JP3567178B2 - Method for preparing oil sample for X-ray fluorescence analysis and method for analyzing oil sample using the same - Google Patents
Method for preparing oil sample for X-ray fluorescence analysis and method for analyzing oil sample using the same Download PDFInfo
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Description
【０００１】
【発明の属する技術分野】
本発明は、油試料に含まれるＣｌを蛍光Ｘ線分析するための油試料の調製法およびそれを用いた油試料の分析方法に関する。
【０００２】
【従来の技術】
ガソリン、灯油、軽油、重油、その他の重質油等の石油製品や、石油製品の原料となる石油半製品（基材油）等の油試料におけるＣｌの含有率については、従来より、蛍光Ｘ線分析、微量電量滴定、電位差滴定、酸水素炎燃焼法などにより、分析を行っている。
【０００３】
【発明が解決しようとする課題】
さて、油に含まれるＣｌのうち、有機系Ｃｌがダイオキシンの原因となるのに対し、無機系Ｃｌがプラントの腐食や製品の品質に関わる等、それらが含まれることによる弊害の内容が異なることや、除去方法が異なることに鑑みれば、油試料に含まれるＣｌを無機系、有機系のタイプ別に分析することには、プロセス管理や品質管理を行う上で大きな意義がある。しかし、前記従来の分析は、いずれも、油試料におけるＣｌ全体の含有率、すなわち、無機系、有機系を問わないトータルＣｌの分析であり、無機系Ｃｌのみ、または、有機系Ｃｌのみを分析することはできなかった。
【０００４】
本発明は前記従来の問題に鑑みてなされたもので、油試料に含まれる無機系Ｃｌ を抽出して蛍光Ｘ線分析するために前記油試料を調製する方法、および、それを用いて油試料におけるＣｌの含有率を無機系、有機系のタイプ別に求める分析方法を提供することを目的とする。
【０００５】
【課題を解決するための手段】
前記目的を達成するために、本願第１の発明は、油試料に含まれる無機系Ｃｌ を抽出して蛍光Ｘ線分析するために前記油試料を調製する方法であって、以下の手順に従う。まず、水または過酸化水素水と前記油試料とを容器に採取し、油試料が重質油の場合には８０℃に加温する。そして、前記油試料中のワックス分と油分とを溶解する溶媒を添加して前記容器内の混合液をエマルジョン状態にすることにより、前記無機系Ｃｌを前記水または過酸化水素水に抽出して水溶液とする。さらに、前記エマルジョン状態の混合液から前記水溶液が分離するのを促進する極性溶媒を添加する。最後に、分離した前記水溶液をろ紙に点滴して乾燥させる。
【０００６】
本願第１の発明によれば、油試料に含まれるＣｌのうち無機系Ｃｌのみを水溶液として抽出、分離して、ろ紙上で乾燥させて濃縮するので、無機系Ｃｌのみについて、真空中で十分な感度での蛍光Ｘ線分析が可能となり、１ｐｐｍ程度の微量分析ができる。
【０００７】
本願第１の発明においては、前記極性溶媒を添加した後、前記混合液に超音波を照射することにより、さらに前記分離を促進することができる。
【０００８】
本願第２の発明は油試料の分析方法であって、前記第１の発明の調製法を用いて蛍光Ｘ線分析により油試料における無機系Ｃｌの含有率を求め、その油試料におけるＣｌ全体の含有率から差し引いて、その油試料における有機系Ｃｌの含有率を求める。
【０００９】
本願第２の発明によれば、前記第１の発明の調製法を用いて蛍光Ｘ線分析により油試料における無機系Ｃｌの含有率を求め、前記従来の分析方法のいずれかにより求めた同じ油試料におけるＣｌ全体の含有率から差し引いて、その油試料における有機系Ｃｌの含有率を求めるので、油試料におけるＣｌの含有率を無機系、有機系のタイプ別に求めることができる。
【００１０】
【発明の実施の形態】
以下、本発明の第１実施形態の方法について、説明する。この方法は、石油製品や石油製品の原料となる石油半製品（基材油）等の油試料に含まれる無機系Ｃｌを抽出して蛍光Ｘ線分析するために前記油試料を調製する方法であって、図１のフローチャートのように以下の手順に従う。まず、水または過酸化水素水と油試料とを容器に採取する。ここでは、あらかじめＮａＯＨで洗浄した１００ｍｌの分液漏斗に、蒸留水５ｍｌを採取し（ステップ１）、その蒸留水の上に浮遊するように油試料５ｇを採取し（ステップ２）、浮遊した油試料の流動性をあげエマルジョン状態になりやすいように、分液漏斗を約８０℃に加温する（ステップ３、特に油試料が重質油である場合に行う）。
【００１１】
なお、油試料に含まれる無機系ＣｌはＮａＣｌとしてであることが多いが、ごくまれに、塩素ガスが含まれる場合がある。その場合には加温により塩素ガスが飛散することが考えられるが、加温が必要となる重質油等には塩素ガスが含まれることはなく、一方、塩素ガスが含まれ得る軽質油等では加温の必要がないので、実際には、無機系Ｃｌの分析において、加温による塩素ガスの飛散が問題となることはない。
【００１２】
そして、油試料中のワックス分と油分とを溶解する溶媒を添加して容器内の混合液をエマルジョン状態にすることにより、無機系Ｃｌを水または過酸化水素水に抽出して水溶液とする。ここでは、トルエン（キシレン等の溶解力の強い溶媒でもよい）５ｍｌを添加して（ステップ４）、３分間、圧抜きをしながら攪拌し、分液漏斗内の混合液をエマルジョン状態にすることにより、無機系Ｃｌを蒸留水に抽出して水溶液とする（ステップ５）。ただし、ワックス分を含まない油試料や軽質油の油試料については、トルエンを添加しなくても蒸留水に抽出することができる。
【００１３】
さらに、エマルジョン状態の混合液から前記水溶液が分離するのを促進する極性溶媒を添加する。ここでは、アセトン（エタノール、イソプロピルアルコール等のアルコール類でもよい）を添加して、軽く攪拌する（ステップ６）。最後に、分離した前記水溶液をろ紙に点滴して乾燥させる。ここでは、１２時間程度静置して、前記水溶液（無機系Ｃｌを抽出した蒸留水）を分離し（ステップ７）、分離した水溶液を５０μｌずつ２回ろ紙（斑点紙、点滴紙）に点滴して乾燥させる（ステップ８）。このろ紙を蛍光Ｘ線分析用の試料とする。
【００１４】
第１実施形態の方法によれば、油試料に含まれるＣｌのうち無機系Ｃｌのみを水溶液として抽出、分離して、ろ紙上で乾燥させて濃縮するので、無機系Ｃｌのみについて、真空中で十分な感度での蛍光Ｘ線分析が可能となり、１ｐｐｍ程度の微量分析ができる。
【００１５】
次に、第２実施形態の方法について説明する。この方法は、前記第１実施形態の方法において、極性溶媒を添加した後、エマルジョン状態の混合液に超音波を照射することにより、さらに前記水溶液（無機系Ｃｌを抽出した蒸留水）の分離を促進する方法である。ここでは、処理をいっそう迅速簡便にするために、油試料および用いる溶媒の量をより少なくして、図２のフローチャートのように以下の手順に従う。まず、あらかじめＮａＯＨで洗浄した１０ｍｌの試験管に、蒸留水２ｍｌを採取し（ステップ１）、その蒸留水の上に浮遊するように油試料１ｇを採取し（ステップ２）、浮遊した油試料の流動性をあげエマルジョン状態になりやすいように、試験管を約８０℃に加温する（ステップ３、特に油試料が重質油である場合に行う）。
【００１６】
そして、トルエン（キシレン等の溶解力の強い溶媒でもよい）２ｍｌを添加して（ステップ４）、３分間、圧抜きをしながら攪拌し、試験管内の混合液をエマルジョン状態にすることにより、無機系Ｃｌを蒸留水に抽出して水溶液とする（ステップ５）。ただし、ワックス分を含まない油試料や軽質油の油試料については、トルエンを添加しなくても蒸留水に抽出することができる。
【００１７】
さらに、アセトン（エタノール、イソプロピルアルコール等のアルコール類でもよい）を添加し、軽く攪拌する（ステップ６）。そして、試験管を超音波洗浄機に入れ約６０度に加温しながら、試験管内の混合液に１時間程度超音波を照射して、前記水溶液（無機系Ｃｌを抽出した蒸留水）を分離し（ステップ７）、分離した水溶液を５０μｌずつ２回ろ紙に点滴して乾燥させる（ステップ８）。このろ紙を蛍光Ｘ線分析用の試料とする。第２実施形態の方法によれば、前記第１実施形態の方法と同様の作用効果がある上に、処理をいっそう迅速簡便にできる。
【００１８】
次に、第３実施形態の方法について、説明する。この方法は、石油製品や石油製品の原料となる石油半製品（基材油）等の油試料の分析方法であって、前記第１または第２実施形態の調製法を用いて蛍光Ｘ線分析により油試料における無機系Ｃｌの含有率を求め、その油試料におけるＣｌ全体の含有率から差し引いて、その油試料における有機系Ｃｌの含有率を求める。
【００１９】
ここでは、まず、前記第１実施形態の調製法を用いて蛍光Ｘ線分析により油試料における無機系Ｃｌの含有率を１ｐｐｍレベルで求める。次に、従来の蛍光Ｘ線分析により、同じ油試料におけるＣｌ全体の含有率を求める。すなわち、油試料を液体試料ホルダに充填し、その試料窓をフィルムで覆ってＨｅ雰囲気で１次Ｘ線を照射して、発生するＣｌの蛍光Ｘ線強度に基づいてＣｌ全体の含有率を求める。この場合にも、１ｐｐｍレベルで求めることができる。そして、Ｃｌ全体の含有率から無機系Ｃｌの含有率を差し引いて、その油試料における有機系Ｃｌの含有率を求める。したがって、有機系Ｃｌの含有率も１ｐｐｍレベルで求められる。
【００２０】
このように、第３実施形態の方法によれば、油試料におけるＣｌの含有率を無機系、有機系のタイプ別に求めることができる。特に、Ｃｌ全体の含有率を従来の蛍光Ｘ線分析で求めれば、タイプ別分析を、迅速簡便に、しかも、１ｐｐｍ程度の微量域で行うことができる。
【００２１】
【発明の効果】
以上詳細に説明したように、本発明の蛍光Ｘ線用の油試料の調製法によれば、油試料に含まれるＣｌのうち無機系Ｃｌのみについて、蛍光Ｘ線分析が可能となり、１ｐｐｍ程度の微量分析ができる。また、本発明の油試料の分析方法によれば、油試料におけるＣｌの含有率を無機系、有機系のタイプ別に求めることができる。
【図面の簡単な説明】
【図１】本発明の第１実施形態の蛍光Ｘ線用の油試料の調製法を示すフローチャートである。
【図２】本発明の第２実施形態の蛍光Ｘ線用の油試料の調製法を示すフローチャートである。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a method for preparing an oil sample for X-ray fluorescence analysis of Cl contained in an oil sample and a method for analyzing an oil sample using the same.
[0002]
[Prior art]
The Cl content in oil samples such as gasoline, kerosene, light oil, heavy oil, and other heavy oils, and semi-finished petroleum (base oil), which is a raw material for petroleum products, has been determined by fluorescence X Analysis is performed by line analysis, microcoulometric titration, potentiometric titration, oxyhydrogen flame combustion method, and the like.
[0003]
[Problems to be solved by the invention]
By the way, among Cl contained in oil, organic Cl causes dioxin, whereas inorganic Cl affects plant corrosion and product quality. In view of the fact that the removal method is different, analyzing Cl contained in an oil sample for each of inorganic and organic types has great significance in performing process control and quality control. However, the conventional analysis is an analysis of the total content of Cl in an oil sample, that is, the analysis of total Cl regardless of whether it is inorganic or organic. Only the inorganic Cl or only the organic Cl is analyzed. I couldn't.
[0004]
The present invention has been made in view of the above-mentioned conventional problems, and a method for extracting an inorganic Cl 2 contained in an oil sample and preparing the oil sample for X-ray fluorescence analysis, and an oil sample using the same. It is an object of the present invention to provide an analysis method for determining the Cl content in each of inorganic and organic types.
[0005]
[Means for Solving the Problems]
In order to achieve the above object, the first invention of the present application is a method for preparing an oil sample for extracting inorganic Cl 2 contained in the oil sample and performing X-ray fluorescence analysis, according to the following procedure. First, water or hydrogen peroxide solution and the oil sample are collected in a container, and when the oil sample is heavy oil, heated to 80 ° C. Then, by adding a solvent that dissolves the wax component and the oil component in the oil sample to bring the mixed solution in the container into an emulsion state, the inorganic Cl is extracted into the water or hydrogen peroxide solution. Make it an aqueous solution. Further, a polar solvent that promotes separation of the aqueous solution from the mixed liquid in the emulsion state is added. Finally, the separated aqueous solution is dropped on a filter paper and dried.
[0006]
According to the first aspect of the present invention, only the inorganic Cl out of the Cl contained in the oil sample is extracted as an aqueous solution, separated, dried on a filter paper and concentrated, so that only the inorganic Cl is sufficient in vacuum. X-ray fluorescence analysis with high sensitivity is possible, and trace analysis of about 1 ppm can be performed.
[0007]
In the first invention of the present application, the separation can be further promoted by irradiating the mixed solution with ultrasonic waves after adding the polar solvent.
[0008]
The second invention of the present application is a method for analyzing an oil sample, wherein the content of inorganic Cl in the oil sample is determined by X-ray fluorescence analysis using the preparation method of the first invention, and the total Cl in the oil sample is determined. Subtract from the content to determine the content of organic Cl in the oil sample.
[0009]
According to the second invention of the present application, the content of inorganic Cl in an oil sample is determined by X-ray fluorescence analysis using the preparation method of the first invention, and the same oil determined by any of the conventional analysis methods is used. Since the content of organic Cl in the oil sample is obtained by subtracting the content of Cl from the entire sample, the content of Cl in the oil sample can be obtained for each of the inorganic and organic types.
[0010]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, the method of the first embodiment of the present invention will be described. This method is a method of extracting an inorganic Cl contained in an oil sample such as a petroleum product or a petroleum semi-finished product (base oil) as a raw material of the petroleum product and preparing the oil sample for X-ray fluorescence analysis. Then, the following procedure is followed as in the flowchart of FIG. First, water or hydrogen peroxide and an oil sample are collected in a container. Here, 5 ml of distilled water was collected in a 100 ml separatory funnel that had been washed with NaOH in advance (step 1), and 5 g of an oil sample was collected so as to float on the distilled water (step 2). The separatory funnel is heated to about 80 ° C. to increase the fluidity of the sample and easily form an emulsion state (Step 3, especially when the oil sample is heavy oil).
[0011]
In addition, the inorganic Cl contained in the oil sample is often NaCl, but may rarely contain chlorine gas. In that case, chlorine gas may be scattered by heating, but heavy oil that needs heating does not contain chlorine gas, while light oil that can contain chlorine gas, etc. Since heating is not necessary, scattering of chlorine gas due to heating does not actually pose a problem in the analysis of inorganic Cl.
[0012]
Then, a solvent that dissolves the wax component and the oil component in the oil sample is added to bring the mixed solution in the container into an emulsion state, whereby inorganic Cl is extracted into water or aqueous hydrogen peroxide to form an aqueous solution. Here, 5 ml of toluene (a solvent having a strong dissolving power such as xylene) may be added (step 4), and the mixture is stirred for 3 minutes while depressurizing to make the mixture in the separating funnel into an emulsion state. The inorganic Cl is extracted into distilled water to obtain an aqueous solution (step 5). However, an oil sample containing no wax or an oil sample of light oil can be extracted into distilled water without adding toluene.
[0013]
Further, a polar solvent that promotes the separation of the aqueous solution from the mixture in an emulsion state is added. Here, acetone (alcohols such as ethanol and isopropyl alcohol) may be added and lightly stirred (step 6). Finally, the separated aqueous solution is dropped on a filter paper and dried. Here, the aqueous solution (distilled water from which inorganic Cl was extracted) was separated by standing for about 12 hours (step 7), and the separated aqueous solution was dropped on filter paper (speckled paper, drip paper) twice in 50 μl portions. And dried (step 8). This filter paper is used as a sample for X-ray fluorescence analysis.
[0014]
According to the method of the first embodiment, of the Cl contained in the oil sample, only the inorganic Cl is extracted as an aqueous solution, separated, dried on a filter paper, and concentrated. X-ray fluorescence analysis with sufficient sensitivity is possible, and a trace analysis of about 1 ppm can be performed.
[0015]
Next, the method of the second embodiment will be described. According to this method, in the method of the first embodiment, after adding a polar solvent, the mixture in an emulsion state is irradiated with ultrasonic waves to further separate the aqueous solution (distilled water from which inorganic Cl is extracted). A way to promote. Here, in order to make the processing more rapid and simple, the amounts of the oil sample and the solvent to be used are reduced, and the following procedure is followed as in the flowchart of FIG. First, 2 ml of distilled water was collected in a 10 ml test tube which had been washed with NaOH in advance (step 1), and 1 g of an oil sample was collected so as to float on the distilled water (step 2). The test tube is heated to about 80 ° C. so as to increase the fluidity and easily become an emulsion state (Step 3, especially when the oil sample is heavy oil).
[0016]
Then, 2 ml of toluene (which may be a solvent having a strong dissolving power such as xylene) is added (step 4), and the mixture is stirred for 3 minutes while depressurizing to bring the mixture in the test tube into an emulsion state. The system Cl is extracted into distilled water to make an aqueous solution (step 5). However, an oil sample containing no wax or an oil sample of light oil can be extracted into distilled water without adding toluene.
[0017]
Further, acetone (alcohols such as ethanol and isopropyl alcohol may be added) is added, and the mixture is gently stirred (step 6). Then, while placing the test tube in an ultrasonic cleaner and heating it to about 60 degrees, the mixture in the test tube is irradiated with ultrasonic waves for about 1 hour to separate the aqueous solution (distilled water from which inorganic Cl was extracted). Then, the separated aqueous solution is dropped on a filter paper twice by 50 μl and dried (step 8). This filter paper is used as a sample for X-ray fluorescence analysis. According to the method of the second embodiment, the same operation and effect as those of the method of the first embodiment can be obtained, and further, the processing can be performed more quickly and simply.
[0018]
Next, a method of the third embodiment will be described. This method is an analysis method for an oil sample such as a petroleum product or a semi-finished petroleum (base oil) which is a raw material of the petroleum product. X-ray fluorescence analysis is performed using the preparation method of the first or second embodiment. , The content of inorganic Cl in the oil sample is obtained, and the content of organic Cl in the oil sample is obtained by subtracting the content of Cl from the whole oil sample.
[0019]
Here, first, the content of inorganic Cl in the oil sample is determined at the 1 ppm level by X-ray fluorescence analysis using the preparation method of the first embodiment. Next, the content of total Cl in the same oil sample is determined by conventional X-ray fluorescence analysis. That is, an oil sample is filled in a liquid sample holder, the sample window is covered with a film, primary X-rays are irradiated in a He atmosphere, and the content of the entire Cl is determined based on the fluorescent X-ray intensity of the generated Cl. . Also in this case, it can be determined at the 1 ppm level. Then, the content of the inorganic Cl is subtracted from the content of the entire Cl to determine the content of the organic Cl in the oil sample. Therefore, the content of organic Cl is also required at the 1 ppm level.
[0020]
As described above, according to the method of the third embodiment, the Cl content in the oil sample can be determined for each of the inorganic and organic types. In particular, if the total content of Cl is determined by conventional X-ray fluorescence analysis, analysis by type can be performed quickly and simply, and in a very small range of about 1 ppm.
[0021]
【The invention's effect】
As described above in detail, according to the method for preparing an oil sample for fluorescent X-rays of the present invention, only the inorganic Cl among the Cl contained in the oil sample can be subjected to fluorescent X-ray analysis. Enables microanalysis. Further, according to the oil sample analysis method of the present invention, the Cl content in the oil sample can be determined for each of the inorganic and organic types.
[Brief description of the drawings]
FIG. 1 is a flowchart showing a method for preparing an oil sample for fluorescent X-rays according to a first embodiment of the present invention.
FIG. 2 is a flowchart showing a method for preparing an oil sample for X-ray fluorescence according to a second embodiment of the present invention.
Claims (4)
水または過酸化水素水と前記油試料とを容器に採取し、
前記油試料中のワックス分と油分とを溶解する溶媒を添加して前記容器内の混合液をエマルジョン状態にすることにより、前記無機系Ｃｌを前記水または過酸化水素水に抽出して水溶液とし、
前記エマルジョン状態の混合液から前記水溶液が分離するのを促進する極性溶媒を添加し、
分離した前記水溶液をろ紙に点滴して乾燥させる蛍光Ｘ線分析用の油試料の調製法。A method for preparing the oil sample for extracting inorganic Cl 2 contained in the oil sample and performing X-ray fluorescence analysis,
Water or hydrogen peroxide solution and the oil sample are collected in a container,
By adding a solvent that dissolves the wax component and the oil component in the oil sample to make the mixed solution in the container an emulsion state, the inorganic Cl is extracted into the water or hydrogen peroxide solution to form an aqueous solution. ,
Adding a polar solvent that promotes separation of the aqueous solution from the mixture in the emulsion state,
A method for preparing an oil sample for X-ray fluorescence analysis, wherein the separated aqueous solution is dropped on filter paper and dried.
前記極性溶媒を添加した後、前記混合液に超音波を照射することにより、さらに前記分離を促進する蛍光Ｘ線分析用の油試料の調製法。In claim 1,
A method for preparing an oil sample for X-ray fluorescence analysis, in which the separation is further promoted by irradiating the mixed solution with ultrasonic waves after adding the polar solvent.
前記油試料が石油製品またはその原料となる石油半製品であり、
前記水が蒸留水であり、
前記容器が分液漏斗または試験管であり、
前記ワックス分と油分とを溶解する溶媒がトルエンまたはキシレンであり、
前記極性溶媒がアセトン、エタノールまたはイソプロピルアルコールである蛍光Ｘ線分析用の油試料の調製法。In claim 1 or 2,
The oil sample is a petroleum product or a semi-finished petroleum that is a raw material thereof,
The water is distilled water,
The container is a separatory funnel or a test tube;
The solvent that dissolves the wax component and the oil component is toluene or xylene,
A method for preparing an oil sample for fluorescent X-ray analysis, wherein the polar solvent is acetone, ethanol or isopropyl alcohol.
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