volume of fluid has been charged (this will vary greatly depending on the sample
being analysed), close the fill valve, immerse the pressure vessel in liquid nitrogen and open the
pressure vessel valve. When the pressure vessel has reached liquid nitrogen temperature; this
could take a couple of minutes; switch the pressure transducer to enable mode. As the gas
distils, the solenoid valve will open at the set pressure and close again at the ‘Hys’ value. A good
rate is when the solenoid valve opens and closes every 3 or 4 seconds, but this is not critical. To
adjust the distillation rate the liquid nitrogen level can be adjusted so that more or less of the
glass receiver is exposed to the atmosphere.
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Eventually, it will be necessary to completely expose the glass receiver to the atmosphere.
Warm the glass receiver to just above room temperature. When the pressure is stable, i.e. the
solenoid valve does not open for a long period of time, lower the SP1 value in stages until the
pressure will not reduce any further. Switch the solenoid valve to ‘hold open’ mode and leave
until the fluid is no longer de-gasing (approx 20 – 30 minutes).
If the volume of condensate liquid, is low, it may be necessary to do addition fills of the glass
receiver and pressure vessel in order to collect reasonable volumes for compositional analysis. If
in doubt, ask a supervisor. If an addition fill is required, reimmerse the glass receiver in liquid
nitrogen by raising the lab jack. Switch the pressure transducer to disable mode and shut the
pressure vessel. Repeat the fill, remembering to reset the pressure SP1 value. Once a suitable
volume of fluid has been charge, repeat the warming up process until the fluid is no longer de-
gassing.
Record the pressure. Close the pressure vessel valve and fill the system with air via the
evacuation valve and again record pressure. Remove glass receiver, cap, clean to remove any
water and re-weigh. Disconnect the pressure vessel, replace blank and store in a safe place to
allow the vessel to warm to room temperature. Clean pressure vessel to remove any water and
re-weigh.
Heat soak the pressure vessel for a minimum of 12 hrs before sampling the gas to ensure the gas
is homogeneous.

Fill in all of the cryogenic distillation worksheet (AD/2108) including the calculation for estimated
density. If several samples are being worked on that are from the same conditions, the
estimated density should be approximately constant. If this is not the case, discuss the result
with a supervisor.

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DETERMINATION OF C2-C36+ HYDROCARBONS IN PETROLEUM LIQUIDS IN

REMOTE LABORATORIES

This Work Instruction is a mandatory requirement, and forms part of the Approved Integrated
Management System. Alterations are not permitted without the prior approval of the relevant
department senior supervisor.
1. PURPOSE
This procedure outlines the determination of C2 to C36+ hydrocarbons in transparent and opaque
petroleum liquids in the range 0.001 – 50 weight %. The following isomers are individually
identified: iso butane, neo pentane, iso pentane, benzene, toluene, ethylbenzene, m+p xylene
and o xylene. Pristane is included in the C17 group and phytane in included in the C18 group.

2. AUTHORITY
This work instruction is written and maintained with the authority of the relevant document
owner.

3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this
work instruction.

4. PROCEDURE
4.1. Outline
Samples are introduced into a gas chromatograph, equipped with a capillary column
coated with a non polar stationary phase, using an auto injector. Following vaporisation
hydrogen carrier gas carries the sample through the column where it is separated into
individual components which are detected by a flame ionisation detector. The
concentration of the components is determined in mass % either by normalising the
peak areas for transparent petroleum liquids which are fully recovered or by the
gravimetric addition of an internal standard for opaque liquids. For opaque liquids the
amount of unrecovered material is also calculated. A solvent blank is subtracted from
the sample and standard chromatograms prior to integration of peak areas in order to
remove baseline drift due to column bleed. Peak areas of the identified aromatic
components are corrected for detector response factors before calculating the
composition.

4.2. Apparatus
- Gas chromatograph equipped with split/splitless inlet, flame ionisation detector.
The oven should be capable of producing repeatable oven ramps of 0-350°C.
- Column, a fused silica capillary column 25m long by 0.20mm id with a 0.33µm
coating of a non polar stationary phase.
- Data Acquisition System, a computer based chromatography data system capable
of accurately and repeatedly measuring the retention time and areas of eluting
peaks. The system should be able to acquire data at a rate of 10 Hz or better.
- Auto injector, suitable for use with the GC.
- Glass Syringes, 10µl, 50µl, 500µl and 1000µl

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REMOTE LABORATORIES
- 2ml Disposable plastic syringes and needles.

4.3. Reagents and Materials

- Gases – All gases should pass through the appropriate gas filters before they
enter the gas chromatograph.
- Hydrogen minimum 99.98% purity
- Synthetic or blended air
- Dichloromethane, minimum 99% Purity
- Discrimination Blends quantitative blends of n alkanes in the range C6 – C12 and
C8 – C44. See WI 2410 Preparation of verification standards for liquid
hydrocarbon analysis In Remote Laboratories for details
- Reference Gas Oil – ASTM D2887 Reference Gas Oil
- Reference Crude Standard – Bulk supply of crude oil sample with defined limits
and water content less than 0.5%.
- n-Hexene minimum 99.8% purity, the purity should be checked and measured by
GC before use.

4.4. Safety Precautions

- Eye protection and protective clothing must be worn as detailed in WI 1612
Personal Protective Equipment (PPE).
- Ensure pipe work is in good condition and the appropriate fittings used.
- All dilutions should be prepared in the fume cupboard.
- Needles must be disposed of in sharps container.

4.5. Quality Control

Discrimination blends consisting of n-alkanes covering the range C6 – C44 must be run
before each batch of samples. These blends are used to check the split linearity,
recoveries should be within 95-105% recovery. If recoveries fall outside these limits
without explanation (as interpreted by the relevant supervisor/senior supervisor) then
one or more of the following steps may be taken:
• A repeat run of the discrimination blend is performed.
• The liner is checked for movement of the glass wool plug and adjusted as
necessary.
• The liner is replaced.
• The injector assembly is thoroughly cleaned and parts changed as necessary.
• The detector is cleaned and the jet replaced as necessary.
• A replacement column is installed.
Reference gas oil or crude oil standards are run before and after samples to check that
the instrument is performing consistently throughout the run. A quality index (QI)
system is employed as a measure of the quality of the results of standards. The index is
calculated as follows:

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DETERMINATION OF C2-C36+ HYDROCARBONS IN PETROLEUM LIQUIDS IN

REMOTE LABORATORIES
The analysis is assigned an initial index of 100. The concentration of each component is
compared to the relevant control limits for that standard. If an individual result falls
within the upper and lower warning limits then a marker value of zero is given to that
component. It the result falls within the upper and lower warning limits and the upper
and lower action limits the component is assigned a marker value of 1. If the result is
outside of the action limits then the component is assigned a marker value of 3 (10 for
C36+). The sum of the individual marker values is subtracted from 100 and the result is
the QI for that standard. A QI of ≥ 90 is indicative of a satisfactory result.
If QC control standards are outside the specified range the samples run between those
standards will be repeated where circumstances allow.

4.6. Sample Handling

1. Samples should be labelled with a minimum of the request number, job number and
cylinder number.
2. Condensates from cryogenic-distillations contain significant amounts of light
components and must not be allowed to warm up must be stabilised with cold
solvent and transferred to a cold vial immediately. The amount of solvent added
depends upon the amount of condensate recovered see chart below.
NB. DO NOT use plastic syringes or pipettes with condensates or DCM.
<100 mg sampleDilute to 2ml with DCM
100-400 mg sample Dilute to 4ml with DCM
>400 mg sampleDilute to minimum 7ml with DCM depending on amount
recovered.
A supply of vials and solvent should be kept in the refrigerator in readiness for these
dilutions.
3. Store all other samples in refrigerator until required.
4. Allow samples to reach ambient temperature before preparing dilutions.
5. Check samples to ensure they are fully mobile before proceeding with preparation
warm samples if necessary.
6. Viscous or waxy samples should be warmed until fluid.
7. All solvent additions should be carried out in a fume hood.

4.7. Sample Preparation

4.7.1. Balance Calibration Check
The calibration of the balance should be checked each day before it is used.
Check the weights of the 0.05g, 2.0g, 10g and 100g calibration check weights
and record the results in the balance log book. If the measured weights differ
from actual weights by more than ± 0.0005g for 0.05g and 2.0g or ±0.001g for
10g and 100g then perform an internal calibration following manufacturer’s
instructions and record in the log book.

4.7.2. n-Hexene Purity Check

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DETERMINATION OF C2-C36+ HYDROCARBONS IN PETROLEUM LIQUIDS IN

REMOTE LABORATORIES
The purity of each bottle of n-hexene should be checked before using as a
standard. The hexene should be assigned a request number prior to analysis.
Take 20µl of n-hexene and dilute to 2ml with DCM, and run on GC. The area%
of the n-hexene peak is used as the purity of the standard. Note the purity on
the bottle with the date of analysis and request number.
4.7.3. Black Oil (Opaque) Samples
1. All samples should be run at least in duplicate.
2. The vial must be labelled with the request number and cycle number.
3. Weigh a 2ml screw cap vial, record weight.
4. Measure approximately 1ml of sample using a disposable syringe; add to
vial avoiding getting any sample around the neck of the vial. Replace lid and
reweigh vial recording weight on worksheet.
5. Measure 40µl n-hexene using a glass syringe, add to sample through
septum. DO NOT invert. Reweigh the vial and record weight on the
worksheet.
6. Remove the cap and quickly add DCM up to the neck of the vial, replace
cap and mix well.
NB. DO NOT use plastic syringes or pipettes with DCM.
7. Store dilutions in refrigerator until required.
8. Calculate wt% internal standard using INTSTD template, save template in
the appropriate manner.

4.7.4. Condensate Samples

1. All samples should be run at least in duplicate.

2. The vial must be labelled with the request number and cycle number.
3. Fill a 2ml vial to the neck with DCM and replace the lid.
4. Measure approximately 200-500µl using a glass syringe, add to vial and mix
well.
NB. DO NOT use plastic syringes or pipettes with condensates or DCM.
5. Store dilutions in refrigerator until required.

4.8. Building a Sequence

1. Open a previous sequence in File Editor.
2. For standards edit the table as follows:
Column Heading Enter
Raw File Base Name Standard name followed by batch/request number
as appropriate. For blanks use B[Date].
Cycle No. Next consecutive number.
Sample Name [Standard Name][description][ReqNo/Batch No.]
Run[Run No.]

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DETERMINATION OF C2-C36+ HYDROCARBONS IN PETROLEUM LIQUIDS IN

REMOTE LABORATORIES
Method File Name Select relative method
Vial Number Auto injector position
Request Request Number
3. Save sequence as QAddmmyy.
4. For samples edit the table as follows:
Column Heading Enter
Raw File Base Name Request Number. For standards the standard name
should precede the request number
Cycle No. Replicate number
Sample Name [Company][Job No.][Bottle No.][Description].
Method File Name Select relevant method for sample type.
Internal Std. Amount Wt% n- Hexene or 1 if internal standard is not used
Request Request Number
All other entries are default values.
6. Save sequence as SAddmmyy.

4.9. Analysis Procedure

1. Ensure that the auto injector wash bottles are clean & full and the waste bottles are
empty.
2. Load vials into auto injector tray, warming each one between hands if required.
3. Download sequence.
4. Manually start the instrument when ready.

4.10. Baseline Subtraction

Select a suitable baseline and subtract from all runs save file as [Req No.]BS.[Cycle
No.].RAW. The same baseline must be used for all standards and samples of the same
type.

4.11. Processing Results

Integrate the baseline subtracted files ensuring that the solvent peak is not integrated.
Check that individually identified isomers are labelled correctly.
1. Bind the files as [Req No.][Cycle No.]BS[Blank No.].
2. Calculate the results using the relevant template.
3. The QI will automatically be calculated where appropriate and added to data log.
4. Save standard report as [Standard name][Req No.][Cycle No.]BS[Blank No.].
5. Save sample report as L[Req No.][Replicate].
4.12. Calculation
For samples fully recovered the mass wt% of each component is calculated as follows:
Mass% component i = Ai x RRFi x 100
Σ(Ai x RRFi)

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Where:
Ai = area of peak for component i
RRFi = relative mass response factor for component i. Use a relative response factor
of 1 for all components except benzene (0.89), toluene (0.94), ethyl benzene
and xylenes (0.97)
For samples where internal standard is added:
Calculate the mass% internal standard as follows:
Mass% Internal standard = W3 – W2 x 100 x P
W3 – W1

Where:
W1 = Mass of vial
W2 = Mass of vial + sample
W3 = Mass of vial + sample + n-hexene
P = purity factor of n hexane determined by GC analaysis

Calculate internal standard recovery as follows:

RecovHex = (A Hex / A Tot x 100) / CHex x 100

Calculate C36+ recovery as follows:

Recov 36+ = ((A 36+ / AHex) x CHex) x (100 / (100 – CHex))

Calculate recovery as follows:

Recovery = ΣC C1-C35 + Recov 36+

Calculate unrecovered material as follows:

Mass% Unrecovered material = 100 - Recovery

Calculate the mass wt% of each component as follows:

Mass% component i = (((A i x RRF i) / A Hex) x C Hex) x (100 / 100 – C Hex)

Calculate the mass wt% of C36+ as follows:

Mass% C36+ = Recov 36+ + (100 – Recovery)

Where:
RecovHex = n-Hexene recovery
A Hex = Area of n-Hexene peak
A Tot = Sum of areas of all peaks in sample + area of n-hexene peak
A 36+ = Area of C36+ peak
Ai = Area of peak for component i
CHex = Mass% internal standard

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REMOTE LABORATORIES
RRFi =
relative mass response factor for component i. Use a relative response
factor of 1 for all components except benzene (0.89), toluene (0.94),
ethyl benzene and xylenes (0.97)
Recov 36+ = Mass% of integrated C36 peak
ΣC C1-C35 = Sum of the mass% of components C1-C35

4.13. Reporting Results

Once all of the data has been processed and all QA standards are within limits, the
baseline subtracted .BND files for all standards and samples should be sent to the FAC
Reading to be checked. Results should NOT be reported to clients without first being
checked.
The average mass wt% of each component should be reported to the nearest 0.001%.
There may be occasions when it is necessary to report results outside of the expected
limits when this is acceptable for the customers requirements. Such results should first
be approved by the relevant senior supervisor.

4.14. Uncertainty
For condensate samples the estimated uncertainties are shown below:
- For C2-C29 components the estimated uncertainty is ± 6% relative at 95% confidence
limits.
- For C30+ fractions the estimated uncertainty is ± 11% relative at 95% confidence
limits.

For opaque samples the estimated uncertainties are shown below:

- For C2-C35 components the estimated uncertainty is ± 8% relative at 95% confidence
limits.
- For C36+ fractions the estimated uncertainty is ± 12% relative at 95% confidence
limits.
- Results may be reported outside of these uncertainties if the results are considered
to be acceptable by the customer.

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SATELLITE LAB: CCE/SATURATION PRESSURE- BLACK OIL SYSTEM

This Work Instruction is a mandatory requirement, and forms part of the Approved Integrated
Management System. Alterations are not permitted without the prior approval of the Senior Technical
Manager or the relevant Department Supervisor.

1. PURPOSE
This is the procedure to use when it is necessary to use CCE/Saturation pressure in a Satellite
Lab Black Oil System (SLS).

2. AUTHORITY
This work instruction is written and maintained with the authority of the Senior Technical
Manager or the relevant document owner.

3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this
work instruction.

4. PROCEDURE
4.1. Outline
A sample of reservoir fluid has been charged to a Satellite Lab Black Oil System (SLS).
The saturation pressure is then determined at reservoir temperature, or any other
temperature specified by the client.
The saturation pressure measurement can also be performed in conjunction with
experiments such as Reservoir flash, Separator tests and Differential liberations in order
to measure the liquid volume in the (SLS).
The test can be extended to perform a constant composition expansion (CCE) to
determine relative volume, coefficient of compressibility, and Y-function.

4.2. Safety Precautions for Handling Liquids and Gases under Pressure
- Staff should be familiar with all associated Risk Assessments and COSHH Risk
Assessments before proceeding.
- Eye protection and protective clothing be worn. WI0025 Personal Protective
Equipment.
- Ensure pipe work is in good condition and that end connectors are compatible.

4.3. Quality Assurance

- Ensure all equipment is in calibration before commencement of work.
- Record next calibration date on the worksheet.
Note: Reservoir (or client specified) temperature must be obtained in writing from the
client before you start any work at temperature. The temperatures (and pressures)
recorded on the sampling sheets are usually at flowing conditions.
Once reservoir pressure is known then ALL experiments should be performed above this
where possible.
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SATELLITE LAB: CCE/SATURATION PRESSURE- BLACK OIL SYSTEM

4.4. Method
Check to see if the fluid under investigation contains H2S; if so consult WI/0015 as to the
correct safety measures.
Charge between 20 – 25 cc fluid to the cell at the charging and allow to stabilise at
experimental temperature (WI/0102).
Manually shuttle the sample between pump A and pump B two to three times to
provide agitation to stabilise the sample (this is useful to provide a rough starting
volume for the PV software).
(This work instruction has been written for use with PV program version 1.0.)
Ensure the fluid is all in Pump A (this is required for the software to work).
▪ Load the PV program and ensure connection between the ISCO pumps and the
software (i.e. the correct pressure and volumes are displayed on the computer).
▪ Enter the following parameters into the PV software.
▪ Maximum pressure is set to below 10’000 psig (if possible 9000psig is recommended)
▪ Maximum flow rate is set to 10mls/min
▪ Pressure stabilisation tolerance (PST) is set to a value between 2 and 5. A PST of 2 is
recommended for PV/CCE relationship measurements. Checks between Diff and Sep
test stages can have a PST of 5
▪ Enter the volume of the first stage (usually slightly smaller than the current volume)
and the increments you wish to use for the PV.
▪ Choose the number of PV points, ideally to give 5 points above and 5 points below
the saturation pressure. If you are using the PV program to stabilise the sample run 1
point.
▪ Enter the file name and check the directory path
If only the saturation pressure is required, then press the ‘start PV’ button (it may be
necessary to press this twice).
If the test is to be extended to run a CCE, before starting the PV:
▪ Choose the number of CCE points required usually between 15-20. This can vary, in
that higher saturation pressures may require more points and lower ones less.
Ensure the ‘Perform CCE’ button is highlighted and press the ‘start PV’ button. The
program should start shuttling the sample.
Start the Druck logging program in order to log the calibrated gauge.
1. If running the druck logging program and PV program on separate computers,
ensure that check the computer times read the same.
2. On the druck logging software, set the path and filename.
3. Set the loggin interval to 10 seconds. For CCE’s if they are to be left running
overnight a larger interval may be more appropriate.
4. Set the program running.
Note: For the CCE measurement a relatively small volume of sample should be charged
in order to reach the lower pressures <500 psig.

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SATELLITE LAB DENSITY MEASUREMENTS OF LIVE FLUIDS - BLACK OIL SYSTEM

This Work Instruction is a mandatory requirement, and forms part of the Approved Integrated
Management System. Alterations are not permitted without the prior approval of the Senior Technical
Manager or the relevant Department Supervisor.

1. PURPOSE
This is the procedure to use when it is necessary to perform Satellite Lab density measurements
of live fluids from Satellite Lab Black Oil System (SLS).

2. AUTHORITY
This work instruction is written and maintained with the authority of the Senior Technical
Manager or the relevant document owner.

3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this
work instruction.

4. PROCEDURE
4.1. Outline
To determine the density of a live fluid.

4.2. Safety Precautions for Handling Liquids and Gases under Pressure
- Staff should be familiar with all associated Risk Assessments and COSHH Risk
Assessments before proceeding.
- Eye protection and protective clothing be worn. WI/0025 Personal Protective
Equipment.
- Ensure pipe work is in good condition and that end connectors are compatible.

4.3. Quality Assurance

- Ensure all equipment is in calibration before commencement of work.
- Record next calibration date on worksheets.

4.4. Method
Check to see if the fluid under investigation contains H2S; if so consult WI/0015 as to the
correct safety measures.
1. Charge approx. 30 cc fluid to Satellite Lab Black Oil System and heat to flash
temperature, allowing a minimum of 4 hours at temperature, with the system in
constant pressure mode.
2. Use the pV program to stabilise fluid in single phase (See WI/0104), select a
pressure covered within the saturation pressure measurement.
3. Evacuate and weigh the denisty coil and attach to the SLS typically using the
external valve on the oven wall.

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SATELLITE LAB DENSITY MEASUREMENTS OF LIVE FLUIDS - BLACK OIL SYSTEM

4. Fill the lines to the density coil, bleed any air out. Ideally, try whenever possible to
use 1/16” line between coil and SLS. This keeps the sample volume loss to a
minimum when you bleed the line. Displace any entire line volume during this
bleed. This will ensure that the line contains air free single phases fluid. If any leaks
are detected in the line to the coil, isolate the SLS before attempting to tighten, as
this may cause total line failure.
5.Allow pressure to stabilise, pump must be reading 0.0000 ml/min, record volume.
6. Displace approximately 10 cc of fluid under constant pressure, before closing the
valve on the density coil.
7. Allow pressure to stabilise, pump must be reading 0.0000 ml/min, record volume.
8. Close valve on the side of the oven to isolate the SLS and disconnect the coil.
9. Weigh the denisty coil. The coil and especially the threads of the valves must be
clean and dry prior to weighing.
Use the pV sheet to determine the pump correction factor.
10. Repeat steps 3-9 until two measurements consistent to the third decimal place are
obtained.

4.5. Apparatus

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SATELLITE LAB: DIFFERENTIAL VAPORISATION

This Work Instruction is a mandatory requirement, and forms part of the Approved Integrated
Management System. Alterations are not permitted without the prior approval of the Senior Technical
Manager or the relevant Department Supervisor.
1. PURPOSE
This is the procedure to use when it is necessary to perform a differential vaporisation test.

2. AUTHORITY
This work instruction is written and maintained with the authority of the Senior Technical
Manager or the relevant document owner.

3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this
work instruction.

4. PROCEDURE
4.1. Outline
In a differential vaporisation test, the gas in the solution at reservoir temperature (or
any other test temperature) is liberated in six or more stages at more or less equal
pressure drops, between fluid saturation pressures and abandonment pressure. The
experiment simulates the process in an oil reservoir as the pressure declines, assuming
that the greater gas mobility, compared with that of the liquid, allows the gas to escape
preferentially, leaving a liquid which becomes progressively heavier.
The experiment determines the solution GOR, gravity and Z factor of the gas evolved at
each stage and the oil volume factor at each stage, usually using residual liquid at STP as
the reference volume.

4.2. Safety Precautions for Handling Liquids and Gases under Pressure
- Staff should be familiar with all associated Risk Assessments and COSHH Risk
Assessments before proceeding.
- Eye protection and protective clothing must be worn. Personal Protective
Equipment.
- Ensure pipe work is in good condition and that end connectors are compatible.

4.4. Method
Check to see if the fluid under investigation contains H2S; if so consult as to the correct
safety measures.
It may be useful to have slightly smaller pressure drops in the first stages and the last.
The last stage is usually taken as 500 psia although some clients will specify others.
1. Charge 60 - 80cc fluid to the Satellite Lab pVT system and heat to required
temperature, allowing a minimum of 4 hours at temperature, with the system in
constant pressure mode.
2. Perform a saturation pressure measurement.

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SATELLITE LAB: DIFFERENTIAL VAPORISATION

3. Stabilise the fluid at the first chosen take-off pressure by agitating the fluid
between the two pumps, allow to stand at stage pressure for one hour before
recording the volume.
4. Whilst the system is standing the following steps can be performed. Weigh glass
receiver empty and select a suitable calibrated gas collection vessel in order to trap
as much gas as possible.
5. Note atmospheric pressure and ambient temperature evacuate collection system
(see apparatus diagram below)
6. For stages above 1000 psi, the Satellite Lab system pumps are set in constant
pressure and the control valve is slowly cracked open to allow the gas cap out –
(the ISCO pumps should maintain the pressure.) These two actions are balanced to
provide the removal of gas at a constant controlled pressure and flow rate. It is
advisable to do these things slowly to retain maximum control (0.5-2 mls /min)
If the pressure is below 1000 psi, run the pumps in constant flow (2-6 mls/min) and
keep the pressure constant by balancing the opening / closing the valve and the
flow rate.
When using this method a stable flow/ pressure can be achieved, but may take a 1-
2 mls of flow to do so.
7. Remove all the gas phase and collect for analysis, once the collection system has
reached atmospheric pressure, close the balloon and any remaining gas can go
through a gasometer.
8. Once all the gas phase has been removed, you will see a pressure spike/pumps stop
running, close the system and allow the pumps to stabilise. Record the end point.
9. Weigh glass receiver + Fluid.
10. Return the fluid to single phase and perform a saturation pressure measurement. If
the saturation pressure is much higher than the stage pressure repeat stages 3-10.
Ensure all additional volumes of gas or condensate are recorded.
11. Once the saturation pressure measurement is within 15 psi of the stage pressure,
proceed to the next stage pressure and repeat the above steps until the last stage
is reached.
12. After the saturation pressure has been determined for the last stage and is ok. The
residual fluid is then flashed to atmospheric conditions.
13. Measure the density / gravity of stock tank oil.
14. Return the fluid to single-phase and stabilise using the pV program. Perform a live
fluid density measurement on the remaining fluid.

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SATELLITE LAB: DIFFERENTIAL VAPORISATION

4.5. Apparatus

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SATELLITE LAB: RECOMBINATION

This Work Instruction is a mandatory requirement, and forms part of the Approved Integrated
Management System. Alterations are not permitted without the prior approval of the Senior Technical
Manager or the relevant Department Supervisor.

1. PURPOSE
This is the procedure should be adopted when performing a recombination using the Satellite
Lab PVT system with a pressurised fluid sample.

2. AUTHORITY
This work instruction is written and maintained with the authority of the Senior Technical
Manager or the relevant document owner.

3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this
work instruction.

4. PROCEDURE
4.1. Outline
Following a separator oil flash and a compositional anaylsis of the separator Gas, a
mathematically recombined composition is calculated using the corrected field
separator gas:oil ratio. Separator oil and separator gas are physically recombined in a PV
cell using the corrected field separator gas:oil ratio, in order to provide us with a
representative reservoir fluid sample

4.2. Safety Precautions for Handling Liquids and Gases under Pressure
- Staff should be familiar with all associated Risk Assessments and COSHH Risk
Assessments before proceeding.
- Eye protection and protective clothing be worn. Personal Protective Equipment
- Ensure pipe work is in good condition and that end connectors are compatible.
- Ensure the maximum working pressures of the sample cylinder and pipe work are
not exceeded.

4.3. Quality Assurance

Ensure all equipment is in calibration before commencement of work. Record next
calibration date on the worksheet.

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SATELLITE LAB: RECOMBINATION

4.4. Apparatus

Top Valve
Pump Top Valve Remote PVT Cell

Pressure Oil Sample Oil Sample

Gauge

Water/Glycol Pump A Pump B

Pump B: Stop

Pump A: Constant Pressure

Transfer Pump

4.5. Method
The separator oil is flashed in single phase. The composition of the separator gas is
determined.
The field separator GOR is then corrected for laboratory use. There may be occasions
where a specified GOR is provided by the client which does not require correction.
Fill in the field Fpv and Fg values on the sample data sheet of the workbook. These
are be taken off the sampling sheets.
Fpv = 1 Fg = 1
Z s.g.

The laboratory Fpv and Fg are calculated from the separator gas Z factor and specific
gravity, which are derived from the gas compositions. The Z factor is calculated at
separator conditions.
The field GOR is taken from the sample sheet. The figure is checked by dividing the
gas rate by the oil rate. The field oil rate can be expressed as “dead” stock tank
barrels or “live” separator barrels.
It is very important that the correct data is introduced to the sample data sheet. If
both rates are given then introduce both the worksheet. The worksheet uses then
more reliable separator barrels (if present). If the oil rate on the sampling sheets is
only expressed in STB then the workbook will convert by dividing the Bo from the
separator oil flash to give Sep. Bbl.
The field GOR is then corrected by using the Fpv and Fg values from the field and lab.
This is done on the “data for recombination” sheet within the workbook.

Corrected GOR =Fpv X Fg (lab) X Field GOR

Fpv x Fg (field)

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SATELLITE LAB: RECOMBINATION

To obtain the mathematical recombined composition use the sheet within the
workbook which adds the separator products together to give a estimate of the
reservoir fluid.
1. The separator gas is heat soaked at above the separator temperature, using the
large oven or heating bands. The contact pressure of the separator gas at separator
temperature should be equal or greater than the separator pressure.
2. In order to put enough gas for recombination in the measuring equipment to satisfy
the required GOR a gas compressor is used. Be aware that as the gas is removed
from the source cylinder the pressure may drop below the dew point of the
separator gas causing compositional differentiation. To avoid this do not use the
booster for more than a few minutes. The hot separator gas container is rolled to
ensure a homogenous sample and connected to the recombination cell via the
compressor The booster cell (usually a 1 litre Proserv cylinder) is attached to a
transfer pump via the bottom valve. The connecting line is pressured to 6000 psig
and checked for leaks before the bottom valve is opened into the water side below
the piston. The gas sample is attached to the top valve of the evacuated booster
cylinder and the line bleed to purge any air from the line. If the gas is known to
contain H2S pre evacuate the line rather than bleed the line. A three way valve is
used to evacuate and dispose of the H2S safely. The top valve is then opened and
gas passes into the booster cell. If available the gas booster is used to increase the
gas pressure within the recombination cell to the extent to satisfy the required
GOR.
3. Once the gas has been transferred to the recombination cell this is pressure up to
6000psi and the volume of water injected is noted.
4. The volume of separator gas required to achieve a total recombined volume of
around 500cc of reservoir fluid should be pre-calculated.
5. The gas bottle is agitated and the required volume charged to the Satellite Lab
system, (note; the dead space is not required).
6. Once the system has been charged, the evacuated cylinder selected for the
recombined sample is connected to the Satellite Lab system, the connecting line
filled and bled to remove any air contamination. The system is allowed to stabilise
and volumes recorded. The target cylinder valve is cracked open and the required
amount of gas is transferred. This may involve more than one pump load, in which
case additional gas is charged to the Satellite Lab system and the process repeated
as in stage 5.
7. The Satellite Lab system is evacuated and heated to separator temperature. The
separator liquid should already be restored to above sampling temperature and
pressure.
8. The exact volume of separator liquid is calculated.
9. The required volume of separator liquid is then charged to the Satellite Lab system.
(Note the charge and transfer pressures should be the same pressure as used
during the live fluid density measurement.
10. The system is allowed to stabilise prior to the transfer of the separator liquid.
11. The recombination cylinder containing a known volume of separator gas is
connected to the Satellite Lab system, the connecting line filled with separator
liquid and bled to remove any air contamination. The system is allowed to stabilise
and volumes recorded. The target cylinder valve is cracked open and the required

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SATELLITE LAB: RECOMBINATION

amount of liquid is transferred. (note; this may involve more than one pump load, in
which case additional gas is charged to the Satellite Lab system and the process
repeated.
12. The recombined fluid is then pressured up into single-phase and prepared for
validation of the recombination.

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REMOTE LAB: SEPARTATOR TEST

This Work Instruction is a mandatory requirement, and forms part of the Approved Integrated
Management System. Alterations are not permitted without the prior approval of the Fluids Laboratory
Manager or the relevant department senior supervisor.

1. PURPOSE
This is the procedure to use when it is necessary to carry out an onsite separator test.
2. AUTHORITY
This work instruction is written and maintained with the authority of the Fluids Laboratory
Manager or the relevant document owner.
3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this
work instruction.
4. PROCEDURE
4.1. Outline
A multi-stage separator test simulates the passage of the reservoir fluid from reservoir
conditions, through a series of separators, which are maintained at specific pressures
and temperatures. Each stage usually, but not always, steps down the pressure and
temperature from reservoir to stock tank conditions.
A portion of the reservoir fluid is charged to the Remote Lab PVT cell and after the
saturation pressure is checked at reservoir temperature (see Remote Lab WI/2603) the
gas is removed in a number of stages. Each stage of removal is at a fixed temperature
and pressure, as requested by the client. The test determines the GOR, gravity and Z
factors of the gas evolved, oil volume factor and fluid density for each stage, usually
using residual liquid at STP as the reference volume.
4.2. Safety Precautions for Handling Liquids and Gases Under Pressure
- Eye protection and protective clothing must be worn.
- Ensure pipe work is in good condition and that end connectors are compatible.
4.3. Quality Assurance
- Ensure all equipment is in calibration before commencement of work.
- Record next calibration date on worksheets.
Reservoir temperature must be obtained in writing from the client before you start any
work at temperature. The temperatures (and pressures) recorded on the sampling
sheets are usually at flowing conditions.
If reservoir pressure is known then ALL experiments should be performed above this
where possible.

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REMOTE LAB: SEPARTATOR TEST

4.4. Apparatus

4.5. Method
1. Charge 30 cc fluid to the Remote Lab pVT system and heat to the reservoir
temperature, allowing a minimum of 4 hours for thermal stability, with the system
in constant pressure mode (WI 2601).
2. Perform a saturation pressure measurement (See WI/2603) to establish the initial
saturation volume and pressure. The saturation pressure should be known from
other experiments and it may be useful to check and access the validity of the
current charge.
3. Stabilise the fluid at the first stage separator conditions by agitating the fluid
between the two pumps (a minimum of three complete shuffles), leave stabilising
for 1 hour and record the volume. As this will normally involve cooling the system it
is important to leave sufficient time to achieve thermal stability.
4. Weigh glass receiver empty and select a suitable calibrated gas collection vessel in
order to trap as much gas as possible. At this stage the glass receiver is in line to
collect any of the heavier components from the gas phase that may condense at
room conditions.
5. Note atmospheric pressure and ambient temperature and evacuate the gas
collection system (see apparatus diagram above). Record the evacuated pressure
within the gas collection system.
6. For stages above 1000 psi, the Remote Lab system pumps are set in constant
pressure and the control valve is slowly cracked open to allow the gas cap out –
(the ISCO pumps should maintain the pressure.) These two actions are balanced to
provide the removal of gas at a constant controlled pressure and flow rate. It is
advisable to do these things slowly to retain maximum control (2-4 mls /min).

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REMOTE LAB: SEPARTATOR TEST

If the pressure is below 1000 psi, run the pumps in constant flow (2-6 mls/min) and
keep the pressure constant by balancing the opening / closing the valve and the
flow rate.
When using this method a stable flow / pressure can be achieved, but may take a 1-
2 mls of flow to do so.
7. Remove all the gas phase and collect for analysis, once the collection system has
reached atmospheric pressure, close the balloon and any remaining gas can go
through a gasometer meter. The end point is determined by one of two ways;
a. If running in constant pressure the pressure gauge will jump and the pumps will
almost stop.
b. If running in constant flow the pressure gauge will jump up. At this stage stop the
pumps and return the system to the take off pressure.
8. Once all the gas phase has been removed, close the system and allow the pumps to
stabilise. Record the end point.
9. If both pumps are required for expansion, allow the fluid to stabilise for 1 hour and
remove the majority of the gas, leaving around 10 – 20cc gas cap. Stabilise the
system as per step 3 and remove the remaining gas.
10. If the fluid cannot be expanded sufficiently and requires “bleeding” down then
leave for 1 hour, bleed down to required pressure and leave for a further hour prior
to removing the gas as per stage 9.
11. Where all the gas cannot be collected into one balloon, the volumes and a sub-
sample will need to be taken for each stage of the process.
12. If condensate has been produced in sufficient quantity then weigh the now wet
glass receiver and sub sample for compositional analysis. The produced condensate
is part of the gas phase composition and should be mathematically added to the
composition of the dry gas.
13. Return the fluid in the Isco pump to single phase and perform a saturation pressure
measurement. If the saturation pressure is much higher than the stage pressure
repeat stages 3-10. Ensure all additional volumes of gas or condensate are
recorded. As well as providing at quality check on the phase separation this will
also provide the volume of the remaining liquid in the cell for Bo determination.
14. Once the saturation pressure measurement is within 15 psi of the stage pressure,
proceed to the next stage pressure and repeat the above steps until the last
requested stage is reached. It is normal for the clients to provide stage conditions
that reflect their production plants. It will normally NOT INCLUDE stock tank
conditions, 14.7 psia and 60°F. Even when the client does give you these we do not
carry out the above procedure for stock tank conditions. It has been found that
quality of the test is greatly increased by flashing out the liquid in single phase as
describe in points 12-17.
15. After completion of the last specified stage return the fluid to single phase by
performing a single point pV (WI/2603).
16. Perform a single stage flash on the fluid (WI/2605).
17. Collect and analyse the phases.
18. Measure the density / gravity of stock tank oil.

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REMOTE LAB: SEPARTATOR TEST

19. After the flash perform a saturation pressure measurement to obtain the volume
left in the cell (See W/2603)
20. Return the fluid to single-phase and stabilise using the pV program. Perform a live
fluid density measurement on the remaining fluid (See WI 2604).

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REMOTE LAB SINGLE STAGE FLASH SEPARATION OF LIVE FLUIDS

This Work Instruction is a mandatory requirement, and forms part of the Approved Integrated
Management System. Alterations are not permitted without the prior approval of the Senior Technical
Manager or the relevant Department Supervisor.

1. PURPOSE
This is the procedure to use when it is necessary to perform a single stage flash separation test.
2. AUTHORITY
This work instruction is written and maintained with the authority of the Senior Technical
Manager or the relevant document owner.
3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this
work instruction.
4. PROCEDURE
4.1. Outline
As part of the sample validation process a portion of single phase fluid at separator,
reservoir or sampling pressure and temperature is metered from the Remote Lab pVT
system into the Remote Lab flash unit, to allow liquid and gas to separate at
atmospheric pressure and ambient temperature. The gas evolved is measured by
partial pressure and a wet test meter, and a sub-sample is collected into a weighed
vessel for compositional analysis. The mass and specific gravity of the residual oil are
determined and corrected to STP.

4.2. Safety Precautions for Handling Liquids and Gases under Pressure
- Eye protection and protective clothing be worn. WI0025 Personal Protective
Equipment.
- Ensure pipe work is in good condition and that end connectors are compatible.
- Ensure suitable screening devices are used wherever possible.

4.4. Quality Assurance

- Ensure all equipment is in calibration before commencement of work.
- Record next calibration date on worksheets.

Reservoir temperature must be obtained in writing from the client before you start any
work at temperature. The temperatures (and pressures) recorded on the sampling
sheets are usually at flowing conditions.
If reservoir pressure is known then ALL experiments should be performed above this
where possible.

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REMOTE LAB SINGLE STAGE FLASH SEPARATION OF LIVE FLUIDS

4.5. Apparatus

4.6 Method
Check to see if the fluid under investigation contains H2S; if so consult WI/0015 as to the
correct safety measures.
1. Charge approx. 80cc fluid to Remote Lab pVT system and heat to flash
temperature, allowing a minimum of 4 hours at temperature, with the system in
constant pressure mode (See WI/0102)
2. Use the pV program to stabilise fluid in single phase (See WI/0104).
3. Weigh glass receiver empty and select a suitable calibrated gas collection vessel in
order to trap as much gas as possible and a minimum of 10cc fluid. If the lab
temperature is significanly warmer than 16C / 60F, a water/ice bath should be used
to cool the glass receiver.
4. Note atmospheric pressure and ambient temperature evacuate collection system
(see apparatus diagram below).
5. Option 1 – Low GOR fluids - Flush the gasometer several times with Helium,
connect to flash unit and evacuate the whole flash system. Open to gasometer and
fill with Helium, repeat several times until confident flash system is full of Helium at
STP.
6. Option 2 – High GOR Fluids – Once the system has been evacuuated and the gas
collection vessel pressure recorded and closed, flush the entire system several
times with Helium to ensure that the flash unit is full of Helium at STP. Connect to a
wet test meter and record the initial reading. Follow steps 7 & 8, allowing the
produced gas to flow through the wet test meter until a minimum of 2 times the
manifold volume of the flash unit have passed through. Slowly open the valve at
the top of the gas collection vessel to begin sub-sampling the gas, taking care to
ensure that there is always flow through the wet test meter (i.e. it is constantly
turning and opening the valve only causes it to slow down). Once the vessel is full
the wet test meter should speed up again (another check if you are not sure is to

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REMOTE LAB SINGLE STAGE FLASH SEPARATION OF LIVE FLUIDS

open the balloon valve further, observing the wet test meter – if it slows more then
the balloon is not full yet). Note the final pressure in the gas vessel (this should be
atmospheric pressure) and the final reading on the wet test meter.
7. Set the ISCO transfer pump to run in constant pressure mode
8. Open the pVT system valve and flash sufficient fluid for analysis, a minimum of 10cc
STO is required. (The fluid should be flashed in a controlled manner at
approximately 3-5mls / minute ensuring the pressure is kept relatively stable)
9. Collect and record the produced phases for analysis, noting the final pressure of the
collection system.
10. Once flash is complete close all valves and disconnect.
11. Weigh glass receiver + Fluid. If a water/ice bath has been used, care must be taken
that it is completely dry on the outside before weighing.
12. Measure density/gravity of stock tank fluid. A minimum of two consistent readings
is required.

If insufficient fluid is collected, repeat stages 3 – 11.

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DETERMINATION OF DYNAMIC VISCOSITY BY CAPILLARY VISCOMETER

This Work Instruction is a mandatory requirement, and forms part of the Approved Integrated Management System.
Alterations are not permitted without the prior approval of the Senior Technical Manager or the relevant
Department Supervisor.

1. PURPOSE
This is the procedure to use when it is necessary to determine the dynamic viscosity of a pressurised fluid
using a capillary viscometer.
2. AUTHORITY
This work instruction is written and maintained with the authority of the Senior Technical Manager or the
relevant document owner.
3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this work
instruction.
4. PROCEDURE
4.1. Outline
The volume factor or pump factor for mercury-free syringe pumps are close to, but not exactly
one. The true factor is dependent on pressure and temperature and is different for all pumps. It is
therefore necessary for all mercury-free syringe pumps used for volumetric work to be calibrated
at a reference pressure.
4.2. Apparatus
Two microprocessor controlled pumps are connected via a capillary loop. A differential pressure
transducer (Validyne) is connected across both ends of the capillary loop. The pump cylinders and
loop are maintained at constant temperature within an air bath.
There are no valves and a minimum number of fittings along the flow path of the fluid. The
capillary loop has been fitted so that it has the largest diameter possible to reduce centrifugal
Dean vortices. Note that it is a circular shape, not elliptical. There are no sharp bends anywhere
along the flow path. All of the system tubing is a much larger internal diameter than the capillary
itself, e.g. 1/8” large bore when using 1/16” / 0.5 mm internal diameter capillary.
The differential pressure transducer must be installed with a bypass manifold to prevent
stretching the diaphragm when charging, draining or during rapid fluid flow. It is better to use 1/8”
wide bore tubing either side of the bypass valve itself, to reduce differential pressure if flowing
through the bypass valve.

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DETERMINATION OF DYNAMIC VISCOSITY BY CAPILLARY VISCOMETER

4.3. Safety Precautions

- Staff should be familiar will all the associated Risk Assessment and COSHH Risk Assessments
before proceeding.
- Eye protection and protective clothing be worn.
- Ensure pipe work is in good condition and that end connectors are compatible.
- Ensure suitable screening devices are used wherever possible.

4.4. Method
Check to see if the fluid under investigation contains H 2S; if so consult as to the correct safety
measures.
The sample fluid must be filtered via a 2 micron sinter or equivalent when charging. Particulates
will interfere with the viscosity measurements and may also block the capillary. The differential
pressure transducer bypass valve must be left open when charging.
1. Start with nearly all of the fluid in pump B and a small amount in pump A. Run pump A in
constant pressure mode at the pressure of interest and set pump B to the required flowrate.
Please note, that for lower pressures pump A may need to be ran in refill mode..
2. Start collecting data from the differential pressure transducer (AD 0094).
3. Once pump B is stable, take a ‘zero’ reading from the differential pressure transducer with the
bypass open, noting the time.
4. Set the first flow rate on pump A and start flowing, noting the time and flow rate.
5. Close the bypass valve.
6. Wait until differential pressure is as stable as possible then note the reading and the flow rate.
7. Increase pump A flow to the next flow rate and repeat step 6, do this for a total of at least five
flow rates.
8. Check Reynold’s and Dean numbers. Perform more measurements if required.

If pump A runs empty, open the bypass and shut ONE of the differential pressure transducer
isolation valves. Flow fluid back to pump A. Open isolation valve and start as (1.) at next flow rate.

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DETERMINATION OF DYNAMIC VISCOSITY BY CAPILLARY VISCOMETER

The set of flow rates depends on the viscosity of the fluid and the maximum range of the
differential pressure transducer. For very thin fluids the Dean number will be the limiting factor
and lower flow rates will have to be used, resulting in very small differential pressures. With more
viscous fluids, the differential pressure transducer range will limit how fast flow can be through
the capillary.
Typically measurements are performed at five pressure setpoints above saturation pressure, and
as required below saturation.
In the single phase region, perform each set of flow rates at each pressure, starting at the highest
pressure. When adjusting fluid pressure, ensure that the differential pressure transducer bypass is
open.
For measurements below saturation pressure, prepare the fluid by depressurising and expelling all
of the liberated gas from the apparatus. Restabilise the fluid at 50 – 100 psi higher than the new
saturation pressure and measure viscosity at that pressure as per single phase method.
4.4.1. Calibration
Each capillary must be calibrated to determine the average internal diameter over the
range of working conditions. This involves measuring a fluid of known viscosity at
temperatures and pressures covering the range of working conditions, and back
calculating the internal diameter from the results. A minimum of four measurements are
required. The capillary is then assigned the calculated internal diameter.
A repeat run should be performed at measurement temperature and pressures using a
fluid of known visosity to check the results are within limits and any adjustments made.

4.5. Calculation

Viscosity is calculated from the differential pressure measured across the length of the tube using
Pouseille’s equation:
Where:
 Pr 4
=
8Ql
= viscosity (Pascal seconds, Pa.s)
= Pi
P = differential pressure (Pascals, Pa)
r = internal radius of tube (metres, m)
Q = flow rate of fluid (metres cubed per second, ms-3)

l = length of tube (metres, m)

This assumes that the flow within the tube is laminar. Laminar flow is determined by calculating
Dean and Reynolds numbers:

2Q
Re =
r
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DETERMINATION OF DYNAMIC VISCOSITY BY CAPILLARY VISCOMETER

Where:
Re = Reynold’s number (dimensionless)
Q = flow rate (metres cubed per second, ms-3)
= density (kilogrammes per metre cubed, kgm-3)
= Pi
r = internal radius of the tube (metres, m)
= viscosity (Pascal seconds, Pa.s)

Flow is said to be laminar r when Re < 2000.

De = 2 Re
R

Where:
De = Dean number (dimensionless)
Re = Reynold’s number (dimensionless)
r = internal radius of the tube (metres, m)
R = helical radius of the tube (metres, m)
Flow is said to be laminar when the De < 10.

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OIL EMULSION STUDY

This Work Instruction is a mandatory requirement, and forms part of the Approved Integrated
Management System. Alterations are not permitted without the prior approval of the Fluids Laboratory
Manager or the relevant departmental senior supervisor.
1. PURPOSE
This is the procedure to use when carrying out an oil emulsion study.
2. AUTHORTITY
This work instruction is written with the authority of the Business Development Manager and
may not be amended without his or his designated nominee, the Fluids Laboratory Managers
written approval.
3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this
work instruction.
4. PROCEDURE
4.1. Outline
Emulsion characteristics of heavy and light oils are carried out using this apparatus. A
range of emulsions are made with varying water cuts, these emulsions are then allowed
to settle isothermally. The effect of demulsifiers on the oil can also be measured in the
following experiment.
4.2. Apparatus
- Hamilton Beach mixer with mixing cup and flexible mixing head or equivalent.
- Centrifuge tubes and rack - check all graduations on tubes are visible.
- 250 ml and 50 ml measuring cylinders.
- Water bath and temperature controller.
- Stopwatch.
- Clamps, bossheads and stands.
- Metal cans (500 ml or 1 L).
- Polythene bottles (500 ml or 1 L).
- Brand Transferpettor or similar to measure small volumes of demulsifier.

4.3. Chemicals
- Synthetic formation water (SFW) (keep in polythene bottle).
- Crude oil (keep in metal cans tightly capped).
- Treating chemicals, scale inhibitor, corrosion inhibitor, demulsifier.

4.4. Method
1. Set the water bath to the required temperature.
2. Treat SFW with required concentration of scale inhibitor and the oil with corrosion
inhibitor as appropriate. It is important to only treat the whole batch of SFW with
scale inhibitor if all the water will be used on the same day.
3. Allow the following to come to temperature in the water bath:

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OIL EMULSION STUDY

- Treated SFW
- Crude oil
- Measuring cylinders
- Hamilton Beach cup or metal can for emulsion mixing
- Centrifuge tube in rack
4. Measure out appropriate volumes of oil and water into respective heated cylinders
and pour into Hamilton Beach cup. A total volume of 200ml is required to ensure
complete mixing.

5. Add the corrosion inhibitor and scale inhibitor to the oil/water and mix for 60 seconds
at the lowest speed setting. If a demulsifier performance is to be tested, the
demulsifier should be added during this mixing stage at the 50 seconds point. Always
run a blank containing no additives as a reference.

6. Immediately after the mixing is complete, pour the resulting solution equally into two
centrifuge tubes and start the timer.

7. Record the time/volume separated after 30 seconds, 1, 2, 5, 10, 15, 20 and 30

minutes, or as appropriate. Also note the water and interface quality at the
aforementioned intervals.

Results:

Average the results of the duplicates and report the results in graphical form. This
should relate the residual water in oil (% - Y axis) against time taken for separation (min
- X axis). Figure 1 below illustrates the normal reporting format and typical laboratory
demulsifier concentrations. Generally there is an order of magnitude difference
between the laboratory and field concentrations e.g. a 250 ppm demulsifier
requirement in the lab tests generally translates to a 25 ppm demulsifier requirement in
the field.

Figure 1
Field Name : Test Temp Deg. C : Demulsifier Number : % Water Cut
100
% Water Retained of
Original Added

80
60 400 ppm
40 500 ppm

20
0
1 2 5 10 15 20 30
Separation Time (mins)

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DETERMINATION OF KINEMATIC VISCOSITY BY MODIFIED IP 71

This Work Instruction is a mandatory requirement, and forms part of the Approved Integrated Management System.
Alterations are not permitted without the prior approval of the Senior Technical Manager or the relevant
Department Supervisor.

1. PURPOSE
This procedure should be used when determining the kinematic viscosity of a liquid petroleum product.
The procedure is a modified version of IP 71.

2. AUTHORITY
This work instruction is written and maintained with the authority of the Senior Technical Manager or the
relevant document owner.

3. RESPONSIBILITY
It is the responsibility of all staff at the Fluid Analysis Centre to ensure compliance with this work
instruction.

4. PROCEDURE
4.1. Outline
This procedure outlines the measurement of kinematic viscosity of both transparent and opaque
petroleum liquids using reverse flow viscometers. It is a modification of IP 71 the modifications
to the standard are detailed below.

4.2. Safety Precautions

- Staff should be familiar with all associated Risk Assessments and COSHH Risk Assessments
before proceeding.

4.3. Modifications to IP 71
This procedure differs from the published standard in the following respects:
• The temperature measuring device has an accuracy of ± 0.1°C
• Viscometers are cleaned with non alkaline cleaning material.
• Samples are not stirred or shaken to avoid including Hg dust in the test sample.
• Samples are not filtered (10.2 of IP 71) when charging the viscometer.
• Steps to remove thermal history of the sample (10.1.1-10.1.6 of IP 71) are not taken.
However waxy or viscous samples are heated in an oven at 80°C for a minimum of 30
minutes. Samples are not stirred or shaken to avoid including Hg dust in the test sample.

4.4. Verification of Viscosity Tubes

The calibration of glass viscometers is verified on a 6 monthly cycle using certified reference
standards as detailed in section 7 of IP 71. The measured viscosity should be within ± 1% of the
certified value. If the measured viscosity varies by more than 1% the viscometer tube should be
thoroughly cleaned using non alkaline cleaning agent and dried. Repeat the measurement.
NOTE: Silicone viscosity standards should not be used with glass viscometer tubes as it is very
difficult to remove silicones completely from glass surfaces.

4.5. Apparatus
- Viscometer. BS/IP/RF U-tube reverse flow viscometer with traceable certificate of
calibration. See IP 71 for details.

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DETERMINATION OF KINEMATIC VISCOSITY BY MODIFIED IP 71

- Viscometer Holder. As detailed in IP 71 Section 6.2.
- Temperature controlled bath. As detailed in IP 71 section 6.3.
- Temperature Measuring Device. The accuracy of this device is ± 0.1°C which is not in
accordance with IP 71.
- Timing device.
- Disposable pipettes.
- Rubber bungs for viscosity tubes.

4.6. Reagents and Materials

- Certified viscosity reference standards.
- Non alkaline cleaning agent.
- Toluene and Safesol for cleaning tubes. Solvents are not filtered as in section 5 of IP71.
- Acetone for drying tubes. Solvents are not filtered as in section 5 of IP71.

4.7. Determination of Viscosity of Transparent Liquids

Follow the procedure in section 9 of IP 71. See Annex C of IP71 for theoperating instructions to
charge the BS/IP/RF U-tube reverse flow viscometer.
Worksheets should be completed in full when recording data.
The viscosity should be measured in duplicate using different tubes of the same size where
possible. Results should not differ by more than ± 2% relative. If results are outside of these
limits the tubes should be cleaned with solvent and the measurement repeated. If the results are
still outside of these limits then clean the tubes with non alkaline cleaning agent and repeat.

4.8. Determination of Viscosity of Opaque Liquids

Charge sample and follow the procedure in section 10.2.1-10.4 of IP 71. See Annex C of IP71 for
theoperating instructions to charge the BS/IP/RF U-tube reverse flow viscometer.
Worksheets should be completed in full when recording data.
The viscosity should be measured in duplicate using different tubes of the same size where
possible. Results should not differ by more than ± 2% relative. If results are outside of these
limits the tubes should be cleaned with solvent and the measurement repeated. If the results are
still outside of these limits then clean the tubes with non alkaline cleaning agent and repeat.

4.9. Cleaning of the Viscometer

Follow the procedure in section 11 of IP 71. Non alkaline cleaning agent is used in place of
chromic acid. Viscometers are dried in an oven at 80°C for a minimum of 30 minutes.

4.10. Calculation
The calculation is detailed in section 12 of IP 71.

4.11. Reporting Results

For viscosities up to 10 cSt the mean viscosity is reported to the nearest 0.01 cSt at the
temperature of the test. For viscosities greater than 10 cSt the mean viscosity is reported to the
nearest whole number at the temperature of the test.

Precision
The difference between successive measurements by the same operator should not differ by
more than ± 2% relative.
The uncertainty is estimated to be ± 5% relative at 95% confidence limits.

VAPS-PVT-WI-018/Rev.00/03 May 2015 / Page 2 of 2

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