儀器本身性能帶來的誤差
1 複色光對比耳定律的偏離
bierdinglvchenglideqiantitiaojianshirusheguangshidanseguang,danshijingduzaigaodeyiqi,jishishishuangdanseqidefenguangguangduji,yezhinenghuodejinhudansedeguang,wufahuodechundanseguang,tarengranhanyouxiazhaiguangtongdai,juyoufuseguangdexingzhi。erfuseguanghuidaozhibierdinglvdezhenghuofupianli。gudingxiafengdeziwaifenguangguangdujiguangpudaikuanyibanwei1nm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、jianceqilingmindudoujiaodi,zasanguangdeyingxianggengweixianzhu。zasanguangxianzhiyiqidefenxishangxiankeyinqiyanzhongdeceliangwucha,shijigongzuozhong,zaidingliangfenxishi,yibanzaixishoufenghuoqifujinchuceliangyangpinxiguangdu,ruguozaifenxibochangchuhanyouzasanguang,zheshiyangpindetouguanglvjiaoxiao,erzasanguangdabufentouguo,shiceliangxiguangdudiyuzhenshixiguangdu。
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 波長和吸光度準確度
yangpindemeiyigezhidoushizaiyidingdebochangxiacedede,ruguobochangwuchahenda,cechudezhikendingbuzhun。xiguangduzhunqueduyeshiyonghuduiyiqidezhijieyaoqiu,gengyingyinqizugoudezhongshi。guojiajiliangjiandingguichengguidingshuangguangshuziwaikejianfenguangguangdujitoushebizhunqueduweiA級±0.6%, B級±1.0%。
測量條件的選擇
1 參比溶液和溶劑的選擇
fenguangguangdujideceliangshijishangshiyitongguocanbichideguangqiangduzuoweirusheguangqiangdulaicedingshiyangdexiguangdu,xiantiaojieyiqishitouguocanbichirongyedexiguangduweiling,ranhourangtongyishuguangtongguoyangpin,shidexiguangdubijiaozhenshidifanyingdaicewuzhidenongdu,suoyicanbirongyedexuanzefeichangzhongyao。ruguojinyoudaicewuzhiyuxiansejidefanyingchanwuyouxishou,keyongchunrongjihuozhengliushuizuocanbirongye。ruguoxiansejiyouyanse,bingzaicedingbochangxiayouxishou,zeyongxiansejirongyezuocanbirongye,suojiarenxiansejijiqitashijideliang,yushiyangzhongdejiaruliangyingyizhi。ruguoyangpinzhongqitazufenbenshendeyanseduicedingyouganrao,ersuoyongxiansejimeiyanse,zeyongbujiaxiansejideyangpinrongyezuocanbiye。
正確選擇合適的溶劑,對提高分析的準確度起重要作用。為減小溶劑中雜質的影響,應選擇高純度的溶劑;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 測試波長的選擇
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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