JP2002286596A - Preparation method of preparing oil sample for fluorescent x-ray analysis, and analytical method of analyzing oil sample using the same - Google Patents
Preparation method of preparing oil sample for fluorescent x-ray analysis, and analytical method of analyzing oil sample using the sameInfo
- Publication number
- JP2002286596A JP2002286596A JP2001087741A JP2001087741A JP2002286596A JP 2002286596 A JP2002286596 A JP 2002286596A JP 2001087741 A JP2001087741 A JP 2001087741A JP 2001087741 A JP2001087741 A JP 2001087741A JP 2002286596 A JP2002286596 A JP 2002286596A
- Authority
- JP
- Japan
- Prior art keywords
- oil sample
- oil
- inorganic
- analysis
- content
- 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
Landscapes
- Analysing Materials By The Use Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Description
【０００１】[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。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】[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。2. Description of the Related Art The content of Cl in petroleum products such as gasoline, kerosene, light oil, heavy oil, and other heavy oils, and oil samples such as semi-finished petroleum (base oil) used as a raw material of petroleum products is as follows. Conventionally, analysis has been performed by X-ray fluorescence analysis, microcoulometric titration, potentiometric titration, oxyhydrogen flame combustion method, and the like.
【０００３】[0003]
【発明が解決しようとする課題】さて、油に含まれるＣ
l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。Now, C contained in the oil will be described.
Among them, organic Cl causes dioxin, whereas inorganic Cl affects plant corrosion and product quality. In view of this, analyzing Cl contained in an oil sample by inorganic or organic type has great significance in performing process control and quality control. However, the conventional analysis described above 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. I couldn't.
【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。[0004] The present invention has been made in view of the above-mentioned conventional problems, and extracts inorganic Cl contained in an oil sample to obtain a fluorescent X-ray.
A method of preparing the oil sample for X-ray analysis, and
It is an object of the present invention to provide an analytical method for determining the Cl content in an oil sample by inorganic and organic types using the same.
【０００５】[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。In order to achieve the above object, a first invention of the present application is a method for preparing an oil sample for extracting inorganic Cl contained in the oil sample and performing X-ray fluorescence analysis. And follow the procedure below. First, water or a 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 water. 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】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。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 vacuumed. X-ray fluorescence analysis with sufficient sensitivity is possible, and a trace analysis of about 1 ppm can be performed.
【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。In the first aspect of the present invention, the separation can be further promoted by irradiating the mixed solution with ultrasonic waves after adding the polar solvent.
【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。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 content of the inorganic Cl in the oil sample is determined. The content of organic Cl in the oil sample is determined by subtracting from the content of Cl as a whole.
【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。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 content is determined by any of the conventional analysis methods. Then, the content of organic Cl in the oil sample is determined by subtracting the content of Cl from the whole oil sample in the same oil sample.
It can be determined by organic type.
【００１０】[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５
ｍｌ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）。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, a method according to a 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 a hydrogen peroxide solution and an oil sample are collected in a container. Here, distilled water 5 was placed in a 100 ml separatory funnel that had been washed with NaOH in advance.
5 ml of an oil sample (Step 2) so as to float on the distilled water (Step 2), and a separating funnel so as to increase the fluidity of the suspended oil sample and easily form an emulsion state. To about 80 ° C. (Step 3, especially when the oil sample is heavy oil).
【００１１】なお、油試料に含まれる無機系ＣlはＮaＣ
l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。The inorganic Cl contained in the oil sample is NaC
It is often as l, but very rarely contains chlorine gas. In that case, chlorine gas may be scattered by heating, but heavy oils that need to be heated do not contain chlorine gas, while light oils that can contain chlorine gas In this case, there is no need for heating, and in practice, scattering of chlorine gas due to heating does not pose a problem in the analysis of inorganic Cl.
【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。Then, a solvent dissolving the wax component and the oil component in the oil sample is added to make the mixed solution in the container into an emulsion state, whereby the inorganic Cl is extracted into water or hydrogen peroxide solution, and the aqueous solution is extracted. And 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,
The mixed liquid in the separating funnel is made into an emulsion state, whereby 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】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。Further, a polar solvent which promotes separation of the aqueous solution from the mixed liquid in an emulsion state is added.
Here, acetone (alcohols such as ethanol and isopropyl alcohol may be added) is 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 allowing to stand for about 12 hours (step 7), and the separated aqueous solution was separated by 50 μl for 2 hours.
The filter paper (droplet paper, drip paper) is drip-dried and dried (step 8). This filter paper is used as a sample for X-ray fluorescence analysis.
【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。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 filter paper and concentrated.
Only for X-ray fluorescence X-ray analysis with sufficient sensitivity in vacuum, a trace analysis of about 1 ppm can be performed.
【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Ｃ
l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）。Next, the method of the second embodiment will be described. This method is the same as the method of the first embodiment, except that after adding a polar solvent, the mixed solution in an emulsion state is irradiated with ultrasonic waves to further add the aqueous solution (inorganic C
This is a method for promoting the separation of distilled water from which l has been extracted. Here, in order to make the processing quicker and simpler, 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 placed in a 10 ml test tube previously washed with NaOH.
(Step 1), and 1 g of an oil sample is collected so as to float on the distilled water (Step 2). Heat to 80 ° C. (Step 3, especially if the oil sample is heavy oil).
【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。Then, 2 ml of toluene (a solvent having a strong dissolving power such as xylene) may be added (step 4),
The mixture is stirred for 3 minutes while depressurizing, and the mixture in the test tube is made into an emulsion state, whereby inorganic Cl is extracted into distilled water to form 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】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。Further, acetone (alcohols such as ethanol and isopropyl alcohol may be added) is added,
Stir lightly (step 6). Then, while placing the test tube in an ultrasonic cleaner and heating it to about 60 ° C., 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 effects as those of the method of the first embodiment can be obtained, and further, the processing can be performed more quickly and simply.
【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。Next, the 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) used as 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 determined, and the content of organic Cl in the oil sample is determined by subtracting the content of Cl from the entire oil sample.
【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Ｃ
l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。Here, first, the inorganic C in the oil sample was analyzed by X-ray fluorescence analysis using the preparation method of the first embodiment.
The l content is determined at the 1 ppm level. Next, the content of the entire 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, and the primary X
Irradiation is performed to determine the content of Cl as a whole based on the intensity of the fluorescent X-rays of Cl generated. 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】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。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 content of Cl as a whole 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】[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。As described above in detail, according to the method for preparing an oil sample for fluorescent X-rays of the present invention, fluorescent X-ray analysis can be performed only on inorganic Cl among Cl contained in the oil sample. Thus, a trace analysis of about 1 ppm can be performed. 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.
【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。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.
【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。FIG. 2 is a flowchart illustrating a method for preparing an oil sample for fluorescent X-rays according to a second embodiment of the present invention.
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 2G001 AA01 BA04 CA01 LA04 NA04 RA02 RA20 2G052 AA08 AB01 AB11 AD26 AD52 EA03 FD09 FD18 GA19 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 2G001 AA01 BA04 CA01 LA04 NA04 RA02 RA20 2G052 AA08 AB01 AB11 AD26 AD52 EA03 FD09 FD18 GA19
Claims (4)
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、 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。1. A method of preparing an oil sample for extracting inorganic Cl contained in an oil sample and performing X-ray fluorescence analysis, wherein water or hydrogen peroxide and the oil sample are collected in a container. 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 water. An aqueous solution, a polar solvent that promotes the separation of the aqueous solution from the mixed liquid in the emulsion state is added, and the separated aqueous solution is dropped on a filter paper and dried.
Preparation of oil samples for line analysis.
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。2. The method for preparing an oil sample for X-ray fluorescence analysis according to claim 1, wherein the mixture is irradiated with ultrasonic waves after the addition of the polar solvent to further promote the separation.
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。3. The method according to claim 1, wherein the oil sample is a petroleum product or a semi-finished petroleum as a raw material thereof, the water is distilled water, the container is a separating funnel or a test tube, A method for preparing an oil sample for fluorescent X-ray analysis, wherein the solvent dissolving the wax component and the oil component is toluene or xylene, and the polar solvent is acetone, ethanol or isopropyl alcohol.
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
を求める油試料の分析方法。4. The content of inorganic Cl in an oil sample is determined by X-ray fluorescence analysis using the preparation method according to any one of claims 1 to 3, and is subtracted from the content of Cl as a whole in the oil sample. An oil sample analysis method for determining the content of organic Cl in an oil sample.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001087741A JP3567178B2 (en) | 2001-03-26 | 2001-03-26 | Method for preparing oil sample for X-ray fluorescence analysis and method for analyzing oil sample using the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001087741A JP3567178B2 (en) | 2001-03-26 | 2001-03-26 | Method for preparing oil sample for X-ray fluorescence analysis and method for analyzing oil sample using the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2002286596A true JP2002286596A (en) | 2002-10-03 |
| JP3567178B2 JP3567178B2 (en) | 2004-09-22 |
Family
ID=18942950
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001087741A Expired - Fee Related JP3567178B2 (en) | 2001-03-26 | 2001-03-26 | Method for preparing oil sample for X-ray fluorescence analysis and method for analyzing oil sample using the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3567178B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007502967A (en) * | 2003-08-20 | 2007-02-15 | メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフトング | Method for extraction and concentration of hydrophilic compounds diffused or dispersed in a hydrophobic liquid matrix |
| CN110987986A (en) * | 2018-08-14 | 2020-04-10 | 中国石油天然气股份有限公司 | Analysis method for inorganic matters in shaft plug of oil and gas well |
-
2001
- 2001-03-26 JP JP2001087741A patent/JP3567178B2/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007502967A (en) * | 2003-08-20 | 2007-02-15 | メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフトング | Method for extraction and concentration of hydrophilic compounds diffused or dispersed in a hydrophobic liquid matrix |
| CN110987986A (en) * | 2018-08-14 | 2020-04-10 | 中国石油天然气股份有限公司 | Analysis method for inorganic matters in shaft plug of oil and gas well |
| CN110987986B (en) * | 2018-08-14 | 2022-08-02 | 中国石油天然气股份有限公司 | Analysis method for inorganic matters in shaft plug of oil and gas well |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3567178B2 (en) | 2004-09-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Sharafi et al. | Trace determination of lead in lipsticks and hair dyes using microwave‐assisted dispersive liquid–liquid microextraction and graphite furnace atomic absorption spectrometry | |
| Katoch | Analytical techniques in biochemistry and molecular biology | |
| Ma et al. | Ultrasound-assisted emulsification–microextraction combined with flame atomic absorption spectrometry for determination of trace cadmium in water samples | |
| Jiang et al. | Cloud point extraction combined with electrothermal atomic absorption spectrometry for the speciation of antimony (III) and antimony (V) in food packaging materials | |
| Liang et al. | Speciation of As (III) and As (V) in water samples by dispersive liquid-liquid microextraction separation and determination by graphite furnace atomic absorption spectrometry | |
| Sun et al. | Determination of trace nickel in water samples by cloud point extraction preconcentration coupled with graphite furnace atomic absorption spectrometry | |
| Zhang et al. | Ultrasound-assisted emulsification solidified floating organic drop microextraction for the determination of trace cadmium in water samples by flame atomic absorption spectrometry | |
| Amjadi et al. | Reverse micelle coacervate-based extraction combined with electrothermal atomic absorption spectrometry for the determination of arsenic in water and oyster tissue samples | |
| Miranda-Andrades et al. | Combination of ultrasonic extraction in a surfactant-rich medium and distillation for mercury speciation in offshore petroleum produced waters by gas chromatography cold vapor atomic fluorescence spectrometry | |
| Bahar et al. | Determination of copper in human hair and tea samples after dispersive liquid-liquid microextraction based on solidification of floating organic drop (DLLME-SFO) | |
| Luong et al. | Combined organic biomarker and use-wear analyses of stone artefacts from Liang Bua, Flores, Indonesia | |
| Abdolmohammad-Zadeh et al. | Ligandless cloud point extraction for trace nickel determination in water samples by flame atomic absorption spectrometry | |
| Mendes et al. | Development of an eco-friendly method for the determination of total polychlorinated biphenyls in solid waste by gas chromatography-mass spectrometry | |
| Pereira et al. | Multivariate assessment of extraction conditions for the fractionation analysis of mercury in oily sludge samples using cold vapor atomic fluorescence spectrometry | |
| López-García et al. | Determination of very low amounts of free copper and nickel ions in beverages and water samples using cloud point extraction assisted by silver nanoparticles | |
| JP2002286596A (en) | Preparation method of preparing oil sample for fluorescent x-ray analysis, and analytical method of analyzing oil sample using the same | |
| Hosseini | Simultaneous concentration and determination of cadmium and lead ions using in situ solvent formation microextraction method based on functionalized ionic liquid | |
| US3058813A (en) | Apparatus for oxidation of organic liquids | |
| Ma et al. | Optimization of ultrasonic‐assisted extraction of 3‐monochloropropane‐1, 2‐diol (MCPD) and analysis of its esters from edible oils by gas chromatography–mass spectrometry | |
| Pinel et al. | Determination of trace amounts of total tin in water using extraction followed by graphite furnace atomic absorption spectrometry with an oxidising matrix modifier | |
| Lemos et al. | Spectrophotometric determination of mercury in water samples after preconcentration using dispersive liquid–liquid microextraction | |
| Krasnodêbska-Ostrêga et al. | Ultrasound-assisted acetic acid extraction of metals from soils | |
| Perera et al. | Techniques to Characterize PFAS Burden in Biological Samples: Recent Insights and Remaining Challenges | |
| Dadfarnia et al. | Selective cloud point extraction and preconcentration of trace amounts of cadmium prior to flame atomic absorption spectrometric determination | |
| Borges et al. | Determination of cadmium in sediments and in sewage sludge by slurry sampling electrothermal atomic absorption spectrometry using iridium as permanent modifier |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20040406 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20040409 |
|
| R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| LAPS | Cancellation because of no payment of annual fees |