9999RO C DG DG00 OP PRO 0001 A01 Laboratory Operating Procedures

RUMAILA PROJECT
Custody Transfer Metering System
Laboratory Procedures
9999RO-C-DG-DG00-OP-PRO-0001
08/02/2020
Rev. Description Originator Review Approved Date
Matthew Pollard
A01 Draft for Comment 08/02/2020
Martin Leckonby
This document is the property of Rumaila Field Development.

It must not be stored, reproduced or disclosed to others without written authorisation from the Company
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ROO Operations
Custody Transfer Metering System - Laboratory Procedures

Revision Description Sheet
Rev Para Revision Description

A01 Issue for Comment
Hold No Section Description of Hold

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ROO Operations
CONTENTS
1.0 INTRODUCTION ........................................................................................................... 5
1.1 Background ...................................................................................................................................... 5
1.2 Responsibilities ................................................................................................................................ 5
1.3 Requirements .................................................................................................................................. 5
2.0 LABORATORY GUIDELINES ...................................................................................... 6

2.1 General ............................................................................................................................................ 6
2.2 HSE.................................................................................................................................................. 6
2.2.1 Hazards........................................................................................................................................ 6
2.2.2 Access ......................................................................................................................................... 6
2.2.3 Storage ........................................................................................................................................ 6
2.2.4 Equipment and Procedures ......................................................................................................... 6
2.2.5 Personal Protective Equipment ................................................................................................... 7
2.2.6 Maintenance ................................................................................................................................ 7
2.2.7 Cleaning and Housekeeping........................................................................................................ 7
2.2.8 Record Keeping ........................................................................................................................... 7
2.2.9 Training and Supervision ............................................................................................................. 8
3.0 LABORATORY PROCEDURES .................................................................................. 9

3.1 Laboratory Equipment ................................................................................................................. 9
3.2 Sample Identification ................................................................................................................... 9
3.3 Analysis Requirements ................................................................................................................ 9
3.3.1 Density Measurement .................................................................................................................. 9
3.3.2 Salt Content ................................................................................................................................. 9
3.3.3 Base Sediment & Water (BS&W) .............................................................................................. 10
3.3.4 Water Content ........................................................................................................................... 10
3.3.4 Sediment by Extraction ............................................................................................................. 10
3.4 Traceability................................................................................................................................. 10
3.5 Sample and Analysis Reporting ................................................................................................ 11
3.6 Record Keeping ......................................................................................................................... 11
3.7 Loss of Sample .......................................................................................................................... 11
3.8 Discrepancies ............................................................................................................................ 12
4.0 SAMPLING EQUIPMENT ........................................................................................... 13

4.1 Jet-Mix Pump ................................................................................................................................. 13
4.2 Automatic Sampler ........................................................................................................................ 13
4.3 Sample Probe & Mixing Nozzle ..................................................................................................... 13

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4.4 Sample Controller .......................................................................................................................... 13
4.5 Sample Receivers .......................................................................................................................... 13
4.6 Can Weighing Equipment .............................................................................................................. 14
4.7 Water in Oil Monitor ....................................................................................................................... 14
4.8 Manual Sampling ........................................................................................................................... 14
4.9 Composite Sample – Sediment Analysis....................................................................................... 14
5.0 STANDARD TEST PROCEDURES ........................................................................... 15

5.1 Index .............................................................................................................................................. 15
5.1.1 Metering System Sample Handling ........................................................................................... 16
5.1.2 Composite Samples................................................................................................................... 18
5.1.3 Determination of Density using Digital Density Analyser .......................................................... 20
5.1.4 Salt in Crude Oil by the Electrometric Method........................................................................... 22
5.1.5 Water and Sediment in Crude Oil by the Centrifuge Method .................................................... 26
5.1.6 Water in Crude using Coulometric Karl Fischer Titration .......................................................... 29
5.1.7 Sediment in Crude Oils and Fuel Oils by the Extraction Method .............................................. 32
5.1.8 Sample Cylinder Cleaning Procedure ....................................................................................... 39

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1.0 INTRODUCTION
1.1 Background
This document defines the activities necessary to ensure the laboratories on Rumaila are operated in
compliance with all relevant measurement and laboratory standards. It also details the standard test
procedures and equipment required to analyse metering system representative samples to ensure all
contractual obligations are being fulfilled.
1.2 Responsibilities
Responsibility for overseeing Laboratory activities are performed in accordance with the appropriate
standards lies with North and South Laboratory Managers.
It is also the responsibility of the Laboratory Manager to ensure sample integrity is maintained during
transit. These activities should be co-ordinated with the ROO Metering Department. Laboratory results
will be distributed to the required personnel on completion of tests.
The Metering Department will be responsible for all sampling activities and sample handling that take
place at the metering stations.
1.3 Requirements
It is a requirement that the crude oil produced at Rumaila is analysed to ensure that the quality is within
best industry standards limits. Quality measurements are based on samples that are collected at the
Metering Stations either, manually or automatically, using equipment and procedures that have been
highly scrutinised, tested and documented within the global industry standard communities.
It is important that the same analytical procedures are employed by both ROO and BOC to ensure
analysis results are as coincident as possible within the limits of experimental/analytical error [as
discussed in the respective standardised methods in section 5 of this document].
It is a ROO requirement that the laboratory is operated safely by suitably qualified personnel and that all
waste is disposed of in an environmentally responsible manner and that equipment is maintained to an
acceptable standard.

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2.0 LABORATORY GUIDELINES
2.1 General
Good standard laboratory practices are essential when handling and testing crude oil samples for
custody transfer measurement purposes. All personnel involved in the measurement system shall be
fully aware of the importance of representative sampling and sample handling. All measurement system
components are maintained to very specific standards and the laboratory quality measurements should
be no different.
These guidelines shall make the laboratory personnel aware of the steps required to maintain sample
integrity and produce repeatable, accurate results for every test.
2.2 HSE
It is the responsibility of the ROO Laboratory Manager to ensure that all personnel involved with
sampling and analysis of crude oils are aware of the hazards and controls. Significant risks to
personnel and equipment are likely if good laboratory practices are not followed.
2.2.1 Hazards
Laboratory personnel must be aware of the following:
 Hazards from chemicals and process fluids that are handled in the laboratory. MSDS
(Material Safety Data Sheets) for each chemical to be available in each laboratory.
 Health risks and COSHH (Control of Substances Hazardous to Health) procedures
 Workplace exposure limits for the process fluids, chemicals and reagents handled in the
laboratory
 Hot solvent [increased fire risk].
2.2.2 Access
 Access to the laboratory, during day to day operations should be restricted to authorised
personnel only
 The laboratory and store should be secured when not occupied
 Locate the work away from doors and walkways to prevent draughts interfering with tests
2.2.3 Storage
 The laboratory store should be well organised, well lit, well ventilated and have sufficient
storage space
 Laboratory should provide eyewash equipment close to the worksite
 Segregate incompatible materials and segregate waste.
 Provide suitable fire extinguishing equipment.
2.2.4 Equipment and Procedures
Control Equipment
Lab controls include:
 A fume cupboard. The cupboard should have a sash and be deep enough to contain all
equipment and chemicals. The extract from the cupboard shall be routed to a safe location
and will include extract filters will be installed to prevent discharge of contaminants. A flow
indicator should be used to show that extraction is working correctly.
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 The laboratory shall always have a good standard of natural ventilation.

 The laboratory will always have measured-volume dispensers to avoid pouring chemicals
or reagents.
Control Procedures
 All work with hazardous substances shall be done in the fume cupboard.
 All samples for degassing shall be stored in the fume cupboard with the cap removed
 Cupboard sash should always be positioned at the right height to allow sufficient airflow
and a restriction on opening.
 All waste chemicals shall be kept in a labelled waste bottle stored in the fume cupboard.
Waste chemicals or reagents should not be poured down sinks or into drains.
 Ensure fire extinguishers are available and functional.
2.2.5 Personal Protective Equipment
 Eye protection shall be worn for all laboratory and analysis work
 Single-use nitrile or PVC gloves shall be worn during sampling activities and will be
discarded at the end of each task.
2.2.6 Maintenance
The following routine maintenance of control equipment will be carried out by appropriate
laboratory personnel.
 Visual inspection of control equipment before starting analysis

 Airflow indicators on the fume cupboard should be checked on a weekly basis using an
anemometer.
Maintenance activities shall be recorded in the laboratory logbook.
2.2.7 Cleaning and Housekeeping
The laboratory will be kept clean and tidy at all times.
Waste
 Solvent wastes will be collected separately for safe disposal
 Oil samples and hydrocarbon waste will be disposed in an ‘oily waste’ container
 Needles, broken glass etc. shall be stored in a ‘sharps’ container for safe disposal.
All laboratory waste will be disposed in a safe and environmentally friendly manner in accordance
with ROO procedures.
2.2.8 Record Keeping
Each Laboratory in the Rumaila Concession shall maintain a logbook, to record daily activities
performed in the Laboratory. These shall include but not be limited to, analytical calibration
records/results, chemical usage, performed analyses and associated results, details of aliquots
taken for future analyses.

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2.2.9 Training and Supervision
 All laboratory personnel shall be suitably trained in the use of laboratory equipment, control
equipment and the appropriate safe work procedures.
 All personnel will be aware of the hazards and risks involved in sampling and analysis of
hazardous chemicals.
 Training records should be kept for laboratory personnel, including competency
assessments which are regularly reviewed.
On-going training will be carried in the form of toolbox talks on:
 How to use equipment properly

 How to check equipment is operating correctly
 Calibration of analysers
 Good record keeping
 How to clean up spills correctly
 What to do if something goes wrong

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3.0 LABORATORY PROCEDURES
3.1 Laboratory Equipment
The ROO Laboratories will utilise the following analysis equipment for export metering system samples:
Analysis Test Method Equipment

Density ASTM D5002 Digital Density Analyser
Salt Content ASTM D3230 Salt in Crude Analyser
Water Content ASTM D4928 Karl Fischer Coulometric Titrator
Base Sediment & Water (BS&W) ASTM D4007 Heated Centrifuge
Extraction apparatus, sample
Sediment by Extraction ASTM D473
thimble and analytical balance
General laboratory equipment; centrifuge, balance, thermometers, glassware etc. will be used as part of
day to day activities.
3.2 Sample Identification
On completion of sampling, the representative sample receiver will be removed from its location within
the metering station quality module and prepared for transportation. The sample receiver should be
transported by road to the laboratory.
Sample receivers should be capped and packed singularly into suitably sturdy transport containers to
prevent damage to the cylinder. The containers should be labelled with the following information and
tracked:
 Place at which the sample was extracted

 Date and at what time sampling was completed
 Sample tag number or serial number of the sample receiver
 Type of fluid being sampled
 Quantity of fluid represented by the sample
 Full name and signature of person responsible for collecting the sample
 Sample volume and cylinder pressure.
 Hazard identification
3.3 Analysis Requirements
Samples from the metering station will be taken on a daily basis and analysed in the laboratory. This
section will detail the analysis requirements such as accuracy, tolerance & frequency.
3.3.1 Density Measurement
Crude oils with a density between 0.75 and 0.95 g/ml that can be handled in a normal fashion as
liquids at test temperatures between 15 and 35°C are best analysed in accordance with ASTM
D5002. Analysis by digital density analyser is the preferred method.
If the analyser result is in doubt the hydrometer method of determining density shall be used to
confirm the result.

3.3.2 Salt Content
The primary salt measurement will be made using a portable Salt in Crude analyser in compliance
with ASTM D3230. This analysis measures total chlorides in crude rather than just Salt measured
by the extraction and titration method. The range of concentration is 0 – 150 PTB, if the sample
concentration is greater than 150 PTB, the sample must be analysed ‘by dilution’ with the Salt in
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Crude analyser OR in accordance with the ASTM D 2547 Method of Determination of Salt by
Extraction method.
In the event that Salt in Crude analyser results are in doubt, the analyser zero point should be
checked using a zero-salt solution. It may be necessary to verify the analyser results against the
extraction method but operators should be aware that the extraction results will almost always be
lower due to the type of measurement.
Note: As a minimum, a ‘blank’ (zero salt) solution test should be carried out daily for each analyser
and on each new batch of mixed alcohols.
3.3.3 Base Sediment & Water (BS&W)
BS&W in % volume will be measured by using the centrifuge method ASTM D4007. Sediment
content in % volume will be determined by subtracting the water content from the BS&W value.
3.3.4 Water Content

Daily oil samples are required to be analysed in the laboratory. The BS&W analysis by centrifuge
shall be performed first to indicate the water content and determine which analysis method is to be
used.
For water content below 5% v/v the Karl Fischer coulometric method shall be used. At Rumaila this
will be done in accordance with ASTM D4928-00. This method is intended for the direct
determination of water content over the range of 0.02 to 5% volume in crude oil, containing less
than 500ppm sulphur as either mercaptan sulphur or ionic sulphur or both.
Tests will be carried out in accordance with best industry practices.
In the event that water content of the sample is above 5% the Karl Fischer method shall not be
used.
Alternative methods such as ASTM D4007 may be used to water content by centrifuge but it
should be noted that the centrifuge method is not preferred as the amount of water detected is
almost always lower than the actual water content.
3.3.4 Sediment by Extraction

Oil samples provided to the laboratory shall have aliquots of equal measure taken on a daily basis
to be used to perform a weekly, Sediment by Extraction analysis. This shall typically be 100mL.
The composite sample shall be then prepared in accordance with best industry practices and
section 4.9, 5.1.1 and 5.1.2 of this procedure.
The Sediment by Extraction analysis shall be performed in accordance with ASTM D473.

3.4 Traceability
To maintain traceability of the laboratory measurements, it is essential to carry out calibrations of the
analysers and equipment in accordance with the manufacturer’s recommendations. Calibrations should
be done at the correct frequency, following recognised calibration procedures using certified reagents.
Laboratory personnel should be suitably trained in the use of the equipment and the appropriate
calibration techniques.

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3.5 Sample and Analysis Reporting
All laboratory results shall be reported as they are obtained. Standard analysis record sheets will be
used as part of normal activities and will include test information detailed in Section 5 of this document.
Sample analysis results will be sent to BOC Measurement Department daily after confirmation of the
results.
3.6 Record Keeping
Laboratory records will be kept containing the following information:
 Test Results
 Laboratory and Test Procedures
 Audit checks
 Analysis equipment calibrations
Sampling and analysis results shall be held on file as a hard copy and stored on the network server
electronically. It is good oilfield practice to keep these records for a minimum of one year available for
annual auditing of the documentation.
Sample result records should include the following:
 Place at which the sample was drawn

 Date and time at which sampling commenced
 Date and time sampling was completed
 Quantity of fluid represented by the sample
 The number of grabs taken by the sampler
 Sample can size
 Sample temperature before / after mixing
 Mixing time. The total mixing period should be recorded.
 All analytical readings inclusive of outliers
 Mean average final result
The reported analysis results should include the following information:
 A unique sample number that can be cross referenced to the sample details and the laboratory
equipment and calibration records.
 Date and time of analysis
 Analysis result.
3.7 Loss of Sample
In the event that sample is not available at the end of the sampling period, it is necessary that a formal
procedure exists that details what actions are required by all parties involved with the metering system
and laboratory.
Loss of sample may be the result of component failure on the sampling system or use of incorrect
procedures. Loss of sample does not necessarily mean that no sample has been collected; it may mean
that the sample is unrepresentative of the exported fluids during the sample period.
If the reason for the sample loop shut down is for routine maintenance, i.e. 6m air check of the density
transducer, the maintenance department should pre-warn BOC and make them aware that
representative sampling for the period shall not be possible.
If the shutdown duration is known and is not expected to last more than 24 hours, it may be prudent to
use an average of previous day analysis results and the day following shutdown.

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The length of the sample system shutdown will determine whether the average values method can be
used.
If the routine shutdown is expected to last for over 24 hours, it may be necessary to carry out manual
sampling. Manual sampling is covered in Section 4.8 of this document. BOC measurement department
to be informed of any problem with the sampling system and manual sampling operations.
3.8 Discrepancies
A back-up sample should be taken daily and kept in the lab for a period of one week. In the event of
discrepancies with the analysis results the back-up sample should be analysed at the ROO laboratory
and witnessed by ROO, BOC and, if available, 3rd party lab representatives.
Any unusual or unexpected results should be flagged and re-sampled and / or re-analysed.

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4.0 SAMPLING EQUIPMENT
The quality system is designed to produce a representative automatic sample in accordance with ISO
3171. The main sample loop component and their functions within the system are detailed below.
4.1 Jet-Mix Pump
The jet-mix pump is connected to the sample spool inlet and outlet connections and is used to mix
export fluids to create a sample representative of all exports. A centrifugal pump is driven by an electric
motor and the fluids are recirculated back into the sample spool where mixing is achieved, mixing is
considered representative when the velocity through the sample loop has a velocity between 40 and
200% of the main line velocity, these are considered iso-kinetic conditions and are a requirement of
automatic sampling standards such as ISO 3171.
The inlet to the pump is protected from large pieces of debris by an inline filter that is monitored for
blockages using a differential pressure transmitter. Flow through the sample loop should always be
greater than 3.5m3/hr, below this a low flow alarms will be initiated that will prevent sampling.
4.2 Automatic Sampler
Automatic grab samplers are installed, designed to grab 1cc with every operation. The frequency of the
grabs is determined by the total measured flow through the skid but the grab size will not vary. Sampler
is operated with instrument air actuated by a Solenoid Valve. Back pressure is kept on the sample with
the use of a back pressure control valve.
4.3 Sample Probe & Mixing Nozzle
Sample from the fast loop is injected at the upstream sampling point on the sample spool. The mixing
nozzle is designed to inject the sample loop flow back into the line in such a way that any stratified
water at the bottom of the line is agitated and mixed with line fluids. The sample probe is the inlet to the
sampling system and this is located downstream of the mixing nozzle.
4.4 Sample Controller
Grab sampling shall be carried out in flow proportional mode. The metering control system calculates
the required grab frequency from the system flowrate and sends a 0.5 second pulse to the automatic
sample solenoid valve. Maximum sample rate is 1 grab per second.
It is the responsibility of the operations department to ensure the correct sampler settings are entered
prior to starting the sampler.
In addition to calculating grab rate, the metering control system also controls automatic can changeover
using analogue and digital signals from the can weighing equipment. Sample receiver ‘A’ or ‘B’ can be
manually selected by the operator but will not start to fill unless certain interlocks have been met, i.e. a
can is in place and it is less than 80% full.
4.5 Sample Receivers
At each station two [2] 20 litre sample receivers are installed. Hard piped connections transmit the
sampler to the receiver through the change-over equipment. The sample receivers are installed directly
under the grab sampler to enable the downward flow of crude into the receiver and to avoid liquid traps.

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4.6 Can Weighing Equipment
Each sample can has a load cell that produces an analogue 4-20mA output. The system is used to
detect when the empty cans are in position and the actual sample collected. The collected volume will
be compared to the number of grabs taken and used to monitor long term performance of the grab
sampler.
4.7 Water in Oil Monitor
A Low-Cut Phase Dynamics water in oil monitor is installed on the sample loop. The water in oil monitor
uses microwaves to detect water in oil content and the analyser produces a continuous 4-20mA output
to the measurement system so that Net totals can be calculated. The analyser accuracy is ±1.0% and
its results should only be used for indication.
4.8 Manual Sampling
Manual sampling should be carried out at a point in the process that is known to provide a fully
homogenised sample, preferably from the centre 1/3 of the line and in accordance with the manual
sampling standards such as ISO 3170. The Quality Module which is part of the Metering Station
conforms to these requirements.
If the Auto Sampler is offline but the quality module sample loop pump is still online and operational, the
manual sample shall be taken from the manual sampling point inside the Quality Module cabinet into the
standard Auto Sampler Cylinder.
If the Auto-Sampler is offline and the quality module sample pump is offline, the Laboratory Manager
shall be informed and the manual sample shall be taken by the Laboratory Technician from the ‘Main
Export Line’ sample point.
In the event of an auto sampler failure, manual samples will be taken every 4 hours.
 Metering Station Operator is to inform the Metering Superintendent immediately when a problem is
discovered.
 Metering Superintendent to inform ROO Metering Engineer immediately.
 Metering Station Operator to begin filling sample can manually “ONLY IF” the sample pump is
running.
 Standard Laboratory handling and preparation of the sample shall be adhered to.
 Procedures to include:
o Section 3.3.1 Density using Digital Density Analyser
o Section 3.3.2 SiC Analysis
o Section 3.3.3 Water Cut by Karl Fischer
o Section 3.3.4 BS&W by centrifuge
o Section 3.3.5 Sediment by Extraction
 Lab Tech to fill in analysis results form.
4.9 Composite Sample – Sediment Analysis
Sediment analysis shall be performed as standard on a weekly basis, utilising a composite sample
made up from the previous 7 days.
During each of the 7 previous days, a sample shall be prepared as per section 5.1.1. and an aliquot of
typically 100mL withdrawn for storage.
Each of the 7 day’s worth of samples used to make the composite weekly sample for sediment analysis,
shall be clearly marked with the date, degassing station and be of equal volume.
The composite sample shall then be prepared as per section 5.1.1 and 5.1.2, ready for analysis.
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5.0 STANDARD TEST PROCEDURES
5.1 Index
5.1.1 MET-LP-001 – Metering System Sample Handling

5.1.2 MET-LP-002 – Composite Samples and Analysis
5.1.3 MET-LP-003 – Determination of Density using Digital Density Analyser
5.1.4 MET-LP-004 – Salt in Crude Oil by the Electrometric Method
5.1.5 MET-LP-005 – Water & Sediment in Crude Oil by the Centrifuge Method
5.1.6 MET-LP-006 – Water in Crude Oil using Coulometric Karl Fischer Titration
5.1.7 MET-LP-007 – Sediment by Extraction
5.1.8 MET-LP-008 – Sample Cylinder Cleaning Procedure

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5.1.1 Metering System Sample Handling
Title: Metering System Sample Handling
Document Number: MET-LP-001
Revision: Rev 0
Frequency: Daily
Applies to: Rumaila Metering Station

Rumaila Laboratory
Equipment & Consumables: Transit Cases

Labels
Acceptance Criteria: N/A
Skill Level: Operator
Relevant Standards: Good Laboratory Practices
Reference Documents: MET-OP-005 Automatic Sampler Operating Procedure
Responsibility: Operations & Laboratory
1.0 Sample Events
1. Prior to use, sample cylinders shall be cleaned to remove any contaminants that will affect
subsequent samples. This should be done using a suitable solvent followed by drying with
methanol. Refer to Section 5.1.6 of this document for the sample cylinder cleaning procedure.
2. Representative samples of approximately 1 - 2 litres will be supplied to the laboratory daily.
3. On completion of the transfer period the operations personnel will complete the sampler
operations procedure MET-OP-005 and remove the sample receiver. ROO laboratory personnel
should witness removal of the sample receiver.
4. The sample receiver should be placed into a suitable transit case.
5. Sample should be labelled in accordance with Section 2.5 of this procedure.
6. Sample should be transported to the assigned degassing station laboratory.
7. Delivery shall be witnessed by the ROO Assistant Technician Manager as well as a

representative from BOC.
8. The sample receiver shall be inspected for damage and any signs of leakage since removal from
the metering station.
9. When all parties have confirmed sample integrity has been maintained, the sample receiver
should be placed in the sample cylinder mixing bench. Inlet and outlet quick connect fittings
should be fitted.
10. Sample mix pump should be run for approximately 15 mins to ensure the sample is
homogenous, and then extracted into two containers using the correct attachments.

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11. Back up samples shall be drawn off into suitable storage containers, labelled and stored in the
ROO lab for a period of 1 week in case of discrepancy in the analysis results.

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5.1.2 Composite Samples
Title: Composite Samples
Revision: Rev 0
Frequency: As Required
Applies to: Rumaila Laboratory
Equipment & Consumables: See Below

API MPMS 8.3
Reference Documents: MET-OP-005 Automatic Sampler Operating Procedure
Responsibility: Operations & Laboratory
1.0 Introduction
It is preferable that analytical tests be conducted using test specimens that have been drawn directly
from the primary container. However, it is recognised that all sampling methods do not permit this
nor do requirements to transport and store samples.
The number of transfers using intermediate containers between the initial sampling operation and the
analytical test should be minimised as each use of intermediate containers increases the potential for
loss of light hydrocarbons, loss of water or inefficient mixing and contamination of the sample from
external sources.
Before the sample aliquot is transferred from one container to another, a homogeneous mix must be
created and maintained until the transfer is complete, as per Section 5.1.1. [MET-LP-001].
This procedure will detail the apparatus required to create a 7-day composite sample for Sediment
by Extraction analysis.
2.0 Apparatus
Item Description Comment

1 Representative sample as
prepared in Section 5.1.1 of
procedure MET-LP-001
2 Syringes At least 100ml in volume
3 Secondary Containers Adequately prepared secondary containers
clearly marked with sample date and location of
sample.
4 Benchtop insertion For mixing of individual and composite samples
mixer/stirrer/homogeniser

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3.0 Compositing Procedure
1. Prior to use, secondary sample containers shall be cleaned to remove any contaminants that will
affect subsequent samples and analyses. This should be done using a suitable solvent followed
by drying with methanol. Refer to Section 5.1.8 for further guidance.
2. Prepare sample using procedure described in Section 5.1.1 [MET-LP-001].
3. Transfer 100ml sample aliquot to previously prepared secondary sample container.
4. Clearly mark the secondary sample container with the date of the specific production day, the
date which the sample was withdrawn and the Degassing Station which the sample is from.
5. Steps 1 to 4 are to be repeated each day until a total of 7 separate samples are available.
6. When compositing the 7 individual 100ml samples to make a total composite volume of 700ml,
the individual 100ml daily samples are to be individually mixed using a pre-cleaned benchtop
insertion mixer/stirrer/homogeniser to ensure a homogenous solution, then decanted into an
adequately prepared secondary sample container of sufficient volume for the 700ml composite
sample.
7. The 700ml composite sample is then to be mixed using a pre-cleaned benchtop insertion
mixer/stirrer/homogeniser to ensure a homogenous solution, for no longer than 15 minutes.
8. A sample shall then be withdrawn from the homogenous solution, refer to 5.1.7 for further
guidance.

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5.1.3 Determination of Density using Digital Density Analyser
Title: Determination of Density using Digital Density Analyser
Revision: Rev 0
Frequency: Daily

Rumaila Laboratory

ASTM D 5002
Reference Documents:
Responsibility: Laboratory
1.0 Introduction
This procedure will detail the apparatus required to determine the density of crude oil sampled using
a digital density analyser. It will also include step by step instruction for the use of the density
analysis equipment.
2.0 Apparatus

2 Digital Density Analyser Anton Paar 4500M
3 Syringes At least 2ml in volume with adaptor to connect
to the inlet of the analyser
4 Certified Thermometer Calibrated and graduated to 0.1°C
5 Water Redistilled, freshly boiled and cooled reagent
water for use as primary calibration standard
6 Acetone For use flushing and drying the sample tubes
7 n-Nonane, n-tridecane or Pure material that the density is known for
cyclohexane 99% purity calibration of the analyser, see manufacturers
recommendations
3.0 Sampling
The representative contents of the export line are collected in the sample receiver and transported to
the laboratory. Mixing is done to ensure a homogenous sample for analysis. Refer to procedure
MET-LP-001.

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4.0 Calibration
Digital density analyser should be calibrated in accordance with manufacturer’s recommendations.

This should be done when the analyser is first turned on and when the test temperature is changed.
The calibration should be carried out at the same temperature that the density of the sample is to be
measured, therefore it is important that the laboratory temperature is stable and the correct
temperature control equipment is used.
Calibrations should be carried out weekly during routine operation but may be done more frequently
if the calibration and test results are suspect.
Only traceable certified calibration fluids shall be used to adjust analyser constants.
5.0 Test Procedure
1. Calibrate analyser in accordance with manufacturer’s recommendations.

2. Mix sample within the sample mixer and extract using suitable syringe.
3. Introduce around 0.7ml of crude oil into the clean dry sample tube of the density meter. Leave
the syringe in place and plug the exit port.
4. Turn on the illumination light and examine the sample tube carefully for bubbles. Make sure
there is no presence of bubbles and the tube is filled completely.
5. Turn off the light and ensure test temperature remains constant.
6. Allow the sample to stabilise and re-check for bubbles in the sample tube. If bubbles cannot
be seen verify the analyser readings are stable, air bubbles will cause instability.
7. If stable readings are not observed after a few minutes, then repeat the injection with a new
sample into the tube.
8. After the instrument displays a steady reading to four significant figures for density and T-
value. Record the final result.
9. Flush and dry the sample tube and check the analyser reading in air prior to introducing
another sample
10. If the test result is suspected, a second test should be carried out to verify repeatability.
Repeatability is the difference between successive test results obtained by the same operator
with the same equipment testing the same sample. Repeatability limits should not exceed the
value in the table below more than 1 test in 20.
11. The results should be compared against the BOC result to verify reproducibility.
Reproducibility is the difference between two single and independent results, obtained by
different operators working in different laboratories on identical test sample using the same
test method. Reproducibility should not exceed the value in the table below more than 1 test in
20.
Extract from ASTM 5002.
12. Results for density should include units and test temperature.
e.g. density at 15°C = 0.8549 g/ml or 854.9 kg/m3

API gravity at 60°F = 35.25

Page 21 of 40

ROO Operations
5.1.4 Salt in Crude Oil by the Electrometric Method
Title: Salt in Crude Oil by the Electrometric Method
Revision: Rev 0
Frequency: Daily

Rumaila Laboratory

ASTM D 3230
ASTM D 2547 IP77 Determination of Salt by Dual Extraction
1.0 Introduction
This procedure will detail the apparatus and test method required to determine salt in crude oil
sampled at the Metering Station using the electrometric method.
2.0 Limitations
The reference test method is ASTM D 3230. The standard covers the determination of the
approximate chloride (salts0 concentration in crude oil. The range of concentration covered is 0 to
500 mg/kg or 0 to 150 lb/1000bbl (PTB) as chloride concentration / volume of oil.
If Salt content is found to be greater than 150 PTB the sample shall be analysed ‘by dilution’ using
the Salt in Crude analyser or ASTM D 2547 Method of Determination of Salt by Extraction Method.
The test method uses conductivity in the crude oil due to the presence of common chlorides, such as
sodium, calcium and magnesium. Other conductive materials may be present in the crude oil.
3.0 Sampling
The representative contents of the export line is collected in the sample receiver and transported to
MET-LP-001.

Page 22 of 40

ROO Operations
4.0 Apparatus

1 Electrometric Chloride Apparatus See ASTM D 3230 Annex A1 (A1.1)
2 Test Cell Components See ASTM D 3230 Annex A1 (A1.2)
3 Test Beaker See ASTM D 3230 Annex A1 (A1.2.1)
4 10 mL Pipette
5 10 mL graduated cylinder
6 100 ml Cylinders With stoppers
7 General laboratory glassware Volumetric and graduated pipettes and
volumetric flasks
8 Water Reagent grade water
9 Mixed alcohol solvent 63 volumes of l-butanol
37 volumes of absolute methyl alcohol
3 mL of water per Litre of above mixture
10 Calcium Chloride Solution Transfer 1.00 ±0.01g of CaCl2 into a 100mL
volumetric flask and dissolve in 25mL water.
Dilute to the mark with mixed alcohol solvent.
11 Magnesium Chloride Solution Transfer 1.00 ±0.01g of MgCl2 into a 100mL
12 Sodium Chloride Solution Transfer 1.00 ±0.01g of NaCl2 into a 100mL
13 Refined Neutral Oil (Paraffin) Any refined chloride free oil of approximately 20
cSt viscosity at 40°C and free of additives.
Paraffin will be used for this method.
14 Mixed Salts Solution Combine 10.0mL of the CaCl2 solution, 20mL of
Concentrated the MgCl2 solution, and 70mL of the NaCl
solution, mix thoroughly.
15 Mixed Salts Solution Transfer 10mL of the concentrated mixed
Diluted chlorides solution into a 1000ml volumetric
flask, and dilute to the mark with mixed alcohol
solvent.
16 Xylene Reagent grade
5.0 Preparation
1 Install apparatus on a flat surface in accordance with manufacturer’s recommendations.
2 Prepare analyser for operation in accordance with manufacturer’s instructions for calibrating,
checking, and operating.
3. Thoroughly clean and dry all parts of the test beaker, the electrodes, and its accessories
before starting the test, being sure to remove any solvent that had been used to clean the
apparatus.

Page 23 of 40

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6.0 Calibration
1. Conductivity of solutions is affected by the temperature of the sample when measurements

are made. The temperature of the test sample at the time of measurement shall be within
3°C of the temperature at which the calibration curves were made.
2. Set up a blank measurement. Into a dry, 100mL graduated, glass stoppered mixing cylinder,
add 15mL of xylene. From a 10mL pipet (total delivery) or 10mL graduated cylinder, add 10mL
of paraffin. Rinse the 10mL pipet or graduated cylinder with xylene until free of oil. Make up to
50mL with xylene. Stopper and shake cylinder vigorously for approximately 60s to effect
solution. Dilute to 100mL with mixed alcohol solvent. Again, shake cylinder vigorously for
approximately 30 seconds to affect the solution, and allow to stand for 5 mins. Pour solution
into a dry 100ml beaker.
3. Place electrodes into the solution. When electrode current is greater than 0.25mA at 125Vac,
water or another conductive impurity is present and its source must be found and eliminated
before calibration can be completed. Determine a blank measurement each time fresh xylene
or mixed solvent is used.
4. Prior to calibration, set up the test in the same way as the blank measurement. Before adding
mixed solvents, add a quantity of dilute mixed salts solution, in accordance with table 1, below.
Quantity to be added should be appropriate to the range of salt contents in the crude.
Complete the calibration fluid set-up in accordance with step 2.
5. Immediately place electrodes into the solution in the beaker, making sure the upper edge of
the electrode plates is below the surface of the solution. Adjust indicated electrode voltage to a
series of values. At each voltage note current reading and record the voltage displayed and
current to the nearest 0.01mA. Remove electrodes from the solution, rinse with xylene, and
allow them to dry.
6. Repeat procedure in sections 4 & 5, using other volumes of mixed salts solution as needed to
cover range of chloride contents of interest.
7. Subtract value obtained for the blank measurement from the indicated current readings of
each standard sample, and plot chloride content readings against net current readings for
each voltage on log paper or in a spreadsheet.
Completed calibration sheets to be provided to BOC.

Page 24 of 40

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7.0 Test Procedure
1. To a dry, 100mL graduated, glass stoppered cylinder, add 15mL of xylene and, using the
same type of volume transferring device used for calibration, 10mL pipette or 10mL graduated
flask, transfer a 10mL sample of the crude oil into the 100mL cylinder. Rinse the 10mL pipette
or graduated cylinder with xylene until free of oil. Make up to 50mL with xylene. Stopper and
shake the cylinder vigorously for approximately 60 s. Dilute to 100ml with mixed alcohol
solvent, and again shake vigorously for approximately 30s. After allowing the solution to stand
for approximately 5 min, pour into a dry test beaker.
2. Immediately place the electrodes into the solution in the beaker, making sure the upper edge
of the electrode plates is below the surface of the solution. Adjust the indicated electrode
voltage to a series of values. At each voltage note the current reading and record voltage
displayed and current to the nearest 0.01mA. Remove electrodes from the solution, rinse with
xylene and allow them to dry.
3. Subtract value obtained for the blank measurement from the test measurement to obtain the
net current reading. From the calibration graph, read the indicated salt concentration
corresponding to the net current (mA) reading of the sample.
4. Report the following information: Concentration in PTB as electrometric chloride in crude per
Test Method ASTM D 3230.
5. If the test result is suspected, a second test should be carried out to verify repeatability.
value below more than 1 test in 20.
r = repeatability
X = the average of two test results in mg/kg
Y = the average of two test results in lb/1000bbl (PTB)
6. ROO results should be compared against the BOC result to verify reproducibility.
test method. Reproducibility should not exceed the value below more than 1 test in 20.
0.75
R (mg/kg) = 2.7803 X
0.75
R (lb/1000bbl) = 2.069 Y
R = reproducibility
X = the average of two test results in mg/kg
Y = the average of two test results in lb/1000bbl (PTB)

Page 25 of 40

ROO Operations
5.1.5 Water and Sediment in Crude Oil by the Centrifuge Method
Title: Water and Sediment in Crude Oil by the Centrifuge Method
Revision: Rev 0
Frequency: Daily

Rumaila Laboratory

ASTM D 4007

1.0 Introduction
This procedure will detail the apparatus and test method required to determine the sediment and
water content of crude oil by the centrifuge method.
Note: This analysis method is to be completed prior to the Karl Fischer (MET-LP-005) analysis to
give an indication of the water content to ensure it is within the limits of the KF Analyser.
2.0 Apparatus

1 Representative sample as prepared
in Section 5.1.1 of procedure MET-
LP-001
2 Centrifuge
3 Circulating Constant Temperature
Bath
4 100ml ASTM Centrifuge Tubes 203mm Tube length.
5 Water Saturated Toluene
6 Demulsifier Chemical
3.0 Sampling
MET-LP-001.

Page 26 of 40

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4.0 Procedure
1. Ensure sample is thoroughly mixed, if the sample is not mixed, analysis results will be
inconsistent and unreliable.
2. Fill two centrifuge tubes to 50ml with sample directly from sample container. No other means
of measurement should be used.
3. With a pipette, add 50ml of water saturated toluene. Read the TOP of the meniscus at both 50
and 100ml marks. If volumes are not exact the results will have errors.
4. Add 0.2 ml of demulsifer solution to each tube. Stopper tubes tightly and invert tubes 10 times
to ensure oil and solvent are mixed.
5. Loosen stoppers and slightly immerse tubes to the 100ml mark for at least 15 mins in the
water bath maintained at 60°C ± 3°C. Secure stoppers again and invert tubes 10 times to
ensure adequate mixing.
6. Place tubes in trunnion cups on opposite sides of the centrifuge. Retighten stoppers and spin
for 10 mins at a minimum relative centrifugal force of 600, approximately 1500 rpm.
7. Immediately after the centrifuge comes to rest, read combined volume of water and sediment
at the bottom of each test tube to nearest 0.05ml (from 0.1 - 1ml) and to nearest 1ml above
1ml graduations. Below 0.1 ml estimate to nearest 0.025 ml. See Figure 2 for procedure for
reading the sediment and water level in the tube.
8. Return tubes without mixing to the centrifuge and spin for another 10 mins at the same rate.
9. Repeat this operation until combined volume of water and sediment remains constant for two
consecutive readings. Normally not more than 2 spinnings are required.
10. Sample temperature during the entire procedure should be maintained at 60°C ±3°C.
11. Add results from the 2 tubes and express as percent by volume of water and sediment.
12. Trace will only be reported if no visible water and sediment is visible in both tubes.
5.0 Water Saturation Procedure
Toluene, as received is relatively dry and if used in as received condition, will dissolve a portion of or
even all of any water present in the crude oil sample. This will reduce sediment and water level in the
sample. To determine water and sediment accurately by centrifuge on a crude oil sample, the
toluene must first be saturated at centrifuge test temperature.
1. Adjust the water bath to 60°C ±3°C.
2. Fill a glass bottle with 700-800 mL of toluene. Add 25mL water. Screw cap on bottle and
shake vigorously for 30 seconds.
3. Loosen cap and place bottle in the water bath for 30 mins. Remove bottle, tighten cap and
shake cautiously for 30 secs.
4. Repeat step 3, three times.
5. Allow bottle with water toluene mixture to sit in the water bath for 48hours before using.

Page 27 of 40

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Page 28 of 40

ROO Operations
5.1.6 Water in Crude using Coulometric Karl Fischer Titration
Title: Water in Crude using Coulometric Karl Fischer Titration
Revision: Rev 0
Frequency: Daily

Rumaila Laboratory

ASTM D 4928
1.0 Introduction
This procedure will detail the apparatus and test method required to determine water content of the
crude oil sampled using the coulometric Karl Fischer titration method.
Note: This analysis method is to be completed after the BS&W (MET-LP-005 Centrifuge) so that the
water content can be determined to ensure it is within the limitations of the KF Analyser.
2.0 Limitations
Coulometric Karl Fischer titration in accordance with ASTM D 4928 covers measurement of water in
the range from 0.02 to 5 volume %.
Mercaptan (RSH) and sulphide (S¯ or H2S) as sulphur are known to interfere with this test method,
but at levels of less than 500 ppm, the interference from these compounds is insignificant.
Note: If the BS&W analysis (MET-LP-004) shows water content greater than 5% then the KF
analysis method is not to be used.
3.0 Sampling
MET-LP-001.

Page 29 of 40

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4.0 Apparatus

2 Karl Fischer Titration Analyser
3 Syringes Glass syringes preferred with LUER fittings and
hypodermic needles.
10µL (0.1µL graduations)
250µL, 500µL and 1000µL for samples
(5µL, 10µL & 20µL graduations)
4 Water Type IV Reagent grade water
5 Xylene Reagent grade Xylene (< than 0.05% water)
6 Karl Fischer Reagents Reagents to be replaced weekly or when
required. Expiry dates to be monitored.
Reagent pack consists of 1 x 100ml bottle
anode solution. 1 x 5ml ampule of cathode
solution.
5.0 Preparation of Apparatus
1. Follow manufacturer’s directions for preparation and operation of the titration apparatus.
2. Seal all joints and connections to the vessel to prevent atmospheric moisture from entering the
apparatus.
3. Add to the anode (outer) compartment the contents of 1 x 100ml bottle of anode solution.
4. Add to the cathode (inner) compartment the contents of 1 x 5ml ampule of cathode solution.
5. Turn on analyser and start magnetic stirrer. Allow residual moisture in titration vessel to be
titrated until the end point is reached. Analyser should indicate ‘ready’ on the digital display.
6. Monitor reagent performance by injecting 10µL of pure water. This should be done initially and
every 10 determinations thereafter. If the result is outside 10,000 ±200µg replace both cathode
and anode solutions.
6.0 Test Procedure
1. Calibrate analyser in accordance with manufacturer’s recommendations.
2. From Table 1, select a sample size based on expected water content, %.
3. Starting with a clean dry syringe of suitable capacity, withdraw at least three portions of
sample and discard to waste. Immediately withdraw a further portion of sample, expel any gas
in the syringe, clean the needle with a tissue, and record the volume to the nearest 1 or 10µL
as appropriate.

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4. Insert the needle through the port inlet septum, start the titration, and with the tip of the needle
just below the liquid surface, inject the entire contents of the syringe. After the end point is
reached, record the digital readout on the instrument the micrograms titrated.
5. Calculate the volume % water in crude oil sample as follows:
V1
Water content, volume % = X 100%
V2
V1 = volume of water titrated, µL (same as the µg of water reported by the titrator)
V2 = volume of sample used, µL
6. Report water content to nearest 0.0001% volume %.
7. If test result is suspected, a second test should be carried out to verify repeatability.
value in the table below more than 1 test in 20.
Repeatability r = 0.056 (X^2/3)
X = sample mean from 0.02 to 5 volume %
8. ROO results should be compared against the BOC result to verify reproducibility.
test method. Reproducibility should not exceed the value in the table below more than 1 test in
20.
Reproducibility R = 0.112 (X^2/3)
X = sample mean from 0.02 to 5 volume %
9. Repeatability / Reproducibility Intervals
Extract from ASTM D 4928

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ROO Operations
5.1.7 Sediment in Crude Oils and Fuel Oils by the Extraction Method
Title: Sediment by Extraction Method
Revision: Rev 0
Frequency: Weekly

Rumaila Laboratory

ASTM D-473
Reference Documents: API MPMS 10.1 – Sediment and Water
1.0 Introduction
This procedure will detail the apparatus and test method required to determine the sediment in crude
oil sampled.
2.0 Limitations
Sediment in Crude Oils and Fuel Oils by the Extraction Method in accordance with ASTM D 473
covers measurement of sediment in the range from 0.01 to 0.4 mass %.
3.0 Sampling
The representative contents of the export line are collected in the sample receiver on a daily basis
and transported to the laboratory. Mixing is done to ensure a homogenous sample for analysis. Refer
to procedure MET-LP-001.
For each of the single days which are combined to produce the 7-day weekly composite sample for
analysis, 100ml aliquots shall be withdrawn, clearly marked and held at the laboratory. Only on the
day of analysis for Sediment by Extraction, shall the 7 aliquots be combined and mixed in
accordance with MET-LP-002. This is to allow potentially erroneous samples to be omitted so as not
to incorrectly bias the analysis.

Page 32 of 40

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4.0 Apparatus

1 Representative sample as prepared in
Section 5.1.1 of procedure MET-LP-001
2 Extraction Flask Wide-neck (Erlenmeyer) flask of 1-L
capacity, with a minimum external neck
diameter of 50 mm.
3 Condenser Condenser in the form of a metal coil
approx. 25 mm in diameter and 50 mm
in length attached to, and with the ends
projecting through, a lid of sufficient
diameter to cover the neck of the flask
as shown in Fig. 1. The coil shall be
made from stainless steel, tin, tin-plated
copper, or tin-plated brass tubing having
an outside diameter of 5 to 8 mm and a
wall thickness of 1.5 mm. If constructed
of tin-plated copper or brass, the tin
coating shall have a minimum thickness
of 0.075 mm. The exposed surface of
the coil for cooling purposes is about
115 cm2.
4 Extraction Thimble Extraction thimble shall be of a
refractory porous material, pore size
20.0 to 30.0 μm (certified by the
manufacturer), 25 mm in diameter by 70
mm in height, weighing not less than 15
g and not more than 17 g. Suspend the
thimble from the condenser coil by
means of a basket so that it hangs
approx. midway between the surface of
the extracting solvent and the bottom of
the condenser coil.
5 Thimble Basket The thimble basket shall be corrosion-
resistant, shall be made of platinum,
stainless steel, nickel-chromium alloy, or
similar material, and shall meet the
design and dimension requirements in
Fig. 2.
6 Water Cup Use a water cup when testing a sample
determined to have a water content
greater than 10 % volume
(see Fig. 1, Apparatus B). The cup shall
be made of glass, conical in shape,
approximately 20 mm in diameter and
25 mm deep, and have a capacity of
approximately 3 mL. A glass hook fused
on the rim at one side is so shaped that
when hung on the condenser the cup
hangs with its rim reasonably level. In
this procedure, suspend the thimble
basket as shown in Fig. 1, Apparatus A
by means of the corrosion-resistant wire
looped over the bottom of the condenser
coil and attached to the basket supports,
or as in Fig. 1, Apparatus B, where the
wire supports of the basket are attached
to hooks soldered to the underside of
the condenser lid.

Page 33 of 40

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7 Heat Source Use a source of heat, preferably a hot

plate operated under a ventilated hood,
suitable for vaporizing toluene
(Warning—Flammable.)
8 Analytical balance Use an analytical balance, with an
accuracy of 0.1 mg. Verify the balance,
at least annually, against weights
traceable to a national standards body.
9 Non-aerating Mixer Use a non-aerating mixer, meeting the
verification of mixing efficiency
requirements specified in Practice D
5854 (API Chapter 8.3). Either insertion
mixers or circulating mixers or
circulating external mixers are
acceptable provided they meet the
criteria in Practice D 5854 (API Chapter
8.3).
10 Oven Use an oven capable of maintaining a
temperature
of 115 to 120°C (240 to 250°F).
11 Cooling Vessel Use a desiccator without desiccant as a
cooling vessel.
12 Thermometer Use a thermometer capable of
measuring the temperature of the
sample to the nearest 1°C (2°F).

Page 34 of 40

ROO Operations
Fig. 1 Extraction Apparatus for Determination of Sediment

Page 35 of 40

ROO Operations
Fig. 2 Basket Thimble Support

Page 36 of 40

ROO Operations
6.0 Preparation of Apparatus
1. For referee tests, use a new extraction thimble prepared in accordance with Step 2 below. For
routine tests, thimbles may be reused. When reusing thimbles, the extraction to constant mass
for one determination should be considered as the preliminary extraction for the succeeding
determination. After several determinations (the accumulated sediment may be sufficient to
interfere with further determinations), follow the procedure described in Step 3 to remove the
combustible portion of the accumulated sediment. Avoid excessive reuse of thimbles, as over
time the pores become clogged with inorganic material resulting in falsely high results. When
in doubt regarding a higher than normal result, discard the thimble and retest using a new
thimble.
2. Preparation of a New Thimble - Rub the outside surface with fine sandpaper and remove all
loosened material with a stiff brush. Give the thimble a preliminary extraction with the toluene,
allowing the solvent to drip from the thimble for at least 60 minutes. Then dry the thimble for
60 minutes at a temperature of 115 to 120°C (240 to 250°F); cool in a cooling vessel, for 60
minutes and weigh to the nearest 0.1 mg. Repeat the extraction until the masses of the
thimble after two successive extractions do not differ by more than 0.2 mg.
3. Preparation of a Used Thimble - Remove the combustible portion of the accumulated

sediment by heating the thimble to a dull red heat for 20 min (preferably in an electric furnace
maintained at approximately 750°C (1380°F)). Subject the thimble to a preliminary extraction
as described in Step 2 before using it for another determination.
7.0 Test Procedure
1. Place an estimated 10-gram test portion of the sample in the thimble immediately after the
sample has been mixed. Do not attempt to adjust this estimated 10-gram portion to any exact
predetermined amount. Weigh the thimble plus test portion to the nearest 0.01 g. Add 150 mL
to 200 mL of toluene to the flask. Place the thimble in the extraction apparatus, place on the
heat source, and extract with the hot toluene for 30 min after the solvent dripping from the
thimble becomes colourless. Ensure that the rate of extraction is such that the surface of the
mixture of oil and toluene in the thimble does not rise higher than to within 20 mm of the top.
2. When testing samples determined to have a water content greater than 10 % volume, use the
assembly shown in Fig. 1, Apparatus B. In this procedure, remove any water in the test portion
as its toluene azeotrope and is collected in the water cup, where it separates as a bottom
layer. The toluene layer overflows into the thimble. If the cup becomes full of water, allow the
apparatus to cool and empty the cup.
3. After the extraction is completed, dry the thimble for 60 minutes at 115 to 120°C (240 to
250°F) in the oven; cool in the cooling vessel, for 60 minutes; and weigh to the nearest 0.1
mg.
4. Repeat the extraction, allowing the solvent to drip from the thimble for at least 60 minutes but
not longer than 75 minutes; dry, cool and weigh the thimble as described in step 6. Repeat this
extraction for further 60-minute periods, if necessary, until the masses of the dried thimble plus
sediment after two successive extractions do not differ by more than 0.2 mg.
5. Calculate the sediment content of the sample as a percentage by mass of the original sample.
Where:
S = sediment content of the sample as a percentage by mass
M1 = mass of the thimble in grams
M2 = mass of the thimble plus test portion in grams
M3 = mass of the thimble plus sediment in grams

Page 37 of 40

ROO Operations
6. Report the sediment content of the sample, as sediment by extraction, as a percentage by

mass, rounded to the nearest 0.01% mass.
7. Test report shall also contain any details necessary for the complete identification of the
product tested; any deviation, by agreement or otherwise, from the procedure specified; and
the date of the test.
8. Report that the sample missing procedure was performed in accordance with the procedures
specified in D 5854 (API Chapter 8.3). Report the temperature of the sample before and after
mixing. If test result is suspected, a second test should be carried out to verify repeatability.
8.0 Precision and Bias
The precision of the test method, as based on mass percent and as obtained by statistical
examination of interlaboratory test results in the range of 0 to 0.4%, is described as follows:
 Repeatability – The difference between successive test results, obtained by the

same operator with the same apparatus under constant operating conditions on
identical test material, would, in the long run, in the normal and correct operation of
the test method exceed the following value in only one case in twenty:
r = 0.017 + 0.255 S
Where:
r = repeatability of the test
S = average result as a percentage by mass, of the values being compared.
 Reproducibility – The difference between two single and independent test results
obtained by different operators working in different laboratories on identical test
material. Would, in the long run, in the normal and correct operation of the test
method, exceed the following value in only one case in twenty:
R = 0.033 + 0.255 S
Where:
R = reproducibility of the test
S = average result as a percentage by mass, of the values being compared.
 Bias – The procedure in this test method has no bias because the value of
sediment can be defined only on terms of the test method.

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ROO Operations
5.1.8 Sample Cylinder Cleaning Procedure
Title: Sample Cylinder Cleaning Procedure
Revision: Rev 0
Frequency: Before cylinders are used / on completion of laboratory testing

Rumaila Laboratory

ASTM D-5854
1.0 Introduction
This procedure will detail the equipment, chemicals and technique required to clean and prepare the
metering system sample cylinders to an acceptable standard prior to use.
2.0 Limitations
N/A
3.0 Apparatus
 Sample Receiver Cylinder

 Cylinder hose connections
 Acetone
 Methanol
 Lint free cloths
 Lab Personnel PPE
4.0 Preparation
On completion of sampling activities, ensure all remaining sample from the cylinder is drained into a
suitable waste container. Cleaning should begin directly after sampling activities to achieve best
results – if cylinders are left for long periods without cleaning it may be necessary to carry out deep
cleaning using more corrosive chemicals to remove built in deposits.

Page 39 of 40

ROO Operations
5.0 Cleaning Procedure
1 The sample cylinder is designed to drain naturally and has polished internal surfaces.
On completion of sampling all remaining liquids should be drained from the cylinder. Care
must be taken to ensure all sediment is removed as this may contaminate future samples.
2 Flush the cylinder with Toluene or Acetone. Dispose of chemicals into the appropriate
waste container. Repeat flushing twice before placing the container in a clean, dry location.
Do not use soap and water to clean as this method may leave contaminants inside the
cylinder.
3 Rinse out with Methanol and leave to dry in air to ensure all moisture is removed from the
receiver.
4 Remove the cylinder cap. Clean the rubber seal with a dry lint free cloth and inspect for
damage.
5 Before the cylinder is used, its condition should be cross checked by a different laboratory
technician.
6 Complete the laboratory logbook with specific sample receiver details; serial number etc

Page 40 of 40

9999RO C DG DG00 OP PRO 0001 A01 Laboratory Operating Procedures

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This document is the property of Rumaila Field Development.

1.2 Responsibilities ................................................................................................................................ 5

1.3 Requirements .................................................................................................................................. 5

2.0 LABORATORY GUIDELINES ...................................................................................... 6

3.0 LABORATORY PROCEDURES .................................................................................. 9

4.0 SAMPLING EQUIPMENT ........................................................................................... 13

4.2 Automatic Sampler ........................................................................................................................ 13

4.3 Sample Probe & Mixing Nozzle ..................................................................................................... 13

4.4 Sample Controller .......................................................................................................................... 13

4.5 Sample Receivers .......................................................................................................................... 13

4.6 Can Weighing Equipment .............................................................................................................. 14

4.7 Water in Oil Monitor ....................................................................................................................... 14

4.8 Manual Sampling ........................................................................................................................... 14

4.9 Composite Sample – Sediment Analysis....................................................................................... 14

5.0 STANDARD TEST PROCEDURES ........................................................................... 15

This document is the property of Rumaila Field Development.

This document is the property of Rumaila Field Development.

2.0 LABORATORY GUIDELINES

Laboratory personnel must be aware of the following:

2.2.4 Equipment and Procedures

Lab controls include:

 The laboratory shall always have a good standard of natural ventilation.

2.2.5 Personal Protective Equipment

 Visual inspection of control equipment before starting analysis

Maintenance activities shall be recorded in the laboratory logbook.

2.2.7 Cleaning and Housekeeping

The laboratory will be kept clean and tidy at all times.

2.2.8 Record Keeping

This document is the property of Rumaila Field Development.

2.2.9 Training and Supervision

On-going training will be carried in the form of toolbox talks on:

 How to use equipment properly

This document is the property of Rumaila Field Development.

3.0 LABORATORY PROCEDURES

3.1 Laboratory Equipment

Analysis Test Method Equipment

3.2 Sample Identification

 Place at which the sample was extracted

3.3 Analysis Requirements

3.3.1 Density Measurement

3.3.3 Base Sediment & Water (BS&W)

3.3.4 Water Content

Tests will be carried out in accordance with best industry practices.

3.3.4 Sediment by Extraction

This document is the property of Rumaila Field Development.

3.5 Sample and Analysis Reporting

3.6 Record Keeping

Laboratory records will be kept containing the following information:

Sample result records should include the following:

 Place at which the sample was drawn

The reported analysis results should include the following information:

3.7 Loss of Sample

This document is the property of Rumaila Field Development.

This document is the property of Rumaila Field Development.

4.0 SAMPLING EQUIPMENT

4.1 Jet-Mix Pump

4.2 Automatic Sampler

4.3 Sample Probe & Mixing Nozzle

4.4 Sample Controller