JPS63284463A - Method for determining decomposition residue of crosslinking agent of crosslinked polyethylene - Google Patents
Method for determining decomposition residue of crosslinking agent of crosslinked polyethyleneInfo
- Publication number
- JPS63284463A JPS63284463A JP11815487A JP11815487A JPS63284463A JP S63284463 A JPS63284463 A JP S63284463A JP 11815487 A JP11815487 A JP 11815487A JP 11815487 A JP11815487 A JP 11815487A JP S63284463 A JPS63284463 A JP S63284463A
- Authority
- JP
- Japan
- Prior art keywords
- crosslinking agent
- decomposition residue
- internal standard
- crosslinked polyethylene
- agent decomposition
- 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
- 239000003431 cross linking reagent Substances 0.000 title claims abstract description 22
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 20
- 229920003020 cross-linked polyethylene Polymers 0.000 title claims abstract description 13
- 239000004703 cross-linked polyethylene Substances 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title claims description 7
- 238000011088 calibration curve Methods 0.000 claims abstract description 4
- 238000000638 solvent extraction Methods 0.000 claims abstract description 3
- 239000012086 standard solution Substances 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 6
- 239000012488 sample solution Substances 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract 3
- 239000007788 liquid Substances 0.000 abstract 3
- 238000001514 detection method Methods 0.000 abstract 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 9
- ZWRUINPWMLAQRD-UHFFFAOYSA-N nonan-1-ol Chemical compound CCCCCCCCCO ZWRUINPWMLAQRD-UHFFFAOYSA-N 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- OIGWAXDAPKFNCQ-UHFFFAOYSA-N 4-isopropylbenzyl alcohol Chemical compound CC(C)C1=CC=C(CO)C=C1 OIGWAXDAPKFNCQ-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- XYLMUPLGERFSHI-UHFFFAOYSA-N alpha-Methylstyrene Chemical compound CC(=C)C1=CC=CC=C1 XYLMUPLGERFSHI-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000010813 internal standard method Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- -1 polyethylene Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、架橋ポリエチレンの架橋度を把握するための
架橋剤分解残さ定量法、とくにはガスクロマトグラフ質
量分析装置による架橋ポリエチレンの架橋剤分解残さ定
量法に関するものである。Detailed Description of the Invention (Industrial Application Field) The present invention relates to a method for quantifying crosslinking agent decomposition residue in order to understand the degree of crosslinking of crosslinked polyethylene, and in particular, a method for quantifying crosslinking agent decomposition residue in crosslinked polyethylene using a gas chromatograph mass spectrometer. It is related to quantitative methods.
（従来技術とその問題点）
従来、架橋ポリエチレンの架橋度を把握するための架橋
剤分解残さの定量法としては、液体クロマトグラフィー
、ガスクロマトグラフィーなどにより行なわれていたが
、得られるクロマトグラムの目的成分のピークが共存す
る他成分のピークと重なり、目的成分の正確な定量を阻
害することがあったほか、分析装置への試料注入量が変
化すると精度が悪くなるという欠点があった。さらに、
従来の検出器は質量分析の場合に比べて一桁以上も低感
度のため詳細な情報を得るには不十分であった・
（問題点を解決するための手段）
本発明者らは上記問題点の解決のため鋭意検討の結果、
架橋ポリエチレンを溶媒抽出して得られる抽出液に、内
部標準溶液を加えてガスクロマトグラフ質量分析装置に
より各成分に分離し、この内部標準溶液および架橋剤分
解残さに対応する複数の化合物のＭ／Ｚ （Ｚは荷電を
、Ｍは質量を表わす）の各イオン量を測定し、内部標準
溶液に対応する化合物と架橋剤分解残さに対応する化合
物の応答イオン量（ピーク面積またはピーク高さ）の比
を求め、あらかじめ標準溶液を用いて作成した検量線よ
り各架橋剤分解残さの試料溶液中の濃度を求めることに
より、架橋ポリエチレンからの複数の架橋剤分解残さを
同時に精度良く検出定量できることを見出し、本発明を
完成するに至ったものである。(Prior art and its problems) Conventionally, liquid chromatography, gas chromatography, etc. have been used to quantify the crosslinking agent decomposition residue in order to determine the degree of crosslinking of crosslinked polyethylene. In addition to the fact that the peak of the target component overlaps with the peak of other coexisting components, which sometimes impedes accurate quantification of the target component, there is also a drawback that accuracy deteriorates when the amount of sample injected into the analyzer changes. moreover,
The sensitivity of conventional detectors is more than one order of magnitude lower than that of mass spectrometry, so it was insufficient to obtain detailed information. (Means for solving the problem) The present inventors have solved the above problem. As a result of intensive study to resolve the issue,
An internal standard solution is added to the extract obtained by solvent extraction of crosslinked polyethylene and separated into each component using a gas chromatograph mass spectrometer, and the M/Z of multiple compounds corresponding to this internal standard solution and crosslinking agent decomposition residue is determined. Measure the amount of each ion (Z represents charge and M represents mass), and calculate the ratio of the response ion amount (peak area or peak height) of the compound corresponding to the internal standard solution and the compound corresponding to the crosslinking agent decomposition residue. By determining the concentration of each crosslinking agent decomposition residue in the sample solution from a calibration curve prepared in advance using standard solutions, we discovered that it is possible to simultaneously detect and quantify multiple crosslinking agent decomposition residues from crosslinked polyethylene with high accuracy. This has led to the completion of the present invention.
つぎに１本発明の方法を、ポリエチレンの架橋剤として
ジクミルパーオキサイドを用いた場合の架橋剤分解残さ
の定量法を例として、より具体的に説明する。Next, the method of the present invention will be explained in more detail by taking as an example a method for quantifying the decomposition residue of a crosslinking agent when dicumyl peroxide is used as a crosslinking agent for polyethylene.
まずヘキサンまたはアセトン８０醜ｌを抽出溶剤として
、試料２ｇをソックスレー抽出器に入れ、６時間抽出す
る。この抽出液を１００ｇ＋１メスフラスコに移し入れ
、これに内部標準ｎ−ノニルアルコールの０．５容量％
のヘキサン溶液を２ｍｌ加えてヘキサンで標線まで希釈
する。この溶液を試料としてガスクロマトグラフ質量分
析装置によりｎ−ノニルアルコールおよびジクミルパー
オキサイドの分解残さであるα−メチルスチレン、アセ
トフェノン、クミルアルコールの各化合物に対応するＭ
／Ｚ：８３．１１８．１０５．１２１の各イオンをマス
フラグメントグラフィーにより測定する。得られるＭ／
Ｚ：１１８．１０５．１２１のマスフラグメントグラム
のそれぞれα−メチルスチレン、アセトフェノン、クミ
ルアルコールの保持時間におけるピーク面積またはピー
ク高さと。First, using 80 liters of hexane or acetone as an extraction solvent, 2 g of the sample was placed in a Soxhlet extractor and extracted for 6 hours. Transfer 100g of this extract to a volumetric flask and add 0.5% by volume of the internal standard n-nonyl alcohol.
Add 2 ml of hexane solution and dilute to the marked line with hexane. Using this solution as a sample, a gas chromatograph mass spectrometer was used to determine the M
/Z: Each ion of 83.118.105.121 is measured by mass fragmentography. Obtained M/
Z: The peak area or peak height at the retention time of α-methylstyrene, acetophenone, and cumyl alcohol in the mass fragment gram of 118.105.121.
Ｍ／Ｚ：８３のマスフラグメントグラムのｎ−ノニルア
ルコールの保持時間におけるピーク面積またはピーク高
さの比を求め、あらかじめ標準溶液を用いて作成した検
量線により各架橋剤分解残さの試料溶液中の濃度を求め
る。M/Z: The ratio of the peak area or peak height at the retention time of n-nonyl alcohol in the mass fragment gram of 83 was determined, and the ratio of the peak area or peak height in the sample solution of each crosslinking agent decomposition residue was determined using a calibration curve prepared in advance using a standard solution. Find the concentration.
検体架橋ポリエチレン中の含有量は次式によって算出す
る。The content in the sample crosslinked polyethylene is calculated using the following formula.
架橋ポリエチレン中の架橋剤分解残さ量（％）本発明の
方法は、ジクミルパーオキサイド以外の架橋剤を用いた
架橋ポリエチレンの定量にも同様にして適用することが
できる。Crosslinking agent decomposition residue amount (%) in crosslinked polyethylene The method of the present invention can be similarly applied to the quantitative determination of crosslinked polyethylene using crosslinking agents other than dicumyl peroxide.
（発明の効果）
本発明によれば、
■ガスクロマトグラフの検出器に質量分析装置を使用し
て特定のＭ／Ｚにより成分の検出をしているので、共存
する他成分の妨害を受けずに定量を行なうことができる
、
■内部標準法により測定を行なっているので、精度良く
定量を行なうことができる、
などの効果を奏するため、従来法に比べて一桁以上の高
感度化が達成され、絶縁材料の基本物性研究、品質管理
、押出し条件設定など広範な利用が期待される。(Effects of the Invention) According to the present invention, ■ Since a mass spectrometer is used as a gas chromatograph detector to detect components at a specific M/Z, there is no interference from other coexisting components. Quantitative measurements can be performed with high accuracy because measurements are performed using the internal standard method.As a result, sensitivity is one order of magnitude higher than that of conventional methods. It is expected to be used in a wide range of applications, including research on the basic physical properties of insulating materials, quality control, and setting extrusion conditions.
Claims (1)
、内部標準溶液を加えてガスクロマトグラフ質量分析装
置により各成分に分離し、この内部標準溶液および架橋
剤分解残さに対応する複数の化合物のＭ／Ｚ（Ｚは荷電
を、Ｍは質量を表わす）の各イオン量を測定し、内部標
準溶液に対応する化合物と架橋剤分解残さに対応する化
合物の応答イオン量（ピーク面積またはピーク高さ）の
比を求め、あらかじめ標準溶液を用いて作成した検量線
より各架橋剤分解残さの試料溶液中の濃度を求めること
により、複数の架橋剤分解残さを同時に検出定量するこ
とを特徴とする架橋ポリエチレンの架橋剤分解残さ定量
法。1. Add an internal standard solution to the extract obtained by solvent extraction of cross-linked polyethylene, separate it into each component using a gas chromatograph mass spectrometer, and calculate the M of multiple compounds corresponding to this internal standard solution and cross-linking agent decomposition residue Measure the amount of each ion /Z (Z represents charge, M represents mass), and calculate the response ion amount (peak area or peak height) of the compound corresponding to the internal standard solution and the compound corresponding to the crosslinking agent decomposition residue. A cross-linked polyethylene characterized in that a plurality of cross-linking agent decomposition residues can be detected and quantified simultaneously by determining the concentration of each cross-linking agent decomposition residue in a sample solution from a calibration curve prepared in advance using a standard solution. A method for quantifying crosslinking agent decomposition residue.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11815487A JPS63284463A (en) | 1987-05-15 | 1987-05-15 | Method for determining decomposition residue of crosslinking agent of crosslinked polyethylene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11815487A JPS63284463A (en) | 1987-05-15 | 1987-05-15 | Method for determining decomposition residue of crosslinking agent of crosslinked polyethylene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63284463A true JPS63284463A (en) | 1988-11-21 |
Family
ID=14729432
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11815487A Pending JPS63284463A (en) | 1987-05-15 | 1987-05-15 | Method for determining decomposition residue of crosslinking agent of crosslinked polyethylene |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63284463A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04235345A (en) * | 1991-01-09 | 1992-08-24 | Nec Corp | Method and apparatus for measuring average molecular weight of organic polymer compound |
| JP2017181284A (en) * | 2016-03-30 | 2017-10-05 | 住友ゴム工業株式会社 | Method of quantifying component of rubber composition |
-
1987
- 1987-05-15 JP JP11815487A patent/JPS63284463A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04235345A (en) * | 1991-01-09 | 1992-08-24 | Nec Corp | Method and apparatus for measuring average molecular weight of organic polymer compound |
| JP2017181284A (en) * | 2016-03-30 | 2017-10-05 | 住友ゴム工業株式会社 | Method of quantifying component of rubber composition |
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