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<h1>氣相色譜法測定液氧中碳?xì)浠衔锏臐舛?/h1> <div id="bfbfzpp" class="authorTimeSource"> <span>作者：</span> <span>時間：2013-12-26</span> <span>來源：網(wǎng)絡(luò)</span> <link rel="stylesheet" type="text/css"/> <span style="float:right; width:130px;margin-right:0px; text-align:right;"> <div id="55dj555" class="nav0"> <ul> <li><a href="javascript:void(0);"><img src="http://www.ex-cimer.com/event/action/images/icon_add_4.png" width="20" border="0" align="absmiddle" />加入技術(shù)交流群</a> <ul> <li style="text-align:center;"><img src="http://www.ex-cimer.com/event/company/images/code_1.jpg" width="130"><br />掃碼加入<br />和技術(shù)大咖面對面交流<br />海量資料庫查詢</li> </ul> </li> </ul> </div> </span> <span style="float:right; width:30px;margin-right:0px; text-align:right;"><a rel="nofollow">收藏</a></span> </div> <div id="rj55lff" class="hAd4_Afinal20a_back">  <iframe id='a890e388' name='a890e388' src='https://ad.eepw.com.cn/www/delivery/afr.php?zoneid=88&cb=INSERT_RANDOM_NUMBER_HERE' frameborder='0' scrolling='no' width='660' height='60'><a target='_blank'><img src='https://ad.eepw.com.cn/www/delivery/avw.php?zoneid=88&cb=INSERT_RANDOM_NUMBER_HERE&n=a635e61e' border='0' alt='' /></a></iframe> </div> <div style="margin-top:28px;"></div> <div id="vp3h5n5" class="content" id="contentDiv" style="position:relative;"> <div id="rjf5j55" class="ad_300x180_Afinal13_back">  <iframe id='a225770a' name='a225770a' src='https://ad.eepw.com.cn/www/delivery/afr.php?zoneid=87&cb=INSERT_RANDOM_NUMBER_HERE' frameborder='0' scrolling='no' width='300' height='200'><a target='_blank'><img src='https://ad.eepw.com.cn/www/delivery/avw.php?zoneid=87&cb=INSERT_RANDOM_NUMBER_HERE&n=a576c0a2' border='0' alt='' /></a></iframe> </div> <span id="contentlabels" style="font-size:14px;"><li id="ppd5p11" class=tob_wzb_lbp sizset="50" sizcache05922916163652967="3"><P>　　空分設(shè)備長期運行后，入塔空氣中殘存的微量乙炔和其他<a class="contentlabel" href="http://www.ex-cimer.com/news/listbylabel/label/碳?xì)浠衔?><em>碳?xì)浠衔?/em></a>在<a class="contentlabel" href="http://www.ex-cimer.com/news/listbylabel/label/液氧"><em>液氧</em></a>中必然會逐漸濃縮，當(dāng)含量超過其溶解度時就會出現(xiàn)固體顆粒析出，從而構(gòu)成了對空分生產(chǎn)的極大危害。為確?？辗窒到y(tǒng)長周期安全運行，所以對<a class="contentlabel" href="http://www.ex-cimer.com/news/listbylabel/label/液氧"><em>液氧</em></a>中乙炔和其他<a class="contentlabel" href="http://www.ex-cimer.com/news/listbylabel/label/碳?xì)浠衔?><em>碳?xì)浠衔?/em></a>的含量進(jìn)行分析監(jiān)測，以便為空分生產(chǎn)提供可靠的分析依據(jù)。</P><P sizset="50" sizcache05922916163652967="3">　　1 分析所用<span id="bnj555r" class=hrefStyle>儀器</SPAN></P><P sizset="51" sizcache05922916163652967="3">　　HZT-02型痕量總烴色譜分析儀。電腦數(shù)據(jù)處理氫氣發(fā)生器高純氮氣一瓶<span id="rrn5hzp" class=hrefStyle>儀表</SPAN>空氣。</P><P>　　氣源要求：要求氫氣必須為超純且干燥?？諝鉃闊o油且干燥空氣，采用瓶裝氮氣作載氣，純度為99.995%以上。</P><P>　　2 分析方法</P><P>　　2.1色譜柱的選擇</P><P>　　若要成功地分析樣品，必須針對分析對象正確選擇柱子的類型，柱長和內(nèi)徑等。以便能快速高效地分析樣品。</P><P>　　色譜柱選擇：根據(jù)廠家提供及日常分析所需選用1米不銹鋼調(diào)試柱和1#濃縮柱總之色譜柱是決定分離好壞的核心，一只質(zhì)量好的色譜柱應(yīng)該拄效高，選擇性好，內(nèi)壁惰性和使用溫度范圍寬</P><P>　　2.2載氣及其流速的選擇</P><P>　　對一定的色譜柱和試樣來說，有一個最佳載氣流速，此時柱效最高。此外，還必須考慮檢測器的類型，不同類型的檢測器對載氣有不同的要求。尤其是使用氫焰離子檢測器(FID)時，最大靈敏度需要一定<a class="contentlabel" href="http://www.ex-cimer.com/news/listbylabel/label/濃度"><em>濃度</em></a>的含有所需化合物的標(biāo)準(zhǔn)樣品來優(yōu)化流量，用該標(biāo)樣在不同載氣，空氣和氫氣流量進(jìn)行實驗來確定產(chǎn)生最大響應(yīng)的流量，其中起決定作用的變量是氫氣和載氣的比率。</P><P>　　根據(jù)廠家提供和實驗，我們廠選定以下進(jìn)樣系統(tǒng)的壓力：</P><P>　　載氣：0.08MPa氫氣：0.04MPa空氣：0.055MPa</P><P>　　2.3柱溫的選擇</P><P>　　柱溫是一個重要的操作參數(shù)，直接影響分離度和分析速度。首先柱溫不能超過柱子的最高使用溫度。一般提高柱溫使各組分揮發(fā)靠近，不利于分離，若柱溫太低，則峰形變寬，柱效下降，分析時間延長。選擇的一般原則是在使最難分離的組分盡可能好的分離前提下，盡可能地采用較低的柱溫，但以峰形不拖位尾，保留時間適當(dāng)為基準(zhǔn)。若試樣的沸點范圍較寬，宜采用程序升溫。具體操作條件的選擇應(yīng)根據(jù)不同的實際情況而定。</P><P>　　我們所要分析的是C4以內(nèi)的氣態(tài)烴，沸點范圍雖然不是太寬，但對柱溫的改變也相當(dāng)靈敏。一般若恒溫可以滿足分析要求時，盡量不采用程序升溫，經(jīng)過實驗，我們將柱溫設(shè)定為50度，檢測器溫度100度。</P><P>　　2.4分析法的選擇</P><P>　　從理論上來講，分析方法有歸一法，內(nèi)標(biāo)法和外標(biāo)法三種。但是<a class="contentlabel" href="http://www.ex-cimer.com/news/listbylabel/label/液氧"><em>液氧</em></a>中<a class="contentlabel" href="http://www.ex-cimer.com/news/listbylabel/label/碳?xì)浠衔?><em>碳?xì)浠衔?/em></a>組分含量是不能確定的，各組分<a class="contentlabel" href="http://www.ex-cimer.com/news/listbylabel/label/濃度"><em>濃度</em></a>范圍變化不大，屬同質(zhì)痕量組分的氣體樣品分析。根據(jù)這些特性，外標(biāo)法比較適合，且方便而快捷。所以我們采用外標(biāo)法作為定量分析。具體做法即通過標(biāo)樣分析，求出對應(yīng)組分的校正因子。近而求出對應(yīng)組分的含量。校正因子的測定是關(guān)鍵，因為若想得到各組分的準(zhǔn)確含量，必須確保校正因子準(zhǔn)確無偏差，進(jìn)樣量多少要適中，一般為1ml。</P><P>　　色譜峰定量之前，必須首先定性。我們所分析的標(biāo)樣是混合氣體，必須將各成份一一定性，即配制和混合氣體中<a class="contentlabel" href="http://www.ex-cimer.com/news/listbylabel/label/濃度"><em>濃度</em></a>相當(dāng)?shù)母鲗?yīng)單一組份，分別進(jìn)樣分析定性。</P><P>　　3 結(jié)論</P><P sizset="52" sizcache05922916163652967="3">　　采用氫火焰離子化氣相<span id="5lp3vfd" class=hrefStyle>色譜儀</SPAN>可以圓滿解決液氧中碳?xì)浠衔锏姆治鰡栴}，而且也可分析液空，氧槽中碳?xì)浠衔?。而且穩(wěn)定性好，操作方便，保證了空分的安全生產(chǎn)。</P></LI> </span>  <div class="3fznjhx" id="coverDiv" class="article_reg" style="width:100%;overflow:hidden;display:none;z-index:10;position:absolute;left:0;background:#fff;"> <center> <img src="https://webstorage.eepw.com.cn/images/display/reg.jpg" border="0" usemap="#Map" /> <map name="Map" id="Map"> <area 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