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</p><p>比色皿( 又名吸收池，樣品池) 用來裝參比液、樣品液。配套在光譜分析儀器上，如分光光度計(jì)，血線蛋白分析儀，粒度分析儀等。比色皿是分光光度計(jì)的重要配件，一般為長方體，其底及兩側(cè)為磨毛玻璃，另兩面為光學(xué)玻璃制成的透光面粘結(jié)而成。</p><p> </p><p>比色皿的制造工藝有兩種, 一種是粘合劑粘合而成, 另一種是高溫熔融而成。比色皿的材料通常來源于石英、熔凝硅石和光學(xué)玻璃。常用比色皿的形狀有方形、矩形和圓筒形, 容量一般為幾毫升。也有用于少量試樣的微型或超微型毛細(xì)管皿。另外還有高、低溫恒溫比色皿。比色皿按照使用的波長范圍分為可見光系列(稱玻璃比色皿)，紫外可見光系列(稱石英比色皿)，紅外光系列(稱紅外石英比色皿)。</p><p> </p><p>紫外光度實(shí)驗(yàn)中的比色皿通常使用玻璃比色皿和石英比色皿，玻璃比色皿是用光學(xué)玻璃制成的比色皿，只能用于可見光區(qū)，適用于330～1000nm 波長范圍，石英比色皿是用熔融石英( 氧化硅) 制成的比色皿，既適用于紫外光區(qū)，也可用于可見光區(qū)，適用于200～400nm波長范圍。</p><p> </p><p>利用石英和玻璃比色皿在紫外光區(qū)和可見光區(qū)有無吸收的差異，在紫外光區(qū)時(shí)，由于玻璃比色皿強(qiáng)烈吸收紫外光，對實(shí)驗(yàn)數(shù)據(jù)和結(jié)果有影響，石英比色皿不吸收紫外光，不會(huì)影響數(shù)據(jù)，因此在紫外光區(qū)不使用玻璃比色皿而使用石英比色皿。而在可見光區(qū)，玻璃的影響非常小，可忽略，和石英比色皿一樣均可以使用，但考慮到節(jié)約經(jīng)濟(jì)的因素，由于玻璃比色皿的價(jià)格遠(yuǎn)遠(yuǎn)低于石英比色皿，通常選擇可見光區(qū)使用玻璃比色皿，紫外光區(qū)使用石英比色皿。</p><p> </p><p>比色皿的鑒別</p><p> </p><p>比色皿透光面是由能夠透過所使用的波長范圍的光的材料制成。在200-350nm工作的比色皿適用于紫外區(qū)，必須使用石英或熔熔硅石制成透光面的石英比色皿。石英比色皿既可用于紫外區(qū)又可用于可見區(qū)，但是價(jià)格一般比較貴哦，所以要根據(jù)使用波長選擇比色皿，如果不用紫外區(qū)的話，用普通玻璃比色皿就行了，一則浪費(fèi)沒必要，二則，嘿嘿，摔碎了也不心疼，哈哈。而普通硅酸鹽光學(xué)玻璃制成的透光面的比色皿，只能用于350nm至1000nm的可見區(qū)。(好象還能到2000nm，不過在這里不做討論了)。</p><p> </p><p>1、直觀法</p><p> </p><p>通過視覺、聽覺的不同感*法觀察和比較比色皿的外觀及澄清程度來進(jìn)行辨別。</p><p> </p><p>(1) 比色皿上通常會(huì)有字母標(biāo)識(shí)，玻璃比色皿口沿處有“G”( Glass 玻璃) ，而石英比色皿口沿處有“Q”( Quartz 石英) 或者“QS /S”( Quartz Glass 石英玻璃) 。</p><p> </p><p>(2) 如果沒有字母標(biāo)識(shí)或者標(biāo)識(shí)已磨損，可以在口沿處由上往下看，如果棱面發(fā)綠就是玻璃的，透明或發(fā)白就是石英的。更確切地說，普通玻璃的斷口是淺綠的，硼酸玻璃的斷口是泛白的，而石英的斷面是透明的。</p><p> </p><p>(3) 可以聽聲辨別，石英敲擊的聲音比較清脆，玻璃器皿敲擊時(shí)發(fā)出的聲音發(fā)悶。</p><p> </p><p>(4) 石英比玻璃的硬度大，如果把兩個(gè)比色皿對磨，石英比色皿磨損微小，而玻璃比色皿磨損比較大。</p><p> </p><p>(5) 可用白熾燈照射，透光度高的是玻璃比色皿，而石英比色皿里面應(yīng)當(dāng)稍渾濁。</p><p> </p><p>[注]: 以上都是快速簡單的鑒別方法，除非是光學(xué)專業(yè)人士，否則極易由于個(gè)人差異產(chǎn)生誤差，一般情況只能作為權(quán)宜之法。并且現(xiàn)在的制備工藝，無論是玻璃比色皿還是石英比色皿外觀都是澄清透明，厚度、質(zhì)量差別不大，因此僅通過這些感官的直觀鑒別方法在是不可取的。</p><p> </p><p>2、機(jī)試法</p><p> </p><p>使用紫外可見分光光度計(jì)來鑒別玻璃、石英比色皿和配對比色皿。</p><p> </p><p>現(xiàn)行國家檢定規(guī)程規(guī)定石英比色皿在250nm下吸光度應(yīng)小于0.07abs，若吸光度大于0.07abs 則為玻璃比色皿。</p><p> </p><p>比色皿內(nèi)不放置任何樣品，以空氣為介質(zhì)，波長設(shè)置250nm，調(diào)零。將比色皿放置在樣品道，吸光值小于0.07abs的是石英的，反之是玻璃的。</p><p> </p><p>比色皿的使用</p><p> </p><p>在使用比色皿時(shí),兩個(gè)透光面要*平行,并垂直置于比色皿架中,以保證在測量時(shí),入射光垂直于透光面,避免光的反射損失,保證光程固定。</p><p> </p><p>比色皿一般為長方體，其底及兩側(cè)為磨毛玻璃，另兩面為光學(xué)玻璃制成的透光面采用熔融一體、玻璃粉高溫?zé)Y(jié)和膠粘合而成。所以使用時(shí)應(yīng)注意以下幾點(diǎn)：</p><p> </p><p>(1) 拿取比色皿時(shí)，只能用手指接觸兩側(cè)的毛玻璃，避免接觸光學(xué)面，用力不可過大。同時(shí)注意輕拿輕放，防止破損。</p><p> </p><p>(2) 比色皿中不應(yīng)長期盛放含有腐蝕玻璃物質(zhì)的溶液。</p><p> </p><p>(3) 比色皿高溫后易爆裂，因此不應(yīng)放在火焰或電爐上加熱或干燥箱內(nèi)烘烤。</p><p> </p><p>(4) 當(dāng)比色皿里面被污染，應(yīng)用無水乙醇清洗，并晾干或及時(shí)擦拭干凈。</p><p> </p><p>(5) 比色皿的透光面不應(yīng)與硬物或臟物接觸。比色皿使用時(shí)請勿碰撞。</p><p> </p><p>(6)盛裝溶液時(shí)，高度應(yīng)為比色皿的2 /3 處，光學(xué)面如有殘液可先用濾紙輕輕吸附，然后再用鏡頭紙或絲綢順著同一方向擦拭。</p><p> </p><p>(7)比色皿中的液體，應(yīng)沿毛面傾斜，慢慢倒掉，不要將比色皿翻轉(zhuǎn)，直接口向下放在干凈的濾紙上吸干剩余液，然后用蒸餾水沖洗比色皿內(nèi)部倒掉(操作同上)避免液體外流，使第2次測量時(shí)不用擦拭比色皿，不致因擦拭帶來的誤差。</p><p> </p><p>(8)比色前將各個(gè)比色皿中裝入蒸餾水，在比色波長下進(jìn)行比較，誤差在±0.001吸光度以內(nèi)的比色皿選出4-8個(gè)進(jìn)行比色測定，可避免因比色皿差異造成測量誤差</p><p> </p><p>(9)比色皿在使用后，應(yīng)立即用水沖洗干凈。必要時(shí)可用1：1的鹽酸浸泡，然后用水沖洗干凈。</p><p> </p><p>(10)在測量時(shí)如對比色皿有懷疑，可自行檢測?？蓪⒉ㄩL選擇在實(shí)際使用的波長上，將一套比色皿都注入蒸餾水，將其中一只的透射比調(diào)至95%(數(shù)顯儀器調(diào)置100%)處，測量其它各只的透射比，凡透射比之差不大于0.5%即可配套使用。</p><p> </p><p>前人用過的經(jīng)驗(yàn)</p><p> </p><p>1 使用前將比色皿在2%的硝酸溶液中浸泡24小時(shí)，然后用水，蒸餾水依次沖洗干凈，擦干。</p><p> </p><p>2 比色前將各個(gè)比色皿中裝入蒸餾水，在比色波長下進(jìn)行比較，誤差在±0.001吸光度以內(nèi)的比色皿選出4-8個(gè)進(jìn)行比色測定，可避免因比色皿差異造成測量誤差。</p><p> </p><p>3 比色皿中的液體，應(yīng)沿毛面傾斜，慢慢倒掉，不要將比色皿翻轉(zhuǎn)，直接口向下放在干凈的濾紙上吸干剩余液，然后用蒸餾水沖洗比色皿內(nèi)部倒掉(操作同上)避免液體外流，使第2次測量時(shí)不用擦拭比色皿，不致因擦拭帶來的誤差。</p><p> </p><p>比色皿管理維護(hù)</p><p> </p><p>(1) 按照實(shí)驗(yàn)中所使用的波長來選擇相應(yīng)的比色皿( 玻璃或者石英) ，紫外光區(qū)用石英比色皿，而可見光區(qū)既可以使用玻璃比色皿，又可以使用石英比色皿?？紤]到價(jià)格問題，可見光區(qū)選用玻璃比色皿。盡量做到專人或者專組，用完清理后就交回。這樣不易搞混不同的比色皿，也不影響比色皿間的配對。</p><p> </p><p>(2) 盡量做到每個(gè)實(shí)驗(yàn)每臺(tái)紫外分光光度計(jì)有的配套比色皿，不相互混用。如有交叉使用，可記錄在冊，下次恢復(fù)正常。</p><p> </p><p>(3) 用完即清洗，清洗后在通風(fēng)陰涼處干燥，等*干燥后放入相應(yīng)裝具中。放置時(shí)，裝具保持清潔干燥，比色皿應(yīng)秉承“光面朝上，毛面在兩側(cè)”的原則，這樣便于抓取兩毛面拿出使用，不易弄污光面。</p><p> </p><p>關(guān)于比色皿配對與比色皿誤差測定的說明：</p><p> </p><p>比色皿配對比較麻煩，一般在分光光度法測定時(shí)采用比色皿誤差測定后進(jìn)行樣品的測定。</p><p> </p><p>1、比色皿配對</p><p> </p><p>樣品溶液先配成吸收度在0.6～0.8之間的濃度測定，然后用同批溶劑將溶液稀釋一倍，再測吸收度。</p><p> </p><p>從供試品溶液的配制起，平行操作兩次，并注明測定時(shí)的溫度。</p><p> </p><p>同一臺(tái)儀器測定所得二份結(jié)果間的偏差應(yīng)不超過l%。當(dāng)結(jié)果符合要求后，對各臺(tái)儀器測得的平均值進(jìn)行統(tǒng)計(jì)，若相對標(biāo)準(zhǔn)偏差不超過1.5%，則以測得的平均值為相應(yīng)藥物的吸收系數(shù)。</p><p> </p><p>現(xiàn)行的國家檢定規(guī)程中規(guī)定配對的兩只比色皿間差值不得超過±0.5%。因?yàn)樵诳梢姽鈪^(qū)，玻璃比色皿和石英比色皿都可以使用，所以可利用每對比色皿間的透光率直接進(jìn)行比較。</p><p> </p><p>使用4對比色皿，在波長500nm 下，以空氣和純水為介質(zhì)，使用透光率T 進(jìn)行測量，將每組比色皿中的一只透射率調(diào)為100%，測量另外一只透光率，凡透射率之差不大于5% ( △T = 0.005 =0.5%) ，即可配對使用。</p><p> </p><p>2、比色皿誤差測定與樣品測定</p><p> </p><p>1）任意取用2只清潔比色皿。</p><p>2）2只比色皿中加入相同的空白溶液。</p><p>3）以其中的任何一只比色皿為空白皿，調(diào)節(jié)儀器的吸收度為0;</p><p>4）測定另一只比色皿的吸收度，測得值為A0。用此比色皿測定樣品，儀器的顯示值為A，則樣品的真實(shí)測得值A(chǔ)樣=A-A0</p><p> </p><p>談到實(shí)驗(yàn)中的紫外分光光度法，大家更多關(guān)注的是紫外分光光度計(jì)的儀器性能等等，而往往忽略了比色皿，但是您知道嗎，小小的比色皿其實(shí)也有很多講究，而且對實(shí)驗(yàn)結(jié)果的影響也很明顯。</p><p> </p><p>比色皿的洗滌</p><p> </p><p>分光光度法中比色皿潔凈與否是影響測定準(zhǔn)確度的因素之一。因此，比色皿必須保持清潔和無傷痕，選擇正確的洗凈方法：玻璃和石英比色皿通?？捎美渌峄蚓凭?、丙酮、正己烷等有機(jī)溶劑清洗。</p><p> </p><p>應(yīng)按照測定的各種試劑，采用溶解中和的方法進(jìn)行清洗，原則上是: 一不能損壞比色皿的結(jié)構(gòu)和透光性能; 二能夠采用中和溶解的方法來達(dá)到比色皿干凈如初的效果。而分光光度計(jì)中比色皿潔凈與否，則是影響測定準(zhǔn)確度的因素之一。</p><p> </p><p>比色皿清洗液</p><p> </p><p>濃鹽酸：甲醇：水=1：4：3</p><p>如果比色皿被有機(jī)物污染，宜用鹽酸—乙醇(1：2)混合液浸洗，也可用相應(yīng)的有機(jī)溶劑如醇醚混合物浸泡洗滌。如：油脂污染可用石油醚浸洗，鉻天青顯色劑污染可用硝酸(1：2)浸洗等。比色皿不可用堿液洗滌，也不能用硬布、毛刷刷洗。</p><p>鉻酸洗液效果不錯(cuò)，但浸泡時(shí)間不宜過長，否則會(huì)腐蝕掉比色皿的粘接劑使其散架。另外因?yàn)樗鼤?huì)在比色皿壁上吸附而出現(xiàn)一層鉻化物的薄膜，這種薄膜很難去除，鉻酸清洗后的比色皿在紫外區(qū)間基本不透光，導(dǎo)致不能使用。</p><p>稀釋的酸浸泡，效果不錯(cuò)，但酸濃度不能太高。</p><p>也可用冷的或溫?zé)岬?40~50℃)陰離子表面活性劑的碳酸鈉溶液(2%)浸泡，可加熱10分鐘左右。對于有色物質(zhì)的污染可用HCL(3mol/L)-乙醇(1+1)溶液洗滌。</p><p>有色物質(zhì)污染的比色皿用鹽酸:乙醇(1:2)浸泡一段時(shí)間,顏色就去掉了。</p><p> </p><p>清洗步驟</p><p> </p><p>1.比色皿用完后應(yīng)當(dāng)先用適當(dāng)溶劑沖洗，注意里外都要洗到。如果溶劑無毒的話，可以裝入一半溶劑后，用手指按住比色皿的兩端，用力搖晃，次數(shù)應(yīng)當(dāng)是不少于三次。</p><p>2.然后用大量的自來水沖洗，這一步對水溶液和鹽溶液非常重要。當(dāng)然如果所用溶劑不親水這步可以放棄。</p><p>3.后再用去離子水清洗,注意里外都要洗到，如果溶劑不親水的這一步也可放棄。</p><p>4.洗完后不要刻意的將比色皿擦干，虛放在比色皿盒內(nèi),不用蓋上讓其自然揮干。</p><p> </p><p>注意</p><p>清洗在用后立即進(jìn)行,否則樣品干后就更難處理;</p><p>洗好的比色皿應(yīng)當(dāng)是透明,沒有水跡的;</p><p>經(jīng)常使用的比色皿可以在洗凈后浸泡在純水或分析純乙醇里中保存。</p> </div> <div id="c2wplovdesa" class="NyPro_PrevNext"> <p class="NyProPrev"><img 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