JP2003014721A - Measurement method of relative volatility - Google Patents
Measurement method of relative volatilityInfo
- Publication number
- JP2003014721A JP2003014721A JP2002126190A JP2002126190A JP2003014721A JP 2003014721 A JP2003014721 A JP 2003014721A JP 2002126190 A JP2002126190 A JP 2002126190A JP 2002126190 A JP2002126190 A JP 2002126190A JP 2003014721 A JP2003014721 A JP 2003014721A
- Authority
- JP
- Japan
- Prior art keywords
- compound
- peak area
- relative volatility
- phase
- liquid
- 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.)
- Pending
Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は相対揮発度を測定す
る方法に関し、詳しくは、密閉容器中の２種の液体化合
物が混合された液相部と気相部とを、別々に、ガスクロ
マトグラフに導入し、各相毎に検出された各化合物のピ
ーク面積から、蒸留の基礎物性値である相対揮発度を簡
便に測定する方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for measuring relative volatility, and more particularly to a gas chromatograph in which a liquid phase part and a gas phase part in which two kinds of liquid compounds are mixed in a closed container are separately provided. The present invention relates to a method for simply measuring the relative volatility, which is the basic physical property value of distillation, from the peak area of each compound detected in each phase introduced in.
【０００２】[0002]
【従来の技術】従来、相対揮発度は、気相部の組成につ
いては、予め調製した２種の化合物の高純度品を用いて
ガスクロマトグラフの検量線を作成し、該検量線と各化
合物のピークの面積とから求め、一方、液相部の組成に
ついては、上記気相部の組成の場合と同様、上記検量線
と各化合物のピークの面積とから求めるか、或いは、密
閉容器中に仕込んだ混合液の重量比により求めていた。2. Description of the Related Art Conventionally, regarding the relative volatility, regarding the composition of the gas phase part, a calibration curve of a gas chromatograph was prepared by using high purity products of two kinds of compounds prepared in advance, and the calibration curve and each compound Obtained from the area of the peak, on the other hand, for the composition of the liquid phase portion, as in the case of the composition of the gas phase portion, or from the area of the peak of the calibration curve and each compound, or charged in a closed container It was calculated from the weight ratio of the mixed liquid.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、上記密
閉容器における２種の液体化合物の相対揮発度αは、下
式（２）
α＝（ｙ１／ｘ１）／（ｙ２／ｘ２） （２）
［式中、αは化合物２に対する化合物１の相対揮発度
を、ｘ１は液相中の化合物１のモル分率を、ｘ２は液相
中の化合物２のモル分率を、ｙ１は気相中の化合物１の
モル分率を、ｙ２は気相中の化合物２のモル分率を表
す。］により算出されるが、上式（２）中のモル分率ｘ
１、ｘ２、ｙ１及びｙ２を、各々、下式（３）〜（６）
ｘ１＝（Ａｘ１・ｆＡ１）／｛（Ａｘ１・ｆＡ１）＋（Ａｘ２・ｆＡ２）｝
（３）
ｘ２＝（Ａｘ２・ｆＡ２）／｛（Ａｘ１・ｆＡ１）＋（Ａｘ２・ｆＡ２）｝
（４）
ｙ１＝（Ａｙ１・ｆＡ１）／｛（Ａｙ１・ｆＡ１）＋（Ａｙ２・ｆＡ２）｝
（５）
ｙ２＝（Ａｙ２・ｆＡ２）／｛（Ａｙ１・ｆＡ１）＋（Ａｙ２・ｆＡ２）｝
（６）
［式中、Ａｘ１は液相中の化合物１のピーク面積を、Ａ
ｘ２は液相中の化合物２のピーク面積を、Ａｙ１は気相
中の化合物１のピーク面積を、Ａｙ２は気相中の化合物
２のピーク面積を、ｆＡ１はガスクロマトグラフに導入
した化合物１の量とピーク面積を点綴して得られる直線
の傾きを、ｆＡ２はガスクロマトグラフに導入した化合
物２の量とピーク面積を点綴して得られる直線の傾きを
表す。］により求める必要があったため、多大の労力を
要していた。However, the relative volatility α of the two liquid compounds in the above-mentioned closed container is expressed by the following formula (2) α = (y 1 / x 1 ) / (y 2 / x 2 ) ( 2) [wherein α is the relative volatility of compound 1 to compound 2, x 1 is the mole fraction of compound 1 in the liquid phase, x 2 is the mole fraction of compound 2 in the liquid phase, y 1 represents the mole fraction of compound 1 in the gas phase, and y 2 represents the mole fraction of compound 2 in the gas phase. ], The molar fraction x in the above formula (2)
1 , x 2 , y 1 and y 2 are respectively represented by the following formulas (3) to (6) x 1 = (Ax 1 · f A1 ) / {(Ax 1 · f A1 ) + (Ax 2 · f A2 ). } (3) x 2 = ( Ax 2 · f A2) / {(Ax 1 · f A1) + (Ax 2 · f A2)} (4) y 1 = (Ay 1 · f A1) / {(Ay 1 · f A1) + (Ay 2 · f A2)} (5) y 2 = (Ay 2 · f A2) / {(Ay 1 · f A1) + (Ay 2 · f A2)} (6) [ wherein , Ax 1 is the peak area of Compound 1 in the liquid phase,
x 2 was the peak area of compound 2 in the liquid phase, Ay 1 was the peak area of compound 1 in the gas phase, Ay 2 was the peak area of compound 2 in the gas phase, and f A1 was the gas chromatograph. The slope of a straight line obtained by stippling the amount of compound 1 and the peak area, and f A2 represents the slope of a straight line obtained by stippling the amount of compound 2 and the peak area introduced into the gas chromatograph. ], It required a great deal of labor.
【０００４】[0004]
【課題を解決するための手段】本発明者は、上記問題点
を解決すべく鋭意検討した結果、式（１）
α=（Ａｙ１／Ａｘ１）／（Ａｙ２／Ａｘ２） （１）
［式中、αは化合物２に対する化合物１の相対揮発度
を、Ａｘ１は液相中の化合物１のピーク面積を、Ａｘ２
は液相中の化合物２のピーク面積を、Ａｙ１は気相中の
化合物１のピーク面積を、Ａｙ２は気相中の化合物２の
ピーク面積を表す。］を用いると、相対揮発度が容易に
算出できることを見出して、本発明を完成するに至っ
た。Means for Solving the Problems As a result of intensive studies to solve the above-mentioned problems, the present inventor has found that equation (1) α = (Ay 1 / Ax 1 ) / (Ay 2 / Ax 2 ) (1) [Wherein α is the relative volatility of Compound 1 with respect to Compound 2, Ax 1 is the peak area of Compound 1 in the liquid phase, Ax 2
Represents the peak area of compound 2 in the liquid phase, Ay 1 represents the peak area of compound 1 in the gas phase, and Ay 2 represents the peak area of compound 2 in the gas phase. ], It was found that the relative volatility can be easily calculated, and the present invention has been completed.
【０００５】即ち、本発明は、密閉容器中の２種の液体
化合物が混合された液相部と気相部とを、別々に、ガス
クロマトグラフに導入し、各相毎に検出された各化合物
のピーク面積を計測し、次いで、上式（１）から相対揮
発度を算出することを特徴とする相対揮発度の測定方法
を提供するものである。以下、本発明を詳細に説明す
る。That is, according to the present invention, a liquid phase part and a gas phase part in which two kinds of liquid compounds in a closed container are mixed are separately introduced into a gas chromatograph, and each compound detected for each phase is detected. The present invention provides a method for measuring relative volatility, which comprises measuring the peak area of, and then calculating the relative volatility from the above formula (1). Hereinafter, the present invention will be described in detail.
【０００６】[0006]
【発明の実施の形態】本発明において用いられる密閉容
器は、２種の液体化合物が混合された液相部と気相部と
を、別々に、ガスクロマトグラフに導入可能なものであ
ればよく、特に限定されるものではないが、例えば、ゴ
ム栓付のガラス製のサンプル瓶等が挙げられる。密閉容
器中の２種の液体化合物は互いに相溶性のものであり、
他に上記液体化合物と互いに相溶性の第三の液体化合物
ｎを含んでいてもよい。この場合の基準化合物２に対す
る化合物ｎの相対揮発度αｎは、下式（７）
αｎ＝（Ａｙｎ／Ａｘｎ）／（Ａｙ２／Ａｘ２） （７）
［式中、αｎは化合物２に対する化合物ｎの相対揮発度
を、Ａｘｎは液相中の化合物ｎのピーク面積を、Ａｘ２
は液相中の化合物２のピーク面積を、Ａｙｎは気相中の
化合物ｎのピーク面積を、Ａｙ２は気相中の化合物２の
ピーク面積を表す。］により、算出される。BEST MODE FOR CARRYING OUT THE INVENTION The closed container used in the present invention may be any as long as it can separately introduce a liquid phase part and a gas phase part in which two kinds of liquid compounds are mixed into a gas chromatograph, Although not particularly limited, examples thereof include a glass sample bottle with a rubber stopper. The two liquid compounds in the closed container are compatible with each other,
In addition, a third liquid compound n compatible with the above liquid compound may be contained. In this case, the relative volatility α n of the compound n with respect to the reference compound 2 is represented by the following formula (7) α n = (Ay n / Ax n ) / (Ay 2 / Ax 2 ) (7) [wherein, α n is The relative volatility of compound n with respect to compound 2, Ax n is the peak area of compound n in the liquid phase, and Ax 2
Represents the peak area of compound 2 in the liquid phase, Ay n represents the peak area of compound n in the gas phase, and Ay 2 represents the peak area of compound 2 in the gas phase. ] Is calculated.
【０００７】本発明において用いられるガスクロマトグ
ラフとしては、例えば、気相部を採取する際に、上記密
閉容器中で気液平衡状態になっている気相蒸気が放熱に
より凝縮しないように、保温機能を有したシリンジ、或
いは、恒温槽付のヘッドスペースガスサンプラーが付属
されたものが好ましい。The gas chromatograph used in the present invention has, for example, a heat retention function so that the vapor phase vapor in a vapor-liquid equilibrium state in the closed container is not condensed by heat dissipation when the vapor phase portion is sampled. It is preferable to use a syringe having a head space gas sampler with a constant temperature bath.
【０００８】[0008]
【実施例】以下、実施例により、本発明を更に詳細に説
明する。例中の「％」は、重量％である。The present invention will be described in more detail with reference to the following examples. "%" In the examples is% by weight.
【０００９】実施例１
７０℃に保温したトルエンとｎ−へキサンの混合液（下
記表１の液相）を、密閉容器（１）、恒温槽（２）及び
シリンジ（３）を有する図１に記載のガスクロマトグラ
フ（４）に導入し、各化合物のピーク面積をインテグレ
ーターで計算させた。次いで、上式（１）により、トル
エンに対するｎ−へキサンの相対揮発度αを算出して、
表１の値を得た。Example 1 A mixed liquid of toluene and n-hexane (liquid phase shown in Table 1 below) kept at 70 ° C. was placed in a closed container (1), a thermostat (2) and a syringe (3). Introduced into the gas chromatograph (4) described in 1 above, the peak area of each compound was calculated by an integrator. Then, the relative volatility α of n-hexane to toluene is calculated by the above formula (1),
The values in Table 1 were obtained.
【００１０】 表 １ 液相中のｎ−へキサン（％） 相対揮発度α ９９．４ ２．９６ ９８．８ ３．０９ ９６．７ ３．３８ ８９．１ ３．３７ ６７．９ ３．８７ [0010] Table 1 N-Hexane (%) in liquid phase Relative volatility α 99.4 2.96 98.8 3.09 96.7 3.38 89.1 3.37 67.9 3.87
【００１１】[0011]
【発明の効果】本発明によれば、密閉容器中の液体化合
物の混合液（液相部）と対応する気相部とを、別々にガ
スクロマトグラフに導入することにより、簡便に相対揮
発度を求めることができる。EFFECTS OF THE INVENTION According to the present invention, the relative volatility can be easily adjusted by separately introducing the liquid mixture (liquid phase portion) of the liquid compound in the closed container and the corresponding gas phase portion into the gas chromatograph. You can ask.
【図面の簡単な説明】[Brief description of drawings]
【図１】本発明の実施例で用いた装置FIG. 1 is an apparatus used in an embodiment of the present invention.
【図２】ガスクロマトグラムの例[Fig. 2] Example of gas chromatogram
１・・密閉容器、２・・恒温槽、３・・シリンジ、４・
・ガスクロマトグラフ、５・・インテグレーター1 ... Closed container, 2 ... Constant temperature bath, 3 ... Syringe, 4 ...
・ Gas chromatograph, 5 ・ ・ Integrator
───────────────────────────────────────────────────── フロントページの続き (72)発明者 楢原 英夫 大阪市此花区春日出中３丁目１番98号 住 友化学工業株式会社内 (72)発明者 山本 盛夫 大阪市此花区春日出中３丁目１番98号 住 友化学工業株式会社内 ─────────────────────────────────────────────────── ─── Continued front page (72) Inventor Hideo Narahara 3-1,98-1 Kasugade, Konohana-ku, Osaka Tomo Chemical Co., Ltd. (72) Inventor Morio Yamamoto 3-1,98-1 Kasugade, Konohana-ku, Osaka Tomo Chemical Co., Ltd.
Claims (2)
た液相部と気相部とを、別々に、ガスクロマトグラフに
導入し、各相毎に検出された各化合物のピーク面積を計
測し、次いで、下式（１）から相対揮発度を算出するこ
とを特徴とする相対揮発度の測定方法。 α=（Ａｙ１／Ａｘ１）／（Ａｙ２／Ａｘ２） （１） ［式中、αは化合物２に対する化合物１の相対揮発度
を、Ａｘ１は液相中の化合物１のピーク面積を、Ａｘ２
は液相中の化合物２のピーク面積を、Ａｙ１は気相中の
化合物１のピーク面積を、Ａｙ２は気相中の化合物２の
ピーク面積を表す。］1. A liquid phase part in which two liquid compounds are mixed in a closed container and a gas phase part are separately introduced into a gas chromatograph, and the peak area of each compound detected for each phase is measured. A method for measuring relative volatility, which comprises measuring and then calculating the relative volatility from the following formula (1). α = (Ay 1 / Ax 1 ) / (Ay 2 / Ax 2 ) (1) [wherein α is the relative volatility of compound 1 with respect to compound 2, and Ax 1 is the peak area of compound 1 in the liquid phase. , Ax 2
Represents the peak area of compound 2 in the liquid phase, Ay 1 represents the peak area of compound 1 in the gas phase, and Ay 2 represents the peak area of compound 2 in the gas phase. ]
ッドスペースガスサンプラーを用いて、気相部をガスク
ロマトグラフに導入する請求項１に記載の方法。2. The method according to claim 1, wherein the gas phase part is introduced into the gas chromatograph by using a syringe or a headspace gas sampler which can be kept warm by a heater.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002126190A JP2003014721A (en) | 2001-04-27 | 2002-04-26 | Measurement method of relative volatility |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001132014 | 2001-04-27 | ||
| JP2001-132014 | 2001-04-27 | ||
| JP2002126190A JP2003014721A (en) | 2001-04-27 | 2002-04-26 | Measurement method of relative volatility |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2003014721A true JP2003014721A (en) | 2003-01-15 |
Family
ID=26614434
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2002126190A Pending JP2003014721A (en) | 2001-04-27 | 2002-04-26 | Measurement method of relative volatility |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2003014721A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005026717A1 (en) * | 2003-09-10 | 2005-03-24 | Astellas Pharma Inc. | Method of analyzing vaporization pattern of solvent and solvent vacuum vaporization device |
-
2002
- 2002-04-26 JP JP2002126190A patent/JP2003014721A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005026717A1 (en) * | 2003-09-10 | 2005-03-24 | Astellas Pharma Inc. | Method of analyzing vaporization pattern of solvent and solvent vacuum vaporization device |
| JPWO2005026717A1 (en) * | 2003-09-10 | 2006-11-24 | アステラス製薬株式会社 | Solvent evaporation pattern analysis method and solvent vacuum evaporation apparatus |
| US7758317B2 (en) | 2003-09-10 | 2010-07-20 | Astellas Pharma Inc. | Method of analyzing vaporization pattern of solvent and solvent vacuum vaporization device |
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