JP2005274524A - Method and kit for diagnosing deterioration of oil transformer - Google Patents
Method and kit for diagnosing deterioration of oil transformer Download PDFInfo
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Abstract
Description
本発明は、油入変圧器の経年劣化度をフルフラールの含有量に応じて診断することのできる診断方法および該診断方法に使用される診断剤キットに関する。 The present invention relates to a diagnostic method capable of diagnosing the degree of aging of an oil-filled transformer according to the content of furfural, and a diagnostic agent kit used in the diagnostic method.
〔発明の背景〕
一般的に油入変圧器では、コイルの絶縁のために紙（絶縁紙）が用いられている。この絶縁紙は、放熱作用に優れるものの、経年により劣化するという欠点を有する。絶縁紙が劣化すると、例えば油入変圧器の近くに落雷した場合や外部短絡事故が発生した場合に、大電流が油入変圧器に流れ込み、電線間に生じた電磁機械力で絶縁紙が砕けてコイルがショートし、油入変圧器が使用不能となることがある。従って、油入変圧器では絶縁紙の劣化度を診断することが非常に重要である。
BACKGROUND OF THE INVENTION
Generally, in an oil-filled transformer, paper (insulating paper) is used for insulating a coil. Although this insulating paper has an excellent heat dissipation function, it has a drawback that it deteriorates with age. When insulation paper deteriorates, for example, when lightning strikes near an oil-filled transformer or when an external short circuit accident occurs, a large current flows into the oil-filled transformer and the insulation paper is crushed by the electromagnetic mechanical force generated between the wires. If the coil is short-circuited, the oil-filled transformer may become unusable. Therefore, in an oil-filled transformer, it is very important to diagnose the degree of deterioration of the insulating paper.
〔従来の技術〕
従来より、絶縁紙が劣化するとその重合度が低下してフルフラールが生成し、これが絶縁油中に溶出することが知られている。また、絶縁紙の引張り強度、平均重合度残率及びフルフラールの生成量には相関関係があることも知られている。従って、絶縁油中に溶出したフルフラールの量を測定すれば、絶縁紙の劣化度、即ち油入変圧器の劣化度を診断することができる。従来、この絶縁油中に溶出したフルフラールの量の測定は、高速液体クロマトグラフィーを使用して行っていた。しかしながら、高速液体クロマトグラフィーの取り扱いは煩雑であり、また高速液体クロマトグラフィー自体のコストが高いという問題があった。そこでｐ−ニトロフェニルヒドラジン溶液を使用する方法が提供されている（例えば特許文献１参照）。
[Conventional technology]
Conventionally, it is known that when the insulating paper is deteriorated, the degree of polymerization is reduced to generate furfural, which is eluted in the insulating oil. It is also known that there is a correlation between the tensile strength of the insulating paper, the average polymerization degree residual rate, and the amount of furfural produced. Therefore, if the amount of furfural eluted in the insulating oil is measured, the degree of deterioration of the insulating paper, that is, the degree of deterioration of the oil-filled transformer can be diagnosed. Conventionally, the amount of furfural eluted in this insulating oil has been measured using high performance liquid chromatography. However, the handling of high performance liquid chromatography is complicated, and the cost of high performance liquid chromatography itself is high. Therefore, a method using a p-nitrophenylhydrazine solution is provided (see, for example, Patent Document 1).
上記ｐ−ニトロフェニルヒドラジン溶液を使用する診断方法では、絶縁油中のフルフラールをアセトニトリル溶液によって抽出する。この方法では絶縁油の分解によって生成する他のアルデヒドも抽出され、フルフラールの量の測定を妨害し正確な診断が困難である、と云う問題点がある。
上記絶縁油の分解によって生成する他のアルデヒドはＣ１〜Ｃ１８の範囲のアルデヒドであり、特にＣ数の高いアルデヒドの割合が多く、該アルデヒドがフルフラールの量の測定を妨害する。
In the diagnostic method using the p-nitrophenylhydrazine solution, furfural in insulating oil is extracted with an acetonitrile solution. This method has a problem that other aldehydes generated by the decomposition of the insulating oil are also extracted, which hinders measurement of the amount of furfural and makes accurate diagnosis difficult.
Other aldehydes produced by the decomposition of the insulating oil are aldehydes in the range of C1 to C18, and particularly the proportion of aldehydes having a high C number is high, and the aldehyde interferes with the measurement of the amount of furfural.
本発明は上記従来の課題を解決するための手段として、絶縁油中のフルフラールを水またはアルコールまたは水−アルコール混合溶媒によって抽出し、該抽出液に２，４−ジニトロフェニルヒドラジン溶液とアルカリを添加して該抽出液を発色せしめ、該発色によって油入変圧器の劣化を診断する油入変圧器劣化診断方法を提供するものである。
上記水またはアルコールまたは水−アルコール混合溶媒には塩化ナトリウムが添加されていることが望ましく、また該絶縁油は油入変圧器内の絶縁紙から溶出したものである。
更に本発明では、水またはアルコールまたは水−アルコール混合溶媒と、２，４−ジニトロフェニルヒドラジン溶液と、アルカリとを組合わせてなる油入変圧器劣化診断剤キットが提供される。上記水またはアルコールまたは水−アルコール混合溶媒には塩化ナトリウムが添加されていることが望ましい。
As a means for solving the above-mentioned conventional problems, the present invention extracts furfural in insulating oil with water, alcohol, or a water-alcohol mixed solvent, and adds a 2,4-dinitrophenylhydrazine solution and an alkali to the extract. Thus, the present invention provides an oil-filled transformer deterioration diagnosis method for coloring the extract and diagnosing deterioration of the oil-filled transformer by the color development.
It is desirable that sodium chloride is added to the water, alcohol or water-alcohol mixed solvent, and the insulating oil is eluted from the insulating paper in the oil-filled transformer.
Furthermore, the present invention provides an oil-filled transformer deterioration diagnostic kit comprising a combination of water or alcohol or a water-alcohol mixed solvent, a 2,4-dinitrophenylhydrazine solution, and an alkali. It is desirable that sodium chloride is added to the water, alcohol or water-alcohol mixed solvent.
〔作用〕
本発明にあっては、絶縁油中のフルフラール（２−フルフラール）を水またはアルコールまたは水−アルコール混合溶媒である抽出溶媒によって抽出する。上記水またはアルコール、特にＣ数３以下の低級アルコールを抽出溶媒として使用すると、絶縁油中の種々なアルデヒドのうちＣ数の大きな高分子量のアルデヒドは、上記極性溶媒に難溶であり、溶媒中に殆ど溶出しない。
更に絶縁油はＣ１８の炭化水素を主成分としており、したがって劣化によって生成するアルデヒドはＣ１８以下のものであることが推測されるが、絶縁油中のアルデヒドの大部分は高分子量のものである。
したがって上記極性溶媒を使用すると、絶縁油中の高分子量のアルデヒドの大部分を除去することが出来、フルフラールを精度よく分析することが出来る。
本発明で使用する２，４−ジニトロフェニルヒドラジンは酸性溶液中で、アルデヒド類と反応して２，４−ジニトロフェニルヒドラゾンを生成し、アルカリを添加してアルカリ性にすれば赤色に発色する。この反応は定量的に行われるから、抽出液中にフルフラールのみ存在する場合には、フルフラールを定量することが出来る。
更に絶縁油は劣化によって金属石けんを生成する。上記金属石けんは界面活性作用を有するので、絶縁油中に金属石けんが存在すると、絶縁油と抽出溶媒との分離が困難になる。このような場合には抽出溶媒中に塩化ナトリウムを添加すれば、絶縁油と抽出溶媒との分離が容易になる。
[Action]
In this invention, the furfural (2-furfural) in insulating oil is extracted with the extraction solvent which is water, alcohol, or a water-alcohol mixed solvent. When the above water or alcohol, especially a lower alcohol having 3 or less carbon atoms is used as an extraction solvent, a high molecular weight aldehyde having a large C number among various aldehydes in insulating oil is hardly soluble in the polar solvent. Hardly eluted.
Furthermore, the insulating oil is mainly composed of C18 hydrocarbons. Therefore, it is estimated that the aldehyde produced by the degradation is C18 or less, but most of the aldehyde in the insulating oil has a high molecular weight.
Therefore, when the polar solvent is used, most of the high molecular weight aldehyde in the insulating oil can be removed, and furfural can be analyzed with high accuracy.
The 2,4-dinitrophenylhydrazine used in the present invention reacts with aldehydes in an acidic solution to produce 2,4-dinitrophenylhydrazone, and when it is made alkaline by adding an alkali, it develops a red color. Since this reaction is performed quantitatively, when only furfural is present in the extract, furfural can be quantified.
Furthermore, insulating oil produces metal soap due to deterioration. Since the metal soap has a surface-active action, if the metal soap is present in the insulating oil, it is difficult to separate the insulating oil from the extraction solvent. In such a case, if sodium chloride is added to the extraction solvent, the insulating oil and the extraction solvent can be easily separated.
〔効果〕
したがって本発明では、高価な装置を使用することなく、簡便かつ正確に油入変圧器の劣化度を判断することが出来る。
〔effect〕
Therefore, in the present invention, the deterioration degree of the oil-filled transformer can be determined easily and accurately without using an expensive device.
以下、本発明を詳細に説明する。
本発明の対象とする変圧器は、コイルの絶縁のために絶縁紙が使用されており、かつ絶縁油が使用されている油入変圧器である。該絶縁紙としては、一般的にセルロースからなるものが用いられる。また、絶縁油としては、一般的にナフテン系炭化水素、芳香族炭化水素およびパラフィン系炭化水素を含む炭化水素混合物や、パラフィン系炭化水素からなるものが用いられ、これら絶縁油であれば本発明の診断を行うことができる。
Hereinafter, the present invention will be described in detail.
The transformer which is the subject of the present invention is an oil-filled transformer in which insulating paper is used for coil insulation and insulating oil is used. As the insulating paper, one made of cellulose is generally used. Further, as the insulating oil, generally, a hydrocarbon mixture containing naphthenic hydrocarbon, aromatic hydrocarbon and paraffinic hydrocarbon, or one made of paraffinic hydrocarbon is used. Can be diagnosed.
本発明では、まず油入変圧器の絶縁油に対して、フルフラール分の抽出処理を施す。通常、油入変圧器から絶縁油を一定量取り出し、それに対してフルフラールの抽出を行う。絶縁油を取り出す量は特に限定されず、劣化診断を行うことのできる範囲であればよい。一般的には、２〜２００ml程度で足りる。
絶縁油からのフルフラールの抽出は、常法によって行うことができる。例えば、絶縁油に所定の溶剤を加え、よく振とうする。抽出に使用する溶媒としては、水またはアルコールまたは水−アルコール混合溶媒である抽出溶媒を使用する。アルコールはメタノール、エタノール、イソプロパノール等のＣ３以下の低級アルコールを使用する。
上記極性溶媒を抽出溶媒として使用することによって、前記したように絶縁油中のフルフラールを選択的に抽出することが出来る。絶縁油と該抽出溶媒との体積比は、１：１〜１：４であるのが好ましい。また、振とうは１〜３分間程度行うのが好ましい。
In the present invention, first, the furfural component is extracted from the insulating oil of the oil-filled transformer. Usually, a certain amount of insulating oil is taken out from the oil-filled transformer, and furfural is extracted from it. The amount of the insulating oil taken out is not particularly limited as long as the deterioration diagnosis can be performed. Generally, about 2 to 200 ml is sufficient.
Extraction of furfural from insulating oil can be performed by a conventional method. For example, a predetermined solvent is added to the insulating oil and shaken well. As a solvent used for extraction, an extraction solvent which is water, alcohol, or a water-alcohol mixed solvent is used. As the alcohol, a C3 or lower lower alcohol such as methanol, ethanol or isopropanol is used.
By using the polar solvent as an extraction solvent, it is possible to selectively extract furfural in insulating oil as described above. The volume ratio between the insulating oil and the extraction solvent is preferably 1: 1 to 1: 4. The shaking is preferably performed for about 1 to 3 minutes.
更に該抽出溶媒に塩化ナトリウムを添加する場合には、上記抽出溶媒１００mlに対して通常塩化ナトリウムを０．５〜１．５ｇ添加する。 Further, when sodium chloride is added to the extraction solvent, 0.5 to 1.5 g of sodium chloride is usually added to 100 ml of the extraction solvent.
上記抽出処理を行った後、静置して、フルフラールを抽出した溶媒層（抽出処理液）を分離し採取する。前記したように絶縁油が劣化により金属石けんを含有する場合でも、該抽出溶媒に塩化ナトリウムが添加されていると、絶縁油と抽出溶媒との分離は明確に行なわれ、抽出処理液の採取は容易になる。該抽出処理液は下層に分離する。抽出処理液が得られたら、その抽出処理液を所望なれば濾過した後、２，４−ジニトロフェニルヒドラジンを添加混合する。抽出処理液中にフルフラールが存在すれば、該フルフラールと２，４−ジニトロフェニルヒドラジンとは酸性条件下で反応を起こす。
２，４−ジニトロフェニルヒドラジンは、一般的には希塩酸水溶液に溶解して使用する。上記２，４−ジニトロフェニルヒドラジン溶液の濃度は、１〜５ｇ／Ｌであるのが好ましく、特に２ｇ／Ｌであるのが好ましい。
希塩酸水溶液としては通常０．５〜１．５質量％塩酸水溶液を使用する。
After performing the above extraction treatment, the mixture is allowed to stand, and the solvent layer (extraction treatment liquid) from which furfural has been extracted is separated and collected. As described above, even when the insulating oil contains metal soap due to deterioration, when sodium chloride is added to the extraction solvent, the separation of the insulating oil and the extraction solvent is clearly performed, and the extraction treatment liquid is collected. It becomes easy. The extraction processing liquid is separated into lower layers. When an extraction treatment liquid is obtained, the extraction treatment liquid is filtered if desired, and then 2,4-dinitrophenylhydrazine is added and mixed. If furfural is present in the extraction treatment liquid, the furfural and 2,4-dinitrophenylhydrazine react under acidic conditions.
2,4-Dinitrophenylhydrazine is generally used by dissolving in dilute hydrochloric acid aqueous solution. The concentration of the 2,4-dinitrophenylhydrazine solution is preferably 1 to 5 g / L, and particularly preferably 2 g / L.
As the dilute hydrochloric acid aqueous solution, a 0.5 to 1.5 mass% hydrochloric acid aqueous solution is usually used.
抽出処理液と上記２，４−ジニトロフェニルヒドラジン溶液との混合比（体積）は、１：１〜１：４であるのが好ましい。
上記抽出処理液に２，４−ジニトロフェニルヒドラジン溶液を添加した後は室温で３０分程度放置して反応を進行させてもよいが、６０〜８０℃で３０秒〜２分加熱するのが好ましい。このように加熱することにより、フルフラールと２，４−ジニトロフェニルヒドラジンとの反応を効率よく進行させることができる。
The mixing ratio (volume) of the extraction treatment liquid and the 2,4-dinitrophenylhydrazine solution is preferably 1: 1 to 1: 4.
After the 2,4-dinitrophenylhydrazine solution is added to the extraction treatment solution, the reaction may be allowed to proceed at room temperature for about 30 minutes, but it is preferable to heat at 60 to 80 ° C. for 30 seconds to 2 minutes. . By heating in this way, the reaction between furfural and 2,4-dinitrophenylhydrazine can proceed efficiently.
次に、上記反応液にアルカリを添加する。アルカリとしては、水酸化カリウム、水酸化ナトリウム等を使用することができ、好ましくは、水酸化カリウムを使用する。
このアルカリは、一般的には３〜７質量％の水溶液として使用する。
Next, an alkali is added to the reaction solution. As the alkali, potassium hydroxide, sodium hydroxide or the like can be used, and potassium hydroxide is preferably used.
This alkali is generally used as a 3 to 7% by mass aqueous solution.
上記反応液とアルカリ水溶液との混合比（体積）は、１：２〜１：４であるのが好ましく、特に１：３であるのが好ましい。
以上のように上記反応液とアルカリとを混合すると、フルフラールと２，４−ジニトロフェニルヒドラジンとの反応物が赤色に発色する。
従って、この発色の程度を測定することにより、絶縁紙、ひいては油入変圧器の劣化度を診断することができる。
The mixing ratio (volume) of the reaction solution and the aqueous alkali solution is preferably 1: 2 to 1: 4, and particularly preferably 1: 3.
As described above, when the reaction solution and the alkali are mixed, the reaction product of furfural and 2,4-dinitrophenylhydrazine develops a red color.
Therefore, by measuring the degree of color development, it is possible to diagnose the degree of deterioration of the insulating paper and thus the oil-filled transformer.
例えば、フルフラールの含有量が既知の絶縁油について、本発明の方法に従って発色させた標準試料を用意しておけば、この標準試料の色と比較することにより、診断対象の絶縁油中のフルフラールの含有量が分かり、油入変圧器の劣化度を診断することができる。
色の比較は目視によって行うこともできるが、例えば分光光度計を使用すれば、さらに正確に行うことができる。分光光度計を使用する場合、４７０nmにおける吸光度を測定するのが好ましい。このように分光光度計を使用すると、絶縁油中における１０ppm 以下の含有量のフルフラールを測定することができる。
本発明では、標準試料、あるいはそれを用いた検量線を作製しておけば、実際に劣化度診断を行う際に高速液体クロマトグラフィーを使用する必要がないため、低コストで、また煩雑な操作を行うことなく、油入変圧器の劣化度の診断を行うことができる。
For example, if a standard sample colored in accordance with the method of the present invention is prepared for an insulating oil with a known furfural content, the color of the furfural in the insulating oil to be diagnosed can be compared with the color of this standard sample. The content can be understood and the deterioration degree of the oil-filled transformer can be diagnosed.
The color comparison can be performed by visual observation, but can be performed more accurately by using, for example, a spectrophotometer. When using a spectrophotometer, it is preferable to measure the absorbance at 470 nm. When the spectrophotometer is used in this way, it is possible to measure furfural having a content of 10 ppm or less in the insulating oil.
In the present invention, if a standard sample or a calibration curve using the standard sample is prepared, it is not necessary to use high performance liquid chromatography when actually diagnosing the degree of deterioration. The deterioration degree of the oil-filled transformer can be diagnosed without performing the operation.
〔アルデヒド類の除去試験〕
種々の抽出溶媒によって絶縁油中のフルフラール抽出の際のアルデヒド除去を検討した。
試験は使用油１０mlに対して純水、５質量％エタノール水溶液および２０質量％エタノール水溶液１０mlをそれぞれ別々に加え１分間の振とうにより抽出を行った後静置し、抽出層の非水系メンブランフィルター（０．４５μｍ）ろ液に２，４−ジニトロフェニルヒドラジン溶液を加え、高速液体クロマトグラフに導入した。使用油中のアルデヒドはアセトニトリルを抽出溶媒として同様の操作を行って評価した。尚、高速液体クロマトグラフでの分析は炭素数１〜９のアルデヒドを対象とした。
試験結果を表１に示す。
[Aldehyde removal test]
The removal of aldehyde during extraction of furfural in insulating oil was investigated with various extraction solvents.
For the test, pure water, 10% aqueous ethanol solution and 10% aqueous 20% ethanol solution were separately added to 10 ml of the oil used, extracted by shaking for 1 minute, and allowed to stand, and then the non-aqueous membrane filter of the
The test results are shown in Table 1.
表１によれば、使用油に含まれるアルデヒド類は炭素数１（ホルムアルデヒド）から存在し、分子量の増加とともに含有量が増える傾向が認められる。
純水、５質量％エタノール水溶液および２０質量％エタノール水溶液での除去を行った試料には、すべてのアルデヒドに対して除去効果が見られた。
また純水、５質量％エタノール水溶液、２０質量％エタノール水溶液を溶媒として使用すると、Ｃ４以上のアルデヒドは全く抽出されず、Ｃ３以下のアルデヒドも極く微量しか抽出されないことが確認出来る。
According to Table 1, aldehydes contained in the oil used are present from carbon number 1 (formaldehyde), and the tendency for the content to increase with increasing molecular weight is recognized.
Samples that had been removed with pure water, 5% by mass ethanol aqueous solution, and 20% by mass ethanol aqueous solution showed a removal effect on all aldehydes.
Moreover, when pure water, 5 mass% ethanol aqueous solution, and 20 mass% ethanol aqueous solution are used as a solvent, it can be confirmed that C4 or higher aldehyde is not extracted at all, and that C3 or lower aldehyde is extracted only in a very small amount.
以下、実施例により本発明を更に具体的に説明するが、本発明の範囲はこれらの実施例に限定されるものではない。
〔調製例１〕
２，４−ジニトロフェニルヒドラジン溶液の調製
２，４−ジニトロフェニルヒドラジン（関東化学株式会社製，ＧＲ）２００mgをビーカーに取り、１容量％の塩酸水溶液１００mlに溶解した後ろ紙でろ過した。
〔調製例２〕
水酸化カリウム溶液の調製
約８０mlの純水をビーカーに取り、水酸化カリウム（関東化学株式会社製，ＧＲ）５ｇを加え溶解した後、純水を加え１００mlとした。
〔調製例３〕
抽出溶媒の調製
約６０mlの純水をビーカーに取り、エタノール２０ml（キシダ化学株式会社製，ＧＲ）を加え攪拌した後、純水を加え１００mlとした後、１ｇの塩化ナトリウム（キシダ化学株式会社製，ＧＲ）を加え溶解させた。
〔調製例４〕
２−フルフラール標準液の調製
２−フルフラール（和光純薬工業株式会社製，ＧＲ）１. ０００ｇをビーカーに取り、アセトニトリルに溶解後、１Ｌメスフラスコに移し、アセトニトリルを加えて定容した。この溶液を純水で５０倍に希釈した後、段階的に２００mlメスフラスコに採取して純水で定容することにより０．５〜２．０mg／Ｌの２−フルフラール標準液を作成した。
EXAMPLES Hereinafter, the present invention will be described more specifically with reference to examples. However, the scope of the present invention is not limited to these examples.
[Preparation Example 1]
Preparation of 2,4-dinitrophenylhydrazine solution 200 mg of 2,4-dinitrophenylhydrazine (manufactured by Kanto Chemical Co., Inc., GR) was taken in a beaker and filtered with a back paper dissolved in 100 ml of 1% by volume hydrochloric acid aqueous solution.
[Preparation Example 2]
Preparation of potassium hydroxide solution Approximately 80 ml of pure water was placed in a beaker, 5 g of potassium hydroxide (manufactured by Kanto Chemical Co., Inc., GR) was added and dissolved, and then pure water was added to make 100 ml.
[Preparation Example 3]
Preparation of extraction solvent Approximately 60 ml of pure water was placed in a beaker, 20 ml of ethanol (manufactured by Kishida Chemical Co., Ltd., GR) was added and stirred, pure water was added to make 100 ml, and 1 g of sodium chloride (manufactured by Kishida Chemical Co., Ltd.). , GR) was added and dissolved.
[Preparation Example 4]
Preparation of 2 -Furfural Standard Solution 2-Furfural (Wako Pure Chemical Industries, Ltd., GR) 1.000 g was taken in a beaker, dissolved in acetonitrile, transferred to a 1 L volumetric flask, and acetonitrile was added to adjust the volume. After diluting this solution 50 times with pure water, it was collected stepwise into a 200 ml volumetric flask and made up to volume with pure water to prepare a 0.5-2.0 mg / L 2-furfural standard solution.
〔実施例１〕
２−フルフラール標準液をそれぞれサンプルビンに採取し、２，４−ジニトロフェニルヒドラジン溶液２mlをそれぞれ加えて攪拌した後、３０分間静置した。これに水酸化カリウム溶液０．５mlを加え攪拌した後、再び１分間静置して得られた液について波長４７０nmにおける吸光度を分光光度計（日本分光株式会社製Ｕｂｅｓｔ−３０）で測定したところ、図１に示すような２−フルフラール濃度と吸光度の関係を示す検量線が得られた。次に、使用期間がことなる各種油入変圧器から１０ｇづつの絶縁油を採取した。各絶縁油をサンプルビンに取り、抽出溶媒１０mlを加え１分間よく振とうした。その後静置し、界面が一定したところで、下層（抽出溶液層）の溶液５mlをシリンジに取った。シリンジにろ紙（クロマトディスク１３Ｎ／ジーエルサイエンス製）を取付けた後、溶液をろ過しながら別のサンプルビンに採取した。この溶液に２，４−ジニトロフェニルヒドラジン溶液２mlを加えて攪拌した後、３０分間静置した。これに水酸化カリウム溶液０．５mlを加え攪拌した後、再び１分間静置して得られた液について波長４７０nmにおける吸光度を測定した。この吸光度と図１に示す２−フルフラール濃度と吸光度の関係を示す検量線から各絶縁油中のフルフラール含有量を推測した。
一方、同じ絶縁油について高速液体クロマトグラフィー（島津製作所製１０ＡＤ）を使用してフルフラール含有量を測定した。その結果、抽出溶媒によって８０％程度のフルフラールが回収され、図２に示すような高い相関が得られた。
[Example 1]
Each 2-furfural standard solution was collected in a sample bottle, 2 ml of a 2,4-dinitrophenylhydrazine solution was added and stirred, and then allowed to stand for 30 minutes. After adding 0.5 ml of potassium hydroxide solution to this and stirring, the absorbance at a wavelength of 470 nm was measured with a spectrophotometer (Ubest-30 manufactured by JASCO Corporation) for the liquid obtained by standing again for 1 minute. A calibration curve showing the relationship between 2-furfural concentration and absorbance as shown in FIG. 1 was obtained. Next, 10 g of insulating oil was sampled from various oil-filled transformers with different usage periods. Each insulating oil was taken into a sample bottle, and 10 ml of extraction solvent was added and shaken well for 1 minute. Then, the mixture was allowed to stand, and when the interface was fixed, 5 ml of the lower layer (extraction solution layer) solution was taken into a syringe. After attaching filter paper (Chromatodisc 13N / manufactured by GL Science) to the syringe, the solution was collected in another sample bottle while filtering. To this solution, 2 ml of 2,4-dinitrophenylhydrazine solution was added and stirred, and then allowed to stand for 30 minutes. After adding 0.5 ml of potassium hydroxide solution to this and stirring, the absorbance at a wavelength of 470 nm was measured for the liquid obtained by allowing to stand again for 1 minute. The furfural content in each insulating oil was estimated from a calibration curve showing the relationship between this absorbance and the 2-furfural concentration and absorbance shown in FIG.
On the other hand, the furfural content was measured using high performance liquid chromatography (Shimadzu 10AD) for the same insulating oil. As a result, about 80% of furfural was recovered by the extraction solvent, and a high correlation as shown in FIG. 2 was obtained.
本発明では油入り変圧器の劣化度を簡便かつ正確に診断することが出来る。 In the present invention, the deterioration degree of the oil-filled transformer can be easily and accurately diagnosed.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008224563A (en) * | 2007-03-15 | 2008-09-25 | Mitsubishi Electric Corp | Method for analyzing carbonyl compound in oil |
| KR100995709B1 (en) | 2008-12-23 | 2010-11-19 | 한국전기연구원 | Load management equipment for oil filled transformers |
| CN106124701A (en) * | 2016-06-21 | 2016-11-16 | 林光琴 | Power transformer performance monitoring system |
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| CN106124701A (en) * | 2016-06-21 | 2016-11-16 | 林光琴 | Power transformer performance monitoring system |
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