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              水分儀的幾種主要測試方法分析

              文章出處:未知人氣: 76 發布時間:2019-01-27 11:14

                各種水分測定儀的比較

                市售的水分測定儀有很多,按測試方法分有以下幾種:

                紅外線干燥法、鹵素快速水分儀類儀器,此類水分儀特點:體積小,測定范圍比較寬,精確度較高,性能較穩定適合0.01%-的水分測量、結構簡單,價格低廉。但是次水分儀測試含有易揮發物質的產品時不太適合。

                卡爾費休庫侖法類儀器,主要原理:利用化學反應后電導率變化計算,結構復雜,體積較大,測定精確度高,適合水分含量在100PPm(0.01%)以下的測定。它一般用于陰離子聚合等對水分有非常嚴格要求的化工、醫藥等行業產品測定,價格較高,該類儀器有一個不好的特點,就是更換溶劑時不容易找平衡。比較適合每日上百次的多頻次測試。

                卡爾費休容量法,結構比較簡單,精確度好,適合水分含量10PPm-10%的測定,一般用于對水分有嚴格要求的化工、醫藥和包裝等行業產品測定,可以看出,對于一般液體化工產品,測定的水分含量時,應該使用卡爾費休容量法水分測定儀,可以滿足每日數十次以下測定的要求,且經濟性比較好。該儀器有一個特點,就是測試時可以通過目測觀察儀器是否正常(在滴定終點時顯示淺咖啡色)。

              水分儀的幾種主要測試方法分析

                卡爾費休容量法水分測定的測定原理

                卡爾費休容量法測定水分含量時,主要依據電化學反應:

                I2+2eó2I-

                在反應池的溶液中同時存在I2和I-時,該反應在電極的正負兩端同時進行,即在一個電極上I2被還原,而在另一個電極上I-被氧化,因此在兩個電極之間有電流通過。如果溶液中只有I-而無I2同時存在,則兩個電極間沒有電流通過。

                卡爾費休試劑中含有效成分吡啶和碘等物質,把其計量滴入反應池,能與待測溶液中的水發生如下化學反應:

                H2O+SO2+I2+3C5H 5N→2C5H5N·HI+C5 H5N·SO3

                C5H5N·SO3+CH3 OH→C5H5N·HSO4CH3

                C5H5N·HI→C5H5N·H++ I-

                該反應持續進行,不斷消耗水,生成I-,一直到反應滴定終點,水分消耗完畢。這時,溶液有微量未發生反應的卡爾費休試劑存在,才能發生I2和I-同時存在的情況,兩個鉑電極之間的溶液開始導電,由電流指示達到終點,停止滴定。從而通過計量已消耗的卡爾費休試劑體積(容量)來標定溶液中的水分含量。

                卡爾費休電量法的測定原理

                電量法,是基于將試樣溶于含有一定碘的特殊溶劑的電解液后,水即消耗碘,但所需的碘不再是用已標定過的含碘試劑去進行滴定,而是通過電解過程,使溶液中的碘離子在陽極氧化為碘:

                2Iˉ—2e ─→I2

                所產生的碘又與樣品中的水反應。其終點用雙鉑電極指示。當電解液中碘濃度恢復到原定濃度時,停止電解。然后根據法拉第電解定律:

                C M i·t

                m=---------×----- = ---------

                96500 n 10722

                計算出待測試樣的水分含量。

                選購水分測定儀的注意事項

                對于市售的各種卡爾費休容量法水分測定儀,建議化工廠家根據性價比排列,選擇購買時注意以下幾點:

                1、 選擇時考慮自動型儀器。手動的水分測定儀需要試驗者對玻璃滴定管中的試劑進行目測,在達到終點后也需要手動關閉,因各人動作習慣不同而遲延,會帶來不必要的誤差。

                2、 選擇時應考慮購買全密閉測試系統。裸露的卡爾費休試劑因為碘的存在,非常容易吸收水分,待測樣品也應盡量避免空氣中水分溶入而產生誤差的情況。

                3、 應考慮計量泵的壽命問題。計量泵是屬于容量法水分儀的關鍵部分,卡爾費休試劑又是腐蝕性很高的試劑,應盡量選購由氟塑料等耐腐蝕的材料制成的計量泵,防止產生泄漏,導致儀器的報廢。

                4、 電極問題。該部分屬于儀器的核心部件,一方面應具有較高的靈敏度,另一方面,因其測試時浸泡在試驗池中,選擇配備優質的鉑電極儀器,以保持電極壽命。

                另外,要得到精確的測試結果,水分測定儀在使用過程中除了要嚴格按照規程操作外,還應該注意以下問題(以ZD-2型全自動水分測定儀為例):

                ■系統全密閉問題。卡爾費休試劑液路部分連接一定要緊固,從試劑瓶到計量泵再到反應池,否則發生試劑泄漏將直接影響測試結果。其不密閉的另一個問題是測試時由于卡爾費休試劑在試驗中吸收空氣水分,會導致滴定終點延遲。

                ■取樣的準確問題。在標定卡爾費休試劑時需要取用10mg水,盡量使用10ul取樣器,這樣不但準確、速度快,還能夠防止水滴粘附。同樣地,取用甲醇試劑、乙酯也有類似的問題,取放完畢后應注意盡量縮短反應池打開的時間。

                ■磁性攪拌速度調整。在反應池中,因為滴定試劑加入時在局部,與電極不在一處,因此攪拌速度以快到不形成湍流為止,這樣可以最快達到終點。

                ■滴定速度設定應先快后慢。滴定時先快速以盡量縮短試驗時間,而在接近終點時應變慢,這樣可提高計量精確度。

                ■當日試驗完畢后,一定要排空系統中的卡爾費休試劑,然后用甲醇清洗干凈,千萬不能用水清洗系統,因為其不容易揮發,將造成下次試驗時卡爾費休試劑標定不實。

                ■水分測定儀應該遠離強磁場,避免工作時電子顯示跳動,出現不正常現象。

                手動的水分測定儀,因為必須使用玻璃自動滴定管計量卡爾費休試劑和甲醇溶劑,而玻璃滴定管本身因為平衡壓力的關系,又必須與外界接通。除了上面需要注意的方面外,在使用時,還應該注意以下兩點:

                ■系統盡量密閉。手動的水分測定儀需要在吸球管路和玻璃滴定管上口加接填充干燥劑的U型管,以便減少空氣水分對測試結果的干擾。在空氣相對濕度大于70%的環境下,應盡量不安排水分測試。

                ■在調整滴定管的滴定速度時,調整到1滴/秒。滴定速度太快將導致到達終點時產生的延時誤差較大;而滴定速度太慢則會延長測試的過程,上述干擾容易導致遲遲不到達終點。

                卡爾費休容量法水分測定過程

                在卡爾費休容量法水分測定儀中,有幾種可供選擇的種類,其連接、測定也有所不同,但測定的基本過程相似。其測定過程如下:

                1、 消除溶液空白

                在反應池中加入無水甲醇試劑10-15ml(浸沒電極),打開滴定管開始注液,將卡爾費休試劑注入反應池,直至甲醇中的微量水分完全反應完畢,儀器將自動停止并發出報警聲。

                2、 標定卡爾費休試劑

                按復零鍵,用容量為10ul的取樣器取10mg(10ul)蒸餾水放入反應池中,按滴定開始鍵,儀器開始自動滴定,到達終點時蜂鳴器響,到達終點時指示燈亮,此時數碼管顯示的就是10mg水所消耗的卡爾費休液的體積數,由此可計算出每毫升卡爾費休消耗的水的量。

                F=10/A

                式中:F-每毫升卡爾費休溶液消耗水的量

                10—稱取水的質量(毫克)

                A一滴定所消耗的卡爾費休試劑的量

                3、 測定水分含量

                按復零鍵,用取樣器取10ml被測的樣品,加入反應池中。按滴定開始鍵,開始進行滴定,到達終點時蜂鳴器響,終點指示燈亮,其結果按下式計算:

                水分含量=A1×F/10000

                式中:A1一樣品所消耗的卡爾費休溶液的體積量

                F一每毫升卡爾費休液消耗水的質量

                10000指加入10ml樣品的質量數。

                上述兩步反應式綜合計算得:乙酯水分含量=

                卡爾費休方法可用于各種有機化工產品(醛、酮類產品需要配備另外的試劑)。

                精確測定產品中的水分含量,不但可事先避免生產中的質量問題,把損失降低到最小程度,而且可與原料廠家進行有據交涉,退換不適用的產品。 但是對于操作人員來說一定要注意,因為此方法需要用試劑,而試劑呢又特別容易對人體構成危害。所以操作的時候一定要佩戴防護措施!!1

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