HAPSITE-ER-定量方法编辑培训

HAPSITEER/SmartPlusTrainingHAPSITEER/SmartPlus培训AdvancedQuantitativeMethodWriting编辑高级定量方法2Copyright©2009CourseOutline课程概要Introduction前言StandardPreparation标样准备StandardAnalysis标样分析DevelopingtheCalibrationLibrary建立校准曲线库QuantitativeMethodVerification定量方法验证SIMQuantSIM定量3Copyright©2009Introduction前言Aquantitativemethodisusedtocalculateconcentrationsofchemicalsthatarecontainedinthemethodcalibrationlibrary定量方法用于计算包含在方法校准库内的化合物浓度Foreachquantitativemethod:对于每个定量方法:•Determinethechemicalstobeanalyzed确定要分析的化合物•Determinethecalibrationrangeoftheanalytes确定分析的校准范围•Preparestandardsforthecalibrationlibrary为校准库准备标样•UseaHAPSITEERorSmartPlusdefaultmethodasatemplatetocreateaspecificquantitativemethod用HAPSITEER或SmartPlus默认方法作为创建特定定量方法的模板•Createacalibrationlibrary创建校准曲线库•Verifythemethod验证方法校准4Copyright©2009DetermineSamplingMethod确定采样方法Thecalibrationrangemustencompassthehighestacceptablelimit校准范围必须包含可接受的最高限值•Forthisexercise,acalibrationrangeof~1ppmandlowerwillbecreated本例中,将创建~1ppm和较低的校准范围NOTE:Foranaccuratecalibration,aminimumofthreeconcentrationsofthestandardarerecommended注:为精确校准,建议至少三个标准浓度5Copyright©2009DeterminetheBackgroundEnvironment确定本底环境Runablankoutsidetheareaofinterestusing在感兴趣区域外运行空样•ER_Air_Tri-Bed_PPM_StandardfortheER对于ER,用ER_Air_Tri-Bed_PPM_Standard•Air_Tri-Bed_PPM_StandardfortheSmartPlus对于SmartPlus,Air_Tri-Bed_PPM_StandardItisnecessarytoestablishabaselineblankincleanairtodeterminetheenvironmentoutsideofthesamplingarea为确定采样区域外的环境,建立清洁空气中的基线空样是必要的6Copyright©2009StandardPreparation标准准备SyringePreparationforSampling为采样准备取样针SyringeTechniques取样针技术CreatingCalibrationStandards创建校准标准AirSampleConcentrationCalculations空气样品浓度计算7Copyright©2009SyringePreparationforSampling为采样准备取样针Topreparethesyringeforsampling:为采样准备取样针:•Inserttheneedleintoavialofmethanol将针头插入甲醇瓶中•Drawtheplungertothe10µLmarktofillthewithmethanol拉柱塞至10微升标记处,用甲醇注入芯管•Expelthemethanolintoawastevial将甲醇排入废瓶中•Repeatthisprocessthreetimesbeforeandaftersyringeuse在取样针使用前和使用后,重复这个过程三次8Copyright©2009Practicepropersyringetechniqueusingmethanol用甲醇练习正确的取样针技术•Drawthesyringeplungerbacktothe1µlmark抽回针管柱塞至1微升标记处•Insertthetipofthesyringeneedleintothemethanol将针头的针尖插入甲醇中•Becarefulnottomovetheplunger注意不要移动柱塞•Carefullydrawtheplungerbacktothe4.5µlmark小心地将柱塞抽回至4.5微升标记处•Withdrawthesyringefromthevial从样瓶中撤回针管•Becarefulnottomovetheplunger注意不要移动柱塞SyringeTechniques取样针技术9Copyright©2009SyringeTechniques取样针技术•Drawtheplungerbacktothe6µLmark抽回柱塞至6微升标记处•Verifythatthereisa3.5µLplugofliquidbetweenthe1µLand4.5µLmark证实在1微升与4.5微升标记之间有3.5微升液柱•Injectthisliquidintoawastevial将这些液体注入废瓶中•Disregardsmallairpocketsthatmayappearneartheplunger不管柱塞附近可出现的小空气泡•Repeatthissameproceduretopreparethestandard重复同样顺序准备标样10Copyright©2009CreatingCalibrationStandards创建校准标准Forthisexercise,thesamplebeingusedisthe2000µg/mLSpexCertiPrepBTEXStandard本练习中,使用的样品为2000微克/毫升的SpexCertiPrepBTEX标准•Thisstandardisamixtureofbenzene,tolueneethylbenzene,o-xylene,p-xylene(BTEX)这个标准是苯,甲苯,乙苯,邻二甲苯,对二甲苯的混合物(BTEX)11Copyright©2009CreatingCalibrationStandards创建校准标准Preparethesamplesin1LTedlarbagsorequivalent准备样品于1升的Tedlar袋或等效物中•Usinga1LAirSyringe,inject1Lofbackgroundairusedfortheblankintoa1LTedlarbag用1升的空气针管,将1升本底空气用作空样,注入1升的Tedlar袋•Labelthebag“Bag5”将袋标志为“袋5”•Injecttheamountofstandardindicatedbelowintothebag按下表将标准的量注入袋中NOTE:Tosavetimeinclass,chromatographicdatafrompreviousrunsforBags1-4willbeused注:为节省时间,将使用先前运行的袋1-4的色谱数据12Copyright©2009AirSampleConcentrationCalculationsWhentheliquidsampleisinjectedintothebag,theconcentrationofeachchemicalbecomesdependantuponitsmolecularweight•TheIdealGasLawtakesintoconsiderationtheinteractionofaliquidchemicalasitismixedintoagasmatrix•PV=nRTistheIdealGasLaw•P=Pressure(inkPa);standardpressureis101.235kPa•V=Volume(inL)•n=molesoftheanalyte(foundfromitsmolecularweight)•R=GasConstant(8.314(LxkPaxmol-1xK-1))•T=Temperature(inKelvins);standardtemperatureis298.15KTheexamplecalculationforbenzeneinBag5isshownonthenextslide13Copyright©2009空气样品浓度计算当将液体样品注入袋中时,每种化合物的浓度取决于它的分子量•当液体化合物混合入气体混合物时,理想气体定律考虑其相互作用•PV=nRT是理想气体定律•P=压强(仟帕);标准压强为101.235kPa•V=容积(升)•n=分析物的克分子数(从它的分子量得到)•R=气体常数(8.314(升x仟帕x克分子-1xK-1))•T=温度(K);标准温度为298.15K袋5中苯的实例计算示于下页中14Copyright©2009AirSampleConcentrationCalculationsPVbenzene=nRTVbenzene=nRT/PWhere:n=2000µg/mLx2.5µLx1mL/1000µLx1mol/78gx1g/(1x106µg)R=8.314LxkPa/molxKT=298.15KP=1/101.235kPaThen:Vbenzene=0.000001568L=1.568x10-6LOriginalStandardConcentrationAmountofsampleinjectedMolecularweightofbenzene15Copyright©2009空气样品浓度计算PV苯=nRTV苯=nRT/P其中:n=2000微克/毫升x2.5微升x1毫升/1000微升x1克分子/78克x1克/(1x106微克)R=8.314升x仟帕/克分子xKT=298.15KP=1/101.235仟帕于是:V苯=0.000001568升=1.568x10-6升初始标准浓度样品注入量苯的分子量16Copyright©2009AirSampleConcentrationCalculationsDividethevolumeofanalytebythevolumeofairorN2intheTedlarbagtofindtheconcentrationinppmvVBenzene=1.568x10-6L=1.568ppmvVAir1Lppmvstandsforpartspermillionpervolume•Thisisthemeasurementofasampleinpartspermillioninavolumeofagasmatrix17Copyright©2009空气样品浓度计算将分析物的容积除以在Tedlar袋中空气或氮气的容积得到浓度ppmvV苯=1.568x10-6升=1.568ppmvV空气1升ppmv代表百万分之几/容积•这是测量样品在气体基质容积中百万分之几18Copyright©2009AirSampleConcentrationCal