分析與條件的影響
理li論lun上shang,任ren何he分fen析xi方fang法fa都dou有you一yi定ding的de誤wu差cha,且qie不bu同tong分fen析xi方fang法fa誤wu差cha存cun在zai較jiao大da的de差cha異yi。在zai化hua學xue分fen析xi中zhong,通tong常chang的de標biao準zhun方fang法fa對dui準zhun確que度du有you一yi定ding的de要yao求qiu,允yun許xu的de誤wu差cha也ye是shi相xiang對dui的de。有you的de檢jian測ce項xiang目mu,由you於yu分fen析xi方fang法fa本ben身shen存cun在zai一yi定ding的de局ju限xian性xing,而er造zao成cheng加jia標biao回hui收shou率lv值zhi偏pian低di或huo偏pian高gao。
如:采cai用yong馬ma弗fu爐lu高gao溫wen灰hui化hua處chu理li樣yang品pin,一yi些xie容rong易yi揮hui發fa的de元yuan素su測ce定ding回hui收shou率lv偏pian低di的de原yuan因yin正zheng是shi由you於yu高gao溫wen使shi待dai測ce元yuan素su揮hui發fa損sun失shi引yin起qi的de。因yin此ci,通tong過guo測ce定ding回hui收shou率lv的de結jie果guo,可ke在zai一yi定ding程cheng度du上shang證zheng明ming方fang法fa的de準zhun確que性xing。
加標量的水平及其準確性的影響
在zai化hua學xue分fen析xi中zhong,由you於yu待dai測ce物wu質zhi都dou是shi在zai一yi定ding的de濃nong度du範fan圍wei內nei才cai具ju有you某mou個ge特te定ding的de準zhun確que度du,超chao出chu該gai範fan圍wei,可ke能neng會hui產chan生sheng較jiao大da的de誤wu差cha。在zai做zuo加jia標biao回hui收shou時shi,當dang樣yang品pin中zhong待dai測ce物wu含han量liang較jiao低di時shi。加jia入ru標biao準zhun物wu質zhi太tai少shao,測ce得de回hui收shou率lv誤wu差cha較jiao大da;加jia入ru標biao準zhun物wu質zhi太tai多duo,則ze會hui改gai變bian待dai測ce物wu質zhi在zai加jia標biao樣yang品pin和he樣yang品pin中zhong的de測ce定ding背bei景jing,也ye可ke能neng會hui產chan生sheng較jiao大da的de誤wu差cha。因yin此ci在zai進jin行xing加jia標biao回hui收shou時shi,加jia標biao量liang的de水shui平ping要yao適shi當dang,太tai高gao或huo太tai低di都dou不bu會hui得de到dao預yu期qi的de效xiao果guo,通tong常chang應ying注zhu意yi以yi下xia兩liang點dian。
一是標準加入的量要明顯高於檢出限,二是要盡量與分析組分的含量一致,但同時考慮又不能超出方法檢測的容許範圍。
例如:在(zai)分(fen)光(guang)光(guang)度(du)分(fen)析(xi)中(zhong),當(dang)樣(yang)品(pin)中(zhong)待(dai)測(ce)物(wu)含(han)量(liang)較(jiao)高(gao)時(shi),加(jia)入(ru)標(biao)準(zhun)物(wu)質(zhi)過(guo)高(gao),使(shi)加(jia)標(biao)後(hou)測(ce)定(ding)值(zhi)接(jie)近(jin)方(fang)法(fa)的(de)檢(jian)出(chu)上(shang)限(xian),這(zhe)樣(yang)測(ce)得(de)加(jia)標(biao)樣(yang)中(zhong)待(dai)測(ce)物(wu)的(de)誤(wu)差(cha)較(jiao)大(da),加(jia)標(biao)後(hou)引(yin)起(qi)的(de)濃(nong)度(du)增(zeng)量(liang)在(zai)方(fang)法(fa)測(ce)定(ding)上(shang)限(xian)濃(nong)度(du)c的0.4~0.6倍之間為宜。
加標體積影響
tongchangqingkuangxia,jinguanyinjiabiaoerzengdaleshiyangtiji,yangpinfenxiguochengzhongyouzhengfahuoxiaojiedengkeshirongyetijisuoxiaodecaozuojishushi,yangpinjingchulihouzhongxindingrongbingbuhuiduifenxijieguochanshengyingxiang。danjiabiaotijiguoda,rongyiyinjiaruguoduorongjiyingxiangjiancejieguo。
如:在zai采cai用yong濃nong酸suan消xiao解jie樣yang品pin時shi。過guo多duo加jia入ru水shui溶rong液ye。使shi酸suan濃nong度du太tai低di,可ke能neng影ying響xiang樣yang品pin效xiao果guo。當dang加jia入ru標biao準zhun物wu質zhi是shi有you機ji溶rong劑ji時shi,加jia標biao量liang過guo多duo,則ze會hui造zao成cheng溶rong劑ji和he標biao準zhun物wu質zhi難nan以yi在zai水shui中zhong溶rong解jie,從cong而er因yin溶rong解jie度du問wen題ti造zao成cheng對dui加jia標biao回hui收shou率lv的de影ying響xiang。
youyujiabiaohuishoulvshiyanxuyaocaozuorenyuanjingguoyixiliecaozuobuzhouwancheng,chulejiabiaodebuzhouwai,qitarenheyuyangpinjianceyouguandecaozuobuzhoudoukenengyingxiangjiabiaoyangpinheyuanyangpinzhongdaicezufendejieguo,suoyi,zhexiecaozuorenyuandeshuipingjunzhijieyingxianghuishoulvdejieguo。
通常情況下,樣品待測組分本底值(原含量)不能過大。樣品本底值太大,加標量無法與之匹配,回收量的相對誤差就大,回收率偏差即大;反之回收率偏差即小。因此,在低濃度區加標回收率要受樣品中本底值的影響更為明顯。
回hui收shou率lv試shi驗yan的de前qian提ti是shi樣yang品pin足zu夠gou均jun勻yun,即ji樣yang品pin及ji加jia標biao樣yang品pin本ben底di值zhi差cha異yi可ke以yi忽hu略lve。反fan之zhi,如ru果guo樣yang品pin均jun勻yun較jiao差cha,樣yang品pin及ji加jia標biao樣yang品pin本ben底di值zhi差cha異yi較jiao大da,加jia標biao樣yang品pin與yu樣yang品pin中zhong待dai測ce物wu質zhi含han量liang的de差cha值zhi將jiang不bu僅jin僅jin是shi加jia標biao物wu質zhi的de測ce定ding值zhi,即ji為wei加jia標biao回hui收shou試shi驗yan采cai用yong的de兩liang份fen待dai測ce定ding樣yang品pin與yu樣yang品pin中zhong待dai測ce物wu質zhi含han量liang的de差cha值zhi及ji加jia標biao物wu質zhi總zong和he的de測ce定ding值zhi。因yin此ci,如ru加jia標biao樣yang中zhong待dai測ce物wu質zhi本ben底di偏pian高gao,回hui收shou率lv將jiang偏pian高gao,反fan之zhi則ze偏pian低di。樣yang品pin間jian差cha異yi過guo大da,將jiang得de到dao錯cuo誤wu的de回hui收shou率lv結jie果guo。
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