分(fen)光(guang)光(guang)度(du)計(ji)是(shi)利(li)用(yong)物(wu)質(zhi)對(dui)光(guang)的(de)選(xuan)擇(ze)性(xing)吸(xi)收(shou)的(de)特(te)性(xing),以(yi)較(jiao)純(chun)的(de)單(dan)色(se)光(guang)作(zuo)為(wei)入(ru)射(she)光(guang),測(ce)定(ding)物(wu)質(zhi)對(dui)光(guang)的(de)吸(xi)收(shou),從(cong)而(er)對(dui)物(wu)質(zhi)進(jin)行(xing)定(ding)性(xing)或(huo)定(ding)量(liang)分(fen)析(xi)的(de)儀(yi)器(qi)。在(zai)使(shi)用(yong)過(guo)程(cheng)中(zhong)常(chang)常(chang)會(hui)出(chu)現(xian)測(ce)量(liang)誤(wu)差(cha),這(zhe)些(xie)誤(wu)差(cha)又(you)是(shi)如(ru)何(he)產(chan)生(sheng)的(de)呢(ne)?
儀器本身性能帶來的誤差
1 fuseguangduibierdinglvdepianlibierdinglvchenglideqiantitiaojianshirusheguangshidanseguang,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,shenzhishijinami。guangpudaikuanyinggaishiyuexiaoyuehao,danshisuizheguangpufenbianlvdetigao,yiqidelingmindujiangdi,suoyixuanzeyiqishiyaozonghekaolvgezhongtiaojiandeyingxiang。dangrongyenongdujiaoxiaoqiedanseguangjiaochunshi,kejinsirenweifuhebierdinglv。
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 bochanghexiguangduzhunqueduyangpindemeiyigezhidoushizaiyidingdebochangxiacedede,ruguobochangwuchahenda,cechudezhikendingbuzhun。xiguangduzhunqueduyeshiyonghuduiyiqidezhijieyaoqiu,gengyingyinqizugoudezhongshi。guojiajiliangjiandingguichengguidingshuangguangshuziwaikejianfenguangguangdujitoushebizhunqueduweiA級±0.6%, B級±1.0%。
測量條件的選擇
1 參(can)比(bi)溶(rong)液(ye)和(he)溶(rong)劑(ji)的(de)選(xuan)擇(ze)分(fen)光(guang)光(guang)度(du)計(ji)的(de)測(ce)量(liang)實(shi)際(ji)上(shang)是(shi)以(yi)通(tong)過(guo)參(can)比(bi)池(chi)的(de)光(guang)強(qiang)度(du)作(zuo)為(wei)入(ru)射(she)光(guang)強(qiang)度(du)來(lai)測(ce)定(ding)試(shi)樣(yang)的(de)吸(xi)光(guang)度(du),先(xian)調(tiao)節(jie)儀(yi)器(qi)使(shi)透(tou)過(guo)參(can)比(bi)池(chi)溶(rong)液(ye)的(de)吸(xi)光(guang)度(du)為(wei)零(ling),然(ran)後(hou)讓(rang)同(tong)一(yi)束(shu)光(guang)通(tong)過(guo)樣(yang)品(pin),使(shi)得(de)吸(xi)光(guang)度(du)比(bi)較(jiao)真(zhen)實(shi)地(di)反(fan)映(ying)待(dai)測(ce)物(wu)質(zhi)的(de)濃(nong)度(du),所(suo)以(yi)參(can)比(bi)溶(rong)液(ye)的(de)選(xuan)擇(ze)非(fei)常(chang)重(zhong)要(yao)。如(ru)果(guo)僅(jin)有(you)待(dai)測(ce)物(wu)質(zhi)與(yu)顯(xian)色(se)劑(ji)的(de)反(fan)應(ying)產(chan)物(wu)有(you)吸(xi)收(shou),可(ke)用(yong)純(chun)溶(rong)劑(ji)或(huo)蒸(zheng)餾(liu)水(shui)作(zuo)參(can)比(bi)溶(rong)液(ye)。如(ru)果(guo)顯(xian)色(se)劑(ji)有(you)顏(yan)色(se),並(bing)在(zai)測(ce)定(ding)波(bo)長(chang)下(xia)有(you)吸(xi)收(shou),則(ze)用(yong)顯(xian)色(se)劑(ji)溶(rong)液(ye)作(zuo)參(can)比(bi)溶(rong)液(ye),所(suo)加(jia)人(ren)顯(xian)色(se)劑(ji)及(ji)其(qi)它(ta)試(shi)劑(ji)的(de)量(liang),與(yu)試(shi)樣(yang)中(zhong)的(de)加(jia)入(ru)量(liang)應(ying)一(yi)致(zhi)。如(ru)果(guo)樣(yang)品(pin)中(zhong)其(qi)它(ta)組(zu)分(fen)本(ben)身(shen)的(de)顏(yan)色(se)對(dui)測(ce)定(ding)有(you)幹(gan)擾(rao),而(er)所(suo)用(yong)顯(xian)色(se)劑(ji)沒(mei)顏(yan)色(se),則(ze)用(yong)不(bu)加(jia)顯(xian)色(se)劑(ji)的(de)樣(yang)品(pin)溶(rong)液(ye)作(zuo)參(can)比(bi)液(ye)。正(zheng)確(que)選(xuan)擇(ze)合(he)適(shi)的(de)溶(rong)劑(ji),對(dui)提(ti)高(gao)分(fen)析(xi)的(de)準(zhun)確(que)度(du)起(qi)重(zhong)要(yao)作(zuo)用(yong)。為(wei)減(jian)小(xiao)溶(rong)劑(ji)中(zhong)雜(za)質(zhi)的(de)影(ying)響(xiang),應(ying)選(xuan)擇(ze)高(gao)純(chun)度(du)的(de)溶(rong)劑(ji);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 ceshibochangdexuanzedangyongfenguangguangdujiduirongyejinxingcedingshi,shouxianxuyaoxuanzeheshideceliangbochang。xuanzedeyijushigaibeicerongyedexishouquxian。zaiyibanqingkuangxia,womenzongshixuanzezuidaxishoubochangzuoweiceliangbochang,zheyangkeyitigaolingmindu。erzaiyouxieqingkuangxiazuidaxishoufenghenjianrui、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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