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style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">空白試驗(yàn)值偏高的原因</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">空白試驗(yàn)測(cè)得的結(jié)果偏高，原因有很多，我們從實(shí)際例子來分析原因。</span></span></p><p style="margin-left:0.0000pt"> </p><p style="margin-left:0.0000pt"><strong><span style="font-size:9.5pt"><span style="font-family:arial">一、水中石油類空白</span></span></strong></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">【分析原因】</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">1.四氯化碳對(duì)空白值的影響</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">大部分市售四氯化碳都存在空白值高的問題，所以四氯化碳用環(huán)保級(jí)，紅外型。</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">2.無水硫酸鈉對(duì)空白值得影響</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">用純水處理過的無水硫酸鈉直接用于實(shí)驗(yàn)空白值普遍偏高，經(jīng)過四氯化碳沖洗的無水硫酸鈉測(cè)定空白值會(huì)有所降低。</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">3.硅酸鎂對(duì)空白值得影響</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">將硅酸經(jīng)過四氯化碳預(yù)處理過的空白值也會(huì)明顯下降</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">4.漏斗對(duì)空白值得影響</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">漏斗和濾紙污染、不潔凈都會(huì)使空白值偏高，都需要用四氯化碳預(yù)處理</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">5.器皿清潔度對(duì)空白值的影響</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">試劑對(duì)空白值得影響很大，但在實(shí)驗(yàn)全過程當(dāng)中所接觸的全部器皿對(duì)空白值得影響也不容忽視。</span></span></p><p style="margin-left:0.0000pt"> </p><p style="margin-left:0.0000pt"><strong><span style="font-size:9.5pt"><span style="font-family:arial">二、水質(zhì)中氨氮空白</span></span></strong></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">【分析原因】</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">1.測(cè)定使用的蒸餾水被污染，含有影響實(shí)驗(yàn)結(jié)果的雜質(zhì)，比如蒸餾水含氨。</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">2.試管、移液管等儀器沒有清洗*，這些因素對(duì)實(shí)驗(yàn)結(jié)果也有較大的影響。</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">3.實(shí)驗(yàn)所用的無氨水質(zhì)量不佳，含氨量比較高，導(dǎo)致實(shí)驗(yàn)得到的空白值偏高，這是主要的原因。</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">4.在配制酒石酸鉀鈉和鈉氏試劑時(shí)出現(xiàn)較大偏差，導(dǎo)致實(shí)驗(yàn)所用的試劑純度（酒石酸鉀鈉、鈉氏試劑）不佳，從而導(dǎo)致實(shí)驗(yàn)得到的空白值偏高。</span></span></p><p style="margin-left:0.0000pt"> </p><p style="margin-left:0.0000pt"><strong><span style="font-size:9.5pt"><span style="font-family:arial">三、總氮空白值偏高的原因？</span></span></strong></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">【分析原因】</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">1、試劑的配制</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">堿性過硫酸鉀的配制過程十分重要，掌握不好，會(huì)影響消解效果，對(duì)測(cè)定結(jié)果產(chǎn)生一定的影響。配制該溶液時(shí)，可分別稱取過硫酸鉀和氫氧化鈉，兩者分開配制，再混合定容，或者先配制氫氧化鈉溶液，待其溫度降到室溫后再加入過硫酸鉀溶解。若二者在一只燒杯中溶于水，應(yīng)緩慢加水，同時(shí)攪拌，防止氫氧化鈉放熱使溶液溫度過高引起局部過硫酸鉀失效。</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">2、玻璃器皿的洗滌</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">所使用的玻璃器皿應(yīng)先用（1+9）鹽酸浸泡后，再用無氨水沖洗數(shù)次才能使用，否則，也會(huì)造成空白值偏高或平行性較差的情況。</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">3、比色時(shí)的注意事項(xiàng)</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">該項(xiàng)目的測(cè)定涉及兩個(gè)波長(zhǎng)（220nm和275nm），建議在測(cè)定完一組樣品的同一波長(zhǎng)后，再調(diào)整到另一波長(zhǎng)，統(tǒng)一測(cè)定，不要測(cè)完一個(gè)樣品的兩個(gè)吸光度后再換另一個(gè)樣品，這樣反復(fù)調(diào)整波長(zhǎng)會(huì)引起一定的測(cè)量誤差。</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">4、試劑的選擇</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">堿性過硫酸鉀消解紫外分光光度法測(cè)定總氮的過程中，過硫酸鉀是至關(guān)重要的試劑。首先，試劑的純度關(guān)系到空白值的高低、測(cè)定結(jié)果的準(zhǔn)確度。一般普通分析純過硫酸鉀的總氮含量不超過0.005%，但由于試劑質(zhì)量存在差異，有些廠家、批次的試劑含氮量常常達(dá)不到這個(gè)要求，致使空白值偏高。因此，有條件的話建議使用優(yōu)級(jí)純?cè)噭?，盡量降低試劑中的含氮量，從而降低實(shí)驗(yàn)空白值。</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">5、實(shí)驗(yàn)用水及試劑的質(zhì)量檢驗(yàn)</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">若實(shí)驗(yàn)的空白值不夠理想，則需要對(duì)實(shí)驗(yàn)用水及試劑進(jìn)行檢驗(yàn)，以選擇出含氮量低的水和試劑，獲得理想的空白值。</span></span></p><p style="margin-left:0.0000pt"><span style="font-size:9.5pt"><span style="font-family:arial">由于檢測(cè)儀器和玻璃量器定期檢定，以及采取了全面的質(zhì)量管理措施，因此，若測(cè)定的空白實(shí)驗(yàn)值太大，一般是化學(xué)藥品純度不夠，配制的試液變質(zhì)或被污染等原因。應(yīng)重新配制試液，返工重測(cè)該批樣品，直至空白實(shí)驗(yàn)值合格。</span></span></p> </div> <div id="aqgwbbhhdpu" class="NyPro_PrevNext"> <p class="NyProPrev"><img 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