jiangyangpinguanfangrujiarebao,yongjinshujiarebaojiagudinghao,ranhouzaijiangyangpinguanzhuangdaotuoqizhankoushang。zaisuoyouxuyaotuoqideyangpindouzhuangdaotuoqizhankouhou,kaishituoqi,zheshibeixuantuoqizhandezhishidengdianliang,zaixiangyingtuoqizhandeshuziwenkongqishangshezhiyuchuliwendu300℃。若樣品在300℃會(hui)分(fen)解(jie),則(ze)應(ying)設(she)置(zhi)較(jiao)低(di)的(de)溫(wen)度(du)。應(ying)該(gai)將(jiang)脫(tuo)氣(qi)溫(wen)度(du)清(qing)楚(chu)地(di)寫(xie)入(ru)打(da)印(yin)報(bao)告(gao)中(zhong)。脫(tuo)氣(qi)開(kai)始(shi)後(hou),計(ji)算(suan)機(ji)將(jiang)自(zi)動(dong)控(kong)製(zhi)樣(yang)品(pin)管(guan)內(nei)壓(ya)力(li)逐(zhu)漸(jian)降(jiang)低(di)並(bing)加(jia)熱(re)。
duiyufenmoyangpindetuoqi,xuyaozhixingyixiaguocheng,yibimianyangpinyinchouzhenkongyangdaoguanjingbingzusaituoqizhanzhongdelvwang,shenzhiwuranfamenxitongzaochenglouqi。gaifangfayunyongyufenzishai,qingzhifenmohekenenghanyoudaliangshuiqihuotanqinghuahewudeyangpin。yangpinqianchuliguochengruxia:
1.將空樣品管連同其填充棒一起稱毛重,方法同前述。
2.將樣品裝入樣品管後,插回填充棒,並在樣品管頸口處填塞少量合適的玻璃毛。
3.設置初始溫度90℃,並在該溫度下抽真空10±1分鍾。
4.填加溫度至100℃,再抽真空10分鍾。
5.在110℃重複步聚3,這時所有的水會被有效地去除。
6.增加溫度至300℃,如果樣品吸附的雜質氣較多,則應先在150℃真空脫氣2-4小時。
在最少2個小時脫氣後,檢查樣品以確保脫氣完全。分子篩和其他吸濕性樣品應該至少脫氣4小時。如果可能,最好能脫氣過夜。檢查脫氣效果的方法是:在zai手shou動dong狀zhuang態tai下xia關guan閉bi歧qi管guan和he連lian接jie真zhen空kong泵beng的de閥fa門men,如ru果guo樣yang品pin管guan或huo歧qi管guan內nei壓ya力li穩wen定ding或huo上shang升sheng極ji為wei緩huan慢man,則ze說shuo明ming脫tuo氣qi完wan全quan,可ke以yi用yong來lai分fen析xi。如ru果guo不bu是shi,則ze延yan長chang或huo重zhong複fu脫tuo氣qi過guo程cheng。
guandiaojiarebaowendu,qingqingdijiangyangpinguancongjiarebaozhongtuichu,jiangyangpinguanlengquezhishiwen,zheshiyangpinguanzhongbeihuitianhaiqi,suijikeyicongtuoqizhanquxia。ruoshiyonglebolimaosai,xuquchubinglijigaishangyuchengkongguanshixiangtongdesaizi。chengzhongzhi0.1mg,減除毛重,即為脫氣樣品的重量。
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