乙二胺氣相層析分析方法之研究

The Determination of Ethylenediamine using Gas Chromatography

乙二胺是一種鹼性的揮發性無色液體，在空氣中容易潮解，而且含有令人討厭的臭魚腥味，在工業上的用途相當廣泛，主要是在製造染料、架橋劑、乳化劑、紡織潤滑劑、抗凍劑、殺菌劑、合成蠟、聚氨樹脂、和腐蝕抑制劑的工業上，作為化學反應的中間體使用。作業場所如果沒有適當的污染防治措施，則揮發出來的乙二胺蒸氣可經由呼吸器官的吸入或皮膚的接觸吸收，造成作業勞工的健康傷害，短時間暴露在含乙二胺蒸氣的作業環境空氣中，會造成人體眼睛、鼻子和喉嚨的刺激，長期暴露在含乙二胺的作業環境空氣下，則會引起人體皮膚炎、過敏性鼻炎、氣管炎、氣喘、鼻塞、咳嗽、肝臟和腎臟疾病等之職業傷害。對於空氣中微量揮發性有機化學物質的定量分析，氣相層析儀是一般實驗室最普遍使用的一種方法，因為這種方法具有強大的解析能力、選擇度和靈敏度高等優點。但是直接以氣相層析儀來分析微量胺類化合物則有困難，因為胺類化合物有容易吸附在層析儀系統、注射針和容器等缺點，但是如果能先經過合適的衍生物反應，將胺類化合物反應成具揮發性的衍生物，則可望順利解決此一問題，本研究係參考美國國立職業安全衛生研究所（National Institute for Occupational Safety and Health, NIOSH）建議之P&CAM 276乙二胺採樣分析方法，並配合國內環境加以改良，以矽膠管吸附乙二胺，然後以甲醇當脫附劑脫附處理後，添加過量的苯甲醛到脫附液中和乙二胺反應成衍生物，再利用火燄離子偵測器／氣相層析儀來定量偵測濃度，其中衍生物並以氣相層析質譜儀確認。

Ethylenediamine (EDA) is a thick, colorless, alkaline, hydrophilic fuming liquid with an ammonia-like odor. EDA is used as raw material or reaction intermediate in the manufacture of chelating agents, fungicides, corrosion inhibitors, polyamide resins, synthetic waxes and pharmaceuticals. Ethylenediamine can affect the body if it is inhaled, comes in contact with the eyes or skin, or is swallowed. It may enter the body through the skin. Short-term exposure to ethylenediamine vapors may cause irritation of the eyes, nose, mucous membranes, and respiratory tract. Repeated or prolonged over-exposure to ethylenediamine may cause dermatitis, skin rash and asthma. Liver, kidney, and lung damage may occur from repeated exposure to this chemical. The current OSHA standard for ethylenediamine is 10 parts of ethylenediamine per million parts of air (ppm) averaged over an eight-hour work shift. For the determination of traces of volatile organic compounds in air, gas chromatography is the generally preferred method, due to its combined features of separation power, selectivity and sensitivity. Gas chromatographic trace analysis of amines is not without problems due to their marked tendency to absorb in the chromatographic system, syringes, sample containers, etc. Trace analysis of amines by direct injection of free amines using gas chromatography is not suitable. These problems can be solved by suitable derivatization procedures. The project is to find a suitable method for the trace analysis of ethylenediamine in occupational environment atmosphere. Sampling is performed by absorbing ethylenediamine on a silica gel tube. The sorbent sections are transferred into glass vials and desorbed by treating with methanol. Benzaldehyde is added to undergo derivatization reaction and form 1,2-(dibenzylidene-amino)ethane derivatives. The desired derivative was confirmed by gas chromatography/mass spectrometry . The solution of derivative is analyzed by gas chromatography with flame ionization detector. The concentration of ethylenediamine is determined by the peak area of the derivative.