JPS60169754A - Quantitative analysis of sulfur contained in rubber material - Google Patents
Quantitative analysis of sulfur contained in rubber materialInfo
- Publication number
- JPS60169754A JPS60169754A JP59026770A JP2677084A JPS60169754A JP S60169754 A JPS60169754 A JP S60169754A JP 59026770 A JP59026770 A JP 59026770A JP 2677084 A JP2677084 A JP 2677084A JP S60169754 A JPS60169754 A JP S60169754A
- Authority
- JP
- Japan
- Prior art keywords
- sulfur
- rubber material
- specimen
- solution
- tube type
- 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
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 40
- 239000011593 sulfur Substances 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title abstract description 14
- 238000004445 quantitative analysis Methods 0.000 title description 2
- 238000000034 method Methods 0.000 claims abstract description 15
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical group [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 13
- 238000001649 capillary isotachophoresis Methods 0.000 claims description 6
- 239000003082 abrasive agent Substances 0.000 claims 1
- 239000000567 combustion gas Substances 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 description 6
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 3
- 229910001626 barium chloride Inorganic materials 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000011088 calibration curve Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000002218 isotachophoresis Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/44—Resins; Plastics; Rubber; Leather
- G01N33/445—Rubber
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Combustion & Propulsion (AREA)
- Molecular Biology (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は、ゴム材料に含まれる硫黄の定量分析方法に関
し、更に詳しくは、ゴム材料、特にゴム絶縁材料に含ま
れるごく微量の硫黄を短時間で精度よく定量分析する方
法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for quantitatively analyzing sulfur contained in rubber materials, and more specifically, for quantitatively analyzing extremely small amounts of sulfur contained in rubber materials, particularly rubber insulating materials, in a short time and with high precision. Regarding the method.
従来、ゴム材料に含まれる硫黄の定量分析は、材料を酸
素加圧下のポンプ内で燃焼させ、燃焼ガスを吸収液に吸
収させ、塩化バリウム溶液を添加し、生じる硫酸バリウ
ム沈殿を枦取して高温で焼き秤量することによって行な
われていた。しｈ化、この方法では、ポンプ内で燃焼さ
せる時の材料燃焼量に制限があるので、定量下限が高（
な１）、微量の硫黄分の定量は不可能である。また、塩
化バリウムを添加してからの硫酸バリウム沈殿熟成のた
め一昼夜放置し、更に沈殿枦取後高温で焼くので、長時
間を要する。更に、この方法では、操作にかなりの技量
を必要とするので、測定誤差が大鰺い。Conventionally, quantitative analysis of sulfur contained in rubber materials has been carried out by burning the material in a pump under pressurized oxygen, absorbing the combustion gas into an absorption liquid, adding barium chloride solution, and removing the resulting barium sulfate precipitate. This was done by baking and weighing at high temperatures. In this method, there is a limit to the amount of material burned when burning in the pump, so the lower limit of quantification is high (
1) It is impossible to quantify trace amounts of sulfur. In addition, it takes a long time because barium chloride is added, barium sulfate is precipitated, and the product is allowed to stand for a day and night, and after the precipitate is removed, it is baked at a high temperature. Furthermore, this method requires a considerable amount of skill to operate, so measurement errors are large.
本発明者らは、細管式等速電気泳動分析装置を用いると
、微量の硫黄を精度よく短時間で定量で鰺ることを見い
出し、本発明を完成するに至った。The present inventors have discovered that by using a capillary type isotachophoresis analyzer, trace amounts of sulfur can be quantified with high accuracy and in a short time, and have completed the present invention.
本発明の要旨は、細管式等速電気泳動分析方法装置によ
ってゴム材料に含まれる全硫黄または遊離硫黄を定量分
析する方法に存する。The gist of the present invention resides in a method for quantitatively analyzing total sulfur or free sulfur contained in a rubber material using a capillary isotachophoresis analysis method device.
本発明の方法の手順を説明する。（１）試料から遊離さ
れた硫黄（例えば、燃焼ガスの形で）を吸収液（例えば
、Ｈ２Ｏ２水溶液、Ｂｒ２水）に吸収させ、硫黄を硫酸
イオンにする。（２）マイクロシリンジによって硫酸イ
オンを含む吸収液を細管式等速電気泳動分析装置へ注入
し、硫酸イオンを定量し、試料中の硫黄含量をめる。The procedure of the method of the present invention will be explained. (1) Sulfur liberated from the sample (eg, in the form of combustion gas) is absorbed into an absorption liquid (eg, H2O2 aqueous solution, Br2 water) to convert sulfur to sulfate ions. (2) Inject the absorption liquid containing sulfate ions into a capillary isotachophoresis analyzer using a microsyringe, quantify the sulfate ions, and calculate the sulfur content in the sample.
本発明の方法の特長は、少量の試料で非常に精度よく定
量で外、分析所要時間も非常に短いことである。加えて
、操作にはあまり技量を要さないので、特に沈でんのが
取、秤量の必要がないので測定誤差は非常に小さい。The feature of the method of the present invention is that it can be quantitatively determined with very high accuracy using a small amount of sample, and the time required for analysis is also very short. In addition, the operation does not require much skill, and there is no need to take or weigh the sediment, so the measurement error is very small.
第１図に、硫黄標準液の検量線を示すが、（）、１μｇ
までの硫黄を測定でとる。Figure 1 shows the calibration curve of the sulfur standard solution, (), 1 μg
Measure the amount of sulfur up to.
ゴム材料に合皮れる硫黄には、全硫黄と遊離硫黄があり
、本発明の方法をこの両方に適用する場合の手順を説明
する。There are two types of sulfur that can be applied to rubber materials: total sulfur and free sulfur, and the procedure for applying the method of the present invention to both types will be explained.
１）全硫黄の定量
粉末化したゴム材料約３０ｍ８を、酸素封入した燃焼用
フラスコ内で燃焼させ、燃焼ガスを１１２０２水溶液（
例えば０．５重量％水溶液２０ｍ１）に吸収させ、硫酸
イオンとする。硫酸イオンを含む吸収液をマイクロシリ
ンジによって細管式等速電気泳動分析装置に注入する。1) Determination of total sulfur Approximately 30m8 of powdered rubber material is burned in a combustion flask filled with oxygen, and the combustion gas is converted into an aqueous solution of 11202 (
For example, it is absorbed into 20 ml of a 0.5% aqueous solution to form sulfate ions. An absorption liquid containing sulfate ions is injected into a capillary isotachophoresis analyzer using a microsyringe.
検出ピーク開のゾーン長さから硫酸イオン量を定量し、
試料中の全硫黄量を算出する。試料３０ＩＩ１ｇで１０
−２重量％のオーダーまで正確に測定できる。分析所要
時間は約３０２）遊離硫黄の定量
粉末化したゴム材料をア七トンで還流下８時間抽出する
。抽出液中の硫黄をＢｒ２水によって硫酸イオンに酸化
し、以下１）全硫黄の場合と同様な繰作を行ない、細管
式等速電気泳動分析装置によって測定する。Quantify the amount of sulfate ions from the length of the open detection peak zone,
Calculate the total amount of sulfur in the sample. 10 for 1g of sample 30II
- Can be accurately measured down to the order of 2% by weight. The time required for the analysis is approximately 302) Determination of free sulfur The powdered rubber material is extracted under reflux with A7T for 8 hours. The sulfur in the extract is oxidized to sulfate ions with Br2 water, and the same procedure as in the case of 1) total sulfur is performed, followed by measurement using a capillary isotachophoresis analyzer.
本発明の方法は、ゴム材料、特にゴム絶縁材料の硫黄含
量を定量するのに有用であるが、ゴム材料以外でのＶ＆
量の硫黄の定量にも適用可能である。Although the method of the present invention is useful for quantifying the sulfur content of rubber materials, especially rubber insulation materials,
It is also applicable to the determination of the amount of sulfur.
以下に実施例および比較例を示し、本発明を更に詳しく
説明する。EXAMPLES The present invention will be explained in more detail by showing Examples and Comparative Examples below.
実施例
全硫黄量が既知であるゴム材料を粉末化した試料３２．
６３ｍｇを酸素封入した燃焼用フラスコ内で燃焼させた
。燃焼ガスを０．５％Ｈ２Ｏ２水溶液２０ｍｊ２ に吸
収させ、この硫酸イオンを含む吸収液７０μ夕をマイク
ロシリンジによって細管式等速電気泳動分析装置に注入
した。検出ピーク間のゾーン長さから硫酸イオン量を定
量し、試料中の全硫黄量を算出すると、全硫黄量０．１
１０ 重量％であった。測定所要時間は約３０分間であ
った。Example Sample 32, which is a powdered rubber material with a known total sulfur content.
63 mg was combusted in a combustion flask filled with oxygen. The combustion gas was absorbed into 20 mj2 of a 0.5% H2O2 aqueous solution, and 70 μm of this absorption liquid containing sulfate ions was injected into a capillary isotachophoresis analyzer using a microsyringe. When the amount of sulfate ions is determined from the zone length between the detected peaks and the total amount of sulfur in the sample is calculated, the total amount of sulfur is 0.1.
It was 10% by weight. The time required for the measurement was approximately 30 minutes.
比較例
実施例と同じ試料５００．０■を酸素加圧下のポンプ内
で燃焼させた。燃焼ガスを吸収液に吸収させてから塩化
バリウム水溶液を加えるとすぐに沈殿が生じたが、−昼
夜放置した。この硫酸バリウムの沈殿を枦取し、高温で
焼き重量を測定し、全硫黄量を算出すると ０．１０７
重量％であった。Comparative Example 500.0 cm of the same sample as in the example was burned in a pump under pressurized oxygen. When the barium chloride aqueous solution was added after the combustion gas was absorbed into the absorption liquid, precipitation occurred immediately, but the mixture was allowed to stand day and night. The barium sulfate precipitate was collected, the weight was measured at high temperature, and the total sulfur content was calculated as 0.107.
% by weight.
上記の操作にはたいへんな技量を要した。また測定には
、まる２日を要した。The above operations required great skill. Furthermore, the measurement took two full days.
第１図は、硫ｆｉｔ’標準液の検量線を示す。 特許出願人 住友電気工業株式会社 代 理 人 弁理士 前出 葆 （外２名）第１図 挑寅會 （ＩＡＩ） FIG. 1 shows the calibration curve of the sulfur fit' standard solution. Patent applicant: Sumitomo Electric Industries, Ltd. Representative Patent Attorney (explained above) (2 others) Figure 1 Challenger Association (IAI)
Claims (1)
まれる全硫黄または遊離硫黄を定量分析する方法。 ２、硫黄を酸化して硫酸イオンにした後定量分析する特
許請求の範囲第１項に記載の方法。[Claims] 1. A method for quantitatively analyzing total sulfur or free sulfur contained in rubber abrasive material using a capillary isotachophoresis analyzer. 2. The method according to claim 1, wherein sulfur is oxidized to sulfate ions and then quantitatively analyzed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59026770A JPS60169754A (en) | 1984-02-14 | 1984-02-14 | Quantitative analysis of sulfur contained in rubber material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59026770A JPS60169754A (en) | 1984-02-14 | 1984-02-14 | Quantitative analysis of sulfur contained in rubber material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS60169754A true JPS60169754A (en) | 1985-09-03 |
Family
ID=12202524
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59026770A Pending JPS60169754A (en) | 1984-02-14 | 1984-02-14 | Quantitative analysis of sulfur contained in rubber material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60169754A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH021689A (en) * | 1988-06-10 | 1990-01-05 | Fuji Photo Film Co Ltd | Microfilm retrieving/reading device |
| JPH021688A (en) * | 1988-06-10 | 1990-01-05 | Fuji Photo Film Co Ltd | Microfilm retrieving/reading device |
-
1984
- 1984-02-14 JP JP59026770A patent/JPS60169754A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH021689A (en) * | 1988-06-10 | 1990-01-05 | Fuji Photo Film Co Ltd | Microfilm retrieving/reading device |
| JPH021688A (en) * | 1988-06-10 | 1990-01-05 | Fuji Photo Film Co Ltd | Microfilm retrieving/reading device |
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