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自動定氮儀實驗中影響結果的因素和解決方法

更新時間:2022-01-17      點擊次數:885
   自動定氮儀適用于(yu)食品(pin)(pin)、飲料(liao)、醫藥、農(nong)林漁業、礦山、化工等(deng)生產企業,以(yi)及高(gao)等(deng)院(yuan)校、科研(yan)院(yuan)所、環境監測(ce)、土肥站、農(nong)機站、質量(liang)監督檢驗等(deng)科研(yan)檢測(ce)單位對食品(pin)(pin)、乳制品(pin)(pin)、天然(ran)橡膠、乳膠、種子、土壤、植株、飼料(liao)、礦石、污泥及化學(xue)沉淀(dian)物等(deng)樣品(pin)(pin)中對蛋(dan)白質含(han)量(liang)的智能(neng)化測(ce)定。
  自動定氮儀實驗中影響結果的因素(su)和解決方法:
  自動(dong)(dong)(dong)定(ding)(ding)氮(dan)(dan)儀(yi)是(shi)根據蛋白質(zhi)中氮(dan)(dan)的含(han)量(liang)恒定(ding)(ding)的原理(li),通過測(ce)定(ding)(ding)樣品中氮(dan)(dan)的含(han)量(liang)從而計算蛋白質(zhi)含(han)量(liang)的儀(yi)器。因其(qi)蛋白質(zhi)含(han)量(liang)測(ce)量(liang)計算的方法叫做自動(dong)(dong)(dong)定(ding)(ding)氮(dan)(dan)法,故被稱為自動(dong)(dong)(dong)定(ding)(ding)氮(dan)(dan)儀(yi),又名(ming)蛋白質(zhi)測(ce)定(ding)(ding)儀(yi)、粗(cu)蛋白測(ce)定(ding)(ding)儀(yi)。一般(ban)分為全自動(dong)(dong)(dong)自動(dong)(dong)(dong)定(ding)(ding)氮(dan)(dan)儀(yi)和自動(dong)(dong)(dong)自動(dong)(dong)(dong)定(ding)(ding)氮(dan)(dan)儀(yi),自動(dong)(dong)(dong)定(ding)(ding)氮(dan)(dan)儀(yi)廣(guang)泛應用于(yu)食品加(jia)工(gong)、谷(gu)物(wu)、飼料、水、土壤、制藥(yao)、環保、畜牧、土肥、環境檢(jian)測(ce)、醫藥(yao)、農藥(yao)、科(ke)研、教學、質(zhi)量(liang)監督等領(ling)域,進行氮(dan)(dan)或者蛋白質(zhi)含(han)量(liang)的測(ce)定(ding)(ding),還可用于(yu)銨鹽(yan)、揮(hui)發性鹽(yan)基氮(dan)(dan)等的檢(jian)測(ce),自動(dong)(dong)(dong)定(ding)(ding)氮(dan)(dan)儀(yi)具有高(gao)靈(ling)敏度,分析速度快(kuai),應用范圍廣(guang),所需(xu)試樣少,設備(bei)和操作比較(jiao)簡(jian)單(dan)等特(te)點(dian)。
  檢測樣品(pin)氮(dan)含量(liang),如果(guo)你選擇(ze)的是(shi)自(zi)(zi)(zi)動(dong)(dong)定氮(dan)儀(yi),那(nei)么(me)第一步(bu)是(shi)消(xiao)解樣品(pin),第二(er)步(bu)是(shi)蒸餾的過程,第三(san)步(bu)是(shi)滴(di)定計算氮(dan)含量(liang)結(jie)果(guo)。不管(guan)自(zi)(zi)(zi)動(dong)(dong)定氮(dan)儀(yi)經歷發展到(dao)什么(me)階(jie)段(duan),只要是(shi)自(zi)(zi)(zi)動(dong)(dong)定氮(dan)法,使用(yong)自(zi)(zi)(zi)動(dong)(dong)定氮(dan)儀(yi)都(dou)必須經過前面提到(dao)的三(san)個步(bu)驟(zou)。影(ying)響回收率的原(yuan)因(yin)必然跟這(zhe)三(san)步(bu)有密切的關系。分析原(yuan)因(yin)如下:
  1.消(xiao)解(jie)過(guo)程(cheng)中,消(xiao)解(jie)儀或者消(xiao)化(hua)爐溫度過(guo)低或者時(shi)間不足,樣(yang)品未*消(xiao)解(jie),或者消(xiao)化(hua)樣(yang)品時(shi)有掛壁(bi)現(xian)象產生。
  2.鹽酸(suan)或(huo)者(zhe)硫酸(suan)標準溶液放置(zhi)時間過(guo)長(chang),造(zao)成溶度不準。(建(jian)議時間不要(yao)(yao)超過(guo)1個月,超過(guo)需要(yao)(yao)重新配置(zhi))
  3.定氮儀蒸餾裝置冷凝管(guan)或防濺(jian)管(guan)有(you)破損,產生的氨氣泄漏。
  4.收集液(硼酸(suan)液)太少,未能沒(mei)過接收管(guan)出(chu)口。
  5.鹽(yan)酸或(huo)者(zhe)硫酸標準(zhun)溶(rong)液濃(nong)度(du)太高(gao)。(手動(dong)滴定(ding)時容易出(chu)現回(hui)收率偏低)
  6.收集氨氣的收集液溫度超過一定溫度時,氨氣容(rong)易(yi)被逃逸。
  7.指示劑沒有避光(guang)保存或者放(fang)置時(shi)間(jian)過長,導致指示劑失效(xiao)。(建議時(shi)間(jian)不要(yao)超過1個月(yue)且須避光(guang)保存,超過需(xu)要(yao)重新配(pei)置)
  消(xiao)(xiao)(xiao)(xiao)(xiao)化(hua)(hua)(hua)(hua)爐(lu)必須要有(you)(you)效(xiao)地溫(wen)(wen)度控(kong)制(zhi),有(you)(you)消(xiao)(xiao)(xiao)(xiao)(xiao)化(hua)(hua)(hua)(hua)爐(lu)程序升溫(wen)(wen)控(kong)制(zhi),就能有(you)(you)效(xiao)滿(man)足樣品(pin)(pin)(pin)的需要,而望(wang)海(hai)紅(hong)外(wai)消(xiao)(xiao)(xiao)(xiao)(xiao)化(hua)(hua)(hua)(hua)爐(lu)是專家經驗算法PID控(kong)溫(wen)(wen),20階(jie)段的程序升溫(wen)(wen),可(ke)根據樣品(pin)(pin)(pin)性(xing)質(zhi)設定分階(jie)段的調節溫(wen)(wen)度高低(di)尤其是可(ke)調升溫(wen)(wen)速率,杜絕(jue)樣品(pin)(pin)(pin)在消(xiao)(xiao)(xiao)(xiao)(xiao)化(hua)(hua)(hua)(hua)過程中的掛壁現象。消(xiao)(xiao)(xiao)(xiao)(xiao)化(hua)(hua)(hua)(hua)爐(lu)孔間溫(wen)(wen)度如果(guo)不均勻,會(hui)使得(de)樣品(pin)(pin)(pin)消(xiao)(xiao)(xiao)(xiao)(xiao)化(hua)(hua)(hua)(hua)有(you)(you)些(xie)*有(you)(you)些(xie)會(hui)沒有(you)(you)消(xiao)(xiao)(xiao)(xiao)(xiao)化(hua)(hua)(hua)(hua)好,而且望(wang)海(hai)紅(hong)外(wai)消(xiao)(xiao)(xiao)(xiao)(xiao)化(hua)(hua)(hua)(hua)爐(lu)能解決一系列(lie)問題,消(xiao)(xiao)(xiao)(xiao)(xiao)化(hua)(hua)(hua)(hua)爐(lu)是通過紅(hong)外(wai)加熱、石英輻射的方(fang)式來加熱的,加熱非(fei)常的均勻。控(kong)溫(wen)(wen)可(ke)控(kong),樣品(pin)(pin)(pin)還原性(xing)好。
  冷(leng)(leng)凝(ning)(ning)管(guan)在(zai)定(ding)(ding)氮儀中是(shi)(shi)一(yi)個很重要的(de)(de)部件,他的(de)(de)冷(leng)(leng)凝(ning)(ning)效(xiao)(xiao)果決定(ding)(ding)了定(ding)(ding)氮儀的(de)(de)品質, 望海的(de)(de)冷(leng)(leng)凝(ning)(ning)管(guan)是(shi)(shi)自有的(de)(de)技術,可(ke)以達到降(jiang)低冷(leng)(leng)凝(ning)(ning)時間,提高冷(leng)(leng)卻液的(de)(de)冷(leng)(leng)卻效(xiao)(xiao)果。
  望(wang)海自動定(ding)氮儀,具有(you)(you)對蒸餾杯的溫度實時檢測(自有(you)(you)技術),集液瓶內溫度過(guo)高儀器(qi)停止蒸餾,溫度下降(jiang)后自動繼續蒸餾剩余時間,確保(bao)氨氣不被逃逸。
  在(zai)做(zuo)樣(yang)品檢測試驗時(shi)(shi),請嚴格(ge)按照(zhao)自動(dong)定(ding)(ding)(ding)氮(dan)儀操(cao)作規程,包括消解時(shi)(shi)的(de)溫度(du)(du)設置,催化(hua)劑的(de)配比規則,消解時(shi)(shi)間(jian)等(deng)等(deng),其次不管是(shi)手(shou)動(dong)滴(di)定(ding)(ding)(ding)的(de)半自動(dong)定(ding)(ding)(ding)氮(dan)儀,還是(shi)自動(dong)滴(di)定(ding)(ding)(ding)打印(yin)計算數據的(de)全自動(dong)自動(dong)定(ding)(ding)(ding)氮(dan)儀,蒸餾時(shi)(shi)堿液必須過(guo)量(liang),*反(fan)應完成,實時(shi)(shi)觀察蒸餾時(shi)(shi)氨氣被收集(ji)的(de)溫度(du)(du),顏色(se)的(de)變化(hua),最后是(shi)滴(di)定(ding)(ding)(ding)時(shi)(shi),標準(zhun)酸濃度(du)(du)的(de)配比,滴(di)定(ding)(ding)(ding)泵前(qian)期的(de)校準(zhun),如果是(shi)手(shou)動(dong)滴(di)定(ding)(ding)(ding)時(shi)(shi)注(zhu)意搖(yao)晃(huang)收集(ji)瓶手(shou)法等(deng)等(deng),任何一(yi)個細(xi)節都會(hui)導致自動(dong)定(ding)(ding)(ding)氮(dan)儀回收率偏低。