Cement Lab Introduction

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 Schlumberger Private
© Schlumberger 2008

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.
Revision History
Rev. Date Description Reviewed

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/Prepared by
1.0 May 15, 2009 Introduction to Laboratory Testing Deepak Khatri/Jan Liu
Learning Objectives
• Laboratory Functions
• Key Slurry properties and the testing in the laboratory
• Laboratory testing standards & procedures

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• 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

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– 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

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Dry Blended Cement

XRD, FTIR
Set Cement

XRD, FTIR, microscopic
Mix water

Ionic content:
– Sulphates, chlorides, hardness
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

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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

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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:
100%

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<0 Compatible 95:5
0-40 Possibly incompatible 75:25
40-70 Slightly incompatible
50:50
25:75
70-110 Definitely incompatible
5:95
>110 Severely incompatible
100%
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Sample Preparation
 Sample Preparation

Use representative samples.

Sample acquisition

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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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Slurry Design
 Slurry Properties
Free Fluid & Slurry Sedimentation

Water separation from static slurry

Migrates upward, accumulates in
pockets or at top of cement column. Weight of

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Volume of
Sample Weight of Removed S.G. of Slurry Density of
3
Number Sample (g) Water (g) (g/cm) Slurry (ppg)

Varying density gradients in the cement Top 1
2
18.11
14.81
14.01
11.39
1.26
1.26
10.49
10.55

column 3
4
5
14.72
16.73
14.36
11.33
12.81
10.94
1.26
1.27
1.28
10.54
10.60
10.65
6 16.4 12.56 1.27 10.59

Results in unstable slurries, annular Bottom

7
8
16.01
19.04
12.34
14.37
1.26
1.29
10.53
10.75

bridging, incomplete zonal isolation Average Density: 1.27 10.59

Density

Balance sub-surface pressures
 Slurry Properties - cont.
Pumpability (Slurry Consistency)

Length of time slurry remains in a pumpable Instrument: 940 Left 940 L
Well ID CCS08002-1R-D186-Exp
Customer SLB
Comments: Retest of Exp D186 at 16.40 ppg 1500 psi and 65 F (room temp.).

100 5 100
Test Start: 1/10/2008 2:25:18 PM
Test Stop: 1/10/2008 6:02:18 PM
30 Bc @ 2:01:05
70 Bc @ 3:01:05
100 Bc @ 3:36:50

fluid state (Job Time + 2 hr or Job Time x

90 90

80 4 80

70 70

1.5 hr, whichever is higher)

60 3 60

Consistency (Bc)
Temperature (°F)

Pressure (kpsi)
50 50

40 2 40

30 30

Bearden Consistency (Bc)

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20 1 20

10 10

0 0 0
0:00 0:30 1:00 1:30 2:00 2:30 3:00 3:30 4:00
Time (HH:MM)

Fluid Loss Schlumberger Test File Name: 940 L-CCS08002-1R.tst Page 1

Slurry dehydration during placement phase

Rheology 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

70
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

60

Slurry flow modeling

50
Shear Stress (Pa)
40

Mixability at surface

30 0 20
10

0 50 100 150 200 250 300 350 400 450 500 550 600
S h e a r R a te ( 1 /s )
Set Cement Properties - I
Compressive strength
Tensile strength

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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;

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– Loss of compressive strength
– Stress cracking
Strength Retrogression

Cement CSH Gel Breakdown begin at >230o F.
Permeability

Lightweight slurries
Testing Process

LAB ANALYSIS
REQUEST

SLURRY DENSITY

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FREE FLUID FLUID LOSS
TEST TEST

RHEOLOGY

CEMENT - SPACER - MUD COMPRESSIVE STRENGTH

COMPATABILITY TEST

THICKENING TIME
TEST

LABORATORY REPORT
Laboratory Procedures & Equipment

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 Laboratory Analysis Request - (LAR)
Submitted to lab requesting formulation of
cement slurry
Designate additives available for slurry
Request specific performance parameters;

Density

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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

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Material Weight Absolute Volume Volume Weight Volume
(lbs) (gal) (gal) (gram) (ml)
Class G Cement 94 0.0382 3.59 42637.7 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
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

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– 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

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

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Free Fluid Test (API RP10B-2 sect. 15)

Slurry placed in 250ml graduated glass test tube

Free water (ml) measured after 2 hours

Slurry sedimentation also checked
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

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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

For slurries that dehydrate in less than 30 minutes, API

Fluid Loss value is obtained by either:

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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
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)

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– 300 rpm Approximation:
– 200 rpm Pv=(θ300 – θ100) x 1.5
– 100 rpm
– 60 rpm Τy= θ300 – Pv
– 30 rpm
– 6 rpm Use LabDB to calculate
– 3 rpm 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;

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10 seconds & 10 minutes
BOB (Stationary)
Rotational Ramp-up Ramp-down Ratio Average
Speed
(rpm)
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
Rotational Sleeve
100 100 115 0.87 107.5
200 137 147 0.93 142
300 170 170
Initial slurry temperature – 150 o F
Final slurry temperature – 146 o F
Rheological properties reported at average temperature – 148 o F Slurry Cup
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
Reported in Bearden units of consistency (Bc)

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Upper fluid limit: 70 Bc to 100 BC
API RP10B-schedules

Casing (1g - 11g)

Liners (22 - 32)

Squeeze cementing (12 - 21)

Refer to In-Touch ID is 4718717 for Laboratory Request

Checklist
 API Schedules
Pressure and Temperature changes
Effect on Thickening Time
Realistic Laboratory Evaluation
Computer Simulation (CemCADE)

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New Instrumentation
D e p th = 1 2 4 0 7 ft
210

A PI B H CT
G e o t h . P r o f ile
A n n u lu s
200
190
180
Temp. History (degF)
170
160
150
140
130

0 10 20 30 40 50 60 70 80 90
T im e (m in )
 Thickening Time Test Curves
Temperature
deg.F Instrument: 940 Left 940 L Test Start: 1/10/2008 2:25:18 PM 30 Bc @ 2:01:05

0 100 200 300 400 500 Well ID CCS08002-1R-D186-Exp

Customer SLB
Test Stop: 1/10/2008 6:02:18 PM 70 Bc @ 3:01:05
100 Bc @ 3:36:50
Comments: Retest of Exp D186 at 16.40 ppg 1500 psi and 65 F (room temp.).

140
130 100 5 100

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120 Bc 90 90

110 80 4 80

100 70 70

90
60 3 60
80 Temp.

Consistency (Bc)
Temperature (°F)

Pressure (kpsi)
70 50 50

60
Time (min)

40 2 40

50 30 30

40 20 1 20

30
10 10
20
10 0 0 0
0:00 0:30 1:00 1:30 2:00
Time (HH:MM)
2:30 3:00 3:30 4:00

0
Bc 50 100 Schlumberger Test File Name: 940 L-CCS08002-1R.tst Page 1
Pressurized Curing Chamber

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

Set cement strength under downhole conditions

Apparatus;

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Curing Bath (ATM pressure & 82oC)

Curing Chamber (3000 psi & 193oC)
Procedure.
Measurement Unit
Other methods
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
Proper filling cell

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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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UCA Chart
Laboratory Analysis Report

At the conclusion of Cement Slurry

formulation and subsequent testing a
report is produced outlining the

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following;

Well Information

Slurry Design

Lab Test results

Comments

Charts (TT, UCA)
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 API RP 10B-2 – Section 9
consistometer
Fluid Loss HPHP fluid loss cell API RP 10B-2 – Section 10
Compressive Strength Water bath, curing chamber API RP 10B-2 – Section 7

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Hydraulic press
Free Fluid 250 ml graduated cylinder API RP 10B-2 – Section 15
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
Spacer/Wash/Cement Compatibility Rotational viscometer API RP 10B-2 – Section 16
Reverse Emulsion Tester CEM- Section 2B5
Coupons, grid
Sedimentation test API RP 10B-2 – Section 15
Foam cement Closed mixer cup API RP10B-4
Specification for Cements Various API Spec 10A

Note: API RP10B-2 = ISO 10426-2

Also CEM- Section 6 lists all Schlumberger cement test procedures
Other Equipments and Tests

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Blend specific gravity measurement – Gas
Pycnometer

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Spacer Surfactant Selection Testing
Coupon Test Grid Test Reverse Emulsion Test

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Foam Cement Mixing & Foam cement Generator
under pressure

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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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