1、Designation: C1156 03 (Reapproved 2011)Standard Guide forEstablishing Calibration for a Measurement Method Used toAnalyze Nuclear Fuel Cycle Materials1This standard is issued under the fixed designation C1156; the number immediately following the designation indicates the year oforiginal adoption or
2、, 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 guide provides the basis for establishing calibrationfor a measurement met
3、hod typically used in an analyticalchemistry laboratory analyzing nuclear materials. Guidance isincluded for such activities as preparing a calibration proce-dure, selecting a calibration standard, controlling calibratedequipment, and documenting calibration. The guide is genericand any required tec
4、hnical information specific for a givenmethod must be obtained from other sources.1.2 The guidance information is provided in the followingsections:SectionGeneral Considerations 4Calibration Procedure 5Calibration Standard 6Control of Calibrated Equipment 7Documentation 8Keywords 91.3 This standard
5、does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM S
6、tandards:2C1009 Guide for Establishing a Quality Assurance Programfor Analytical Chemistry Laboratories Within the NuclearIndustryC1068 Guide for Qualification of Measurement Methods bya Laboratory Within the Nuclear IndustryC1128 Guide for Preparation of Working Reference Mate-rials for Use in Anal
7、ysis of Nuclear Fuel Cycle MaterialsC1210 Guide for Establishing a Measurement SystemQuality Control Program for Analytical Chemistry Labo-ratories Within the Nuclear IndustryC1215 Guide for Preparing and Interpreting Precision andBias Statements in Test Method Standards Used in theNuclear IndustryC
8、1297 Guide for Qualification of Laboratory Analysts forthe Analysis of Nuclear Fuel Cycle Materials2.2 ISO Standard:ISO 17025 General Requirements for the Competence ofCalibration and Testing Laboratories33. Significance and Use3.1 Calibration is a fundamental part of making measure-ments and its ef
9、fect on the quality of measurement data issignificant. Thus, sufficient attention must be given to calibra-tion when it is established for a measurement method so thatthe data produced will be acceptable. The use of an inappro-priate calibration standard, inadequate instructions for calibra-tion, an
10、d poor documentation of the calibration process areexamples of circumstances that can adversely affect the valid-ity of a calibration. Thus, the calibration process must conformto criteria established to ensure the validity of calibrationresults. Such criteria are given in Guide C1009, in whichcalib
11、ration is identified as a component of laboratory qualityassurance (see Fig. 1). This guide expands upon those criteriato provide more comprehensive guidance for establishingcalibration.3.2 The manner of calibration and other technical require-ments for calibrating a measurement method are usuallyes
12、tablished when a method is first introduced into a laboratory,which may be through validation and qualification as definedby Guide C1068 (see Fig. 1). However, calibration involvesmore than the technical aspects of the calibration process. Theother dimension of the process is the operational require
13、mentsthat are necessary to ensure that calibration results are validand that they are documented and verifiable should theirintegrity be questioned. The provisions of this guide provide1This guide is under the jurisdiction of ASTM Committee C26 on Nuclear FuelCycle and is the direct responsibility o
14、f Subcommittee C26.08 on Quality Assur-ance, Statistical Applications, and Reference MaterialsCurrent edition approved June 1, 2011. Published June 2011. Originallyapproved in 1990. Last previous edition approved in 2003 as C1156 03. DOI:10.1520/C1156-03R11.2For referenced ASTM standards, visit the
15、ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10
16、036, http:/www.ansi.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.those operational requirements and should be consideredwhenever calibration is planned and established.4. General Considerations4.1 The degree of attention and e
17、ffort given to calibrationshould depend on how the measurement data are to be used. Inthe analysis of nuclear materials, for example, measurementdata produced for the control and accountability of nuclearmaterial would normally require more attention than dataproduced for process control during the
18、processing of thatmaterial. The areas in which the level of attention and effortcould vary are: the calibration standard, number of calibrationpoints, frequency of calibration, and frequency of calibrationverification.4.2 Many of the provisions of this guide would not apply tothe calibration of cert
19、ain instruments when their calibration isan integral part of the analysis procedure involving a simpleone- or two-step adjustment of a meter or gage. The pH meteris an example when a buffer is used to adjust the meter justbefore a pH reading is taken for a sample solution.4.3 There are generally two
20、 approaches regarding frequencyof calibration. In one case, the method is calibrated each timeit is used. In the other, calibration is established for a specifiedperiod of time, and the method must be recalibrated before thattime period elapses to retain calibration. When a calibrationperiod is used
21、, calibration verification should be used. Acalibration period might be defined in terms of weeks ormonths, or defined as a run of a series of samples over arelatively short period of time. In the latter case, calibrationverification could involve analyzing a standard periodicallyduring the sample r
22、un, for example, after every fifth sample.4.4 When calibration is being planned and established, astatistician should be consulted regarding the treatment ofcalibration data, the frequency of calibration, the frequency ofcalibration checks, and the criteria that determine when cali-bration has been
23、achieved (see Guide C1215 Guide).4.5 The organizational responsibility and authority for cali-bration should be defined and documented. Normally, respon-sibility for calibrating an individual method rests with theanalyst using the method. If the responsibility for calibrating aninstrument or class o
24、f instruments is contracted to anotherorganization, the laboratory is still responsible for ensuring thatcalibration requirements are being met by the organizationdoing the calibration.5. Calibration Procedure5.1 Calibration should be established as a written procedure.The procedure should provide i
25、nstructions for those doing thecalibration, and it should document the basis for calibration,which can be used to substantiate the validity of the calibrationprocess, should that be required.5.2 PreparationThe calibration procedure can be pre-pared as a separate procedure from the one written for th
26、emeasurement method or it can be a section of the methodsprocedure as long as the provisions given in 5.3 are addressed.If the former approach is used, the applicable measurementmethod should be clearly identified in the calibration proce-dure. The calibration procedure should be reviewed for tech-n
27、ical adequacy and approved by management. The provisionscontained in the Procedure section of Guide C1009 regardingthe preparation, review, and approval of procedures should beconsidered. Also, calibration procedures should be revised,distributed, and controlled according to the provisions in thePro
28、cedure section of Guide C1009.5.3 ContentThe following subjects should be addressed inthe procedure:5.3.1 Identification of the equipment or portion of themeasurement apparatus that requires calibration,5.3.2 Identification of the calibration standard or standardsthat will be used and inclusion of i
29、nstructions for the prepara-tion, pretreatment, and use of the standard(s) as appropriate;5.3.3 A statement of the required frequencies of calibrationand calibration verification as appropriate and a description ofany situations or conditions that would alter the frequencies;5.3.4 Instructions, in a
30、 step-by-step format, for performingthe calibration, including applicable instructions for calculationof the slope of the calibration curve, preparation of a calibra-tion curve, or other treatment of the calibration data (forexample, corrections for environmental conditions) required tofinalize the
31、calibration process.5.3.5 Criteria that establish when the method or equipmentneeds recalibration.6. Calibration Standard6.1 Calibration standards are reference materials. A certifiedreference material (CRM) is the highest level of standard in themetrological hierarchy of reference materials, follow
32、ed by aworking reference material (WRM). The level of referencematerial is governed by the rigor, care, and overall effort putinto the preparation and characterization of the material. GuideC1128 provides a definition of CRM and WRM and addressesthe various factors that affect the quality of referen
33、ce materials.6.2 SelectionThe level of a standard required for calibra-tion depends on the requirements for the measurement data tobe produced. Selection should be based on these requirements;FIG. 1 Quality Assurance of Analytical Laboratory DataC1156 03 (2011)2for example, a CRM should not be selec
34、ted when a lower levelstandard would suffice. Availability, stability, traceability to anational measurement base, and other considerations that couldaffect selection (see Guide C1128).6.3 PreparationPreparation may vary from making asimple dilution of a stock (master) solution to a majorpreparation
35、 and characterization effort as described in GuideC1128. In some situations, a pretreatment of the standard mightbe required before use. Instructions for the preparation orpretreatment of the standard should be included in the calibra-tion procedure, or at least a reference to such instructionsshoul
36、d be given. If the standard is a pre-prepared standard thatrequires simply taking a packaged unit for a one-time use, or ifit is a physical standard (as opposed to a chemical standard)that is used repeatedly, then the source and description of thestandard should be included in the calibration proced
37、ure.6.4 UseIf special storage or handling practices are re-quired to protect the integrity of the standard, those practicesshould be provided in the calibration procedure. Protecting theintegrity of standards in terms of packaging and storage isaddressed in Guide C1128.7. Control of Calibrated Equip
38、ment7.1 IdentificationEquipment requiring calibration shouldbe uniquely identified. The identification should be marked onthe equipment (for example, with tags, labels, or markings) andon related calibration records.7.2 Calibration StatusThere should be a process forkeeping a current indication of c
39、alibration status. Status can beindicated on the calibrated equipment with a label stating whencalibration was done and when it expires. An alternative wouldbe to document status in the data record system used to recordcalibration data and results. Those records should be readilyavailable to show cu
40、rrent status.7.3 UseCalibration equipment should be used andhandled in a manner to help ensure that calibration will remainvalid during the calibration period. If there is a reason tobelieve that calibration has become invalid during the calibra-tion period, the equipment should not be used until th
41、esituation has been evaluated and corrected (if necessary).7.4 Out-of-CalibrationIf a calibration time period ex-pires, the equipment involved should be recalibrated or re-moved from service. It should not be used to generatemeasurement data.8. Documentation8.1 Documentation should provide the evide
42、nce and sup-port for judgments regarding the quality of measurement dataand should provide historical evidence needed for futurereviews and evaluations of the data (see the Control of Recordssection of Guide C1009).8.2 Data RecordThe laboratory data record system shouldbe used to document calibratio
43、n (see the Laboratory Recordssection of Guide C1009). For each piece of equipment,calibration records should identify the person performing thecalibration, calibration date, calibration procedure, standardsused, calibration data, special observations during calibration,and a description of actions t
44、aken as a result of any out-of-calibration conditions.9. Keywords9.1 calibration; calibration procedure; calibration standard;certified reference material (CRM); laboratory equipmentASTM International takes no position respecting the validity of any patent rights asserted in connection with any item
45、 mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical commi
46、ttee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a me
47、eting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive,
48、 PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).C1156 03 (2011)3
