Drilling Fluids Materials

API SPECIFICATION 13A

NINETEENTH EDITION, OCTOBER 2019

API MONOGRAM PROGRAM EFFECTIVE DATE: OCTOBER 1, 2020 ADDENDUM 1, APRIL 2020

Special Notes

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Copyright © 2019 American Petroleum Institute

Foreword

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1. Scope 1

2. Normative References 1

3. Terms, Definitions, Symbols, and Abbreviations. 1

   1. Terms and Definitions 1

   2. Symbols 2

   3. Abbreviations 4

4. Requirements 5

   1. Quality Control Instructions 5

   2. Use of Test Standard Materials in Checking Testing Procedures 5

   3. Records Retention 5

5. Calibration 5

   1. Coverage 5

   2. Equipment Requiring Calibration 6

   3. Calibration Intervals 12

6. Packaged Material 13

   1. Description 13

   2. Apparatus-Pallets 13

   3. Apparatus-Bags 14

   4. Marking-Palletized Material 14

   5. Marking-Bags 14

   6. Pallet Covers 15

   7. Package Mass 15

   8. Storage 15

   9. Recycling 15

7. Barite 15

   1. Principle 15

   2. Reagents and Apparatus-Measuring Barite Density by the Le Chatelier Flask Method 16

   3. Procedure-Measuring Barite Density by Le Chatelier Flask Method 16

   4. Calculation-Barite Density by Le Chatelier Flask Method 17

   5. Reagents and Apparatus-Measuring Water-soluble Alkaline Earths as Calcium in Barite 18

   6. Procedure-Measuring Water-soluble Alkaline Earth Metals as Calcium in Barite 18

   7. Calculation-Measuring Water-soluble Alkaline Earths as Calcium in Barite 19

   8. Reagents and Apparatus-Measuring Barite Residue Greater than 75 µm 19

   9. Procedure-Measuring Barite Residue Greater than 75 µm 20

   10. Calculation-Barite Residue Greater than 75 µm 20

   11. Reagents and Apparatus-Measuring Barite Particles Less than 6 µm in Equivalent

       Spherical Diameter by Sedimentation Method 20

   12. Procedure-Measuring Barite Particles Less than 6 µm in Equivalent Spherical Diameter by Sedimentation Method 21

   13. Calculation-Barite Particles Less than 6 µm in Equivalent Spherical Diameter by Sedimentation Method 22

8. Hematite (Haematite) 27

   1. Principle 27

   2. Reagent and Apparatus-Measuring Hematite Density by Le Chatelier Flask Method 28

   3. Procedure-Measuring Hematite Density by Le Chatelier Flask Method 28

      v

      
      

   4. Calculation-Hematite Density by Le Chatelier Flask Method 29

   5. Reagents and Apparatus-Measuring Water-soluble Alkaline Earth Metals as Calcium in Hematite . 29

   6. Procedure-Measuring Water-soluble Alkaline Earth Metals as Calcium in Hematite 30

   7. Calculation-Water-soluble Alkaline Earth Metals as Calcium in Hematite 31

   8. Reagents and Apparatus-Measuring Hematite Residue Greater than 75 µm and 45 µm 31

   9. Procedure-Measuring Hematite Residue Greater than 75 µm and 45 µm 32

   10. Calculation-Hematite Residue Greater than 75 µm and 45 µm 32

   11. Reagents and Apparatus-Measuring Hematite Particles Less than 6 µm in Equivalent Spherical Diameter by the Sedimentation Method 33

   12. Procedure-Measuring Hematite Particles Less than 6 µm in Equivalent Spherical Diameter by the Sedimentation Method 33

   13. Calculation-Hematite Particles Less than 6 µm in Equivalent Spherical Diameter by the

       Sedimentation Method 34

9. Bentonite 37

   1. Principle 37

   2. Reagents and Apparatus-Measuring Properties of a Bentonite Suspension 37

   3. Procedure-Measuring Rheological Properties of a Bentonite Suspension 38

   4. Calculation-Measuring Rheological Properties of a Bentonite Suspension 38

   5. Procedure-Measuring the Filtrate Volume of a Bentonite Suspension 39

   6. Calculation-Filtrate Volume of a Bentonite Suspension 39

   7. Reagents and Apparatus-Measuring Bentonite Residue of Greater than 75 µm 39

   8. Procedure-Measuring Bentonite Residue Greater than 75 µm 40

   9. Calculation-Bentonite Residue Greater than 75 µm 40

10. Non-treated Bentonite 40

    1. Principle 40

    2. Reagents and Apparatus-Measuring Properties of a Non-treated Bentonite Solution 41

    3. Procedure-Measuring Yield Point-Plastic Viscosity Ratio of a Non-treated Bentonite Suspension. . 41

    4. Calculation-Yield Point-Plastic Viscosity Ratio of a Non-treated Bentonite Suspension 42

    5. Procedure-Measuring the Plastic Viscosity of a Dispersed Non-treated Bentonite Suspension 42

    6. Procedure-Measuring the Filtrate Volume of a Dispersed Non-treated Bentonite Suspension 43

    7. Calculation-Filtrate Volume of a Dispersed Non-treated Bentonite Suspension 43

11. Attapulgite 44

    1. Principle 44

    2. Reagents and Apparatus-Measuring Properties of an Attapulgite Suspension 44

    3. Procedure-Measuring 600 r/min Dial Reading of an Attapulgite Suspension 44

    4. Reagent and Apparatus-Measuring Attapulgite Residue Greater than 75 µm 45

    5. Procedure-Measuring Attapulgite Residue Greater than 75 µm 45

    6. Calculation-Residue of Attapulgite Greater than 75 µm 46

    7. Reagent and Apparatus-Measuring Moisture Mass Fraction of Attapulgite 46

    8. Procedure-Measuring Moisture Mass Fraction of Attapulgite 46

    9. Calculation-Moisture Mass Fraction of Attapulgite 47

12. Sepiolite 47

    1. Principle 47

    2. Reagents and Apparatus-Measuring Properties of a Sepiolite Suspension 47

    3. Procedure-Measuring 600 r/min Dial Reading of a Sepiolite Suspension 48

    4. Reagents and Apparatus-Measuring Sepiolite Residue Greater than 75 µm 48

    5. Procedure-Measuring Sepiolite Residue Greater than 75 µm 49

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    6. Calculation-Sepiolite Residue Greater than 75 µm 49

    7. Reagents and Apparatus-Measuring Moisture Mass Fraction of Sepiolite 49

    8. Procedure-Measuring Moisture Mass Fraction of Sepiolite 50

    9. Calculation-Moisture Mass Fraction of Sepiolite 50

13. Technical-grade, Low-viscosity Carboxymethyl Cellulose (CMC-LVT) 50

    1. Principle 50

    2. Qualitative Determination of Starch or Starch Derivatives in a CMC-LVT Sample 51

    3. Reagents and Apparatus-Measuring Properties of CMC-LVT Water-soluble Polymers 53

    4. Procedure-Measuring 600 r/min Dial Reading of CMC-LVT Deionized Water Solution 53

    5. Procedure-Measuring Filtrate Volume of CMC-LVT Clay Suspension 54

    6. Calculation-Filtrate Volume of a CMC-LVT Clay Suspension 55

14. Technical-grade, High-viscosity Carboxymethyl Cellulose (CMC-HVT) 55

    1. Principle 55

    2. Qualitative Determination of Starch or Starch Derivatives in a CMC-HVT Sample 56

    3. Reagents and Apparatus-Measuring Properties of CMC-HVT Water-soluble Polymers 58

    4. Procedure-Measuring 600 r/min Dial Reading of CMC-HVT Deionized Water Solution 59

    5. Procedure-Measuring 600 r/min Dial Reading of a CMC-HVT 40 g/L Saltwater Solution 59

    6. Procedure-Measuring 600 r/min Dial Reading of a CMC-HVT Saturated Saltwater Solution 60

    7. Procedure-Measuring Filtrate Volume of a CMC-HVT Clay Suspension 60

    8. Calculation-Filtrate Volume of a CMC-HVT Clay Suspension 61

15. Starch 61

    1. Principle 61

    2. Reagents and Apparatus-Measuring Properties of a Starch Suspension 62

    3. Procedure-Measuring 600 r/min Dial Reading of a Starch 40 g/L Saltwater Suspension 63

    4. Procedure-Measuring Filtrate Volume of a Starch 40 g/L Saltwater Suspension 63

    5. Calculation-Filtrate Volume of a Starch 40 g/L Saltwater Suspension 64

    6. Procedure-Measuring 600 r/min Dial Reading of a Starch Saturated Salt Suspension 64

    7. Procedure-Measuring Filtrate Volume of a Starch in Saturated Salt Suspension 65

    8. Calculation-Filtrate Volume of a Starch in Saturated Salt Suspension 65

    9. Apparatus-Measuring Starch Residue Greater than 2000 µm 65

    10. 0Procedure-Measuring Starch Residue Greater than 2000 µm 65

16. Low-viscosity Polyanionic Cellulose (PAC-LV) 66

    1. Principle 66

    2. Qualitative Determination of Starch or Starch Derivatives in a PAC-LV Sample 66

    3. Measuring Moisture Mass Fraction of a PAC-LV Sample 68

    4. Reagents and Apparatus-Measuring Apparent Viscosity of a PAC-LV Sea Salt Solution 69

    5. Procedure-Measuring Apparent Viscosity of a PAC-LV Sea Salt Solution 69

    6. Calculation-Apparent Viscosity of a PAC-LV Sea Salt Solution 70

    7. Reagents and Apparatus-Measuring Filtrate Volume of a PAC-LV Suspension 70

    8. Procedure-Measuring Filtrate Volume of a PAC-LV Suspension 71

    9. Calculation-Filtrate Volume of PAC-LV Suspension 72

17. High-viscosity Polyanionic Cellulose (PAC-HV) 72

    1. Principle 72

    2. Qualitative Determination of Starch or Starch Derivatives in PAC-HV Sample 73

    3. Measuring Moisture Mass Fraction of a PAC-HV Sample 75

    4. Reagents and Apparatus-Measuring Apparent Viscosity of a PAC-HV Sea Salt Solution 75

       
       

    5. Procedure-Measuring Apparent Viscosity of a PAC-HV Sea Salt Solution 76

    6. Calculation-Apparent Viscosity of a PAC-HV Sea Salt Solution 77

    7. Reagents and Apparatus-Measuring Filtrate Volume of a PAC-HV Suspension 77

    8. Procedure-Measuring the Filtrate Volume of a PAC-HV Suspension 78

    9. Calculation-Filtrate Volume of PAC-HV Suspension 79

18. Drilling-grade Xanthan Gum 79

    1. Principle 79

    2. Qualitative Determination of Starch or Starch Derivatives in a Xanthan Gum Sample 80

    3. Qualitative Determination of Guar in a Xanthan Gum Sample 82

    4. Measuring Moisture Mass Fraction of a Xanthan Gum Sample 84

    5. Measuring Particle Size of a Xanthan Gum Sample. 85

    6. Reagents and Apparatus-Measuring the Viscosity of a Xanthan Gum Solution 87

    7. Procedure-Preparation of the Synthetic Seawater. 87

    8. Procedure-Preparation of the Xanthan Gum Polymer Solution 88

    9. Procedure-Measuring the Viscosity of a Xanthan Gum Solution 88

    10. Measuring Low-shear-rate Viscosity of a Xanthan Gum Solution 88

    11. Calibration of Direct-indicating Viscometer (R1-B1 Geometry, F0.2 Spring) 89

19. OCMA-grade Bentonite 90

    1. Principle 90

    2. Reagents and Apparatus-Measuring Properties of an OCMA-grade Bentonite Suspension 91

    3. Procedure-Measuring Rheological Properties of an OCMA-grade Bentonite Suspension 91

    4. Calculation-Rheological Properties of an OCMA-grade Bentonite Suspension 92

    5. Procedure-Measuring the Filtrate Volume of an OCMA-grade Bentonite Suspension 92

    6. Calculation-Filtrate Volume of an OCMA-grade Bentonite Suspension 92

    7. Reagents and Apparatus-Measuring OCMA-grade Bentonite Residue of Greater than 75 µm 93

    8. Procedure-Measuring OCMA-grade Bentonite Residue of Greater than 75 µm 93

    9. Calculation-OCMA-grade Bentonite Residue of Greater than 75 µm 94

Annex A (informative) API Monogram Program Use of the APi Monogram by Licensees 95

Annex B (informative) Test Precision 99

Annex C (informative) Examples of Calculations 104

Annex D (informative) API Reference Material Program 109

Biblography 112

Tables

1. Dial Reading Tolerances with Various Calibration Fluids, F-1 Spring (or Equivalent)

   in Motor-driven, Direct-indicating Viscometer 10

2. Barite Physical and Chemical Requirements 16

3. Viscosity of Water at Various Temperatures 25

4. Values of Effective Depth Based on Readings on Hydrometer ASTM 151H

   Used in Specific Sedimentation Cylinder 26

5. Sample Constant, Ks, for Barite (80.0 g Sample) 27

6. Hematite Chemical and Physical Specifications 27

7. Sample Constant, Ks, for Hematite (80.0 g Sample). 36

8. Bentonite Physical Specifications 37

9. Non-treated Bentonite Physical Specifications 41

   
   

10. Attapulgite Physical Specifications 44

11. Sepiolite Physical Specifications 47

12. CMC-LVT Physical Specifications 51

13. CMC-HVT Physical Specifications 56

14. Starch Physical Specifications 62

15. PAC-LV Physical Requirements 66

16. PAC-HV Physical Requirements 73

17. Xanthan Gum Physical Requirements 80

18. OCMA-grade Bentonite Physical Specifications 90

1. Test Precision for Barite 100

2. Test Precision for Hematite 100

3. Test Precision for Bentonite 101

4. Test Precision for Non-treated Bentonite 101

5. Test Precision for OCMA-grade Bentonite 101

6. Test Precision for Reference (Calibration) Bentonite 101

7. Test Precision for Attapulgite 102

8. Test Precision for Sepiolite 102

9. Test Precision for CMC-LVT 102

10. Test Precision for CMC-HVT 103

11. Test Precision Starch 103

1. Example Hydrometer Calibration Sheet 104

2. Example Hydrometer Datasheet (Barite) 105

3. Example Hydrometer Datasheet (Hematite) 107

1. Product Specification for SEBC 110

2. Typical Chemical Analysis for SEBC 110

3. Typical Particle Analysis for SEBC 111

4. SEBC Mineralogy from X-ray Diffraction 111

This Standard covers materials that are in common usage in petroleum and natural-gas drilling fluids. These materials are used in bulk quantities, can be purchased from multiple sources and are available as commodity products. No single-source or limited-source products are included, nor are specialty products.

Standards are published to facilitate communication between purchasers and manufacturers, to provide interchangeability between similar equipment and materials purchased from different manufacturers and/or at different times and to provide an adequate level of safety when the equipment or materials are utilized in the manner and for the purposes intended. This Standard provides minimum requirements and is not intended to inhibit anyone from purchasing or producing materials to other standards.

The purpose of this Standard is to provide product specifications for materials manufactured for use in oil- and gas- well drilling fluids. The materials covered are barite, hematite, bentonite, non-treated bentonite, Oil Companies Material Association (OCMA)-grade bentonite, attapulgite, sepiolite, technical grade low-viscosity carboxymethyl cellulose (CMC-LVT), technical grade high-viscosity carboxymethyl cellulose (CMC-HVT), starch, low-viscosity polyanionic cellulose (PAC-LV), high-viscosity polyanionic cellulose (PAC-HV), and drilling-grade xanthan gum.

A survey of the industry found that only the American Petroleum Institute (API) issued testing procedures and specification standards for these materials.

Annex A (informative) discusses the use of the API Monogram by Licensees, Annex B provides the test precision, Annex C (informative) details examples of calculations, and Annex D discusses the API Reference Material Program.

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

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 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, First edition, June 2017 (Editorial Revision, November 2017). This numbering format is different than that used in API 13A 18th 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).

Drilling Fluids Materials

1. Scope

   
   

   This specification covers physical properties and test procedures for materials manufactured for use in oil- and gas-well drilling fluids. The materials covered are barite; hematite; bentonite; non-treated bentonite; OCMA-grade bentonite; attapulgite; sepiolite; technical grade, low-viscosity carboxymethyl cellulose (CMC-LVT); technical grade, high-viscosity carboxymethyl cellulose (CMC-HVT); starch; low-viscosity polyanionic cellulose (PAC-LV); high-viscosity polyanionic cellulose (PAC-HV); and drilling-grade xanthan gum. This specification is intended for the use of manufacturers, distributors, and end users of named products. Annex A (informative) contains information on the API Monogram Program and requirements for the approved use of the API Monogram by licensees.

   
   

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

   
   

   ASTM D422-63 1, Standard Test Method for Particle-size Analysis of Soils

   
   

   ASTM E11, Standard Specification for Woven Wire Test Sieve Cloth and Test Sieves ASTM E77, Standard Test Method for Inspection and Verification of Thermometers ASTM E161, Standard Specification for Electroformed Material and Test Sieves

   ASTM E617, Standard Specification for Laboratory Weights and Precision Mass Standards ISO 386 2, Liquid-in glass laboratory thermometersPrinciples of design, construction and use NIST National Bureau of Standards Monograph 150 3, Liquid-In-Glass Thermometry

3. Terms, Definitions, Symbols, and Abbreviations

3.1 Terms and Definitions

For the purposes of this document, the following terms and definitions apply.

3.1.1

ACS reagent grade

Chemicals that meet purity standards as specified by the ACS 4.

3.1.2

flash side

Side containing residue (“flash”) from stamping, or the side with concave indentation.

1 ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428, www.astm.org.

2 International Organization for Standardization, Chemin de Blandonnet, 8, CP401, 1214 Vernier Geneve, Switzerland, www.iso.org.

3 National Institute of Standards and Technology, 100 Bureau Drive, Stop 3460, Gaithersburg, MD 20899, www.nist.gov.

4 American Chemical Society, 1155 Sixteenth Street NW, Washington, DC 20036, www.acs.org.

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