Recommended Practice for Laboratory Testing of Drilling Fluids

ANSI/API RECOMMENDED PRACTICE 13I EIGHTH EDITION, MARCH 2009

REAFFIRMED, MARCH 2016

ISO 10416:2008 (Identical), Petroleum and natural gas industries—Drilling fluids—Laboratory testing

Special Notes

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Copyright © 2009 American Petroleum Institute

API Foreword

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ii

Contents Page

API Foreword ii

Foreword vii

Introduction viii

1. Scope 1

2. Normative references 1

3. Terms and definitions 2

4. Symbols and abbreviations 3

5. Barite 6

   1. Principle 6

   2. Reagents and apparatus 6

   3. Sampling 7

   4. Calculation of moisture content 7

   5. Sieve analysis 7

   6. Sedimentation analysis 8

6. Barite performance 12

   1. Principle 12

   2. Reagents and apparatus 12

   3. Base drilling fluid preparation 13

   4. Rheology test 13

   5. Calculation 14

7. Abrasiveness of weighting materials 14

   1. Principle 14

   2. Reagents and apparatus 15

   3. Determination of abrasion 15

8. Mercury in drilling fluid barite 17

   1. Principle 17

   2. Reagents and apparatus 17

   3. Preparation of standards 19

   4. Sample digestion 19

   5. Check for recovery of Hg during digestion 20

   6. Analysis of standards and samples 20

   7. Calculation 20

9. Cadmium and lead in drilling fluid barite 21

   1. Principle 21

   2. Reagents and apparatus 21

   3. Preparation of combined cadmium and lead standards 22

   4. Sample digestion 22

   5. Analysis of standards and samples 22

   6. Calculation 23

10. Arsenic in drilling fluid barite 23

    1. Principle 23

    2. Reagents and apparatus 24

    3. Preparation of standards 25

    4. Sample digestion 25

    5. Analysis of standards and samples 26

    6. Calculation 26

11. Bridging materials for regaining circulation 26

    1. Principle 26

    2. Apparatus 27

    3. Preparation of test drilling fluid 27

    4. Static slot test 27

    5. Dynamic slot test 28

    6. Static marble bed test 28

    7. Dynamic marble bed test 28

    8. Static ball bearings (BB shot) bed test 29

    9. Dynamic ball bearings (BB shot) bed test 29

12. Filtration-control agents 29

    1. Principle 29

    2. Reagents and apparatus 29

    3. General instructions for preparation of base drilling fluids 31

    4. Salt-saturated drilling fluid 31

    5. High-hardness, salt-saturated drilling fluid 32

    6. 10 % potassium chloride (KCl) drilling fluid 32

    7. Pre-hydrated bentonite slurry 33

    8. Modified seawater drilling fluid 33

    9. Low-salinity drilling fluid 33

    10. Lime-treated drilling fluid 34

    11. Low solids, non-dispersed drilling fluid 34

    12. Freshwater lignosulfonate drilling fluid 35

    13. Initial performance test 35

    14. Performance after heat ageing 36

13. Methylene blue test for drilled solids and commerical bentonite 36

    1. Methylene blue capacity of drill solids 36

    2. Methylene blue capacity of commercial bentonite 39

    3. Solids content 40

14. Deflocculation test for thinner evaluation 41

    1. Principle 41

    2. Reagents and apparatus 42

    3. Procedure for moisture content 43

    4. Calculation of moisture content 43

    5. Preparation of drilling fluid base 43

    6. Calculation 44

    7. Determination of rheological properties 44

    8. Calculation of thinner efficiency 46

15. Testing base oils used in drilling fluids 46

    1. General 46

    2. Reagents and apparatus 46

    3. Density, relative density (specific gravity), or API gravity-hydrometer method (see ISO 3675). 46

    4. Density and relative density of liquids using a digital density meter (see ASTM D 4052) 47

    5. Kinematic viscosity of transparent and opaque oils — Calibrated capillary tube method (see ISO 3104) 47

    6. Distillation (see ISO 3405) 47

    7. Aniline point and mixed aniline point (see ISO 2977:1997) 48

    8. Pour point (see ISO 3016) 48

    9. Flash point by Pensky-Martens closed tester (see ISO 2719) 49

    10. Aromatics content (see IP 391 or ASTM D 5186) 49

16. Potassium ion content — Ion-selective electrode method 50

    1. Principle 50

    2. Reagents and apparatus 50

    3. Preparation of electrodes 51

    4. Operational check of electrode system 51

    5. Measurements using a meter with direct concentration readout capability 52

    6. Measurements with instruments that provide either a digital or an analogue readout in millivolts 52

17. Calcium ion content — Ion-selective electrode method 53

    1. Principle 53

    2. Reagents and apparatus 53

    3. Preparation of electrodes 54

    4. Operational check of electrode system 55

    5. Measurements using a meter with direct concentration readout capability 55

    6. Measurements with instruments that provide either a digital or an analogue readout in millivolts 55

18. Sodium ion content — Ion-selective electrode method 56

    1. Principle 56

    2. Reagents and apparatus 57

    3. Preparation and operational check of the electrode system 57

    4. Measurements using a meter with a direct concentration-readout capability 58

    5. Measurements using a meter with readout in millivolts 58

19. Density of solids — Stereopycnometer method 59

    1. Principle 59

    2. Apparatus 59

    3. Procedure — Stereopycnometer method 59

    4. Calculation — Stereopycnometer method 60

20. Density of solids — Air comparison pycnometer method 61

    1. Principle 61

    2. Apparatus 61

    3. Procedure — Air comparison pycnometer method 61

    4. Calculation — Air comparison pycnometer method 61

21. Ageing of water-based drilling fluids 62

    1. Principle 62

    2. Practices common to preparation, handling and testing over all temperature ranges 62

    3. Drilling fluid sample preparation and ageing at ambient temperature 63

    4. Drilling fluid ageing at moderate temperatures [ambient to 65 °C (150 °F)] 64

    5. Drilling fluid ageing at substantially elevated temperatures [over 65 °C (150 °F)] 66

    6. Inertness and chemical compatibility in high-temperature ageing cells 68

    7. Obtaining supplies and services for the ageing of drilling fluid samples 69

22. Ageing of oil-based drilling fluids 69

    1. Principle 69

    2. Apparatus 70

    3. Practices common to preparation, handling and testing over all temperature ranges 71

    4. Drilling fluid ageing at ambient temperatures 72

    5. Drilling fluid ageing at moderate temperatures [ambient to 65 °C (150 °F)] 73

    6. Drilling fluid ageing at substantially elevated temperatures [over 65 °C (150 °F)] 74

    7. Inertness and chemical compatibility in high-temperature ageing cells 75

    8. Obtaining supplies and services for the ageing of drilling fluid samples 76

23. Shale-particle disintegration test by hot rolling 76

    1. Principle 76

    2. Reagents and apparatus 77

    3. Procedure 77

    4. Calculation 78

24. Drilling fluid materials — High-viscosity polyanionic cellulose (PAC-HV) (regular) 79

    1. Principle 79

    2. Determination of moisture content 79

    3. Procedures with test fluid containing PAC-HV 80

25. Drilling fluid materials — Low-viscosity polyanionic cellulose (PAC-LV) 82

    1. Principle 82

    2. Determination of moisture content 83

    3. Procedures with test fluid containing PAC-LV 83

26. Preparation and evaluation of invert-emulsion drilling fluids 86

    1. Principle 86

    2. Reagents and apparatus 86

    3. Mixing of the initial drilling fluid 87

    4. Testing the properties of the initial drilling fluid 88

    5. Preparation of the sample contaminated by seawater 88

    6. Preparation of the sample contaminated by base evaluation clay 89

    7. Preparation of the sample contaminated by mixed-salt brine 89

    8. Procedure for hot-rolling 89

    9. Procedure for static ageing 89

    10. Procedure for testing after heat ageing 90

27. High-temperature/high-pressure filtration testing of drilling fluids using the permeability plugging apparatus and cells with set-screw-secured end caps 90

    1. Principle 90

    2. Safety considerations 90

    3. Apparatus — Permeability-plugging apparatus (PPA) with set-screw-secured end caps 92

    4. Procedure for high-temperature/high-pressure (HTHP) filtration 94

    5. Test conclusion and disassembly 97

    6. Data reporting 99

28. High-temperature/high-pressure filtration testing of drilling fluids using the permeability- plugging apparatus and cells with threaded end caps 100

    1. Principle 100

    2. Safety considerations 100

    3. Apparatus — Permeability-plugging apparatus (PPA) with threaded end caps 102

    4. Procedure for high-temperature/high-pressure (HTHP) filtration 104

    5. Test conclusion and disassembly 106

    6. Data reporting 108

Bibliography 110

Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights.

ISO 10416 was prepared by Technical Committee ISO/TC 67, Materials, equipment and offshore structures for petroleum, petrochemical and natural gas industries, Subcommittee SC 3, Drilling and completion fluids, and well cements.

This second edition cancels and replaces the first edition (ISO 10416:2002), which has been technically revised.

Introduction

This International Standard, which establishes testing methodologies for drilling fluid materials, is based on API RP 13I, seventh edition/ISO 10416:2002 [2]. This International Standard was developed in response to a demand for more exacting testing methodologies. The tests contained herein were developed over several years by a group of industry experts and were identified as being those which can yield reproducible and accurate results. The tests are anticipated to be performed in a laboratory setting, but can be applicable in a field situation with more rigorous apparatus and conditions than normally found in a drilling fluid field-test kit.

These tests are designed to assist in the evaluation of certain parameters for drilling fluids, with these properties not necessarily used for the maintenance of a drilling fluid in field use. The tests provide either more precision or different properties than those given in the field-testing standards ISO 10414-1 and ISO 10414-2.

It is necessary that users of this International Standard be aware that further or differing requirements can be needed for individual applications. This International Standard is not intended to inhibit a vendor from offering, or the purchaser from accepting, alternative equipment or engineering solutions for the individual application. This may be particularly appropriate where there is innovative or developing technology. Where an alternative is offered, the vendor should identify any variations from this International Standard and provide details.

As with any laboratory procedure requiring the use of potentially hazardous chemicals, the user is expected to have received proper knowledge and training in the use and disposal of these chemicals. The user is responsible for compliance with all applicable local, regional, and national regulations for worker and local health, safety and environmental liability.

This International Standard contains footnotes giving examples of apparatus, reagents and sometimes the supplier(s) of those materials that are available commercially. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO/API of the products named. Equivalent products may be used if they can be shown to lead to the same results.

API Recommended Practice 13I/ISO 10416

Petroleum and natural gas industries — Drilling fluids — Laboratory testing

1. Scope

   This International Standard provides procedures for the laboratory testing of both drilling fluid materials and drilling fluid physical, chemical and performance properties. It is applicable to both water-based and oil-based drilling fluids, as well as the base or “make-up” fluid.

   
   

   It is not applicable as a detailed manual on drilling fluid control procedures. Recommendations regarding agitation and testing temperature are presented because the agitation history and temperature have a profound effect on drilling fluid properties.

   
   

2. Normative references

The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 91-1:1992, Petroleum measurement tables — Part 1: Tables based on reference temperatures of 15 °C and 60 °F

ISO 2719, Determination of flash point — Pensky-Martens closed cup method

ISO 2977:1997, Petroleum products and hydrocarbon solvents — Determination of aniline point and mixed aniline point

ISO 3007, Petroleum products and crude petroleum — Determination of vapour pressure — Reid method

ISO 3016, Petroleum products — Determination of pour point

ISO 3104, Petroleum products — Transparent and opaque liquids — Determination of kinematic viscosity and calculation of dynamic viscosity

ISO 3405:2000, Petroleum products — Determination of distillation characteristics at atmospheric pressure

ISO 3675, Crude petroleum and liquid petroleum products — Laboratory determination of density — Hydrometer method

ISO 3696:1987, Water for analytical laboratory use — Specification and test methods

ISO 3839, Petroleum products — Determination of bromine number of distillates and aliphatic olefins — Electrometric method

ISO 10414-1:2008, Petroleum and natural gas industries — Field testing of drilling fluids — Part 1: Water-based fluids

ISO 10414-2:—1), Petroleum and natural gas industries — Field testing of drilling fluids — Part 2: Oil-based fluids

1) To be published. (Revision of ISO 10414-2:2002)