fenguangguangdujishiliyongwuzhiduiguangdexuanzexingxishoudetexing,yijiaochundedanseguangzuoweirusheguang,cedingwuzhiduiguangdexishou,congerduiwuzhijinxingdingxinghuodingliangfenxideyiqi。zaishiyongguochengzhongchangchanghuichuxianceliangwucha,zhexiewuchayoushiruhechanshengdene?
儀器本身性能帶來的誤差
1 複fu色se光guang對dui比bi耳er定ding律lv的de偏pian離li比bi耳er定ding律lv成cheng立li的de前qian提ti條tiao件jian是shi入ru射she光guang是shi單dan色se光guang,但dan是shi精jing度du再zai高gao的de儀yi器qi,即ji使shi是shi雙shuang單dan色se器qi的de分fen光guang光guang度du計ji,也ye隻zhi能neng獲huo得de近jin乎hu單dan色se的de光guang,無wu法fa獲huo得de純chun單dan色se光guang,它ta仍reng然ran含han有you狹xia窄zhai光guang通tong帶dai,具ju有you複fu色se光guang的de性xing質zhi。而er複fu色se光guang會hui導dao致zhi比bi耳er定ding律lv的de正zheng或huo負fu偏pian離li。固gu定ding狹xia縫feng的de紫zi外wai分fen光guang光guang度du計ji光guang譜pu帶dai寬kuan一yi般ban為wei1nm或2nm,可調狹縫的可以做到0.1nm;可見分光光度計帶寬6nm、snm,甚(shen)至(zhi)十(shi)幾(ji)納(na)米(mi)。光(guang)譜(pu)帶(dai)寬(kuan)應(ying)該(gai)是(shi)越(yue)小(xiao)越(yue)好(hao),但(dan)是(shi)隨(sui)著(zhe)光(guang)譜(pu)分(fen)辨(bian)率(lv)的(de)提(ti)高(gao),儀(yi)器(qi)的(de)靈(ling)敏(min)度(du)降(jiang)低(di),所(suo)以(yi)選(xuan)擇(ze)儀(yi)器(qi)時(shi)要(yao)綜(zong)合(he)考(kao)慮(lv)各(ge)種(zhong)條(tiao)件(jian)的(de)影(ying)響(xiang)。當(dang)溶(rong)液(ye)濃(nong)度(du)較(jiao)小(xiao)且(qie)單(dan)色(se)光(guang)較(jiao)純(chun)時(shi),可(ke)近(jin)似(si)認(ren)為(wei)符(fu)合(he)比(bi)耳(er)定(ding)律(lv)。
2 雜散光的影響雜散光是指進入檢測器的處於待測波長光譜帶寬範圍外的其他波長組分,它是光譜測量中誤差的主要來源。產生原因有:分光光度計的色散元件、反射鏡、透鏡及單色器內壁灰塵等。在分光光度計工作波段邊緣波長處,由於單色器透光率、光源輻射強度、檢(jian)測(ce)器(qi)靈(ling)敏(min)度(du)都(dou)較(jiao)低(di),雜(za)散(san)光(guang)的(de)影(ying)響(xiang)更(geng)為(wei)顯(xian)著(zhu)。雜(za)散(san)光(guang)限(xian)製(zhi)儀(yi)器(qi)的(de)分(fen)析(xi)上(shang)限(xian)可(ke)引(yin)起(qi)嚴(yan)重(zhong)的(de)測(ce)量(liang)誤(wu)差(cha),實(shi)際(ji)工(gong)作(zuo)中(zhong),在(zai)定(ding)量(liang)分(fen)析(xi)時(shi),一(yi)般(ban)在(zai)吸(xi)收(shou)峰(feng)或(huo)其(qi)附(fu)近(jin)處(chu)測(ce)量(liang)樣(yang)品(pin)吸(xi)光(guang)度(du),如(ru)果(guo)在(zai)分(fen)析(xi)波(bo)長(chang)處(chu)含(han)有(you)雜(za)散(san)光(guang),這(zhe)時(shi)樣(yang)品(pin)的(de)透(tou)光(guang)率(lv)較(jiao)小(xiao),而(er)雜(za)散(san)光(guang)大(da)部(bu)分(fen)透(tou)過(guo),使(shi)測(ce)量(liang)吸(xi)光(guang)度(du)低(di)於(yu)真(zhen)實(shi)吸(xi)光(guang)度(du)。
3 儀器噪聲對測t的影響儀器噪聲也是儀器的一個重要指標,它表征儀器做稀溶液的能力。是疊加在待測量的分析信號中的不需要的信號,掃描100%T和0%T線,可觀察到分光光度計的絕對噪聲水平,如果儀器噪聲較大,會掩蓋較小的測量信號,一般用噪音的二倍來表示儀器的靈敏度。
4 波bo長chang和he吸xi光guang度du準zhun確que度du樣yang品pin的de每mei一yi個ge值zhi都dou是shi在zai一yi定ding的de波bo長chang下xia測ce得de的de,如ru果guo波bo長chang誤wu差cha很hen大da,測ce出chu的de值zhi肯ken定ding不bu準zhun。吸xi光guang度du準zhun確que度du也ye是shi用yong戶hu對dui儀yi器qi的de直zhi接jie要yao求qiu,更geng應ying引yin起qi足zu夠gou的de重zhong視shi。國guo家jia計ji量liang檢jian定ding規gui程cheng規gui定ding雙shuang光guang束shu紫zi外wai可ke見jian分fen光guang光guang度du計ji透tou射she比bi準zhun確que度du為weiA級±0.6%, B級±1.0%。
測量條件的選擇
1 canbirongyeherongjidexuanzefenguangguangdujideceliangshijishangshiyitongguocanbichideguangqiangduzuoweirusheguangqiangdulaicedingshiyangdexiguangdu,xiantiaojieyiqishitouguocanbichirongyedexiguangduweiling,ranhourangtongyishuguangtongguoyangpin,shidexiguangdubijiaozhenshidifanyingdaicewuzhidenongdu,suoyicanbirongyedexuanzefeichangzhongyao。ruguojinyoudaicewuzhiyuxiansejidefanyingchanwuyouxishou,keyongchunrongjihuozhengliushuizuocanbirongye。ruguoxiansejiyouyanse,bingzaicedingbochangxiayouxishou,zeyongxiansejirongyezuocanbirongye,suojiarenxiansejijiqitashijideliang,yushiyangzhongdejiaruliangyingyizhi。ruguoyangpinzhongqitazufenbenshendeyanseduicedingyouganrao,ersuoyongxiansejimeiyanse,zeyongbujiaxiansejideyangpinrongyezuocanbiye。zhengquexuanzeheshiderongji,duitigaofenxidezhunqueduqizhongyaozuoyong。weijianxiaorongjizhongzazhideyingxiang,yingxuanzegaochunduderongji;溶劑應不與待測物質發生化學反應;待測物在溶劑中要有一定的溶解度;在測定的波長範圍內,溶劑本身沒有吸收,注意常用溶劑的最短可用波長;當用揮發性大的溶劑時,測量過程中吸收池應加蓋。
2 測ce試shi波bo長chang的de選xuan擇ze當dang用yong分fen光guang光guang度du計ji對dui溶rong液ye進jin行xing測ce定ding時shi,首shou先xian需xu要yao選xuan擇ze合he適shi的de測ce量liang波bo長chang。選xuan擇ze的de依yi據ju是shi該gai被bei測ce溶rong液ye的de吸xi收shou曲qu線xian。在zai一yi般ban情qing況kuang下xia,我wo們men總zong是shi選xuan擇ze最zui大da吸xi收shou波bo長chang作zuo為wei測ce量liang波bo長chang,這zhe樣yang可ke以yi提ti高gao靈ling敏min度du。而er在zai有you些xie情qing況kuang下xia最zui大da吸xi收shou峰feng很hen尖jian銳rui、吸收過大或附近有幹擾存在,就不能選最大吸收波長,而必須在保證有一定靈敏度的情況下,選擇吸收曲線中的其它波長進行測定(曲線較平坦處對應的波長),以消除幹擾。繪製吸收曲線是正確選擇波長的有效手段和方法。
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