1284198 九、發明說明： 【發明所屬之技術領域】 及於備，關—種快速化學物質檢測預處理之方法 车：n:括種可將取樣預處理時間大幅縮小’加快對 _ 發11或低揮發性之待分析化學物f取樣的 預處理時間’轉低可偵測極限。 【先前技術】 S白知在對複雜樣品巾的有機物進行分析時，通常採用 的疋液/夜相萃取(Uquid^iquid extracti〇n，LLE)和固相萃 取法jS〇hdPhaSeextracti〇n，spE)等技術。但這些方法都 存在著不同程度上的缺陷，如：費用高、操作複雜、費時 間及有毒的有機溶劑對人體的侵害。 而美國SUPELCO推出的一種固相微萃取法（s〇lid phase microextraction，SPME )技術克服了以前傳統的樣品 預處理技術的缺陷，它無需溶劑和複雜裝置，它能直接從 液體或氣體樣品中採集揮發和非揮發性的化合物，可以直 接在氣相層析儀（GC)，氣相層析/質譜（gc/MS)，聯用儀 和液相層析儀(HPLC)上分析，且能與任何型號的氣相和液 相層析儀連用，有手動和自動進樣兩種。 另，一種頂上空間萃取法（headspace method，HS)在 過去多年年中，在分析測試過程中，頂空方法已逐漸用於 檢測食品、血液、土壤、水、泥衆、化妝品、肥皂、制藥 和包裝物中的揮發物。在一些國家，比如日本，使用靜態 頂空方法取代了動態頂空方法。近幾年來，頂空方法在我 1284198 國得到較廣泛的應用。 頂空技術包括幾種不同的進樣技術。主要包括有動態 頂空或叫做吹掃捕集、固相微萃取、靜態頂空技術等。其 中以靜態頂空技術作為一種新技術的應用而得到廣泛的 推廣。靜態頂空技術（簡稱頂空進樣技術）主要用於測量那 些在200攝氏度下可揮發的被分析物，以及比較難於進行 前處理的樣品。 應用頂空技術在分析測試過程中具備許多優勢。使用 頂空進樣可以非常有效地減少用於樣品前處理的時間，並 且節省許多的經費，無需從基體中提取被分析物以進行液 體進樣；通常’測量樣品中的揮發性組分要比測量整個的 液態樣品要乾淨，這就減少了進樣系統維護的時間和費 用；另外’在許多應用中’頂空方法中注人的樣品溶劑的 含量比液體進樣中所含溶劑量少，這樣，溶劑訊號峰就變 J從而可以減少，谷劑訊號峰對感興趣的測定組分訊號峰 的干擾。 中篇=法普遍應用於環境樣品土壤、泥漿和水等基體 分析。例如，水中三氯甲烷、四氯化碳、三 :於盆成八：乙烯，、二溴甲烷等這樣-類揮發性有機物’ 此，、相關二-t人對人和動物的肝臟造成嚴重危害，因 此相關的官理部門岳丨丨兮 污水等嚴格的控制指標°=用水、水源水、排放 技術進行監測分析工作。A測部門廣泛應用頂空進樣 但前述所題之方法，在其使用上都有一最大之缺失， 1284198 那就取樣預處理時間摄3 污染物的採樣，而無多使用於揮發性有機 有機污染物進行採樣。’乂冋的半揮發性或難揮發性 【發明内容】 斜=是’本發明之主要目的在於解決上述習知之缺生 針對如何將取樣預處理_ 〇缺失， 在數分鐘㈣成。 ^ n㈣處理程序可 本發明另—目㈣在可對神發性、性 發性之待分析化學物質取樣，且預處理時間短。低揮 本發明再-目的係在增加該待分析之化學 樣測定量，降低可偵測極限。 、、 本發明再-目的係在取樣預處理上不需使用有機溶 ㈣不只可降低操作成本，也免除使財機溶劑所衍 生之安全問題、健康問題、及廢棄溶劑處理問題。 本發明係將汽化瓶設置於該微波裝置之内部連接一 控制溫度裝置，且該汽化瓶内部置有一磁子。利用一磁子 帶動裝置帶動該汽化瓶内部之磁子轉動，當待測定化學物 質置於該汽化瓶時，藉由轉動該磁子可攪動該待測定化學 物質使其均勻，同時利用該微波裝置之電磁波輕射快速^ 使該樣品液之分子活化運動，導致該樣品液中待分析測定 之化學物質可很在極短的時間内汽化至頂空控溫採樣管 之内管。再藉由該頂空控溫採樣管之入水孔與出水孔之水 循環之進出，可控制内管之溫度，也因為該溫度的控制， 該汽化之化學物質將冷卻成一雲霧狀，而操作時該吸附介 1284198 質於頂，，溫採樣管内管之位置係依待分析測定之化學 物質由氣態轉成液態之雲霧狀所定，藉此該待分析測定之 化學物質可為樣品吸收裝置之吸附介質所吸收（附）。 【實施方式】 有關本發明的詳細技術内容及其較佳實施例，茲配合 圖式說明如次。 口 請參閱「第1圖」所示，為本發明之設備示意圖。此 設備包括：一微波裝置10，如習用所知之微波爐；一汽化 瓶20 ’該汽化瓶20係設置於該微波裝置1〇之内部，且該 汽化瓶20内部置有一磁子71。一磁子帶動裝置7〇，係設 置於該微波爐1Q内部底面，且位於該汽化瓶2〇下方，藉 此磁子帶動裝置70可帶動該汽化瓶20内部之磁子71轉曰 動’藉由該磁子71的轉動，當待測定化學物質於該汽化 瓶20時，藉由轉動該磁子71可擾動該待測定化學物質使 其均勻。 又，該微波裝置1〇内部尚包括一選自玻璃、塑膠、 或陶究等有機絲機材料其中之—所製成之循環冷卻水 罩50’該循裱冷卻水罩5〇係設於該汽化瓶2〇與該磁子帶 動裝置70 f曰1，且罩住該該磁子帶動裝置7〇，藉此消弱微 波功率’使該磁子帶動裝置7〇不受微波之輻射影響。該 循裱冷部水罩50有一入水孔51與一出水孔52，内壁與外 壁間有-充滿保護水層之循環空間53，依〆般微波之特 性，該循環空間53厚度最佳須2公分以上。 一頂空控溫採樣管30，係包含一入水孔31與一出水 1284198 孔32外接溫控水循環機（圖中未示）之同心管式水流式控溫 管，下方有一連接段33透過該微波裝置10頂面之一穿孔 11與>又化瓶20 口連接，上方有—固定環34。其中，該頂 空控溫採樣管30與循環冷卻水罩50告缺玎利用同一循環 / 田,、、、 水糸統（圖中未示）達到其水循環之目的。直該頂空控溫採 樣管30之控溫方式除水循環之方式外，尚玎為機械控溫、 電氣控溫、及冷凍晶片控溫。 40可固定於該頂空控溫採樣管3()上方，而使該吸附介質 41於頂空控溫採樣管3G控溫冷卻之时，且高度位於三 入水^i與_出水孔32間’用以吸收(附)經操作本發明 設備時頂空控溫採樣管3G内管之汽化化學物質。 又，該吸附介質41須根據所分析物的分子量、揮發 性和極性選擇其材質。 一樣品吸收裝置40，該樣品吸收裝置40係可為一固 相微萃取（SPME)裝置，且該樣品吸收裝置4()之一端設 有吸附 '貝41 ’藉由前述之固定環％，樣品吸收裝置 現就其操作方法說明如下，請參閱「第2圖」所卜 為本發明之實施樣㈣意圖U方便看清楚内部，圖中該 微波裝置1G之mx開财絲*)。本發明之快速化 質檢測預處理之方法包括下列階段： 第-階段’首先將樣品(液體或固態粉末之待檢驗物) 置入汽化瓶20 ’酌加水份及調節酸鹼值成一樣品液6〇， 其中該樣品液60之祕值係依所待分析敎 所調節。 貝 1284198 第二階段，使磁子71受磁子帶動裝置70作動而授 該樣品液60使其均勻，同時利用該微波裝置10之電 品液6〇 ’促使該樣品液6〇中待分析測 疋之化子物貝 >飞化至頂空控溫採樣管3〇之内管。此 藉由該頂空控溫採樣管30之入水孔31與出水孔Μ之^ 循環之進出，可控制内管之溫度，也因為該溫度的控制， 之化學：質將冷卻成一雲霧狀61 ’而操作時該吸附 "、於頂空控溫採樣管3G内管之位置係依待分析測 =!質由氣態轉成液態之雲霧狀61所定，藉此該待 二吸收^化學物f可為樣品吸收裝置4G之吸附介質41 特性該微波照射功率係依待分析測定之化學物質之 數昭例如：於水樣(土壤）中採樣氯紛在最佳研究參 波照射功率歸，該吸附介㈣萃取採樣時間約 功刀率^料水樣中多料香族碳氫化合物(PAHs)在照射 、笛fWT，該吸附介質41萃取採樣時間約30分鐘。 學物^階段’將吸收(附)於吸附介質41之待分析測定化 = 主入氣相層析分離暨配屬各式檢測器作分析。 雜質66於表面活性劑、高分子聚合物和固體樣品中的微量 土壤中頁""分析、水樣的環境分析、食品中的香料分析、 縱火^各式科物分析、朗農㈣分析、 10之二炸物樣品的法醫分析等’本發明利用了微波裝置 且其备蚀約122讓’對應頻率為2450 MHz之電磁波， 、θ樣品液60内的分子和它—起以相同的頻率振盪 !284198 使樣品液60中分子與分子間的運動越來越激烈， =主轉動’互相碰撞和摩擦，從喊生熱量，將可在很短 冷、](數刀鐘）内將待分析測定之化學物質的汽化，此 二化，程的加快’也加快了待分析物質到吸附介質μ週 w的置’導致吸附介f 41可快速的吸附其足夠測定之量， 且操作簡便。 對於半揮發性、難揮發性、或低揮發性之待分析物質 也將因為電磁波之特性加快其分子的振盪，加快其揮發 性，使其短時間内汽化。這也對一些樣品液6〇中待分析 之化學物質的取樣量有正面的功效，不會因為待分析之化 學物質含量少而不易取得足夠檢測的量，大大降低可偵測 極限。 同時’本發明取樣預處理上，因為不需使用有機溶 劑’如此不只可降低操作成本，也免除使用有機溶劑所衍 生之安全問題、健康問題、及廢棄溶劑處理問題。 上述僅為本發明之較佳實施例而已，並非用來限定本 發明實施之範圍，即凡依本發明申請專利範圍所做的均等 變化與修飾，皆為本發明專利範圍所涵蓋。 【圖式簡單說明】 第1圖’為本發明之設備示意圖。 第2圖’為本發明之實施樣態示意圖。 【主要元件符號說明】 10 :微波裝置 11 :穿孔 11 1284198 20 :汽化瓶 30 :頂空控溫採樣管 31、 51 :入水孔 32、 52 :出水孔 33 :連接段 34 :固定環 40 :樣品吸收裝置 41 :吸附介質 50 :循環冷卻水罩 53 :循環空間 60 :樣品液 61 :雲霧狀 70 ··磁子帶動裝置 磁子 711284198 IX. Description of the invention: [Technical field to which the invention belongs] and the method for preparing and pre-processing a rapid chemical substance detection vehicle: n: Enclosure can greatly reduce the sampling pretreatment time 'accelerate to _ hair 11 or low The pretreatment time of the volatile analyte f sample to be sampled 'turns low to detect the limit. [Prior Art] S Baizhi is commonly used in the analysis of organic matter in complex sample towels. Uquid^iquid extracti〇n (LLE) and solid phase extraction method jS〇hdPhaSeextracti〇n, spE) And other technologies. However, these methods have various defects, such as high cost, complicated operation, time-consuming and toxic organic solvents. SUPELCO's s〇lid phase microextraction (SPME) technology overcomes the shortcomings of previous traditional sample pretreatment techniques. It does not require solvents and complex devices. It can be directly collected from liquid or gas samples. Volatile and non-volatile compounds can be directly analyzed by gas chromatography (GC), gas chromatography/mass spectrometry (gc/MS), combined instrumentation and liquid chromatography (HPLC), and can Any type of gas phase and liquid chromatograph is used, both manual and automatic. In addition, a headspace method (HS) has been used in the past seven years. During the analysis and testing process, the headspace method has been gradually used to detect food, blood, soil, water, mud, cosmetics, soap, pharmaceuticals. And volatiles in the package. In some countries, such as Japan, the static headspace method is used instead of the dynamic headspace method. In recent years, the headspace method has been widely used in my country of 1284198. Headspace technology includes several different injection techniques. It mainly includes dynamic headspace or called purge and trap, solid phase microextraction, and static headspace technology. Among them, static headspace technology has been widely promoted as a new technology application. Static Headspace Technology (referred to as Headspace Injection Technology) is primarily used to measure analytes that are volatile at 200 degrees Celsius and samples that are difficult to pretreat. The application of headspace technology has many advantages in the analysis and testing process. The use of headspace injection can very effectively reduce the time spent on sample preparation and saves a lot of money, without the need to extract analytes from the matrix for liquid injection; usually 'measure the volatile components in the sample. Measuring the entire liquid sample is clean, which reduces the time and expense of maintenance of the injection system; in addition, 'in many applications, the amount of solvent injected into the headspace method is less than the amount of solvent contained in the liquid injection. In this way, the solvent signal peak becomes J, which can reduce the interference of the peak signal peak to the signal peak of the component of interest. The middle part = method is generally applied to the analysis of substrates such as soil, mud and water in environmental samples. For example, chloroform, carbon tetrachloride, and tri-carbon in water: eight kinds of volatile organic compounds such as ethylene, dibromomethane, etc., and the related two-t humans cause serious harm to human and animal livers. Therefore, the relevant government department Yuelu sewage and other strict control indicators ° = water, water source, emission technology for monitoring and analysis. The A measurement department widely uses the headspace injection, but the method described above has a biggest deficiency in its use. 1284198 Then sample the pretreatment time to take 3 samples of pollutants, and not use it for volatile organic organic pollution. The object is sampled. Semi-volatile or difficult-to-volatile 【 [Abstract] The main purpose of the present invention is to solve the above-mentioned conventional deficiencies. How to pre-sample the sample _ 〇, in a few minutes (four). ^ n (4) Processing Procedures The present invention can also be used to sample the chemical substances to be analyzed for migraine and sexuality, and the pretreatment time is short. The low-side of the present invention is to increase the amount of the chemical sample to be analyzed and to reduce the detectable limit. Further, the present invention is not intended to use organic solvents in sampling pretreatment. (IV) not only reduces operating costs, but also eliminates safety problems, health problems, and disposal problems of waste solvents derived from the solvent of the machine. In the present invention, a vaporization bottle is disposed inside the microwave device to be connected to a control temperature device, and a magnetizer is disposed inside the vaporization bottle. Using a magneto-driven device to drive the magnetron inside the vaporization bottle to rotate, when the chemical to be determined is placed in the vaporization bottle, the magnet to be measured can be agitated by rotating the magnet to make it uniform, and the microwave device is used at the same time The electromagnetic wave is lightly shot quickly ^ The molecular activation of the sample liquid is activated, so that the chemical substance to be analyzed and determined in the sample liquid can be vaporized into the inner tube of the headspace temperature control sampling tube in a very short time. The temperature of the inner tube can be controlled by the water inlet and outlet of the water inlet hole and the water outlet hole of the headspace temperature control sampling tube, and because of the temperature control, the vaporized chemical substance will be cooled into a cloud shape, and the operation time should be cooled. The adsorption medium 1284198 is at the top, and the position of the inner tube of the temperature sampling tube is determined according to the cloud state in which the chemical substance to be analyzed and measured is converted from a gaseous state to a liquid state, whereby the chemical substance to be analyzed and determined can be the adsorption medium of the sample absorption device. Absorption (attached). [Embodiment] The detailed technical content of the present invention and its preferred embodiments are described in conjunction with the drawings. Please refer to the "Figure 1" for a schematic view of the device of the present invention. The apparatus comprises: a microwave device 10, such as a microwave oven as known; a vaporization bottle 20' is disposed inside the microwave device 1 and a magnetizer 71 is disposed inside the vaporization bottle 20. A magnetic sub-drive device 7 is disposed on the inner bottom surface of the microwave oven 1Q and located under the vaporization bottle 2〇, whereby the magneto-driven device 70 can drive the magnetism 71 inside the vaporization bottle 20 to rotate. The rotation of the magnet 71 causes the chemical to be measured to be disturbed by rotating the magnet 71 when the chemical to be measured is in the vaporization bottle 20. Moreover, the microwave device 1 further includes a circulating cooling water cover 50 ′ which is made of an organic silk machine material selected from the group consisting of glass, plastic, or ceramics, and the circulating cooling water cover 5 is attached thereto. The vaporization bottle 2 is coupled to the magnet drive device 70 f曰1 and covers the magnet drive device 7〇, thereby weakening the microwave power 'to make the magnet drive device 7〇 unaffected by the microwave radiation. The circulating water portion cover 50 has a water inlet hole 51 and a water outlet hole 52. The inner wall and the outer wall have a circulation space 53 filled with a protective water layer. According to the characteristics of the microwave, the circulation space 53 preferably has a thickness of 2 cm. the above. A top air temperature control sampling tube 30 is a concentric tube type water flow temperature control tube which comprises a water inlet hole 31 and a water outlet 1284198 hole 32 externally connected to a temperature control water circulation machine (not shown), and a connection section 33 passes through the microwave. One of the top surfaces of the device 10 has a perforation 11 and is connected to the bottle 20 and has a fixing ring 34 thereon. Wherein, the headspace temperature control sampling tube 30 and the circulating cooling water cover 50 are insufficient to use the same cycle/field, water, and water system (not shown) to achieve the purpose of water circulation. Straight to the temperature control method of the headspace temperature control sample tube 30, in addition to the water circulation mode, it is also controlled by mechanical temperature control, electrical temperature control, and frozen wafer temperature control. 40 can be fixed above the headspace temperature control sampling pipe 3 (), and the adsorption medium 41 is controlled by the headspace temperature control sampling pipe 3G, and the height is located between the three inlet waters ^i and the water outlet holes 32. The vaporization chemical used to absorb (attach) the inner tube of the headspace temperature control sampling tube 3G when the apparatus of the invention is operated. Further, the adsorption medium 41 is selected based on the molecular weight, volatility and polarity of the analyte. a sample absorption device 40, which may be a solid phase microextraction (SPME) device, and one end of the sample absorption device 4 () is provided with an adsorption 'Bei 41' by the aforementioned fixed ring %, sample The absorption device will now be described as follows. Please refer to the "Fig. 2" for the embodiment of the present invention. (IV) It is intended to make it easy to see the inside. In the figure, the mx of the microwave device 1G is opened*). The method for rapid chemical detection pretreatment of the present invention comprises the following stages: Stage-stage 'Firstly placing a sample (liquid or solid powder to be tested) into a vaporization bottle 20' discriminates water and adjusts pH to a sample liquid 6〇, wherein the secret value of the sample solution 60 is adjusted according to the analysis to be analyzed. In the second stage of the shell 1284198, the magnetic element 71 is actuated by the magneto-driven device 70 to impart uniformity to the sample liquid 60, and the electrolysis liquid 6〇' of the microwave device 10 is used to promote the sample liquid to be analyzed.疋之化子物贝> Flight to the inner tube of the headspace temperature control sampling tube. The temperature of the inner tube can be controlled by the inlet and outlet of the water inlet hole 31 and the water outlet hole of the headspace temperature control sampling tube 30, and also because of the temperature control, the chemical substance will be cooled into a cloud shape 61 ' In operation, the adsorption ", the position of the inner tube of the 3G in the headspace temperature control sampling tube is determined according to the analysis of the measurement = the quality is changed from the gaseous state to the liquid cloud 61, whereby the chemical absorption f can be The adsorption medium of the sample absorption device 4G is characterized in that the power of the microwave irradiation is determined according to the number of chemical substances to be analyzed, for example, the sampling of chlorine in the water sample (soil) is performed in the best study of the reference wave irradiation power. (4) The sampling time of the extraction is about 30 minutes for the extraction time of the adsorbent medium 41 in the water sample of the multi-fragrance hydrocarbons (PAHs) in the water sample. The learning phase ^ will be absorbed (attached) to the adsorption medium 41 to be analyzed and determined = primary gas chromatography separation and associated detectors for analysis. Impurity 66 in surfactants, high molecular polymers and trace soils in solid samples. "" analysis, environmental analysis of water samples, fragrance analysis in food, arson, various scientific analysis, Langon (4) analysis , for example, a forensic analysis of a sample of 10 defrosted explosives, etc. The present invention utilizes a microwave device and it erodes about 122 to make an electromagnetic wave corresponding to a frequency of 2450 MHz, and the molecules in the θ sample solution 60 and the same frequency Oscillation! 284198 makes the movement of molecules and molecules in sample liquid 60 more and more intense, = the main rotation 'colliding and rubbing each other, from shouting heat, will be able to be analyzed in a very short cold,] (number of knives) The vaporization of the chemical substance is measured, and the acceleration of the process is also accelerated by the fact that the adsorption of the substance to be adsorbed to the μ week of the adsorption medium is such that the adsorption medium f 41 can rapidly adsorb the amount of the measurement, and the operation is simple. For substances that are semi-volatile, difficult to volatility, or low in volatility, the molecular oscillations are accelerated by the characteristics of electromagnetic waves, and their volatility is accelerated to vaporize them in a short time. This also has a positive effect on the sampling amount of the chemical to be analyzed in some of the sample liquids. It is not easy to obtain a sufficient amount of detection due to the small amount of chemical substances to be analyzed, and the detectable limit is greatly reduced. At the same time, the sampling pretreatment of the present invention does not require the use of an organic solvent, which not only reduces the operating cost, but also eliminates the safety problems, health problems, and disposal problems of waste solvents derived from the use of organic solvents. The above are only the preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and all variations and modifications made by the scope of the present invention are covered by the scope of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic view of the apparatus of the present invention. Fig. 2 is a schematic view showing an embodiment of the present invention. [Main component symbol description] 10: Microwave device 11: Perforation 11 1284198 20: Vaporized bottle 30: Headspace temperature control sampling tube 31, 51: Water inlet hole 32, 52: Water outlet hole 33: Connection section 34: Fixing ring 40: Sample Absorbing device 41: Adsorption medium 50: Circulating cooling water hood 53: Circulating space 60: Sample liquid 61: Cloud-like 70··Magnetic driving device Magnet 71