氣相色譜儀的組(zu)成及使用要求(qiu)

氣相色譜(pu)儀是一(yi)種常用(yong)的分(fen)析儀(yi)器，適用(yong)于分(fen)析具(ju)有(you)一(yi)定(ding)蒸氣壓且熱穩定(ding)性好的組分(fen)，對(dui)氣體(ti)試樣和受熱易(yi)揮發的有(you)機(ji)物可直接(jie)進行分(fen)析。今天(tian)我們(men)主要來介紹一(yi)下氣相色(se)譜儀(yi)的組成及使(shi)用(yong)要求，希望(wang)可以幫助用(yong)戶(hu)更(geng)好的應用(yong)產(chan)品。

一、儀器的(de)組成

氣相色譜儀由載氣源、進樣(yang)部(bu)分、色譜柱(zhu)(zhu)、柱(zhu)(zhu)溫箱、檢測器(qi)和數據處理系(xi)統組成(cheng)。進樣(yang)部(bu)分、色譜柱(zhu)(zhu)和檢測器(qi)的溫度均在控制狀態。

二、對儀器的使用要求(qiu)

1、對儀(yi)器的一般要求(qiu)

(1)載氣源氣體氦、氮和氫可(ke)用作氣相色譜法的流動(dong)相，可(ke)根(gen)據供試(shi)品的性質和檢測器種類選擇載氣，除另有規定外，常用載氣為氮氣。

(2)進(jin)(jin)(jin)樣(yang)(yang)(yang)(yang)部分進(jin)(jin)(jin)樣(yang)(yang)(yang)(yang)方(fang)式一(yi)般(ban)可采用溶液直接進(jin)(jin)(jin)樣(yang)(yang)(yang)(yang)或(huo)頂空(kong)進(jin)(jin)(jin)樣(yang)(yang)(yang)(yang)。采用溶液直接進(jin)(jin)(jin)樣(yang)(yang)(yang)(yang)時，進(jin)(jin)(jin)樣(yang)(yang)(yang)(yang)口溫(wen)度應高于柱溫(wen)30～50℃。頂空(kong)進(jin)(jin)(jin)樣(yang)(yang)(yang)(yang)適(shi)用于固體和液體供試品中(zhong)揮發性組分的分離和測(ce)定。

(3)色譜柱根據需要(yao)選擇(ze)。新填充(chong)柱和(he)毛細(xi)管柱在使用前需老化以除去(qu)殘留溶劑(ji)及低分子量的(de)聚合物，色譜柱如長期未用，使用前應老化處(chu)理(li)，使基線穩定(ding)。

(4)柱溫(wen)箱(xiang)柱溫(wen)箱(xiang)溫(wen)度(du)的(de)波動會影響(xiang)色譜(pu)分析結果的(de)重現性(xing)，因(yin)此柱溫(wen)箱(xiang)控溫(wen)度(du)應在±1℃，且(qie)溫(wen)度(du)波動小于(yu)每小時0.1℃。

(5)檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)適合(he)(he)氣(qi)(qi)(qi)相(xiang)色譜(pu)法的(de)檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)有火(huo)(huo)(huo)焰(yan)(yan)離(li)子化(hua)檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)(FID)、熱導檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)(TCD)、氮磷(lin)檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)(NPD)、火(huo)(huo)(huo)焰(yan)(yan)光度(du)(du)檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)(FPD)、電子捕(bu)(bu)獲檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)(ECD)、質(zhi)譜(pu)檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)(MS)等。火(huo)(huo)(huo)焰(yan)(yan)離(li)子化(hua)檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)對碳氫(qing)化(hua)合(he)(he)物(wu)(wu)響應良好，適合(he)(he)檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)大多數的(de)藥物(wu)(wu);氮磷(lin)檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)對含氮、磷(lin)元素(su)的(de)化(hua)合(he)(he)物(wu)(wu)靈敏度(du)(du)高(gao);火(huo)(huo)(huo)焰(yan)(yan)光度(du)(du)檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)對含磷(lin)、硫元素(su)的(de)化(hua)合(he)(he)物(wu)(wu)靈敏度(du)(du)高(gao);電子捕(bu)(bu)獲檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)適于含鹵素(su)的(de)化(hua)合(he)(he)物(wu)(wu);質(zhi)譜(pu)檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)還能給出供(gong)試品(pin)某(mou)個成分(fen)相(xiang)應的(de)結構(gou)信息，可(ke)用(yong)(yong)于結構(gou)確證。除(chu)另有規定外，火(huo)(huo)(huo)焰(yan)(yan)離(li)子化(hua)檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)一(yi)(yi)般(ban)用(yong)(yong)氫(qing)氣(qi)(qi)(qi)作(zuo)為(wei)燃氣(qi)(qi)(qi)，空氣(qi)(qi)(qi)作(zuo)為(wei)助燃氣(qi)(qi)(qi)。在使用(yong)(yong)火(huo)(huo)(huo)焰(yan)(yan)離(li)子化(hua)檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)時，檢(jian)(jian)(jian)(jian)(jian)(jian)測(ce)(ce)(ce)(ce)器(qi)(qi)(qi)(qi)溫(wen)度(du)(du)一(yi)(yi)般(ban)應高(gao)于柱溫(wen)，并不(bu)得低(di)于150℃，以免水汽凝結，通常(chang)為(wei)250～350℃。

(6)數據處(chu)理系(xi)(xi)統(tong)目前多用(yong)計算機工(gong)作(zuo)站。藥(yao)典規定(ding)，各品(pin)種項下規定(ding)的色(se)譜條件，除載(zai)(zai)氣、檢測器、固(gu)定(ding)液品(pin)種及特殊的色(se)譜柱材料不得改(gai)(gai)變外，其余如色(se)譜柱內徑、長度(du)、載(zai)(zai)體牌號、粒度(du)、固(gu)定(ding)液涂(tu)布濃(nong)度(du)、載(zai)(zai)氣流速、柱溫、進樣量(liang)、檢測器的靈敏度(du)等，均(jun)可適當(dang)改(gai)(gai)變，以適應具體品(pin)種并符合系(xi)(xi)統(tong)適用(yong)性(xing)試驗的要求。一(yi)般色(se)譜圖(tu)約于30min內記(ji)錄完畢。

2、系統適用性試驗

除另有規定(ding)外，照液相色譜法項下的規定(ding)。

三、測定方法

(1)內標法加校(xiao)正(zheng)因子(zi)測(ce)定供試品中某個(ge)雜質或(huo)主(zhu)成分含量

(2)外標法測(ce)定(ding)供(gong)試晶中某個雜(za)質或主成分含量

(3)面積歸(gui)一(yi)化法(fa)

上述1～3法的具(ju)體(ti)內(nei)容均(jun)同液相(xiang)色譜法的相(xiang)應規定。