JPH0690191B2 - Molecular Weight Distribution Analysis Method of Ethylene Methacrylic Acid Elastomer - Google Patents
Molecular Weight Distribution Analysis Method of Ethylene Methacrylic Acid ElastomerInfo
- Publication number
- JPH0690191B2 JPH0690191B2 JP17411790A JP17411790A JPH0690191B2 JP H0690191 B2 JPH0690191 B2 JP H0690191B2 JP 17411790 A JP17411790 A JP 17411790A JP 17411790 A JP17411790 A JP 17411790A JP H0690191 B2 JPH0690191 B2 JP H0690191B2
- Authority
- JP
- Japan
- Prior art keywords
- methacrylic acid
- ethylene methacrylic
- molecular weight
- weight distribution
- elastomer
- 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.)
- Expired - Lifetime
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はエチレンメタクリル酸系エラストマーの分子量
分布分析法に関する。さらに詳しくは，ゲルパーミエー
ションクロマトグラフィ（以下,GPCという）を用いたエ
チレンメタクリル酸系エラストマーの品質管理，性能評
価等の好適な分子量分布分析法に関する。TECHNICAL FIELD The present invention relates to a molecular weight distribution analysis method for ethylene methacrylic acid-based elastomers. More specifically, it relates to a suitable molecular weight distribution analysis method such as quality control and performance evaluation of ethylene methacrylic acid-based elastomer using gel permeation chromatography (hereinafter referred to as GPC).
〔従来の技術〕 エチレンメタクリル酸系エラストマーの特徴として，下
記の点が挙げられる。[Prior Art] The characteristics of the ethylene methacrylic acid-based elastomer are as follows.
１）耐スクラッチ性 ２）耐候性 ３）ヒンジ特性 ４）スクイズ特性 ５）シボ転写性 ６）軽量 ７）耐薬品性 これらの特徴を生かして，エチレンメタクリル酸系エラ
ストマーは家電製品のケース，事務機器のケース，光学
機器のケース，文房具，自動車の外装部品などに使用さ
れている。1) Scratch resistance 2) Weather resistance 3) Hinge characteristics 4) Squeeze characteristics 5) Texture transferability 6) Light weight 7) Chemical resistance Taking advantage of these characteristics, ethylene methacrylic acid-based elastomers can be used for household electrical appliances cases and office equipment. It is used for cases, optical equipment cases, stationery, automobile exterior parts, etc.
これらの各用途に要求されるエチレンメタクリル酸系エ
ラストマーの品質も様々であり，これに応じてエチレン
メタクリル酸系エラストマーの品質を管理する必要があ
る。The quality of the ethylene methacrylic acid-based elastomer required for each of these uses varies, and it is necessary to control the quality of the ethylene methacrylic acid-based elastomer accordingly.
しかしながら，エチレンメタクリル酸系エラストマーは
上記のように耐薬品性に優れており今までエチレンメタ
クリル酸系エラストマーを溶解する適当な溶媒がなく，
エチレンメタクリル酸系エラストマーの分子量分布測定
は行われていなかった。However, ethylene methacrylic acid-based elastomers have excellent chemical resistance as described above, and until now there is no suitable solvent for dissolving ethylene methacrylic acid-based elastomers,
The molecular weight distribution of the ethylene methacrylic acid-based elastomer has not been measured.
上記の課題を解決するため，この発明はエチレンメタク
リル酸系エラストマーの品質管理や性能評価が可能な分
析法を提供しようとするものであり，エチレンメタクリ
ル酸系エラストマー分子量分布分析法を確立するもので
ある。In order to solve the above problems, the present invention is intended to provide an analytical method capable of quality control and performance evaluation of ethylene methacrylic acid type elastomer, and establishes an ethylene methacrylic acid type elastomer molecular weight distribution analytical method. is there.
本件発明者は鋭意検討の結果，エチレンメタクリル酸系
エラストマーはシクロヘンサンに加熱溶解することを見
いだし本発明をなすに至った。As a result of diligent studies, the inventors of the present invention have found that an ethylene methacrylic acid-based elastomer is heated and dissolved in cyclohensan, and have completed the present invention.
すなわち本発明は,GPCによりエチレンメタクリル酸系エ
ラストマーの分子量分布を測定する方法であって，エチ
レンメタクリル酸系エラストマーをシクロヘキサンで加
熱溶解し，これをシクロヘキサンを移動相としてGPCに
付して，その溶解液を示差屈折計で検出することによ
り，前記エチレンメタクリル酸系エラストマーの分子量
分布を測定することを特徴とするエチレンメタクリル酸
系エラストマーの分子量分布分析法である。That is, the present invention is a method for measuring the molecular weight distribution of an ethylene methacrylic acid-based elastomer by GPC, in which an ethylene methacrylic acid-based elastomer is heated and dissolved with cyclohexane, and this is subjected to GPC with cyclohexane as a mobile phase, and the dissolution thereof is performed. A molecular weight distribution analysis method for ethylene methacrylic acid-based elastomers, characterized in that the molecular weight distribution of the ethylene methacrylic acid-based elastomer is measured by detecting the liquid with a differential refractometer.
前記した本発明の構成によれば，エチレンメタクリル酸
系エラストマーのシクロヘキサンの溶液を，シクロヘキ
サンからなる移動相中に導入してGPCに付すことによ
り，エチレンメタクリル酸系エラストマーの分子量分布
を効率良く・かつ正確に分析できる。According to the above-described configuration of the present invention, a solution of ethylenemethacrylic acid-based elastomer in cyclohexane is introduced into a mobile phase composed of cyclohexane and subjected to GPC, whereby the molecular weight distribution of the ethylenemethacrylic acid-based elastomer is efficiently and Can be analyzed accurately.
シクロヘキサンを用いる理由としては，エチレンメタク
リル酸系エラストマーの分子量分布に対応した溶離をし
やすいからである。GPCの検出器として示差屈折計を用
いる。これはエチレンメタクリル酸系エラストマーの分
子量分布の検出に優れているからである。The reason for using cyclohexane is that it is easy to elute corresponding to the molecular weight distribution of ethylene methacrylic acid elastomer. A differential refractometer is used as a detector of GPC. This is because it is excellent in detecting the molecular weight distribution of the ethylene methacrylic acid elastomer.
GPCは，例えば多孔性スチレン−ジビニルベンゼン系重
合体球状微粒子を充てん剤としたカラムに，分析しよう
とする試料を移動相溶媒に溶解させた溶液を付し，試料
分子の大きいものから順に分子のサイズ別に分離させ，
試料分子の量を分析するものである。GPC is, for example, a column containing porous styrene-divinylbenzene polymer spherical particles as a packing material and a solution of the sample to be analyzed dissolved in a mobile phase solvent. Separate by size,
The amount of sample molecules is analyzed.
本発明において，上記エチレンメタクリル酸系エラスト
マーがシクロヘキサンに加熱溶解されて注入用溶液が調
整された後，これがシクロヘキサンを移動相とするGPC
に付される。この場合，エチレンメタクリル酸系エラス
トマー溶解用のシクロヘキサンと移動相のシクロヘキサ
ンとは同一であることが，装置の操作上好ましい。In the present invention, the above ethylene methacrylic acid-based elastomer is heated and dissolved in cyclohexane to prepare a solution for injection, which is then used as a GPC containing cyclohexane as a mobile phase.
Attached to. In this case, it is preferable for the operation of the apparatus that the cyclohexane for dissolving the ethylene methacrylic acid-based elastomer be the same as the cyclohexane for the mobile phase.
前記において，エチレンメタクリル酸系エラストマーは
シクロヘキサンに0.4重量％程度加熱溶解後，その溶解
部分をメンブランフィルタ（孔系:0.45μｍ）でろ過
し，そのろ液200μＬがHPLCに注入される。In the above, the ethylene methacrylic acid-based elastomer was dissolved in cyclohexane by heating at about 0.4% by weight, the dissolved portion was filtered through a membrane filter (pore system: 0.45 μm), and 200 μL of the filtrate was injected into HPLC.
一方,GPCで用いる分離カラムとしては，汎用の高分子ゲ
ルを充てんしたものが使用可能であり，例えばビニルア
ルコールコポリマーの充てんカラムが好適な例として挙
げられる。On the other hand, as the separation column used in GPC, a column packed with a general-purpose polymer gel can be used, and a column packed with a vinyl alcohol copolymer is a suitable example.
また,GPC自体は汎用のものを使用できる。In addition, GPC itself can be general purpose.
以下，図面および測定例により本発明方法を詳細に説明
する。なお，本発明は下記の実施例に限定されるもので
はない。第１図は，この発明の方法を実施する装置の一
例の構成説明図である。この図において,1は移動相貯留
槽,2は送液ポンプ,3はマニュアルインジェクタ,4はカラ
ム,5はカラムオーブン,6は示差屈折計,7はデータ処理装
置である。Hereinafter, the method of the present invention will be described in detail with reference to the drawings and measurement examples. The present invention is not limited to the examples below. FIG. 1 is a structural explanatory view of an example of an apparatus for carrying out the method of the present invention. In this figure, 1 is a mobile phase storage tank, 2 is a liquid feed pump, 3 is a manual injector, 4 is a column, 5 is a column oven, 6 is a differential refractometer, and 7 is a data processor.
移動相１からポンプ２によりあらかじめ溶離液を流し，
定常状態を作る。注入された試料は溶離液によりカラム
オーブン５中のカラム４に送られ，検出器６（示差屈折
計）により分子量分布が検出される。このデータをデー
タ処理装置７で処理し，分子量分布の計算を行う。The eluent is made to flow from the mobile phase 1 by the pump 2 in advance,
Create a steady state. The injected sample is sent to the column 4 in the column oven 5 by the eluent, and the detector 6 (differential refractometer) detects the molecular weight distribution. This data is processed by the data processor 7 to calculate the molecular weight distribution.
以上装置を用いて，下記の分析条件により分析を行っ
た。Using the above equipment, analysis was performed under the following analysis conditions.
（１）分析条件 カラム;Asahipak GS−510H （（株）島津製作所製） （7.6mmI.D.x250mmL） 移動相；シクロヘキサン 流 量;0.5mL/min 温 度;40℃ 検出器;RID−6A（示差屈折計） （（株）島津製作所製） ボラリティ；＋ 感 度;16x10-6RIUFS 上記分析条件で分析した結果を第２図に示す。この第２
図によりGPCを用いてエチレンメタクリル酸系エラスト
マーが分析できることが確認できた。(1) Analytical conditions Column; Asahipak GS-510H (manufactured by Shimadzu Corporation) (7.6mmI.D.x250mmL) Mobile phase; Cyclohexane flow rate; 0.5mL / min temperature; 40 ° C detector; RID-6A ( Differential refractometer) (manufactured by Shimadzu Corporation) Volatility; + Sensitivity; 16x10 -6 RIUFS Figure 2 shows the results of analysis under the above analytical conditions. This second
From the figure, it was confirmed that the ethylene methacrylic acid-based elastomer could be analyzed using GPC.
なお，第２図の縦軸は信号強度，横軸は保持容量を表
す。The vertical axis of FIG. 2 represents the signal intensity and the horizontal axis represents the storage capacity.
本発明は，エチレンメタクリル酸系エラストマーの溶離
液としてシクロヘキサンを用い,GPCの移動相としてシク
ロヘキサンを用い，検出手段として示差屈折計を用いた
GPCによって分析することにより，エチレンメタクリル
酸系エラストマーの分子量分布の測定を効率良く正確に
行うことができた。In the present invention, cyclohexane is used as an eluent of ethylene methacrylic acid-based elastomer, cyclohexane is used as a mobile phase of GPC, and a differential refractometer is used as a detection means.
By GPC analysis, the molecular weight distribution of ethylene methacrylic acid elastomer could be measured efficiently and accurately.
そして，得られた分子量分布によりエチレンメタクリル
酸系エラストマーの品質管理，性能評価が簡単に行える
という特別な効果を有する。The obtained molecular weight distribution has a special effect that the quality control and performance evaluation of the ethylene methacrylic acid-based elastomer can be easily performed.
第１図は本発明方法を実施する装置の一例の構成説明
図，第２図は本発明エチレンメタクリル酸系エラストマ
ーの溶解液についての分子量分布を表すクロマトグラム
である。 1:移動相貯留槽、2:送液ポンプ 3:マニュアルインジェクタ 4:カラム、5:カラムオーブン 6:示差屈折計、7:データ処理装置FIG. 1 is an explanatory view of the constitution of an example of an apparatus for carrying out the method of the present invention, and FIG. 2 is a chromatogram showing the molecular weight distribution of a solution of the ethylene methacrylic acid elastomer of the present invention. 1: Mobile phase reservoir, 2: Liquid transfer pump 3: Manual injector 4: Column, 5: Column oven 6: Differential refractometer, 7: Data processing device
Claims (1)
クロヘキサンで加熱溶解し，これをシクロヘキサンを移
動相としてゲルパーミエーションクロマトグラフカラム
に付し，該カラムからの溶離液を示差屈折計で検出する
ことを特徴とするエチレンメタクリル酸系エラストマー
の分子量分布分析法。1. An ethylene methacrylic acid-based elastomer is heated and dissolved in cyclohexane, which is applied to a gel permeation chromatograph column with cyclohexane as a mobile phase, and the eluent from the column is detected by a differential refractometer. Method of molecular weight distribution analysis of ethylene methacrylic acid elastomer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17411790A JPH0690191B2 (en) | 1990-06-29 | 1990-06-29 | Molecular Weight Distribution Analysis Method of Ethylene Methacrylic Acid Elastomer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP17411790A JPH0690191B2 (en) | 1990-06-29 | 1990-06-29 | Molecular Weight Distribution Analysis Method of Ethylene Methacrylic Acid Elastomer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0462472A JPH0462472A (en) | 1992-02-27 |
| JPH0690191B2 true JPH0690191B2 (en) | 1994-11-14 |
Family
ID=15972940
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP17411790A Expired - Lifetime JPH0690191B2 (en) | 1990-06-29 | 1990-06-29 | Molecular Weight Distribution Analysis Method of Ethylene Methacrylic Acid Elastomer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0690191B2 (en) |
-
1990
- 1990-06-29 JP JP17411790A patent/JPH0690191B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0462472A (en) | 1992-02-27 |
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