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石墨爐的升(sheng)溫(wen)模式
  • 發布日期:2023-05-08      瀏覽次數:217
    • 商(shang)品馬斯曼爐(lu)是通過分(fen)步(bu)升溫(wen)(wen)使(shi)石墨(mo)管到(dao)達原子化溫(wen)(wen)度(du),升溫(wen)(wen)模式(shi)是指由溫(wen)(wen)度(du)T1升至T2所用的途徑或方(fang)式(shi),而這(zhe)些升溫(wen)(wen)模式(shi)又要符合石墨(mo)爐(lu)原子吸(xi)收(shou)分(fen)析(xi)法的要求。現分(fen)述如下(xia)。

      1.斜坡(po)升(sheng)溫與階梯升(sheng)溫

      斜坡升(sheng)溫(wen)是(shi)指施加于石墨(mo)管兩(liang)端的電(dian)流(liu)電(dian)壓或(huo)功率的大小隨(sui)(sui)時(shi)(shi)間(jian)線性上升(sheng),且由(you)兩(liang)個參數(shu)(shu)(shu)決定,一是(shi)由(you)起(qi)始溫(wen)度T1和(he)(he)要求達到的T2,二是(shi)由(you)T1到達T2所需(xu)(xu)的時(shi)(shi)間(jian)△t。一旦這兩(liang)個參數(shu)(shu)(shu)選定,升(sheng)溫(wen)速率dT/dt也就確(que)定了,dT/dt在數(shu)(shu)(shu)學上稱斜率。在△T不(bu)變的情(qing)況下,隨(sui)(sui)著所需(xu)(xu)的時(shi)(shi)間(jian)△t的增加dT/dt變小,即升(sheng)溫(wen)變得(de)平緩(huan)(huan);而所需(xu)(xu)的時(shi)(shi)間(jian)△t不(bu)變時(shi)(shi),△T減小將使(shi)dT/dt變小,升(sheng)溫(wen)亦變得(de)平緩(huan)(huan)。不(bu)同升(sheng)溫(wen)方式(shi)的效果(guo)是(shi)不(bu)同的,因為它(ta)與樣品的性質和(he)(he)數(shu)(shu)(shu)量有關(guan)。

      斜(xie)坡(po)升(sheng)溫(wen)有(you)以下優(you)點:①避免干燥階段中樣品(pin)的(de)(de)濺(jian)散(san);②能有(you)效地(di)消除(chu)分子(zi)(zi)吸(xi)收的(de)(de)影響,較(jiao)好(hao)地(di)符合基體(ti)中每一(yi)組分的(de)(de)蒸發溫(wen)度,③可(ke)以使一(yi)些用快速升(sheng)溫(wen)不(bu)能測(ce)(ce)(ce)(ce)定的(de)(de)元(yuan)素(su)被(bei)檢測(ce)(ce)(ce)(ce)出(chu)來。例如(ru)在大(da)量(liang)銅中測(ce)(ce)(ce)(ce)定鎘。快速升(sheng)溫(wen)由(you)于大(da)量(liang)銅的(de)(de)分子(zi)(zi)吸(xi)收覆(fu)蓋了微量(liang)鎘的(de)(de)信(xin)號,不(bu)能測(ce)(ce)(ce)(ce)定鎘;但在斜(xie)坡(po)升(sheng)溫(wen)時,鎘可(ke)被(bei)檢測(ce)(ce)(ce)(ce)出(chu)來。

      斜(xie)坡升(sheng)溫(wen)方式的(de)是(shi)使(shi)石墨管緩慢平穩地逐(zhu)漸上升(sheng)到所要求(qiu)的(de)溫(wen)度(du),對多組分復雜基體(ti)物質(zhi)的(de)蒸發(fa)分離除去十分有效。

      斜(xie)坡(po)升溫(wen)程(cheng)序可由一個或多個斜(xie)坡(po)升溫(wen)過(guo)程(cheng)及過(guo)程(cheng)之間的(de)溫(wen)度保持階段組成(cheng)的(de),是石(shi)墨(mo)爐原子化器的(de)一種升溫(wen)程(cheng)序。

      階梯升(sheng)(sheng)(sheng)溫(wen)(wen)(wen)(wen)又(you)稱脈(mo)沖(chong)升(sheng)(sheng)(sheng)溫(wen)(wen)(wen)(wen),與斜坡升(sheng)(sheng)(sheng)溫(wen)(wen)(wen)(wen)方式比較(jiao),由(you)起(qi)始溫(wen)(wen)(wen)(wen)度(du)T1和(he)要求達到的溫(wen)(wen)(wen)(wen)度(du)T2的時間(jian)△t,從理論上(shang)講(jiang)為(wei)零,實際△t不(bu)可能為(wei)零與斜坡升(sheng)(sheng)(sheng)溫(wen)(wen)(wen)(wen)相比是(shi)陡然(ran)升(sheng)(sheng)(sheng)溫(wen)(wen)(wen)(wen),易引起(qi)石墨(mo)管中(zhong)樣(yang)品(pin)的飛濺,優點是(shi)升(sheng)(sheng)(sheng)溫(wen)(wen)(wen)(wen)速度(du)快。階梯升(sheng)(sheng)(sheng)溫(wen)(wen)(wen)(wen)程(cheng)序由(you)多個階梯升(sheng)(sheng)(sheng)溫(wen)(wen)(wen)(wen)過(guo)程(cheng)及過(guo)程(cheng)之間(jian)的溫(wen)(wen)(wen)(wen)度(du)保(bao)持階段(duan)組成,主要用在灰化階段(duan),使(shi)用時應充(chong)分(fen)考慮(lv)樣(yang)品(pin)的狀態,溶劑是(shi)否已除盡。否則,會使(shi)樣(yang)品(pin)造成飛濺。

      2.大(da)功率升(sheng)溫(wen)(快速升(sheng)溫(wen))

      早期(qi)的(de)(de)石(shi)(shi)(shi)(shi)墨(mo)(mo)爐(lu)(lu)電(dian)(dian)(dian)源加熱(re)(re)(re)石(shi)(shi)(shi)(shi)墨(mo)(mo)管(guan)時(shi),施加于(yu)石(shi)(shi)(shi)(shi)墨(mo)(mo)管(guan)的(de)(de)功(gong)(gong)(gong)率是依據達到平(ping)衡以后的(de)(de)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)度(du)(du)(du)(du)來(lai)確定(ding)(ding)的(de)(de),即升(sheng)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)速(su)(su)率實際上(shang)與設(she)定(ding)(ding)的(de)(de)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)度(du)(du)(du)(du)有(you)關(guan),這(zhe)就造成了(le)石(shi)(shi)(shi)(shi)墨(mo)(mo)管(guan)的(de)(de)時(shi)間(jian)(jian)不等溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)性(xing)。后來(lai)的(de)(de)石(shi)(shi)(shi)(shi)墨(mo)(mo)爐(lu)(lu)電(dian)(dian)(dian)源改進了(le)設(she)計,將維(wei)持原(yuan)子(zi)(zi)化(hua)(hua)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)度(du)(du)(du)(du)和(he)(he)加熱(re)(re)(re)石(shi)(shi)(shi)(shi)墨(mo)(mo)管(guan)兩個功(gong)(gong)(gong)能分(fen)開,石(shi)(shi)(shi)(shi)墨(mo)(mo)管(guan)的(de)(de)升(sheng)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)速(su)(su)率只取決于(yu)初始(shi)的(de)(de)加熱(re)(re)(re)功(gong)(gong)(gong)率,而與原(yuan)子(zi)(zi)化(hua)(hua)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)度(du)(du)(du)(du)無(wu)關(guan)。在電(dian)(dian)(dian)路上(shang)用(yong)(yong)一(yi)個大(da)(da)功(gong)(gong)(gong)率可控(kong)硅(gui)將二者分(fen)開,通(tong)電(dian)(dian)(dian)開始(shi)可控(kong)硅(gui)全(quan)(quan)(quan)導(dao)通(tong),電(dian)(dian)(dian)源的(de)(de)最大(da)(da)電(dian)(dian)(dian)流加于(yu)石(shi)(shi)(shi)(shi)墨(mo)(mo)管(guan)上(shang)使之急速(su)(su)升(sheng)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen),若(ruo)用(yong)(yong)時(shi)間(jian)(jian)控(kong)制(zhi)的(de)(de)可控(kong)硅(gui)全(quan)(quan)(quan)導(dao)通(tong)時(shi)間(jian)(jian)△t后,其(qi)導(dao)通(tong)角立即被關(guan)小至預(yu)先(xian)設(she)定(ding)(ding)的(de)(de)原(yuan)子(zi)(zi)化(hua)(hua)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)度(du)(du)(du)(du)的(de)(de)位(wei)置。石(shi)(shi)(shi)(shi)墨(mo)(mo)管(guan)由較(jiao)(jiao)高(gao)(gao)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)度(du)(du)(du)(du)降至原(yuan)子(zi)(zi)化(hua)(hua)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)度(du)(du)(du)(du)并(bing)維(wei)持此即最大(da)(da)功(gong)(gong)(gong)率升(sheng)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)方式。若(ruo)采(cai)用(yong)(yong)光學元(yuan)件測定(ding)(ding)并(bing)控(kong)制(zhi)石(shi)(shi)(shi)(shi)墨(mo)(mo)管(guan)的(de)(de)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)度(du)(du)(du)(du),可控(kong)硅(gui)全(quan)(quan)(quan)導(dao)通(tong)升(sheng)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)至設(she)定(ding)(ding)的(de)(de)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)度(du)(du)(du)(du),其(qi)導(dao)通(tong)角立即被關(guan)小并(bing)維(wei)持;20世(shi)紀80年代前后,具(ju)有(you)最大(da)(da)功(gong)(gong)(gong)率升(sheng)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)功(gong)(gong)(gong)能的(de)(de)石(shi)(shi)(shi)(shi)墨(mo)(mo)爐(lu)(lu)電(dian)(dian)(dian)源商(shang)品問(wen)世(shi),隨后又出現了(le)具(ju)有(you)光控(kong)最大(da)(da)功(gong)(gong)(gong)率升(sheng)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)的(de)(de)石(shi)(shi)(shi)(shi)墨(mo)(mo)爐(lu)(lu)電(dian)(dian)(dian)源;到了(le)20世(shi)紀80年代后期(qi),幾(ji)乎所有(you)的(de)(de)商(shang)品石(shi)(shi)(shi)(shi)墨(mo)(mo)爐(lu)(lu)儀(yi)器都具(ju)有(you)了(le)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)度(du)(du)(du)(du)控(kong)制(zhi)系(xi)統,使在原(yuan)子(zi)(zi)化(hua)(hua)過程中石(shi)(shi)(shi)(shi)墨(mo)(mo)管(guan)的(de)(de)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)度(du)(du)(du)(du)環(huan)境(jing)有(you)了(le)較(jiao)(jiao)大(da)(da)的(de)(de)改善,為(wei)石(shi)(shi)(shi)(shi)墨(mo)(mo)爐(lu)(lu)原(yuan)子(zi)(zi)吸收分(fen)析(xi)法的(de)(de)應用(yong)(yong)和(he)(he)發展提供了(le)有(you)利的(de)(de)條件。通(tong)過50多(duo)(duo)個元(yuan)素(su)的(de)(de)分(fen)析(xi)比較(jiao)(jiao)得(de)出結(jie)論:使用(yong)(yong)最大(da)(da)功(gong)(gong)(gong)率升(sheng)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)工作模(mo)式,能提高(gao)(gao)難熔元(yuan)素(su)的(de)(de)峰高(gao)(gao)測量(liang)的(de)(de)靈敏度(du)(du)(du)(du),對(dui)熱(re)(re)(re)解(jie)石(shi)(shi)(shi)(shi)墨(mo)(mo)管(guan)效果尤其(qi)明顯;使許多(duo)(duo)元(yuan)素(su)的(de)(de)最佳(jia)原(yuan)子(zi)(zi)化(hua)(hua)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)度(du)(du)(du)(du)降低,延長了(le)石(shi)(shi)(shi)(shi)墨(mo)(mo)管(guan)的(de)(de)壽命和(he)(he)改善了(le)分(fen)析(xi)精密(mi)度(du)(du)(du)(du)。光控(kong)最大(da)(da)功(gong)(gong)(gong)率升(sheng)溫(wen)(wen)(wen)(wen)(wen)(wen)(wen)技(ji)術將使這(zhe)些長處得(de)以充分(fen)發揮。

      快(kuai)速升(sheng)(sheng)溫(wen)(wen)(wen)的(de)(de)升(sheng)(sheng)溫(wen)(wen)(wen)速率可達(da)2000℃/s以(yi)上。在(zai)原(yuan)子(zi)(zi)化階段(duan),采用(yong)(yong)快(kuai)速升(sheng)(sheng)溫(wen)(wen)(wen)往往能使待(dai)測元(yuan)(yuan)素(su)在(zai)極短的(de)(de)時(shi)間內實(shi)現(xian)原(yuan)子(zi)(zi)化,以(yi)獲得更高(gao)的(de)(de)瞬時(shi)峰(feng)值吸(xi)收信(xin)號。這(zhe)種升(sheng)(sheng)溫(wen)(wen)(wen)方(fang)式使用(yong)(yong)的(de)(de)有效原(yuan)子(zi)(zi)化溫(wen)(wen)(wen)度較低,可延長石墨管的(de)(de)壽命,對難熔元(yuan)(yuan)素(su)有較高(gao)的(de)(de)靈(ling)敏度,但快(kuai)速升(sheng)(sheng)溫(wen)(wen)(wen)在(zai)干(gan)燥階段(duan)可能使樣(yang)品濺散(san)和(he)在(zai)灰化階段(duan)引起灰化損(sun)失(shi)。


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