隨著(zhu)科技的(de)進步,科研人員(yuan)的(de)努力(li),定氮儀已(yi)邁上一(yi)個(ge)新的(de)臺階并(bing)在食(shi)品測定中發揮著(zhu)重要作用。在保(bao)證準確度的(de)前提(ti)下,定氮儀將向更簡(jian)便、高效、系統化(hua)、自(zi)動化(hua)、智能化(hua)等方向迅(xun)猛發展,以滿足各行業的(de)不同需求。 注意事項:
上機(ji)測定(ding)(ding):儀器稀釋水(shui)采用(yong)中(zhong)性(xing)去離(li)(li)子(zi)水(shui);蒸(zheng)(zheng)(zheng)汽發生瓶內的(de)(de)水(shui)必須保(bao)持酸(suan)性(xing);硼(peng)酸(suan)吸(xi)收(shou)液配制(zhi)時(shi)(shi)應(ying)用(yong)中(zhong)性(xing)去離(li)(li)子(zi)水(shui),避免堿(jian)(jian)(jian)性(xing)物質的(de)(de)混入(ru)(ru),盛裝硼(peng)酸(suan)吸(xi)收(shou)液的(de)(de)容器應(ying)刷洗(xi)干凈(jing);堿(jian)(jian)(jian)液應(ying)用(yong)中(zhong)性(xing)去離(li)(li)子(zi)水(shui)配置(zhi);滴(di)(di)定(ding)(ding)用(yong)的(de)(de)標準(zhun)(zhun)酸(suan)必須按照標準(zhun)(zhun)配制(zhi)和(he)標定(ding)(ding)。上機(ji)測試(shi)樣品前,應(ying)打開儀器預熱,放一支消(xiao)化管空蒸(zheng)(zheng)(zheng)一次(ci),排除蒸(zheng)(zheng)(zheng)餾(liu)(liu)(liu)管路中(zhong)的(de)(de)空氣。蒸(zheng)(zheng)(zheng)餾(liu)(liu)(liu)時(shi)(shi)必須加(jia)堿(jian)(jian)(jian),加(jia)入(ru)(ru)堿(jian)(jian)(jian)的(de)(de)作(zuo)用(yong)一是(shi)(shi)中(zhong)和(he)硫酸(suan),二是(shi)(shi)使溶(rong)液處于強堿(jian)(jian)(jian)性(xing),這樣才能使 (NH4)2SO4變(bian)成NH3被硼(peng)酸(suan)吸(xi)收(shou),通常(chang)是(shi)(shi)消(xiao)化取用(yong)濃硫酸(suan)的(de)(de)四倍體積(40%NaOH)。硫酸(suan)銅可作(zuo)為催化劑,并(bing)在蒸(zheng)(zheng)(zheng)餾(liu)(liu)(liu)時(shi)(shi)作(zuo)堿(jian)(jian)(jian)性(xing)反應(ying)指示劑,氫氧(yang)化鈉是(shi)(shi)否(fou)足量(liang).可借(jie)助硫酸(suan) 銅在堿(jian)(jian)(jian)性(xing)條(tiao)件(jian)下(xia)生成的(de)(de)褐(he)色沉淀或深藍色的(de)(de)銅氨絡(luo)離(li)(li)子(zi)指示。若溶(rong)液的(de)(de)顏(yan)色不改變(bian),則說(shuo)明所加(jia)的(de)(de)堿(jian)(jian)(jian)液不足。蒸(zheng)(zheng)(zheng)餾(liu)(liu)(liu)是(shi)(shi)否(fou)完全(quan),半自(zi)動(dong)定(ding)(ding)氮儀可用(yong)精(jing)密(mi) pH試(shi)紙(zhi)測冷凝(ning)(ning)管的(de)(de)冷凝(ning)(ning)液來確定(ding)(ding),中(zhong)性(xing)說(shuo)明已蒸(zheng)(zheng)(zheng)餾(liu)(liu)(liu)完全(quan)。全(quan)自(zi)動(dong)定(ding)(ding)氮儀目前主要(yao)(yao)是(shi)(shi)以蒸(zheng)(zheng)(zheng)餾(liu)(liu)(liu)體積與設置(zhi)時(shi)(shi)間(經(jing)驗(yan)值(zhi))確保(bao)蒸(zheng)(zheng)(zheng)餾(liu)(liu)(liu)完全(quan)。蒸(zheng)(zheng)(zheng)餾(liu)(liu)(liu)結束(shu)后,滴(di)(di)定(ding)(ding)主要(yao)(yao)是(shi)(shi)是(shi)(shi)分為人工滴(di)(di)定(ding)(ding)和(he)機(ji)器自(zi)動(dong)滴(di)(di)定(ding)(ding)計算(suan)和(he)打印(yin)實驗(yan)結果。要(yao)(yao)求操(cao)作(zuo)者根據實際情(qing)況,按照要(yao)(yao)求操(cao)作(zuo)。
2、樣(yang)(yang)品(pin)前處(chu)理(li):樣(yang)(yang)品(pin)應盡量(liang)選取具有代表性的(de)(de),大塊的(de)(de)固體樣(yang)(yang)品(pin)應用(yong)粉碎設(she)備(bei)打得細小(xiao)均勻,液體樣(yang)(yang)要混合均勻。
3、模塊化(hua)(hua)(hua)消(xiao)(xiao)解裝置消(xiao)(xiao)化(hua)(hua)(hua)樣品(pin):消(xiao)(xiao)化(hua)(hua)(hua)過程中(zhong),首先確保濃硫(liu)酸量足(zu)夠,如樣品(pin)脂肪含(han)量較(jiao)高時(shi),應適當增加硫(liu)酸量;其次(ci)對某些樣品(pin)炭(tan)化(hua)(hua)(hua)易產(chan)生泡沫(mo),這時(shi)可采用sh520消(xiao)(xiao)解爐曲(qu)線升溫(wen)或(huo)手(shou)動控制升溫(wen),讓(rang)消(xiao)(xiao)解溶(rong)液沸(fei)騰均勻后再提高消(xiao)(xiao)解溫(wen)度(du),直(zhi)至消(xiao)(xiao)化(hua)(hua)(hua)液呈透(tou)明藍綠色再消(xiao)(xiao)化(hua)(hua)(hua)0.5h或(huo)1h。因為炭(tan)化(hua)(hua)(hua)過程中(zhong),升溫(wen)速度(du)過快(kuai)會使樣品(pin)溢出消(xiao)(xiao)化(hua)(hua)(hua)管或(huo)濺起(qi)粘附在管壁導致無(wu)法消(xiao)(xiao)化(hua)(hua)(hua)完全(quan)而造(zao)成氮損失,影響結果準確性(xing)。