一、 氣路管路、進樣器、注射器的清洗
清(qing)洗(xi)氣(qi)路(lu)連(lian)接(jie)管(guan)時(shi),應(ying)首(shou)先(xian)將(jiang)該(gai)管(guan)的(de)兩(liang)端(duan)接(jie)頭(tou)拆(chai)下(xia),再(zai)將(jiang)該(gai)段(duan)管(guan)線(xian)從(cong)色(se)譜(pu)儀(yi)中(zhong)取(qu)出(chu),這(zhe)時(shi)應(ying)先(xian)把(ba)管(guan)外(wai)壁(bi)灰(hui)塵(chen)擦(ca)洗(xi)幹(gan)淨(jing),以(yi)免(mian)清(qing)洗(xi)完(wan)管(guan)內(nei)壁(bi)時(shi)再(zai)產(chan)生(sheng)汙(wu)染(ran)。清(qing)洗(xi)管(guan)路(lu)內(nei)壁(bi)時(shi)應(ying)先(xian)用(yong)無(wu)水(shui)乙(yi)醇(chun)進(jin)行(xing)疏(shu)通(tong)處(chu)理(li),這(zhe)可(ke)除(chu)去(qu)管(guan)路(lu)內(nei)大(da)部(bu)分(fen)顆(ke)粒(li)狀(zhuang)堵(du)塞(sai)物(wu)及(ji)易(yi)被(bei)乙(yi)醇(chun)溶(rong)解(jie)的(de)有(you)機(ji)物(wu)和(he)水(shui)分(fen)。在(zai)此(ci)疏(shu)通(tong)步(bu)驟(zhou)中(zhong),如(ru)發(fa)現(xian)管(guan)路(lu)不(bu)通(tong),可(ke)用(yong)洗(xi)耳(er)球(qiu)加(jia)壓(ya)吹(chui)洗(xi),加(jia)壓(ya)後(hou)仍(reng)無(wu)效(xiao)可(ke)考(kao)慮(lv)用(yong)細(xi)鋼(gang)絲(si)捅(tong)針(zhen)疏(shu)通(tong)管(guan)路(lu)。如(ru)此(ci)法(fa)還(hai)不(bu)能(neng)使(shi)管(guan)線(xian)暢(chang)通(tong),可(ke)使(shi)用(yong)酒(jiu)精(jing)燈(deng)加(jia)熱(re)管(guan)路(lu)使(shi)堵(du)塞(sai)物(wu)在(zai)高(gao)溫(wen)下(xia)炭(tan)化(hua)而(er)達(da)到(dao)疏(shu)通(tong)的(de)目(mu)的(de)。
yongwushuiyichunqingxiwanqiluguanluhou,yingkaolvguanluneibishifouyoubuyibeiyichunrongjiedewuranwu。rumeiyou,kejiaregaiguanxianbingyongganzaoqitiduiqichuisao,jiangguanxianzhuanghuiyuanqiludaiyong。ruguoyoufenxiyangpinguochengpandingqiluneibikenenghaiyouqitabuyibeiyichunrongjiedewuranwu,kezhenduijutiwuzhirongjietexingxuanzeqitaqingxiye。xuanzeqingxiyedeshunxuyingxianshiyonggaofeidianrongji、而後再使用低沸點溶劑浸泡和清洗。可供選擇的清洗液有萘烷、N、N-二甲基酰胺、甲醇、蒸餾水、丙酮、乙醚、氟裏昂、石油醚、乙醇等。
對進樣器(包括汽化室)deqingxiyingyishutongweixiandao。tongchangzaijinyangqizhongdedusaiwushijinyanggediandesuipian,yangpinzhongbeitanhualedegaofeidianwu,duizhexiegutaizazhikeyongbuxiugangtongzhenshutong,ranhouzaiyongyichunhuobingtongchongxi。weileshiqingxigengchedi,kexuanyong2:1:4的H2SO4/HNO3/H2O混合溶液先對進樣器清洗,然後再用蒸餾水,最後再用丙酮、或乙醇清洗。清洗完後烘幹,裝上儀器通載氣半小時,加熱到120℃待幾小時後即可正常工作。在拆裝進樣器時需注意不要碰斷加熱器引線或使引線碰到外殼;測ce溫wen元yuan件jian也ye應ying在zai裝zhuang回hui進jin樣yang器qi之zhi後hou,按an原yuan先xian測ce溫wen點dian裝zhuang回hui。通tong常chang測ce溫wen元yuan件jian和he進jin樣yang器qi加jia熱re體ti是shi緊jin密mi接jie觸chu的de,如ru距ju離li過guo大da將jiang會hui造zao成cheng過guo高gao的de汽qi化hua溫wen度du5%氫氧化鈉水溶液、蒸餾水、丙酮、氯仿,最後用真空泵抽幹。。
zhusheqishiyongqiankexianyongbingtongqingxi,yimiandianwuyangpin,danzuihaohaishiyongdaizhusheyangpinduizhusheqibenshenzuoyierciqingxi。qingxishizhinengxiruyangpin,paichuyangpinshiyaozaiyangpinpingzhiwai。zhusheqizaishiyongjieshuhouyaolijiqingxi,yimianbeiyangpinzhongdegaofeidianwuzhidianwu。yibanchangyongxiashurongyeyiciqingxi:
二、檢測器的清洗
在色譜儀操作過程中,檢測器有時會被流失的固定相及樣品中的高沸點成分、易(yi)分(fen)解(jie)或(huo)有(you)腐(fu)蝕(shi)性(xing)的(de)物(wu)質(zhi)玷(dian)汙(wu)。此(ci)時(shi)應(ying)對(dui)檢(jian)測(ce)器(qi)進(jin)行(xing)清(qing)洗(xi)。清(qing)洗(xi)時(shi)可(ke)分(fen)三(san)種(zhong)情(qing)況(kuang),一(yi)種(zhong)是(shi)玷(dian)汙(wu)物(wu)質(zhi)僅(jin)限(xian)於(yu)高(gao)沸(fei)點(dian)成(cheng)分(fen),通(tong)常(chang)可(ke)將(jiang)檢(jian)測(ce)器(qi)加(jia)熱(re)到(dao)最(zui)高(gao)使(shi)用(yong)溫(wen)度(du)後(hou),再(zai)通(tong)入(ru)載(zai)氣(qi),即(ji)可(ke)清(qing)除(chu)。第(di)二(er)種(zhong)情(qing)況(kuang)是(shi)檢(jian)測(ce)器(qi)僅(jin)存(cun)在(zai)程(cheng)度(du)較(jiao)輕(qing)的(de)玷(dian)汙(wu),此(ci)時(shi)可(ke)用(yong)蒸(zheng)汽(qi)清(qing)洗(xi)的(de)方(fang)法(fa)。過(guo)程(cheng)是(shi)在(zai)進(jin)樣(yang)口(kou)注(zhu)入(ru)幾(ji)十(shi)微(wei)升(sheng)蒸(zheng)餾(liu)水(shui)或(huo)丙(bing)酮(tong)等(deng)溶(rong)劑(ji),待(dai)1~2xiaoshihou,jianzhajixianshifoupingwenjike。disanzhongqingkuangshizaishangshuliangzhongjiandanfangfabunengjiejuewentishisuocaiyongdechediqingxifangfa,cifangfayaoqiuchaizhuangjianceqi,tongshihaiyaoxuanzeshiyiderongji,jisuoxuanzederongji,jiyaonengrongjiedianwuwu,youbuduijianceqizaochengxindewuranhesunhuai。cishiqingxiguohoudebujianbuyaozhijieyongshoumo。
1、熱導檢測器(TCD)的清洗
將丙酮、乙醚、十氫萘等溶劑裝滿檢測器的測量池,浸泡一段時間(約20分鍾)後(hou)傾(qing)出(chu),反(fan)複(fu)進(jin)行(xing)多(duo)次(ci)至(zhi)所(suo)傾(qing)出(chu)的(de)溶(rong)液(ye)比(bi)較(jiao)幹(gan)淨(jing)為(wei)止(zhi)。當(dang)選(xuan)用(yong)一(yi)種(zhong)溶(rong)劑(ji)不(bu)能(neng)洗(xi)淨(jing)時(shi),可(ke)根(gen)據(ju)玷(dian)汙(wu)物(wu)的(de)性(xing)質(zhi)先(xian)選(xuan)用(yong)高(gao)沸(fei)點(dian)溶(rong)劑(ji)進(jin)行(xing)浸(jin)泡(pao)清(qing)洗(xi),然(ran)後(hou)再(zai)用(yong)低(di)沸(fei)點(dian)溶(rong)劑(ji)反(fan)複(fu)清(qing)洗(xi)。洗(xi)淨(jing)後(hou),加(jia)熱(re)趕(gan)去(qu)溶(rong)劑(ji),將(jiang)檢(jian)測(ce)器(qi)裝(zhuang)回(hui)到(dao)儀(yi)器(qi)上(shang),再(zai)加(jia)熱(re)通(tong)載(zai)氣(qi)衝(chong)洗(xi)數(shu)小(xiao)時(shi)後(hou),即(ji)可(ke)使(shi)用(yong)。
2、氫火焰離子化檢測器(FID)的清洗
當FID玷汙不太嚴重時,可不必卸下清洗,此時隻需要將色譜柱取下,用一根管子將進樣口與檢測器聯接起來,然後通載氣將檢測器恒溫升至120℃以上。再從進樣口中注入20微升左右的蒸餾水,接著再用幾十微升乙醇或氟裏昂113溶劑進行清洗(用丙酮也可,但應注意,有的色譜儀氫焰室中噴嘴不適宜用丙酮清洗)。在此溫度下保持1~2小時檢查基線是否平穩,若仍不理想,可重複上述操作或按下麵方法處理。
當玷汙比較嚴重時,須拆下檢測器清洗。方法是先拆下收集極、極化極、噴嘴等,若噴嘴是石英材料製成的,先將其放在水中進行浸泡過夜;若噴嘴是不鏽鋼等材料做成,則可與電極等一起,先小心用300~400號細砂紙打磨,再用適當溶劑(如1:1的甲醇與苯)進行浸泡。也可用超聲波清洗,最後用甲醇洗淨,放置於烘箱中烘幹。注意勿用氯仿、二氯甲烷一類的含鹵素的溶劑。以免與聚乙烯材料作用,導致噪聲增加。
清(qing)洗(xi)後(hou)的(de)各(ge)部(bu)件(jian),要(yao)用(yong)鑷(nie)子(zi)取(qu),勿(wu)用(yong)手(shou)摸(mo)。烘(hong)幹(gan)後(hou)裝(zhuang)配(pei)時(shi)也(ye)要(yao)小(xiao)心(xin),否(fou)則(ze)會(hui)再(zai)度(du)玷(dian)汙(wu)。裝(zhuang)入(ru)儀(yi)器(qi)後(hou),先(xian)通(tong)載(zai)氣(qi)半(ban)小(xiao)時(shi),再(zai)點(dian)火(huo)升(sheng)高(gao)檢(jian)測(ce)室(shi)溫(wen)度(du),最(zui)好(hao)先(xian)在(zai)120℃保持幾小時之後,再升至工作溫度。
手機版




