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密閉微波制樣系統機械及電路常見異常現象分析

熱度0票  瀏覽141次 時間:2014年6月25日 13:28
密閉微波制樣系統機械及電路常見異常現象分析
文/金宇

密閉微波制樣系統是采用2450MHz 微波頻率的微波在密閉增
壓的條件下加熱,達到樣品消解的一種新興而高效的樣品處理技
術。在微波加熱過程中會產生高壓,操作不當會發生消解罐爆裂
甚至爆炸的危險。本文就這一系統機械及電路上常出現的異常現
象作一詳細分析并提出相對應的排除故障辦法及預防措施。

【關鍵詞】微波加熱 電器元件 額定電壓 主控電路板

1 前言
微波加熱是直接通過物質吸收微波能量來達到快速加熱的目的。用密閉容器又能同時
獲得高溫、高壓,不僅可以提高反應速率,而且可提高試樣的分解能力,從而達到理想的消
解效果。具有自動控壓和控溫的密閉微波溶樣是目前世界上樣品前處理最先進和最理想的方
法之一,它具有樣品處理完全、徹底,速度快(是傳統方法的 10-100 倍),污染少等常規
方法無可比擬的優越性。
密閉微波制樣系統是采用 2450MHz 微波頻率的微波在密閉增壓的條件下加熱,易產生
高壓、超壓。同時,樣品處理有化學反應,樣品的千差萬別使處理過程更具復雜性和危險
性,操作不當就可能造成消解罐爆裂甚至爆炸的危險。現以新儀 MDS 系列為例將密閉微波
制樣系統在使用過程中出現的常見機械、電路故障進行分析并提出相應的處理辦法和預防措施。

2 密閉微波制樣系統故障處理方法
(1)當顯示屏顯示的數字已到設定的壓力,微波已停止加熱,微波指示燈已熄滅,但
顯示屏上的顯示壓力數字沒有停止并迅速上升。這是壓力過沖造成的。一般是由于樣品中
含有大量有機物,其某些成分達到一定壓力 /溫度時發生激烈反應。這種現象應對含有大量
有機物和成分復雜的樣品(如化妝品等)進行樣品預處理并要處理適度;對不了解其化學性
質的樣品,第一工步壓力小于 0.5Mpa,第二工步壓力小于 1Mpa。待劇烈反應完成后再慢
慢增加壓力至所需設定的壓力和時間,同時適量減少樣品稱樣量;

(2)在正常加熱過程中,顯示數字突然不規則的跳動,從正數跳成負數,同時聽到“吱
吱”聲,一會兒又恢復正常。這種現象是由于進線電壓波動較大引起的。常規儀器額定電壓
應為 220V±10%,如果實驗室電壓變動范圍過大,會影響到儀器的穩定性,需先檢查進線電
壓是否在此范圍內,并最好加裝穩壓電源;

(3)在加熱過程中,消解爐右下部發出類似放鞭炮的響聲。此故障多是由于工作池過
于潮濕和酸霧的腐蝕造成的,致使消解爐的主控電路板上的高壓線包發生短路。遇到此故障
須立即關閉電源并拔掉電源,檢查工作池內是否過于潮濕或者有酸霧腐蝕。將儀器放置至干
燥處,打開儀器后部蓋板,檢查主控電源電路板,更換損壞的電器元件;

(4)儀器使用過程中,連續工作較長時間,消解了很多樣品的情況下,儀器突然停止
工作,面板無任何反應。出現此故障有兩種可能。一是消解爐的控制電路出現故障,依次檢
查電源保險絲、控制電路板上電源控制元件,多見電容、可控硅燒壞;二是由于連續工作,
消解爐過熱,熱敏電阻起過熱保護而斷路,待儀器冷卻后在啟動即可;

(5)主機通電時,顯示屏不亮,按“復位”鍵也無任何反應。此故障過見于儀器的電源保
險絲燒壞。關上爐門,按“啟動”鍵,此儀器有兩個保險絲,若能啟動,則說明小保險絲燒
壞,若不能啟動,則說明大保險絲燒壞。關閉電源,打開儀器后部的保險絲盒,取出備用保
險絲更換即可;

(6)在正常加熱過程中,突然顯示壓力的數字上升變慢或不動、數字亂跳,同時可聞
到酸味,通過觀察窗看到溶樣杯鼓底。此現象表明消解罐正在泄露,應立即停止加熱并調換
溶樣杯和密封碗,并在消解罐罐底放墊板。

(7)加熱過程中突然發出“砰”的一聲巨響,是爐門門鉤脫落,爐膛變形,消解罐炸
裂、揭頂、脫底。這種現象是由于彈性體、溶樣杯、活塞密封圈老化變硬、變形,罐內消解
的樣品可能有爆炸性成分,致使罐內壓力無限增大,也可能是消解罐罐蓋和罐底有傷痕造成
的。為避免此類情況發生,應注意對未知樣品必須控制樣品稱量 0.05-0.1g,對可能有劇烈反
應的樣品須進行預處理;消解前必須檢查彈性體、外罐罐蓋、罐底是否有傷痕及老化。檢查
方法:將罐蓋、罐體座底對著光亮處,在光線的透視下,檢查其轉角處和泄氣孔周圍是否有
內傷和裂紋。

3 密閉微波制樣系統預防故障的措施
(1)為防止觸電,必須確保儀器良好接地;
(2)消解爐內未放入加熱物前不要啟動消解爐,以免空載運行損壞儀器;
(3)進出排氣孔要保持通暢,以免消解過程過熱而觸發熱保護裝置啟動;
(4)消解罐所有部件必須干燥,確保無顆粒物粘附(除溶樣杯內);
(5)外罐體和外罐蓋須對著光亮檢查內壁有無裂縫,避免消解時發生危險;
(6)對可能產生突發性反應的樣品,如脂肪、油、硝化甘油、芳香族化合物、化妝品中的發膏、香波之類的樣品,必須先進行預處理;
(7)當壓力上升到 1.5Mpa 時,微波會立刻停止加熱,以防止意外,萃取時壓力最高到 2.0Mpa。
作者單位新疆維吾爾自治區科學器材服務中心 新疆維吾爾自治區烏魯木齊市 830000



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