液(ye)相色(se)譜(pu)儀由儲(chu)液(ye)器、泵(beng)、進樣器、色(se)譜(pu)柱、檢測器、記錄儀等幾部(bu)分(fen)組成。下面介紹下液(ye)相色(se)譜(pu)儀常見(jian)故障的處理方法。

1、柱壓高原因

(1)緩沖(chong)液鹽(yan)分(fen)如(乙酸(suan)銨等)沉(chen)積于柱內;

(2)樣(yang)品(pin)污染沉(chen)積(ji)。處(chu)理(li)對于(yu)**種情況先用(yong)40～50℃的純(chun)水(shui)(shui),低速正向沖(chong)(chong)(chong)(chong)(chong)(chong)洗(xi)(xi)(xi)柱(zhu)(zhu)子(zi),待柱(zhu)(zhu)壓逐漸(jian)下(xia)降后(hou),相(xiang)應提高流速沖(chong)(chong)(chong)(chong)(chong)(chong)洗(xi)(xi)(xi),柱(zhu)(zhu)壓大幅度下(xia)降后(hou),用(yong)常溫純(chun)水(shui)(shui)沖(chong)(chong)(chong)(chong)(chong)(chong)洗(xi)(xi)(xi),之后(hou)用(yong)純(chun)甲(jia)醇(chun)沖(chong)(chong)(chong)(chong)(chong)(chong)洗(xi)(xi)(xi)柱(zhu)(zhu)子(zi)30分鐘(zhong);對于(yu)**種情況,由(you)樣(yang)品(pin)的沉(chen)積(ji)引起(qi)污染的C18柱(zhu)(zhu),和純(chun)水(shui)(shui)反向沖(chong)(chong)(chong)(chong)(chong)(chong)洗(xi)(xi)(xi)柱(zhu)(zhu)子(zi),然(ran)后(hou)換成甲(jia)醇(chun)沖(chong)(chong)(chong)(chong)(chong)(chong)洗(xi)(xi)(xi),接著用(yong)甲(jia)醇(chun)+異(yi)丙醇(chun)(4+6)沖(chong)(chong)(chong)(chong)(chong)(chong)洗(xi)(xi)(xi)柱(zhu)(zhu)子(zi)(沖(chong)(chong)(chong)(chong)(chong)(chong)洗(xi)(xi)(xi)時間的長短由(you)樣(yang)品(pin)污染的情況而定),再用(yong)換成甲(jia)醇(chun)沖(chong)(chong)(chong)(chong)(chong)(chong)洗(xi)(xi)(xi),然(ran)后(hou)用(yong)純(chun)水(shui)(shui)沖(chong)(chong)(chong)(chong)(chong)(chong)洗(xi)(xi)(xi),*后(hou)甲(jia)醇(chun)沖(chong)(chong)(chong)(chong)(chong)(chong)洗(xi)(xi)(xi)正向沖(chong)(chong)(chong)(chong)(chong)(chong)洗(xi)(xi)(xi)柱(zhu)(zhu)子(zi)30分鐘(zhong)以上。

2、流動(dong)相內(nei)(nei)有(you)氣泡(pao)(pao),關閉(bi)泵,打(da)開(kai)泄壓閥(fa),打(da)開(kai)purg鍵,清(qing)洗(xi)(xi)脫氣,氣泡(pao)(pao)不(bu)斷從(cong)過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi)冒(mao)出(chu),進入(ru)流動(dong)相,無論打(da)開(kai)purge鍵幾次,都無法**不(bu)斷產生的氣泡(pao)(pao)。原(yuan)因過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi)長期(qi)沉(chen)浸(jin)(jin)于(yu)乙酸銨等(deng)緩(huan)沖(chong)液內(nei)(nei),過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi)內(nei)(nei)部由于(yu)霉菌的生長繁殖,形成菌團,阻塞了過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi),緩(huan)沖(chong)液難以流暢地通過(guo)(guo)(guo)過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi),空(kong)氣在泵的壓力作用下經(jing)過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi)進入(ru)流動(dong)相。處理過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi)浸(jin)(jin)泡(pao)(pao)于(yu)5%硝(xiao)酸溶液中,超聲清(qing)洗(xi)(xi)幾分鐘即(ji)(ji)可(ke);亦可(ke)將過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi)浸(jin)(jin)泡(pao)(pao)于(yu)5%硝(xiao)酸溶液中12～36小(xiao)時(shi),輕(qing)輕(qing)震蕩幾次,再將過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi)用純(chun)水(shui)清(qing)洗(xi)(xi)幾次,打(da)開(kai)泄壓閥(fa),打(da)開(kai)purge鍵清(qing)洗(xi)(xi)脫氣,如(ru)仍有(you)氣泡(pao)(pao)不(bu)斷從(cong)過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi)冒(mao)出(chu),繼(ji)續將過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi)浸(jin)(jin)泡(pao)(pao)于(yu)5%硝(xiao)酸溶液中,如(ru)沒有(you)氣泡(pao)(pao)不(bu)斷從(cong)過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi)中冒(mao)出(chu),說明過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi)內(nei)(nei)部的霉菌菌團已(yi)被(bei)硝(xiao)酸破壞,流動(dong)相可(ke)以流暢地通過(guo)(guo)(guo)過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi)。打(da)開(kai)泄壓閥(fa),打(da)開(kai)泵,流速調(diao)至1.0～3.0ml/min,純(chun)水(shui)沖(chong)洗(xi)(xi)過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi)1小(xiao)時(shi)左右。即(ji)(ji)可(ke)將過(guo)(guo)(guo)濾(lv)(lv)(lv)器(qi)(qi)(qi)(qi)清(qing)洗(xi)(xi)干凈。關閉(bi)泄壓閥(fa),純(chun)甲醇(chun)沖(chong)洗(xi)(xi)半小(xiao)時(shi)即(ji)(ji)可(ke)。

3、既無壓力指示,又(you)無液體流過。

(1)泵密封(feng)墊圈(quan)磨損;

(2)大量氣泡進入泵(beng)體。處(chu)理對于(yu)**種情況(kuang),更換密(mi)封(feng)墊圈;對于(yu)**種情況(kuang),在泵(beng)作用(yong)的同時,用(yong)一(yi)個50ml的玻(bo)璃針筒在泵(beng)的出口處(chu)幫(bang)助(zhu)抽出空氣。

4、峰面積重復性不佳。

(1)進樣閥漏(lou)液;

(2)加樣針(zhen)不到位(wei)。

處(chu)理對于(yu)**種情況(kuang)更(geng)換進樣(yang)(yang)(yang)閥墊圈;對于(yu)**種情況(kuang)保(bao)證加樣(yang)(yang)(yang)針(zhen)插到(dao)底(di),注射(she)樣(yang)(yang)(yang)品(pin)溶液(ye)后須快速(su)、平穩地(di)從LOAD狀態轉換到(dao)INJECT狀態,以保(bao)證進樣(yang)(yang)(yang)量的(de)(de)(de)(de)準確(que)。日(ri)常(chang)工作(zuo)中,液(ye)相色譜(pu)儀(yi)的(de)(de)(de)(de)保(bao)養非常(chang)重(zhong)要(yao),如(ru)要(yao)注意(yi)不要(yao)讓空氣進入輸(shu)液(ye)系統(tong)和高壓(ya)泵中,儲(chu)(chu)液(ye)器內(nei)的(de)(de)(de)(de)溶液(ye)如(ru)長時(shi)間未用(yong)應清洗儲(chu)(chu)液(ye)器并更(geng)換溶液(ye),每(mei)次(ci)用(yong)完色譜(pu)儀(yi)后緩沖液(ye)要(yao)用(yong)純水沖洗干凈(jing),防止無機鹽析出或(huo)沉(chen)積(ji);樣(yang)(yang)(yang)品(pin)的(de)(de)(de)(de)前(qian)處(chu)理也很重(zhong)要(yao),任何樣(yang)(yang)(yang)品(pin)都要(yao)盡可(ke)能地(di)去除(chu)雜質,完全溶解(jie),盡量減少(shao)對色譜(pu)柱的(de)(de)(de)(de)污染(ran),以延(yan)長色譜(pu)柱的(de)(de)(de)(de)使用(yong)壽命,同時(shi)避免(mian)(mian)注射(she)過(guo)濃的(de)(de)(de)(de)樣(yang)(yang)(yang)品(pin)溶液(ye),以免(mian)(mian)殘留液(ye)在進樣(yang)(yang)(yang)閥內(nei)析出固體引起堵塞;色譜(pu)柱作(zuo)好標(biao)記,用(yong)于(yu)不同分析目的(de)(de)(de)(de)的(de)(de)(de)(de)色譜(pu)柱不要(yao)混用(yong)等(deng)。

5、出峰(feng)不(bu)佳,峰(feng)分(fen)叉。

(1)色譜柱被(bei)污染(ran);

(2)柱(zhu)(zhu)(zhu)頭填(tian)料(liao)(liao)(liao)塌(ta)陷。處理對于**種情(qing)況,先用(yong)純(chun)(chun)水反向沖(chong)(chong)(chong)洗(xi)(xi)(xi)柱(zhu)(zhu)(zhu)子,然(ran)(ran)后(hou)換成甲(jia)(jia)醇沖(chong)(chong)(chong)洗(xi)(xi)(xi),接著用(yong)甲(jia)(jia)醇+異(yi)丙(bing)醇(4+6)沖(chong)(chong)(chong)洗(xi)(xi)(xi)柱(zhu)(zhu)(zhu)子(沖(chong)(chong)(chong)洗(xi)(xi)(xi)時(shi)間(jian)的(de)(de)(de)長短由樣品污染的(de)(de)(de)情(qing)況而定),再(zai)(zai)換成甲(jia)(jia)醇沖(chong)(chong)(chong)洗(xi)(xi)(xi),然(ran)(ran)后(hou)用(yong)純(chun)(chun)水沖(chong)(chong)(chong)洗(xi)(xi)(xi),*后(hou)甲(jia)(jia)醇沖(chong)(chong)(chong)洗(xi)(xi)(xi)正(zheng)向沖(chong)(chong)(chong)洗(xi)(xi)(xi)柱(zhu)(zhu)(zhu)子30分鐘以上(shang)。如沖(chong)(chong)(chong)洗(xi)(xi)(xi)后(hou)依然(ran)(ran)出峰不(bu)(bu)佳,則考慮**種情(qing)況。對于**種情(qing)況,擰(ning)開柱(zhu)(zhu)(zhu)頭,檢查柱(zhu)(zhu)(zhu)填(tian)料(liao)(liao)(liao)是否硬結或塌(ta)陷。去除硬結部分(污染的(de)(de)(de)填(tian)料(liao)(liao)(liao)),裝入新填(tian)料(liao)(liao)(liao),滴(di)一滴(di)甲(jia)(jia)醇,填(tian)料(liao)(liao)(liao)下陷,再(zai)(zai)填(tian),用(yong)與柱(zhu)(zhu)(zhu)內(nei)徑(jing)相同的(de)(de)(de)頂(ding)端平(ping)(ping)滑的(de)(de)(de)不(bu)(bu)銹鋼桿壓緊,再(zai)(zai)填(tian)平(ping)(ping),滴(di)甲(jia)(jia)醇,再(zai)(zai)壓緊反復幾次,直至裝滿填(tian)平(ping)(ping)。柱(zhu)(zhu)(zhu)頭用(yong)甲(jia)(jia)醇沖(chong)(chong)(chong)洗(xi)(xi)(xi)干(gan)凈,擦凈柱(zhu)(zhu)(zhu)外壁的(de)(de)(de)填(tian)料(liao)(liao)(liao),擰(ning)緊柱(zhu)(zhu)(zhu)頭,用(yong)純(chun)(chun)甲(jia)(jia)醇沖(chong)(chong)(chong)洗(xi)(xi)(xi)30分鐘以上(shang)。

6、壓力波(bo)動大,流量(liang)不穩定。

原因(yin)系統中有(you)空氣(qi)或(huo)者(zhe)單向閥(fa)的寶石球(qiu)和(he)閥(fa)座之(zhi)間夾(jia)有(you)異物,使(shi)得兩者(zhe)不能密封。處(chu)理工(gong)作(zuo)中注意(yi)觀察流動(dong)相(xiang)的量,保證不銹鋼濾器(qi)沉入儲液器(qi)瓶底,避免吸入空氣(qi),流動(dong)相(xiang)要(yao)充分(fen)脫氣(qi)。如為單向閥(fa)和(he)閥(fa)座之(zhi)間夾(jia)有(you)異物,拆(chai)下單向閥(fa),放入盛有(you)丙酮(tong)的燒杯用(yong)超聲波(bo)清洗。