仪器确认-附件9-pH计确认-中英文

PA/PH/OMCL(13)863R欧盟OMCL仪器确认附件9：pH计(中英文)ourPreferredPartnertoComplianceOMCLNetworkoftheCouncilofEurope

QUALITYMANAGEMENTDOCUMENT

PA/PH/OMCL(13)863R

QUALIFICATIONOFEQUIPMENT

ANNEX9:CALIBRATION/QUALIFICATIONOFPH-METERSOMCL质量管理文件PA/PH/OMCL(13)863R

仪器验证

附件9：pH计校正/确认FulldocumenttitleandreferenceQualificationofEquipmentAnnex9:Calibration/QualificationofpHMetersPA/PH/OMCL(13)863R文件全名和索引号设备确认附件9：pH计校正/确认PA/PH/OMCL(13)863RDocumenttypeGuidelineLegislativebasisDateoffirstadoption首次采纳日期Dateoforiginalentryintoforce1stNovember2015首次生效日期DateofentryintoforceofreviseddocumePrevioustitles/otherreferences/lastvalidversion

旧文件题目/其它索引号/最后有效版本CustodianOrganisationThepresentdocumentwaselaboratedbytheOMCLNetwork/EDQMoftheCouncilofEurope监管机构现行文件由OMCL网络/EDQM起草ConcernedNetwork相关网络ANNEX9OFTHEOMCLNETWORKGUIDELINE“QUALIFICATIONOFEQUIPMENT”

CALIBRATION/QUALIFICATIONOFpHMETERSOMCL网络指南“仪器验证”之

附件9：pH计校正/确认INTRODUCTION概述Thisdocumentisthe9thAnnextothecoredocument“QualificationofEquipment”，whichtakentogethershouldbeusedwhenplanning,performinganddocumentingthequalificationprocessofpHmeters.ThecoredocumentcontainstheintroductionandgeneralformsforLevelIandIIofqualification,whicharecommontoalltypesofinstruments.本文件是核心文件“仪器确认”的第9个附件。在规划、实施和记录pH计的确认过程时应将本文件与核心文件一起使用。核心文件包括第I级和第II级确认的概述和通用表格，所有类型的仪器都是通用的。Annex9containsinstrument-relatedrecommendationsonparameterstobecheckedatLevelIIIandIVofqualificationandthecorrespondingtypicalacceptancelimits,aswellaspracticalexamplesonthemethodologythatcanbeusedtocarryoutthesechecks.附件9包括与仪器相关第III级和第IV级确认所需检查的参数的建议，以及对应的一般可接受限度，还有可以用来实施这些检查的方法学实际案例。AIMANDSCOPEOFTHEGUIDELINE本指南的目标和范围ThisguidelinedescribestherequirementsforpHmetersusedfordeterminationofpHinaqueoussolutions.Ifmeasurementsaremadeoftestsolutionsofanon-aqueousorpartiallynon-aqueouscharacter,suspensionsoremulsions,onasystemcalibratedasdescribedabove,thepHreadingcanonlybeconsideredtobeanapproximationofthetruevalue(apparentpH).Appropriateelectrodesshouldbeusedforsuchtypesofmeasurement.本指南描述了用于测定水溶液pH值的pH计的要求。如果所检测的是非水性溶液，或者是部分非分水溶性、混悬液或乳液，采用上述方法校正的系统进行检测，所获得的pH读数只能用为真值（表征pH值）的近似值。此类检测需要使用适当的电极。ThegeneralprinciplesofpHmeasurementtogetherwithapparatusandmethodsareprovidedinPh.Eur.Chapter2.2.3.‘PotentiometricdeterminationofpH’.pH测量和仪器及方法的通则在欧洲药典第2.2.3章“电位法测定pH值”中给出。CONSIDERATIONSFORLEVELIANDIIOFEQUIPMENTQUALIFICATION第I级和第II级仪器确认中的考虑AtlevelIofthequalificationofapHmeter(selectionofinstrumentsandsuppliers)itisrecommendedtoselectamanufacturerofpHmetersthatcansatisfytheneedsofthelaboratoryandworksunderISO9001certification.AtlevelIIofthequalificationofapHmeter(installationandreleaseforuse)itisrecommendedtocheckallrequirementssetduringtheselectionoftheinstrument,andcalibrationshouldbeperformedbeforeputtingintoservicebyanaccreditedexternalservicesupplier,orinternallybyappropriatelyqualifiedpersonnel,usingcertifiedreferencebuffersaccordingtoanapprovedprocedure.在pH计第I级确认(仪器和供应商选择)中，建议选择可以满足化验室需求的pH计生产商，并且在ISO9001认证体系下运行。在pH计第II级确认(安装和放行使用)中，建议检查所有仪器选择中设定的要求，在由经过认证的外部服务商提供服务，或者由内部具备适当资质的人员接手管理之前要进行校正。校正要使用经过认证的标准缓冲液根据批准的程序进行。MANAGEMENTOFELECTRODES电极管理Beforemeasurement,theelectrode(s)is(are)checkedvisually.Theelectrodesshouldbeappropriatelystoredaccordingtorecommendationsofthemanufacturer(e.g.inastorageelectrolyte).Refillableelectrodesshouldbecheckedtoensurethattheleveloftheinnerelectrolyteissatisfactoryandnobubblesarepresentintheglassbulb.Thediaphragmofthereferenceelectrodeshouldalsobechecked.Beforefirstuse,orifithasbeenstoredoutofelectrolyte,itisusuallynecessarytoconditiontheelectrodeaccordingtotherecommendationofthemanufacturer.在开始测量之前，要对电极进行目视检查。电极应根据生产商的建议适当存贮(例如，放在电解液中)。可以重装的电极应进行检查，以保证内部电解液液面高满足要求，在玻璃泡里没有气泡。参比电极的隔层也要进行检查，。在首次使用之前，或者如果已经脱离电解液存贮了很久，通常需要根据生产商的建议调整电极。IfthestabilisationofpHistooslow(longresponsetime)oriftherearedifficultiesincalibration,theelectrodewillprobablyneedtobecleanedorreplaced.Cleaningproceduredependsonthetypeofsampleusedasprescribedinthemanual.Regularcleaningisrecommended.如果pH值稳定过程太慢(响应时间太长)，或者难以校正，则电极可能需要进行清洁或替换。清洁程序取决于手册中所述的受测样品类型。建议定期进行清洁。CALIBRATIONANDMEASUREMENTCONDITIONS校正和测量调整Thecalibrationconsistsofthedeterminationoftheslopeandtheoffsetofthemeasuringsystem.校正包括测定斜率和测量系统补偿。Unlessotherwiseprescribedinthemethod,allmeasurementsareperformedatthesametemperature(±2.5°C)usuallybetween20and25°C.ThevariationofpHwithrespecttotemperatureofanumberofreferencebuffersolutionsusedforcalibrationisgiveninPh.Eur.Chapter2.2.3..Forthetemperaturecorrection,whennecessary,followthemanufacturer'sinstructions.TheapparatusisusuallycalibratedwithtwobuffersolutionswhichshouldbechosensothattheexpectedpHvalueofthetestsampleliesinbetweenthepHvaluesofthebuffersolutions.Therangeshouldbeatleast2pHunits.ThepHofathirdbuffersolutionofintermediatepHreadoffonthescalemustnotdifferbymorethan0.05pHunitsfromthevaluecorrespondingtothissolution.Ifthedeviationisgreaterthan+/-0.05units,thismaybebecausetherangeofthebufferschosenwastoobroadandrecalibrationwithadifferentsystemofbuffersmaybenecessary.除方法中另有要求外，所有测量均应在相同温度（士2.5°C）下进行，通常是20到25°C。在欧洲药典第2.2.3章中给出了校正所用的一系列标准缓冲液的pH值在不同温度下的波动值。必要时，要根据生产商的指导进行温度修正。仪器通常采用2个缓冲液进行校正，受测样品的预计pH值应该落在这2个缓冲液pH值之间。2个缓冲液pH值所覆盖范围至少为2个pH单位。用于中间pH值读数的第3个缓冲液的pH值必须与受测样品的读数值相关不超过0.05。如果偏差大于+/—0.05单位，则可能是因为所选的缓冲液的范围太宽，可能需要采用另一个缓冲液系统重新校正。Alternatively,amulti-pointcalibrationmaybeperformedtocoverawiderpH-range.InthatcaseitmaybenecessarytousemorethanonebuffersolutionfortheverificationdependingontheexpectedpHvaluesofthetestsamples.也可以采用多点校正来覆盖更宽的pH范围。在这种情况下，根据受测样品的预期pH值，可能有必要使用多于1种缓冲液来核对。Thereferencebuffersolutionsshouldpreferablybecertifiedreferencematerials.Otherwise,buffersolutionsmaybepreparedasgiveninPh.Eur.Chapter2.2.3.Theseshouldbetraceabletoprimarystandards.参照缓冲液最好是经过认证的对照材料。也可以根据EP第2.2.3章中给出的方法来配制缓冲液。这时应能追溯到基准对照物。Immersetheelectrodesinthesolutiontobeexaminedandtakethereadinginthesameconditionsasforthebuffersolutions.将电极浸在被测溶液中，在和缓冲液相同的条件下读数。Regularcalibrationshavetobeperformedasgiveninparagraph6.必须根据第6段中给出的方法进行日常校正。Allsolutionstobeexaminedandthereferencebuffersolutionsmustbepreparedusingcarbondioxide-freewaterR.所有溶液都要检查，标准缓冲液必须使用无二氧化碳的试剂用水来配制。STORAGEofbuffersolutions缓冲溶液的存贮Storebuffersolutionsinsuitablechemicallyresistant,tightcontainers,suchastypeIglassbottlesorplasticcontainerssuitableforaqueoussolutions.Buffersolutionsmadeinhouse-shouldnotbekeptformorethan3monthsatroomtemperature.Forcommerciallyavailablebuffersolutions,manufacturers'recommendationsshouldbetakenintoaccount.将缓冲液存贮在适当的耐化学腐蚀的密闭容器中，例如I类玻璃瓶，或适合水性溶液的塑料容器。公司内部配制的缓冲液在室温下保存时间不应超过3个月。市售缓冲液，要考虑生产商的建议。LEVELIIIANDIVQUALIFICATIONOFPHMETERSpH计的