Schlumberger Dowell Lab Manual | Weighing Scale | Calibration

Schlumberger Dowell

UKI Drilling Fluids Laboratory Testing Field Manual

Prepared by : P. Tomkins (EATC)

Issued :

March 1997

Field Manual Compiled by : M. Sanders (UKI)
Contributions: P. Tomkins (EATC) M. Sanders (UKI) P. Way (SCR) M. Hodder (SRPC-D) Reviewed by: D. Williamson P. Drecq M. Sanders M. Davison

UKI

Revision 2.0 - 1997

Forward The 1997 UKI Drilling Fluids Laboratory Testing Field Manual was based upon on an abbreviated version of the EATC/UKI Laboratory Procedures Manual, Revision 2.0, January 1997. All the procedures have been reviewed for technical content, and altered accordingly to satisfy local UKI requirements. However, if errors or discrepancies are noted please pass your comments back the UKI laboratory in Aberdeen. You can find us on e.mail at “dflab@aberdeen.dowell.slb.com”. This will help improve any future additions. Copies will be supplied with each drilling fluids engineering test kit. Please ensure that they are returned. A copy can also be found in the UKI Lab’s Public folder. All copies will be deemed as being uncontrolled documents.

__________________________

Mark Sanders, UK Laboratory Manager

2

Revision 2.0

Table of Contents :
1 Health and Safety
1.1Introduction 1.2Laboratory Code of Practice 1.3Sample Management 1.3.1 1.3.2 1.3.3 Sample Labelling Sample Storage Waste Disposal 5 5 7

Page 5

7 7 8 9 9 11

1.4Sample Shipping 1.5Dowell Non-Analysis Agreements 1.5Useful HSE Contacts

2

Laboratory Equipment and Chemicals
2.1Introduction 2.2Drilling Fluids Product line & C - Codes (Updated May 1996) 2.3Standard Mud Kit 2.4Summary of Equipment and Chemicals required for Basic Testing 2.5Equipment Calibration and Maintenance 2.5.1 2.5.2 2.5.3 2.5.4 2.5.5 2.5.6 2.5.7 2.5.8 2.5.9 Calibration Records CAL/EAF/001 - Mud Balance CAL/EAF/002 - Pressurised Mud Balance CAL/EAF/003 - HTHP Fluid loss CAL/EAF/004 - Retort CAL/EAF/005 - Fann 35 Rheometer CAL/EAF/006 - OFI Emulsion Stability Meter CAL/EAF/007 - Electronic and Mechanical Balances CAL/EAF/008 - Maintenance of Mixers and Ageing Cells 21 22 23 24 25 26 27 28 29 30 12 12 17 18

3

Laboratory Mixing Procedures
3.1Introduction 3.2Technical Notes 3.3Mixing Procedures 3.3.1 3.3.2 3.3.3 DF/EAF/003 - Low Temperature Water-Based Muds DF/EAF/004 - High Temperature Water-Based Muds DF/EAF/006 - Oil and Synthetic Based Muds 31 32 31

31

32 34 37

3

Revision 2.0

Pore Plugging Apparatus 5.4.3.High Temperature / High Pressure Filtration DFT/EAF/005 .4.pH DFT/EAF/008 .5 4.3Physical Properties 4.3 DFT/EAF/015 .4.1 4.7 DFT/EAF/021 .Back Flow Tester 5.Low Temperature / Low Pressure Filtration DFT/EAF/004 .5 DFT/EAF/019 .3.4.Methylene Blue Test (CEC) for Mud Solids and Shales 5 Non-Routine Laboratory Testing Procedures 5.7 DFT/EAF/007 .4Chemical Properties 4.Mud Weight Determination DFT/EAF/002 .Total Hardness DFT/EAF/011 .6 DFT/EAF/020 .4.4 4.HTHP Rheology .6 4.3 4.Calcium Hardness DFT/EAF/012 .1Introduction 4.4.2 4.3.Fann 70 5.3 4.3.Particle Size Analysis 5.Page 4 Routine Laboratory Testing Procedures 4.0 .2 4.Retort . Oil and Solids DFT/EAF/006 .4 DFT/EAF/016 .1 4.3.Water.2API References 4.Alkalinity DFT/EAF/009 .Chloride DFT/EAF/010 .5 4.2 DFT/EAF/013 .3.1 Introduction 5.Mud Solids Monitor (MSM*) 5.Sand Content 50 50 51 53 55 57 58 60 39 41 41 41 45 46 48 49 39 39 4.4.4 4.Soluble Carbonates DFT/EAF/013 .Fluids Ion Monitor (FIM*) 76 72 73 75 61 61 67 61 * Mark of Schlumberger 4 Revision 2.5 DFT/EAF/001 .Viscosity and Gel Strength DFT/EAF/003 .

2 DRILLING FLUIDS LABORATORY CODE OF PRACTICE ∑ Maintain good housekeeping . 1. SAFE AND ALL TIMES. ∑ Be familiar with Hazard warning labels and MSDS before using a chemical. 1. use pipette fillers provided! ∑ Tirtaions must be performed in fume cupboards." ∑ Make yourself aware of all. OIES. P. ∑ ALL chemicals used in the laboratory must have a corresponding MSDS which can be obtained from."KEEP WORK AREA CLEAN.O. such as rotary mixers or drills. ∑ No trailing hair or clothing such as scarves or ties. All laboratory staff should receive suitable safety training and have a thorough understanding of the relevant legal requirements. always follow the procedure documented in this manual or API 13B to ensure quality control. Box 20. Using these methods of communication one can improve the safety and efficiency of your working environment. The Netherlands ∑ When performing a test or experiment. in many countries the aspects of laboratory activities are governed by specific legislation and every person engaged in laboratory work must be familiar with this. Safe working practices are paramount in this environment. particularly if using equipment with moving parts.Section 1 Health and Safety 1. ∑ No mouth pipetting. ∑ All laboratory analysis requests for the UKI laboratory MUST be recorded and documented in the file provided by either the district or region. DQM (Dowell Quality Management) can be implemented efficiently in the laboratory by using the quality improvement plan (QIP) and risk identification reports (RIR). 4780 AA Moerdijk.1 HEALTH AND SAFETY IN THE LABORATORY INTRODUCTION Safety is a legitimate concern and required function of all Dowell laboratories world-wide. . Henk Romijn. ∑ No food or drink. ∑ No smoking. Emergency exits Eye wash stations First aid boxes NEAT AT ∑ The wearing of safety spectacles is mandatory.

“under pressure”. Always add acid/alkali to water.3) Follow the local disposal procedure for acid/alkali and solvent waste. ∑ Be aware of what to do in the event of a spillage or other accident.3.Section 1 Health and Safety ∑ When handling acids/alkalis/solvents:Use a fume cupboard (if available) Wear gloves Follow storage procedures for segregation of non-compatible materials (See EAF procedure . heavy objects or glassware where they are hard to reach or liable to fall.Section 1. "acid mixing" etc.unlabelled substances present a hazard in themselves. ∑ Clean up spillage promptly and dispose of waste according to local guidelines ∑ Dispose of sharps and broken glass in the appropriate containers. "wet floor". "hot". Rub in “Travabon” skin protection cream and DO NOT use gloves . ∑ Dispose of muds and cements according to the local guidelines. not vice versa ∑ When handling ULTIDRILL base oil:OR Rub in “Stoko Emulsion” skin protection cream (optional) and wear nitrile gloves ∑ Never store hazardous chemicals. ∑ Label all containers and glassware clearly and mark any hazards . ∑ Use kick-step or ladder to reach high shelves or cupboards. never unwrapped in a bin. ∑ Do not lift heavy items alone. ∑ Label any temporary hazards in the lab e.g.

3.2 STORAGE OF SAMPLES Samples must be stored in clearly labelled. airtight containers.3 Health and Safety SAMPLE MANAGEMENT Samples to give to clients.4.) then these storage times can be increased. 1. The biggest single problem is moisture. Solvents and acids must be stored in separate cupboards. Chemical purchasing dept (see introduction). The use of sample numbers which include the year (as described in Section 2. air tight seals. (ii) Samples sent to clients must be clearly marked with the following : Sample name and number Date Hazard warning label Address and phone number of the supplying laboratory. If storage conditions are good (low humidity.Section 1 1. etc. and that the label is securely fixed. the sample number is clearly visible. A MATO ( Material Transfer Order) is required and a small charge may be levied.3. 1. Each laboratory must establish its own sample storage policy. Remember : Always make sure that containers are properly resealed after taking out a sample. Consult the MSDS for details. which in many cases is dictated by the storage space available. it should not be necessary to keep mud or brine samples (from a rig or brine plant) for longer than 3 months or 1 month after completion of the well whichever is most appropriate. Highly corrosive materials must be stored on suitable trays which limit damage caused by accidental spillage. identifies the product or sample name.1 SAMPLE LABELLING All samples used in the laboratory must have the proper hazard warning label. The front of these cupboards must be clearly labelled with the appropriate hazard label. away from direct sunlight and extremes of temperature and humidity. . Make sure that the label. All solvents labelled as highly flammable must be stored in a metal cupboard or bin. As a rule. can be ordered from Pumptech.1) is a very convenient way of identifying old samples for disposal. This affects primarily polymers and salts. The recommended maximum storage times are given in Section 1. or to serve as lab standards. For proprietary Dowell products a non-analysis agreement must be signed by the client or external laboratory prior to sending.

if local authorities permit.g. but check local regulations first. (v) Solvents Collect in sealed metal containers.8. properly labelled. Consult your local HSE representative for disposal instructions. (ii) Oil-based and Synthetic-based muds All oil mud waste must be collected and drummed for return to mud plant or proper disposal (e. Neutralisation is typically performed by adding the acid or alkali to a large volume of water until the pH is measured to be between 6 . should the landfill fail and pollute the groundwater. It will be advantageous to encourage drilling fluids laboratory staff to separate wastes into the following categories: The following general principles apply : (i) Water-based muds Small quantities can normally be disposed of down the drain. Never put oil mud waste down the drain. incineration). as the waste is effectively destroyed and is no longer a liability of the originator. the waste remains the responsibility of the originator. Sodium bicarbonate can also be used to render acidic solutions neutral. who maybe liable for future damage. incineration is to be preferred. (iv) Mud additives Follow the guidance given in the MSDS.3. however. consult your local HSE representative. For larger amounts. consult your local HSE representative.Section 1 Health and Safety 1. or if in doubt. .3 WASTE DISPOSAL Two methods of disposing of waste material are generally available: ∑ ∑ Incineration Landfilling Of the two. If in doubt. In landfills. (vi) Aqueous acids and alkalis Aqueous acids and alkalis may be neutralised and disposed of via the drains. Do not mix different solvents as resulting mixture could be explosive.

O. Non-Analysis agreements may be required when shipping proprietary Dowell products to client or third party testing laboratories. .2) Ensure that an MSDS is included with all chemicals (mandatory in many countries).5 DOWELL NON-ANALYSIS AGREEMENTS A Dowell Non-Analysis agreement must be signed by operator and third party laboratories before any proprietary chemicals are sent out. Whenever samples are sent out from the laboratory. The MSDS for each additive must be supplied also. However. Copies are available from the address shown below : Orders from Europe and Africa: Publications Assistant International Air Transport Association IATA Center 33 Route de l'Aeroport P. The current edition of these regulations is 37 th Edition.4 SAMPLE SHIPPING The UN shipping number for each chemical provides information about the packaging requirements for transportation by air freight. The IATA regulations are revised annually.25 (22) 798-35-53 415586 IATA GENEVA GVATPXB 1. A template of such an agreement is detailed in Figure 1. The chemicals commonly sent out by Drilling Fluids do not have a UN number and therefore are not considered hazardous for shipping. (iii) Check to make sure that the product is safely packaged. check that the packaging is in accordance with published International Air Transport Association (IATA) regulations. some products do have UN numbers and are considered hazardous. Box 672 CH-1215 Geneva 15 Airport Switzerland Tel : Fax : Telex : Cable : Teletype : (22) 799. The current UKI Non-Analysis Agreement is detailed over leaf. a list of the additives and quantities must be sent to freight company and they will assess the hazard. the following checks must be carried out : (i) (ii) Check contents and labelling (see section 1. This document should be signed. which came to effect on the 1st January 1996. If a mixture of chemicals is to be sent. in duplicate. If sending samples by air.3.25.Section 1 Health and Safety 1. by the Client or third party testing lab and filed accordingly. This is a legally binding document which ensures that no additives or fluid samples are analysed without prior authorisation.

) Limited Gentlemen: It is our understanding that Company Name is interested in evaluating certain proprietary materials to be supplied to you by Schlumberger Evaluation & Production Services (U. If you are willing to undertake these obligations. 199____. and to supply. to destroy any portion of the material not used for the above stated purpose. to receive and evaluate samples provided hereunder and to inform Schlumberger of the results of said evaluation and to retain in confidence and not to release nor reveal the results of said evaluation or any confidential information to any third party without the prior written consent of Schlumberger.K. Scotland. have analyzed or otherwise attempt to ascertain the chemical composition of said materials without the prior written consent of Schlumberger. please indicate acceptance by signing and returning one original of this agreement. (4) This agreement is personal to the parties and is nonassignable. Schlumberger is willing to furnish you limited research quantities of same on the condition that you will use them only for this stated purpose and that you agree: (1) (2) (3) not to analyze. SCHLUMBERGER EVALUATION & PRODUCTION SERVICES (U. a division of Schlumberger Evaluation & Production Services (U.) Limited. “COMPANY NAME” BY _______________________________ NAME ____________________________ TITLE ____________________________ .K. not to transmit any portion thereof to any third party.K. Dowell Division. Dowell division (“Schlumberger”). To facilitate your evaluation of this material. at Schlumberger’s request. Westhill Industrial Estate.Section 1 Health and Safety Non-Analysis Agreement Date “Company name” Re: Blanket Non-Analysis Agreement with Dowell. Aberdeenshire AB32 6TQ. written confirmation of destruction to Schlumberger Evaluation & Production Services (U.) Limited.K. Schlumberger is willing to permit you to evaluate these materials but considers the chemical composition to be confidential and proprietary to Schlumberger. Westhill.) LIMITED (DOWELL DIVISION) BY__________________________________ John Sudderth Vice President AGREED TO AND ACCEPTED this _____ day of ____________. and prior to any termination date hereof. and any formulations of articles containing same in a form susceptible to analysis.

dowell.dowell.6 HSE CONTACTS FOR DRILLING FLUIDS For information on safety assessments Adrian Roach PCF.com . Par Cornwall UK Tel: (44) 1726 818810 Fax: (44) 1726 818818 E_mail: roach@st-austell.slb. Box 20 4780 AA Moerdijk The Netherlands Tel: (31) 168 332761 Fax: (31) 168 327653 E_mail: romijn@moerdijk.O.slb.com For information on MSDS of Drilling Fluids additives Henk Romijn OIES P.Section 1 Health and Safety 1.St Austell c/o ECC Research Labs Par Moor Rd.

To ensure the physical and chemical properties of the mud are measured accurately. although there are numerous exceptions where third party chemicals are utilised and therefore given C-Codes. Product Aluminium Sulphate Aluminium Stearate Ammonium Thiocyanate Antifoam A Antifoam S AP-21 Aquapac Regular Aquapac LV Attapulgite Barite API Barite OCMA Barite ARTEP Benex Bentonite extender Bentonite API Bentonite OCMA Biozan Blen-Fyber Blown Asphalt Borax Breake-M Bridgesal Plus Bridgesal Plus super fine Brinewate A Calcium bromide 52% liq (sg = 1.1 INTRODUCTION Essential equipment and chemicals are required to set-up a district drilling fluids support laboratory.Section 2 Laboratory Equipment and Chemicals 2. It is a fundamental prerequisite of all drilling fluids laboratories that equipment is calibrated and chemicals are within their respective shelf life. Most chemical additives are proprietary to Dowell. A stock of drilling fluids additives is required for mixing the fluids in question.5) The majority of chemical additives and testing chemicals have a “shelf life”. Equipment must be kept clean and maintained with the appropriate calibration procedures in accordance with ISO 9001. past which they are regarded as aged and deteriorated. LABORATORY EQUIPMENT AND CHEMICALS 2.1 DRILLING FLUIDS PRODUCT LINE AND C-CODES The products are listed alphabetically and the shelf life given is a guideline.70) Calcium bromide Powder 95% C Code C134 C133 C322 C187 C188 C135 C329 C330 C136 C100 C138 C137 C139 C189 C101 C140 C359 C717 C141 C360 C696 C366 C364 C957 C370 C372 Shelf life 3 yrs 3 yrs 3 yrs 3 yrs 2 yrs 3 yrs 1 yr 1 yr 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 1 yr 3 yrs 3 yrs 1 yr Primary Function Flocculant Tracer Defoamer Defoamer Deflocculant Viscosifier Fluid loss additive Viscosifier (high salinity) Weighting agent Weighting agent Weighting agent Bentonite extender Bentonite extender Viscosifier Viscosifier Viscosifier LCM Fluid Loss Control Cross linker Breaker Bridging agent Bridging agent Completion fluid Completion fluid Completion fluid 2 yrs . it is essential that all mud testing equipment is properly maintained and that the calibration is checked on a regular basis. 2. (see section 2.

Section 2 Laboratory Equipment and Chemicals C143 C376 C400 C408 C145 C302 C300 C104 C419 C420 C147 C431 C153 C149 C152 C148 C552 C457 C160 C191 C485 C906 C163 C164 C167 C500 C115 C193 C169 C171 C105 C106 C195 C196 C197 C538 C174 C175 C176 C1003 C178 C179 C541 C116 C180 C128 C129 C843 C182 C543 C844 C185 C117 C551 C121 3 yrs 3 yrs 2 yrs 3 yrs 2 yrs 2 yrs 3 yrs 2 yrs 2 yrs 3 yrs 2 yrs 2 yrs 1 yr 1 yr 1 yr 1 yr 2 yrs 2 yrs 3 yrs 3 yrs 1 yr 1 yr 1 yr 1 yr 2 yrs 3 yrs 1 yr 3 yrs 3 yrs 1 yr 3 yrs 3 yrs 2 yrs 2 yrs 3 yrs 3 yrs 6 mths 2 yrs 2 yrs 2 yrs 2 yrs 2 yrs 2 yrs 2 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 1 yr Completion fluid Weighting agent Completion fluid Completion fluid Dispersant Fluid loss additive Fluid loss additive pH control Fluid loss additive Lost circulation material Dispersant Depressant Viscosifier Fluid loss additive Fluid loss additive Fluid loss additive Defoamer Defoamer Lost circulation material Surfactant Fluid loss additive/ Viscosifier Fluid loss additive Fluid loss additive/ Viscosifier Fluid loss additive Dispersant Ester based oil Fluid loss additive (VISPLEX) Viscosifier Fluid loss additive Viscosifier Inhibition Inhibition Fluid loss additive Fluid loss additive Water Wetting Agent Torque Reducer Shale Inhibitor Shale Inhibitor Shale Inhibitor Shale Inhibitor Bridging agent Bridging agent Completion Additive Shale Inhibitor (QUADRILL) Bridging agent Bridging agent Bridging agent Bridging agent Bridging agent Bridging agent Bridging agent Biocide Biocide Detergent Viscosifier Calcium bromide liquor Calcium carbonate Calcium chloride Calcium chloride liquor 35/37% Calcium lignosulphonate CALOFLO 100 CALOTEMP Caustic soda Causticized lignite Cellophane flakes Chrome-free lignosulphonate Chrome lignite CMC Hi Vis Tech CMC Lo Vis Tech CMC Lo Vis Pure CMC Lo Vis Pure Defoamer Defoam 2 Di-Plug Drilling detergent Drispac Plus Regular Drispac Plus Superlo Drispac Regular Drispac Superlo Ferrochrome lignosulphonate Finagreen Base Oil FLOPLEX* GELTEMP Gilsonite Guar Gum Gypsum HF100 Shale Stabiliser HI-TEMP* Fluid Loss Additive HI-TEMP II Fluid Loss Additive HYMUL* IDBEADS IDBOND L IDBOND P IDBOND P100 IDBOND PRD IDBRIDGE* IDBRIDGE L IDBRINE P* IDCAP* IDCARB 10 IDCARB* 75 IDCARB 150 IDCARB 300 IDCARB 600 IDCARB 1500 IDCARB 3000 IDCIDE* L IDCIDE P IDCLEAN IDF-FLR* .

Section 2 Laboratory Equipment and Chemicals C122 C186 C200 C202 C203 C118 C204 C120 C119 C205 C206 C207 C208 C556 C215 C216 C228 C227 C229 C230 C845 C232 C235 C236 C237 C238 C579 C578 C242 C846 C240 C243 C581 C584 C245 C246 C248 C250 C123 C252 C124 C254 C256 C257 C259 C260 C261 C263 C264 C265 C267 C268 C638 C640 C274 1 yr 3 yrs 3 yrs 3 yrs 2 yrs 1 yr 1 yr 1 yr 1 yr 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 2 yrs 3 yrs 2 yrs 2 yrs 2 yrs 2 yrs 2 yrs 2 yrs 1 yr 1 yr 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 2 yrs 2 yrs 1 yr 1 yr 1 yr 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 1 yr 1 yr 2 yrs 3 yrs 1 yr 1 yr 1 yr 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs Fluid loss additive Surfactant Corrosion Inhibitor Corrosion Inhibitor Corrosion Inhibitor Fluid loss additive Fluid loss additive Fluid loss additive Fluid loss additive Flocculant Flocculant Flocculant Flocculant Flocculant Stuck pipe freeing agent Stuck pipe freeing agent Breaker Viscosifier Viscosifier Lubricant Lubricant Lubricant Viscosifier Fluid loss additive Scale Inhibitor Scale Inhibitor Weighting agent Bridging agent Bridging agent Weighting agent Weighting agent Oxygen Scavenger Oxygen Scavenger Oxygen Scavenger H2S Scavenger Lost circulation material Dispersant Shale Stabiliser Shale Stabiliser Dispersant Viscosifier Viscosifier Viscosifier Detergent Viscosifier (completion fluids) H2S Scavenger Viscosifier Thinner Primary emulsifier Primary emulsifier Fluid loss additive Low end rheological modifier Polymeric stabiliser Polymeric stabiliser Fluid loss additive IDF-FLR XL IDFAC* Surfactant IDFILM* 220X IDFILM 620 IDFILM 820X IDFLO* IDFLO B IDFLO HTR IDFLO LT IDFLOC* IDFLOC C IDFLOC OC2P IDFLOC P IDFLOC S IDFREE* IDFREE UW IDHEC* Breaker IDHEC IDHEC L IDLUBE* IDLUBE XL IDLUBE 330 IDPAC* IDPAC XL IDPLEX* 100 IDPLEX K IDSALT* 75 IDSALT 250 IDSALT C IDSALT* FK IDSALT FS * IDSCAV* 110 IDSCAV 210 IDSCAV 510 IDSCAV ES IDSEAL* IDSPERSE* XT IDTEX* IDTEX W IDTHIN* 500 IDVIS* IDVIS D IDVIS L IDWASH* IDWORK* IDZAC* INSTAVIS* INTERDRILL* DEFLOC Thinner INTERDRILL EMUL INTERDRILL EMUL HT Emulsifier INTERDRILL FL Emulsifier INTERDRILL LO-RM Rheological INTERDRILL LOPOL CP INTERDRILL LOPOL VX INTERDRILL NA .

Section 2 Laboratory Equipment and Chemicals C612 C275 C269 C276 C281 C620 C282 C621 C622 C283 C285 C286 C103 C107 C289 C290 C111 C292 C675 C294 C213 C214 C295 C296 C108 C298 C706 C707 C714 C125 C126 C299 C719 C331 C723 C727 C989 C217 C301 C109 C110 C764 C302 C304 C305 C776 C850 C465 C306 C501 C958 C218 C219 C222 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 1 yr 1 yr 1 yr 3 yrs 3 yrs 3 yrs 3 yrs 2 yrs 1 yr 1 yr 2 yrs 1 yr 1 yr 3 yrs 2 yrs 1 yr 3 yrs 3 yrs 1 yr 1 yr 1 yr 2 yrs 2 yrs 3 yrs 1 yr 2 yrs 2 yrs 2 yrs 2 yrs 2 yrs 2 yrs 3yrs 3 yrs 3 yrs 3 yrs 1 yr 1 yr 1 yr 3 yrs 3 yrs 3 yrs Fluid loss additive Oil wetting agent Rheological modifier Fluid loss additive Viscosifier Scale Dissolver Scale Dissolver Surfactant Surfactant H2S Scavenger Flocculant Lost circulation material Fluid loss additive Emulsifier activator Liquid casing Base fluid Lost circulation material Lost circulation material Lost circulation material Lost circulation material Deflocculant Fluid loss additive Fluid loss additive Inhibition pH control Tracer Fluid loss additive Inhibition Polymer temperature extender Polymer temperature extender/ pH buffer Polymer temperature extender Viscosifier Fluid loss additive Viscosifier Shale stabiliser Lubricant Viscosifier (high salinity’s) Viscosifier Dispersant calcium treatment cement treatment Completion fluid Base fluid Tracer Fluid loss additive/lubricant Fluid loss additive/lubricant Shale stabiliser Shale stabiliser Fluid loss additive Fluid loss additive Fluid loss additive/Viscosifier Fluid loss additive Fluid loss additive Fluid loss additive INTERDRILL NA HT INTERDRILL OW INTERDRILL RM INTERDRILL S INTERDRILL VISTONE INTERSOLV* H INTERSOLV XFE INTERTREAT* 1600 INTERTREAT 1777 Ironite Sponge KWICKCLEAN* KWICKSEAL* Lignite Lime Liquid casing Magnesium chloride Mica Mud Fiber OML Fiber Lost Circulation Oyster Shells POLYLIG Deflocculant POLYTEMP* Fluid Loss Polydrill Potassium Chloride Potassium Hydroxide Potassium Iodide Potassium Lignite Potassium Nitrate PST-100 Temperature PTS-200* Temperature PTS-300* Temperature RHEOPOL * RHEOPOL XL RHEOPOL GX SAFEDRILL SAFELUBE Salt Gel SM(X)* Sodium Acid Pyrophosphate (SAPP) Soda ash Sodium Bicarbonate Sodium Bromide Sodium Chloride Sodium Nitrate Soltex Soltex (Potassium) STAPLEX 500 Shale Stabiliser STAPLEX 650 Shale Stabiliser Starch Thixsal FL7 plus Thixsal plus TRUDRILL S* Fluid Loss Additive TRUFLO* 100 Fluid Loss Additive TRUFLO MVO Fluid Loss Additive .

Section 2 Laboratory Equipment and Chemicals C220 C221 C224 C225 C226 C380 C382 C383 C385 C384 TBA TBA C127 C132 C828 C830 C313 C314 C315 C316 C130 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 3 yrs 1 yr 1 yr 2 yrs 3 yrs 1 yr 1 yr 3 yrs 3 yrs 3 yrs Primary emulsifier Organophillic clay extender Oil wetting agent Viscosifier Viscosifier Base fluid Primary emulsifier Secondary emulsifier Deflocculant Oil wetting agent Fluid loss additive Fluid loss additive Viscosifier Viscosifier Weighting agent Lost circulation material Viscosifier Viscosifier Completion brine H2S Scavenger H2S Scavenger TRUMUL* Emulsifier TRUPLEX* Extender TRUSPERSE* Wetting Agent TRUVIS* Viscosifier TRUVIS HT Viscosifier ULTIDRILL base fluid ULTIDRILL EMUL HT ULTIDRILL FL ULTIDRILL DEFLOC ULTIDRILL OW Ven-Chem 208 Ven-Chem 222 VISPLEX* Viscosifier VISPLEX II Viscosifier Watesal-A Wood Fiber (C830) XC polymer XCD polymer Zinc Bromide Liquor (C315) Zinc Carbonate (C316) Zinc Oxide (C130) .

500 F) Large & Small bottle brushes Teflon Tape Steel Wool Test Procedures Manual Laminated Safety Posters (non-returnable) Chemicals Aktaflo E 250 m L Ammonium Hydroxide (Buffer) 60mL Bromo Cresol Green 60mL Buffers at pH 4.1N 250mL Sodium Hydroxide 1N 250mL Sodium Perchlorate Soln 250 mL Sulphuric Acid 0.1N 250mL Sulphuric Acid 5N 60mL 1 1 each 1 1 1 1 each 1 1 1 1 1 2 1 1 2 1 2 1 each 2 4 1 1 2 2 2 2 10 5 5 10 5 3 3 3 3 1 1 2 2 1 2 each 2 each 1 roll 3 1 1 1 2 2 1 each 4 15 1 1 2 4 2 2 2 1 5 2 1 2 2 2 2 2 1 1 1 2 4 * * * * * * * * * * * * * * * * * * * * * * * * WBM / OBM OBM OBM / WBM WBM OBM / WBM OBM / WBM OBM / WBM OBM / WBM OBM WBM WBM WBM OBM / WBM OBM / WBM KCl WBM OBM / WBM OBM / WBM OBM / WBM OBM / WBM OBM / WBM WBM KCl WBM OBM / WBM OBM WBM * * * * * * * * * * * * * * * * * * * * * * * * * * * 2.14 Hand Crank Centrifuge Marsh Funnel Mud Cups Sand Content Kit Calibration Fluid Glassware & Miscellaneous 10mL Measuring Cylinder 25mL Measuring Cylinder 50mL Measuring Cylinder 250mL Measuring Cylinder 1 mL Syringe 2 mL Syringe 5 mL Syringe 10mL Syringe 20mL Syringe 1 mL Pipette 2 mL Pipette 5 mL Pipette 10mL Pipette Pipette Pump Glass Stirring Rod 100 mL Beaker 100 mL + 250 mL Conical Flasks Plastic Wash Bottle 500 mL Stem Thermometers (0 .box Garret Gas Train (including 'O' Rings & Drager Tubes & excluding Chemicals) Pressurised Mud Balance + spare 'O' Rings Baroid Mud Balance Ohaus Balances .4 TEST SUMMARY OF EQUIPMENT AND CHEMICALS FOR BASIC DRILLING FLUIDS TESTING SUBSTRATE EQUIPMENT COMMENTS .Section 2 2.0282N 250mL Silver Nitrate 0.02N 250mL Sulphuric Acid 0.Small & Triple Beam pH Meter pH paper 7 .3 Rig : Laboratory Equipment and Chemicals STANDARD MUD KIT STANDARD MUD KIT SMK No : Quantity Serial Number Material Out ( ) If Included Material Backloaded Quantity Returned Status ( ) If Calibrated Operator : Equipment Description Transformer (Step Up / Step Down) Fann Viscometer .01M 250mL Exosol (IPA/Xylene 50:50) litre Hydrogen Peroxide 3 % 250mL Manver Indicator 60mL Methylene Blue 250mL Methyl Orange 60mL Nitrous Oxide Cartridges box Phenolphthalien 60mL Potassium Chloride Standard 250mL Potassium Chromate (5%) 60mL Potassium Hydroxide 8N 60mL Silver Nitrate 0.7 & 10 500mL Calver II box of 25 caps Carbon Dioxide Cartridges box Defoamer (Octanol) 60 mL Distilled Water 25 litre EDTA 0.220 F & 50 .282N 250mL Sodium Hydroxide 0.6 speed & Stainless Steel Viscometer Cup Thermo cup 10mL Retort 50mL Retort Hamilton Beach Mixer & Stainless Steel Cup Hot Plate with Magnetic Stirrer Emulsion Stability Meter HT/HP Filter Press Complete + spare 'O' Rings & Filter Papers API Filter Press complete + spare gaskets API Mesh Screens API Filter Paper .

in size (90mm No.5" No. 10ml. Heating jacket Graduated cylinders Pressurised Nitrogen to 600 psi Filter Papers Pressure Regulators to 1000 psi Thermometer Spares Retort Cells (complete) Heating jacket Heating Elements Graduated cylinders Steel wool Pipe cleaners Spatula Water wetting agent Sieve Funnel Glass measuring tube Conical flask Syringe Hot plate Glass stirring rod Graduated cylinder Pipette Hydrogen Peroxide Sulphuric Acid Methylene Blue Solution Filter Papers Check Voltage/ Hertz Check Voltage/ Hertz Steel.20 % 250cc Glass. etc.Section 2 Density Funnel Viscosity Rheology PV.50ml 3. 50 or equiv) 5ml. Check Grub screws and 'O' rings Check voltage 5ml. 10ml. receiver. 5ml.0 ml 3% solution 50ml in dropper bottle 3. 50ml preferred Check voltage Check voltage Same volume as cell Grade 'OO' To fit cell Small bottle 200 mesh 2.50ml 'O' rings etc. stand. Range 0-250°F Calibrate weekly with DI water Calibrate weekly with DI water Mud 7.20g/litre USP grade Large Diameter HTHP Filtrate Mud Oil/Water/Solids content Mud Sand Content Mud Cation Exchange Capacity Mud .1 sq. 50 or equiv) Steel. 10ml Check voltage 50ml Graduated 1. To fit sieve graduated 0 . size (2. Gel Strengths API Filtrate Laboratory Equipment and Chemicals Mud Mud Mud Mud Balance Pressurised Mud Balance Marsh Funnel Mud Cup Viscometer Thermocup Thermometer Filtration Cell Pressurised Nitrogen to 100 psi Filter Papers Pressure Regulators to 200 psi Graduated cylinders Spares Filtration cell. range to 500°F 'O' rings etc. 20ml. YP. 20ml.5" dia.55 in sq.

0. 10ml 1. etc. reagent grade In dropper bottle Preferably 0. 2. tubes.Section 2 Laboratory Equipment and Chemicals SUBSTRATE EQUIPMENT COMMENTS Calibrate daily Store in DI water pH 4. 1x1ml 0.02N (N/50) Chloride determination 0.25% in deionised water Carbonate Determination c/w flowmeter. pH sticks Distilled Water Thermometer Mud and Filtrate Glass syringes Plastic syringes Plastic titration vessels Volumetric pipette Graduated pipettes Sulphuric Acid Hydrochloric Acid Sodium Hydroxide Solution Barium Chloride Solution Phenolphthalein Indicator Methyl Orange Indicator Bromophenol Blue Indicator Distilled Water Filtrate or Aqueous phase in OBM Ceramic Titration Vessel Sulphuric Acid Phenolphthalein Indicator Potassium Chromate Indicator Silver Nitrate Solution Distilled Water Ceramic Titration Vessel Hot plate Graduated Pipettes pH Sticks EDTA solution Sodium Hydroxide Buffer Solution Calcium Indicator Acetic Acid Sodium Hypochlorite Masking Agent Ammonia Buffer Garrett Gas Train Regulator Nitrogen Cartridges Drager Gas Bag Stopcock & tubing Drager Hand Pump Drager CO2 analysis tubes Hypodermic syringes Hypodermic needles Sulphuric Acid Octanol Defoamer Spare Septa Distilled Water Mud/Filtrate Alkalinity (Mf/Pf) (P1/P2) Preferably 0.02N 1N NaOH Calver II or Hydroxy Naphthol Blue Glacial 5.02N (N/50) 0. 2x10ml 1.02N (N/50) 0.282N or0.0ml. 10ml 0.05 µS conductivity .05 µS conductivity 0. 2x10ml.0ml 1. 5ml 5ml.0.01M.0.1N (N/10) 10% at pH 7 TEST pH Mud and Filtrate Meter Electrodes Buffer Solutions.0ml. 1 litre capacity 0.05 µS conductivity Divalent Ion Analysis (Ca and Mg) Filtrate or Aqueous phase in OBM 1x5ml.5" / 21 gauge 5N.5ml. diffuser. pH 7. pH 10. etc.0282N in dark bottles Preferably 0.01% 1.0 Narrow & wide ranges In wash bottle Glass 1ml. bottles.

5x H2s 100/a. (versenate method) Filtrate 0.01M.0g NaClO4 in 100ml Dist. 0. 2x100ml 250ml Calcium Sulphate Detn.5ml.05 µS conductivity 6N Octyl Alcohol Total Sulphides (Alka Seltzer Method) Mud 2. regulators.5ml. etc. 1x3. 2x5.5m.Section 2 Laboratory Equipment and Chemicals SUBSTRATE Filtrate TEST Potassium Determination (Perchlorate Method) (STPB Method) EQUIPMENT Centrifuge Centrifuge tubes Pipettes Syringe Sodium Perchlorate solution Standard Potassium Chloride Soln. Distilled water STPB solution Quaternary Ammonium Salt Soln. 2x10ml 2x25ml.0-5.0ml.2%/A 5N reagent grade 1.5ml.02N 1N NaOH Calver II or Hydroxy Naphthol Blue Glacial 5. 1x1. 5x H2s 0.0ml 10ml 150.0-ml. 1x2.5ml 25ml Preferably 0. 1x1.0ml.0ml. Water 14.05 µS conductivity Tubing.5" / 21 gauge In dropper bottle Soluble Sulphides (Garrett Gas Method) Filtrate . 2.25% in deionised water 1x2.0g KCl in 100ml distilled water In wash bottle 20g / 80ml distilled water In dropper Bottle 1x2. flowmeter.0ml. 3x10ml 50ml Preferably 0. Sodium Hydroxide Solution Bromophenol Blue Indicator Graduated Pipettes Graduated Cylinders Beakers Filter Funnel Filter Paper EDTA solution Buffer solution Calcium Indicator Acetic Acid Sodium Hypochlorite Solution Masking Agent Volumetric pipettes Graduated cylinder Ceramic titration vessel Hotplate pH sticks Deionised Water Hydrochloric Acid Defoamer Hydrogen Sulphide Test Paper Alka Seltzer Tablets Test Bottle & Cap Colour Comparison Chart Syringe Graduated cylinder Distilled Water Garrett Gas Train (complete) N2 or CO2 cartridges Drager Analysis Tubes Lead Acetate Paper Discs Sulphuric Acid Hypodermic syringes Hypodermic needles Octanol defoamer COMMENTS Must be capable of 1800rpm Must be 10ml Kolmer type 1x0. 2x10ml 1.

For example. In order to control and monitor calibration effectively. 10ml 1.1N N/10 Made up from a 50/50 Xylene/IPA Preferably 0.0ml. Each item has a record sheet/sheets and every time a particular instrument is checked for calibration. Notes : (i) In some instances. In the case of expensive items like Fann viscometers. each piece of equipment which requires calibration must be given a serial number. many calibration problems with Fann viscometers are due to bent bobs which can be replaced.05 µS conductivity 2.5 EQUIPMENT CALIBRATION AND MAINTENANCE PROCEDURES This section gives the calibration methods for all major items of drilling fluid test equipment and also procedures for ensuring that proper records are kept. the results must be recorded. 10ml 2 x 100 ml 2. Any equipment that goes out of calibration and cannot be repaired must not be used.0ml. 5ml COMMENTS 5ml. it is possible to bring the calibration back to within specification by changing out only a part of the equipment. the equipment must be cleaned and visually inspected so that obvious defects can be remedied. specialised external contractors can be used for repair. The procedure and frequencies given are based on the manufacturer's recommendations. 10ml 400 ml 0. so that its calibration status can be easily accessed. .Section 2 Laboratory Equipment and Chemicals SUBSTRATE Mud TEST Alkalinity & Lime (OBM only) EQUIPMENT Glass syringes Plastic syringes Graduated measuring cylinder Graduated pipettes Magnetic Stirrer and stirrer bar Beaker Sulphuric Acid Exosol Phenolphthalein Indicator Distilled Water 1ml. Regular calibration must be carried out on equipment used in the laboratory. A calibration sticker must be completed and attached to the equipment. (ii) Prior to calibration check. It should be assumed that any unmarked equipment has not been calibrated.

Instrument : Manufacturer and model : Serial Number : Calibration procedure : Calibration frequency : Calibration limits : Responsibility : INSTRUMENT CALIBRATION/MAINTENANCE RECORD TEMPLATE DATE RESULT COMMENTS SIGNED .1 Laboratory Equipment and Chemicals Calibration Records Blank calibration sheets for the equipment in the mud kit are given below.5. Figure 2.Section 2 2.

Do not let either end of the balance touch the case during this process .e.34 lbs/gal and is marked with a longer scale division called the water line. remove the screw cover from the weight adjustment compartment and add or remove lead shot until the balance is correctly calibrated. but its calibration must be checked to ensure accurate results are obtainable. (it is balanced when the bubble is equidistant from the centre lines). 2 3 4 5 6 7 8 Calibration frequency : Weekly . The measurement reading should be 8. Place the knife edge of the balance onto the fulcrum and check the reading by moving the rider along the arm. If the mud balance gives improper readings. the arrow pointing to the mark). Place the base stand on a level surface.it can pick up dirt and give a false ready.Mud Balance 2.2 The calibration of the mud balance is unlikely to change. approximately room temperature. 1 Ensure the balance is thoroughly cleaned as even small deposits of mud on the balance or rider can cause improper readings. Record the reading from the side of the rider nearest the balance cup. unless damaged in some way. Dry off any excess water from the outside of the balance. Fill the balance cup with fresh water. Tap the side of the balance several times to remove any entrained air and then place the lid onto the balance cup by pushing it downwards with a slow rotating motion until it is firmly seated.Section 2 Laboratory Equipment and Chemicals PROCEDURE CAL/EAF/001 . The temperature of the water must be at 70°F (21°C). The following method should be adhered to.5. (i. Check that it is not physically damaged. Ensure that some water is forced through the vent hole.

rinse off the cup and threads with water and then screw the threaded cap on the cup. 2 3 4 5 6 7 8 9 10 11 12 Calibration frequency : Weekly . Draw the position rod upwards.Pressurised Mud Balance Unless damaged.34 lb/gal and is marked with a longer scale division called the water line. Any excess water will be discharge through the check valve. the calibration of a pressurised mud balance us unlikely to change. Once the pressure is actuated and the valve has closed. Pressurise the cup by pushing downwards on the cylinder housing and piston rod simultaneously. When the lid has been placed on the cup.5 cm). reconnect the empty plunger and push downwards on the cylinder housing. Place the base stand on a level surface. thus filling the cylinder with water. The reading should be 8.5. approximately room temperature. when the level bubble is centred between two black marks.e. its calibration is equally important. To release the pressure. 1 Ensure the balance is thoroughly cleaned. Fill the balance cup with fresh water. Submerge the nose of the plunger in the water with the piston rod completely depressed. pull the check valve up in the closed position. Check that it is not physically damaged. Place the lid on the cup with the attached check valve in the down (open) position. The cup must be filled to a level slightly below the upper edge of the cup -approximately 1/4" (0. remove the screw cover from the weight adjustment compartment and add or remove lead shot until the balance is correctly calibrated. but due to the crucial nature of the results it provides. Push the lid downward into the mouth of the cup until surface contact is made between the outer skirt of the lid and the upper edge of the cup. Place the balance on the knife edge and slide the weight left or right until the beam is balanced i. disconnect the plunger. as even small deposits of mud on the balance arm or rider can cause incorrect readings.Section 2 Laboratory Equipment and Chemicals 2. The cup can then be emptied and dried off.3 PROCEDURE CAL/EAF/002 . Push the nose of the plunger onto the machine O' ring surface of the valve. The temperature of the water should be at 70°F (21°C). If the balance gives incorrect readings. The valve. lid and cylinder should be frequently greased with a waterproof grease. The following method must be adhered to.

e. The certificate number is given in the gauge inspection column.e. 1 2 3 Check the lead and plug for wear and replace if necessary Plug in and place the thermometer in the jacket thermometer housing.5 on the adjustment scale. Allow to stand for 30 minutes. There should be no loss of pressure from either regulator. Care must be taken releasing the pressure and dismantling the equipment. 4 5 6 7 8 9 Safety Notes : 1 2 Notes : All pressure gauges are calibrated yearly. Therefore.4 PROCEDURE CAL/EAF/003 . (see section 4. top regulator : 600 psi).HTHP Fluid Loss Equipment Faulty equipment when using high temperatures and high pressures can lead to serious accidents. All apparatus must be cold and under zero pressure before maintenance or calibration begins. it is essential that all equipment is maintained and calibrated. not sticking against the scale or glass). ST 508 Digital thermometers calibration records should be traceable to national standards.e. If it does not . bottom regulator : 100 psi. The filter screen must be checked for wear (i.Section 2 Laboratory Equipment and Chemicals 2.5. sharp ends or holes) and replaced if required.4) Pressure gauge calibration frequency : Annually Annually Digital thermometer calibration frequency : . The grub screws and screw wells must be checked for wear and replaced if necessary. The pilot light should come on when the temperature has stabilised. This is the uppermost temperature required of the equipment.3. ‘O’ rings and valves must be checked for wear or blockage and replaced if required. Allow the jacket to heat up to 350°F. during this period. Check that the pressure gauges are not damaged and that the needles are free (i. approximately 6.replace it. Maintenance frequency : monthly Never use nitrous oxide cartridges on HT/HP equipment. in addition to inaccurate data. Connect regulators to HT/HP cell and pressurise to working conditions (i. Each gauge is individually identified and referenced to a calibration certificate.

0. (v) Reweigh sample container with water and lid Results 50 mL Retort = 50 g deionised water (+/.5 Laboratory Equipment and Chemicals PROCEDURE CAL/EAF/004. Temperature (i) (ii) (iii) Control : Place thermocup in heating block Switch on retort Once retort temperature has stabilised (i.5. Place the empty sample chamber with lid on an electronic balance and tare.e. (iii) Fill sample chamber with deionised water and replace lid.Section 2 2. (iv) 3. counterclockwise to make it cooler).1 g) Temperature Control calibration frequency : Chamber volume calibration frequency : Annually Monthly . (Clockwise to make it hotter.000°F +/50°F (50 mL retort) as measured with a calibrated thermocouple or digital thermometer. Adjust control screw if necessary. 2.50°F (10 mL retort) and 1.0.25 g) 20 mL Retort = 20 g deionised water (+/.Retort 1. the temperature should be 600°F +/. ensuring some water is displaced through drain hole. indicator light has gone off). (iv) Place a finger over the drain hole and dry sample container surface thoroughly. Chamber (i) (ii) Volume Clean and dry the sample chamber (50ml or 20 ml) thoroughly. Visual Inspection : The following must be checked for wear and replaced as necessary : Check list Cable Plugs Sockets Retort chamber (for cracking) Also check the screw threads for damage and ensure that the retort can be properly assembled.

The Dow Corning 200 calibration fluid can be obtained from OFI or from : Hilton Instruments 32 Holland Street Aberdeen AB2 3UL Tel. followed by the 300 reading. 6. Check readings against calibration chart (as supplied with each batch of oil). 7.Fann 35 Rheometer 2. 3. As a minimum. (44) 224 620121 Fax : (44) 224 20125 This company also undertakes viscometer repairs. N. 1.5. 2. Viscometer calibration frequency : Thermometers calibration frequency : Monthly Annually . Ensure the bob. of the fluid corresponds with calibration chart ref. Check the ref. 5. Fill the heating cup with the Dow Corning 200 calibration fluid and adjust the heating cup until the fluid reaches the correct level on the rotor (marked by line). digital thermometer or mercury thermometer. If the viscometer is found to be out of calibration. Record figures from the chart. Note : the chart from the supplier will normally only give the 300 rpm reading. rotor and heating cup are clean and dry.6 1. using either a calibrated thermocouple. no. it must be re-calibrated by trained laboratory personnel.B. ST 508 digital thermometers calibration records should be traceable to national standards. 2. Start the viscometer on the 600 rpm reading and record. The readings obtained should be within 2 points of those specified on the calibration chart. allowing at least two minutes on each speed for the dial to stabilise. Check and record the temperature of the calibration fluid. 4. For the 600 rpm reading simply multiply the 300 rpm reading by two. readings should be taken at both 300 and 600 rpms.Section 2 Laboratory Equipment and Chemicals PROCEDURE CAL/EAF/005 .

4. Any reading less than these will warrant replacement of the probe. the reading should be 915 volts +/. Probe Condition It is essential that the probe is scrupulously clean before checking is initiated.5. cracks or loose connections). If the reading is outside the specification refer to stage 4 for re-calibration of the meter. The reading should be 1999 or >2000 depending on the age of the meter. On the ESM 30.OFI Emulsion Stability Meter Make : OFI Model : ESM-20/ESM-30 1. Remove the circuit board plastic cover. the reading should be 750 volts +/.e.5%. Calibration frequency : Monthly . b. located at the top left corner of the display. If this is indicated replace the batteries (9 volt alkaline) 2. Meter Condition Place the calibration probe into the probe socket and depress the power source button. Battery Condition Check the low battery indicator. Check the probe for any damage (i.Section 2 2. 3. C. connect the probe to the meter and immerse the electrodes at the tip of the probe in clean diesel/base oil. On the ESM 20.7 Laboratory Equipment and Chemicals PROCEDURE CAL/EAF/006 .2%. Repeat step 2 until correct reading is obtained with the calibration probe. Meter Re-calibration a. If there are no visible defects. Make a small adjustment to potentiometer R5 and recheck reading with calibration probe.

0g 100g 1 kg 0.0g. 10g & 100g Calibration frequency : monthly Weight calibration frequency : yearly N.0.0. M25/MW 465-134 and M29/MW 475-159).0g.B.05g +/-0. The weights recorded must be within the error limits as stated below. 2 4.0.0.5g +/-0. Sauter balance model RC8021 d. Ref: UK National Physical Laboratory (NPL) certified E2 standards of mass. Each weight should be traceable to national standards.Electronic and Mechanical Balances 2.Section 2 Laboratory Equipment and Chemicals PROCEDURE CAL/EAF/007 .01g. 1. Ohaus balance model 311-00 b. 2.1g +/-0.0kg .001g Calibration weight to use 10g and 100g 100g & 1 kg 1.1g +/-0. Balance a.00g 1kg 1. Repeat stage 2 with weight no. For electronic balances.8 Ideally every balance should be checked with a minimum of two calibration weights which span the scale on which the balance is being used.5g +/.0g. it is recommended that calibration is carried out by the manufacturer or by external contractors as far as possible.5. 1. 1 on the balance plate and record figure given by balance.10.5g +/. Oertling balance model LA164 Error limits Balance Ohaus model 311-00 Ohaus model 311-00 Ohaus model 760-00 Ohaus model 760-00 Sauter Sauter Mettler Mettler Mettler Oertling Oertling Calibration weight 10g 100g 100g 1 kg 1. 10. Mettler balance model PE3600 e.100. NPL ref. 10.100.05g +/.5g +/-0.01g 100g Error +/.0g & 1 kg 0. Ensure the calibration weights and balance plate are thoroughly clean and zero the balance. Ohaus balance model 760-00 c. 3.0g .01g +/-0.0g & 1 kg 1.0g. .100.0g. Place calibration weight no.0002g +/-0.

(ii) Ageing Cells/Bombs Clean hot rolling bombs thoroughly after use.. Check shaft speeds regularly using a calibrated tachometer. If ageing temperatures exceed 300 deg F. Check the rolling bombs periodically for signs of corrosion.B. N.Maintenance of Mixing and Ageing 2. Grease the threads and grub screws.5. Use anti-stick compound. . Check valve stems and O' rings for wear and corrosion and replace regularly.Section 2 Laboratory Equipment and Chemicals PROCEDURE CAL/EAF/008 . Variations in above can affect results. Note that stainless steel bombs will corrode if used regularly with salt-containing water base muds. by loss of weight). then replace valve stem ‘O’ rings as a matter of course. Inconel alloy bombs are available for this application and will last much longer (but are expensive).g.9 Equipment (i) Hamilton Beach Mixers / Silverson Mixers Keep mixers clean when not in use. If possible. designate specific bombs for water based muds and oil-based muds (iii) Ovens Inspect ovens regularly and check that the chain drive is not slack Check that fan is working The temperature must be monitored with a calibrated thermocouple connected to a chart recorder. Check mixer heads (blades) regularly for wear (e. This does not need to be done routinely but should be done as a calibration check on each oven once a month.

∑ The LAR template has been included at the back of the manual. ∑ Always use pre-hydrated bentonite unless otherwise stated. It is widely recognised that consistent mixing of laboratory drilling fluids formulations is a critical process in ensuring representative and reproducible final fluid properties. mixing time. ∑ Measure all product additions by weight if possible. 3. concise and achievable. These procedures are given as general guidelines for WBM and OBM preparations and are not specific to individual formulations. ∑ Duplicate formulations to ensure results are repeatable. that if not controlled can result in widely differing properties for any given formulation. Copies can also be obtained from the UKI laboratory.Section 3 Laboratory Testing Procedures LABORATORY MIXING PROCEDURES INTRODUCTION 3 3. ∑ Adjust pH to desired value.1 The following sub-sections describe the standard procedures for the preparation of drilling fluids samples in EAF laboratories. ∑ Document in detail all lab results and observations. ∑ PLEASE CONTACT THE UKI LABORATORY LABORATORY PROCEDURES IF REQUIRED FOR FURTHER DETAILS ON . shear history and ageing conditions are just a few of the many variables. (LAR) is completed and issued prior to commencing laboratory work to ensure the objectives are clear. It is for this reason that mixing procedures must be standardised. Factors such as.2 TECHNICAL NOTES ∑ Ensure a “Laboratory Analysis Request”. ∑ Ensure correct grade of bentonite is used. order of addition. before and after hot rolling.

3. 7. Allow one minute between each addition. 4. Mix for a further 4 minutes. Mix for 5 minutes on low speed (11. 5. C. Rev Dust. 4. Add all other liquid additives. 2.. E. excluding barite and simulated drill solids).1 (350 ml . Add all other powdered additives slowly into the vortex over a one minute period. Mix for a further 5 minutes.g. OCMA drilled solids. 3.g. Hymod Prima) Continue to mix the whole mud for the remaining time in the hour i. ensuring that all polymer has completely dispersed and that none adheres to the sides of the mixing vessel or the mixer shaft. Barite) slowly into the vortex over a 2 minute period. Mix for a further 4 minutes.polymer muds QUADRILL LT A a) b) c) d) e) B.g. 14 minutes 2.. Readjust pH if necessary.1 pH ORDER OF ADDITION Prehydrated bentonite (as described in DF/EAF/001) Fresh water or seawater Polymeric additive Salts s Caustic soda Weighting agent Simulated drilled solids e. adding these slowly via a syringe over a 1 minute period. Mix for a further 8 minutes. 6.g. 3. (Note : this 5 minute mixing is not required if no bentonite or salt is added!) Add high molecular weight viscosifying and encapsulating polymers slowly into the vortex over a five minute period.Low Temperature Water-Based Muds 3. Rev Dust.3.. Add the simulated drilled solids into the vortex over a 1 minute period. . 5. 1.1 g Hamilton beach mixer and cup Weighing boats Spatula pH meter: precision ± 0. Freshwater bentonite muds Seawater bentonite muds Bentonite / polymer muds Lime muds Gyp muds Polymer muds Salt saturated muds KCl . 8.e. Hymod Prima. Staplex 500.000 rpm ± 300 rpm) and adjust the pH as required with caustic soda. EQUIPMENT Balance: precision ± 0. PROCEDURE Add the required weight of prehydrated bentonite followed by the required amount of water and salts to a Hamilton beach cup.1 Lab Barrel) This procedure is generally applicable for the following drilling fluid systems. Add the weighting material (e. (E.Section 3 Laboratory Testing Procedures PROCEDURE DF/EAF/003 . 1.

then dropwise addition of a defoamer (Octanol or Antifoam S) may be added to alleviate the situation. Rheopol GX. Idcide Barite. hold the pH probe against side of "cup". Idflo. Hymod Prima . Idpac XL. Cover and allow to stand for 1 hour before testing to allow the fluid to equilibrate and any entrained air to escape. Haematite Rev Dust. Idcap. (iv) When measuring pH. Idpac.but if any occur mop up immediately. it is recommended that a caustic soda solution (e. Staplex 650. XCD. Use drop wise from dropper bottle (ii) Disposable plastic gloves and safety glasses are to be worn at all times. IDF-FLR. SUMMARISED MIXING PROCEDURE FOR LOW TEMPERATURE WATER-BASED MUDS ORDER OF ADDITION Prehydrated Gel Salts Viscosifying / Encapsulating Polymers Fluid loss Control additives Other liquid additives Weighting agent Drilled Solids Add after Time (mins) 0 5 15 25 30 35 45 Addition time (mins) 1 5 1 1 1-2 1 Mix time Examples of typical products (mins) in the Dowell DF line. Cool mixture in a water bath. 50% w/w) be used for pH adjustment. CMC HV. Biozan. Test and age as required. 5 9 5 4 4 8-9 14 Non-Treated Bentonite KCl. Guar. Safety Notes : ∑ Adjusting pH (i) Unless the quantity of caustic soda is defined in the formulation.g. 10. Do not allow it to touch the rotating shaft. Visplex II IDF-FLR XL. Idbond. OCMA. Procedural notes : ∑ Ensure temperature of fluid does not exceed 150 0F during the mixing process by mix.Section 3 Laboratory Testing Procedures 9. ∑ If excessive foaming occurs during mixing. CaSO4. ∑ Final mud formulations must be performed in duplicate to ensure reproducibility and ultimately reliability. Idlube. when handling caustic soda (solid or solution). Floplex Staplex 500. Idfilm. NaCl. . Micromax. (iii) Prevent splashes . Ca(OH)2 Idvis.

. 5. 4. 4. A a) b) c) d) e) B. Add black powders (gilsonite. Mix for a further 4 minutes Adjust pH of fluid to appropriate value over a 5 minute period Add polymeric additives slowly into the vortex over a five minute period. (E. EQUIPMENT Balance: precision ± 0. Barite) slowly into the vortex over a 2 minute period. Rheology can be quite easily be controlled with the use of bentonite or other viscosifying natural ( Attapulgite. . Rev Dust. 5. ensuring that all the powder has completely dispersed. Invariably. Rheology and tight Fluid loss control. Mix for a further 5 minutes.High Temp Water-Based Muds (350 ml . 6.g. 1. 6. 3. it is necessary to have several fluid loss additives in a formulation to synergistically lower the HTHP fluid loss. is the main problem and is more often than not difficult to optimise in the laboratory. Add the dispersants (E. Add the weighting material (e. There are two key prerequisites to formulating a desirable HTHP WBM. 6. Laponite).1 pH ORDER OF ADDITION Prehydrated bentonite (as described in DF/EAF/001) Fresh water or seawater Salts Black Powders Caustic soda Polymeric Additives Weighting agent Dispersants Simulated drilled solids PROCEDURE Add the required weight of prehydrated bentonite followed by the required amount of water and salts to a Hamilton beach cup. Mix for 5 minutes on low speed (11.. 7.g. CALODRILL HITEMP QUADRILL HT HTHP fluids are generally described as those which are temperature stable above ~ 300 Deg F. 1.g.3.1 Lab Barrel) This procedure is generally applicable for the following drilling fluid systems.) slowly into the vortex over a one minute period. IDSPERSE XT) slowly into the vortex over a 1 minute period..1 g Hamilton beach mixer and cup Weighing boats Spatula pH meter: precision ± 0. Mix for a further 8 minutes. 7. The HTHP fluid loss control. IDTHIN 500. 3. sepiolite) or synthetically produced clay minerals (Hectorite.000 rpm ± 300 rpm) and adjust the pH as required with caustic soda. Mix for a further 4 minutes. ensuring that all polymer has completely dispersed and that none adheres to the sides of the mixing vessel or the mixer shaft. 3.2 PROCEDURE DF/EAF/004 .Section 3 Laboratory Testing Procedures 3. Hymod Prima) 2. Add the simulated drilled solids into the vortex over a 1 minute period. 2. asphaltics. C. lignites etc.

that most HTHP formulations will be intermediate (12 -15ppg) to high (> 15 ppg) mud weights to control formation pressures. This is also the case when trying to reproduce the properties of a field mud: if possible. then dropwise addition of a defoamer may be added to alleviate the situation. Procedural notes : ∑ Ensure temperature of fluid does not exceed 150 0F during the mixing process. ∑ If excessive foaming occurs during mixing. it is important to ensure that the same stock of barite is used by both laboratories in order to achieve reproducible results. Test and age as required.g. ∑ Final mud formulations must be performed in duplicate to ensure reproducibility and ultimately reliability. 9 minutes 9. Do not allow it to touch the rotating shaft. 50% w/w) be used for pH adjustment.e. when handling caustic soda (solid or solution). (iii) Prevent splashes . . it is recommended that w/w caustic soda solution (e. hold the pH probe against side of "cup". It is important to recognise that two barites that pass API specifications can produce muds with very different properties. a sample of the rig barite should be obtained. (iv) When measuring pH. When formulating muds for a customer's or independent laboratory to reproduce. ∑ It stands to reason. Cover and allow to stand for 1 hour before testing to allow the fluid to equilibrate and any entrained air to escape. Safety Notes : a. 10. Use drop wise from dropper bottle (ii) Disposable plastic gloves and safety glasses are to be worn at all times. Barite quality can have very large effects on mud properties.Section 3 Laboratory Testing Procedures 8. Continue to mix the whole mud for the remaining time in the hour i. The barite loading in the fluid will therefore be significant. especially at high mud weights.but if any occur mop up immediately. Adjusting pH (i) Unless the quantity of caustic soda is defined in the formulation.

5 9 4 5 8-9 4 9 Non-Treated Bentonite KCl. OCMA.temp II Barite. 50 % NaOH or KOH Caloflo 100. Hi -Temp. Driscal D. Haematite Idthin 500. Polytemp.Section 3 Laboratory Testing Procedures SUMMARISED MIXING PROCEDURE FOR HIGH TEMPERATURE WATER-BASED MUDS ORDER OF ADDITION Prehydrated Gel Salts Black Powders pH Adjustment Polymeric additives Weighting agent Dispersant Drilled Solids Add after Time (mins) 0 5 15 20 25 35 45 50 Addition time (mins) 1 1 5 5 1-2 1 1 Mix time Examples of typical products (mins) in the Dowell DF line. Polydrill. Hymod Prima . Micromax. Idperse XT Rev Dust. NaCl Calotemp. Hi . Soltex.

Section 3

Laboratory Testing Procedures
3.3.3 PROCEDURE DF/EAF/005 -Oil and Synthetic Based Muds

(350 ml - 1 Lab Barrel)

This procedure is generally applicable for the following drilling fluid systems; TRUDRILL INTERDRILL ULTIDRILL Oil based muds are extremely sensitive to shear history. Unlike WBM’s they require a critical amount of shear to develop the properties completely. A a) b) c) d) B. EQUIPMENT Balance: precision ± 0.1 g Hamilton beach mixer and cup Weighing boats Spatula ORDER OF ADDITION (unless otherwise requested)

1. Base Oil 2. Primary Emulsifiers E.g. TRUMUL and EMUL 3. Secondary Emulsifiers E.g. TRUSPERSE and FW 4. Organophillic Clay E.g. VISTONE and TRUVIS 5. Organo-polymers E.g. TRUFLO 100 6. Black powders E.g. INTERDRILL S, SOLTEX, TRUDRILL S 7. Lime 8. Brine 9. Weighting agent 10. Simulated drilled solids C. 1. PROCEDURE Place a Hamilton Beach cup on a balance. Add the required weight of Base oil to a Hamilton beach cup. Add the required weight of primary and secondary emulsifiers slowly using a syringe to the cup. Add the lime. Mix for 5 minutes on low speed (11,000 rpm ± 300 rpm) . Add the organophillic clay slowly into the vortex over a 1 minute period, ensuring that all the clay has completely dispersed and that none adheres to the sides of the mixing vessel or the mixer shaft. Mix for a further 4 minutes. Add polymeric additives slowly into the vortex over a 1 minute period. Mix for a further 4 minutes. Add black powders (gilsonite, asphaltics, lignites etc.) slowly into the vortex over a 1 minute period, ensuring that all the powder has completely dispersed. Mix for a further 4 minutes Add the brine phase (usually pre-dissolved calcium chloride in water) slowly into the vortex over a 2 minute period. Mix for a further 8 minutes. Add the weighting material (e.g.. Barite) slowly into the vortex over a 2 minute period. Mix for a further 8 minutes. Add the simulated drilled solids into the vortex over a 1 minute period. (E.g.. Rev Dust, Hymod Prima) Continue to mix the whole mud for the remaining time in the hour.

2.

3. 3.

4. 5. 6. 8.

Section 3

Laboratory Testing Procedures

9. Cover and allow to stand for 30 minutes before testing to allow the fluid to equilibrate and any entrained air to escape. 10. Test and age as required.

Safety Notes : (i) The mixing of fluids should be carried out in an enclosed mixing room, if possible, ensuring that the extraction system is operating. (ii) When testing base oils having flash points of 70°C or lower, the mixing temperature must be controlled at least 10°C lower than the flash point. Mixing of muds using crude oil with low flash points (< 20°C) is not allowed by this method. Procedural notes : ∑ Ensure temperature of fluid does not exceed 150 0F during the mixing process. ∑ Final mud formulations must be performed in duplicate to ensure reproducibility and ultimately reliability. SUMMARISED MIXING PROCEDURE FOR OIL AND SYNTHETIC BASED MUDS

ORDER OF ADDITION
Base Oil Emulsifiers/ wetting agents Organophillic Clay Polymeric additives Black Powders Lime Brine Weighting agent Drilled Solids

Add after Time (mins) 0 0 5 10 15 20 25 35 45

Addition time (mins) 1 1 1 1 1 2 2 1

Mix time Examples of typical products (mins) in the Dowell DF line. 4 4 4 4 4 8 8 19 HDF 200, Ultidrill, diesel Emul, Emul HT, Trumul, O/W, Trusperse, FL Truvis, Vistone Truflo 100, Alcomer , Dovamul Trudrill S, Interdrill S, Soltex, Gilsonite, Lignites Lime CaCl2 Barite, Micromax, Haematite Rev Dust, OCMA, Hymod Prima

Section 3

Laboratory Testing Procedures ROUTINE TESTING PROCEDURES
INTRODUCTION

4
4.1

The mud testing procedures used by Dowell are based on the API Recommended Practice 13B-1 First Edition 1st June 1995, for Standard Testing Procedures for Water Based Drilling fluids and API Recommended Practice 13B-2 Second Edition, 1st December 1995, for Standard Testing procedures for Oil based Drilling Fluids and API Recommended Practice 13J First Edition 1986, for Testing of Heavy Brines. API publications can be obtained from; API Publications Department 1220 L Street NW, Washington, DC 20005 - USA

fax : (1) 202 682 8537

4.2

API REFERENCES

(i) Tests applicable to both OBM and WBM - API recommended practices. 1. Mud weight (density) 2. Viscosity and gel strength 3. Filtration LTLP 3. Filtration HTHP 4. Water, oil and solids 5. Shear strength measurement Using Shearometer tube RP 13B-1 RP 13B-2 RP 13B-1 RP 13B-2 RP 13B-1 RP 13B-2 RP 13B-1 RP 13B-2 RP 13B-1 RP 13B-2 RP 13B-1 RP 13B-2 Page 5-8 Page 5-8 Page 9-11 Page 9-12 Page 12-13 Page 11-12 Page 13-15 Page 13-14 Page 16-18 Page 15-18 Page 39 Page 28

(ii) Tests specific to WBM - API recommended practices 1. Sand 2. Methylene blue capacity 3. pH 4. Chemical analysis 4.1 Alkalinity and lime content 4.2 Chloride content 4.3 Total hardness 4.4 Calcium 4.5 Magnesium 4.6 Formaldehyde 4.7 Sulphide 4.8 Carbonate 4.9 Potassium > 5000 mg/l 4.10 Potassium < 5000 mg/l 5. Resistivity RP 13B-1 RP 13B-1 RP 13B-1 RP 13B-1 RP 13B-1 RP 13B-1 RP 13B-1 RP 13B-1 RP 13B-1 RP 13B-1 RP 13B-1 RP 13B-1 RP 13B-1 RP 13B-1 Page 19 Page 20-21 Page 22-23 Page 24-26 Page 26 Page 26-27 Page 28 Page 29 Page 29-30 Page 30-33 Page 33-35 Page 35-37 Page 37-38 Page 40

(iii) Tests specific to OBM - API recommended practices 1. Chemical analysis of OBM 1.1 Alkalinity of whole mud 1.2 Whole mud chlorides 1.3 Whole mud calcium 2. Electrical stability RP 13B-2 RP 13B-2 RP 13B-2 RP 13B-2 Page 19 Page 19-20 Page 20 Page 20 Page 21-22

(iv) Additional procedures - API recommended practices

Inspection and Rejection 3. Removal of air or gas from Mud prior to testing 2.Section 3 Laboratory Testing Procedures RP 13B-1 RP 13B-2 RP 13B-1 RP 13B-2 RP 13B-1 RP 13B 2 RP 13B-1 Page 41 Page 43 Page 44 Page 44 Page 45 Page 45 Page 42-43 1. Rig site sampling 4. Drill pipe corrosion ring coupons . Sampling.

PROCEDURE .5 as for the standard mud balance procedure When the lid has been placed on the cup. pull the check valve up in the open position. is balanced by a fixed counterweight at the other end. 1. 4.ft. A level bubble is mounted on the beam to allow accurate balancing. 2.Mud Weight Determination The Mud Balance is used for mud weight determinations and is the recommended equipment ii the API 13B standard procedures for testing drilling fluids. whilst at the same time forcing the piston rod inwards. with a sliding weight rider free to move along the graduated scale. leading to inaccurate mud weight measurements on the standard mud balance.5 lb/cu.3. to free any trapped gas.3 Laboratory Testing Procedures PHYSICAL TESTING 4. 6. Approximately 50 pounds of force or greater should be maintained on the piston rod. Balance is achieved when the bubble is directly under the centre line. It is designed such that the mud cup. Follow steps 1 . 3. A EQUIPMENT Standard Mud Balance Pressurised Mud Balance B 1. 10 g/l). PROCEDURE . The balance operates in much the same way as standard mud balance except the lid of the mud cup has a check valve. The piston rod is then drawn up.Standard Mud Balance Instrument base must be set on a flat level surface Measure and record the mud temperature Fill the mud cup with the mud to be tested Replace cap until it is firmly seated. wipe the outside of the cup clean and dry. at one end of the beam. 5. Place the beam on the base support and balance it by using the rider along the graduated scale. . The pressurising plunger is similar to operating a syringe. By pressurising the mud cup the entrained air volume can be decreased to a minimum. Holding cap firmly on mud cap ( with cap hole covered ) wipe the outside of the cup until it is clean and dry.01 g/ml .Pressurised Mud Balance C A problem with many drilling fluids is that they contain considerable amounts of entrained gas. The plunger is filled by submersing the nose of the plunger in the drilling fluid with the piston rod in the completely inward position. thereby filling the plunger with fluid. The nose of the plunger is then placed into the female 'O' ring on top of the cap. 2. 3.1 PROCEDURE DFT/EAF/001 . 0. The sample is pressurised by maintaining a downward force on the cylinder housing in order to hold the check valve open.1 lb/gal ( or 0.0. The mud balance is accurate to within +/.Section 3 4. 4. insuring some of the mud is expelled through the hole on top.

e. Procedural notes : ∑ Ensure fluid is at room temperature ( 77 deg F) prior to testing. disconnect the plunger and weigh the fluid as in step 6 of the standard mud balance procedure. i. . Laboratory Testing Procedures The check valve in the lid is pressure actuated. Once the check valve is closed. closing when a pressure is applied.Section 3 5. 6. The valve is therefore closed by gradually easing up on the cylinder housing while maintaining pressure on the piston rod.

Re-stir the mud for 10 seconds and then allow to stand for 30 minutes. 9. The outer cylinder or rotor sleeve is driven at a constant rotational velocity. 3. Wait for dial reading to settle before taking the reading. 11. Dispose of waste mud in container provided in the Drilling Fluids Laboratory.220 0F PROCEDURE Pour mud sample into sample cup until it reaches the level line. Pull switch at back right towards the operator. 6. Stir mud at high speed for 10 seconds and then allow to stand for 10 seconds. NOTE: All gel strength readings are reported in lb/ 100 sq. 7. bob. 10. 6. A a) b) c) d) B 1. 100. and the dial attached to the bob indicates displacement of the bob. Mud cup Stopwatch Thermometer 32 .Section 3 4. Push switch located to the back right away from the operator to change rpm to 300 and record the dial reading as above. The rotor sleeve should now be rotating at 300 rpm in the mud sample. and rotor sleeve immediately after use. The rotation of the rotor sleeve in the fluid produces a torque on the inner cylinder or bob. This is the standard procedure recommended by API 13B for field testing water based drilling fluids.2 Laboratory Testing Procedures PROCEDURE DFT/EAF/002 . powered by a two speed synchronous motor to obtain speeds of 3. Turn on viscometer at mains and ensure the gear knob on top of instrument is pushed completely down and that switch located to the back right is pushed away from the operator. The rotor sleeve should now be rotating at 600 rpm in the mud sample. Wash and dry the sample cup. . For a more extensive rheogram the torque at rpm's 100 and 200 can also be measured by pulling the gear knob completely upwards. Instrument constants have been adjusted so that the Bingham plastic viscosity and yield point can be obtained by using the readings at 300 rpm and 600 rpm. Rotate at 3 rpm and record the reading on the dial. 110 volt. 12.Viscosity and Gel Strength Drilling fluid is contained in the annular space between two concentric cylinders. 200. Rotate at 3 rpm and record the reading on the dial. Wait for temperature to increase and settle at 120 Deg F before measuring the rheology. 4. Record the temperature of the mud sample Immerse bob and rotor sleeve into the mud until it reaches the scribed level on the rotor sleeve ( just over the two holes ) by raising the viscometer stand. 2. Locate sample cup in viscometer stand using the 3 locating pins on the bottom.ft or Pa . EQUIPMENT Fann 35. this is the 10 second or initial gel strength. this is the 30 minute gel strength. 8. Rotate at 3 rpm and record the reading on the dial. 5. Re-stir the mud for 10 seconds and then allow to stand for 10 minutes. this is the 10 minute gel strength.3. 300 and 600.

200 rpm reading PV = 300 rpm reading .6 rpm reading 3.32 log (600 reading / 300 reading) 600 reading / 1022 n Note: If the 600 rpm reading is off scale then the PV and YP can be calculated as follows.Plastic Viscosity 600 rpm reading / 2 (2 * 3 rpm reading) . YP = ( 2 x 100 rpm reading) .300 rpm reading Plastic Viscosity (PV) Centipoises (cP) Yield Point (YP) (lb/100 ft2) Apparent Viscosity Centipoises (cP) Yield Stress (YS) Power Law Index (n) Consistency Index (K) (lb/100 ft2) = = = = = 300 rpm reading .YP .Section 3 Laboratory Testing Procedures C CALCULATION = 600 rpm reading .

Section 3 4.Whatman No 50 paper) c) Low Pressure Nitrogen supply (100 psi) d) Stop Clock e) 10 and 25 ml measuring cylinders C 1. At the end of 30 minutes close valve and measure the filtrate volume in mls (cc's) per 30 minutes as the API filtrate. Fill cup to 3/4 full. Save filter paper handling with care and wash filter cake with a gentle stream of distilled water. for ionic analysis by FIM and/or titration techniques. Report any other observations.7. 6. discard mud into mud waste container only (located in Drilling Fluids Lab). CALCULATION API FLUID LOSS RELATIVE API FLUID LOSS * SPURT LOSS * = 30 min Reading = (30 min Reading . flexibility etc. 3. Measure and report the thickness of the cake to the nearest 1/32" (0. 4. and the initial mud temperature in degrees F at the start of the test. 2. 9. Insert filter paper on top of 'O' ring Tighten lid by seating and twisting through 90 ° and hand tightening screw. PROCEDURE FOR FANN 128L. Disassemble the cell. Insert neoprene 'O' ring (1/16") until seated tightly.5” b) OFI specially Hardened Filter paper . Open valve and start stop clock. 5. hardness.RELATIVE API FLUID LOSS 7.8 mm). such as texture. IN-SERIES FILTER PRESS Invert filtration cup and place finger over nozzle whilst filling cup with mud. D Relative API Fluid Loss is corrected for spurt loss prior to cake formation . SAVE the filtrate when required. Close the relief valve by pushing inwards and adjust regulator so that a pressure of 100 psi (+/5 psi ) is obtained.in (Alternatively . 11.5 min reading ) x 2 = API FLUID LOSS . colour.3. compressibility. Invert cell and place filtration cell in mounting assembly Place graduated measuring cylinder under drain tube to receive filtrate.Low Temperature/Low Pressure Filtration The low pressure filter press is a static filtration procedure recommended by the API 13B standard procedures for testing drilling fluids.Diameter 3” x Height 2.3 Laboratory Testing Procedures PROCEDURE DFT/EAF/003 . 8. 10.07 sq.Filtration Area 7. A OPERATING PARAMETERS 100 psi Nitrogen for 30 minutes B EQUIPMENT a) Filtration Cell .

4. to allow for thermal expansion.High Temperature/High Pressure 4. Once the sample has reached the desired temperature.5” / Filtration Area 4. 6. or as specified by an operator.5 degrees F. Invert cell and place in filtration mounted heated jacket assembly. 10. Open the bottom valve and start the stop-clock to start filtration experiment. The time for heating the mud sample to the target temperature should not exceed 60 minutes. fill up cell with mud to within 0.5" of the 'O' ring groove. 9. cautiously reduce the pressure by drawing off a portion of the filtrate from the bottom of the receiving vessel. 8.3. B a) b) c) d) e) C 1. Apply 100 psi to both ends of the HPHT cell with the valves still closed. A OPERATING PARAMETERS 500 psi differential pressure Nitrogen for 30 minutes at a temperature of 300 degrees F. 12. Tighten grub screws evenly using the Allan key provided. Insert a thermometer into the HPHT cell. EQUIPMENT HTHP Filtration Cell .0” OFI specially Hardened Filter paper .Diameter 2. 3.4 Filtration The high pressure / high temperature filter press is a static filtration procedure recommended by the API 13B standard procedures for testing drilling fluids at elevated temperatures and pressures. 7.91 sq. 2. With stem valve closed on bottom of cell.Section 3 Laboratory Testing Procedures PROCEDURE DFT/EAF/004 . increase the pressure of the top pressure unit to 600 psi. Open the top valve to apply 100 psi to the mud while heating to prevent the mud from boiling prior to reaching the target temperature.Diameter 3” x Height 3. again ensuring that locking pin is inserted. Collect the filtrate for 30 minutes maintaining the temperature to within +/. Insert filter paper into the cell followed by the bottom cell plate assembly over the filter paper and twist to align with the safety locking lugs. Place the pressure unit on top valve and lock into place using a locking pin Lock the bottom pressure unit to the bottom valve into place. . 5. If the back pressure rises above 100 psi during the test. Ensure all stem valves are tightly closed.in High Pressure Nitrogen supply (600 psi) Stop Clock 10 and 25 ml measuring cylinders PROCEDURE Turn on heated jacket at the mains and insert a thermometer into the jacket and leave to preheat. 11.

8 mm). discard mud into mud waste container only. 15. Disassemble the cell. colour. one can SAVE the filtrate for ionic analysis. hardness. so cool cell to room temperature in a water bath and then bleed off the pressure slowly by opening the valves. Bleed the lines using the relief valves provided. Laboratory Testing Procedures Once the test has finished close the top and bottom valves and shut off the pressure supply from the regulators. 16. Allow filtrate to cool for 30 minutes and then draw off into a graduated 20 ml measuring cylinder and read volume. Report any other observations. Save filter paper handling with care and wash filter cake with a gentle stream of distilled water or base oil. 17. CAUTION . 14. Measure and report the thickness of the cake to the nearest 1/32" (0. such as texture. When filtering water-based muds.Section 3 13.the cell still contains 500 psi pressure. flexibility etc. .

The percent solids. 10 ml. both suspended and dissolved. The volume of oil and water collected is noted and the percent oil. water and solids present in the sample calculated. 5. The volume of liquid. A graduated measuring cylinder is put underneath the condenser discharge. is determined by subtraction of the total liquid from 100%.Section 3 Laboratory Testing Procedures PROCEDURE DFT/EAF/005 . a) b) c) d) e) f) g) h) i B 1.Retort .3. The vapours are then passed through a condenser and collected in a calibrated cylinder. The void space above the calibrated retort cup is filled with steel wool. A EQUIPMENT Three retort sizes are available in the Drilling Fluids Laboratory. A carefully measured sample of mud is placed in a steel cell and then heated until it vaporises. Suspended solids are weighting materials and other low gravity solids such as mud additives and cuttings . Oil and Solids 4. excess oil residue can be removed using lengths of pipe cleaners. The retort is then sealed. 20 ml and 50 ml.g.[Vw+ Vo] = (Mud SG x 100) . water and oil can then be calculated in percent. the condenser attached and the equipment placed into the heating jacket. 3. CALCULATION Volume % water (Vw) Volume % oil (Vo) Volume % solids (Vs) Average SG of Solids = (ml H2O / ml sample) x 100 = (ml Oil / ml sample) x 100 = 100 . 6. The latter is the most commonly used due to its greater precision and accuracy. calibrated retort cup (50 ml). C Sample cup Thermostatically controlled heating element Liquid condenser Pyrex measuring cylinder (50 ml) Fine steel wool Pipe cleaner High temperature silicone grease Defoaming agent Spatula PROCEDURE A homogeneous sample of de-aerated mud which has cooled to approximately 80°F is added to a clean. salt). 2. 7.Water.(Vw+ Vo) Vs The volume % solids includes both suspended solids and dissolved materials (e. Each unit consists of a. The equipment is allowed to cool and solids removed from the retort cup by means of a spatula. The retort heater is switched on and heating is continued until 10 minutes beyond the point at which no more vapour droplets fall from the condenser.5 A retort is used to determine the quantity of liquids and solids in a drilling fluid. 4. dry.

6 Laboratory Testing Procedures PROCEDURE DFT/EAF/006 .Section 3 4. 3.3. Pour the suspension through the clean. 4. By tapping the side of the screen the pouring of the mud through the screen may be facilitated. PROCEDURE Fill the tube with mud to the mark labelled “Mud to Here”. 2. Wash the sand retained on the screen with a stream of base fluid. The material retained on the screen should not be manually pushed through as this will give erroneous results and may also damage the sieve itself. Cover the mouth of the tube with the thumb and shake the tube vigorously. Allow the sand to settle. being careful to remove all solids out of the tube by flushing with base fluid back through the same mesh screen. Wash the apparatus thoroughly after use. then add base fluid to the mark “Base Fluid to Here”. Record the quantity of sand settled in the graduated tube as the sand content of the mud in percent by volume. 5. dry mesh screen. Fit the funnel upside down over the top of the sieve.Sand Content The sand content apparatus consists essentially of a 200 mesh sieve. A 1. a funnel and a glass measuring tube calibrated to read the percentage of particles larger than 74 microns in the mud. . invert slowly turning the tip of the funnel into the mouth of the tube and wash the sand back into the tube with some clean base.

pH = 4. its tolerance to contaminants and allows a geochemical insight into the reactivity of the lithologies being drilled.05 molar in water. dissolved salts and chemicals.) 2. Soft tissues: to blot electrodes. Gives 10. pH = 10. Electrode system: A combination system of a glass electrode for sensing [H+] ions and a standard voltage reference electrode (silver/silver chloride). An acid can be defined as a substance which dissociates in aqueous solution to give hydrogen [H+] ions.H +and OH - Field measurement of drilling fluid (or filtrate) pH and adjustments to the pH are fundamental to controlling water-based drilling fluid properties.02066 molar and disodium hydrogen phosphate at 0.4. whilst a base or alkali gives [OH-] ions. This method is accurate and reliable.0: sodium carbonate at 0.1 PROCEDURE DFT/EAF/007 . c) 1. [H+] .0: Potassium dihydrogen phosphate at 0. The recommended method for pH measurement is with a glass electrode pH meter. Gives 7. Rugged pH instruments are available that automatically temperature compensate the slope and are preferred over the manually adjusted instruments. Complex equilibria exist within aqueous systems that if perturbed can have either a positive or negative affect on the overall properties of the fluid. The term “pH” denotes the negative logarithm of the hydrogen ion.00 pH at 75°F.01 pH at 75°F. and dark coloured liquids cause serious errors in pH paper values. d) e) f) Distilled or deionised water: in spray bottle.) Note: The shelf life of all buffers should not exceed six months before disposal. Note: Colour matching pH paper and sticks are used for field measurements. 32-220°F (0-105°C). Date of preparation of the buffer should be shown on bottles used in the field. Bottles should be kept tightly stoppered.pH . Gives 4.5 pH units. but are not recommended as they are only reliable in very simple water base muds.02934 molar in water. A a) b) EQUIPMENT pH Meter: millivolt range potentiometer calibrated to show pH units for measuring the potential between a glass membrane electrode and a standard “reference” electrode.025 molar and sodium bicarbonate at 0. constructed as a single electrode. being free of interferences if a high quality electrode system is used with a properly designed instrument.025 molar in water. .Section 3 Laboratory Testing Procedures 4. activity in aqueous solutions (activity and concentration are equal only in dilute solutions). Mud solids. pH expresses acidity or alkalinity of an aqueous solution.0: potassium hydrogen phthalate at 0. Readability is normally about 0. pH = 7.) 3.4 CHEMICAL TESTING Chemical analysis of the aqueous phase of a drilling fluid is of paramount importance in understanding the stability of the fluid. Buffer solutions: Three solutions to calibrate and set the slope of the pH meter prior to sample measurement. 4. Thermometer: glass.01 pH at 75°F.

but is more accurate than indicator solution.c.c. distilled water. Mud additives. The data collected can also be used to estimate the concentrations of hydroxyl (OH-). CO3—and OH- 4.) j.g. Hypodermic syringe: 2. add 0. Mf Measure one or more c.4. The source and nature of the alkalinity is often as important as the fact that some alkalinity exists. PROCEDURE . Hydroxyl ions Hydroxyl + Carbonate Carbonate Carbonate + bicarbonate Bicarbonate A a.) g. Knowledge of the mud and filtrate alkalinity is essential to ensure proper control of mud chemistry. drop by drop from the pipette. the endpoint can be taken when the pH drops to 8. particularly some deflocculants.) B 1.2 Alkalinity can be considered as the acid-neutralising power of a substance.Section 3 Laboratory Testing Procedures PROCEDURE DFT/EAF/008 .) k.Filtrate Alkalinity: Pf. Titration vessel: 100-150 c. pH meter: optional.5 c. while alkalinity resulting from carbonates and/or bicarbonates may have adverse effects on mud performance and stability. Add two or more drops of phenolphthalein indicator solution. and one 10 c.Alkalinity . If the sample is so coloured that the indicator colour change is masked.) f. preferably white.c. carbonate (CO3-2) and bicarbonate (HCO3-) ions in the drilling fluid.c. as measured with a pH meter. while stirring. require an alkaline environment to function properly. Alkalinity measurements can be made on either the whole mud (designated with the subscript m) or on the filtrate (subscript f).) e.) b.) i. ethyl or methyl alcohol made up to 100 c. Methyl Orange Indicator solution: 0.) d. Alkalinity arising from hydroxyl ions is generally accepted as being beneficial. EQUIPMENT Sulphuric acid solution: standardised 0. with distilled water. of filtrate to the titration vessel. Mud stable and in good condition Stable and in good condition Unstable but can be controlled Stable but difficult to control Unstable and very difficult to control . Distilled water free of carbon dioxide (by boiling) Stirring rod. 2.2 g dissolved in 100 c.3.02 g in 100 c. until the pink colour disappears.) c.c.c. e.c.c.c.HCO3-. If the indicator turns pink. Bromophenol Blue: 0.02 Normal (N/50) Phenolphthalein indicator solution: 1 g dissolved in 60 c.02N sulphuric acid. Volumetric pipettes: 1 c. distilled water (instead of methyl orange for dark filtrates.c. Graduated pipettes: one 1 c.) h.

c. while stirring.c.c. Report the phenolphthalein alkalinity of the mud. C 1. Report the methyl orange alkalinity of the filtrate. Dilute that mud sample with 25-50 c.02N sulphuric acid.c. 2. of filtrate required to reach the methyl orange end point (including that amount for the Pf endpoint).c.02N acid required per c. of mud into the titration vessel using a syringe. until the pink colour disappears. 5.c. it can be taken when the pH drops to 8. Add 0. If the endpoint colour change cannot be seen. of mud.02 N standard sulphuric acid until the pink colour disappears.0 c. Mf as the total c. . drop by drop from the pipette.3 as measured by a pH meter. while stirring. of distilled water (free of carbon dioxide by boiling). 4. of filtrate. add two or three drops of methyl orange indicator changes from orange to pink. as the number of c. acid required per c. 3. To the sample which has been titrated to the Pf end point. The endpoint can also be taken when the pH of the sample drops to 4.02 N acid per c. PROCEDURE .3 using a pH meter. Pf.Mud Alkalinity: Pm Measure 1. of 0. Pm. Laboratory Testing Procedures Report the phenolphthalein alkalinity of the filtrate. Add 4-5 drops of phenolphthalein indicator solution and.c. of 0.c.Section 3 3. titrate rapidly with 0. as the number of c.

+ 2Ag+ ◊ AgCl (white precipitate) + NO3◊ Ag2CrO4 (orange-red precipitate) The end point is detected with Potassium Chromate. add acid drop by drop.3 This standard method (Mohr’s method) consists of titrating all chlorides present in the filtrate and expressing the result in terms of sodium chloride.7910 g/l (0. add an additional 2 mL of acid and stir.c. Calcium Carbonate: precipitated. In practice.ions have been removed from solution. preferably white. potassium chromate. an orange-red precipitate. Graduated pipettes: one 1 c. Store in amber or opaque bottle. EQUIPMENT Silver nitrate solution: 4. PROCEDURE Add one or more c. Then add 1 g of calcium carbonate and stir (or until effervescence stops). Sulphuric or nitric acid: standardised 0. The excess Ag+ ions present after all the Cl. the result obtained (expressed in NaCl). Stir while adding silver nitrate solution drop by drop. react with chromate to form silver chromate. Potassium Chromate Indicator solution: 5 g/100 c. chemically pure grade. and in an alkaline medium silver oxide or silver carbonate precipitate.Chloride Determination 4. for example in the presence of calcium and magnesium chlorides. until the colour changes from yellow to orange-red and persists for 30 seconds. while stirring.c. in an acid medium the silver chromate dissolves. distilled water and 5-10 drops potassium chromate.0282 N or equivalent to 0. of 60% alcohol in water solution. in the presence of an indicator. Add 2-3 drops of phenolphthalein solution. of filtrate to the titration vessel. A a) b) c) d) e) f) g) h) i) B 1. Titration vessel: 100-150 c. it is first acidified with nitric acid.4.). Note: This titration must be carried out in a neutral medium because.+ AgNO3 CrO42. The reaction occurs in two steps: Cl. as the filtrate is neutral or alkaline. If the indicator turns pink.c.c. The addition of the nitric acid has the advantage of discolouring the filtrate (partially). This explains why in some cases. The chlorides are precipitated in the form of silver chloride.c.c.to a very small value.02 N (N/50) Phenolphthalein indicator solution: 1 g/100 c. and One 1-c. until the colour disappears.c. Stirring rod. Distilled water: free of carbon dioxide by boiling.Section 3 Laboratory Testing Procedures PROCEDURE DFT/EAF/009 . Record the number of mL silver nitrate solution required to reach the endpoint. can give concentrations greater than the solubility of NaCl. water. . Add 25-30 c. then neutralised with calcium carbonate. If the filtrate is deeply coloured. Since AgCl is less soluble than Ag2 CrO4 the latter cannot form permanently in the mixture until the precipitation of AgCl has reduced the Cl.001 g chloride ion/c.c. 2.

c. 10000 x (0. The factor 1.65) x (Chloride.282 N silver nitrate solution equivalent to 0. mg/l = (Chloride.000 is then changed to 10.0282 N silver nitrate. mg/l) ___ Specific gravity of filtrate (1. (mg/l) = 1000 x (0.01 g/c.000 mg/l.000. calculated as follows: Chloride. mL) filtrate sample mL .Section 3 Note: C Laboratory Testing Procedures If the chloride ion concentration exceeds 10.282 N silver nitrate Chloride.282 N silver nitrate. (mg/l) = To convert units: Chloride. CALCULATION Report the chloride ion concentration of the filtrate in mg/l. (ppm) = Salt (NaCl). mg/l). use 0. mL) filtrate sample mL Or when using 0.

Stir while adding EDTA solution drop by drop. (mg/l) = 400 x (0.Total Hardness Determination 4.02 N EDTA (0. Stirring rod. EDTA-Na + Ca++ + Mg++ -------> EDTA. of filtrate to the titration vessel. until the colour changes from red to blue and persists for 30 seconds. calculated as follows: Total Hardness as calcium.01 M) Ammonia Buffer* in dropper bottle Manver Indicator (solution or crystals) Masking agent**: 1:1:2 mixture by volume of triethanolamine : tetraethylenepentamine : water Deionised water: free of carbon dioxide by boiling. Divalent cations such as these tend to have a detrimental affect on clay and polymer based drilling fluid additives and systems. PROCEDURE Add one or more c. For this reason hardness is typically kept to a minimum and close monitoring of their aqueous concentrations is required. A wine red colour will develop if either calcium or magnesium ions are present. * Ammonia buffer = 54 g Ammonium chloride and 400 mL Ammonium Hydroxide (15 N) made up to 1000 mL with deionised water. preferably white. 2 mL and 5 mL Titration vessel: 100-150 c.4. (mg/l) = Total Hardness as CaCO3. C Report the Total Hardness as calcium ion concentration of the filtrate in mg/l. B 1. it combines to form a complex whose end-point is determined by a suitable indicator.4 The hardness of water or mud filtrate is due primarily to the presence of calcium and magnesium ions. Dilute with approximately 50 mL of deionised water. Record the number of mL EDTA solution required to reach the endpoint.c. When EDTA (sodium salt of ethylene-diaminetetracetic acid) is added to aqueous solutions containing calcium and/or magnesium. mL) filtrate sample mL . Add 4 drops of Ammonia buffer and 2 drops (or crystals) of manver indicator.Section 3 Laboratory Testing Procedures PROCEDURE DFT/EAF/010 . ** 1mL of Masking agent should be added if soluble iron is suspected to be present. Graduated pipettes: one 1 mL.Ca + EDTA.02 N EDTA. CALCULATION 2.Mg + Na+ A a) b) c) d) e) f) g) h) EQUIPMENT 0. mL) filtrate sample mL 1000x (0.c.02 N EDTA.

Calcium Hardness Determination This method allows the selective determination of calcium ions in aqueous solutions. CALCULATION 2. preferably white. calculated as follows: Total Hardness as calcium.02 N EDTA. When EDTA (sodium salt of ethylene-diaminetetracetic acid) is added to aqueous solutions containing calcium and/or magnesium. Add 2 drops of KOH buffer and several grains of Calver II indicator. A wine red colour will develop if calcium ions are present. EDTA-Na + Ca++ -------> EDTA.4. of filtrate to the titration vessel. B 1.02 N EDTA 8N Potassium Hydroxide Buffer (KOH) Calver II Indicator (crystals) Masking agent*: 1:1:2 mixture tetraethylenepentamine : water by volume of triethanolamine : Deionised water: free of carbon dioxide by boiling. PROCEDURE Add one or more c.Calcium Hardness .Ca + Na+ A a) b) c) d) e) f) g) h) EQUIPMENT 0. Swirl to mix.Section 3 4. Stir while adding EDTA solution drop by drop. mL) filtrate sample mL Note: The magnesium hardness = Total Hardness .c. mL) filtrate sample mL 1000x (0. Record the number of mL EDTA solution required to reach the endpoint. it combines to form a complex whose end-point is determined by a suitable indicator. (mg/l) = 400 x (0. (mg/l) = Total Hardness as CaCO3. * 1mL of Masking agent should be added if soluble iron is suspected to be present.c. Stirring rod. Graduated pipettes: one 1 mL.5 Laboratory Testing Procedures PROCEDURE DFT/EAF/011 . Dilute with approximately 50 mL of deionised water. 2 mL and 5 mL Titration vessel: 100-150 c.02 N EDTA. until the colour changes from red to blue and persists for 30 seconds. C Report the Total Hardness as calcium ion concentration of the filtrate in mg/l.

Total soluble carbonates include CO2 and the carbonate (CO32-) and bicarbonate (HC03-) ions. (for acid). prolonged flow will cause the regulator to perform erratically. Sulphuric Acid: approximately 5N. Octanol defoamer in a dropper bottle. converting all carbonates to CO2. Note: Nitrogen is preferred over nitrous oxide as the carrier gas. sulphide analysis) the regulator.c.6 Laboratory Testing Procedures PROCEDURE DFT/EAF/012 . The Gas Train separates the gas from the liquid. CH-308-01) Drager One litre Alcotest Gas Bag: (No 7626425) Drager Multigas Detector Hand Operated Vacuum Pump. A EQUIPMENT The following materials are required to perform the analysis of total soluble carbonates using a solids-free filtrate sample.Soluble Carbonates Determination The concentration of soluble carbonates in a drilling fluid filtrate can be determined more accurately and with less interference’s with a gas train than by those measurements involving alkalinity.0 cc (for sample). Add 5 drops of Octanol defoamer to chamber 1.01 %/a .(No. Hypodermic syringes: one 10 c. and the gas stream is collected in a one litre gas bag (to allow CO2 to mix uniformly) and subsequently drawn through a Drager tube at a fixed flow rate. an inert gas supply (N2 or N2O) with pressure regulator. Hypodermic needles: two 1.e. A reaction between CO2 and a hydrazine chemical causes a crystal violet indicator to turn purple. a) b) c) d) e) f) g) h) i) j) k) Garrett Gas Train: consisting of a transparent plastic gas train. The Drager tube responds to CO2 by progressively staining purple along its length. with the top removed. Model 31 Stopcock: (2-way bore): 8 mm glass with Teflon plug. a floating ball flowmeter and a Drager tube.Section 3 4. Mud filtrate is acidified in a Garrett Gas Train. dry and on a level surface. Because nitrous oxide cools upon expansion and chills the diaphragm in the regulator. and one each 10 cc. Inert Carrier Gas: Nitrogen (N2) bottle with low pressure regulator (preferred). Install the top of the gas train and hand tighten evenly to seal all O-rings. reagent grade. 4.5 inch (38 mm) with 21 gauge needles.4.5 cc and 1. Flexible tubing: Type inert to carbon dioxide Drager CO2 Analysis Tube: marked CO2 0. Add 20 cc deionised water to chamber 1. B PROCEDURE 1. tubing and dispersion tube should be purged with nitrogen or nitrous oxide at this time. Note: If carbon dioxide has been used as the carrier gas in the previous test (i. Make sure the gas train is clean. 3. . or Nitrous oxide (N20) cartridges. 2. 2. The stain length is proportional to the total carbonate in the filtrate. which is then evolved by bubbling an inert carrier gas through the sample.

01 %/a Tube Factor (see Calculation at end) 25.01 %/a CO2 0.75 50 . Attach the Drager hand pump to the downstream end of the Drager tube. Flow carrier gas through the train for one minute to purge air from the system. Operate the pump and count the number of strokes until the bag is empty.1500 250 . 16.Section 3 Laboratory Testing Procedures 5. Slowly inject 10 mL of sulphuric acid into Chamber 1. To check the pump alone. insert a sealed Drager tube into the pump opening and depress bellows. install flexible tubing from the stopcock and bag onto outlet of chamber 3. shut off the flow and close the stopcock. Release the pump so that the gas flows out of the bag and through the Drager tube. Check for leaks in the unit. 13. the pump will remain depressed for several minutes. Break the tip of each end of the Drager tube.0 5. 14. Sample Volume mL 10. Carbonate range mg/L 25 .0 1. suing a clean syringe and needle. Outlet and install it onto the upstream end of the Drager tube. and record the stain length in units marked on the Drager tube. To do this. 15. With the bag fully collapsed. 10. When the bag is firm to the touch (do not burst it!). Fully collapse the gas bag and simultaneously check for leaks. Open stopcock on the gas bag. Observe the purple stain on the Drager tube if carbon dioxide is present in the bag. Inject a measured volume filtrate into chamber 1 through the septum with a syringe and needle. 7.7500 11.000 25. Remove the tubing from Chamber 3. Adjust the dispersion tube to approximately ¼” (5 mm) off bottom.000 25. . With the regulator backed off. Fully depress and release the hand pump. 6. Gently shake the gas train to mix the acid with the sample.0 Drager Tube Identification CO2 0. 8. It will remain depressed if the pump does not leak. With steady hand pressure fully depress the hand pump. connect the gas bag and stopcock to the hand pump (use a used Drager tube as connection and start with the bag essentially empty).. See table below.000 9. connect the carrier gas supply to the glass dispersion tube of chamber 1 using flexible tubing. Open the stopcock on the bag.01 %/a CO2 0. (Include the faint blue tinge in the purple stain length reading) 12. When the bag is completely empty and free of leaks. Restart the gas flow and allow the gas bag to fill steadily during a 10 minute interval. through the rubber septum.

0 . which are generally composed of varying proportions of these clay minerals.7 Shales The cation exchange capacity (CEC) is a measure of the potential reactivity of the clay components of mud solids or shales. Dilute to approximately 50 ml with distilled water and stir. 6. Leave to simmer for about 10 minutes.) 1 ml of the 5 N Sulphuric acid using a clean syringe. Place conical flask on a hotplate and heat gently until simmering. After each addition dip the end of the stirring rod into the solution and apply a drop to the filter paper. reported in lb/bbl or meq/100 g.0 mls of mud into the 125 ml conical flask.200 80 . Add 1ml increments of the methylene blue indicator via a burette and swirl the flask vigorously for 30 seconds.Methylene Blue Test for Mud and 4. Vermiculites Smectites Illites Kaolinite 120 .10 10 . The CEC of shales can generally be classed as follows.150 10 . Whatman No 4 2 x 5ml Syringes 50 ml Burette and clamp stand PROCEDURE (Mud Solids) Measure 2. Add a.74 USP grade) 3% Hydrogen Peroxide 5 N Sulphuric Acid 125 ml Conical Flask 25 ml Graduated Measuring Cylinder Hot plate Stirring Rod Filter paper. 5. Swirl mixture gently to ensure mud solids are completely dispersed within the mixture. b. 4.30 > 30 meq/100g meq/100g meq/100g meq/100g . Cation exchange capacities in clay minerals is not a very precise or fundamental quantity. Some reported CEC’s are as follows.20 20 . as it varies significantly with pH. Clay minerals all exhibit ion exchange behaviour to some degree. 3. EQUIPMENT Methylene Blue Solution ( 3.4. Isomorphous substitution of various cations onto a clay surface depends on the number of available exchange sites per unit weight of solids.Section 3 Laboratory Testing Procedures PROCEDURE DFT/EAF/0013 . Non-dispersive Moderate dispersion Dispersive Highly dispersive A a) b) c) d) e) f) g) h) i) j) B 1.) 15 ml of the 3 % hydrogen peroxide using a measuring cylinder. 2.40 1 -10 meq/100g meq/100g meq/100g meq/100g 80 % of all sedimentary rocks are shales.

The end point is reached when the colour of the blue solids containing droplet migrates away from the nucleus to form a light blue/turquoise halo. Grind shale using a pestle and mortar Weigh 0. E PROCEDURE (Shale) Dry shale at 220 Deg F in an oven for 16 hours. Once you reach the end point it is important to keep stirring the mixture and dropping further solution onto the filter paper to ensure the end point is persistent and has actually been reached. 8.Section 3 Laboratory Testing Procedures 7. 3. Cation exchange is a time dependent process and the solution will go on reacting if all the sites have not been completely exchanged. 2.95 . CALCULATION Bentonite (equivalent) ppb = mls of methylene blue solution X 2.8 in the Mud Solids procedure above. CALCULATION CEC (meq/100g) = mls of methylene blue solution x 1.57 g of powdered shale into the conical flask and repeat steps 2 .5 C D 1.

Worcester. (600 ml beaker. It should be noted that detailed procedures for certain analytical techniques are not given in this manual where a dedicated manual for a specific technique is available.05 . A INSTRUMENT SPECIFICATIONS Malvern Instruments Ltd.550 µm Laser Diffraction using Fraunhofer and/or Mie theories Liquid suspensions only. It was chosen not only for its small “footprint”.1 NON-ROUTINE TESTING PROCEDURES INTRODUCTION Non-routine testing procedures are defined as those which may not be applicable to an EAF district drilling fluids laboratory as the specialised analytical equipment required may not be available. All these procedures are not recognised by the API testing procedures and in most cases have been developed by Dowell technical services to enhance the regional testing capabilities. which is adequate for most oil field applications./FAX . UK. Spring Lane South.Particle Size Analysis (PSA) The Malvern Mastersizer Micro Plus. an instrument based on the low angle laser light scattering (LALLS) is the EAF recommended particle size analyser.05 µm to 550 µm.Section 5Non-Routine Laboratory Testing Procedures 5 5. due to its novel folded optical configuration. Both EATC and in most cases the UKI Aberdeen laboratory can perform any of the following tests on submission of a “Laboratory Analysis Request (LAR) “ form. The instrument is capable of measuring particles in the range of 0. : Particle Size Range : Technique : Sample Type : Operational Control : Sample Dispersion : Weight : Footprint : . 80 ml small volume dispersion unit or 5 ml directly via syringe injection) Computer controlled (P. if required. An ultrasonic probe is also fitted to the unit for breaking up any aggregates that may be present in a sample prior to an analysis. Tel.C.. More detailed procedures can be obtained through EATC by request. WR14 1AT.) with manual overrides for flow rate and ultrasonication Mechanical flow loop and Ultrasonic Probe 32 kilograms 500 mm * 325 mm Manufacturer : Instrument : Model No. but also because of several technical advances in the collecting and processing of data.2 PROCEDURE DFT/EAF/014 . 5.01684 892456/892789 Mastersizer Micro Plus MAF 5001 0. Malvern.

4. Speeds in excess of this create excessive noise and can result in cavitation and bubble formation whereas significantly lower speeds may result in not all of the heavier solids being carried through the sampling system.Document Sample Details Enter desired sample name 5. press the on button and allow the motor to come up to speed. 17. For example the RI of Ultidrill is 1. It is necessary to set the Mastersizer and start its operation before moving on to the fourth dialogue box as this will start the sampling process. 10. Enter any notes e. date. To start the operation click on the fourth dialogue box. Put approximately 500ml of clean base fluid into a beaker and place under the instrument motor. press the space bar. 19. 7. . This will start the Laser Alignment. 11. 21. 2. if known. PROCEDURE Connect the Malvern Mastersizer to a PC by means of a 9-pin cable Malvern software should be installed onto the PC according to the installation procedures on the disk Ensure that both the Mastersizer and the PC are turned on The Mastersizer software includes a row of dialogue boxes at the top of the screen. The machine is now set up and ready to sample. 20. time and any other relevant details 14.4381.g. Analysis and Presentation Accept default settings (Internal-Micro Sample Dispersion Unit) (Instrument Port 1) Set up Analysis . 8. 6.Section 5Non-Routine Laboratory Testing Procedures B 1. 9. Click on the first dialogue box .Set-up Range. 16. The recommended motor speed is 2000rpm. 18. 3. Accept other default settings Set up presentation . We are looking for a laser power in the region of 70 for the first laser and in the region of 6 for the second laser. Follow the on screen instructions To start the operation.Open a Sample File and Load a Record Enter the desired file name and click on OK Click on third dialogue box . sample source. 12.Enter particle density if known (SG of sample) and the refractive Index (RI) of the base fluid. Lower the motor down into the fluid taking care that the suction holes are fully immersed but that the motor does not touch either the bottom or sides of the beaker On the instrument control panel. Click on OK 15. Setting up the software to run an analysis sample is simply a matter of working through the first four of these dialogue boxes in turn and providing the information requested. 13.Load default settings Click on second dialogue box .

(Clicking on the box “Pause after each stage” will automate the set-up procedure. background and sample analysis will proceed automatically without the need to press the space bar between each measurement). the switch between laser alignment. ideally 15% When the desired value is reached.Background” Press the space bar again to start the measurement Obscuration readings should remain very close to 0. i. press the space bar to go onto the Measure Sample stage. Click the Save Record button. 24. Background measurement is complete when the button changes from STOP to START and the message “Press Space Bar to Continue” appears Press the space bar to move to the Inspect phase The Measure Window changes to “Measure . Press the space bar again to start the measurement When the message “Press Space Bar to Continue” appears. 31. 27. 30. obscuration.5 to 1ml of sample mud in a syringe Add sample a little at a time to avoid saturation . Analysis is now complete but results must be saved and reported 25. press it to start the calculation. 35. 29. 23. 28. This should have an obscuration reading in the range 12 .e. When calculation is complete the window will automatically disappear and the results table and graph will be displayed. 26. 33. Caption should read “Measure . A higher obscuration indicates an impure base fluid or the presence of dirt or contamination within the instrument. All data must be down loaded to floppy disks and backup copies made.18%. . The actual amount will depend on the solids content of the sample As material is added the obscuration will increase and the central display column will exhibit a “traffic light” display changing from red to amber and finally to green. There is not sufficient sample to analyse until you are in the green section. This automatically saves the results in the next record of the open file. 32.Inspect” Collect around 0.a very small quantity of mud is required. To save the results 34. Press the space bar to continue the background measurement.0%.Section 5Non-Routine Laboratory Testing Procedures 22.

The next section reports system details such as the sampler used (internal or small volume). Select the required file (containing the desired solids profile) from the list and it will be opened onto the screen. 45. but do not touch window with the paper towel Using a lens tissue clean each window in turn using one simple stroke along the length of the window. 5. Before and after each measurement the system should be flushed through with fresh base fluid. The main axis show particle size against the percentage of solids. 44. 40. thus running the risk of blocking off pores if we are in the reservoir section. 37. 3.Section 5Non-Routine Laboratory Testing Procedures To print a report of the results : 36. This is simply done by lowering the motor into a beaker of clean fluid and allowing to circulate for a few minutes at a minimum of 2000rpm. These include the file name and sample name that was input in the earlier stages along with any notes that were added. The third section is arguably the most important as it details all the results statistics. This desired profile should be loaded on to the computer by clicking on the file command and selecting “Open Sample File” from the menu. 43. The cell window should also be cleaned. This should be obtained by laboratory testing prior to taking the Mastersizer offshore. These include the percentage of particles found in each size range The final section is the graphical plot of the results and is the easiest method of obtaining a quick comparison of results. Do not wipe the window round in several directions. (If you want to open files without superimposing them onto earlier ones the plots already displayed should be erased by clicking the box at the top of the display that shows a graph with a cross through it). 41. . Failure to clean the apparatus will result in “Data Saturation” messages. The easiest method of obtaining a comparison of test results with the desired results is to have a graphical display of the desired solids profile. 6. If this is seen it indicates that the filter cake is poor or even breaking down and that fine particles will be migrating into the formation. any modifications made and the beam obscuration. 4. This is also a simple operation but care must be taken to avoid damage to the window. 38. 39. 1. When carrying out a PSA on a PPA (. 42. Repeat this operation to open the file containing the results you want to compare.Pore plugging Apparatus ) filtrate the most important trend to look for is an increase in fines content of the sample. Cleaning procedure is as follows: Lift motor out of fluid and turn off Open draw fully and turn handle anticlockwise to release window Lift off upper window taking care not to touch the window itself Dry the area around both upper and lower windows with paper towel. Click the Print button Click the “report “option to choose this format Print report The report will be printed out in a similar format to that shown on the screen: Sample details will be displayed at the top of the report. 7. CLEANING AND MAINTENANCE OF PSA Basic cleaning before and after every analysis is essential in order for the machine to operate. The time and date of the analysis are also displayed. This plot will automatically be superimposed on the desired profile that was opened earlier. 2. C.

15. Use the window tool to reinsert the window. To replace the window. The use of a vortex machine may also be necessary to further reduce solids size in the system. Rotate anticlockwise to remove the ring. If the instrument gets particularly dirty. This same procedure must be used every time the system is changed from oil to water based mud and every time use of the machine is ceased. The windows are held in place by “O” rings and can easily by pushed out by applying gentle pressure to the upper surface of the window. 17. It is therefore essential that no solids of a larger size than this are introduced to the system. 10. If the windows have dried. 16. .this will result in permanent damage necessitating window replacement at a cost of $150 per window! Particularly stubborn solids can be removed by gently washing with Acetone from a wash bottle. The cleaning tissue can also be moistened with methanol and white spirit to aid removal of solids. It can be overcome by cleaning the cell windows again and flushing through with base fluid for several minutes. however they are expensive so all precautions must be taken to avoid damage in the first place. breath on them to produce moisture before gently cleaning with a lens tissue in the same way as before. lowering the pump into base fluid and increasing pump speed to 3000rpm. The window has a tapered edge and the widest side must face outward. The aperture between the upper and lower cell windows is only 2mm. Never clean a dry window .Section 5Non-Routine Laboratory Testing Procedures 8.this produces scratches Under no circumstances should materials other than lens tissue be used to clean the cell windows . If they are they can not only damage the lenses but may also become trapped between the windows or in the tubing. 14. In order to ovoid introduction of this size of particle it is recommended that any samples taken from before the shale shakers are run through the mesh of a Marsh Funnel to remove course solids first. The message “Data Saturation” appears . Should the windows become damaged they can easily be changed out. 13. 12. It must be fully home in the mount not simply held by the “O” ring otherwise it will move as pump speed changes and lead to miss-alignment of the lasers. or any case a minimum of every 4 days. Use a lens tissue between your thumb and the window to avoid direct contact and place paper towel on the bench below to catch the window as it comes out. D. TROUBLE SHOOTING 9.This is normally caused during the background measurement phase by poor cleaning practices. 11. the system should be cleaned by flushing with warm soapy water for several minutes. To change out a window follow the procedure below: Open the draw on the Mastersizer housing the cell windows Remove the retaining rings by inserting the pegs on the round removal tool into the holes on the ring. 1. first fit the “O” ring to the retaining ring then gently push the window into position using the same technique as for removal. Check for any leaks by inserting the window. hold in the yellow override button to begin circulation and check that there is no seepage from around the window. With the window draw open.

The pump is turned on but is in the raised position or the cell draw is open. Do you wish to retry?” appears when the Mastersizer starts . In any case. thorough cleaning of the system will be required on completion. 3. Alternatively the cell draw could be open 2. 6. The pump will not start . If this is not the case it could be that the cell top is not properly fitted. there is a fault in the system and Malvern should be contacted to rectify it.Section 5Non-Routine Laboratory Testing Procedures 1. .The pump is not in the solution or the cell window top is not in place. If the message occurs during the analysis phase it is usually due to adding too much sample. If all the above have been checked and the display still continues to flash when the pump is place in water. depending on how saturated the solution has become. Unfortunately it is usually too late to do anything about this now although it may be possible to continue with the measurement and still get reasonable results. The pump display flashes . The message “Instrument is not responding.Check that the communications cable between the Mastersizer and the PC is properly connected to both the instrument and the PC then click “Retry”. If the fluid is particularly viscous it is possible that the pump cannot reach the requested speed and this will cause the display to flash.

clean the cell before using it. A 1. and the speed display should flash briefly if the speed switch is in the "STOP" position. such as haematite or micromax CANNOT be put in the Fann 70 due to the damage that can be done to the torsion magnets. preventing the cell from dropping off the stand.3 PROCEDURE DFT/EAF/015 . Place the rotor assembly into the cell.3 in the Fann 70 manual. If there is any pressurising fluid left over from a previous test remove it from parts of the cell where it may come into contact with the Coupling threads. Take care not to bang it against the pivot point. rotor bearing race and the rotor ball bearing as described in section 6. Lower it gently into place and check that it rotates freely . the rotor assembly. 8. Do not drop the cell into place as that may damage the pivot ball bearing. If necessary replace the pivot bushing.Section 5Non-Routine Laboratory Testing Procedures 5. Building The Test Cell 3. If the "MAN" light on the controller is not flashing press the "START / STOP" key to prevent the controller from heating up or cooling down. 9. 6. until the bob is fitted tightly onto it. Screw the cell baffle snugly into place in the bottom of the Coupling. 4. Fluids containing magnetic particles. Pass a metal rod through the holes in the baffle to tighten it sufficiently. PROCEDURE Turn on the Fann 70 at the main power switch on the console. If they are not. The cell itself. Check the condition of the rotor.HTHP Rheology . If the torsion dial reading stops changing during a test there is a good chance that this is what may have happened.000 psi.Fann 70 The Fann 70 has the capability to measure the rheology of fluids up to 500 deg F and 20. It may press down hard enough to damage the bob's Vee jewel. If the cell baffle is not sufficiently tight then it may unscrew during the test until it touches the top of the bob. Two alarms on the controller. The pressure gauge should light. bob. The fluid will not remain homogeneous due to the magnet at the bottom of the rotor pulling the particles out of the fluid to congregate at the base of the rotor. Screw the bob onto the bob shaft. When the alarms are no longer illuminated the controller can be used. Screw the bob shaft assembly plus the bob through the whole in the cell baffle into the limit stop at the top of the test cell. Press the "HEAT/COOL START" switch until the temperature controller comes on. Ensure that the top of the cell assembly is on it's stand with the locking pin in place. and bob shaft must be free of anything that may contaminate the sample. 10. 2. Filling The Cell . 7. Start with all parts of the cell clean. Remove the cell seal o-ring and backup ring if they are installed. or middle part of the test cell. 5. or cause damage to the threads of the cell. which can be seen at the top left hand corner of the controller will illuminate and switch off by holding the switch in.

Stroke the pump at least 20 times with the pump handle. Place this double syringe into the sample port. 17. Tighten the single connector locking screw at the right hand side of the heating jacket. It may be necessary to rotate the test cell slightly to line up the ports with the connectors. Any more than 15 mL of the sample will cause contamination of the pressurisation fluid in the torsion assembly. Place 140 mL of the sample into the test cell until it reaches the top of the rotor. Place the cell under the Coupling on the stand. Continue pumping until you . Place AntiSeize lubricant on the threads of the sample port. 21. Lift the cell carefully from it's stand into the Hot Well with the plugged sample port facing out of the hot well.Section 5Non-Routine Laboratory Testing Procedures 11. 24. The sample port is to the immediate right of this engraving when looking straight at it. Ensure that there are no air bubbles in the sample by rotating the rotor in the sample. Lubricate the lower threads of the Coupling with a small amount of Anti-Seize grease to prevent thread galling. 13.6 pounds (13. Check that the Reservoir return valve on the pump (round black valve) is closed. If necessary fill with more Marcol 172 oil. 18. Installing The Cell In The Hot Well 20. Lift it up and screw it onto the Coupling until the threads are hand-tight. If during this process resistance is felt before the cell is fully screwed onto the Coupling stop and investigate the cause. 22. 16. Screw the sample port cover into the sample port.) Inject 15 mL of the sample into the sample port until the sample has risen up to just below the sample port in the bob shaft. Open the pressure release valve on the side of the reservoir tubing. 15. 14. The backup ring sits on top of the o-ring with the bevelled side facing down. and continue until you hear a last of air being forced from the plastic drain tube underneath. (This can be located by looking for the engraved "Baroid Model 70" on the top of the cell. 19. Screw on the cap until it is hand tight. which can ruin the cell assembly. The viton 0-ring is placed in the groove first. Apply Anti-Seize lubricant to the threads of the other two ports. Remove the locking pin. The cell can be screwed on tighter with the use of a strap wrench. 23. CAUTION The test cell weighs 29.4 kg) when empty and should be carried with two hands and extreme care. followed by the metal backup ring with the bevelled side down. Check the level of the pressurising fluid in the pump reservoir. baffle and bob are in the correct place. 25. 12. Check that the o-ring and backup ring. Screw in the port connectors until they are hand tight. Unscrew the cell and check that the torsion assembly is not jammed by rotating the top magnet with a non-magnetic wire or rod. Fill a 20 ml syringe with 16 mls of sample and place a 1 mL syringe with no plunger on the end of it. Check that the viton o-ring and backup ring are in place at the top of the cell. Place the o-ring and backup ring into the cell. The torsion assembly may be jammed.

about 25˚C. The "UP" and "DOWN" arrow keys can be used to alter the time that is taken to reach the test temperature. If fluid leaks out of the cell.Section 5Non-Routine Laboratory Testing Procedures obtain a continuous flow of oil from the drain tube and then close the pressure relief valve. "SET PT 1" will appear on the display. A slight pressure leak at the beginning of the test. 35. Use "PARAM CHECK" to scroll through the program parameters. To set an end point for the temperature press "TUNE". if there is one. Programming The Controller 30. This should be equivalent to room temperature. Press "PARAM CHECK". 38. "LAST" then "YES/ UP ARROW" keys. Press "PARAM CHECK". "ASSURED SOAK" will appear in the display. Press "PARAM CHECK". "TIME 3" will appear on the display. 29. 36. When "RAMP AND SOAK ?" appears on the display press the YES/ UP ARROW" key. "SET PT 2" will appear on the display. The time will be displayed as hours : minutes. Press the "NO / DOWN ARROW" key. 28. i. This is equal to the time that the sample of fluid will take to reach the test temperature. "TIME 1" will appear on the display. Press "PARAM CHECK". This is equal to the time that the sample of fluid will stay at the test temperature.e. Press "PARAM CHECK". "SET PT 0" will appear on the display. "CYCLES" will appear on the display. Push the door pin all the way down to lock the shield closed and to properly position the dial sensor in the top of the door. . or to check that the o-ring and backup ring are in the correct position. Press "PARAM CHECK". This is usually left at 0 hours and 00 minutes. This is the number of times that the program will run through the temperature ramps before it stops heating. the solution is to open and close the door slowly. 1000 psi is usually sufficient to see if there is a pressure leak from the test cell in the heating jacket. This is known as the first ramp. This can usually be programmed to be about an hour or slightly less than that if required. This is equal to the test temperature in degrees centigrade. 37. then pressure must be slowly released and the cell must be removed from the well. "TIME 2" will appear on the display. This is usually left at 99 hours and 59 minutes. This is equal to the test temperature in degrees centigrade. 27. Press "PARAM CHECK". viewed on the gauge is quite normal and should stabilise within a few minutes. If no fluid leaks out then the cell is holding pressure. Close the vent valve and pressurise the cell to the desired pressure. If the o-ring has perished under the pressure it must be replaced. 33. Pressurising The Cell 26. If the readings are obviously false due to closing the door too quickly. Usually all that is required is to tighten the seals between the joins of the cell. 32. This is equal to the time that the sample of fluid will take to ramp to the third temperature. This is known as the second ramp. 31. 34. If the cell is not leaking then the door of the hot well can be closed slowly. Using the speed selector button set the fluid spinning at 200 RPM.

When the test cell has cooled to room temperature. 42. 52. 41. . and disconnect the pressure lines at the port Couplings. (This is a well known design fault which will not be rectified in the near future. Dismantle the cell and clean all parts thoroughly with detergent. A vacuum pressure will have built up behind the cell and this must be broken by turning the cell around in the heating jacket. Any sediment from the fluid that may have accumulated around the pivot or in the rotor must be removed. This will take the display back to the temperature of the fluid in the heating jacket. 45. The fluid can be left to heat to the test temperature. If there is a difference between the temperature of the sample and the set point 0 temperature change it until they match. Due to the length of time that is taken to relay the signal to the heater the temperature in the test cell can take up to several hours to stabilise. 51.000 psi and the pressure placed on the cell must NOT be greater than this. Running The Test 40. The cell can now be lifted out of the hot well. "END OF TUNE" will appear on the display. CAUTION The Fann 70's pressure lines are only rated to 20.Section 5Non-Routine Laboratory Testing Procedures 39. press the "START / STOP" key again. Press the "TUNE" key. This will disable the cooling and heating action. Once the cell has cooled to room temperature.) One hour is usually sufficient for this to happen. release the pressure on the cell slowly using the pressure release valve. Once the test is complete. Extreme care must be taken when lifting the cell out of the hot well due to the weight of the cell. decrease the "OUT 2" to 0 %. press the "START / STOP" key on the temperature controller to stop the heating process. Take the desired rheology readings. Press the "MAN" key. as the it takes more than 10 seconds for the motor to activate from stationary! Ending The Test 44. 49. Once the fluid is at the correct temperature adjust the pressure on the cell to what has been requested by the client. When there is no more pressure on the test cell it can be dismantled safely. Press the "START / STOP" key to commence heating the sample. Unscrew the Coupling lock pin. This will start the cooling water. 53. Using the "YES / UP ARROW" turn this to 100 %. Place the cell on it's stand and secure it in place with the locking pin. 50. If required take gel strength's. If the "OUT 2" does not change. 47. 43. The 10 second gel is relatively meaningless. Ensure that the magnet at the bottom of the rotor is clean and that it does not become too worn. 54. 48. Press the "DISPLAY" key until "OUT 2" appears.

Close the shield door. 59. If it is not then the mechanical zero must be reset. Adjust the position of the torsion magnet by loosening the screw and rotating the magnet clockwise or anticlockwise in small amounts. 57. 61. The magnet should be tightened and the shield door closed. Remove the cap of the cell and loosen the Allen screw in the pivot cap. If the reading on the console is within the limits of ± 5 of zero degrees then this is an allowable amount. 60. make the cell up with no fluid in it. Remove the pivot cap. If the reading on the display is at. Dismantle the cell and leave for the next test.Section 5Non-Routine Laboratory Testing Procedures 55. As close to zero as possible within 2 degrees is better. . 58. Disconnect the port connectors and remove the cell from the hot well. Resetting The Mechanical Zero 56. The shaft and bob must also be cleaned and the top and middle parts of the cell must be cleaned so that no fluid blocks the sample port. Once the cell is clean and dry. Place the cell into the hot well and connect the port connectors. Continue moving the magnet until the closest reading to zero can be achieved. Replace the pivot cap. Replace the cell cap. or close to 0 then remove the cell. The pressure ports must also be kept clean so that pressure will not build uncontrollably during a test.

Bleed off the filtrate into a measuring cylinder. The upper valve stem is inserted loosely and the lid fitted in the same manner as the lower cap was. 10. 2. EQUIPMENT a. This is done by inverting the cell and carefully loosening the valve stem.4 PROCEDURE DFT/EAF/016 . The valve stems must now be checked for tightness and the cell inserted in the heating jacket (ensuring that the ALOXIDE disc is on the bottom). If this occurs. Generally. The stem should be tightened into the lower cap and the cap inserted. bleed off some of the filtrate into a measuring cylinder. Before starting it is necessary to check all the “O” rings are in good condition and that the tips of the valve stems are not corroded or blocked. 8. 5. 11. The heating jacket should be set at the desired temperature. 3. close the lower valve stem and then the upper valve stem to isolate the pressure inside the cell. Dismantling should be carried out with care. During the test watch for a pressure build up in the lower unit. The thermometer/temperature probe should be inserted into the cell and the upper and lower pressure units fitted. Loosen the grub screws and carefully remove the cell lid. Open the lower stem and start timing. differential pressures greater than 500 psi should be avoided. b. When the required temperature is reached the upper pressure unit should be adjusted to 100 psi above the required pressure and the lower unit adjusted to 100 psi. Care must be taken not to over tighten any screw as this can result in cracking of the disk. Screws should be tightened gently working on opposite screws in sequence and continuing round the cell until the cap is in place and the screws are flush. 7. The pressure limitations of the cell should be taken into account. 6.) A specially adapted double ended HTHP filter press cell is used for this test. 1. 4. Adjust the upper pressure unit to 200 .Section 5Non-Routine Laboratory Testing Procedures 5.) Aloxide (fused aluminium oxide) disc of desired permeability B.Pore Plugging Apparatus (PPA) The primary function of the PPA is to characterise the bridging efficiency of a fluid by measuring its spurt and mud loss through a ceramic disk of fixed permeability over time. It is important to ensure that all pressure has been bled off prior to loosening the grub screws. The cell should be inverted and the required size of ALOXIDE disc inserted. A.300 psi and open the upper valve stem. 9. After 30 minutes. Record the PPA fluid loss as twice the volume of filtrate collected. This ensures that it is wet and best emulates formation conditions. PROCEDURE The ALOXIDE disc of the required permeability should be soaked in base fluid until bubbles cease to be given off (usually around 5 seconds). . The cell should now be filled with mud to within 1/2” of the upper “O” ring. Ensure that the stem is pointing away from people as the pressure is bled off. This then helps in designing a fluid with the optimum bridging agents present which are best suited to match a formations permeability.

milled thin and fitted with a Parker gate valve and compression fittings. Bottom End cap. The caps spin up or off without tools and are much easier to use than the old style that has been used for years. An O-ring seal should be fitted. Top End cap. PROCEDURE A fixed volume of 350 ml of fluid is flushed through the assembled back-flow cell at 5 psi pressure and at ambient temperature. and the time taken for complete evacuation of the cell noted.) EQUIPMENT 500 ml Double Ended cell (acrylic or stainless steel). including pre-packs.Back-Flow Tester Procedure for “Wire Wrap” Screens The Back-Flow tester is a qualitative means of evaluating in the laboratory the likelihood of a wire wrap screen plugging in the field when a specific fluid is flowed through it. 2.) e. Ideally. The new version should be acceptable to Schlumberger HSE for pressures above 1000 psi (which the old style apparently is not). and tighten retaining grub screws. Buna N. . OFI p/n 170-13 Allen key for grub screws and an adjustable spanner for connections Adjustable stand B. de-ionised water should be used in order to establish a base line value. 2000 psi (OFI p/n 170-24.) d.) b. 5. Generally.Section 5Non-Routine Laboratory Testing Procedures NOTE: Fann has now introduced a new HTHP cell that does not use the set screw secured end caps. fitted with 0-30 psi low pressure gauge and soda siphon assembly. and stainless steel spacers used when testing with single screens.) f. Excluder wire wrap screens Large size O-rings. Set up the back-flow test cell containing the clean wire wrap screen section by carefully fitting the test screen into its retaining ring. Johnson screen disks.) c. 2000 psi (OFI p/n 170-24).5 PROCEDURE DFT/EAF/019 . and at the end of the test deionised water flushed through once again in order to ascertain whether or not any serious plugging had occurred with the test screen. milled at bottom end to accommodate wire wrap screens. of variable screen gauges would be used. A. Place bottom end cap into position. three 350 ml aliquots of test fluid should be used. with valve closed. Initially.) g. 1. a.

If all 3 batches of mud pass through the screen without plugging then the test is considered successful. 7. Fill the cell with 350 mls of either distilled water or screened test fluid. and replace and tighten top end cap. Place graduated beaker/jug under cell and apply 5 psi to cell. Inspect the screen visually for evidence of plugging and report any findings. ∑ ∑ . then repeat steps 3 to 6 with two further 350 ml batches of fresh fluid and the same screen. INTERPRETATION ∑ A successful result is the flow of all 3 batches of fluid through the wire wrap screen at a maximum pressure of 5 psi. and (b) a pressure of 25 psi should be applied to the cell and the evacuation time recorded as before. 10. Open bottom valve and record time to evacuate the cell. i. 9. Complete flow through the wire wrap screen at 25 psi is NOT satisfactory. 6. Release applied pressure if cell becomes plugged BEFORE unscrewing the top regulator. noting that flow times must be similar.e. (a) the volume of fluid collected should be recorded. C. If the screen plugs. However. Incomplete flow indicates that further mud conditioning is required over the shaker screens to preclude screen plugging. 5. If all the fluid passes through the cell.Section 5Non-Routine Laboratory Testing Procedures 3. 8. incomplete flow of any of the three batches at 5 psi. 4. testing at that pressure will quantify the severity of plugging.

the MSM package allows the low gravity solids (LGS) and high gravity solids (HGS) content to be measured much more accurately and faster than with a traditional retort. .Section 5Non-Routine Laboratory Testing Procedures 5. It measures barite. low gravity solids (LGS).Mud Solids Monitor (MSM) The MSM Mud Solids Monitor is a field proven and accurate analytical technique for measuring drilling fluid composition. particularly in the heavily weighted muds that are normally used in critical HTHP wells. Barite/LGS and salt measurements work in all major drilling fluid types except salt saturated water based systems.1% v/v. WHICH CAN BE OBTAINED BY CONTACTING EATC SUPPORT STAFF IF REQUIRED. The MSM package also offers the valuable additional benefit of accurate potassium measurements. either through excessive dilution leading to higher mud costs or more usually by insufficient dilution leading to poor drilling performance and greater chance of major drilling problems and higher overall drilling costs. The LGS is then calculated by closing the mass balance. potassium and chloride concentrations and is an extremely valuable tool for fluids monitoring and for analysis of solids control equipment performance. giving a typical error of +/. potassium and calcium directly and also measures the total liquid phase. The whole analysis process from analysing the sample to obtaining the results takes about 5 minutes. This allows the engineer to monitor potassium depletion rates and ensure that appropriate inhibition levels are maintained. For fluids monitoring. Barite quality is important for drilling fluid performance. A DETAILED OPERATING MANUAL IS AVAILABLE FOR THE MSM.6 PROCEDURE DFT/EAF/020 . LGS cannot be measured with any degree of reliability and the use of this property to control dilution rates can lead to expensive mistakes. The MSM package measures the barite and other ions such as chloride. With the retort. The MSM package can also be used as a quality control tool to analyse barite either in the laboratory or at the rigsite.

data aquisition. Strontium. Calcium. Components in the system are as follows. Formate.Fluids Ion Monitor (FIM) The Fluids Ion Monitor is a low cost fully upgradeable systems to provide ion analysis capabilities for a variety of applications. A DETAILED OPERATING MANUAL IS AVAILABLE FOR THE MSM. Sulphate and Phosphate. chemical suppressor column. Nitrate. pump unit. The FIM is capable of measuring all the major ions in a drilling fluid filtrate to within +/. The system is calibrated by using a external calibration standard solution containing the analyte ions to be measured. The system is based on the principle of ion exchange chromatography. Potassium. The conductance reading is proportional to the concentration of each ion.7 PROCEDURE DFT/EAF/021 . Schlumberger Dowell utilise the FIM quantitatively to measure cations and anions in the aqueous phase of water based drilling fluids. analyte ions are injected on to ion exchange column whereby they are separated according to their hydrated ionic radius and their charge. ion exchange column. WHICH CAN BE OBTAINED BY CONTACTING EATC SUPPORT STAFF IF REQUIRED. Once the ions are separated they pass through a conductivity detector. Barium.1% accuracy in a time frame of 15 minutes. conductivity detector. Chloride. Common analyte ions detected by the FIM are: Sodium. Magnesium. . Bromide.Section 5Non-Routine Laboratory Testing Procedures 5.

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