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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

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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 Overview

5

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

11

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

22

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 Flask Investigation

26

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

Appendix

33

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

Results: Free Fluid 2016 Outliers

50