Introduction To Cement Laboratory Testing

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.
Schlumberger 2008
Revision History
Description
Reviewed
/Prepared by
1.0
Introduction to Laboratory Testing
Deepak Khatri/Jan Liu
May 15, 2009
Rev. Date
Learning Objectives
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
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
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
Performance Testing-Spacers/Washes
Evaluation of the cleaning effect
Compatibility with Cement
Thickening Time
Fluid Loss
Compressive Strength
Rheology
Compatibility with mud
Rheology etc.
Compatibility Testing
FORMULA:
(Highest Reading of fluid combinations) (Highest reading of individual fluids)
Fluid combinations:
<0
Compatible
95:5
0-40
Possibly incompatible
75:25
40-70
Slightly incompatible
50:50
70-110
Definitely incompatible
>110
Severely incompatible
25:75
5:95
100%
100%
Sample Preparation
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
Use representative samples.

Sample acquisition
Slurry Design
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
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
40
Pressure (kpsi)
50
40
30
10
60
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
90
Temperature (F)
20
10
0
0:00
0:30
Schlumberger
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
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
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
Youngs Modulus
Poissons ratio
Shear Bond
Cement - Casing & Cement

- Formation
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
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
FREE FLUID
TEST
Laboratory Procedures & Equipment
Laboratory Analysis Request - (LAR)
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
Material
Constant Speed Blender
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)
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
units are ppg, Kg/m3, SG, and so on

Free Fluid Test (API RP10B-2 sect. 15)
Static and Stirred Fluid Loss Apparatus
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
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
For slurries that dehydrate in less than 30 minutes, API

Fluid Loss value is obtained by either:
Rotational Viscometer (FANN/CHAN 35)
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=(300 100) x 1.5
y= 300 Pv
Use LabDB to calculate
Pv and Ty!
600 rpm not used to calculate Pv and Ty
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
21
24
0.87
22.5
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
Atmospheric Consistometer
Pressurized Consistometer
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
Reported in Bearden units of consistency (Bc)

Upper fluid limit: 70 Bc to 100 BC
API RP10B-schedules
API Schedules
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
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.).
100
Bc
100
90
90
80
80
60
50
40
Pressure (kpsi)
Temperature (F)
70
30
20
Bc
50
100
60
50
40
30
10
Consistency (Bc)
70
Temp.
30 Bc @ 2:01:05
70 Bc @ 3:01:05
100 Bc @ 3:36:50
Time (min)
deg.F
0
140
130
120
110
100
90
80
70
60
50
40
30
20
10
0
20
10
0
0:00
Schlumberger
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
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
High Temperature High Pressure Testing

Ultrasonic Cement Analyzer (UCA)
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 dont 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)
Proper filling cell
UCA Chart
Laboratory Analysis Report
Well Information
Slurry Design
Lab Test results
Comments
Charts (TT, UCA)
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
Thickening Time
Pressurized
consistometer
HPHP fluid loss cell
Free Fluid
Water bath, curing chamber

Hydraulic press
250 ml graduated cylinder
Permeability
Water permeameter
Rheology
Rotational viscometer
Static gel strength
SGSA or Vane rheometer
ISO 10426-6
Expansion & shrinkage
Annular sleeve
API RP 10B-5
Fluid Loss
Compressive Strength
Spacer/Wash/Cement Compatibility Rotational viscometer

Reverse Emulsion Tester
Coupons, grid
Sedimentation test
Foam cement
Closed mixer cup

API RP10B-4
Specification for Cements
API Spec 10A
Various

CEM- Section 2B5
Note: API RP10B-2 = ISO 10426-2

Also CEM- Section 6 lists all Schlumberger cement test procedures
Other Equipments and Tests
Blend specific gravity measurement Gas

Pycnometer
Spacer Surfactant Selection Testing

Coupon Test
Grid Test
Reverse Emulsion Test
Foam Cement Mixing & Foam cement Generator

under pressure
SGSA &Vane Gel Strength Rheometer
Cement Hydration Analyzer
Mechanical Properties Testing
HT-HP Rotational Rheometer

Introduction To Cement Laboratory Testing

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Introduction To Cement Laboratory Testing

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Cement Lab Introduction

An asterisk is used throughout this presentation to denote a mark of

Introduction to Laboratory Testing

Deepak Khatri/Jan Liu

May 15, 2009

XRD, FTIR, microscopic

Performance Testing- Slurries

Operational testing procedures for all slurries (API RP10B-2 or

API Spec 10 - Section 3

Use representative samples.

Migrates upward, accumulates in

Varying density gradients in the cement

Results in unstable slurries, annular

Balance sub-surface pressures

Slurry Properties - cont.

Instrument: 940 Left 940 L

Bearden Consistency (Bc)

Slurry dehydration during placement phase

Test File Name: 940 L-CCS08002-1R.tst

Slurry flow modeling

Set Cement Properties - I

Cement - Casing & Cement

Set Cement Properties - II

Reaction to magnesium and sodium sulfates;

Loss of compressive strength

Laboratory Procedures & Equipment

Laboratory Analysis Request - (LAR)

Submitted to lab requesting formulation of

Class G Cement & 44% water

Calculate for 600 ml

Constant Speed Blender

Slurry Preparation (API RP10B-2 section 6)

Nitrogen (Foam slurries)

Measured with an Atmospheric or Pressurized

Slurry placed in 250ml graduated glass test tube

Free water (ml) measured after 2 hours

Slurry sedimentation also checked

units are ppg, Kg/m3, SG, and so on

Static and Stirred Fluid Loss Apparatus

Fluid Loss Test (API RP10B-2, section 10)

HPHT, high pressure, high temperature (1000 psi)

Backed up by a 60 mesh screen

F30 = Filtrate at 30 minutes

For slurries that dehydrate in less than 30 minutes, API

Rotational Viscometer (FANN/CHAN 35)

Rheology (API RP10B-2, sect. 12)

600 rpm not used to calculate Pv and Ty

Rheology (API RP10B-2, sect. 12)

Initial slurry temperature

Final slurry temperature 146 o F

Thickening Time Test (API RP10B-2, sect. 9)

Casing (1g - 11g)

Refer to In-Touch ID is 4718717 for Laboratory Request

Reported in Bearden units of consistency (Bc)

Pressure and Temperature changes

Temp. History (degF)

Thickening Time Test Curves

100 200 300 400 500

Instrument: 940 Left 940 L

Test File Name: 940 L-CCS08002-1R.tst

Pressurized Curing Chamber

Compressive strength (API RP10B-2, sect. 7)