Introduction to Cement Laboratory Testing
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Cement Lab Introduction Schlumberger Private
An asterisk is used throughout this presentation to denote a mark of Schlumberger. Other company, product, and service names may be trademarks, registered trademarks, or service marks of others.
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© Schlumberger 2008
Revision History Description
Reviewed /Prepared by
1.0
Introduction to Laboratory Testing
Deepak Khatri/Jan Liu
May 15, 2009
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Rev. Date
Learning Objectives
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• Laboratory Functions • Key Slurry properties and the testing in the laboratory • Laboratory testing standards & procedures • Interpretation of laboratory reports & charts for the actual job • Equipment used in the laboratory • Use the Laboratory video as applicable for the Operational school
Laboratory Functions Performance Testing Design Stage – Measurement of slurry properties under downhole conditions.
Execution Stage – Control the quality of the blended material
Evaluation Stage – Investigation of job failure
Analytical Testing Quality control of the slurry components prior to mixing. – Cement – Additives – Mix Water
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Analytical Testing Four types of samples are examined; Cement Powder Chemical Analysis: C3A, C3S, C2S, C4AF and Gypsum Dry Blended Cement
XRD, FTIR, microscopic Mix water
Ionic content: – Sulphates, chlorides, hardness
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XRD, FTIR Set Cement
Performance Testing- Slurries Governed by the API committee on “Standardization of Oilwell Cements” (Com. 10) & ISO Publication consists of; Specification tests for neat cement slurries (API Spec 10A or ISO 10426-1)
Operational testing procedures for all slurries (API RP10B-2 or ISO 10426-2 and others) Procedures designed to simulate downhole conditions
Pressure
Temperature
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Performance Testing-Spacers/Washes Evaluation of the cleaning effect Compatibility with Cement Thickening Time
Fluid Loss
Compressive Strength
Rheology … Compatibility with mud
Rheology etc.
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Compatibility Testing FORMULA: (Highest Reading of fluid combinations) – (Highest reading of individual fluids)
Fluid combinations: 110
Severely incompatible
25:75 5:95 100%
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100%
Sample Preparation
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Sample Preparation
Prior to shipment No additive should be used that is not from actual field samples Sample and handling procedures
API Spec 10 - Section 3 Echoes the requirements of the ‘KSQR’
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Use representative samples. Sample acquisition
Slurry Design
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Slurry Properties Free Fluid & Slurry Sedimentation Water separation from static slurry
Migrates upward, accumulates in pockets or at top of cement column.
Varying density gradients in the cement column
Results in unstable slurries, annular bridging, incomplete zonal isolation Density
Balance sub-surface pressures
Sample Number Top 1 2 3 4 5 6 7 Bottom 8
Weight of Sample (g) 18.11 14.81 14.72 16.73 14.36 16.4 16.01 19.04
Weight of Volume of Removed Water (g) 14.01 11.39 11.33 12.81 10.94 12.56 12.34 14.37 Average Density:
S.G. of Slurry 3 (g/cm) 1.26 1.26 1.26 1.27 1.28 1.27 1.26 1.29
Density of Slurry (ppg) 10.49 10.55 10.54 10.60 10.65 10.59 10.53 10.75
1.27
10.59
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Slurry Properties - cont. Pumpability (Slurry Consistency) Length of time slurry remains in a pumpable fluid state (Job Time + 2 hr or Job Time x 1.5 hr, whichever is higher)
Instrument: 940 Left 940 L Test Start: 1/10/2008 2:25:18 PM Well ID CCS08002-1R-D186-Exp Test Stop: 1/10/2008 6:02:18 PM Customer SLB Comments: Retest of Exp D186 at 16.40 ppg 1500 psi and 65 F (room temp.).
100
90
80
4
40
Pressure (kpsi)
3
2
50
40
30
1
10
0
60
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Bearden Consistency (Bc) Fluid Loss
20
Consistency (Bc)
70
60
30
Slurry dehydration during placement phase Rheology
80
70
50
30 Bc @ 2:01:05 70 Bc @ 3:01:05 100 Bc @ 3:36:50
100
5
90
Temperature (°F)
20
10
0
0 0:00
0:30
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1:00
1:30
2:00 Time (HH:MM)
2:30
3:00
3:30
Test File Name: 940 L-CCS08002-1R.tst
4:00
Page 1
70 60 50 Shear Stress (Pa) 30 40
Mixability at surface
20
10
Slurry flow modeling
0
C e m e n t - S h e a r S tr e s s V s S h e a r R a te @ T e m p e r a tu r e : 2 7 d e g C L a b . d a ta B in g h a m p la s tic m o d e l H e r s c h e l B u lk le y m o d e l Po w e r la w m o d e l
0
50
100
150
200
250 300 350 S h e a r R a te ( 1 /s )
400
450
500
550
600
Set Cement Properties - I Compressive strength Tensile strength Schlumberger Private
Young’s Modulus Poisson’s ratio Shear Bond
Cement - Casing & Cement - Formation
F
Set Cement Properties - II Sulfate Resistance
Reaction to magnesium and sodium sulfates;
Strength Retrogression Cement CSH Gel Breakdown begin at >230o F. Permeability
Lightweight slurries
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– Loss of compressive strength – Stress cracking
Testing Process LAB ANALYSIS REQUEST SLURRY DENSITY FLUID LOSS TEST
RHEOLOGY CEMENT - SPACER - MUD COMPATABILITY
COMPRESSIVE STRENGTH TEST
THICKENING TIME TEST LABORATORY REPORT
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FREE FLUID TEST
Laboratory Procedures & Equipment
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Laboratory Analysis Request - (LAR)
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Submitted to lab requesting formulation of cement slurry Designate additives available for slurry Request specific performance parameters; Density Rheology ( Plastic Viscosity & Yield Point) Fluid Loss Thickening Time Free Water Provide information on well parameters Job Type, Depth, BHT & mix water type etc.
Sample Calculation Sample volume for slurry testing is 600 ml Consider the following slurry composed of;
Class G Cement & 44% water
Class G Cement
Weight (lbs) 94
Absolute Volume (gal) 0.0382
Volume (gal) 3.59
Weight (gram) 42637.7
Volume (ml) 13589.6
Water 44%
41.36
0.1202
4.97
18760.6
18813.5
TOTAL
135.36
8.56
61398.3
32403.1
Calculate for 600 ml ratio equal to Total Volume / 600 ml ratio = 54:1 Use LabDB or SlurryDesigner for calculations
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Material
Constant Speed Blender
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Slurry Preparation (API RP10B-2 section 6) Mixed with a high shear mixer (Warring Blender) Two rotational speeds – 4000 rpm – 12000 rpm Water and Liquid Additives weighed out and added first Add Cement /Solids at 4000 rpm (15 seconds) 12,000 rpm for remaining 35 seconds Mixing procedure not suitable for;
Microspheres (D124)
Nitrogen (Foam slurries)
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Slurry Tests Density Measurement (API RP10B-2 section 6)
Measured with an Atmospheric or Pressurized Balance
Slurry placed in 250ml graduated glass test tube
Free water (ml) measured after 2 hours
Slurry sedimentation also checked
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units are ppg, Kg/m3, SG, and so on Free Fluid Test (API RP10B-2 sect. 15)
Static and Stirred Fluid Loss Apparatus
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Fluid Loss Test (API RP10B-2, section 10) Simulates amount of filtrate lost under pressure against a permeable formation Two types of filter press available; Low pressure (100 psi) – for DF only
HPHT, high pressure, high temperature (1000 psi) HPHT is used for slurry test (simulates conditions) Permeable formation simulated by 325 mesh screen
Backed up by a 60 mesh screen Test Parameters – 30 minute static test Reporting
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Filtrate Loss
F 30 = 2 x Ft ×
30 t
F30 = Filtrate at 30 minutes Ft = Filtrate at Time t = Time in minutes
If slurry does not dehydrate in 30 min, then API Fluid Loss is: F 30 = 2 x Ft
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For slurries that dehydrate in less than 30 minutes, API Fluid Loss value is obtained by either:
Rotational Viscometer (FANN/CHAN 35)
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Rheology (API RP10B-2, sect. 12) Calculated by correlation of shear stress against shear rate Tested with Rotational Viscometer (CHAN/FANN 35) Rotational speed (Shear rate) – – – – – – –
300 rpm 200 rpm 100 rpm 60 rpm 30 rpm 6 rpm 3 rpm
Approximation: Pv=(θ300 – θ100) x 1.5 Τy= θ300 – Pv Use LabDB to calculate Pv and Ty!
600 rpm not used to calculate Pv and Ty
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Rheology (API RP10B-2, sect. 12) 6 rpm and 3 rpm readings needed for HB rheology 3 rpm reading is used to determine the fluid gel strength at; 10 seconds & 10 minutes BOB (Stationary) Rotational Speed (rpm)
Ramp-up
Ramp-down
Ratio
Average
3
21
24
0.87
22.5
6
40
36
1.11
38
30
65
83
0.78
74
60
84
100
0.84
92
100
100
115
0.87
107.5
200
137
147
0.93
142
300
170
Initial slurry temperature –
Rotational Sleeve
170 150 o F
Final slurry temperature – 146 o F Rheological properties reported at average temperature – 148 o F
Slurry Cup
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Atmospheric Consistometer
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Pressurized Consistometer
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Thickening Time Test (API RP10B-2, sect. 9) Determine length of time a slurry remains fluid Pressurized consistometer simulates both;
Temperature Pressure
Casing (1g - 11g) Liners (22 - 32) Squeeze cementing (12 - 21)
Refer to In-Touch ID is 4718717 for Laboratory Request Checklist
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Reported in Bearden units of consistency (Bc) Upper fluid limit: 70 Bc to 100 BC API RP10B-schedules
API Schedules
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Pressure and Temperature changes Effect on Thickening Time Realistic Laboratory Evaluation Computer Simulation (CemCADE) New Instrumentation 210
D e p th = 1 2 4 0 7 ft
180 170 160
130
140
150
Temp. History (degF)
190
200
A PI B H CT G e o t h . P r o f ile A n n u lu s
0
10
20
30
40 50 T im e (m in )
60
70
80
90
Thickening Time Test Curves Temperature
100 200 300 400 500
Instrument: 940 Left 940 L Test Start: 1/10/2008 2:25:18 PM Well ID CCS08002-1R-D186-Exp Test Stop: 1/10/2008 6:02:18 PM Customer SLB Comments: Retest of Exp D186 at 16.40 ppg 1500 psi and 65 F (room temp.).
5
100
Bc
100
90
90
4
80
80
3
60
50
40
Pressure (kpsi)
Temperature (°F)
70
2
30
20
Bc
50
100
60
50
40
30
1
10
0
Consistency (Bc)
70
Temp.
30 Bc @ 2:01:05 70 Bc @ 3:01:05 100 Bc @ 3:36:50
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Time (min)
deg.F
0 140 130 120 110 100 90 80 70 60 50 40 30 20 10 0
20
10
0
0 0:00
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0:30
1:00
1:30
2:00 Time (HH:MM)
Test File Name: 940 L-CCS08002-1R.tst
2:30
3:00
3:30
4:00
Page 1
Pressurized Curing Chamber
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Compressive strength (API RP10B-2, sect. 7) Set cement strength under downhole conditions Apparatus; Curing Bath (ATM pressure & 82oC)
Curing Chamber (3000 psi & 193oC) Procedure. Measurement Unit Other methods
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High Temperature High Pressure Testing Ultrasonic Cement Analyzer (UCA)
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Non-destructive sonic testing (API RP10B-2, sect. 8) Follow manufacturers operating instructions Remove air before filling cell Set pump to pressure simulating well Select proper correlation (A, B, C) - correlations don’t apply for slurries like LiteCRETE, FlexSTONE, etc. Correlation is to cubes and has inherent error Facing specimens and crushing will give different results than cubes (do not report as API strength)
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Proper filling cell
UCA Chart
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Laboratory Analysis Report
Well Information
Slurry Design
Lab Test results
Comments
Charts (TT, UCA)
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At the conclusion of Cement Slurry formulation and subsequent testing a report is produced outlining the following;
Summary of Test Procedures Test Category
Equipment
Procedure Reference
Sampling
Diverted Flow sampler
API RP 10B-2 – Section 4
Slurry Preparation
Two speed mixer
API RP 10B-2 – Section 5
Thickening Time
Pressurized consistometer HPHP fluid loss cell
API RP 10B-2 – Section 9
API RP 10B-2 – Section 7
Free Fluid
Water bath, curing chamber Hydraulic press 250 ml graduated cylinder
Permeability
Water permeameter
API RP 10B-2 – Section 11
Rheology
Rotational viscometer
API RP 10B-2 – Section 12
Static gel strength
SGSA or Vane rheometer
ISO 10426-6
Expansion & shrinkage
Annular sleeve
API RP 10B-5
Fluid Loss Compressive Strength
API RP 10B-2 – Section 10
Spacer/Wash/Cement Compatibility Rotational viscometer Reverse Emulsion Tester Coupons, grid Sedimentation test Foam cement Closed mixer cup
API RP 10B-2 – Section 15 API RP10B-4
Specification for Cements
API Spec 10A
Various
API RP 10B-2 – Section 16 CEM- Section 2B5
Note: API RP10B-2 = ISO 10426-2 Also CEM- Section 6 lists all Schlumberger cement test procedures
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API RP 10B-2 – Section 15
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Other Equipments and Tests
Blend specific gravity measurement – Gas Pycnometer Schlumberger Private
Spacer Surfactant Selection Testing Coupon Test
Grid Test
Reverse Emulsion Test
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Foam Cement Mixing & Foam cement Generator under pressure Schlumberger Private
SGSA &Vane Gel Strength Rheometer
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Cement Hydration Analyzer
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Mechanical Properties Testing
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HT-HP Rotational Rheometer
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