JPS5930049A - Quick analysis of density of antiaging agent in polyethylene - Google Patents
Quick analysis of density of antiaging agent in polyethyleneInfo
- Publication number
- JPS5930049A JPS5930049A JP14128582A JP14128582A JPS5930049A JP S5930049 A JPS5930049 A JP S5930049A JP 14128582 A JP14128582 A JP 14128582A JP 14128582 A JP14128582 A JP 14128582A JP S5930049 A JPS5930049 A JP S5930049A
- Authority
- JP
- Japan
- Prior art keywords
- polyethylene
- fluorescent
- ray
- concentration
- density
- 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
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
Description
【発明の詳細な説明】
この発明はポリエチレン中に含有する老化防止剤の濃度
を迅速にかつ高精度に分析する方法に関するものである
。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for rapidly and highly accurately analyzing the concentration of antiaging agents contained in polyethylene.
従来、ポリエチレン中に含有する老化防止剤の濃度測定
は示差走査熱量計を用いて行なわれている０
しかしながらこの測定法は、化学反応を利用するもので
あるため、１回の測定に長い時間（約６０Ａ分／回）を
要すること、精度が悪いこと、試料を完全に破壊してし
まうので同一試料の再測定ができないこと、反応状況を
把握しなければならないので技術を要すること、などの
難点があり、多数の製品における泡化防止剤の配合量の
良否判定の工業的手段として適しているとは云い難い。Conventionally, the concentration of anti-aging agents contained in polyethylene has been measured using a differential scanning calorimeter. However, since this measurement method uses a chemical reaction, it takes a long time ( Disadvantages include: (approximately 60A min/time), poor accuracy, complete destruction of the sample, making it impossible to remeasure the same sample, and the need to understand the reaction status, which requires skill. Therefore, it is difficult to say that it is suitable as an industrial means for determining the quality of the amount of anti-foaming agent in many products.
そこで本発明者は、よυ迅速にかつ高精度の状態で老化
防止剤の配合組成を知ってポリエチレンの品質管理を行
える工業的な老化防止剤の濃度分析法について種々検討
の結果、この発明に至っだ即ち、この発明はポリエチレ
ン中に含有する４、４′−チオビス−（６−ターシャリ
−ブチル−３−メチルフェノール）、ジラウリル−チオ
−ジ−プロピオネート、メルカプトベンズイミダゾール
等の硫黄Ｓを含む老化防止剤の濃度測定に当って、老化
防止剤中の硫黄Ｓに着目し、Ｃｒ’Ｑ球より放射される
一次Ｘ線をポリエチレンに照射し、そのとき発生する螢
光Ｘ線（ＳのにαＭ）強度を計測し、この計測値から標
準試料の螢光Ｘ線強度測定により求めた検量線をもとに
老化防止剤の濃度を算出せんとするものである。Therefore, the present inventor has conducted various studies on an industrial method for analyzing the concentration of anti-aging agents that can quickly and accurately control the quality of polyethylene by knowing the blending composition of anti-aging agents, and has developed the present invention. That is, this invention is directed to the aging of polyethylene containing sulfur S, such as 4,4'-thiobis-(6-tert-butyl-3-methylphenol), dilauryl-thio-di-propionate, and mercaptobenzimidazole. When measuring the concentration of the inhibitor, we focused on the sulfur S in the antioxidant and irradiated polyethylene with the primary X-rays emitted from the Cr'Q bulb. ) The intensity is measured, and the concentration of the anti-aging agent is calculated from the measured value based on a calibration curve obtained by measuring the fluorescent X-ray intensity of a standard sample.
ここで標準試料としては老化防止剤を含有しないポリエ
チレンおよび１種以上の既知濃度の老化防止剤を含有す
るポリエチレンを用いるものである。Here, as standard samples, polyethylene containing no anti-aging agent and polyethylene containing one or more anti-aging agents at a known concentration are used.
実用ポリエチレン中の老化防止剤含有量は５％以下であ
るが、これが１０％以下の場合でも螢光ＸＩ？ＩＩＪ測
定で得られる検量線は非常に直線性がよくさらにＸｍ強
度のバラツキも非常に小さく、高精度の分析が行えるこ
とがわかった。The content of anti-aging agent in practical polyethylene is 5% or less, but even if it is 10% or less, Fluorescent XI? It was found that the calibration curve obtained by IIJ measurement had very good linearity, and the variation in Xm intensity was also very small, making it possible to perform highly accurate analysis.
測定Ｘ蝉は硫黄Ｇ）のＫＣｌ線（螢光Ｘ稼）でＸ線管球
の加速電圧は２０〜４０ＫＶ、 電流値は３０〜６０
ｍＡ。The X cicada was measured using a sulfur G) KCl ray (fluorescence
mA.
Ｘ線検出型はｌｉ’Ｐｃ （ＦＩ！ｏｗ Ｐｒｏｐｏｒ
ｔｉｏｎａｅＣｏｕｎｔｅｒ）とし、検量線作成用標準
試料の老化防止剤濃度範囲は０〜ｌＯチである。The X-ray detection type is li'Pc (FI!ow Propor
The antioxidant concentration range of the standard sample for creating a calibration curve is 0 to 10.
このようにこの発明においては、ポリエチレン中の老化
防止剤の農産をＳの螢光Ｘ線強度を測定することによシ
、その計数値と標準試料の検量線により求めるものであ
り、
（１）螢光Ｘ ′ＩＪ’Ａ放出現象は熱化学反応と比べ
て極めて高速であるからホリ定も非常に迅速に行える。In this way, in this invention, the agricultural production of the anti-aging agent in polyethylene is determined by measuring the fluorescent X-ray intensity of S, and using the counted value and the calibration curve of the standard sample, (1) Since the fluorescence X'IJ'A emission phenomenon is extremely rapid compared to thermochemical reactions, the Holi determination can also be performed extremely quickly.
（例えばｌ試料の測定時間は１５＋程度である）（２）
デジタル計致であるので高精度の測定１直が得られる。(For example, the measurement time for 1 sample is about 15+) (2)
Since it is a digital measurement, highly accurate measurement can be obtained in one shift.
（３）非破壊測定であるから再測定が可能である。(3) Since it is a non-destructive measurement, re-measurement is possible.
などの利点を有するのである。It has the following advantages.
しかしてこの分析方法は、ポリエチレン中に含有される
Ｏ〜１０襲の老化防止剤の品質管理分析、配合良丙判定
などに何月である。However, this analytical method is useful for quality control analysis, formulation quality determination, etc. of O-10 anti-aging agents contained in polyethylene.
なお老化防止剤を含有せるポリエチレンの測定試料厚さ
がＱ、３ｍ以下の場合は、厚さを揃える必要があるが、
０．３朗以上の場合はその必要７５；ない０螢光Ｘ線（
Ｓのにα線）の強度計数にはＦＰＣが用いられるが、こ
のほか半導体検出器でも差支え・ない０
添付図面は老化防止剤として４．４′−チオ−ビス（６
−ターシャリ−ブチル−３−メチルフェノール）を含有
するポリエチレン標準試料を用いて
Ｃｒ管球 ３０ＫＶ、 ６０ｍＡ計
算管 ＦＰＣ
分光結晶 ＰＥＴ
螢光Ｘ線測定 ７５゜８０
バックグランド測定 ７４゜００
マスク Ａｊ３０ｗｍφ
にて測定してＳＫα線強度の１０秒間の計数値を測定し
て得られたポリエチレン中のＳ濃度（第１図）およびポ
リエチレン中の老化防止剤の濃度（第２図）に対する検
量線を示すものである０In addition, if the thickness of the measured sample of polyethylene containing anti-aging agent is Q, 3m or less, it is necessary to make the thickness the same.
If it is 0.3 ro or more, it is necessary 75; no 0 fluorescent X-ray (
An FPC is used to count the intensity of S and alpha rays, but a semiconductor detector may also be used.
-Tertiary-butyl-3-methylphenol) using a Cr tube 30KV, 60mA calculation tube FPC spectroscopic crystal PET Fluorescent X-ray measurement 75°80 Background measurement 74°00 Mask Aj30wmφ This figure shows a calibration curve for the S concentration in polyethylene (Figure 1) and the concentration of anti-aging agent in polyethylene (Figure 2) obtained by measuring the count value of the SKα ray intensity for 10 seconds. 0
第１図は老化防止剤を含有しないポリエチレンおよび老
化防止剤を含有したポリエチレン標準試料によるポリエ
チレン中のＳ濃度に対する検量線、第２図は同じく老化
防止剤の濃度に対する検量線である。
特許出願人 住友電気工業株式会
社代 埋入 弁理士和１）昭
第１図
第２図
手 続 補 正 書（自発）
昭和５７年 ９月２４日
特許庁長官 殿
１、事件の表示
昭和５７年特許願第１４１２８５号
２、発明の名称
ポリエチレン中の老化防止剤１度の迅速分析法３、補正
をする者
事件との関係 特許出願人
４、代理人
住 所 大阪市大淀区中津１丁目１８番１８号特許
請求の範囲
（１） ポリエチレン中に含有する老化防止剤の濃度
の分析法であって、老化防止剤を含有するポリエチレン
に一次Ｘ線を照射した時に発生する螢光Ｘ線強度を計数
し、この計算値と、予め老化防止剤を含有しないあるい
は既知濃度の老化防止剤を含有するポリエチレンの螢光
Ｘ線測定にて求めた検量線により老化防止剤の濃度を締
出することを特徴とするポリエチレン中の老化防止剤濃
度の迅速分析法。
（２） −次Ｘ線源としてＣｒ管球を用いることを特
徴とする特許請求の範囲７１ 記 のポリエチレン中の
老化防止剤濃度の迅速分析法。
ｆ３） Ｃｒ管球の加速電圧が２０〜４０Ｋｖ、電流
値が３０〜６０−であることを特徴とする特許 求の範
１項記載のポリエチレン中の老化防止剤濃度の迅速分析
法。
手続補正書
昭和５８年４ 月１２日
事件との関係 特許出願人
Ｍ′′１銘称） （２１３）住友電気工業株式会社４
、代理人
８、補正の内容FIG. 1 shows a calibration curve for the S concentration in polyethylene using standard samples of polyethylene without an antiaging agent and polyethylene containing an antiaging agent, and FIG. 2 shows a calibration curve for the concentration of an antiaging agent. Patent applicant Sumitomo Electric Industries Co., Ltd. Patent attorney Kazu 1) Amendment to the procedures in Figure 1 and Figure 2 of the Showa era (spontaneous) September 24, 1980 Commissioner of the Japan Patent Office 1. Indication of the case 1988 Patent Application No. 141285 2, Name of the invention: Method for rapid analysis of anti-aging agents in polyethylene 3, Relationship with the person making the amendment Patent applicant 4, Agent address: 1-18 Nakatsu, Oyodo-ku, Osaka City Claims (1) of Patent No. 18: A method for analyzing the concentration of anti-aging agent contained in polyethylene, which involves counting the intensity of fluorescent X-rays generated when polyethylene containing the anti-aging agent is irradiated with primary X-rays. However, the concentration of the anti-aging agent is determined based on this calculated value and a calibration curve previously determined by fluorescent X-ray measurement of polyethylene that does not contain an anti-aging agent or contains a known concentration of an anti-aging agent. A rapid analysis method for the concentration of antiaging agents in polyethylene. (2) The rapid analysis method for the concentration of anti-aging agent in polyethylene according to claim 71, characterized in that a Cr tube is used as the -order X-ray source. f3) A rapid analysis method for the concentration of an anti-aging agent in polyethylene according to claim 1, characterized in that the accelerating voltage of the Cr tube is 20 to 40 Kv and the current value is 30 to 60 -. Procedural Amendment Relation to the April 12, 1980 Incident Patent applicant M''1 name) (213) Sumitomo Electric Industries, Ltd. 4
, Agent 8, Contents of amendment
Claims (3)
析法であって、老化防止剤を含有するポリエチレンに一
次Ｘ線を照射した時に発生する螢光Ｘ線強度を計数し、
この計算値と、予め老化防止剤を含有しないあるいは既
知濃度の老化防止剤を含 勉−有するポリエチレンの螢
光Ｘ線測定にて求めた検量線によシ老化防止剤の濃度を
算出する。ことを特徴とするポリエチレン中の老化防止
剤濃度の迅速分析法。(1) A method for analyzing the concentration of anti-aging agent contained in polyethylene, in which the intensity of fluorescent X-rays generated when polyethylene containing anti-aging agent is irradiated with primary X-rays is counted,
The concentration of the anti-aging agent is calculated from this calculated value and a calibration curve previously determined by fluorescent X-ray measurement of polyethylene that does not contain an anti-aging agent or contains a known concentration of an anti-aging agent. A rapid analysis method for the concentration of anti-aging agents in polyethylene, characterized by:
するポリエチレン中の老化防止剤濃度の迅速分析法。(2) A rapid analysis method for the concentration of anti-aging agents in polyethylene, characterized in that a Cr tube is used as a -order X-ray source.
が３０〜６０ｍＡであることを特徴とするポリエチレン(3) Polyethylene characterized by the acceleration voltage of the Cr tube being 20 to 40 KV and the current value being 30 to 60 mA.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14128582A JPS5930049A (en) | 1982-08-13 | 1982-08-13 | Quick analysis of density of antiaging agent in polyethylene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14128582A JPS5930049A (en) | 1982-08-13 | 1982-08-13 | Quick analysis of density of antiaging agent in polyethylene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS5930049A true JPS5930049A (en) | 1984-02-17 |
Family
ID=15288331
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14128582A Pending JPS5930049A (en) | 1982-08-13 | 1982-08-13 | Quick analysis of density of antiaging agent in polyethylene |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5930049A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61247961A (en) * | 1985-04-25 | 1986-11-05 | Shin Kobe Electric Mach Co Ltd | Method for measuring mixing ratio of low-density polyethylene and high-density polyethylene |
| JPS63271147A (en) * | 1987-04-28 | 1988-11-09 | Shimadzu Corp | Analysis by fundamental parameter method |
| JPH04110454U (en) * | 1991-01-31 | 1992-09-25 | 荏原商事株式会社 | Greenhouse heating system |
| CN108084568A (en) * | 2018-01-16 | 2018-05-29 | 东莞出入境检验检疫局检验检疫综合技术中心 | RoHS detection xrf analysis quickly screens analytical standard sample and preparation method with Qian, Ge ﹑ Ge ﹑ mercury and bromine in PP |
-
1982
- 1982-08-13 JP JP14128582A patent/JPS5930049A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61247961A (en) * | 1985-04-25 | 1986-11-05 | Shin Kobe Electric Mach Co Ltd | Method for measuring mixing ratio of low-density polyethylene and high-density polyethylene |
| JPS63271147A (en) * | 1987-04-28 | 1988-11-09 | Shimadzu Corp | Analysis by fundamental parameter method |
| JPH04110454U (en) * | 1991-01-31 | 1992-09-25 | 荏原商事株式会社 | Greenhouse heating system |
| CN108084568A (en) * | 2018-01-16 | 2018-05-29 | 东莞出入境检验检疫局检验检疫综合技术中心 | RoHS detection xrf analysis quickly screens analytical standard sample and preparation method with Qian, Ge ﹑ Ge ﹑ mercury and bromine in PP |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Johansson et al. | Elemental trace analysis of small samples by proton induced X-ray emission | |
| EP2185921B1 (en) | Differentiation of lead in surface layers and in bulk samples by x-ray fluorescence | |
| Yao et al. | Element analysis based on energy-dispersive X-ray fluorescence | |
| JP2008268076A (en) | Non-destructive discrimination method, and device | |
| JPWO2007122770A1 (en) | Three-dimensional quantitative method using transmitted X-ray | |
| JP4725350B2 (en) | Transmission X-ray measurement method | |
| JPH03505251A (en) | Methods for measuring thickness and composition of films on substrates | |
| JPH02228515A (en) | Measurement of thickness of coating | |
| JP2014190922A (en) | Foreign substance detection apparatus | |
| JPH0541940B2 (en) | ||
| JPS5930049A (en) | Quick analysis of density of antiaging agent in polyethylene | |
| Glinsman | The practical application of air-path X-ray fluorescence spectrometry in the analysis of museum objects | |
| JP2019109201A (en) | Fluorescent x-ray analysis device and analysis method | |
| JP2017020924A (en) | Resin discrimination device and resin discrimination method | |
| JPH01214748A (en) | Method and apparatus for fluorescent x-ray analysis for minute amount of sample liquid | |
| Milota et al. | PIXE measurements of Renaissance silverpoint drawings at VERA | |
| Nakano et al. | Preparation of standard materials of aerosol particles for X‐ray fluorescence analysis using a small chamber sampling unit | |
| JP2939169B2 (en) | Measuring method for size of optical focus of radioactive ray generating tube | |
| JP4607565B2 (en) | Analysis method and apparatus | |
| JPS6170444A (en) | Concentration analyzing method in electron ray micro-analysis instrument | |
| JP2023156889A (en) | Fluorescent X-ray analyzer | |
| JPH0229983B2 (en) | ||
| USH922H (en) | Method for analyzing materials using x-ray fluorescence | |
| JP3234716B2 (en) | Area measurement method used for X-ray analysis | |
| JP2645227B2 (en) | X-ray fluorescence analysis method |