1、Designation: C 1156 03Standard Guide forEstablishing Calibration for a Measurement Method Used toAnalyze Nuclear Fuel Cycle Materials1This standard is issued under the fixed designation C 1156; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、 revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This guide provides the basis for establishing calibrationfor a measurement method typically u
3、sed 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 technical informat
4、ion 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 does not purpor
5、t 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 Standards:C 1009
6、 Guide for Establishing a Quality Assurance Pro-gram for Analytical Chemistry Laboratories Within theNuclear Industry2C 1068 Guide for Qualification of Measurement Methodsby a Laboratory Within the Nuclear Industry2C 1128 Guide for Preparation of Working Reference Mate-rials for Use in the Analysis
7、of Nuclear Fuel CycleMaterials2C 1210 Guide for Establishing a Measurement SystemQuality Control Program for Analytical Chemistry Labo-ratories Within the Nuclear Industry2C 1215 Guide for Preparing and Interpreting Precision andBias Statements in Test Method Standards Used in theNuclear Industry2C
8、1297 Guide for Qualification of Laboratory Analysts forthe Analysis of Nuclear Fuel Cycle Materials22.2 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 e
9、ffect 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, a
10、nd 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 C 1009, in whichcal
11、ibration 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 usually
12、established when a method is first introduced into a laboratory,which may be through validation and qualification as definedby Guide C 1068 (see Fig. 1). However, calibration involvesmore than the technical aspects of the calibration process. Theother dimension of the process is the operational requ
13、irementsthat are necessary to ensure that calibration results are validand that they are documented and verifiable should their1This guide is under the jurisdiction of ASTM Committee C26 on Nuclear FuelCycle and is the direct responsibility of Subcommittee C26.08 on Quality Assur-ance, Statistical A
14、pplications, and Reference Materials.Current edition approved July 10, 2003. Published August 2003. Originallyapproved in 1990. Last previous edition approved in 1995 as C 1156 95e1.2Annual Book of ASTM Standards, Vol 12.01.3Available from American National Standards Institute, 11 W. 42nd St., 13thF
15、loor, New York, NY 100361Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.integrity be questioned. The provisions of this guide providethose operational requirements and should be consideredwhenever calibration is planned and establish
16、ed.4. General Considerations4.1 The degree of attention and effort 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 mor
17、e attention than dataproduced for process control during the 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 provi
18、sions of this guide would not apply tothe calibration of certain 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 readi
19、ng is taken for a sample solution.4.3 There are generally two 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 el
20、apses to retain calibration. When a calibrationperiod is used, 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
21、 involve analyzing a standard periodicallyduring the sample run, 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
22、, and the criteria that determine when cali-bration has been achieved (see Guide C 1215).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 th
23、e responsibility for calibrating aninstrument or class of 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 establish
24、ed as a written procedure.The procedure should provide instructions 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-p
25、ared as a separate procedure from the one written for themeasurement 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.
26、 The calibration procedure should be reviewed for tech-nical adequacy and approved by management. The provisionscontained in the Procedure section of Guide C 1009 regardingthe preparation, review, and approval of procedures should beconsidered. Also, calibration procedures should be revised,distribu
27、ted, and controlled according to the provisions in theProcedure section of Guide C 1009.5.3 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
28、 standard or standardsthat will be used and inclusion of instructions 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
29、 that would alter the frequencies;5.3.4 Instructions, in a 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, correcti
30、ons for environmental conditions) required tofinalize the 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 i
31、n themetrological hierarchy of reference materials, followed 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. GuideC 1128 provides a definition of CRM and WRM and addr
32、essesthe various factors that affect the quality of reference materials.FIG. 1 Quality Assurance of Analytical Laboratory DataC11560326.2 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
33、requirements;for example, a CRM should not be selected when a lower levelstandard would suffice. Availability, stability, traceability to anational measurement base, and other considerations that couldaffect selection (see Guide C 1128).6.3 PreparationPreparation may vary from making asimple dilutio
34、n of a stock (master) solution to a majorpreparation and characterization effort as described in GuideC 1128. In some situations, a pretreatment of the standardmight be required before use. Instructions for the preparationor pretreatment of the standard should be included in thecalibration procedure
35、, or at least a reference to such instruc-tions should be given. If the standard is a pre-prepared standardthat requires simply taking a packaged unit for a one-time use,or if it is a physical standard (as opposed to a chemicalstandard) that is used repeatedly, then the source and descrip-tion of th
36、e standard should be included in the calibrationprocedure.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 isa
37、ddressed in Guide C 1128.7. Control of Calibrated Equipment7.1 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 s
38、hould be a process forkeeping a current indication of calibration 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 resul
39、ts. Those records should be readilyavailable to show current 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
40、-tion period, the equipment should not be used until thesituation 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.
41、Documentation8.1 Documentation should provide the evidence 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 C 1009).8.2 Data RecordThe laboratory
42、 data record system shouldbe used to document calibration (see the Laboratory Recordssection of Guide C 1009). For each piece of equipment,calibration records should identify the person performing thecalibration, calibration date, calibration procedure, standardsused, calibration data, special obser
43、vations during calibration,and a description of actions taken 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
44、of any patent rights asserted in connection with any item 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 t
45、o revision at any time by the responsible technical committee 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.
46、 Your comments will receive careful consideration at a meeting 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
47、copyrighted by ASTM International, 100 Barr Harbor Drive, 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).C1156033
