1、Designation: D7448 09D7448 16Standard Practice forEstablishing the Competence of Laboratories Using ASTMProcedures in the Sampling and Analysis of Coal and Coke1This standard is issued under the fixed designation D7448; the number immediately following the designation indicates the year oforiginal a
2、doption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice specifies requirements to operate and evaluate the qual
3、ity and management systems in a laboratory thatprovides services with respect to sample collection, sample preparation, or testing of coal, coke, and ash derived from coal or cokeusing ASTM standards that are under the jurisdiction of Committee D05 on Coal and Coke.NOTE 1The word “laboratory” is use
4、d throughout this practice when referring to an organization that provides services in coal sampling or testing,or both. It is recognized, however, that the word may not be appropriate to an organization that does not perform actual laboratory sample testing.1.2 International standard ANS/ISO/IECANS
5、I/ISO/IEC 17025 shall be the governing document specifying requirements formanagement, technical competence and evaluation of a laboratory.NOTE 2An accrediting body or user of laboratory services can also impose technical or non-technical requirements not specifically addressed inANS/ISO/IECANSI/ISO
6、/IEC 17025 provided they do not invalidate the requirements of ANS/ISO/IECANSI/ISO/IEC 17025.1.3 This practice is used to evaluate only those capabilitescapabilities specifically claimed by a laboratory.1.4 All percentages are percent mass fractions unless otherwise noted.1.5 This standard does not
7、purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D
8、121 Terminology of Coal and CokeD3174 Test Method for Ash in the Analysis Sample of Coal and Coke from CoalD4239 Test Method for Sulfur in the Analysis Sample of Coal and Coke Using High-Temperature Tube Furnace CombustionD4749 Test Method for Performing the Sieve Analysis of Coal and Designating Co
9、al SizeD5061 Test Method for Microscopical Determination of the Textural Components of Metallurgical CokeD5515 Test Method for Determination of the Swelling Properties of Bituminous Coal Using a DilatometerD6172 Test Method for Determining the Volume of Bulk Materials Using Contours or Cross Section
10、s Created by DirectOperator Compilation Using Photogrammetric ProceduresD6349 Test Method for Determination of Major and Minor Elements in Coal, Coke, and Solid Residues from Combustion ofCoal and Coke by Inductively Coupled PlasmaAtomic Emission SpectrometryE177 Practice for Use of the Terms Precis
11、ion and Bias in ASTM Test MethodsE456 Terminology Relating to Quality and StatisticsE2554 Practice for Estimating and Monitoring the Uncertainty of Test Results of a Test Method Using Control Chart Techniques2.2 ANS/ISO/IECANSI/ISO/IEC Document:317025 General Requirements for the Competence of Calib
12、ration and Testing Laboratories2.3 ISO Documents:45725-3 Accuracy (Trueness and Precision) of Measurement Methods and ResultsPart 3: Intermediate Measures of Precisionof a Standard Measurement Method1 This practice is under the jurisdiction ofASTM Committee D05 on Coal and Coke and is the direct res
13、ponsibility of Subcommittee D05.24 on QualityAssuranceStatistics.Current edition approved Nov. 1, 2009March 1, 2016. Published December 2009April 2016. Originally approved in 2009. Last previous edition approved in 2009 asD7448-09. DOI: 10.1520/D7448-09.10.1520/D7448-16.2 For referencedASTM standard
14、s, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor,
15、New York, NY 10036, http:/www.ansi.org.4 The boldface numbers in parentheses refer to the list of references at the end of this standard.Available from International Organization for Standardization (ISO), ISOCentral Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva, Switzer
16、land, http:/www.iso.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that
17、 users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15725-6 Accuracy (Truenes
18、s and Precision) of Measurement Methods and ResultsPart 6: Use in Practice of Accuracy Values3. Significance and Use3.1 International standard ANS/ISO/IECANSI/ISO/IEC 17025 promotes the use of documented accountability and qualitycontrol procedures to assure a laboratory and its clients that the lab
19、oratory can produce technically valid data and results in theroutine performance of its sampling, sample preparation and testing activities.3.2 Alaboratory shall useANSI/ISO/IEC 17025 to develop its quality system. Clause 4 ofANS/ISO/IECANSI/ISO/IEC 17025specifies the requirements for sound manageme
20、nt. Clause 5 of ANS/ISO/IECANSI/ISO/IEC 17025 specifies the requirements fortechnical competence for the type of tests or calibrations, or both the laboratory undertakes.3.3 In addition to complying with the requirements of ANS/ISO/IECANSI/ISO/IEC 17025, the Annex of this standard practicecontains i
21、nformation that shall be considered important for the evaluation and operation of a competent Coal and Coke samplingor testing facility, or both. The information in this Annex is presented where it is not otherwise covered in ANS/ISO/IECANSI/ISO/IEC 17025 or the applicable ASTM methods.3.4 Laborator
22、y clients, regulatory authorities, and accreditation bodies that recognize the competence of testing and calibrationlaboratories can use this standard practice as the basis for their evaluation.3.5 The primary significance of this practice is to establish that for a laboratory to generate measuremen
23、ts traceable to SI units,it must:3.5.1 Have a clear understanding of the work requested by the client.3.5.2 Meet the quality system requirements of the internationally accepted ANS/ISO/IECANSI/ISO/IEC 17025 standard.3.5.3 Use test methods which have been shown to be traceable to SI units of measurem
24、entmeasurement.3.5.4 Be able to demonstrate that the laboratory is in statistical control at the time the measurements are made.4. Selection of an Evaluator4.1 The evaluator(s) shall have sufficient technical background to competently evaluate the application of ASTM standardsemployed for the sampli
25、ng, preparation and analysis of coal, coke, and ash derived from coal or coke.4.2 The evaluator(s) shall review the laboratory with the aid of a worksheet or checklist. Worksheets or checklists shall bedeveloped from the requirements of Clause 4 and Clause 5 of ANS/ISO/IECANSI/ISO/IEC 17025 in conce
26、rt with specifictechnical requirements specified in the ASTM standard(s) to be evaluated.4.3 Observations and comments made by the evaluator shall be keyed to item numbers in the checklist.5. Keywords5.1 accuracy; competence; evaluation; laboratory; management; stabilityANNEX(Mandatory Information)A
27、1. FACTORS AFFECTING THE TECHNICAL VALIDITY OF TESTSINTRODUCTIONFactors that can influence the technical validity of tests performed by a laboratory include but arenot limited to:(1) Sampling apparatus operation,(1) Sampling apparatus operation,(2) Sampling procedures,(3) Sample preparation apparatu
28、s,(4) Sample preparation operation,(5) Sample preparation procedures,(6) Laboratory equipment,(7) Laboratory equipment operation,(8) Test methods,(9) Calibration, control and consumable materials,(10) Calibration,(11) Uncertainty of measurement,D7448 162(12) Control charts,(13) Reporting procedures,
29、(14) Qualification of laboratory personnel, and(15) Environmental conditions (sampling, sample preparation and analyses).(2) Sampling procedures,(3) Sample preparation apparatus,(4) Sample preparation operation,(5) Sample preparation procedures,(6) Laboratory equipment,(7) Laboratory equipment opera
30、tion,(8) Test methods,(9) Calibration, control and consumable materials,(10) Calibration,(11) Uncertainty of measurement,(12) Control charts,(13) Reporting procedures,(14) Qualification of laboratory personnel, and(15) Environmental conditions (sampling, sample preparation and analyses).This annex w
31、hile mandatory, identifies several items as a “typical practice”. A “typical practice” isnot to be considered the only correct practice. Typical practices have been included throughout thisAnnex only for the purpose of clarifying the content of this Annex.The extent to which the factors contribute t
32、o the technical validity of results can differ considerablybetween tests. The laboratory shall have procedures that address these factors where these areapplicable and under the laboratorys control.D7448 163ANS/ISO/IECANSI/ISO/IEC 17025 Clause 4.1.5 states:“The laboratory shall have managerial and t
33、echnical personnel who, irrespective of otherresponsibilities, have the authority and resources needed to carry out their duties, including theimplementation, maintenance and improvement of the management system, and to identify theoccurrence of departures from the management system or from the proc
34、edures for performing testsand/or calibrations and to initiate actions to prevent or minimize such departures.”Managerial and technical personnel shall have the authority and resources to implement thepractices specified in this Annex in a manner that ensures laboratory procedures produce data of th
35、etype and quality needed for the intended end use.A1.1 Sampling Apparatus OperationA1.1.1 The laboratory shall have procedures describing acceptance requirements for all sampling equipment.A1.1.2 The laboratory shall have procedures describing verification of all sampling equipment.A1.2 Sampling Pro
36、ceduresA1.2.1 The laboratory shall have sampling procedures describing all processes under its control.A1.2.2 The laboratory shall have procedures describing requirements for bias tests.A1.2.3 The laboratory shall have procedures describing requirements for periodic bias tests after initial bias tes
37、ting and acceptanceof sampling systems.A1.2.4 The laboratory shall have procedures describing requirements for bias tests subsequent to maintenance and or/modificationof sampling systems.A1.3 Sample Preparation ApparatusA1.3.1 The laboratory shall have procedures describing:A1.3.1.1 Acceptance requi
38、rements for all sample preparation equipment.A1.3.1.2 Procedures for verification of all sample preparation equipment.A1.4 Sample Preparation OperationA1.4.1 The laboratory shall have a documented management plan which shall include requirements for:A1.4.1.1 Maintaining a chain of custody for sample
39、s.TABLE A1.1 Using ASTM Standard DesignationsStandard Method DesignationLab AStandard Method DesignationLab B Technically EquivalentASTM D5061-92 ASTM D5061-92(Reapproved 1997)Yes: Reapproval indicates no technical changes to standard D5061. (Note A1.1)ASTM D5061-92 ASTM D5061-92(Reapproved 1997)Yes
40、: Reapproval indicates no technical changes to standard D5061. (Note A1.1)ASTM D5515-94 ASTM D5515-97 No: The lab B year designation is 97. The lab A designation is 94. This indicates technical differ-ences between the two methods.ASTM D6172-98 ASTM D6172-98 Yes: Epsilon indicates an editorial chang
41、e added to improve clarity of use.ASTM D4239-02 ASTM D4239-02a No: The “a” indicates a technical revision occurred in the same year.D7448 164A1.4.1.2 Identifying the source of the sample.A1.4.1.3 Identifying date and time of initial sampling.A1.4.1.4 Identifying the individual(s) responsible for sam
42、pling and sample preparation.A1.4.1.5 Describing test and reserve sample(s) collected at each stage of sampling and sample preparation including date, time,top size and mass.A1.4.1.6 Minimizing contamination at each stage of sampling and sample preparation.A1.4.1.7 Minimizing dust loss and verifying
43、 material recovery at each stage of sampling and sample preparation.A1.4.1.8 Verifying particle size reduction equipment produce samples of the appropriate particle size criteria and homogeneity.A1.4.1.9 Minimizing changes in moisture and or oxidation of the sample(s) during transportation, preparat
44、ion, storage andhandling.A1.4.1.10 Mixing to minimize selection of a biased size fraction at each stage of sampling, including extraction of test portionsfrom the laboratory analysis sample.A1.4.1.11 Recording date and time the sample(s) are received in the laboratory.A1.4.1.12 Verifying compliance
45、or corrective action with respect to all elements of the management plan, or both.A1.4.1.13 Approval of changes or exceptions to the sampling and sample preparation proceduresA1.5 Sample Preparation ProceduresA1.5.1 The laboratory shall have procedures for all stages of sample preparation that are u
46、nder its control.A1.6 Laboratory EquipmentA1.6.1 The laboratory shall utilize equipment that meets the specifications of the relevant sampling/test methods.A1.7 Laboratory Equipment OperationA1.7.1 The laboratory shall have procedures describing equipment set-up and startup where appropriate.A1.7.2
47、Equipment that is operated outside of normal parameters shall be subject to verification.A1.7.3 The laboratory shall have procedures describing the minimum quality control that is required to validate the equipment isin statistical control at the time the measurements are made.A1.7.4 The laboratory
48、shall maintain all original instrument observations in accordance with their records control procedures.A1.8 Test MethodsA1.8.1 Laboratory procedures can consist of standard and non-standard methods.Anon-standard method includes the applicationof a standard method to samples that fall outside the sc
49、ope or validated range of the standard method or that allow conditions oftest which depart from those specified in a standard method.D7448 165A1.8.2 Publications from the AOAC International,(1)5 as well as ISO (5725-32, 3)and ISO 5725-6 describe procedures forestablishing the precision and accuracy of a non-standard method or demonstrating the equivalency of a non-standard method witha standard method.A1.8.3 The laboratory shall identify by ASTM (or other source) designation including revision, all standard and non-standardsampling, sample preparation and test procedu
