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API 2017 Exploration & Production Standards Conference on Oilfield Equipment and Materials,January 16 - 20, 2017
API 10A Cooperative Testing Report
Austin, TX
January 2017
Cooperative Testing Agenda
Charge of SC10/TG02
2016 Cooperative Testing Overview
Results
Cube Dimension Investigation
Free Fluid Flask Investigation
2
CHARGE of SC10/TG2
Task Group on Cooperative Testing (Bill Ulrich)
Coordinate efforts of the cooperative testing program.
Evaluate test results and present results at annual meeting
When necessary as dictated by the results, propose changes in the test procedure to insure results are statistically more accurate.
Coordinate efforts of the work group on compressive strength.
Work Group on Compressive Strength (Gunnar Debruijn)
Continue to evaluate the current specification test method by examining elements including mixing time, curing temperatures, curing time duration, curing baths (static vs. circulating) and cement block breaking procedures. Develop and propose a modified test method to yield improved repeatability.
3
Charge: Task Group Membership
Chair: William Ulrich
Members: Mailing List API
Robert Beirute – Consultant Greg Bernstein – LafargeHolcim John Buflod
Glen Benge – Consultant Jeff Moon – Chandler Ben Coco
Greg Garrison – Consultant Michael Trimble – Buzzi
Dan Mueller – Exxon
Heiko Plack – Dyckerhoff
Scott Podhaisky – LafargeHolcim
Jamie Hayes - Ofite
Scott Saville – Chandler
Paul Sonnier – CSI
2016 Cooperative Testing OverviewShipment Preparation for Cooperative
Sample Preparation
5 1-ton Big Bags obtained and tested for consistency.
Big bags were blended and
randomly tested for consistency.
Samples were prepared in 3 KG hermetically sealed bags.
6
2016 Cooperative Testing OverviewCosts
Costs for 2016 API Cooperative Testing Program US $
Labor for Packaging and Homogenization 4,500
Materials: Bags, Containers Labels, Preparation 7,600
Shipping Costs 23,100
TOTAL 35,200
7
2016 Cooperative Testing OverviewLessons Learned
Big 3 Service Companies (~2/3 of samples)
Ship to one site. (large quantities)
One contact vs multiple contacts
Copy model from Halliburton
Directions not followed (Cooperative Test Cover Letter and Instructions)
Feedback needed for improvement of document
Opportunity to develop a better reporting tool.
Opportunities for Future Cooperative Testing
8
2016 Cooperative Testing Overview
PARTICIPANT PROFILE
SAMPLES SUPPLIED RESULTS REPORTED2010 2012 2014 2016 2010 2012 2014 2016
PETROLEUM COMPANIES 4 5 9 4 4 4 7 4
SERVICE COMPANIES 234 201 267 195 140 143 247 95
HALLIBURTON 110 115 100 60 85 86 98 26
SCHLUMBERGER 111 60 80 73 46 49 80 42
BAKER HUGHES 5 14 74 43 4 1 65 25
OTHERS 8 12 13 19 5 7 4 2
CEMENT PRODUCERS 53 56 31 44 35 44 25 36
INTERESTED PARTIES 4 9 7 18 5 5 6 12
TOTAL SUPPLIED 295 271 314 261 184 196 285 147
Participation of SC10 group
9
** -- More samples results received after reporting deadline
2016 Cooperative Testing OverviewParticipation
101127
152
179
226
295271
314
261
101127
152156
186 184 196285
147
0
50
100
150
200
250
300
350
2000 2002 2004 2006 2008 2010 2012 2014 2016
PA
RTIC
IP
AN
TS
YEAR
Supplied vs Analyzed
TOTAL SUPPLIED TOTAL ANALYSIS
About 50% of sample results returned.
10
*
* -- More samples results received after reporting deadline
Results: 2016 Chemistry
CHEMICAL ANALYSIS (%) 2016 (W/O Exclusions)
API SpecC3S C3A SO3 MgO L.O.I.
48 to 65 3 Max. 3.0 Max 6.0 Max 3.00 Max
AVERAGE 60.15% 1.58% 2.78% 1.44% 0.82%
STD DEV 2.48% 0.46% 0.10% 0.07% 0.13%
COUNT 33 36 38 39 35
*Need to add Insol. Residue in 2018
ASTM C114-15 Table 1 Col 2 Duplicate Analyst Requirement 0.10% 0.16% 0.10%
Type Count Type Count Type Count
Cement Manufacturer 34 Energy/Other 4 Service 2
Lowest standard deviation in years.
Excluded samples – are samples that were not taken into consideration for analysis
Outliers – are samples that are more than 2 Std. Dev. These are facilities that should
review their test results.
12
Results: Chemistry
0
0.05
0.1
0.15
0.2
0.25
2000 2002 2004 2006 2008 2010 2012 2014 2016
SO3 Standard Deviation
STD DEV SO3 ASTM DUPLICATE MAX DIFF
2016 results near ASTM duplicate sample requirement
13
0
0.05
0.1
0.15
0.2
0.25
0.3
2000 2002 2004 2006 2008 2010 2012 2014 2016
MgO Standard Deviation
STD DEV MgO ASTM DUPLICATE MAX DIFF
0
0.05
0.1
0.15
0.2
0.25
2000 2002 2004 2006 2008 2010 2012 2014 2016
LOI Standard Deviation
STD DEV LOI ASTM DUPLICATE MAX DIFF
Results: Schedule 5 –Standard Deviation
1998 2000 2002 2004 2006 2008 2010 2012 2014 2016
STD DEV 13.82 7.87 10.87 13.37 7.78 12.08 9.89 13.16 7.53 4.33
COV 12.45 8.04 10.08 12.15 7.52 11.59 9.28 11.45 6.69 3.70
0
2
4
6
8
10
12
14
0
2
4
6
8
10
12
14
16
CO
V
STD
DEV
AXIS TITLE
SCH 5
Standard Deviation has almost decreased in half in Schedule 5.
14
2 Exclusions and 9 Outliers. Exclusions and Outliers in Appendix
Results: 2016 Schedule 5 – Comparison of Facilities
116
117
118
119
2 2.5 3 3.5 4 4.5 5 5.5
THIC
KET
NIN
G T
IME
TO 1
00
BC
STANDARD DEVIATION
SERVICE CEMENT MANUFACTURER Energy/Other/Consult
16
80
36
2016 SCH 5 Results
AVERAGE 117
STD DEV 4.3
COUNT 132
Good agreement amongst all groups with average and Std. Dev.
15
Results: Compressive Strengths Comparison
2000 2002 2004 2006 2008 2010 2012 2014 2016
STD DEV 257 241 229 341 216 281 149 279 134
COV 36 30 29 37 37 36 33 46 32
0
5
10
15
20
25
30
35
40
45
50
0
50
100
150
200
250
300
350
400
CO
V
ST
DD
EV
8HR 38C Standard Deviation
Steady results for all 3 strengths for Standard Deviation.
Results: 2016 Compressive Strengths Comparison 8HR 38°C
37
15
67
8HR 38oC PSI
AVERAGE 420
STD DEV 134
COUNT 117
A
V
E
R
A
G
E
STD. DEV.
Cement Manufacturer’s standard deviation lower
17
Results: 2016 UCA vs Cube 8 Hr & 24 Hr
18
Relatively good comparison – larger deviation on 24 hr cubes
1998 2000 2002 2004 2006 2008 2010 2012 2014 2016
STD DEV 0.76 0.88 0.96 0.85 0.98 0.87 1.09 0.94 1.07 0.64
COV 16.78 19.47 16.99 18.32 25.45 29.29 26.52 35.47 27.37 21.92
0.00
5.00
10.00
15.00
20.00
25.00
30.00
35.00
40.00
0.40
0.50
0.60
0.70
0.80
0.90
1.00
1.10
1.20
CO
V
STD
DEV
Free Fluid
Results: Free Fluid 2016
Lowest Free Fluid Standard Deviation
19
4 Exclusions and 9 Outliers. Exclusions and Outliers in Appendix
Results: 2016 Free Fluid
Cement Manufacturers had the lowest Standard Deviation
35
18
88
20
Free Fluid %
AVERAGE 2.92
STD DEV 0.64
COUNT 140
Results: Observations
21
Best deviations seen in years
Participation numbers down?
Preparation method?
More precise testing in laboratories?
Other?
Cube Dimension Investigation
Evaluation of whether or not cube dimensions need to be measured?
API vs ASTM Standards
Every cube measured – API
Periodic check of cubes – ASTM
Cubes are not done in – EN
2 in. ± 0.005
2 in. + 0.01 in.to − 0.005 in.
2 in. ± 0.022 in. ± 0.005
2 in. ± 0.02
NewIn Use
New
In Use
to − 0.015 in.2 in. + 0.01 in.
New
In Use
Cube molds need to be measured
and certified every 2 years
23
Cube Dimension - Comparison
No difference observed on cube strength on the dimension extremes
24
8 hr 60°C 24 hr 38°C
8 hr 38°C
> 2 in < 2 in> 2 in < 2 in
> 2 in < 2 in
Cube Dimension Conclusions and Observations
Data indicates an opportunity to eliminate the measurement of cube dimensions.
8 hr and 24 hr shows no major differences.
Opportunity to align with ASTM
Open Discussion in Work Group meeting in Feb. 2017 on where we go from here.
25
Free Fluid Investigation
• Asked participant to provide flask used in measurement
• What type of flasks being used?
• Opportunity to improve specification?
• 500mL conical flask
• ASTM 1404 Type I, Class 2 or ISO 24450
• Type I general purpose with
graduated scale.
• Class 2 wide mouth (#10 stopper)
with heavy duty beaded top.
27
Free Fluid Flasks
172
mm
97 mm
#10 Stopper#10 Stopper
105 mm175 m
m
Both meet specification but still different
28
Free Fluid Flasks
# 7 Stopper
175 m
m102 mm
#7 Stopper
176 m
m
101 mm
#10 Stopper
238 m
m
138 mm
Free Fluid Flasks does not Meet Specification
29
Free Fluid Investigation
30
10 NC
7 NC
51 NC
21 C
10 C
27 C
Non-Compliant Flasks had larger Standard Deviation
NC – Non-Compliant Flask
C – Compliant Flask
Number = Population
Free Fluid Flasks Observations Cement Facilities vs Service
Cement Manufacturer
Service
Entire Population
No variances observed in populations
Free Fluid Conclusions and Observations
Opportunity to improve the specification?
Clarify API 10A specification
Currently in progress with next 10A re-write
Recommendation for a study for FF. variability on flasks.
Opportunity of testing a flask 10/20/30 times with same cement.
Is same testing standard deviation observed?
Small group of testing to verify?
Open Discussion in Work Group meeting in Feb. 2017 on where we go from here.
32
Results: Chemistry
SiO2 Al2O3 Fe2O3 CaO MgO SO3 LOI
AVERAGE 21.46 3.53 4.59 64.20 1.44 2.78 0.82
STD DEV 0.60 0.25 0.14 0.76 0.15 0.10 0.13
EXCLUSIONS SiO2 Al2O3 Fe2O3 CaO MgO SO3 LOI
API16-002 Cement 35
API16-055 Service 69
API16-095 Cement 70
API16-107 Energy 1.94
API16-206 Other 14.3 2 5.3 73.60 0.37
OUTLIERS
API16-008 Service 18.9 2.74 4.15 66.5 1.00 3.14
API16-022 Cement
API16-055 Service 4.93
API16-089 Cement 1.79
API16-090 Cement 4.86
API16-102 Cement
API16-106 Cement 1.19
API16-107 Energy 24.77 4.41 67.07
API16-110 Cement 4.12
API16-111 Cement 2.52
API16-114 Energy 1.13
API16-202 Cement 1.93 1.1534
Results: Chemistry – SO3
0
0.05
0.1
0.15
0.2
0.25
2000 2002 2004 2006 2008 2010 2012 2014 2016
SO3 Standard Deviation
STD DEV SO3 ASTM DUPLICATE MAX DIFF
Exclusions SO3
API16-008 Service 3.14%
API16-107 Energy 1.94%
2016 SO3 Results
AVERAGE 2.78%
STD DEV 0.10%
Outliers SO3
API16-111 Service 2.52%
API16-258 Cement 2.97%
2016 results near ASTM duplicate sample requirement
36
Results: Chemistry – MgO
0
0.05
0.1
0.15
0.2
0.25
0.3
2000 2002 2004 2006 2008 2010 2012 2014 2016
MgO Standard Deviation
STD DEV MgO ASTM DUPLICATE MAX DIFF
Exclusions MgO
API16-206 Other 0.37%
Outliers MgO
API16-008 Service 1.00%
API16-089 Cement 1.79
API16-114 Service 1.13%
API16-202 Cement 1.93%
2016 MgO Results
AVERAGE 1.44%
STD DEV 0.15%
Better than ASTM duplicate sample requirement
Results: Chemistry – LOI
0
0.05
0.1
0.15
0.2
0.25
2000 2002 2004 2006 2008 2010 2012 2014 2016
LOI Standard Deviation
STD DEV LOI ASTM DUPLICATE MAX DIFF
Exclusions LOI
API16-055 Service 69.00%
API16-095 Cement 70.00%
Outliers LOI
API16-055 Cement 1.19%
API16-095 Cement 1.15%
2016 LOI Results
AVERAGE 0.82%
STD DEV 0.13%
Stable results over the years
38
Results: XRD/Rietveld
Alite BeliteAluminate
CubicAluminate
Ortho GypsumHemi-
hydrate Anhydrite Lime
Average 64.78 15.75 0.81 0.66 0.89 0.42 3.11 0.19
STD Dev 3.30 2.88 0.46 0.73 0.58 0.31 1.21 0.10
Count 13 13 11 11 13 9 12 11
Exclusions
API16-010 CEMENT 5.05
API16-055 SERVICE 55 24
API16-201 CEMENT 1.8
API16-205 CEMENT 2.4
OUTLIERS
API16-092 CEMENT 1.45
API16-098 CEMENT 5.62
With 14 Facilities reporting WIDE VARIATION (not a good
statistical analysis)
39
Results: Schedule 5 –Exclusions and Outliers
Exclusions Sch 5 (min)
API16-038 Service 158
API16-054 Service 174
40
Outliers
API16-008 Service 129
API16-044 Service 126
API16-058 Service 127
API16-060 Service 135
API16-064 Service 130
API16-074 Service 127
API16-088 Cement 127
API16-102 Cement 126
API16-220 Service 107
Results: Compressive Strengths Comparison
454379
592
467 449
369
0
100
200
300
400
500
600
700
2000 2002 2004 2006 2008 2010 2012 2014 2016
8HR 60C Standard Deviation
STD DEV 8hr 60
257 241 229
341
216
281
149
279
134
0
50
100
150
200
250
300
350
400
2000 2002 2004 2006 2008 2010 2012 2014 2016
8HR 38C Standard Deviation
STD DEV 8hr 38536
607625
663
594610 612
400
450
500
550
600
650
700
2000 2002 2004 2006 2008 2010 2012 2014 2016
24HR 38C Standard Deviation
STD DEV 24hr 38
15.6
15.8
16
16.2
16.4
16.6
16.8
17
17.2
17.4
17.6
17.8
2 2.5 3 3.5 4 4.5 5
10 S
EC G
EL (
LBF/
100
FT2)
STANDARD DEVIATION
Service Cement Manufacturer Energy/Other/Consult
Results: Rheology – 10 Sec Gel
88
19
12
Possible opportunity for cement manufacturers improvement
10 Sec Gellbf/100 ft2
AVERAGE 17.2
STD DEV 4.24
# OF TESTS 119
Exclusions 10 sec Gel
API16-226 Service 50.8
42
Outliers
In Appendix
15
17
19
21
23
25
27
29
31
4 5 6 7 8 9 10
10 M
IN G
EL (
LBF/
100
FT
2)
STANDARD DEVIATION
Service Cement Manufacturer Energy/Other/Consult
Results: Rheology – 10 Min Gel
19
12
Possible opportunity for cement manufacturers improvement
10 Min Gellbf/100 ft2
AVERAGE 26.5
STD DEV 8.67
# OF TESTS 118
88
Exclusions 10 min Gel
API16-084 Service 72.0
API16-226 Service 48.0 43
Outliers
In Appendix
Results: Rheology – Exclusions & Outliers
Facilities Excluded:
10 minute
Gel
Strength
10 second
Gel
Strength
Rotational
Speed 3
Rotational
Speed 300
API16-043 Service 46.0
API16-084 Service 72.0
API16-226 Service 48.0 50.8 89.0 15.0
Facility Outliers:
API16-021 Cement Manufacturer 26.0 24.5
API16-043 Service 8.9
API16-050 Service 50.0
API16-056 Service 6.5
API16-057 Service 49.0
API16-062 Service 6.0
API16-063 Service 33.0
API16-082 Service 51.2 28.8 23.0
API16-147 Service 27.0
API16-217 Service 46.0 27.0 24.5
API16-238 Service 47.6
API16-243 Service 47.6
API16-248 Service 24.5
44
Results: Cubes (8HR 38oC, 8HR 60oC, 24HR 38oC)Compressive Strengths
24 HOUR -38oC
DATA MINUS EXCLUSIONS
AVERAGE 2840
STD DEV 612
COUNT 103
All of the Exclusions and Outliers are Service Companies
8 HOUR - 38oC
DATA MINUS EXCLUSIONS
AVERAGE 420
STD DEV 134
COUNT 117
8 HOUR - 600C
DATA MINUS EXCLUSIONS
AVERAGE 1930
STD DEV 369
COUNT 117
EXCLUDED 8HR 38oC 8HR 60oC 24HR 38oC
API16-044 Service 1320
API16-048 Service 770
API16-062 Service 750
API16-078 Service 1180
API16-082 Service 1290
API16-143 Service 1620
API16-189 Service 420
API16-220 Service 980
OUTLIERS 8HR 38oC 8HR 60oC 24HR 38oC
API16-056 Service 80
API16-064 Service 790 2700
API16-082 Service 1040
API16-129 Service 980
API16-145 Service 900
API16-161 Service 1150
API16-164 Service 810
API16-218 Service 1040
API16-221 Service 270 1050
API16-226 Service 4260
API16-239 Service 50
45
Results: UCA vs Cube
UCA to Cube Comparison2016
Cubes UCA
8 HOUR -
1000F
8 HOUR -
1000F
AVERAGE 420 AVERAGE 640
STD DEV 134 STD DEV 214
COUNT 117 COUNT 105
Cubes UCA
24 HOUR -
1000F
24 HOUR -
1000F
AVERAGE 2840 AVERAGE 2670
STD DEV 612 STD DEV 287
COUNT 103 COUNT 104
Outliers UCA 8HR Outliers Cubes 24HR
API16-064 Service 1203 API16-062 Service 1590
API16-218 Service 1500
API16-226 Service 4260
Exclusion UCA 8HR Exclusion Cubes 24HR
API16-003 Other 1720 API16-044 Service 1320
API16-220 Service 1704 API16-048 Service 770
API16-082 Service 1290
API16-189 Service 420
API16-220 Service 980
24 HR cubes showed a Large STD Compared to UCA
46
Results: UCA
0
100
200
300
400
500
600
700
800
0.0 50.0 100.0 150.0 200.0 250.0
THIC
KET
NIN
G T
IME
TO 1
00
BC
STANDARD DEVIATION
UCA 8 HR (PSI)
Service Cement Energy/Consult/Other
16
4
85
The difference in the 8 HR UCA Cement Producers is more than
the STD. UCA
8 HR - 1000F
AVERAGE 640
STD DEV 214
COUNT 105
47
Results: UCA – Time to 50 & 500 PSI
TIME TO 50 PSICEMENT OTHERS SERVICE
AVG 4:57 3:47 3:58
STD 0:35 0:57 0:55
COUNT 4 17 85
TIME TO 500 PSI
CEMENT OTHERS SERVICE
AVG 8:54 7:09 7:15
STD 1:01 1:03 1:10
COUNT 4 16 86
Exclusion 50 PSI
API16-065 Service BAD #
Exclusion 500 PSI
API16-003 Other 3:19
Oultier 500 PSI
API16-062 Service 9:46
API16-064 Service 4:55
API16-088 Cement 9:43
API16-094 Cement 9:51
API16-220 Service 4:18
Oultier 50 PSI
API16-003 Other 2:06
API16-066 Service 1:15
API16-094 Service 6:02
API16-209 Service 6:09
Large Standard Deviations on the Time To
48
Results: UCA – 8 Hr & 24 Hr PSI
8 HR PSI
CEMENT OTHERS SERVICE
AVG 391 733 654
STD 120.1 321.6 237.8
COUNT 4 17 92
24 HR PSI
CEMENT OTHERS SERVICE
AVG 2,306 2,733 2,672
STD 485.5 326.3 265.3
COUNT 3 17 84
Exclusion 8 HR
API16-003 Other 1720
API16-220 Service 1704
Large Standard Deviations on the Time To
Exclusion 24 HR
API16-094 Cement 785
API16-237 Service 4120
API16-244 Service 4341
Oultier 8 HR Oultier 24 HR
API16-062 Service 1703
API16-088 Cement 1747
49