Laboratory Testing of Drilling Fluids

API RECOMMENDED PRACTICE 13I NINTH EDITION, DECEMBER 2020

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Copyright © 2020 American Petroleum Institute

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Foreword

Nothing contained in any API publication is to be construed as granting any right, by implication or otherwise, for the manufacture, sale, or use of any method, apparatus, or product covered by letters patent. Neither should anything contained in the publication be construed as insuring anyone against liability for infringement of letters patent.

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Contents

Page

1. Scope 1

   1. Objective 1

   2. Conditions of Applicability 1

2. Normative References 1

3. Terms, Definitions, Abbreviations, and Symbols 2

   1. Terms and Definitions 2

   2. Abbreviations 2

   3. Symbols 3

4. Abrasivity of Weighting Materials 5

   1. Principle 5

   2. Reagents and Apparatus 5

   3. Determination of Abrasivity of Weighting Materials 6

   4. Calculation—Determination of Abrasivity of Weighting Materials 7

5. Filtration-control Agents 7

   1. Principle 7

   2. Reagents and Apparatus 7

   3. General Instructions for Preparation of Base Drilling Fluids 9

   4. Salt-saturated, Drilling Fluid Preparation for Filtration Testing 9

   5. High-hardness, Salt-saturated Drilling Fluid Preparation for Filtration Testing 10

   6. 10 % Potassium Chloride (KCl) Drilling Fluid Preparation for Filtration Testing 10

   7. Pre-hydrated Bentonite Slurry Preparation for Filtration Testing 11

   8. Modified Seawater Drilling Fluid Preparation for Filtration Testing 12

   9. Low-salinity Drilling Fluid Preparation for Filtration Testing 12

   10. Lime-treated Drilling Fluid Preparation for Filtration Testing 13

   11. Low Solids, Non-dispersed Drilling Fluid Preparation for Filtration Testing 13

   12. Freshwater Lignosulfonate Drilling Fluid Preparation for Filtration Testing 14

   13. Initial Performance Filtration Test 14

   14. Low-temperature Filtration Performance Testing after Heat Aging 15

   15. HTHP Testing after Heat Aging 15

6. Methylene Blue Capacity of Drilled Solids and Commercial Bentonite 15

   1. Methylene Blue Capacity of Drill Solids 15

   2. Methylene Blue Capacity of Commercial Bentonite 18

   3. Equations to Calculate Drill Solids Content from Methylene Blue Capacity Results 20

7. Deflocculation Test for Thinner Evaluation 21

   1. Principle 21

   2. Reagents and Apparatus 21

   3. Determination of Moisture Content of Calcium Bentonite 23

   4. Preparation of Drilling Fluid Base for Calcium Bentonite Test 23

   5. Calculation of Solids Content of Calcium Bentonite in Drilling Fluid 23

   6. Determination of Rheological Properties of Calcium Bentonite Drilling Fluid Sample 24

   7. Calculation of Thinner Efficiency 26

8. Potassium Ion Content—Ion-selective Electrode (ISE) Method 26

   1. Principle 26

   2. Reagents and Apparatus 26

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   3. Preparation of Electrodes 27

   4. Operational Check of Electrode System 28

   5. Measurements Using a Meter with Direct Concentration-readout Capability 28

   6. Measurements with Instruments Providing Readout in Millivolts 29

9. Calcium Ion Content—Ion-selective Electrode (ISE) Method 30

   1. Principle 30

   2. Reagents and Apparatus 30

   3. Preparation of Electrodes 31

   4. Operational Check of Electrode System 31

   5. Measurements using a Meter with a Direct Concentration-readout Capability 32

   6. Measurements with Instruments Providing Readout in Millivolts 32

10. Sodium Ion Content—Ion-selective Electrode (ISE) Method 33

    1. Principle 33

    2. Reagents and Apparatus 34

    3. Preparation and Operational Check of the Electrode System 35

    4. Measurements using a Meter with a Direct Concentration-readout Capability 35

    5. Measurements with Instruments Providing Readout in Millivolts 36

11. Preparation and Evaluation of Non-aqueous Fluids (NAFs) 36

    1. Principle 36

    2. Reagents and Apparatus 37

    3. Mixing of the Initial Drilling Fluid 38

    4. Testing the Properties of the Initial Drilling Fluid 39

    5. Preparation of the Sample Contaminated by Seawater 39

    6. Preparation of the Sample Contaminated by Standard Evaluation Base Clay (SEBC) 39

    7. Preparation of the Sample Contaminated by Mixed-salt Brine 40

    8. Procedure for Hot-rolling 40

    9. Procedure for Static Aging 40

    10. Procedure for Testing after Heat Aging 41

12. Testing Base Fluid Properties Used in Non-aqueous Fluids (NAFs) 41

    1. General 41

    2. Reagents and Apparatus 41

    3. Density, Relative Density (Specific Gravity), or API Gravity—Hydrometer Method 41

    4. Density and Relative Density of Liquids Using a Digital Density-meter 42

    5. Kinematic Viscosity of Transparent and Opaque Oils—Calibrated Capillary Tube Method 42

    6. Distillation 42

    7. Aniline Point and Mixed Aniline Point 43

    8. Pour Point 43

    9. Flash Point by Pensky-Martens Closed Tester 43

    10. Aromatics Content 44

13. Testing Particle Size Distribution (PSD) in Drilling Fluids 45

    1. General 45

    2. Dry, Granular-solid Drilling Fluid Particulates 45

    3. PSD in a Non-aqueous Drilling Fluids 45

14. Aging of Water-based Drilling Fluids 45

    1. Principle 45

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    2. Practices Common to the Preparation, Handling, and Testing at all Temperature Ranges 46

    3. Metal Aging Cells 47

    4. Drilling Fluid Sample Preparation and Aging at Ambient Temperature 49

    5. Drilling Fluid Sample Preparation and Aging at Moderate Temperatures [Ambient to 65 °C (150 °F)] 51

    6. Water-based Drilling Fluid Sample Preparation and Aging at Elevated Temperatures [over 65 °C (150 °F)] 52

    7. Contrast between Drilling Fluid Material Performance in Laboratory Testing and Field Environments 53

15. Aging of Non-aqueous Drilling Fluids 53

    1. Principle 53

    2. Apparatus 53

    3. Metal Aging Cells 54

    4. Ovens 56

    5. Practices Common to the Preparation, Handling, and Testing at all Temperature Ranges 56

    6. Non-aqueous Drilling Fluid Aging at Ambient Temperatures 57

    7. Non-aqueous Drilling Fluid Aging at Moderate Temperatures [Ambient to 65 °C (150 °F)] 58

    8. Non-aqueous Drilling Fluid Aging at Elevated Temperatures [over 65 °C (150 °F)] 58

    9. Contrast Between Drilling Fluid Material Performance in Laboratory Testing and Field Environments 59

16. Shale-particle Disintegration Test by Hot-rolling 59

    1. Principle 59

    2. Reagents and Apparatus 59

    3. Procedure 60

    4. Calculation—Shale Disintegration by Hot-rolling 61

17. Measurement of Shear Strength using Shearometer Tube 61

    1. Principle 61

    2. Apparatus 62

    3. Procedure 62

    4. Calculation 62

Annex A (informative) HTHP Filtration Testing of Drilling Fluids using the Permeability-plugging Apparatus (PPA) 64

Annex B (normative) Particle Size Distribution (PSD) Measurement in a Non-aqueous Drilling Fluid using a Laser

Diffraction Instrument 74

Bibliography 81

Figures

1 Spot Tests for End point of Methylene Blue Titration 18

1. Immiscible Mud Clumps form when Alkane-based Mud is Mixed in IPA 77

2. Miscible Olefin-based Mud Fully Dispersed in IPA 77

3. PSD Curves of 70/30 (olefin/water) Mud at Different Flow Rates 78

4. PSD Curves of 70/30 (olefin/water) Mud at Different Flow Rates after 60 s Sonication 78

5. PSD Curves of 70/30 (olefin/water) Mud at 50 % and 75 % Flow Rate after Sonication 79

6. PSD Curves of 70/30 (olefin/water) Mud with Different Duration of Sonication at 100 % Power and the

   50

   Corresponding d

   Values 79

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7. Artifact Peaks Induced by Sonication Disappear over Time 80

Tables

1. API Ceramic Disk Designation and Mean Pore Throat Diameter 67

2. Recommended Minimum Cell Heat-up Pressure and Back-pressure 70

B.1 Average Refractive Index Value of Mineral Components in Drilling Fluids 76

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Introduction

This standard, which establishes testing methodologies for drilling fluid materials, formulations, and various properties, is based on API 13I, Eighth Edition. This 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 a 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 API 13B-1 and API 13B-2.

It is necessary that users of this standard be aware that further or differing requirements can be needed for individual applications. This Standard is not intended to inhibit a vendor from offering, or the purchaser from accepting, alternative equipment or engineering solutions for individual applications. 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 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 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 standard and does not constitute an endorsement by API of the products named. Equivalent products may be used if they can be shown to lead to the same results.

In this standard, quantities expressed in the International System of Units (SI) are also, where practical, expressed in U.S. customary units (USC) in parentheses for information. The values associated with the different units do not necessarily represent a direct conversion of SI units to USC units, or USC units to SI units. Consideration has been given to the precision of the instrument making the measurement. For example, thermometers are typically marked in one-degree increments, thus temperature values have been rounded to the nearest degree.

Calibrating an instrument refers to ensuring the accuracy of the measurement. Accuracy is the degree of conformity of a measurement of a quantity to its actual or true value. Accuracy is related to precision, or reproducibility, of a measurement. Precision is the degree to which further measurements or calculations will show the same or similar results. Precision is characterized in terms of the standard deviation of the measurement. The results of calculations or a measurement can be accurate but not precise, precise but not accurate, neither accurate nor precise, or both accurate and precise. A result is valid if it is both accurate and precise.

This document uses a format for numbers which follows the examples given in API Document Format and Style Manual, October 2020. This numbering format is different than that used in API 13I, Eighth Edition. In this document the decimal mark is a period and separates the whole part from the fractional part of a number. No spaces are used in the numbering format. The thousands separator is a comma and is only used for numbers greater than 10,000 (i.e. 5000 items, 12,500 bags).

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Laboratory Testing of Drilling Fluids

1. Scope

   
   

   1. Objective

      
      

      This standard provides procedures for the laboratory testing of both drilling fluid materials and drilling fluid

      physical, chemical, and performance properties.

      
      

   2. Conditions of Applicability

      
      

      This document is applicable to both water-based and non-aqueous 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.

      
      

      NOTE 1 This document does not include procedures related to testing barite specifications. These procedures are

      presented in API 13A.

      
      

      NOTE 2 This document does not include procedures related to testing barite for mercury, cadmium, and arsenic. These procedures are presented in API 13K.

      
      

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.

API 13A, Specification for Drilling Fluids Materials

API Recommended Practice 13B-1, Recommended Practice for Field Testing Water-based Drilling Fluids

API Recommended Practice 13B-2, Recommended Practice for Field Testing Oil-based Drilling Fluids

ASTM D86 1 , Standard Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure

ASTM D93, Standard Test Methods for Flash Point by Pensky-Martens Closed Cup Tester

ASTM D97, Petroleum Product—Determination of Pour Point

ASTM D287-12b, Standard Test Method for API Gravity of Crude Petroleum and Petroleum Products (Hydrometer Method)

ASTM D445, Standard Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)

ASTM D611, Standard Test Methods for Aniline Point and Mixed Aniline Point of Petroleum Products and Hydrocarbon Solvents

ASTM D1141, Standard Practice for the Preparation of Substitute Ocean Water

1 ASTM International, 100 Barr Harbor Drive, West Conshohoken, PA 19428-2959, www.astm.org.

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