JPH0690188B2 - Molecular weight distribution analysis method for polyarylate - Google Patents
Molecular weight distribution analysis method for polyarylateInfo
- Publication number
- JPH0690188B2 JPH0690188B2 JP14419890A JP14419890A JPH0690188B2 JP H0690188 B2 JPH0690188 B2 JP H0690188B2 JP 14419890 A JP14419890 A JP 14419890A JP 14419890 A JP14419890 A JP 14419890A JP H0690188 B2 JPH0690188 B2 JP H0690188B2
- Authority
- JP
- Japan
- Prior art keywords
- polyarylate
- molecular weight
- weight distribution
- dmf
- gpc
- 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
- 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〕 本発明はポリアリレート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
ィを用いたポリアリレートの品質管理，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 method for analyzing polyarylate molecular weight distribution.
More specifically, it relates to a suitable molecular weight distribution analysis method such as quality control and performance evaluation of polyarylate using gel permeation chromatography.
〔従来の技術〕 ポリアリレートの特徴として，下記の点が挙げられる。
１）強度に優れ，エンジニアリングプラスチックに属す
る,2）耐衝撃性がよく，バネ回復性も良好である,3）耐
熱性が高く，難燃性である,4）寸法安定性がよく，耐摩
耗性，耐薬品性が優れている。[Prior Art] The features of polyarylate are as follows.
1) Excellent in strength and belongs to engineering plastics, 2) Good impact resistance and good spring recovery, 3) High heat resistance and flame retardancy, 4) Good dimensional stability and wear resistance Excellent in chemical resistance and chemical resistance.
これらの特徴を生かして，ポリアリレートは電気関係
（スイッチ，ソケット，コネクタ等），機械関係（カメ
ラ部品，ポンプハウジング等），自動車部品（方向指示
レンズ，計器板レンズ等），その他（目薬容器，義歯，
文具，玩具等）に利用されている。Taking advantage of these features, polyarylate has electrical relations (switches, sockets, connectors, etc.), mechanical relations (camera parts, pump housings, etc.), automobile parts (direction indicating lenses, instrument plate lenses, etc.), and others (eye drop containers, Denture,
It is used for stationery, toys, etc.).
これらの各用途に要求されるポリアリレートの品質も様
々であり，これに応じてポリアリレートの品質を管理す
る必要がある。The quality of polyarylate required for each of these uses is various, and it is necessary to control the quality of polyarylate accordingly.
しかしながら，ポリアリレートは上記のように耐薬品性
に優れており，今までポリアリレートの分子量分布分析
はテトラヒドロフラン（またはクロロホルム）／ヘキサ
フルオロイソプロパノール（以下HFIPという）の混合溶
媒系で測定されていた。HFIPは刺激臭が非常に強く，ま
た価格も高価であるという欠点を有していた。However, polyarylate is excellent in chemical resistance as described above, and until now, the molecular weight distribution analysis of polyarylate was measured in a mixed solvent system of tetrahydrofuran (or chloroform) / hexafluoroisopropanol (hereinafter referred to as HFIP). HFIP had the drawback that it had a very strong pungent odor and was expensive.
上記の課題を解決するため，この発明はポリアリレート
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，刺激臭が少なく，安価な溶媒を用いて，
ポリアリレートの分子量分布分析法を確立するものであ
る。ポリアリレートはジメチルホルムアミド（以下DMF
という）に加熱溶解することを見いだした。In order to solve the above-mentioned problems, the present invention is intended to provide an analytical method capable of quality control and performance evaluation of polyarylate, and uses an inexpensive solvent with less irritating odor,
This establishes a molecular weight distribution analysis method for polyarylate. Polyarylate is dimethylformamide (hereinafter DMF
It was found that it melted by heating.
すなわち，ポリアリレートの溶解液としてDMFを用い，
ゲルパーミエーションクロマトグラフィ（以下GPCとい
う）の移動相としてDMFを用い，検出手段として紫外分
光光度計を用いたGPCによって分析することにより，ポ
リアリレートの分子量分布の測定を効率よく，正確に行
う方法を提供する。That is, using DMF as a solution of polyarylate,
A method for efficiently and accurately measuring the molecular weight distribution of polyarylate by using DMF as a mobile phase of gel permeation chromatography (hereinafter referred to as GPC) and GPC using an ultraviolet spectrophotometer as a detection means is provided. provide.
前記課題を解決するため，本発明方法は,GPCによりポリ
アリレートの分子量分布を測定する方法であって，ポリ
アリレートをDMFで加熱溶解し,DMFを溶離液として用い
たGPCに付して，紫外分光光度計で検出することによ
り，前記ポリアリレートの分子量分布を測定することを
特徴とするポリアリレートの分子量分布分析法である。In order to solve the above-mentioned problems, the method of the present invention is a method for measuring the molecular weight distribution of polyarylate by GPC, in which polyarylate is dissolved by heating with DMF, and subjected to GPC using DMF as an eluent to obtain an ultraviolet light A molecular weight distribution analysis method for polyarylate, characterized in that the molecular weight distribution of the polyarylate is measured by detection with a spectrophotometer.
前記した本発明の構成によれば，ポリアリレートのDMF
の溶液を,DMFからなる移動相中に導入してGPCに付すこ
とにより，ポリアリレート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, polyarylate DMF is used.
By introducing this solution into a mobile phase composed of DMF and subjecting it to GPC, the molecular weight distribution of polyarylate can be analyzed efficiently and accurately.
DMFを用いる理由としては，ポリアリレートの分子量分
布に対応した溶離をしやすいからである。GPCの検出器
として紫外分光光度計を用いる。これはポリアリレート
の分子量分布の検出に優れているからである。The reason for using DMF is that it is easy to elute corresponding to the molecular weight distribution of polyarylate. An ultraviolet spectrophotometer is used as a detector of GPC. This is because it is excellent in detecting the molecular weight distribution of polyarylate.
GPCの検出器として示差屈折計も用いることができる。A differential refractometer can also be used as a GPC detector.
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，上記ポリアリレートがDMFに加熱溶解
されて注入用溶液が調整された後，これがDMFを移動相
とするGPCに付される。この場合，ポリアリレート溶解
用のDMFと移動相のDMF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 polyarylate is heated and dissolved in DMF to prepare an injection solution, which is then applied to GPC having DMF as a mobile phase. In this case, it is preferable for the operation of the device that the DMF for dissolving polyarylate and the DMF for the mobile phase are the same.
前記において，ポリアリレートはDMFに0.2重量％程度加
熱溶解後，メンブランフィルタ（孔径:0.45μｍ）でろ
過し，そのろ液20μＬがHPLCに注入される。In the above, polyarylate was dissolved in DMF by heating at about 0.2% by weight, filtered through a membrane filter (pore size: 0.45 μm), and 20 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，例えば上記のス
チレン−ジビニルベンゼン共重合体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 a separation column used in GPC, a general-purpose polymer gel-filled column can be used, and the above-mentioned styrene-divinylbenzene copolymer-filled column 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。第一図は，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（紫外分光
光度計）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 (ultraviolet spectrophotometer) 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.
分析条件 カラム;Shim−pack GPC−806D,804D, 802D 三本連結（（株）島津製作所製） （各8mmI.D.x300mmL） 移動相;DMF 流 量;1.0mL/min 温 度;40℃ 検出器;SPD−6A（紫外分光光度計） （（株）島津製作所製） 波 長;270nm 感 度;0.32AUFS 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を用いてポリアリレートが分析できること
が確認できた。Analytical conditions Column; Shim-pack GPC-806D, 804D, 802D Triple connection (manufactured by Shimadzu Corporation) (8 mmI.D.x300 mmL each) Mobile phase; DMF flow rate; 1.0 mL / min temperature; 40 ° C detection Instrument; SPD-6A (ultraviolet spectrophotometer) (manufactured by Shimadzu Corporation) Wavelength: 270 nm Sensitivity: 0.32 AUFS The results of analysis under the above analysis conditions are shown in FIG. This second
From the figure, it was confirmed that polyarylate can be analyzed using GPC.
本発明は，ポリアリレートの溶離液としてDMFを用い,GP
Cの移動相としてDMFを用い，検出手段として紫外分光光
度計を用いたGPCによって分析することにより，ポリア
リレート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。The present invention uses DMF as an eluent for polyarylate and
By using DMF as the mobile phase of C and GPC analysis using an ultraviolet spectrophotometer as the detection means, the molecular weight distribution of polyarylate could be measured efficiently and accurately.
また，この分子量分布をGPCにより，簡便に得ることが
できた。Moreover, this molecular weight distribution could be easily obtained by GPC.
さらに，得られた分子量分布によりポリアリレートの品
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。Furthermore, the obtained molecular weight distribution has a special effect that the quality control and performance evaluation of polyarylate can be easily performed.
GPCの移動相に使用されるDMFは価格が安価あり，取扱い
が容易であるという効果も有する。The DMF used in the mobile phase of GPC is inexpensive and easy to handle.
第一図は本発明方法を実施する装置の一例の構成説明
図，第二図は本発明ポリアリレート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:移動相貯留相、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 a configuration explanatory view of an example of an apparatus for carrying out the method of the present invention, and FIG. 2 is a chromatogram showing a molecular weight distribution of a solution of the polyarylate of the present invention. 1: Mobile phase Stored phase, 2: Liquid transfer pump 3: Manual injector 4: Column, 5: Column oven 6: Differential refractometer, 7: Data processor
Claims (1)
よりポリアリレートの分子量分布を測定する方法であっ
て，ポリアリレートをジメチルホルムアミドで加熱溶解
し，ジメチルホルムアミドを溶離液として用いたゲルパ
ーミエーションクロマトグラフィに付して，紫外分光光
度計で検出することを特徴とするポリアリレートの分子
量分布分析法。1. A method for measuring the molecular weight distribution of polyarylate by gel permeation chromatography, which comprises heating polyallylate in dimethylformamide and subjecting it to gel permeation chromatography using dimethylformamide as an eluent. A molecular weight distribution analysis method for polyarylate, which is characterized by detection with an ultraviolet spectrophotometer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14419890A JPH0690188B2 (en) | 1990-05-31 | 1990-05-31 | Molecular weight distribution analysis method for polyarylate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14419890A JPH0690188B2 (en) | 1990-05-31 | 1990-05-31 | Molecular weight distribution analysis method for polyarylate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0436654A JPH0436654A (en) | 1992-02-06 |
| JPH0690188B2 true JPH0690188B2 (en) | 1994-11-14 |
Family
ID=15356498
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14419890A Expired - Lifetime JPH0690188B2 (en) | 1990-05-31 | 1990-05-31 | Molecular weight distribution analysis method for polyarylate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0690188B2 (en) |
-
1990
- 1990-05-31 JP JP14419890A patent/JPH0690188B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0436654A (en) | 1992-02-06 |
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