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<span>水質(zhì)化學(xué)需氧量的測(cè)定重鉻酸鹽法的步驟</span></p> </div>   <div id="b7fjpbd" class="ly_NyNewsdetail"> <h1 class="NyNewsdetail_title">水質(zhì)化學(xué)需氧量的測(cè)定重鉻酸鹽法的步驟</h1> <div id="vtjzfff" class="NyNewsdetail_tips">更新時(shí)間：2019-12-21 點(diǎn)擊次數(shù)：3580</div> <div id="vfj5zlz" class="NyNewsdetail_con"> <p><span style="font-size:10.5000pt"><span style="font-family:宋體"> 對(duì)于COD</span></span><strong><span style="font-size:10.5pt"><span style="font-family:宋體">（</span></span></strong><strong><span style="font-size:10.5pt"><span style="font-family:calibri">COD</span></span></strong><strong><span style="font-size:10.5pt"><span style="font-family:宋體">在線(xiàn)監(jiān)測(cè)儀</span></span></strong><span style="font-size:10.5000pt"><span style="font-family:宋體">）</span></span><span style="font-size:10.5000pt"><span style="font-family:宋體">值小于50 mg/L的水樣，應(yīng)采用低濃度的重鉻酸鉀標(biāo)準(zhǔn)溶液(4.5.2)氧化，加熱回流以后，采用低濃度的硫酸亞鐵銨標(biāo)準(zhǔn)溶液((4.6.4)回滴。 </span></span></p><p><span style="font-size:10.5000pt"><span style="font-family:宋體"> 該方法對(duì)未經(jīng)稀釋的水樣其測(cè)定上限為700 mg/L，超過(guò)此*必須經(jīng)稀釋后測(cè)定。 </span></span></p><p><span style="font-size:10.5000pt"><span style="font-family:宋體"> 對(duì)于污染嚴(yán)重的水樣，可選取所需體積1/10的試料和1/10的試劑，放入10 mm</span></span><span style="font-size:10.5000pt"><span style="font-family:arial">×</span></span><span style="font-size:10.5000pt"><span style="font-family:宋體"> 150mm硬質(zhì)玻璃管中，搖勻后，用酒精燈加熱至沸數(shù)分鐘，觀察溶液是否變成藍(lán)綠色。如呈藍(lán)綠色，應(yīng)再適當(dāng)少取試料，重復(fù)以上試驗(yàn)，直至溶液不變藍(lán)綠色為止。從而確定待測(cè)水樣適當(dāng)?shù)南♂尡稊?shù)。 </span></span></p><p><span style="font-size:10.5000pt"><span style="font-family:宋體"> 取試料(6.2)于錐形瓶中，或取適量試料加水至20.0 ml。</span></span></p><p><span style="font-size:10.5000pt"><span style="font-family:宋體"> 空白試驗(yàn)：按相同步驟以20.0 ml水代替試料進(jìn)行空白試驗(yàn)，其余試劑和試料測(cè)定(7.8)相同，記錄下空白滴定時(shí)消耗硫酸亞鐵銨標(biāo)準(zhǔn)溶液的毫升數(shù)V</span></span><sub><span style="font-size:10.5000pt"><span style="font-family:宋體">1</span></span></sub><span style="font-size:10.5000pt"><span style="font-family:宋體">。</span></span></p><p><span style="font-size:10.5000pt"><span style="font-family:宋體"> 校核試驗(yàn)：按測(cè)定試料((7.8)提供的方法分析20.0 ml鄰苯二甲酸氫鉀標(biāo)準(zhǔn)溶液((4.7)的COD </span></span><strong><span style="font-size:10.5pt"><span style="font-family:宋體">（</span></span></strong><strong><span style="font-size:10.5pt"><span style="font-family:calibri">COD</span></span></strong><strong><span style="font-size:10.5pt"><span style="font-family:宋體">在線(xiàn)監(jiān)測(cè)儀</span></span></strong><span style="font-size:10.5000pt"><span style="font-family:宋體">）</span></span><span style="font-size:10.5000pt"><span style="font-family:宋體">值，用以檢驗(yàn)操作技術(shù)及試劑純度。 </span></span></p><p><span style="font-size:10.5000pt"><span style="font-family:宋體"> 該溶液的理論COD值為500 mg/L，如果校核試驗(yàn)的結(jié)果大于該值的96%，即可認(rèn)為實(shí)驗(yàn)步驟基本上是適宜的，否則，必須尋找失敗的原因，重復(fù)實(shí)驗(yàn)，使之達(dá)到要求。 </span></span></p><p><span style="font-size:10.5000pt"><span style="font-family:宋體"> 去干擾試驗(yàn)：無(wú)機(jī)還原性物質(zhì)如亞硝酸、硫化物及二價(jià)鐵鹽將使結(jié)果增加，將其需氧量作為水樣COD值的一部分是可以接受的。 </span></span></p><p><span style="font-size:10.5000pt"><span style="font-family:宋體"> 該實(shí)驗(yàn)的主要干擾物為氯化物，可加入硫酸汞((4.2)部分地除去，經(jīng)回流后，氯離子可與硫酸汞結(jié)合成可溶性的氯汞絡(luò)合物。 </span></span></p><p><span style="font-size:10.5000pt"><span style="font-family:宋體"> 當(dāng)氯離子含量超過(guò)1000mg/L時(shí)，COD</span></span><strong><span style="font-size:10.5pt"><span style="font-family:宋體">（</span></span></strong><strong><span style="font-size:10.5pt"><span style="font-family:calibri">COD</span></span></strong><strong><span style="font-size:10.5pt"><span style="font-family:宋體">在線(xiàn)監(jiān)測(cè)儀</span></span></strong><span style="font-size:10.5000pt"><span style="font-family:宋體">）</span></span><span style="font-size:10.5000pt"><span style="font-family:宋體">的低允許值為250 mg/L，低于此值結(jié)果的準(zhǔn)確度就不可靠。 </span></span></p><p><span style="font-size:10.5000pt"><span style="font-family:宋體"> 水樣的測(cè)定：于試料((7.4)中加入10.0 ml重鉻酸鉀標(biāo)準(zhǔn)溶液(4.5.1)和幾顆防爆沸玻璃珠(4.9)，搖勻。 </span></span></p><p><span style="font-size:10.5000pt"><span style="font-family:宋體"> 將錐形瓶接到回流裝置(5.1)冷凝管下端，接通冷凝水。從冷凝管上端緩慢加入30 ml硫酸銀-硫酸試劑((4.4)，以防止低沸點(diǎn)有機(jī)物的逸出，不斷旋動(dòng)錐形瓶使之混合均勻。自溶液開(kāi)始沸騰起回流兩小時(shí)。 </span></span></p><p><span style="font-size:10.5000pt"><span style="font-family:宋體"> 冷卻后，用20~30ml水自冷凝管上端沖洗冷凝管后，取下錐形瓶，再用水稀釋至140 ml左右。 </span></span></p><p><span style="font-size:10.5000pt"><span style="font-family:宋體"> 溶液冷卻至室溫后，加入3滴1,10-菲繞琳指示劑溶液((4.8)，用硫酸亞鐵銨標(biāo)準(zhǔn)滴定溶液(4.6)滴定，溶液的顏色由黃色經(jīng)藍(lán)綠色變?yōu)榧t褐色即為終點(diǎn)。記下硫酸亞鐵銨標(biāo)準(zhǔn)滴定溶液的消耗毫升數(shù)V</span></span><sub><span style="font-size:10.5000pt"><span style="font-family:宋體">2</span></span></sub><span style="font-size:10.5000pt"><span style="font-family:宋體">。 </span></span></p> </div> <div id="rd5fvxf" class="ly_PrevNext"> <ul> <li>上一篇：<a href="/szhcy-Article-2073455/">ORP電極的校準(zhǔn)和維護(hù)</a></li> <li>下一篇：<a href="/szhcy-Article-2070174/">總氮的測(cè)定</a></li> </ul> 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