隨(sui)著科技(ji)的(de)進步(bu),科研人員的(de)努力,定(ding)氮儀已邁上一個新的(de)臺階并(bing)在食品(pin)測(ce)定(ding)中發(fa)揮著重要(yao)作用。在保證(zheng)準確(que)度的(de)前提下,定(ding)氮儀將(jiang)向(xiang)更簡便、高效、系統化、自(zi)動(dong)化、智能化等方向(xiang)迅猛發(fa)展,以滿(man)足各(ge)行(xing)業的(de)不同需(xu)求(qiu)。 注(zhu)意事項:
上(shang)機測(ce)定(ding)(ding)(ding):儀(yi)器(qi)稀(xi)釋(shi)水采用中性(xing)去(qu)離子水;蒸(zheng)汽發生(sheng)瓶內的(de)(de)水必須(xu)(xu)保持酸(suan)性(xing);硼(peng)酸(suan)吸(xi)收液(ye)配制(zhi)時(shi)(shi)應用中性(xing)去(qu)離子水,避免堿(jian)(jian)(jian)性(xing)物(wu)質的(de)(de)混入,盛(sheng)裝硼(peng)酸(suan)吸(xi)收液(ye)的(de)(de)容器(qi)應刷(shua)洗干凈;堿(jian)(jian)(jian)液(ye)應用中性(xing)去(qu)離子水配置;滴定(ding)(ding)(ding)用的(de)(de)標準(zhun)酸(suan)必須(xu)(xu)按照標準(zhun)配制(zhi)和(he)標定(ding)(ding)(ding)。上(shang)機測(ce)試樣(yang)品前,應打開儀(yi)器(qi)預熱,放一支(zhi)消化管空(kong)蒸(zheng)一次,排除(chu)蒸(zheng)餾(liu)(liu)(liu)(liu)管路中的(de)(de)空(kong)氣。蒸(zheng)餾(liu)(liu)(liu)(liu)時(shi)(shi)必須(xu)(xu)加堿(jian)(jian)(jian),加入堿(jian)(jian)(jian)的(de)(de)作用一是(shi)(shi)中和(he)硫酸(suan),二是(shi)(shi)使溶液(ye)處(chu)于強堿(jian)(jian)(jian)性(xing),這樣(yang)才能使 (NH4)2SO4變(bian)(bian)成NH3被硼(peng)酸(suan)吸(xi)收,通常是(shi)(shi)消化取用濃硫酸(suan)的(de)(de)四倍體(ti)積(40%NaOH)。硫酸(suan)銅(tong)(tong)可作為催(cui)化劑(ji)(ji),并在蒸(zheng)餾(liu)(liu)(liu)(liu)時(shi)(shi)作堿(jian)(jian)(jian)性(xing)反(fan)應指示(shi)劑(ji)(ji),氫氧化鈉是(shi)(shi)否(fou)足量.可借助硫酸(suan) 銅(tong)(tong)在堿(jian)(jian)(jian)性(xing)條件下生(sheng)成的(de)(de)褐色沉(chen)淀或深藍色的(de)(de)銅(tong)(tong)氨(an)絡離子指示(shi)。若溶液(ye)的(de)(de)顏色不(bu)改變(bian)(bian),則說明所(suo)加的(de)(de)堿(jian)(jian)(jian)液(ye)不(bu)足。蒸(zheng)餾(liu)(liu)(liu)(liu)是(shi)(shi)否(fou)完(wan)全(quan),半自(zi)(zi)動定(ding)(ding)(ding)氮(dan)儀(yi)可用精密 pH試紙測(ce)冷(leng)凝管的(de)(de)冷(leng)凝液(ye)來確(que)定(ding)(ding)(ding),中性(xing)說明已蒸(zheng)餾(liu)(liu)(liu)(liu)完(wan)全(quan)。全(quan)自(zi)(zi)動定(ding)(ding)(ding)氮(dan)儀(yi)目前主要是(shi)(shi)以蒸(zheng)餾(liu)(liu)(liu)(liu)體(ti)積與設(she)置時(shi)(shi)間(jian)(經驗值(zhi))確(que)保蒸(zheng)餾(liu)(liu)(liu)(liu)完(wan)全(quan)。蒸(zheng)餾(liu)(liu)(liu)(liu)結束后,滴定(ding)(ding)(ding)主要是(shi)(shi)是(shi)(shi)分為人工(gong)滴定(ding)(ding)(ding)和(he)機器(qi)自(zi)(zi)動滴定(ding)(ding)(ding)計算和(he)打印實驗結果(guo)。要求操作者(zhe)根據實際情(qing)況(kuang),按照要求操作。
2、樣(yang)品(pin)前處(chu)理:樣(yang)品(pin)應盡量(liang)選取具有代表(biao)性(xing)的,大塊的固體(ti)樣(yang)品(pin)應用粉碎設(she)備(bei)打得細小均(jun)勻,液(ye)體(ti)樣(yang)要混合均(jun)勻。
3、模塊化(hua)(hua)(hua)消解(jie)裝(zhuang)置(zhi)消化(hua)(hua)(hua)樣品:消化(hua)(hua)(hua)過(guo)程(cheng)中(zhong),首先確(que)保(bao)濃硫酸量足(zu)夠,如樣品脂肪(fang)含(han)量較高時(shi),應適當增加硫酸量;其次對某(mou)些樣品炭化(hua)(hua)(hua)易產生泡沫,這時(shi)可采用sh520消解(jie)爐曲(qu)線升溫或手動控(kong)制升溫,讓(rang)消解(jie)溶液(ye)(ye)沸騰均勻后再提高消解(jie)溫度(du),直(zhi)至(zhi)消化(hua)(hua)(hua)液(ye)(ye)呈透明藍綠(lv)色再消化(hua)(hua)(hua)0.5h或1h。因為炭化(hua)(hua)(hua)過(guo)程(cheng)中(zhong),升溫速(su)度(du)過(guo)快會使樣品溢出(chu)消化(hua)(hua)(hua)管(guan)或濺起粘附(fu)在管(guan)壁導致無法消化(hua)(hua)(hua)完全而造成氮(dan)損失,影(ying)響(xiang)結(jie)果準確(que)性(xing)。