不小心用光了流動相,很多空氣被泵抽進了色譜柱,這會損壞我的柱子嗎?怎樣排出空氣恢複柱子?
首先,問題建立在錯誤的假設上。如果流動相沒了,泵的確會吸進去一些空氣,但是並不會持續的讓空氣流經整個係統。這是因為HPLC的泵是設計成專門用來吸取液體的,空氣一旦進入,泵就會失去灌注(lose prime)並(bing)停(ting)止(zhi)工(gong)作(zuo)。當(dang)然(ran),在(zai)泵(beng)完(wan)全(quan)停(ting)止(zhi)之(zhi)前(qian),一(yi)些(xie)氣(qi)泡(pao)可(ke)能(neng)會(hui)進(jin)入(ru)柱(zhu)子(zi),但(dan)是(shi)這(zhe)種(zhong)情(qing)況(kuang)不(bu)會(hui)一(yi)直(zhi)持(chi)續(xu)下(xia)去(qu)。就(jiu)算(suan)由(you)於(yu)某(mou)種(zhong)因(yin)素(su),柱(zhu)子(zi)裏(li)麵(mian)泵(beng)入(ru)了(le)大(da)量(liang)的(de)空(kong)氣(qi),損(sun)壞(huai)柱(zhu)子(zi)可(ke)能(neng)性(xing)也(ye)不(bu)是(shi)很(hen)大(da)。 那na麼me如ru果guo真zhen的de遇yu上shang這zhe種zhong情qing況kuang,該gai如ru何he處chu理li呢ne?當dang然ran是shi要yao把ba空kong氣qi從cong所suo有you通tong道dao裏li排pai出chu來lai。不bu過guo在zai這zhe之zhi前qian最zui好hao把ba柱zhu子zi取qu下xia來lai。首shou先xian換huan上shang新xin的de徹che底di脫tuo氣qi後hou的de流liu動dong相xiang,然ran後hou打da開kai排pai氣qi閥fa進jin行xing正zheng常chang灌guan注zhu (prime the pump),對於有些型號的儀器,可能需要用注射器進行手動灌注。接下來要設定一個較高的流速(比如10 mL/min)並運行幾分鍾來徹底清除泵裏麵以及管道裏麵殘留的空氣。這一步完成之後將流速調至1mL/min 並關閉排氣閥,運行直到徹底沒有氣泡排出。然後將流動相換成100%的甲醇或者乙腈並衝洗一會兒,這兩種有機溶劑的粘度相對較低有助於清除係統管道和柱子中的空氣。 dierbujiushiruhepaichuzhuzizhongdekongqi。jiangzhuzijinkouduanlianshang,baoliuchukouduanbuyaojiejianceqi,keyijieshangyiduanguandaobingyongshaobeihuozhefeiyepingshoujipaichulaideliudongxiang。qidongbengbingzhubuzengdaliusuzhidaozhuyadadao3000-4000 psi (高壓能夠將氣泡壓縮回溶液並排出柱子),持續運行10分鍾左右直到沒有氣泡從柱子的尾端排出。檢測器中可能也會有殘留的氣泡,但是很容易通過衝洗清除。 以yi上shang隻zhi是shi反fan相xiang色se譜pu柱zhu排pai氣qi的de程cheng序xu。對dui於yu其qi他ta類lei型xing的de色se譜pu柱zhu,溶rong劑ji要yao相xiang應ying的de更geng換huan成cheng兼jian容rong的de。如ru果guo柱zhu子zi不bu是shi矽gui基ji的de,要yao特te別bie注zhu意yi柱zhu子zi的de最zui大da允yun許xu柱zhu壓ya。對dui於yu由you於yu長chang期qi儲chu存cun而er變bian幹gan燥zao的de色se譜pu柱zhu,也ye可ke以yi使shi用yong相xiang同tong的de方fang法fa使shi其qi恢hui複fu良liang好hao狀zhuang態tai。 buguo,suirankongqibuhuiduisepuzhuzaochengshizhixingdeshanghai,danshibengzaimeiyouliudongxiangdezhuangtaixiachangshijianyunxingkenenghuisunhuaimifengdian。yinweiliudongxianghaichongdanglehuosaihemifengdianzhijianderunhuaji,meiyouleliudongxiangderunhuazuoyong,mifengdianjiuhenrongyimosun。suoyiyidanliudongxiangyongjinkongqijinrubeng,chulepaichukongqi,haiyaotebiezhuyijianlou。ruguomeiyouguanchadaomingxiandexielu,yaozhuyiguanchabengzaizhengchangyunxingxiadezhuyashifouzhengchanghewending,ruguozhuyameiyouwenti,jiushuomingbengshizhengchangde。ruguoguanchadaozhuyapiandihuozhebodong,shuomingmifengdiankenengmosun,xuyaogenghuanmifengdian。
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