Recommended Practice for Chemical Analysis of Barite

API RECOMMENDED PRACTICE 13K THIRD EDITION, MAY 2011

REAFFIRMED, MAY 2016

Recommended Practice for Chemical Analysis of Barite

Upstream Segment

API RECOMMENDED PRACTICE 13K THIRD EDITION, MAY 2011

REAFFIRMED, MAY 2016

Special Notes

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Copyright © 2011 American Petroleum Institute

Foreword

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iii

Important Information Concerning Use of Asbestos or Alternative Materials

Asbestos is specified or referenced for certain components of the equipment described in some API standards. It has been of extreme usefulness in minimizing fire hazards associated with petroleum processing. It has also been a universal sealing material, compatible with most refining fluid services.

Certain serious adverse health effects are associated with asbestos, among them the serious and often fatal diseases of lung cancer, asbestosis, and mesothelioma (a cancer of the chest and abdominal linings). The degree of exposure to asbestos varies with the product and the work practices involved.

Consult the most recent edition of the Occupational Safety and Health Administration (OSHA), U.S. Department of Labor, Occupational Safety and Health Standards for Asbestos, Tremolite, Anthophyllite, and Actinolite, 29 Code of Federal Regulations Section 1910.1001; the U.S. Environmental Protection Agency, National Emission Standard for Asbestos, 40 Code of Federal Regulations Section 61.140 through 61.156; and the U.S. Environmental Protection Agency (EPA) rule on labelling requirements and phased banning of asbestos products (Sections 763.160-170).

There are currently in use and under development a number of substitute materials to replace asbestos in certain applications. Manufacturers and users are encouraged to develop and use effective substitute materials that can meet the specifications, for and operating requirement of, the equipment to which they would apply.

SAFETY AND HEALTH INFORMATION WITH RESPECT TO PARTICULAR PRODUCTS OR MATERIALS CAN BE OBTAINED FROM THE EMPLOYER, THE MANUFACTURER OR SUPPIER OF THAT PRODUCT OR MATERIAL, OR THE MATERIAL SAFETY DATA SHEET.

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Contents Page

Important Information Concerning Use of Asbestos or Alternative Materials iv

1. Scope 1

2. Normative References 1

3. Terms and Definitions 2

4. Acronyms, Abbreviations, and Symbols 3

5. Wet Analysis Methods 5

   1. Principle 5

   2. Advantages of Wet Chemical Analysis Methods 5

   3. Summary of General Analytical Methods 6

6. Barium Sulfate and Strontium Sulfate 6

   1. Principle 6

   2. Reagents and Materials 6

   3. Apparatus 7

   4. Sampling 8

   5. Procedure—Barium Sulfate Determination 8

   6. Procedure—Strontium Sulfate Determination 9

   7. Calculation 9

7. Silica and Alumina 11

   1. Principle 11

   2. Reagents and Materials 11

   3. Apparatus 12

   4. Procedure—Sample Preparation 13

   5. Procedure—Silica Determination. 13

   6. Procedure—Alumina Determination 14

   7. Calculation 14

8. Hydrochloric Acid Soluble Metals—Sodium, Potassium, Calcium, Magnesium, Iron, Copper, Manganese, Lead and Zinc 15

   1. Principle 15

   2. Reagents and Materials 15

   3. Apparatus 15

   4. Procedure 15

   5. Calculation 16

9. Procedure—Hydrofluoric, Sulphuric, Nitric, Perchloric Acid Soluble Metals—Sodium, Potassium, Calcium, Magnesium, Iron, Copper, Manganese, Lead, and Zinc 16

   1. Principle 16

   2. Reagents and Materials 16

   3. Apparatus 17

   4. Procedure 17

   5. Calculation 18

10. Alternative Methods for Iron 18

    1. Principle 18

    2. Reagents and Materials 19

    3. Apparatus 19

    4. Procedure—Nitric Acid Digestion 20

    5. Calculation—Nitric Acid Digestion 20

    6. Procedure—Aqua Regia Digestion 20

       v

    7. Calculation—Aqua Regia Digestion 21

    8. Procedure—Carbonate Fusion 21

    9. Calculation—Carbonate Fusion 21

11. Water-soluble Materials in Barite 22

    1. Principle 22

    2. Apparatus 22

    3. Procedure 22

    4. Calculation 23

12. Water-soluble Chlorides 23

    1. Principle 23

    2. Reagents and Materials 23

    3. Apparatus 24

    4. Procedure—Water-soluble Chlorides by Titration 24

    5. Calculation—Water-soluble Chlorides by Titration 24

    6. Procedure—Water-soluble Chlorides by Ion Chromatography 24

    7. Calculation—Water-soluble Chlorides by Ion Chromatography 25

13. Water-soluble Sulfates 25

    1. Principle 25

    2. Reagents and Materials 25

    3. Apparatus 25

    4. Procedure—Preparation of Calibration Curve for Turbidity Method 26

    5. Procedure—Analysis for Water-soluble Sulfates by Turbidity Method 26

    6. Calculation—Water-soluble Sulfates by Turbidity Method 26

    7. Procedure—Analysis for Water-soluble Sulfate by Ion Chromatography 27

    8. Calculation—Water-soluble Sulfates by Ion Chromatography 27

14. Water-soluble Carbonates, Bicarbonates, and Hydroxyl Ions 27

    1. Principle 27

    2. Reagents and Materials 27

    3. Apparatus 27

    4. Procedure 27

    5. Calculation 28

15. Water-soluble Phosphates 29

    1. Principle 29

    2. Reagents and Materials 29

    3. Apparatus 29

    4. Procedure—Preparation of Calibration Curve 30

    5. Procedure—Analysis of Samples 30

    6. Calculation 30

16. Loss on Ignition 31

    1. Principle 31

    2. Reagents and Materials, and Apparatus 31

    3. Procedure 31

    4. Calculation 31

17. Siderite Content 32

    1. Principle 32

    2. Reagents and Materials 32

    3. Apparatus 32

    4. Procedure—Extraction 33

    5. Procedure—Iron Content by Atomic Absorption or Inductively Coupled Plasma 33

    6. Calculation—Extraction 33

    7. Procedure—Iron Content by Colorimetric Determination 33

    8. Calculation—Iron Content by Colorimetric Determination 34

       vi

18. Zinc Carbonate and Lead Carbonate 34

    1. Principle 34

    2. Reagents and Materials, and Apparatus 34

    3. Procedure—Extraction 35

    4. Procedure—Lead and Zinc Determination by Atomic Absorption or Inductively Coupled Plasma 35

    5. Calculation 35

19. Total Carbonate 35

    1. Principle 35

    2. Reagents and Materials 36

    3. Apparatus 36

    4. Procedure 37

    5. Calculation 38

20. Acid-soluble Sulfides 38

    1. Principle 38

    2. Reagents and Materials 39

    3. Apparatus 39

    4. Procedure 40

    5. Calculation 41

21. Calcium Hydroxide (Lime) or Cement 41

    1. Principle 41

    2. Reagents and Materials 41

    3. Apparatus 42

    4. Procedure 42

    5. Calculation 42

22. X-ray Fluorescence Analysis 43

    1. Principle 43

    2. Reagents and Materials 44

    3. Apparatus 44

    4. Procedure—Sample Preparation 45

    5. Procedure—Spectral Analysis 47

    6. Calculation 47

23. Heavy Metals in Barite 47

Annex A (informative) Rational Analysis 48

Annex B (informative) Metric “SI” Unit Conversion Table 50

Figures

1 Correction Curve for SrSO4 in BaSO4 11

Tables

1. Minerals Associated With Barite Ore Bodies 2

2. Dräger Tube Identification, Sample Volume, and Tube Factor

to be Used for Various Sulfide Ranges 40

vii

Recommended Practice for Chemical Analysis of Barite

1. Scope

   
   

   1. Barite is used to increase the density of oil well drilling fluids. It is a mined product that can contain significant quantities of minerals other than barium sulfate, which is its main component.

      
      

   2. A list of some minerals commonly associated with barite ores is given in Table 1 with the chemical formulas, mineralogical names, and the densities of the mineral grains.

      
      

   3. The performance of barite in a drilling fluid is related in part to the percentage and type of non-barite minerals distributed in the barite ore. Some of these minerals have little or no effect on drilling fluid properties, but others can degrade these properties and even be harmful to rig personnel.

      
      

   4. It is the objective of this publication to provide a comprehensive, detailed description of the chemical analytical procedures for quantitatively determining the mineral and chemical constituents of barite. These procedures are quite elaborate and will normally be carried out in a well-equipped laboratory.

      
      

2. Normative References

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

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

API Recommended Practice 13I-2009, Recommended Practice for Laboratory Testing of Drilling Fluids

API Manual of Petroleum Measurement Standards (MPMS), Chapter 15, Guidelines for Use of the International System of Units (SI) in the Petroleum and Allied Industries

ISO 10416:2008 1, Petroleum and natural gas industries—Drilling fluids—Laboratory testing

U.S. 29 Code of Federal Regulations (CFR) 2, Section 1910.1001

U.S. 40 Code of Federal Regulations (CFR), Section 61.140 through Section 61.156

U.S. 51 Federal Register (FR), 3738-3759 (January 29, 1986)

1

International Organization for Standardization, 1, ch. de la Voie-Creuse, Case postale 56, CH-1211, Geneva 20,

Switzerland, www.iso.org.

2

The Code of Federal Regulations and Federal Register are available from the U.S. Government Printing Office, Washington,

DC 20402.

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