微量氣體混合物製備及分析方法探討

Preparation for trace gas mixtures and investigation of it’s analytical method

蘇奕菖(Yea-Chung Su)

指導教授 ： 許世興

朝陽科技大學/理工學院/應用化學系碩士在職專班/碩士(2011年)

摘要

從氣體工業的分析數據得知，目前產業界中最廣泛使用的氣體種類為氧、氮、氬及氦氣等，其主要應用於石化工業、環保氣體、實驗室、機械加工、航太工業、電子產業、食品加工、玻璃製造及氣體製造廠。標準氣體可以做為基本測量、儀器量測、儀器校正、生產品質監控等，具有標準量測的依據，氣體中微量的雜質含量一旦超過所要求的標準，就會對電子廠製程或其它工業製程產生嚴重的經濟損失及影響。因此準確量測高純度氣體中雜質含量是非常重要的，唯有準確量測氣體中雜質的含量才能確保氣體純度準確。
本論文有兩個研究主題一是利用重量法製備微量氣體混合物，以兩種基質氣體(氦氣及氧氣)分別與三種不同濃度的微量氣體(氬氣、氮氣和甲烷)混合配製；二是利用美國葛麥克公司(GOW-MAC)所生產的放電離子化偵測器(DID)，此種偵測器可同時檢測Ar、N2及CH4等微量氣體於氦氣及氧氣中的含量。
本研究利用氣相層析儀，以分子篩(molecular sieve；MS)管柱對微量氣體進行分析，連接放電離子化偵測器(DID)及氧氣捕捉器(Oxygen trap，model 75-900)輔助。由於MS管柱無法有效分離氧氣及氬氣，並且氦氣中通常含有微量的氧氣，所以有必要使用氧氣捕捉器事先去除氣體中的氧氣以利氬氣、氮氣及甲烷的定量分析。此方法可探討氣體中微量殘留氣體的含量，準確性與精密性高，實驗簡單，分析時間短，濃度線性關係R2可以到達0.999。

關鍵字

微量氣體 ； 氧氣捕捉器 ； 放電離子化偵測器 ； 重量法 ； 氣體混合物

並列摘要

From the analytical data of gas industry it is known that at present the most widely use of gases are oxygen, nitrogen, argon and helium which are mainly used in petrochemical industry, environmental gases, laboratories, mechanical process, aerospace industry, electronics factory, food process, glass manufacture and gas plant. Standard gases can serve as a measuring tool for the basic measurement, the instrument measurement, instrument calibration and production quality control etc. If the impurities of gases are beyond the request standard, the gas users, which are electronic factories or other industries, will have serious economic loss and impact. It is thus clear that the purity measurement of gases is very important. Therefore, the precise methods of gas purity measurement can ensure the purity of gases.
There are two topics in this thesis. The first topic is to prepare gas with trace mixtures using the gravimetric method. There are two substrate gases (helium and oxygen) and three trace mixtures (argon, nitrogen and methane) were mixed. The second topic is using discharge ionization detector (DID) from GOW-MAC Corporation, UAS. This detector can simultaneously determine the contents of Ar, N2 and CH4 in helium and oxygen gases, respectively.
In this research, gas chromatography with molecular sieve column was used and connected with the discharge ionization detector (DID) and the oxygen trap (Oxygen trap, model 75-900). The molecular sieve column can not effectively separate oxygen as well as argon and usually helium contaminated with trace oxygen, therefore the oxygen trap is required to pre-remove oxygen in order to determine the contents of argon, nitrogen and methane in the gases. This method can analyze the residue of gases with high accuracy and precision, method simple, short run time, and R-square linear-relation of concentration beyond 0.999.

並列關鍵字

trace gas ； gravimetric method ； gas mixtures ； Oxygen trap ； discharge ionization detector

參考文獻

4.劉公典，黃瓊芳，夏儀芝，傅應凱，「歐洲認證參考物質ERM 之研製與發展」Vol. 63, No.3, pp.481~490(2005)

2.N. Majcen, “A need for clearer terminology and guidance in the role of reference materials in method development and validation”, Accreditation and Quality Assurance, Vol. 8, No. 3-4, pp.108-112 (2006).

3.Venelinov T, Sahuquillo A, “Optimizing the uses and the costs of reference materials in analytical laboratories”, Trends in Analytical Chemistry , Vol. 25, No. 5, pp.528-533 (2006).

5.International Standards Organization, “Guide to the Expression of Uncertainty in Measurement”, ISO/IEC Guide 98:(1995)

7.E.E. Hughes, J. Mandel, D.von Lehmden, W.L. Zielinski Jr., A “Procedure for Establishing Traceability of Gas Mixtures to Certain National Institute of Standards and Technology SRM’s, “NIST Special Publication NBSIR 81-2227, Gaithersburg, MD, (1989).