ADDENDUM 1. Page 4, g, add the following

Transcription

1 Date of Issue: January, 2005 Affected Publication: API Specification 10A/ISO , Specification for Cements and Materials for Well Cementing, Twenty-third Edition ADDENDUM 1 Page 4, g, add the following For the period beginning January 17, 2005 and ending January 1, 2010, other than calcium sulfate or water, or both, only chemical additives as required for Chromium VI reduction may be interground or blended with the clinker during the manufacture of Class G well cement. Such additions shall not prevent the well cements from performing its intended purpose. Cement manufactured containing agents to control Chromium VI shall be supplied with information containing a generic chemical description of the reducing agent(s) contained in the cement and the date of the addition of the reducing agent(s) into the cement. Page 5, h, add the following For the period beginning January 17, 2005 and ending January 1, 2010, other than calcium sulfate or water, or both, only chemical additives as required for Chromium VI reduction may be interground or blended with the clinker during the manufacture of Class H well cement. Such additions shall not prevent the well cements from performing its intended purpose. Cement manufactured containing agents to control Chromium VI shall be supplied with information containing a generic chemical description of the reducing agent(s) contained in the cement and the date of the addition of the reducing agent(s) into the cement.

2 Specification for Cements and Materials for Well Cementing API Specification 10A Twenty-third Edition, April 2002 ANSI/API 10A/ISO Effective Date: October 1, 2002 ISO :2000 Petroleum and natural gas industries Cements and materials for well cementing Part 1: Specification

3

4 American Petroleum Institute API Specification 10A/ISO :2000 SPECIAL NOTES API publications necessarily address problems of a general nature. With respect to particular circumstances, local, state, and federal laws and regulations should be reviewed. API is not undertaking to meet the duties of employers, manufacturers, or suppliers to warn and properly train and equip their employees, and others exposed, concerning health and safety risks and precautions, nor undertaking their obligations under local, state, or federal laws. Information concerning safety and health risks and proper precautions with respect to particular materials and conditions should be obtained from the employer, the manufacturer or supplier of that material, or the material safety data sheet. 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. Generally, API standards are reviewed and revised, reaffirmed, or withdrawn at least every five years. Sometimes a one-time extension of up to two years will be added to this review cycle. This publication will no longer be in effect five years after its publication date as an operative API standard or, where an extension has been granted, upon republication. Status of the publication can be ascertained from the API Upstream Segment, telephone (202) A catalog of API publications and materials is published annually and updated quarterly by API, 1220 L Street, N.W., Washington, D.C This document was produced under API standardization procedures that ensure appropriate notification and participation in the developmental process and is designated as an API standard. Questions concerning the interpretation of the content of this standard or comments and questions concerning the procedures under which this standard was developed should be directed in writing to the director/general manager of the Upstream Segment, American Petroleum Institute, 1220 L Street, N.W., Washington, D.C Requests for permission to reproduce or translate all or any part of the material published herein should also be addressed to the director. API standards are published to facilitate the broad availability of proven, sound engineering and operating practices. These standards are not intended to obviate the need for applying sound engineering judgment regarding when and where these standards should be utilized. The formulation and publication of API standards is not intended in any way to inhibit anyone from using any other practices. Any manufacturer marking equipment or materials in conformance with the marking requirements of an API standard is solely responsible for complying with all the applicable requirements of that standard. API does not represent, warrant, or guarantee that such products do in fact conform to the applicable API standard. These materials are subject to copyright claims of ISO, ANSI and API. All rights reserved. No part of this work may be reproduced, stored in a retrieval system, or transmitted by any means, electronic, mechanical, photocopying, recording, or otherwise, without prior written permission from the publisher. Contact the Publisher, API Publishing Services, 1220 L Street, N.W., Washington, D.C Copyright 2002 American Petroleum Institute i

5 API Specification 10A/ISO :2000 American Petroleum Institute API FOREWORD This standard is under the jurisdiction of the API Standards Subcommittee on Well Cements. This API standard is identical with the English version of ISO ISO was prepared by Technical Committee ISO/TC 67, Materials, equipment and offshore structures for petroleum and natural gas industries, SC 3, Drilling and completion fluids, and well cements. For the purposes of this standard, the following editorial changes have been made: See Annex C Ð National Adoption Editorial Changes This standard shall become effective on the date printed on the cover but may be used voluntarily from the date of distribution. API publications may be used by anyone desiring to do so. Every effort has been made by the Institute to assure the accuracy and reliability of the data contained in them; however, the Institute makes no representation, warranty, or guarantee in connection with this publication and hereby expressly disclaims any liability or responsibility for loss or damage resulting from its use or for the violation of any federal, state, or municipal regulation with which this publication may conflict. Suggested revisions are invited and should be submitted to the Upstream Segment, API, 1220 L Street, NW, Washington, DC ii

6 American Petroleum Institute API Specification 10A/ISO :2000 ISO 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 3. 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 standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISOÊ was prepared by Technical Committee ISO/TCÊ67, Materials, equipment and offshore structures for petroleum and natural gas industries, Subcommittee SCÊ3, Drilling and completion fluids, and well cements. ISOÊ10426 consists of the following parts, under the general title Petroleum and natural gas industriesêñ Cements and materials for well cementing: Part 1: Specification Part 2: Recommended practice for testing of well cement Annex A of this standard is for information only. iii

7 API Specification 10A/ISO :2000 American Petroleum Institute Introduction This standard is based on API Specification 10A, Twenty-second Edition/ISO :2000. Users of this standard should be aware that further or differing requirements may 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 the individual application. This may be particularly applicable where there is innovative or developing technology. Where an alternative is offered, the vendor should identify any variations from this standard and provide details. In this standard, where practical, U.S. Customary units are included in brackets for information. iv

8 American Petroleum Institute API Specification 10A/ISO :2000 Contents Page 1 Scope Normative references Terms and definitions Requirements Specification, chemical and physical requirements Sampling frequency, timing of tests and equipment Sampling procedure Fineness tests Procedure Requirements Preparation of slurry for free fluid, compressive strength and thickening time tests Apparatus Procedure Free-fluid test (free water) Apparatus Calibration Procedure Calculation of percent free fluid Acceptance requirements Compressive strength tests Apparatus Procedure Test procedure (derived from ASTM C 109) Compressive strength acceptance criteria Thickening-time tests Apparatus Calibration Procedure Thickening time and consistency Specification acceptance requirements Marking Packing Bentonite Annex A (informative) Calibration procedures for thermocouples, temperature-measuring systems and controllers Annex B (informative) API Monogram Annex C (informative) National Adoption Editorial Changes Bibliography v

9 API Specification 10A/ISO :2000 American Petroleum Institute vi

10 American Petroleum Institute Petroleum and natural gas industriesêñ Cements and materials for well cementingêñ PartÊ1: Specification 1 Scope This standard specifies requirements and gives recommendations for eight classes of well cements, including their chemical and physical requirements and procedures for physical testing. This standard is applicable to well cement Classes A, B, C, D, E and F, which are the products obtained by grinding Portland cement clinker and, if needed, calcium sulfate as an interground additive. Processing additives may be used in the manufacture of cement of these classes. Suitable set-modifying agents may be interground or blended during manufacture of Classes D, E and F. This standard is also applicable to well cement Classes G and H, which are the products obtained by grinding Portland cement clinker with no additives other than calcium sulfate or water. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this part of ISOÊ For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this part of ISOÊ10426 are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. API Specification 13A, Drilling Fluid Materials. ISO , Test sievesêñ Technical requirements and testingêñ Part 1: Test sieves of metal wire cloth. ASTM C 109/C 109M, Standard test method for compressive strength of hydraulic cement mortars (using 2-in or [50- mm] cube specimens). ASTM C 114, Standard test methods for chemical analysis of hydraulic cement. ASTM C 115, Standard test methods for fineness of Portland cement by the turbidimeter. ASTM C 183, Standard practice for sampling and the amount of testing of hydraulic cement. ASTM C 204, Standard test method for fineness of Portland cement by air permeability apparatus. ASTM C 465, Standard specification for processing additions for use in the manufacture of hydraulic cements. ASTM E 220, Standard test method for calibration of thermocouples by comparison techniques. ASTM E 1404, Standard specification for laboratory class conical flasks. 1

11 API Specification 10A/ISO :2000 American Petroleum Institute DIN 12385, Laboratory glassware, conical flasks, wide neck. EN 196-2, Methods of testing cementêñ Part 2: Chemical analysis of cement. EN 196-6, Methods of testing cementêñ Part 6: Determination of fineness. EN 196-7, Methods of testing cementêñ Part 7: Methods of taking and preparing samples of cement. EN , Methods of testing cementêñ Part 21: Determination of the chloride, carbon dioxide and alkali content of cement. 3 Terms and definitions For the purposes of this part of ISOÊ10426, the following terms and definitions apply. 3.1 additive material added to a cement slurry to modify or enhance some desired property NOTE Properties that are commonly modified include: setting time (by use of retarders or accelerators), fluid loss, viscosity, etc. 3.2 Bearden unit of consistency B c measure of the consistency of a cement slurry when determined on a pressurized consistometer 3.3 bulk density mass per unit volume of a dry material containing entrained air 3.4 cement Portland cement ground clinker generally consisting of hydraulic calcium silicates and aluminates and usually containing one or more forms of calcium sulfate as an interground additive 3.5 cement class designation by API to denote the various classifications of API cement according to its intended use 3.6 cement grade designation by API to denote the sulfate resistance of a particular cement 3.7 cement blend mixture of dry cement and other dry materials 3.8 clinker fused materials from the kiln in cement manufacturing that are interground with calcium sulfate to make cement 3.9 compressive strength force per unit area required to crush a set cement sample 2

12 American Petroleum Institute API Specification 10A/ISO : consistometer device used to measure the thickening time of a cement slurry under temperature and pressure 3.11 filtrate liquid that is forced out of a cement slurry during a fluid loss test 3.12 free fluid colored or colorless liquid which has separated from a cement slurry 3.13 neat cement slurry cement slurry consisting of only cement and water 3.14 pressure vessel vessel in a consistometer into which the slurry container is placed for the thickening time test 3.15 slurry container slurry cup container in a pressurized consistometer used to hold the slurry for conditioning purposes or for the thickening time test 3.16 thickening time time for a cement slurry to develop a selected B c NOTE The results of a thickening time test provide an indication of the length of time a cement slurry will remain pumpable under the test conditions. 4 Requirements 4.1 Specification, chemical and physical requirements Classes and grades Well cement shall be specified using the following Classes (A, B, C, D, E, F, G and H) and Grades (O, MSR and HSR). A processing additive or set-modifying agent shall not prevent a well cement from performing its intended functions. a) Class A The product obtained by grinding Portland cement clinker, consisting essentially of hydraulic calcium silicates, usually containing one or more forms of calcium sulfate as an interground additive. At the option of the manufacturer, processing additives may be used in the manufacture of Class A cement, provided such materials in the amounts used have been shown to meet the requirements of ASTM C 465. This product is intended for use when special properties are not required. Available only in ordinary (O) Grade (similar to ASTM C 150, Type I). b) Class B The product obtained by grinding Portland cement clinker, consisting essentially of hydraulic calcium silicates, usually containing one or more forms of calcium sulfate as an interground additive. At the option of the 3

13 API Specification 10A/ISO :2000 American Petroleum Institute manufacturer, processing additives may be used in the manufacture of Class B cement, provided such materials in the amounts used have been shown to meet the requirements of ASTM C 465. This product is intended for use when conditions require moderate or high sulfate-resistance. Available in both moderate sulfate-resistant (MSR) and high sulfate-resistant (HSR) Grades (similar to ASTM C 150, Type II). c) Class C The product obtained by grinding Portland cement clinker, consisting essentially of hydraulic calcium silicates, usually containing one or more forms of calcium sulfate as an interground additive. At the option of the manufacturer, processing additives may be used in the manufacture of Class C cement, provided such materials in the amounts used have been shown to meet the requirements of ASTM C 465. This product is intended for use when conditions require high early strength. Available in ordinary (O), moderate sulfate-resistant (MSR) and high sulfate-resistant (HSR) Grades (similar to ASTM C 150, Type III). d) Class D The product obtained by grinding Portland cement clinker, consisting essentially of hydraulic calcium silicates, usually containing one or more forms of calcium sulfate as an interground additive. At the option of the manufacturer, processing additives may be used in the manufacture of Class D cement, provided such materials in the amounts used have been shown to meet the requirements of ASTM C 465. Further, at the option of the manufacturer, suitable set-modifying agents may be interground or blended during manufacture. This product is intended for use under conditions of moderately high temperatures and pressures. Available in moderate sulfate-resistant (MSR) and high sulfate-resistant (HSR) Grades. e) Class E The product obtained by grinding Portland cement clinker, consisting essentially of hydraulic calcium silicates, usually containing one or more forms of calcium sulfate as an interground additive. At the option of the manufacturer, processing additives may be used in the manufacture of Class E cement, provided such materials in the amounts used have been shown to meet the requirements of ASTM C 465. Further, at the option of the manufacturer, suitable set-modifying agents may be interground or blended during manufacture. This product is intended for use under conditions of high temperatures and pressures. Available in moderate sulfate-resistant (MSR) and high sulfate-resistant (HSR) Grades. f) Class F The product obtained by grinding Portland cement clinker, consisting essentially of hydraulic calcium silicates, usually containing one or more forms of calcium sulfate as an interground additive. At the option of the manufacturer, processing additives may be used in the manufacture of Class F cement, provided such materials in the amounts used have been shown to meet the requirements of ASTM C 465. Further, at the option of the manufacturer, suitable set-modifying agents may be interground or blended during manufacture. This product is intended for use under conditions of extremely high temperatures and pressures. Available in moderate sulfate-resistant (MSR) and high sulfate-resistant (HSR) Grades. g) Class G The product obtained by grinding Portland cement clinker, consisting essentially of hydraulic calcium silicates, usually containing one or more forms of calcium sulfate as an interground additive. No additives other than calcium sulfate or water, or both, shall be interground or blended with the clinker during manufacture of ClassÊG well cement. This product is intended for use as a basic well cement. Available in moderate sulfate-resistant (MSR) and high sulfate-resistant (HSR) Grades. 4

14 American Petroleum Institute API Specification 10A/ISO :2000 h) Class H The product obtained by grinding Portland cement clinker, consisting essentially of hydraulic calcium silicates, usually containing one or more forms of calcium sulfate as an interground additive. No additives other than calcium sulfate or water, or both, shall be interground or blended with the clinker during manufacture of ClassÊH well cement. This product is intended for use as a basic well cement. Available in moderate sulfate-resistant (MSR) and high sulfate-resistant (HSR) Grades. A well cement which has been manufactured and supplied in accordance with this standard may be mixed and placed in the field using water ratios or additives at the userõs discretion. It is not intended that manufacturing compliance with this standard be based on such field conditions Chemical requirements Well cements shall conform to the respective chemical requirements of classes and grades referenced in TableÊ1. Chemical analyses of hydraulic cements shall be carried out as specified in ASTM C 114 (or ENÊ196-2, ENÊ196-21) Physical and performance requirements Well cement shall conform to the respective physical and performance requirements referenced in Table 2 and specified in clauses 6, 7, 8, 9 and 10. 5

15 API Specification 10A/ISO :2000 American Petroleum Institute TableÊ1ÊÑÊChemical requirements Cement Class A B C D, E, F G H ORDINARY GRADE (O) Magnesium oxide (MgO), maximum, % 6,0 NA 6,0 NA NA NA Sulfur trioxide (SO 3 ), maximum, % 3,5 a NA 4,5 NA NA NA Loss on ignition, maximum, % 3,0 NA 3,0 NA NA NA Insoluble residue, maximum, % 0,75 NA 0,75 NA NA NA Tricalcium aluminate (C 3 A), maximum, % NR NA 15 NA NA NA MODERATE SULFATE-RESISTANT GRADE (MSR) Magnesium oxide (MgO), maximum, % NA 6,0 6,0 6,0 6,0 6,0 Sulfur trioxide (SO 3 ), maximum, % NA 3,0 3,5 3,0 3,0 3,0 Loss on ignition, maximum, % NA 3,0 3,0 3,0 3,0 3,0 Insoluble residue, maximum, % NA 0,75 0,75 0,75 0,75 0,75 Tricalcium silicate (C 3 S) maximum, % NA NR NR NR 58 b 58 b minimum, % NA NR NR NR 48 b 48 b Tricalcium aluminate (C 3 A), maximum % (3) NA Total alkali content, expressed as sodium oxide (Na 2 O) equivalent, maximum, % NA NR NR NR 0,75 c 0,75 c HIGH SULFATE-RESISTANT GRADE (HSR) Magnesium oxide (MgO), maximum, % NA 6,0 6,0 6,0 6,0 6,0 Sulfur trioxide (SO 3 ), maximum, % NA 3,0 3,5 3,0 3,0 3,0 Loss on ignition, maximum, % NA 3,0 3,0 3,0 3,0 3,0 Insoluble residue, maximum, % NA 0,75 0,75 0,75 0,75 0,75 Tricalcium silicate (C 3 S) maximum, % NA NR NR NR 65 b 65 b minimum, % NA NR NR NR 48 b 48 b Tricalcium aluminate (C 3 A), maximum, % NA 3 b 3 b 3 b 3 b 3 b Tetracalcium aluminoferrite (C 4 AF) plus twice the tricalcium aluminate (C 3 A), maximum, % Total alkali content expressed as sodium oxide (Na 2 O) equivalent, maximum, % NA 24 b 24 b 24 b 24 b 24 b NA NR NR NR 0,75 c 0,75 c NR = No Requirement; NA = Not Applicable a When the tricalcium aluminate content (expressed as C 3 A) of the cement is 8Ê% or less, the maximum SO 3 content shall be 3Ê%. b The expressing of chemical limitations by means of calculated assumed compounds does not necessarily mean that the oxides are actually or entirely present as such compounds. When the ratio of the percentages of Al 2 O 3 to Fe 2 O 3 is 0,64 or less, the C 3 A content is zero. When the Al 2 O 3 to Fe 2 O 3 ratio is greater than 0,64, the compounds shall be calculated as follows: C 3 A = (2,65 x % Al 2 O 3 ) Ð (1,69 x % Fe 2 O 3 ) C 4 AF = 3,04 x % Fe 2 O 3 C 3 S = (4,07 x % CaO) Ð (7,60 x % SiO 2 ) Ð (6,72 x % Al 2 O 3 ) Ð (1,43 x % Fe 2 O 3 ) Ð (2,85 x % SO 3 ) When the ratio of Al 2 O 3 to Fe 2 O 3 is less than 0,64, the C 3 S shall be calculated as follows: C 3 S = (4,07 x % CaO) Ð (7,60 x % SiO 2 ) Ð (4,48 x % Al 2 O 3 ) Ð (2,86 x % Fe 2 O 3 ) Ð (2,85 x % SO 3 ) c The sodium oxide equivalent (expressed as Na2O equivalent) shall be calculated by the formula: Na 2 O equivalent = (0,658 x % K 2 O) + (% Na 2 O) 6

16 American Petroleum Institute API Specification 10A/ISO :2000 TableÊ2ÊÑÊSummary of physical and performance requirements Well cement Class A B C D E F G H Mix water, % mass fraction of cement (Table 5) Fineness tests (alternative methods) (clause 6) Turbidimeter (specified surface, minimum m 2 /kg) NR NR NR NR NR Air permeability (specified surface, minimum m 2 /kg) NR NR NR NR NR Free fluid content, maximum % (clause 8) NR NR NR NR NR NR 5,9 5,9 Compressive strength test (8-h curing time) (clause 9) Schedule number, Table 6 Final curing temp. C ( F) Final curing pressure MPa (psi) Minimum compressive strength MPa (psi) NA 38 (100) atm. 1,7 (250) 1,4 (200) 2,1 (300) NR NR NR 2,1 (300) 2,1 (300) NA 60 (140) atm. NR NR NR NR NR NR 10,3 (1 500) 10,3 (1 500) 6S 110 (230) 20,7 (3 000) NR NR NR 3,4 (500) NR NR NR NR 8S 143 (290) 20,7 (3 000) NR NR NR NR 3,4 (500) NR NR NR Compressive strength test (24-h curing time) (clause 9) Schedule number, Table 6 9S 160 (320) 20,7 (3 000) NR NR NR NR NR 3,4 (500) Final curing temp. C ( F) Final curing pressure MPa (psi) Minimum compressive strength MPa (psi) NR NR NA 38 (100) Atm. 12,4 (1 800) 10,3 (1 500) 13,8 (2 000) NR NR NR NR NR 4S 77 (170) 20,7 (3 000) NR NR NR 6,9 (1 000) 6,9 (1 000) NR NR NR 6S 110 (230) 20,7 (3 000) NR NR NR 13,8 (2 000) NR 6,9 (1 000) NR NR 8S 143 (290) 20,7 (3 000) NR NR NR NR 13,8 (2 000) NR NR NR 9S 160 (320) 20,7 (3 000) NR NR NR NR NR 6,9 (1 000) NR NR 7

17 API Specification 10A/ISO :2000 American Petroleum Institute TableÊ2ÊÑÊSummary of physical and performance requirements (continued) Well cement Class A B C D E F G H Pressure temperature thickening time test (clause 10) Specification test Schedule number Tables 9 through 13 Maximum consistency (15Êmin to 30 min stirring period) Bc a Thickening time (min./max.) min min. 90 min. 90 min. 90 min. NR NR NR NR 5 30 NR NR NR NR NR NR 90 min. 90 min NR NR NR NR NR NR 120 max. 120 max NR NR NR 100 min. 100 min. 100 min. NR NR 8 30 NR NR NR NR 154 min. NR NR NR 9 30 NR NR NR NR NR 190 min. NR NR a Bearden units of consistency (Bc) obtained on a pressurized consistometer as defined in clause 10 and calibrated as per the same clause. NR = No Requirement 4.2 Sampling frequency, timing of tests and equipment Sampling frequency For well cement Classes C, D, E, F, G and H, a sample for testing shall be taken by either method (1): over a 24-h interval or method (2): on a 1Ê000 ton (maximum) production run. For well cement Classes A and B, a sample for testing shall be taken by either method (1): over a 14-day interval or method (2): on a 25Ê000 ton (maximum) production run. These samples shall represent the product as produced. At the choice of the manufacturer, either method (1) or method (2) may be used Time from sampling to testing Each sample shall be tested for conformance to this standard. All tests shall be completed within seven working days after sampling Specified equipment Equipment used for testing well cements shall comply with TableÊ3. Dimensions shown in FiguresÊ4, 5, 9, and 10 are for cement specification test equipment manufacturing purposes. Dimensional recertification shall not be required. 8

18 American Petroleum Institute API Specification 10A/ISO :2000 TableÊ3ÊÑ Specification test equipment for well-cement manufacturers Test or preparation Well cement classes Clause reference Required equipment Sampling All clause 5 Apparatus specified in ASTM C 183 (or EN 196-7). Fineness A, B, C clause 6 Turbidimeter and auxiliary equipment as specified in ASTM C 115 or air permeability apparatus and auxiliary equipment as specified in ASTM CÊ204 (or EN 196-6) Slurry preparation All clause 7 Apparatus specified in 7.1 Free fluid G, H clause 8 Apparatus specified in 8.1 Atmospheric pressure compressive strength Pressure cured compressive strength A, B, C, G, H clause 9 Apparatus specified in 9.1, except pressure vessel of D, E, F clause 9 Apparatus specified in 9.1 Thickening time All clause 10 Pressurized consistometer specified in Calibration Equipment calibrated to the requirements of this standard is considered to be accurate if calibration is within the specified limits. 5 Sampling procedure One or more of the procedures outlined in ASTM C 183 (or EN 196-7) shall be used to secure a sample of well cement for specification testing purposes. 6 Fineness tests 6.1 Procedure Tests for fineness of well cement shall be carried out in accordance with either the procedure in ASTM C 115 for the turbidimeter test or the procedure in ASTM C 204 (or EN 196-6) by air permeability apparatus for the air permeability test. 6.2 Requirements Acceptance requirements for the fineness test are a minimum specific surface area (expressed in square meters per kilogram) and are as given in TableÊ2. Cement Classes D, E, F, G and H have no fineness requirement. Either of the two fineness test methods (turbidimeter or air permeability test) shall be used, at the discretion of the manufacturer, to determine the fineness. 9

19 API Specification 10A/ISO :2000 American Petroleum Institute 7 Preparation of slurry for free fluid, compressive strength and thickening time tests 7.1 Apparatus Scales The indicated load on scales shall be accurate within 0,1Ê% of the indicated load. Annual calibration is required Weights Weights shall be accurate within the tolerance shown in Table 4. On beam-type scales where the weights are on the beam, the indicated weights shall conform to the requirements given in TableÊ4ÊÑ Permissible variation in weights Weight g Permissible variation g ± 0,5 500 ± 0, ± 0, ± 0, ± 0,15 50 ± 0, Sieves A No. 20 wire cloth sieve (openings 850ʵm), meeting the requirements given in ISO , shall be used for sieving cement prior to slurry preparation Mixing devices The mixing device for preparation of well cement slurries shall be a one liter (or one quart) size, bottom-drive, blade type mixer. Examples of mixing devices in common use are shown in Figure 1. The mixing blade and mixing container shall be constructed of durable corrosion-resistant material. The mixing assembly shall be constructed in such a manner that the blade can be removed for weighing and changing. The mixing blade shall be weighed prior to use and replaced with an unused blade when 10% mass loss has occurred. If water leakage occurs around the bearings, the entire blender blade assembly should be replaced. FigureÊ1ÊÑ Examples of typical cement-mixing devices 10

20 American Petroleum Institute API Specification 10A/ISO : Procedure Sieving Prior to mixing, the cement shall be sieved as described in ASTM C Temperature of water and cement The temperature of the mix water in the container within 60 s prior to mixing shall be 23Ê CʱÊ1Ê C (73Ê FʱÊ2Ê F) and that of the cement within 60Ês prior to mixing shall be 23Ê CʱÊ1Ê C (73Ê FʱÊ2Ê F) Mix water Distilled or deionized water shall be used for testing. The mix water shall be weighed directly into a clean, dry mixing container. No water shall be added to compensate for evaporation, wetting, etc Mixing quantities Slurry component quantities shown in TableÊ5 shall be used for testing. The use of the quantities of components shown in TableÊ5 will result in mix-water percentages (based on the mass of dry cement) consistent with water percentages shown in TableÊ2. TableÊ5ÊÑ Slurry requirements Components Classes A and B Class C Classes D, E, F, H Class G g g g g Mix water 355ʱÊ0,5 383ʱÊ0,5 327ʱÊ0,5 349ʱÊ0,5 Cement 772ʱÊ0,5 684ʱÊ0,5 860ʱÊ0,5 792ʱÊ0, Mixing cement and water The mixing container with the required mass of mix water, as specified in Table 5, shall be placed on the mixer base, the motor turned on and maintained at r/minê±ê200 r/min (66,7 r/sê±ê3,3 r/s) while the cement sample is added at a uniform rate in not more than 15Ês. After all of the cement has been added to the mix water, the cover shall be placed on the mixing container and mixing shall be continued at 12Ê000 r/minê±ê500êr/min (200 r/sê±ê8,3 r/s) for 35 sê±1 s. 8 Free-fluid test (free water) 8.1 Apparatus Consistometer The atmospheric pressure consistometer or the pressurized consistometer described in 10.1 (run at atmospheric pressure) shall be used for stirring and conditioning the cement slurry for determination of free-fluid content. The atmospheric consistometer consists of a rotating cylindrical slurry container, equipped with an essentially stationary paddle assembly, in a temperature controlled liquid bath. It shall be capable of maintaining the temperature of the bath at 27Ê CʱÊ1,7Ê C (80Ê FÊʱÊ3Ê F) and of rotating the slurry container at a speed of 150Êr/minʱ15Êr/min (2,5Êr/sʱÊ0,25Êr/s) during the stirring and conditioning period for the slurry. The paddle and all parts of the slurry container exposed to the slurry shall be constructed of corrosion-resistant materials. See FiguresÊ2, 3, 4 and 5. NOTE The paddle may be used to drive a "potentiometer" (see FiguresÊ2 and 3) to measure slurry viscosity. 11

21 API Specification 10A/ISO :2000 American Petroleum Institute ,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,, Key 1 Cap lock nut 2 Center lock reverse jam nut 3 Dial 4 Pointer 5 Dial and base assembly 6 Spring 7 Collar 8 Bearing 9 Retaining ring 10 Lid 11 Roll pin 12 Shaft FigureÊ2ÊÑ Typical potentiometer mechanism for atmospheric pressure consistometer 12

22 American Petroleum Institute API Specification 10A/ISO : Key 1 Lid (see FigureÊ2) 2 Fill indicating groove 3 Slurry container (see FigureÊ4) 4 Paddle (see FigureÊ5) FigureÊ3ÊÑ Container assembly for typical atmospheric pressure consistometer 13

23 API Specification 10A/ISO :2000 American Petroleum Institute Dimensions in millimeters [inches] 1 3,05 [0,12] 5,33 [0,21] 6,6 [0,26] 2 15,75 [0,62] 3 11,18 [0,44] 133,35 [5,25] 208,03 [8,19] Key 1 2 slots 180 apart 2 Fill-level indicating groove 3 Pivot bearing Tolerances mm [inches],x [,xx] ±Ê0,25 [0,010],xx [,xxx] ±Ê0,13 [0,005] angles ±Ê1 FigureÊ4ÊÑ Container for typical atmospheric pressure consistometer 14

24 American Petroleum Institute API Specification 10A/ISO :2000 Dimensions in millimeters [inches] 205,49 [8,09] 117,35 [4,62] 6,86 [0,27] 7,62 [0,3] 2,79 [0,11] 1,27 [0,05] 13,71 [0,54] 25,4 [1] 4,83 [0,19] 57,15 [2,25] NOTE 1 NOTE 2 Paddle material: type 302 stainless steel 1,0ÊmmÊ Ê7,9Êmm (0,04Êin Ê0,313 in) cold-rolled strip. Shaft material: type 416 steel 6,4ÊmmÊ Ê211,1Êmm (0,25Êin Ê8,313 in) annealed and ground. Tolerances mm [inches],x [,xx] ±Ê0,25 [0,010],xx [,xxx] ±Ê0,13 [0,005] angles ±Ê1 FigureÊ5ÊÑ Paddle for typical atmospheric pressure consistometer 15

25 API Specification 10A/ISO :2000 American Petroleum Institute Scales Scales shall meet the requirements of Test flask A 500 ml conical flask in accordance with ASTM E 1404, Type I, Class 2 or DIN shall be used. See FigureÊ6. Dimensions in millimeters a 1 min. 186 max. f 105 max. b Key a b Wall thickness OD (at widest point) 8.2 Calibration FigureÊ6ÊÑ Conical flask for measurement of free fluid Temperature-measuring system The temperature of the bath shall be measured by thermometer (glass or digital) and/or thermocouple with digital indicator which are accurate to ±Ê1,7Ê C (±Ê3 F). Thermocouples shall be ASTM E 220 classification ÒspecialÓ TypeÊJ. Thermocouples with digital indicators and thermometers shall be checked for accuracy against a certified thermometer, traceable to the reference of the national body responsible for standards of temperature measurement, no less frequently than monthly. Thermocouples with digital indicators and thermometers found outside the acceptable ±Ê1,7Ê C (±Ê3Ê F) range shall be corrected or replaced. See annex A Slurry container rotational speed The rotational speed shall be 150Êr/minʱÊ15Êr/min (2,5Êr/sʱÊ0,25Êr/s). The rotational speed of the slurry container shall be checked no less frequently than quarterly, and corrected if found to be inaccurate Timer The timer shall be accurate to within ±Ê30Ês per hour. It shall be checked for accuracy no less frequently than semiannually, and corrected or replaced if found to be inaccurate. 16

26 American Petroleum Institute API Specification 10A/ISO : Procedure Prepare the slurry according to the procedure in clauseê Fill a clean and dry consistometer slurry container to the proper level Assemble the slurry container and associated parts, place them in the consistometer and start the motor according to the operating instructions of the manufacturer. The interval between completion of mixing and starting of the consistometer shall not exceed 1 min Stir the slurry in the consistometer for a period of 20ÊminʱÊ30Ês. Maintain the bath temperature at 27Ê CʱÊ1,7Ê C (80Ê FʱÊ3Ê F) throughout the stirring period Transfer 790ÊgʱÊ5Êg of Class H slurry or 760ÊgʱÊ5Êg of Class G slurry directly into the clean, dry 500Êml conical flask within 1Êmin. Record the actual mass transferred. Seal the flask with a self-sealing film to prevent evaporation Set the slurry-filled flask on a surface that is nominally level and vibration-free. The air temperature to which the slurry-filled flask is exposed shall be 22,8Ê CʱÊ2,8Ê C (73Ê Fʱ 5Ê F). The temperature sensor for measuring air temperature shall meet the requirements of Let the slurry-filled flask remain undisturbed for a period of 2ÊhʱÊ5Êmin At the end of 2Êh, remove the supernatant fluid that has developed with a pipet or syringe. Measure the volume of supernatant fluid to an accuracy of ± 0,1 ml and record it as milliliters free fluid Convert the milliliters free fluid to a percentage of starting slurry volume (~400 ml depending on recorded initial mass) and express that value as percent free fluid. 8.4 Calculation of percent free fluid Free fluid shall be calculated as a percentage, using the following formula: % FF = V FF ρ X 100 m S where % FF is the free fluid content of the slurry, in percent; V FF ρ NOTE 1 is the volume of free fluid (supernatant fluid) collected, expressed in milliliters; is the specific gravity (expressed in grams per cubic centimeter) of slurry; equal to 1,98 for Class H at 38Ê% water; 1,90 for Class G at 44Ê% water; If the specific gravity of the base cement is other than 3,14, the actual ρ of slurry should be calculated and used. m S EXAMPLE is the initially recorded (starting) mass of slurry, expressed in grams. Calculation of percent free fluid: m S = 791,7 g V FF = 15,1 ml ρ = 1,98 g/cm 3 (Class H) % FF = 15,1 (1,98 ) 100 / 791,7 % FF = 3,78 NOTE 2 cm 3 and ml are assumed to be equal for purposes of calculation. 17

27 API Specification 10A/ISO :2000 American Petroleum Institute 8.5 Acceptance requirements The %ÊFF for well cement of Classes G and H shall not exceed 5,90Ê%. 9 Compressive strength tests 9.1 Apparatus Cube moulds and compressive strength-testing machine Moulds and testing machine for compressive strength tests shall conform to the requirements in ASTM C 109, except that the moulds may be separable into more than two parts. The moulds shall be checked for tolerances and the testing machine shall be calibrated within ±Ê1Ê% of the load range to be measured, at least once every two years Cube mould base and cover plates Generally, plate glass, brass or stainless steel plates having a minimum thickness of 6Êmm (1/4 inch) are used. Cover plates may be grooved on the surface which contacts the top of the cement Water curing bath A curing bath or tank having dimensions allowing the complete immersion of a compressive strength mould(s) in water and capable of maintaining the prescribed test temperatures within ±Ê2Ê CÊ(±Ê3Ê F) of shall be employed. The two types of water curing baths are: Atmospheric pressure curing bath A vessel for curing specimens at atmospheric pressure and temperatures of 66Ê CÊ(150Ê F) or less, having an agitator or circulating system Pressurized curing bath A vessel suitable for curing specimens at temperatures ²Ê160Ê CÊ(320Ê F) and at pressures that can be controlled at 20,7ÊMPaʱÊ0,345ÊMPa (3Ê000ÊpsiʱÊ50 psi). The vessel shall be capable of fulfilling the appropriate specification schedule given in TableÊ Cooling bath The cooling bath dimensions shall be such that the specimen to be cooled from the curing temperature can be completely submerged in water maintained at 27Ê CʱÊ3Ê C (80Ê FʱÊ5Ê F) Temperature-measuring system The temperature-measuring system shall be calibrated to an accuracy of ±Ê2Ê C (±Ê3Ê F) no less frequently than monthly. The procedure described in annex A is commonly used. Two commonly used temperature-measuring systems are: Thermometer A thermometer with a range including 21Ê C to 82Ê C (70Ê F to 180Ê F), with minimum scale divisions not exceeding 1 C (2 F) may be used Thermocouple A thermocouple system with the appropriate range may be used. 18

28 American Petroleum Institute API Specification 10A/ISO :2000 TableÊ6ÊÑÊSpecification schedules for pressurized curing of specimens Schedule number Final curing pressure a MPa (psi) Elapsed time from first application of heat and pressure h: min (±Ê2Êmin) 0:00 0:30 0:45 1:00 1:15 1:30 2:00 2:30 3:00 3:30 4:00 Temperature C ( F) 4S 20,7 (3 000) 27 (80) 47 (116) 49 (120) 51 (124) 53 (128) 55 (131) 59 (139) 64 (147) 68 (155) 72 (162) 77 (170) 6S 20,7 (3 000) 8S 20,7 (3 000) 27 (80) 27 (80) 56 (133) 67 (153) 64 (148) 87 (189) 68 (154) 99 (210) 72 (161) 103 (216) 75 (167) 106 (223) 82 (180) 113 (236) 89 (192) 121 (250) 96 (205) 128 (263) 103 (218) 136 (277) 110 (230) 143 (290) 9S 20,7 (3 000) 27 (80) 73 (164) 97 (206) 120 (248) 123 (254) 127 (260) 133 (272) 140 (284) 147 (296) 153 (308) 160 (320) a The test pressure shall be applied as soon as specimens are placed in the pressure vessel and maintained at the given pressure within the following limits for the duration of the curing period: Schedules 4S through 9S: at 20,7 MPa ±Ê3,4 MPa (3Ê000Êpsi ± 500 psi) Puddling rod Typically, a corrosion-resistant puddling rod of nominal diameter 6Êmm (1/4 inch) is used Sealant Commonly, a sealant having properties to prevent leakage as well as water resistance, when subjected to curing temperatures and pressures specified in TableÊ7, is used to seal specimen mould exterior contact points. 9.2 Procedure Preparation of moulds The moulds and the contact surfaces of the plates shall be clean and dry. The assembled moulds shall be watertight. The interior faces of the moulds and the contact surfaces of the plates are commonly lightly coated with release agent, but may be clean and dry Preparation and placement of slurry Slurry Prepare the cement slurry in accordance with clause 7. 19

29 API Specification 10A/ISO :2000 American Petroleum Institute Placing slurry in moulds Place the slurry in the prepared moulds in a layer approximately one-half of the mould depth and puddle, in an evenlydistributed pattern, 27 times per specimen using the puddling rod. Place slurry in all the specimen compartments before commencing the puddling operation. After puddling the layer, stir the remaining slurry by hand, using a puddling rod or spatula to minimize segregation. Fill the moulds to overflowing, and puddle the same as for the first layer. After puddling, strike off the excess slurry even with the top of the mould using a straightedge. Discard specimens in moulds which leak. Place a clean dry cover plate on top of the mould. For each test determination, not less than three specimens shall be used Elapsed time from mixing to placing in the curing vessel Place the specimens in the curing vessel, and apply temperature and/or pressure according to the appropriate curing schedule at 5ÊminʱÊ15Ês after the end of mixing Curing Curing periods The curing period is the time elapsed from subjecting the specimens to the specified temperature in the curing vessel to testing the specimen for strength. The strength of the specimen shall be tested at the appropriate time as specified in TableÊ7. For specimens cured at atmospheric pressure, the curing period starts when specimens are initially placed in the curing bath preheated to the test temperature. For specimens cured at pressures above atmospheric, the curing period starts with the initial application of pressure and temperature Curing temperature and pressure Curing temperature and pressure shall be as specified in TableÊ7 for the appropriate class of cement. For tests at atmospheric pressure, place the specimens in the water bath preheated to the final curing temperature. For tests at pressure greater than atmospheric, place the specimens in the pressure vessel in water at 27Ê CʱÊ3Ê C (80Ê FʱÊ5Ê F) Specimen cooling Specimens cured at 60Ê C (140Ê F) and below shall be removed from the curing bath 45ÊminʱÊ5Êmin before the time at which they are to be tested, removed from their moulds, and placed in a water bath maintained at 27Ê CʱÊ3Ê C (80Ê FʱÊ5Ê F) for 40ÊminʱÊ5Êmin. For specimens cured at temperatures equal to or greater than 77 C (170Ê F), maintain the maximum scheduled temperature and pressure specified in Table 7 until 1Êh and 45ÊminʱÊ5Êmin prior to the time at which the specimens are to be tested, at which time discontinue heating. During the next 60Êmin ±Ê5Êmin, decrease the temperature to 77Ê C (170Ê F), or less, without reduction in pressure other than that caused by the reduction in temperature. At 45ÊminʱÊ5Êmin prior to the time at which the specimens are to be tested, release the pressure then remaining and remove the specimens from the moulds, transfer to a water bath, and maintain at 27Ê CʱÊ3Ê C (80Ê FʱÊ5Ê F) for 35ÊminʱÊ5Êmin Specimen acceptance Cube test specimens that are damaged shall be discarded prior to testing. If less than two test specimens are left for determining the compressive strength at any given period, a retest shall be made. 9.3 Test procedure (derived from ASTM C 109) Remove specimens from the water bath. Wipe each specimen to remove any loose material from the faces that will be in contact with the bearing blocks of the testing machine. 20

30 American Petroleum Institute API Specification 10A/ISO : Apply the load to specimen faces that were in contact with the plane surfaces of the mould. Place the specimen in the testing machine below the upper bearing block. Prior to the testing of each cube, ascertain that the spherically seated block is free to tilt. Use no cushioning or bedding materials. Employ appropriate safety and handling procedures in testing the specimen The rate of loading shall be 72ÊkNʱÊ7ÊkN (16Ê000ÊlbfʱÊ1Ê600Êlbf) per minute for specimens expected to have strength greater than 3,4 MPa (500 psi). For specimens expected to have strength less than 3,4ÊMPa (500Êpsi), a 18ÊkNʱÊ2ÊkN (4Ê000 lbfê±ê400êlbf) per minute rate shall be used. Make no adjustment in the controls of the testing machine while a specimen is yielding before failure Calculate the compressive strength in megapascals (MPa) (psi). The dimensions of the test faces shall be measured to ±Ê1,6 mm (±Ê1/16 inch) for calculation of the cross-sectional area. 9.4 Compressive strength acceptance criteria The compressive strength of all acceptance test specimens made from the same sample and tested at the same period shall be recorded and averaged to the nearest 69ÊkPa (10Êpsi). At least two-thirds of the original individual specimens and the average of all the specimens tested shall meet or exceed the minimum compressive strength specified in TableÊ7. If less than two strength values are left for determining the compressive strength at any given period, a retest shall be made. TableÊ7ÊÑÊCompressive strength specification requirements Minimum compressive strength at indicated curing period Cement class Schedule No. Final curing temperature a C ( F) Final curing pressure b MPa (psi) 8ÊhʱÊ15Êmin MPa (psi) 24ÊhʱÊ15Êmin MPa (psi) A Ñ 38 (100) atm. 1,7 (250) 12,4 (1 800) B Ñ 38 (100) atm. 1,4 (200) 10,3 (1 500) C Ñ 38 (100) atm. 2,1 (300) 13,8 (2 000) D E F G, H 4S 77 (170) 20,7 (3 000) NR 6,9 (1 000) 6S 110 (230) 20,7 (3 000) 3,4 (500) 13,8 (2 000) 4S 77 (170) 20,7 (3 000) NR 6,9 (1 000) 8S 143 (290) 20,7 (3 000) 3,4 (500) 13,8 (2 000) 6S 110 (230) 20,7 (3 000) NR 6,9 (1 000) 9S 160 (320) 20,7 (3 000) 3,4 (500) 6,9 (1 000) Ñ 38 (100) atm. 2,1 (300) NR Ñ 60 (140) atm. 10,3 (1 500) NR NR = No Requirement a Curing temperature shall be maintained at ± 2 C (± 3 F). b The test pressure shall be applied as soon as specimens are placed in the pressure vessel, and maintained at the given pressure within the following limits for the duration of the curing period: Schedules 4S through 9S: at 20,7ÊMPaʱÊ3,4ÊMPa (3Ê000ÊpsiÊ±Ê 500Êpsi). 21

31 API Specification 10A/ISO :2000 American Petroleum Institute 10 Thickening-time tests 10.1 Apparatus This apparatus shall be a pressurized consistometer consisting of a rotating cylindrical slurry container as shown in Figure 9, equipped with a stationary paddle assembly, as shown in Figure 10, enclosed in a pressure vessel capable of withstanding the pressures and temperatures described in Tables 9, 10, 11, 12 and 13. Typical pressurized consistometers are illustrated in Figures 7 and 8. The space between the slurry container and the walls of the pressure vessel shall be completely filled with a hydrocarbon oil. The selected oil shall have the following physical properties: Viscosity = 7 mm 2 /s to 75 mm 2 /s at 38 C (49 SSU to 350 SSU at 100 F) Specific heat = 2,1 kj/(kg K) to 2,4 kj/(kg K) (0,5 Btu/lb F to 0,58 Btu/lb F) Thermal conductivity = 0,119ÊW/(m K) to 0,133 W/(m K) [0,0685 Btu/(h ft 2 F/ft) to 0,0770 Btu/(h ft 2 F/ft] Specific gravity = 0,85 to 0,91 A heating system capable of raising the temperature of this oil bath at the rate of at least 3Ê C (5Ê F) per minute is required. Temperature-measuring systems shall be provided for determining the temperature of the oil bath and also that of the slurry (see note). The slurry container is rotated at a speed of 150 r/min ± 15 r/min. The consistency of the slurry (as defined in ) shall be measured. The paddle and all parts of the slurry container exposed to the slurry shall be constructed as illustrated in Figures 9 and