JPH07103956A - Gas chromatograph - Google Patents
Gas chromatographInfo
- Publication number
- JPH07103956A JPH07103956A JP5269870A JP26987093A JPH07103956A JP H07103956 A JPH07103956 A JP H07103956A JP 5269870 A JP5269870 A JP 5269870A JP 26987093 A JP26987093 A JP 26987093A JP H07103956 A JPH07103956 A JP H07103956A
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- JP
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- Prior art keywords
- column
- sample
- valve
- gas
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、ガスクロマトグラ
フ、特に試料成分中の水分を良く除去することの出来る
ガスクロマトグラフに関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a gas chromatograph, and more particularly to a gas chromatograph capable of well removing water in sample components.
【０００２】[0002]
【従来の技術】試料を気化させてその成分を分析するガ
スクロマトグラフでは流量切換バルブと成分分離機能を
有するプレカットバルブとを組み合わせて特定の成分を
分離除去して分析カラムへ導入することが多い。特に、
プレカットバルブには微量成分を分析する場合、流路途
中に水分を分離するためのトラップ用カラムが配置され
ることがある。2. Description of the Related Art In a gas chromatograph in which a sample is vaporized and its components are analyzed, a flow rate switching valve and a precut valve having a component separation function are often combined to separate and remove a specific component and introduce it into an analytical column. In particular,
When a trace component is analyzed, the precut valve may be provided with a trap column for separating water in the flow path.
【０００３】図７は従来のガスクロマトグラフによる成
分分析の際のプレカラムから分析カラムへの炭化水素
（ＨＣ）類試料の排出量と導入時間との関係を示すグラ
フである。この図からも分かるように、プレカラムでの
炭化水素（ＨＣ）類と水分との保守時間に差はあるが、
高沸点物質である炭化水素（ＨＣ）類成分を分析対象と
する場合（Ｔ1 時間かけて導入する）水分の量の大半は
分析カラムへ導入されてしまうことになる。FIG. 7 is a graph showing the relationship between the discharge amount of hydrocarbon (HC) samples from the precolumn to the analytical column and the introduction time in the conventional component analysis by gas chromatography. As can be seen from this figure, there is a difference in maintenance time between hydrocarbons (HC) and water in the precolumn,
When a hydrocarbon (HC) component that is a high-boiling substance is used as an analysis target (which is introduced over T 1 hour), most of the amount of water will be introduced into the analytical column.
【０００４】[0004]
【発明が解決しようとする課題】上記するように、成分
分離機能をもつプレカラムを設けたガスクロマトグラフ
では測定成分によっては水分等の不要成分を除去するこ
とが難しい。特に、多量の水分を含む試料を分析する際
この水分のために分離が悪くなったり（特に吸着カラム
を使用するとき）、水素炎イオン化検出器の水素炎が消
えたり、流路中に冷却用カラムトラップが構成されてい
たりするとここで結露が生じてカラムの閉塞が起き分析
が出来なくなる等の問題があった。この発明はかかる課
題に鑑みてなされたものであり、その目的とする所は試
料中に多量の水分等の不要成分があってもこれを殆ど除
去することが可能でより正確な試料分析が可能なガスク
ロマトグラフを提供することにある。As described above, in a gas chromatograph provided with a precolumn having a component separation function, it is difficult to remove unnecessary components such as water depending on the measurement components. In particular, when analyzing a sample containing a large amount of water, this water causes poor separation (especially when using an adsorption column), the hydrogen flame of the hydrogen flame ionization detector disappears, and cooling is performed in the flow path. If a column trap is configured, there is a problem that dew condensation occurs here and blockage of the column occurs, making analysis impossible. The present invention has been made in view of the above problems, and the object thereof is to eliminate most of unnecessary components such as water in a sample, which enables more accurate sample analysis. To provide a simple gas chromatograph.
【０００５】[0005]
【課題を解決するための手段】即ち、この発明は上記す
る課題を解決するために、主要成分中の不要成分を除去
するプレカラムを備えたガスクロマトグラフにおいて、
前記プレカラムには１価又は２価のアルカリ金属とハロ
ゲンとより成る化合物を含有する珪藻土等の担体に保持
させた充填剤を充填したことを特徴とする。That is, in order to solve the above-mentioned problems, the present invention provides a gas chromatograph equipped with a precolumn for removing unnecessary components in the main components,
The pre-column is characterized in that it is filled with a packing material held on a carrier such as diatomaceous earth containing a compound consisting of a monovalent or divalent alkali metal and a halogen.
【０００６】[0006]
【作用】ガスクロマトグラフを上記手段としたときの作
用について添付図（図２乃至図５）及びこれらの符号を
用いて説明する。 試料入口１２より導入された試料は計量管５で採取さ
れ（図２）、次に濃縮管６へ送られ濃縮される（図
３）。該濃縮管６を加熱してパ−ジガス入口１８から
パ−ジガスを導入し、濃縮管６で濃縮した試料をプレカ
ラム７を通しここで試料中の水分を除去してカラム導入
口１７より導入する（図４）。更に、プレカットバル
ブ２の流路を切り換えて元の流路に戻し、パ−ジガスを
プレカラム７へ一定時間導入して不必要成分のバックフ
ラッシュを行う（図５）。以上の乃至の動作により
分析カラムへ導入される試料中の水分量等の不要成分を
少なくすることが可能となり且つバックフラッシュによ
りプレカラム７も元の状態に再生される。The operation when the gas chromatograph is used as the above means will be described with reference to the accompanying drawings (FIGS. 2 to 5) and these reference numerals. The sample introduced from the sample inlet 12 is collected by the measuring pipe 5 (FIG. 2), and then sent to the concentrating pipe 6 to be concentrated (FIG. 3). The concentration tube 6 is heated to introduce a purge gas from a purge gas inlet 18, and the sample concentrated in the concentration tube 6 is passed through a pre-column 7 to remove water in the sample and introduced from the column inlet 17. (Fig. 4). Further, the flow path of the precut valve 2 is switched to return to the original flow path, and purge gas is introduced into the precolumn 7 for a certain period of time to backflush unnecessary components (FIG. 5). By the above operations (1) and (2), unnecessary components such as the amount of water in the sample introduced into the analysis column can be reduced, and the pre-column 7 is also regenerated to its original state by backflushing.
【０００７】[0007]
【実施例】以下、この発明の具体的実施例について図面
を参照して説明する。図１はこの発明のガスクロマトグ
ラフで用いるサンプリングバルブ１とプレカットバルブ
２とカラム３及び検出器４（通常水素炎イオン化検出器
が使用されることが多い）の配管図である。サンプリン
グバルブ１には、流路を切り換えることによりガスの流
入口或いは排出口となる８つのガス流通口Ａ乃至Ｈが設
けられている。当初、これらのガス流通口のうちＣはパ
−ジガス入口（計量管用）１１に、Ａは試料ガス入口１
２に、Ｅは試料ガス出口１３にそれぞれ通じる管路によ
って接続されている。また、該サンプリングバルブ１の
前記ＤとＨとの間の管路には計量管５が接続されてい
る。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Specific embodiments of the present invention will be described below with reference to the drawings. FIG. 1 is a piping diagram of a sampling valve 1, a precut valve 2, a column 3 and a detector 4 (usually a hydrogen flame ionization detector is often used) used in the gas chromatograph of the present invention. The sampling valve 1 is provided with eight gas flow ports A to H which are gas inlets or outlets by switching the flow paths. Initially, among these gas flow ports, C is a purge gas inlet (for measuring pipe) 11 and A is a sample gas inlet 1.
2 and E are connected to each other by conduits leading to the sample gas outlet 13. Further, a measuring pipe 5 is connected to a pipe line between the D and H of the sampling valve 1.
【０００８】前記プレカットバルブ２には、流路を切り
換えることによりガスの流入口或いは排出口となる１０
個のガス流通口Ｉ乃至Ｒが設けられている。これらのガ
ス流通口のうちＩは前記サンプリングバルブ１のガス流
通口Ｇに、Ｒは前記パ−ジガス出口（計量管用）１４
に、Ｌは抵抗管８を介してパ−ジガス出口（プレカラム
用）１５に、Ｍは抵抗管９を介してキャリヤガス入口１
６に、Ｎはカラム導入口１７に、Ｐはパ−ジガス入口
（プレカラム用）１８にそれぞれ通じる管路によって接
続されている。また、該プレカットバルブ２のガス流通
口ＪとＱとの間には濃縮管６が管路によって接続され、
ガス流通口ＫとＯとの間にはプレカラム７が管路によっ
て接続されている。The pre-cut valve 2 serves as a gas inlet or a gas outlet by switching the flow path.
Individual gas flow ports I to R are provided. Among these gas flow ports, I is the gas flow port G of the sampling valve 1 and R is the purge gas outlet (for measuring pipe) 14
Further, L is a purge gas outlet (for pre-column) 15 via a resistance tube 8 and M is a carrier gas inlet 1 via a resistance tube 9.
6, N is connected to a column inlet 17, and P is connected to a purge gas inlet (for pre-column) 18 by pipes. Further, a concentrating pipe 6 is connected between the gas flow ports J and Q of the precut valve 2 by a pipe line,
The precolumn 7 is connected between the gas flow ports K and O by a pipe line.
【０００９】次に、前記プレカットバルブ２に接続され
たプレカラム７には、塩化カルシウム（ＣａＣｌ2 ）を
珪藻土等の担体に保持させた充填剤を充填してある。該
塩化カルシウム（ＣａＣｌ2 ）は、多くは２水塩である
が、炭酸カルシウム又は水酸化カルシウムを塩酸に溶か
した水溶液を濃縮すると３０°Ｃ以下で６水塩が得ら
れ、３０°Ｃ〜４０°Ｃで４水塩が得られ、４０°Ｃ以
上で２水塩が得られ、１７５°Ｃで１水塩が得られ、３
００°Ｃ付近では無水塩が得られる。これらのうち有水
塩はいずれも無色吸水性の結晶で、無水塩は斜方晶であ
る。Next, the pre-column 7 connected to the pre-cut valve 2 is filled with a filler in which calcium chloride (CaCl 2 ) is held in a carrier such as diatomaceous earth. Most of the calcium chloride (CaCl 2 ) is a dihydrate, but when an aqueous solution obtained by dissolving calcium carbonate or calcium hydroxide in hydrochloric acid is concentrated, a hexahydrate is obtained at 30 ° C or lower, and 30 ° C to 40 ° C. Tetrahydrate is obtained at ° C, dihydrate is obtained at 40 ° C or higher, monohydrate is obtained at 175 ° C, and 3
Anhydrous salt is obtained at around 00 ° C. Of these, the hydrated salts are all colorless and water-absorbing crystals, and the anhydrous salts are orthorhombic crystals.
【００１０】プレカラム７に前記塩化カルシウム含有の
充填剤を充填したこの発明のガスクロマトグラフではカ
ラム導入口１７までの間のガス流路途中にサンプリング
バルブ１とプレカットバルブ２とを配置し、試料ガス中
の水分を除去し流路を切り換えてカラム３へ導入するよ
うになっているが、その操作について図２乃至図５を参
照して説明する。 試料入口１２より導入され、サンプリングバルブ１の
計量管５を流通し、試料出口１３より排出されるように
試料を流通させて該計量管５で試料を採取する（図
２）。 次に、サンプリングバルブ１の流路を切り換え、パ−
ジガス入口１１からパ−ジガスを導入し、計量管５で採
取した試料を計量後プレカットバルブ２に接続した濃縮
管６へ送り、該濃縮管６を冷却して試料ガスを濃縮する
（図３）。 プレカットバルブ２の流路を切り換えると共に加熱
（約１００°Ｃに加熱）してパ−ジガス入口１８からパ
−ジガスを導入し、濃縮管６で濃縮した試料をプレカラ
ム７を通しここで試料中の水分を除去してカラム導入口
１７より導入する（図４）。 更に、プレカットバルブ２の流路を切り換えて元の流
路に戻し、パ−ジガス入口１８よりパ−ジガスをプレカ
ラム７へ導入し、一定時間（Ｔ3 時間まで）パ−ジガス
を導入して不必要成分のバックフラッシュを行う（図
５）。 以上の乃至の動作により分析カラムへ導入される試
料中の水分量を少なくすることが可能となり且つバック
フラッシュによりプレカラム７も元の状態に再生され
る。In the gas chromatograph of the present invention in which the pre-column 7 is filled with the above-mentioned calcium chloride-containing filler, the sampling valve 1 and the pre-cut valve 2 are arranged in the gas flow path up to the column inlet 17, and The water is removed and the flow path is switched and introduced into the column 3. The operation will be described with reference to FIGS. 2 to 5. The sample is introduced through the sample inlet 12, flows through the measuring pipe 5 of the sampling valve 1, and flows through the sample outlet 13 so as to be discharged, and the sample is collected by the measuring pipe 5 (FIG. 2). Next, switch the flow path of the sampling valve 1 to
A purge gas is introduced from the digas inlet 11, the sample taken by the measuring pipe 5 is weighed and sent to the concentrating pipe 6 connected to the precut valve 2, and the concentrating pipe 6 is cooled to concentrate the sample gas (FIG. 3). . The flow path of the pre-cut valve 2 is switched and heated (heated to about 100 ° C.) to introduce the purge gas from the purge gas inlet 18, and the sample concentrated in the concentrating tube 6 is passed through the pre-column 7 where Water is removed and introduced through the column inlet 17 (FIG. 4). Further, the flow path of the pre-cut valve 2 is switched to return to the original flow path, the purge gas is introduced into the pre-column 7 through the purge gas inlet 18, and the purge gas is introduced for a fixed time (up to T 3 hours). Backflush necessary components (Fig. 5). By the above-mentioned operations (1) to (3), the amount of water in the sample introduced into the analytical column can be reduced, and the pre-column 7 is also regenerated to its original state by backflushing.
【００１１】図６はこの発明のガスクロマトグラフによ
る成分分析の際のプレカラムから分析カラムへの炭化水
素（ＨＣ）類試料の排出量と導入時間との関係を示すグ
ラフである。この図からも分かるように炭化水素（Ｈ
Ｃ）類成分を分析対象とする場合（Ｔ2 時間かけて導入
する）水分の量の大半は除去されることが分かる。そし
てＴ3 時間までフラットな状態で水分が除去される。FIG. 6 is a graph showing the relationship between the amount of hydrocarbon (HC) sample discharged from the precolumn to the analytical column and the time of introduction in the component analysis by the gas chromatograph of the present invention. As you can see from this figure, hydrocarbons (H
It can be seen that most of the amount of water is removed when the C) component is used as the analysis target (introduced over T 2 hours). Then, moisture is removed in a flat state until T 3 hours.
【００１２】前記プレカラム７に充填した塩化カルシウ
ム（ＣａＣｌ2 ）の充填剤が試料中の水分を除去し且つ
バックフラッシにより再生されるのは次ような作用によ
るものと解される。即ち、上記するように約１００°Ｃ
の恒温槽では塩化カルシウム（ＣａＣｌ2 ）は２水塩の
状態である。そこに多量の水分が導入されると４水塩或
いは６水塩となるが、その後バックフラッシによる水分
を含まないパ−ジガスにより元の２水塩の状態に再生さ
れ、この再生される過程が緩やかで時間を要するため経
過時間に対して排出される水分の量もフラットになるの
である。The reason why the calcium chloride (CaCl 2 ) packing material packed in the pre-column 7 removes water in the sample and is regenerated by back flush is considered to be as follows. That is, as described above, about 100 ° C
In the constant temperature bath, calcium chloride (CaCl 2 ) is in a dihydrate state. When a large amount of water is introduced into it, it turns into tetrahydrate or hexahydrate, and then it is regenerated to the original dihydrate state by the purge gas containing no water due to the back flush, and this regeneration process is performed. Since it is slow and takes time, the amount of water discharged becomes flat with respect to the elapsed time.
【００１３】尚、この発明ではプレカラム７に充填する
充填剤は２価の金属であるカルシウム（Ｃａ）とハロゲ
ン元素の塩素（Ｃｌ）との化合物である塩化カルシウム
（ＣａＣｌ2 ）を主成分とする充填剤としたが、２価の
金属或いは１価の金属例えばナトリウム（Ｎａ）やカリ
ウム（Ｋ）と、ハロゲン元素例えば臭素（Ｂａ）やヨウ
素（Ｉ）との化合物の水塩で吸水性があり且つ再生可能
なものであれば他の化合物も使用可能である。In the present invention, the packing material packed in the pre-column 7 is mainly composed of calcium chloride (CaCl 2 ) which is a compound of calcium (Ca) which is a divalent metal and chlorine (Cl) which is a halogen element. Although it is used as a filler, it is a water salt of a compound of a divalent metal or a monovalent metal such as sodium (Na) or potassium (K) and a halogen element such as bromine (Ba) or iodine (I), and has water absorbability. Other compounds can also be used as long as they are renewable.
【００１４】[0014]
【発明の効果】この発明のガスクロマトグラフは以上詳
述したような構成としたので、多量の水分を含む試料か
ら大部分の水分を除去しガスクロマトグラフによるより
正確な分析が可能となる。特に、微量（ｐｐｍ単位の
量）の試料を分析する場合、検出限界を上げるため多量
の試料を冷却してトラップするが、このとき多量の水分
が存在すると分析の際障害となっていた。しかし本願の
発明の構成により大部分の水分を除去することが可能と
なり水素炎イオン化検出器の水素炎の消失やカラムトラ
ップでの結露による閉塞等を防止することが出来る。Since the gas chromatograph of the present invention is constructed as described in detail above, most of the water is removed from the sample containing a large amount of water, and more accurate analysis by the gas chromatograph becomes possible. In particular, in the case of analyzing a small amount of sample (amount in ppm), a large amount of sample is cooled and trapped in order to raise the detection limit, but the presence of a large amount of water at this time has been an obstacle to the analysis. However, most of the water can be removed by the configuration of the invention of the present application, and the disappearance of the hydrogen flame of the hydrogen flame ionization detector and the blockage due to dew condensation in the column trap can be prevented.
【図１】この発明のガスクロマトグラフで用いるサンプ
リングバルブとプレカットバルブとカラム及び検出器の
配管図である。FIG. 1 is a piping diagram of a sampling valve, a precut valve, a column, and a detector used in the gas chromatograph of the present invention.
【図２】サンプリングバルブの計量管で試料を採取する
状態を示す図である。FIG. 2 is a diagram showing a state in which a sample is collected by a measuring pipe of a sampling valve.
【図３】計量管で採取した試料を計量後プレカットバル
ブに接続した濃縮管で試料ガスを濃縮する状態を示す図
である。FIG. 3 is a view showing a state in which a sample gas is concentrated by a concentrating tube connected to a pre-cut valve after measuring a sample collected by a measuring tube.
【図４】プレカットバルブの濃縮管で濃縮し水分を除去
した試料をカラム導入口へ導入する状態を示す図であ
る。FIG. 4 is a diagram showing a state in which a sample, which has been concentrated by a concentrating tube of a pre-cut valve to remove water, is introduced into a column inlet.
【図５】プレカットバルブの流路を切り換えて元の流路
に戻しパ−ジガスをプレカラムへ導入し不必要成分のバ
ックフラッシュを行う状態を示す図である。FIG. 5 is a diagram showing a state in which the flow path of the pre-cut valve is switched to return to the original flow path, and purge gas is introduced into the pre-column to backflush unnecessary components.
【図６】この発明のガスクロマトグラフによる成分分析
の際のプレカラムから分析カラムへの炭化水素（ＨＣ）
類試料の排出量と導入時間との関係を示す図である。FIG. 6 shows hydrocarbons (HC) from the precolumn to the analytical column in the case of component analysis by the gas chromatograph of the present invention.
It is a figure which shows the discharge amount of a similar sample and the relationship of introduction time.
【図７】従来のガスクロマトグラフによる成分分析の際
のプレカラムから分析カラムへの炭化水素（ＨＣ）類試
料の排出量と導入時間との関係を示す図である。FIG. 7 is a diagram showing the relationship between the discharge amount and the introduction time of a hydrocarbon (HC) sample from a precolumn to an analysis column in the conventional component analysis by gas chromatography.
１ サンプリングバルブ ２ プレカ
ットバルブ ３ カラム ４ 検出器 ５ 計量管 ６ 濃縮管 ７ プレカラム ８、９ 抵
抗管 １１ パ−ジガス入口（計量管用） １２ 試料ガス入口 １３ 試料
ガス出口 １４ パ−ジガス出口（計量管用） １５ パ−ジガス出口（プレカラム用） １６ キャリヤガス入口 １７ カラ
ム導入口 １８ パ−ジガス入口（プレカラム用）1 Sampling valve 2 Pre-cut valve 3 Column 4 Detector 5 Metering tube 6 Concentrating tube 7 Pre-column 8, 9 Resistance tube 11 Page gas inlet (for metering tube) 12 Sample gas inlet 13 Sample gas outlet 14 Page gas outlet (for metering tube) 15 purge gas outlet (for pre-column) 16 carrier gas inlet 17 column inlet 18 purge gas inlet (for pre-column)
───────────────────────────────────────────────────── フロントページの続き (72)発明者 平井 研治 京都市中京区西ノ京桑原町１番地 株式会 社島津製作所三条工場内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Kenji Hirai Inventor Kenji Hirai No. 1 Kuwabara-cho, Nishinokyo, Nakagyo-ku, Kyoto Shimadzu Corporation Sanjo Factory
Claims (1)
ラムを備えたガスクロマトグラフにおいて、前記プレカ
ラムには１価又は２価のアルカリ金属とハロゲンとより
成る化合物を含有する珪藻土等の担体に保持させた充填
剤を充填したことを特徴とするガスクロマトグラフ。1. A gas chromatograph equipped with a pre-column for removing unnecessary components in the main components, wherein the pre-column is held on a carrier such as diatomaceous earth containing a compound consisting of a monovalent or divalent alkali metal and a halogen. A gas chromatograph characterized by being filled with a filling material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26987093A JP3678762B2 (en) | 1993-09-30 | 1993-09-30 | Gas chromatograph |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26987093A JP3678762B2 (en) | 1993-09-30 | 1993-09-30 | Gas chromatograph |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07103956A true JPH07103956A (en) | 1995-04-21 |
| JP3678762B2 JP3678762B2 (en) | 2005-08-03 |
Family
ID=17478365
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26987093A Expired - Fee Related JP3678762B2 (en) | 1993-09-30 | 1993-09-30 | Gas chromatograph |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3678762B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012132781A (en) * | 2010-12-21 | 2012-07-12 | Taiyo Nippon Sanso Corp | Analytical method using gas chromatography and analyzer using gas chromatography |
| CN103983722A (en) * | 2014-04-28 | 2014-08-13 | 华东师范大学 | A gas chromatograph for hydrocarbon component analysis of a catalytic cracking product of gasoline and diesel |
| US9588088B2 (en) | 2013-08-14 | 2017-03-07 | Shimadzu Corporation | Gas sample introduction device |
-
1993
- 1993-09-30 JP JP26987093A patent/JP3678762B2/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012132781A (en) * | 2010-12-21 | 2012-07-12 | Taiyo Nippon Sanso Corp | Analytical method using gas chromatography and analyzer using gas chromatography |
| US9588088B2 (en) | 2013-08-14 | 2017-03-07 | Shimadzu Corporation | Gas sample introduction device |
| CN103983722A (en) * | 2014-04-28 | 2014-08-13 | 华东师范大学 | A gas chromatograph for hydrocarbon component analysis of a catalytic cracking product of gasoline and diesel |
| CN103983722B (en) * | 2014-04-28 | 2015-06-24 | 华东师范大学 | A gas chromatograph for hydrocarbon component analysis of a catalytic cracking product of gasoline and diesel |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3678762B2 (en) | 2005-08-03 |
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