JPH0436653A - Analysis of molecular weight distribution of polypropylene - Google Patents
Analysis of molecular weight distribution of polypropyleneInfo
- Publication number
- JPH0436653A JPH0436653A JP14419790A JP14419790A JPH0436653A JP H0436653 A JPH0436653 A JP H0436653A JP 14419790 A JP14419790 A JP 14419790A JP 14419790 A JP14419790 A JP 14419790A JP H0436653 A JPH0436653 A JP H0436653A
- Authority
- JP
- Japan
- Prior art keywords
- polypropylene
- cyclohexane
- molecular weight
- weight distribution
- eluent
- 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.)
- Granted
Links
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 32
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 32
- -1 polypropylene Polymers 0.000 title claims abstract description 31
- 238000004458 analytical method Methods 0.000 title claims abstract description 11
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003480 eluent Substances 0.000 claims abstract description 7
- 238000005227 gel permeation chromatography Methods 0.000 claims abstract 7
- 238000000034 method Methods 0.000 claims description 8
- 238000005259 measurement Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000003908 quality control method Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- CXWXQJXEFPUFDZ-UHFFFAOYSA-N tetralin Chemical compound C1=CC=C2CCCCC2=C1 CXWXQJXEFPUFDZ-UHFFFAOYSA-N 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 2
- NNBZCPXTIHJBJL-UHFFFAOYSA-N decalin Chemical compound C1CCCC2CCCCC21 NNBZCPXTIHJBJL-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- JTPNRXUCIXHOKM-UHFFFAOYSA-N 1-chloronaphthalene Chemical compound C1=CC=C2C(Cl)=CC=CC2=C1 JTPNRXUCIXHOKM-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000012778 molding material Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はポリプロピレンの分子量分布分析法に関すル。[Detailed description of the invention] [Industrial application field] The present invention relates to a method for analyzing the molecular weight distribution of polypropylene.
さらに詳しくは、ゲ〜バーミエーシ璽ンクロマトグラフ
ィを用いたポリプロピレンの品質管理、性能評価等の好
適な分子量分布分析法に関する。More specifically, the present invention relates to a suitable molecular weight distribution analysis method for quality control, performance evaluation, etc. of polypropylene using Ge-Vermisch chromatography.
ボップロピレンの特徴として、下記の点が挙げられる。 The characteristics of VOPP propylene include the following points.
１）透明で、結晶性である。２）剛性があり。1) Transparent and crystalline. 2) It has rigidity.
成形材料にも用いられる。３）耐摩耗性に優れ、＃熱性
もある２４）！気持性に優れ、耐水、耐薬品性に優れる
うなどであるっ
これらの特徴を生かして、ポリプロピレンはフィルム（
農業用、産業用）９日用品類（キャップ。It is also used as a molding material. 3) Excellent wear resistance and heat resistance 24)! Taking advantage of these characteristics, polypropylene can be used as a film (
Agriculture, industrial use) 9 Daily necessities (caps).
台所用品等）、コンテナ類、紐類（延伸モノフィラメン
１．バンド、ロープ等）、電気関係（テレビ・ラジオケ
ース、テーブルタップ等）、ｌ［ｌ車部品１機械部品、
その他に利用される。kitchen utensils, etc.), containers, strings (stretched monofilament 1. bands, ropes, etc.), electrical equipment (TV/radio cases, table taps, etc.), car parts 1 mechanical parts,
Used for other purposes.
これらの各用途に要求されるボップロピレンの品質も様
々であり、これに応じてポリプロピレンの品質を管理す
る必要がある。The quality of polypropylene required for each of these uses varies, and it is necessary to control the quality of polypropylene accordingly.
しかしながら、ポリプロピレンは上記のように耐薬品性
に優れており、良溶媒としてはテトラリン、デカリン、
α−クロロナフタレンなどがあるが、いずれの溶媒も１
３０℃以上でないと溶解せず・分子量分布を測定するに
は専用の高ｆＡＧＰｃシステムが必要でめった。However, as mentioned above, polypropylene has excellent chemical resistance, and good solvents include tetralin, decalin,
α-chloronaphthalene, etc., but all solvents have 1
It does not dissolve unless the temperature is 30°C or higher, and a dedicated high-fAGPc system is required to measure the molecular weight distribution, which was difficult.
上記の課題を解決するため、この発明はポリプロピレン
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、汎用のＧＰＣシステムでポリプロピレン
の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 aims to provide an analysis method capable of quality control and performance evaluation of polypropylene, and establishes a molecular weight distribution analysis method for polypropylene using a general-purpose GPC system.
すなわち、ポリプロピレンの溶解液トシてシクロヘキサ
ンヲ用い、ゲμパーミエーシミンクロマトグラフイ（以
下ＧＰＣという）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Ｋよシ。That is, it is easier to analyze by GPC using cyclohexane as a solution of polypropylene, cyclohexane as the mobile phase of gel permeability chromatography (hereinafter referred to as GPC), and a differential refractometer as a detection means. .
ポリプロピレンの分子量分布の測定を効率よく。Efficiently measure the molecular weight distribution of polypropylene.
正確に行う方法を提供する。Provide a method to do it correctly.
前記課題を解決するため１本発明方法は、 ＧＰＣＫよ
りポリプロピレンの分子量分布＠：ｉＩＩ定する方法で
あって、ポリプロピレンをシクロヘキサンテ加熱溶解し
、シクロヘキサンを溶離液として用いたＧＰＣに付して
、示差屈折計で検出することによシ、前記ポリプロピレ
ンの分子量分布を測定することを特徴とするポリプロピ
レンの分子量分布分析法である。In order to solve the above problems, one method of the present invention is to determine the molecular weight distribution of polypropylene by GPCK. This is a method for analyzing the molecular weight distribution of polypropylene, characterized in that the molecular weight distribution of the polypropylene is measured by detection with a refractometer.
前記した本発明の構成によれば、ポリプロピレンのシク
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に付すことにょシ、ポリプロピレンの
分子量分布を効率良く、かつ正確に分析できる。According to the configuration of the present invention described above, the molecular weight distribution of polypropylene can be efficiently and accurately analyzed by introducing a solution of polypropylene in cyclohexane into a mobile phase consisting of cyclohexane and subjecting it to GPC.
シクロヘキサンを用いる理出としては、ポリプロピレン
の分子量分布に対応した溶離をしやすいからである６Ｇ
ＰＣの検出器として示差屈折計を用いる。これはポリプ
ロピレン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 according to the molecular weight distribution of polypropylene.
A differential refractometer is used as a PC detector. This is because it is excellent in detecting the molecular weight distribution of polypropylene.
ＧＰＣは１例えば多孔性スチレンージビニμ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１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。In GPC, a solution prepared by dissolving the sample to be analyzed in a mobile phase solvent is applied to a column packed with, for example, spherical fine particles of porous styrene-divinybenzene polymer, and the size of the sample molecules is measured in descending order of size. It separates the sample molecules separately and analyzes the amount of sample molecules.
本発明において、上記ポリプロピレンがシクロヘキサン
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トスるＧＰＣＫ付される。この場
合、ポリプロピレン溶解用のシクロヘキサンと移動相の
シクロヘキサントハ同一であることが、装置の操作上好
ましい。In the present invention, after the polypropylene is heated and dissolved in cyclohexane to prepare a solution for injection, this is subjected to GPCK by tossing cyclohexane as a mobile phase. In this case, it is preferable for the operation of the apparatus that the cyclohexane for dissolving the polypropylene and the cyclohexane for the mobile phase are the same.
前記において、ポリプロピレンはシクロヘキサンＫＯ２
２重量％程度加熱溶解後、メンブランフイμり（孔径：
０．４５μｍ）でろ過し、そのろ＠２００μＬがＨＰＬ
ＣＫ注入される。In the above, polypropylene is cyclohexane KO2
After heating and dissolving about 2% by weight, membrane filtration (pore size:
0.45μm), and the filter @200μL is HPL
CK is injected.
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奄のが使用可能であす１例工ばビニ
ルアＶコールコホ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 a separation column used in GPC, an Amano column filled with a general-purpose polymer gel can be used, and a suitable example is a column packed with a vinyl V-col copolymer.
また、ＧＰＣ自体は汎用のものを使用できる。Moreover, a general-purpose GPC itself can be used.
以下６図面および測定例により不発明方法を詳ＮｉＫ説
明する。なお１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はマニエアルインジェクタ
、４はカラム。The non-inventive method will be explained in detail below with reference to six drawings and measurement examples. Note that the present invention is not limited to the following examples. FIG. 1 is an explanatory diagram of the configuration 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 pump, 3 is a manual injector, and 4 is a column.
５はカラムオープン、６ｉｉ示差屈折計、７はデータ処
理装置である。5 is a column open, 6ii is a differential refractometer, and 7 is a data processing device.
移動相１からポンプ２！ＩＣ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ｆｆＫよυ
カラムオープン５中のカラム４に送られ。Mobile phase 1 to pump 2! The eluent is flowed through the IC in advance to establish a steady state. The injected sample elutes ffK
Sent to column 4 in column open 5.
検出器６（示差屈折計）Ｋ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。The molecular weight distribution is detected by a detector 6 (differential refractometer) K. This data is processed by the data processing device 7.
分子量分布、の計算を行う。Calculate the molecular weight distribution.
以上装置を用いて、下記の分析条件によシ分析を行った
。Using the above apparatus, an analysis was conducted under the following analysis conditions.
分析条件
カラＡ ； Ａｓａｈｉｐａｋ Ｇ５−５１０Ｈ（−島
津製作所製）
（７，６ｍｍ１ 、 Ｄ−ｘ２５０ｔｎｍＬ ）移動相
；シクロヘキサン
流 量； ０．５ ｍ Ｌ／ｍ ｉ ｎ温 度； ４
０℃
検出Ｗ＃１ＲＩＤ−６Ａ（示差屈折計）（−島津製作所
製）
ポラリティ；＋
感 度ｉ ３２ｘｌＯＲＩＵＦ８上記分析条
件で分析した結果を第２図に示す。Analysis conditions A: Asahipak G5-510H (manufactured by Shimadzu Corporation) (7.6 mm1, D-x250 tnmL) Mobile phase: Cyclohexane flow rate: 0.5 mL/min Temperature: 4
0° C. Detection W#1 RID-6A (differential refractometer) (manufactured by Shimadzu Corporation) Polarity; + Sensitivity i 32xlORIUF8 The results of analysis under the above analysis conditions are shown in FIG.
この＠２図によｐＧＰｃを用いてポリプロピレンが分析
できることが確認できた。This @2 diagram confirms that polypropylene can be analyzed using pGPc.
本発明は、ポリプロピレンの溶離液としてシクロヘキサ
ンを用い、ｏｐｃｆ）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針を用いたＧＰＣによって
分析することによシ、ポリエチレンの分子量分布の測定
を効率良く、正確に行うことができ九。移動相にシクロ
ヘキサンを用いることによシ、従来高温ＧＰＣでしか分
析できなかりたポリプロピレンを汎用のＧＰＣシステム
で分析することが可能になった。The present invention efficiently measures the molecular weight distribution of polyethylene by using cyclohexane as an eluent for polypropylene, using cyclohexane as an OPCF mobile phase, and analyzing by GPC using a differential refraction needle as a detection means. Nine things can be done accurately. By using cyclohexane as the mobile phase, it has become possible to analyze polypropylene, which could previously only be analyzed using high-temperature GPC, using a general-purpose GPC system.
また、この分子量分布をＧＰＣによシ、簡便に得る仁と
ができた。Furthermore, it was possible to easily obtain this molecular weight distribution by GPC.
さらに、得られた分子量分布によシポリプロピレンの品
質管理、性能評価が簡単に行えるという特別な効果を有
する口Furthermore, the molecular weight distribution obtained has the special effect of making it easy to perform quality control and performance evaluation of polypropylene.
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プロピレン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：ｖニエアル
インジエクタ
４：カラム ５：カラムオーブン６：示差屈
折計 ７：データ処理装置晃 １ 回
イにオケ＠閘 （分）
第２ 圓Figure 1 is an explanatory diagram of the configuration of an example of an apparatus for carrying out the method of the present invention, and Figure 2 is a chromatogram showing the molecular weight distribution of a solution of the polypropylene of the present invention. 1: Mobile phase storage phase 2: Liquid pump 3: Injector 4: Column 5: Column oven 6: Differential refractometer 7: Data processor Akira
Claims (1)
リプロピレンの分子量分布を測定する方法であつて、ポ
リプロピレンをシクロヘキサンで加熱溶解し、シクロヘ
キサン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、示差屈折計で検出することを特
徴とするポリプロピレンの分子量分布分析法。(1) A method of measuring the molecular weight distribution of polypropylene by gel permeation chromatography, in which polypropylene is heated and dissolved in cyclohexane, subjected to gel permeation chromatography using cyclohexane as an eluent, and detected with a differential refractometer. A molecular weight distribution analysis method for polypropylene characterized by the following.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14419790A JPH0690187B2 (en) | 1990-05-31 | 1990-05-31 | Molecular weight distribution analysis method for polypropylene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14419790A JPH0690187B2 (en) | 1990-05-31 | 1990-05-31 | Molecular weight distribution analysis method for polypropylene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0436653A true JPH0436653A (en) | 1992-02-06 |
| JPH0690187B2 JPH0690187B2 (en) | 1994-11-14 |
Family
ID=15356474
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14419790A Expired - Lifetime JPH0690187B2 (en) | 1990-05-31 | 1990-05-31 | Molecular weight distribution analysis method for polypropylene |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0690187B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6489056B1 (en) | 2000-09-18 | 2002-12-03 | The Gillette Company | Battery including a hydrogen-absorbing cathode material |
-
1990
- 1990-05-31 JP JP14419790A patent/JPH0690187B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6489056B1 (en) | 2000-09-18 | 2002-12-03 | The Gillette Company | Battery including a hydrogen-absorbing cathode material |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0690187B2 (en) | 1994-11-14 |
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