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Cement Lab

Introduction
Module CF116
09 Sep 99

Laboratory Functions

Two types of Laboratory testing :


1. Performance Evaluation
Slurry Design Stage

Measurement of specific slurry properties under simulated


downhole conditions.

Execution Stage

Monitor preparation of blended materials

2. Chemical Characterisation
Quantitative or qualitative analysis of the slurry

components prior to mixing.


Cement
Additives
Mix Fluid

Performance EvaluationSlurries
Governed by the API committee
on Standardisation of Oilwell
Cements (10A & 10B)

Publication consists of;

Test specifications for neat


cement slurries
Operational testing
procedures for all slurries

Procedures designed to simulate

downhole conditions

Pressure

Temperature

Performance EvaluationSpacers/Washes

Evaluation of the cleaning effect

Compatibility with Cement


Thickening Time
Excerpt API Spec 10B
Fluid Loss
Compressive Strength
Rheology
Effects on mud

Rheology

Fluid Compatibility
API Spec. 10 contains the procedures for

measuring the compatibility of fluids.

The effects of a spacer or chemical wash

are investigated.

Compatible fluids result in very equal sets

of Fann 35 readings.
Large difference between test results

indicates incompatibility.
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Chemical Characterization
Four types of samples are examined
Cement Powder
C3A, C3S, C2S, C4AF and Gypsum

Dry Blended Cement


Consistency

Set Cement
Mix water

Sample
Preparation

Sampling
Sample acquisition
Prior to shipment (batch number)
From rig site
ALWAYS use actual field samples & labelled.
Sampling procedures as per API spec 10B

Section 4

Cement & blends at field location


Dry & liquid cement additives at field location
Mixing water

Disposal
Comply with all regulatory requirements

Slurry Design

Slurry Properties
Free Water & Slurry Sedimentation
Water separation from static slurry
Migrates upward, accumulates in pockets

or at top of cement column.

Results in incomplete zonal isolation

Density
Balance sub-surface pressures
Cement final strength

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Slurry Properties - cont.


Pumpability (Slurry Consistency)
Length of time slurry remains in a pumpable

fluid state (Job Time + 1 Hour)


Fluid Loss
Slurry dehydration during placement phase

Rheology
Slurry flow modelling

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Set Cement Properties


Bonding
Cement - Casing & Cement - Formation

Sulfate Resistance
Reaction to magnesium and sodium sulfates;

Loss of compressive strength

Stress cracking

Strength Retrogression
Cement Shrinkage occurs at >230F (110C).

Permeability
Lightweight slurries

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Testing Process
LAB ANALYSIS
REQUEST(LAR)
SLURRY DENSITY

RHEOLOGY

FREE WATER
TEST

FLUID LOSS
TEST

CEMENT - SPACER - MUD


COMPATABILITY

THICKENING TIME
TEST

COMPRESSIVE STRENGTH
TEST

LABORATORY REPORT

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Laboratory
Procedures
& Equipment

Lab Analysis Request (LAR)

Submit LAR to lab requesting a slurry

formulation
Designate additives available for slurry design
Request specific performance parameters;

Density
Rheology ( PV, YP & Gel Strength)
Fluid Loss
Thickening Time
Free Water
Compressive Strength

Provide information on well parameters


Job Type, Depth (MD/TVD)
Temperatures (BHST/BHCT/maxHCT)
Pressure Profiles.

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Laboratory Analysis Report


At the conclusion of Cement Slurry

formulation and subsequent testing a


report is produced outlining the following;
Part 1

Information requested
Summary of results
Conclusions and recommendations

Part 2
Laboratory Tests and Results
Part 3
Appendices as necessary

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Slurry
Properties

LAR Number
Well Conditions

Slurry
Formulation

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Typical LAR format


generated by LabDB*
software

Sample Calculation
Sample volume for slurry testing is 600 ml
Consider the following slurry composed of;
Class G Neat & 44% water
Material
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 = Total Volume / 600 ml
= 54:1

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Slurry Preparation -

API spec 10B

Section 5
Mixed with a high shear mixer (Waring Blender)
Water and Liquid Additives mixed first.
D20 and polymer need to pre-hydrate prior to

adding dispersant and retarder.

Add Cement /Solids & mix at 4000 rpm for 15

sec.

Continue mix at 12,000 rpm for 35 sec.


Mixing procedure not suitable for;
Microspheres (D124)
Foam slurries

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Slurry Tests - Density & FW


Density Measurement (API Spec 10B Section 6)
Pressurized or Atmospheric Balance
Units are ppg, Kg/m3, SG

Free Water Test (API Spec 10 Section 6)


Slurry placed in 250ml graduated glass test

tube
Free water (ml) measured after 2 hours

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Static Fluid Loss -

API Spec 10B

Section 10
Simulates amount of fluid loss under pressure
against a permeable formation
Use HPHT cell (simulates downhole conditions)

P = 1000psi, 93F>T > 194F (90C)

Formation simulated by 325 mesh screen

Backed up by a 60 mesh screen

Conditioning procedures as per Section 10.6 &

10.7
Testing procedure as per Section 10.11

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Filtrate Loss
For slurries that dehydrate in less than 30

minutes, Fluid Loss value is obtained by :


The Relationship

F 30= 2Qt

5.477
t

F30 = Calculated API Filtrate at 30 minu


Qt = Vol (ml) of Filtrate at time t (min)
t = Time in minutes

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Rheology -

API Spec 10B Section 12

Correlation between shear stress and

shear rate
Tested with Viscometer (FANN 35)
Rotational speed (Shear rate)

300 RPM
200 RPM
100 RPM
60 RPM
30 RPM

600 RPM not used.


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Rheology
6 RPM and 3 RPM readings omitted.
3 RPM reading is used to determine

the fluid gel strength at;


10 seconds & 10 minutes

Rotational Sleeve

Slurry Cup

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BOB (Stationary)

Slurry Tests - cont.


Thickening Time

Determine length of time a slurry remains


fluid
Pressurized consistometer simulates both;
Temperature
Pressure
Reported in Beardon units of consistency (BC)
Upper fluid limit (API) 100 BC
API spec 10 for P-T schedules (example Fig B-7 in Well
Cementing)
Casing,

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Liners, Squeeze cementing

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Thickening Time Test Curve


Temperature

Time (min)

0
140
130
120
110
100
90
80
70
60
50
40
30
20
10
0

100
200
deg.F

400

500

Bc

Temp.

Bc

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300

50

100

API Schedules -

API Spec 10B

Section 9.5
Pressure and Temperature
schedules derived from field data
schedules available for casing, liner and
squeeze jobs
P-T effect on Thickening Time
continuous exposure to varying P-T profiles
max P-T not necessarily at same point
TOC will be exposed to max P-T while circulating
New Instrumentation & Refine Procedures
API schedules do not cover all factors
dynamic wellbore simulation tool

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Solution - CemCADE

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BHCT Prediction
degF ( * 100)
0.5

1.5

3.5

2.5

Formation
Annulus
Casing Fluids

Max
HCT
BHCT

Mud Temp. Profile At 180 min

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Slurry Tests - Compressive


Strength
Set cement strength under downhole

conditions
Apparatus;
Curing Bath (ATM pressure & 82 oC)
Curing Chamber (3000 psi & 193 oC)
Procedure.
Measurement Unit
Other methods

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Test Category
Sampling
Slurry Preparation

Summary of Test
Procedures

Slurry Conditioning
Thickening Time
Static Fluid Loss
Compressive Strength
Free Water
Permeability
Rheology
Static Gel Strength
Expansion
Spacer/Wash/Cement
Compatibility
Particle Analysis (Portland
Cement)
Chemical Analysis of Dry Blends
Chemical Analysis of Mix water

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Equipment
Diverter Flow Sampler
2-Speed Propeller Mixer

Atmospheric Consistometer
Atmospheric and Pressurized
Consistometer
HTHP Fluid Loss Cell
Water/cooling Bath, Curing
Chamber, Hydraulic Press, UCA
250ml graduated glass cylinder
Permeameter
Rotational viscometer
Rotational viscometer
Bar mould, Cylindrical sleeves
Rotational viscometer, Fluid loss
cell, Consistometer, Hydraulic
press
Blaine permeameter

Procedure Reference
ASTM C702, API Spec 10(3) & 10B(4)
API Spec 10(5) & 10B(5)
See relevant sections for Free water,
Fluid loss and Rheology in API Spec 10
& 10B
API Spec 10(8) & 10B(9)
API Spec 10(App F) & 10B(10)
API Spec 10(7) & 10B(7 and 8)
API Spec 10(6 and App M) & 10B(15)
API Spec 10(App G) & 10B(11)
API Spec 10(App H) & 10B(12)
API RP 13B(2) & 10B(12.7)
ASTM C151

API Spec 10(App P) & 10B(16)


ASTM C204

UV absorption spectrophotometry ASTM C114


Wet chemical method
API RP 45