CN100405055C - Method for detecting oxidation preventive content in jet fuel - Google Patents
Method for detecting oxidation preventive content in jet fuel Download PDFInfo
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- CN100405055C CN100405055C CNB2005100912361A CN200510091236A CN100405055C CN 100405055 C CN100405055 C CN 100405055C CN B2005100912361 A CNB2005100912361 A CN B2005100912361A CN 200510091236 A CN200510091236 A CN 200510091236A CN 100405055 C CN100405055 C CN 100405055C
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Abstract
The present invention relates to a method for detecting anti-oxidant content in jet fuel, which is characterized in that the anti-oxidant content is detected by using an electrochemical analyzer and a differential pulse voltammetry. The present invention has the characteristics of quickness, convenient operation, high accuracy, few interference factors, convenient electrochemical analyzer and convenient carrying; the present invention can realize the field analysis of samples; the present invention is used for routine analysis, which can more embody the characteristics of the method of quickness and convenience.
Description
Technical field
The present invention relates to the assay method of oxidation preventive content, the electrochemical determination method of oxidation preventive content in particularly a kind of jet fuel.
Background technology
Current, increase year by year with the jet fuel of hydrocracking, hydrofining technology production, and the jet fuel of hydrocracking, hydrofining technology production must add proper quantity of antioxidant such as 2,6 ditertiary butyl p cresol (BHT) to ensure the quality of products.China's regulation need add antioxidant (21 ± 3) mg/L through the jet fuel of hydrogenation production, and this regulation is to use for reference the way of Great Britain and America's western developed country substantially.People such as Bruce studies show that, have only after the antioxidant in the fuel runs out of, and jet fuel just generates superoxide.Therefore, the consumption degree of antioxidant also can help the storage time limit of fuel use department decision fuel with regard to the rotten situation of measurable fuel in the trace analysis fuel, thereby avoids producing in the fuel storage process harm that a large amount of superoxide may cause.
Detect the method that antioxidant is commonly used in the jet fuel at present high performance liquid chromatography, ultraviolet spectroscopy, gas chromatography etc. are arranged.Wherein:
Liquid phase chromatography: Cunningham analyzes antioxidant with high performance liquid chromatography (HPLC), UV-detector; Pearson, Hayes, Mei-Hsia use electrochemical detector analysis of phenols antioxidant 2 with the HPLC method, 6-DI-tert-butylphenol compounds, 2,4-DI-tert-butylphenol compounds, the 6-tert-butyl group-2, the content of 4-xylenol in fuel, wherein Mei-Hsia has done more deep research to 2,6 di t butyl phenol Determination on content in JP-5.Domestic, generally adopting hexane is moving phase, silica gel chromatographic column, use UV-detector and detect, and the record chromatogram.Because of the variation of sample component polarity, the separating power of chromatographic column is descended, cause the repeated non-constant of detection.
Ultraviolet spectroscopy: be subjected to the interference of components such as aromatic hydrocarbons, can not directly measure 2,6 ditertiary butyl p cresol in the jet fuel with the ultraviolet photometry.Adopt the KOH-ethanolic solution of boiling, the antioxidant in the jet fuel is extracted, and in 100 ℃ of water-baths, reach Cu
2+Under the condition that exists, make antioxidant change into annulenones, this material has absorption maximum at the 368nm place, and its range of linearity is 0-30mg/L.Routine adds extraction heat and catalytic process is consuming time longer, once analyzes about 2 hours, and the incompatibility product export is analyzed, and for this reason, has taked microwave abstracting, microwave catalysis technology, has improved oxidation preventive content assay method in the jet fuel.Microwave abstracting can improve the boiling point of solvent with the extract transient heating to more than the atmospheric boiling point, but is unlikely to the decomposition goal composition, has shortened the extraction time, has improved extraction efficiency.The pretreatment can be finished in 10 minutes, and whole test was finished about 20 minutes, had improved work efficiency greatly, also cut down the consumption of energy simultaneously.But this method needs specific microwave pressure sample-dissolving device, though overcome the deficiency of liquid chromatogram measuring method, supplementary equipment therefore makes this method be difficult to popularize.
Gas chromatography method (being called for short the GC/MS method): the 2,6 ditertiary butyl p cresol method adopts single ion scan mode (SIM) in the GC/MS mensuration jet fuel, selects the strongest characteristic ion m/z=205 of 2,6 ditertiary butyl p cresol quantitative.The method has been eliminated the interference of a large amount of hydrocarbon components effectively, can shorten analysis time greatly, improves the sensitivity of quantitative measurement.But expensive instrument and equipment can't make this technology be widely used for the routine analysis of 2,6 ditertiary butyl p cresol in the jet fuel.
In sum, the method that does not also have at present oxidation preventive content in a kind of comparative maturity and the simple and easy to do mensuration jet fuel.
Summary of the invention
The object of the present invention is to provide the assay method of oxidation preventive content in the jet fuel that a kind of cost is low, easy and simple to handle, accuracy in detection is high.
The assay method of oxidation preventive content in a kind of jet fuel, it is characterized in that: with the alkali metal hydroxide alcoholic solution antioxidant in the jet fuel is extracted, utilize electrochemical analyser to adopt the differentiated pulse voltammetry that wherein oxidation preventive content is carried out quantitative test.
Extract is the 0.1M potassium hydroxide-ethanol solution in the said method; The electrode system of described electrochemical analyser is selected glass carbon working electrode for use, the non-water contrast electrode of silver/silver chloride, platinum filament auxiliary electrode.
Concrete condition determination in the said method: initial voltage-0.1V, final voltage+0.5V, voltage increment 0.001～0.005V, amplitude 0.01～0.10V, pulse width 0.02～0.08s, sampling width 0.01～0.04s, time of repose 1.0～2.0s, sensitivity 1 * 10
-5
In the said method, selection-0.1V～+ the differentiated pulse volt-ampere characteristic of the interval described antioxidant standard specimen of 0.1V carries out quantitative test to the testing sample that contains described antioxidant.
Specifically, the present invention at first carries out electrochemical analysis to it to the electrochemical properties application of differential pulse voltammetry of described antioxidant standard specimen under the said determination condition, obtain its family curve, record-0.05V～+ interval its family curve of 0.1V in the volt-ampere peak heights, and related with the corresponding concentration of described antioxidant standard specimen, obtain linear model; Repeat the electrochemical analysis process identical with described antioxidant standard specimen and described testing sample is carried out quantitative test obtain its volt-ampere peak heights value, the described linear model of substitution is by calculating the content of the antioxidant in the testing sample.
More specifically say: the present invention is serial standard specimen and a blank sample of at first preparing antioxidant described in the jet fuel, then it is extracted successively; Utilize electrochemical analyser to adopt the differentiated pulse voltammetry under described condition determination, it to be carried out electrochemical analysis one by one again, obtain the characteristic differentiation pulse volt-ampere characteristic of described antioxidant series standard specimen; Write down in its family curve-0.05V～+ the feature volt-ampere peak heights value in 0.1V interval, and related with the corresponding concentration of described antioxidant series standard specimen, obtain its linear model; The repetition process identical with the electrochemical analysis of described antioxidant series standard specimen carried out quantitative test to described testing sample and obtained its feature volt-ampere peak heights value, and the described linear model of substitution is by calculating the content of antioxidant in the described testing sample.
Above-mentioned antioxidant is 2,6 ditertiary butyl p cresol, 2,6 di t butyl phenol, 2, the 4-DI-tert-butylphenol compounds or the 6-tert-butyl group-2,4-xylenol; The content of above-mentioned antioxidant is good in 10mg/L-30mg/L scope test effect.
Why antioxidant has the low temperature antioxygenic property, and reason just is self by at first oxidation, to have stoped the oxidation of oxygenant to product.Application of differential pulse voltammetry of the present invention characterizes the electrochemical properties of antioxidant 2,6 ditertiary butyl p cresol, and its process is as follows:
One, experimental apparatus and condition
Instrument: electrochemical analyser
Electrode system: 3mm glass carbon working electrode, the non-water contrast electrode of silver/silver chloride, 0.5mm platinum filament auxiliary electrode.
Electrolyte system: 0.1M potassium hydroxide-ethanol solution
Condition determination: initial voltage-0.1V, final voltage+0.5V, voltage increment 0.002V, amplitude 0.05V, pulse width 0.06s, sampling width 0.02s, time of repose 2.0s, sensitivity 1 * 10
-5
Two, step:
Get 0.1M KOH ethanolic solution 2ml in electrolytic cell, add the ethanolic solution of the 2,6 ditertiary butyl p cresol of 1 μ l concentration, 10000 μ l/ml, shake up, carry out electrochemical measurement by the said determination condition;
In above-mentioned solution, adding 2 μ l concentration is the ethanolic solution of the 2,6 ditertiary butyl p cresol of 10000 μ l/ml again, repeats the electrochemical measurement process under the said determination condition;
In above-mentioned solution, adding 2 μ l concentration is the ethanolic solution of the 2,6 ditertiary butyl p cresol of 10000 μ l/ml again, repeats the electrochemical measurement process under the said determination condition.
Obtain the differentiated pulse volt-ampere characteristic of 2,6 ditertiary butyl p cresol under the variable concentrations condition at last, see Fig. 1.Can find by Fig. 1: have the differentiated pulse volt-ampere characteristic of the antioxidant 2,6 ditertiary butyl p cresol of feature in-0.05V-+0.10V interval; Along with the increase of antioxidant 2,6 ditertiary butyl p cresol concentration, feature volt-ampere peak moves to the noble potential direction, and this is typical irreversible adsorption process; Characteristic height ip increases with the increase of antioxidant 2,6 ditertiary butyl p cresol content in the electrolyte system.
In a word, that the present invention has is quick, easy and simple to handle, accuracy is high, be subjected to the few characteristics of disturbing factor, and electrochemical analysing equipment is easy, is easy to carry, and can realize the on-the site analysis to sample, more can embody its quick, easy characteristics especially for routine analysis.
Description of drawings
Fig. 1: the differentiated pulse volt-ampere curve figure of 2,6 ditertiary butyl p cresol;
Fig. 2: be in the embodiment of the invention 1 in blank sample is analyzed the differentiated pulse volt-ampere curve figure of gained;
Fig. 3: be in the embodiment of the invention 1 in standard model is analyzed the differentiated pulse volt-ampere curve figure of gained.
Embodiment
Embodiment 1
To contain antioxidant 2,6 ditertiary butyl p cresol and concentration No. 3 jet fuels in the 10mg/L-30mg/L scope is testing sample.
Condition determination: instrument: electrochemical analyser; Electrode system: 3mm glass carbon working electrode, the non-water contrast electrode of Ag/AgCl, 0.5mm platinum filament auxiliary electrode; Electrolyte system: 0.1M KOH ethanolic solution; Initial voltage-0.1V, final voltage+0.5V, voltage increment 0.002V, amplitude 0.05V, pulse width 0.06s, sampling width 0.02s, time of repose 2.0s, sensitivity 1 * 10
-5
Determination step:
At first the standard specimen to the antioxidant 2,6 ditertiary butyl p cresol carries out electrochemical analysis.
The preparation of deposit standard specimen: accurately take by weighing 0.05g 2, the 6-BHT is in the 50ml beaker, add the jet fuel identical with sample a little, dissolving, and be transferred in the 100ml volumetric flask, constant volume, getting concentration is 2 of 500 μ g/ml, 6-BHT jet fuel solution is the deposit standard specimen.
Standard model solution and the preparation of blank sample solution: in 6 volumetric flasks, add deposit standard specimen 0.5ml respectively, 0.75ml, 1.0ml, 1.25ml, 1.5ml and blank sample, constant volume, get concentration and be respectively 10 μ g/ml, 15 μ g/ml, 20 μ g/ml, series standard sample solution and the blank sample solution of 25 μ g/ml, 30 μ g/ml.
Blank sample is analyzed: get 2ml electrolyte system solution in the taper separating funnel, add the 5ml jet fuel again, carry out extracting operation, be concuss 5 minutes, treat layering after, take off portion's extract, carry out electrochemical measurement by above-mentioned condition determination, get differentiated pulse volt-ampere curve (Fig. 2).
Standard model is analyzed: according to the extraction conditions of blank sample, successively the series standard sample solution is carried out electrochemical measurement under extracting operation and the said determination condition, characteristic differentiation pulse volt-ampere characteristic (Fig. 3);
Write down in the above-mentioned family curve (Fig. 3)-0.05V～+ the feature volt-ampere peak heights value ip in 0.10V interval, and related with the corresponding concentration C of series standard sample, following linear model:
C(μg/ml)＝-2.567×10
-7+7.467×10
-7ip R＝0.9987。
Wherein error at measurment is as shown in the table:
Hence one can see that, use the content that the present invention can detect antioxidant in the jet fuel exactly, exist good linear relationship (antioxidant concentration is in the 10mg/L-30mg/L scope) between the volt-ampere characteristic peak intensity of antioxidant and its concentration, and maximum relative error is less than 4%.
Embodiment 2: the testing sample analysis
In the analysis of testing sample, step is with embodiment 1, and difference only is to change standard model into testing sample.
Claims (8)
1. the assay method of oxidation preventive content in the jet fuel, it is characterized in that: with the alkali metal hydroxide alcoholic solution antioxidant in the jet fuel is extracted, utilize electrochemical analyser to adopt the differentiated pulse voltammetry that wherein oxidation preventive content is carried out quantitative test; In the described method, selection-0.1V～+ the differentiated pulse volt-ampere characteristic of the interval described antioxidant standard specimen of 0.1V carries out quantitative test to the testing sample that contains described antioxidant.
2. the assay method of oxidation preventive content in the jet fuel as claimed in claim 1 is characterized in that: extract is a potassium hydroxide-ethanol solution in the described method; The electrode system of described electrochemical analyser is selected glass carbon working electrode for use, the non-water contrast electrode of silver/silver chloride, platinum filament auxiliary electrode.
3. the assay method of oxidation preventive content in the jet fuel as claimed in claim 2 is characterized in that: described extract is the 0.1M potassium hydroxide-ethanol solution; Condition determination in the described method: initial voltage-0.1V, final voltage+0.5V, voltage increment 0.001～0.005V, amplitude 0.01～0.10V, pulse width 0.02～0.08s, sampling width 0.01～0.04s, time of repose 1.0～2.0s, sensitivity 1 * 10
-5A/V.
4. the assay method of oxidation preventive content in the jet fuel as claimed in claim 1 is characterized in that: described antioxidant is 2,6 ditertiary butyl p cresol, 2,6 di t butyl phenol, 2, the 4-DI-tert-butylphenol compounds or the 6-tert-butyl group-2,4-xylenol.
5. the assay method of oxidation preventive content in the jet fuel as claimed in claim 3, it is characterized in that: at first the electrochemical properties application of differential pulse voltammetry to described antioxidant standard specimen carries out electrochemical analysis to it under condition determination, obtain its family curve, record-0.05V～+ interval its family curve of 0.1V in the volt-ampere peak heights, and related with the corresponding concentration of described antioxidant standard specimen, obtain linear model; Repeat the electrochemical analysis process identical with described antioxidant standard specimen and the described testing sample that contains antioxidant is carried out quantitative test obtain its volt-ampere peak heights value, the described linear model of substitution is by calculating the content of the antioxidant in the testing sample.
6. the assay method of oxidation preventive content in the jet fuel as claimed in claim 3 is characterized in that: at first prepare the serial standard specimen and the blank sample of antioxidant described in the jet fuel, then it is extracted successively; Utilize electrochemical analyser to adopt the differentiated pulse voltammetry under described condition determination, it to be carried out electrochemical analysis one by one again, obtain the characteristic differentiation pulse volt-ampere characteristic of described antioxidant series standard specimen; Write down in its family curve-0.05V～+ the feature volt-ampere peak heights value in 0.1V interval, and related with the corresponding concentration of described antioxidant series standard specimen, obtain its linear model; The repetition process identical with the electrochemical analysis of described antioxidant series standard specimen carried out quantitative test to the described testing sample that contains antioxidant and obtained its feature volt-ampere peak heights value, the described linear model of substitution is by calculating the content of antioxidant in the described testing sample.
7. the assay method of oxidation preventive content in the jet fuel as claimed in claim 5 is characterized in that: described antioxidant is 2,6 ditertiary butyl p cresol, 2,6 di t butyl phenol, 2, the 4-DI-tert-butylphenol compounds or the 6-tert-butyl group-2,4-xylenol; The content of described antioxidant is in the 15mg/L-30mg/L scope.
8. the assay method of oxidation preventive content in the jet fuel as claimed in claim 6 is characterized in that: described antioxidant is 2,6 ditertiary butyl p cresol, 2,6 di t butyl phenol, 2, the 4-DI-tert-butylphenol compounds or the 6-tert-butyl group-2,4-xylenol; The content of described antioxidant is in the 10mg/L-30mg/L scope.
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| CNB2005100912361A CN100405055C (en) | 2005-03-30 | 2005-08-11 | Method for detecting oxidation preventive content in jet fuel |
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| CN102288694B (en) * | 2011-07-04 | 2015-04-01 | 北京泰克美高新技术有限公司 | Device and method for detecting readily oxidizable substances |
| CN102504894B (en) * | 2011-11-21 | 2014-10-08 | 中国人民解放军空军油料研究所 | Additive with high heat stability for jet fuels |
| CN103940889B (en) * | 2014-02-18 | 2016-05-25 | 广西电网公司电力科学研究院 | Utilize the conventional pulse voltammetry of difference to detect the method for Antioxygen Content in Transformer Oil |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4744870A (en) * | 1986-12-23 | 1988-05-17 | University Of Dayton | Method for evaluating the remaining useful life of a lubricant |
| US4764258A (en) * | 1986-12-23 | 1988-08-16 | University Of Dayton | Method for evaluating the remaining useful life of a hydrocarbon oil |
| US5071527A (en) * | 1990-06-29 | 1991-12-10 | University Of Dayton | Complete oil analysis technique |
| CN1335493A (en) * | 2000-07-20 | 2002-02-13 | 广东省电力工业局试验研究所 | Measuring liquid formulation for antioxidant content in oil for electrical power equipment and fast measurement method |
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- 2005-08-11 CN CNB2005100912361A patent/CN100405055C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4744870A (en) * | 1986-12-23 | 1988-05-17 | University Of Dayton | Method for evaluating the remaining useful life of a lubricant |
| US4764258A (en) * | 1986-12-23 | 1988-08-16 | University Of Dayton | Method for evaluating the remaining useful life of a hydrocarbon oil |
| US5071527A (en) * | 1990-06-29 | 1991-12-10 | University Of Dayton | Complete oil analysis technique |
| CN1335493A (en) * | 2000-07-20 | 2002-02-13 | 广东省电力工业局试验研究所 | Measuring liquid formulation for antioxidant content in oil for electrical power equipment and fast measurement method |
Non-Patent Citations (6)
| Title |
|---|
| Rapid, Portable Voltammetric Techniques for PerformingAntioxidant, Total Acid number(TAN) and Total BaseNumber(TBN) Measurements. R E Kauffman et al.Lubrication Engineering,Vol.54 No.1. 1998 |
| Rapid, Portable Voltammetric Techniques for PerformingAntioxidant, Total Acid number(TAN) and Total BaseNumber(TBN) Measurements. R E Kauffman et al.Lubrication Engineering,Vol.54 No.1. 1998 * |
| Voltammetric Determination of theAntioxidantTert-Butylhydroxytolune(BHT) at a Carbon PasteEectrodeModified with Nickle Phthalocyanine. M.Asuncion Ruiz,et al.Electroanalysis,Vol.6 No.5/6. 1994 |
| Voltammetric Determination of theAntioxidantTert-Butylhydroxytolune(BHT) at a Carbon PasteEectrodeModified with Nickle Phthalocyanine. M.Asuncion Ruiz,et al.Electroanalysis,Vol.6 No.5/6. 1994 * |
| 润滑油抗氧剂含量的循环伏安法测定. 史永刚，王德岩，马彦.润滑与密封，第3/163期. 2004 |
| 润滑油抗氧剂含量的循环伏安法测定. 史永刚，王德岩，马彦.润滑与密封，第3/163期. 2004 * |
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