KR20160119613A - Method and apparatus for analyzing oil type and mixing ratio in using Unresolved Complex Mixture of gas chromatography - Google Patents
Method and apparatus for analyzing oil type and mixing ratio in using Unresolved Complex Mixture of gas chromatography Download PDFInfo
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- 238000002156 mixing Methods 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 38
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- 239000012491 analyte Substances 0.000 claims abstract description 13
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 13
- 238000004458 analytical method Methods 0.000 claims description 35
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000003344 environmental pollutant Substances 0.000 abstract description 16
- 231100000719 pollutant Toxicity 0.000 abstract description 16
- 239000003921 oil Substances 0.000 description 81
- 239000003350 kerosene Substances 0.000 description 21
- 239000007789 gas Substances 0.000 description 9
- 230000007613 environmental effect Effects 0.000 description 4
- 239000010687 lubricating oil Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- 238000009614 chemical analysis method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
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- 150000002430 hydrocarbons Chemical class 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
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Abstract
The present invention relates to a method and apparatus for analyzing mixed pollutants by gas chromatography using mixed chromatographic UCM information of gas chromatography, The present invention relates to a method and an apparatus for analyzing mixing ratios of a mixed oil using UCM information of gas chromatography according to the present invention, Gas chromatographic analysis was carried out to obtain a standard sample UCM, and the area ratio of each standard UCM constituting standard sample UCM and the area ratio between standard UCM were calculated, and the ratio of standard UCM to standard UCM according to the mixture ratio Calculating; A gas chromatographic analysis is performed on a sample to be analyzed which contains a plurality of analyte species to be analyzed to obtain a sample UCM to be analyzed and an area of each analyzing UCM constituting the sample UCM to be analyzed and an area between the analyzing UCM Area ratio > Determining a ratio of the UCM area ratio between the species to be analyzed and the UCM area ratio among the species to be analyzed in comparison with the ratio of the UCM area ratio between the species to be analyzed and the standard UCM area ratio according to the species mixing ratio. .
Description
The present invention relates to a method and an apparatus for analyzing mixing ratios of mixed oil using UCM information of gas chromatography. More particularly, the present invention relates to a method and apparatus for analyzing oil contamination mixed with a plurality of oil species using gas chromatography, The present invention relates to a method and an apparatus for analyzing mixing ratios and mixing ratios of mixed oil using UCM information of gas chromatography, which can confirm mixing ratios of oil species and oil species through UCM information of grams.
Oil pollutants leaking into the environmental system are likely to lose initial physical properties (eg, chromaticity), so chemical analysis techniques should be applied to determine the type.
Gas chromatography (GC) analysis is typically used to analyze oil pollutants leaking into the environment. Gas chromatography separates a sample into components by vaporizing the sample through a column, converts each separated component into an electrical signal (peak), and measures the measured peak in comparison with a standard peak (GC peak pattern) It is a method to analyze each component contained. An example of gas chromatographic analysis is disclosed in Korean Patent Application No. 1997-0011902. However, in the case of oil pollutants exposed to the environment for a long period of time, they do not show inherent peak values due to loss of properties, and therefore effective gas chromatography analysis is not performed.
On the other hand, it is possible to identify various types of compounds composing the sample to be analyzed through gas chromatography analysis. However, since it is composed of thousands of compounds in the case of oils, some compounds can not be analyzed by gas chromatography Do. Among the gas chromatographic analysis results, these unidentified substances are referred to as UCM (unresolved complex mixture) (see FIG. 1). The UCM obtained from the gas chromatographic analysis is relatively unaffected by the weathering time and environmental exposure time of the sample to be analyzed, and there is little change in the chromatogram. That is, a peak indicating a specific species on a chromatogram is influenced by environmental conditions (time, weathering, etc.) and its shape is changed. However, UCM is not influenced by environmental conditions and forms a certain shape. Each material has a unique UCM shape, and the UCM of each material remains constant regardless of the exposed environmental conditions.
Recently, UCM is being studied for the analysis of oil pollutants. However, UCM of each material is comparable to the UCM of the sample to be analyzed, as in the conventional gas chromatographic analysis.
DISCLOSURE Technical Problem The present invention has been devised to solve the above problems and it is an object of the present invention to provide a method and apparatus for analyzing oil pollutants mixed with a plurality of oil species using gas chromatography, The present invention relates to a method and an apparatus for analyzing mixing ratios and mixing ratios of mixed oil using UCM information of gas chromatography.
In order to accomplish the above object, the present invention provides a method for analyzing mixing ratio and mixing ratio of mixed oil using UCM information of gas chromatography according to the present invention, in which a plurality of standard specimens are mixed at a specific mixing ratio, Obtaining standard sample UCM, calculating the area ratio of each standard UCM constituting the standard sample UCM and the area ratio between the standard UCM and the standard UCM, and calculating the standard UCM area ratio according to the mixing ratio of the species; A gas chromatographic analysis is performed on a sample to be analyzed which contains a plurality of analyte species to be analyzed to obtain a sample UCM to be analyzed and an area of each analyzing UCM constituting the sample UCM to be analyzed and an area between the analyzing UCM Area ratio > Determining a ratio of the UCM area ratio between the species to be analyzed and the UCM area ratio among the species to be analyzed in comparison with the ratio of the UCM area ratio between the species to be analyzed and the standard UCM area ratio according to the species mixing ratio. .
The step of calculating the standard UCM area ratio according to the mixing ratio of the oil species may include a process of generating a standard sample UCM by performing gas chromatography analysis on a standard sample in which a plurality of standard oil types are mixed at a specific mixing ratio, , Generating standardized graphs for each standard UCM by assigning the two-dimensional coordinates near the maximum intensity point shown in the standard sample UCM to the Gaussian function, and generating a standard graph for each standard UCM, Calculating the area ratio, and calculating the standard UCM area ratio according to the mixing ratio of the species.
The step of calculating the area ratio between the types of UCMs to be analyzed includes the steps of performing gas chromatography analysis on an analysis sample mixed with a plurality of analysis target species to generate a sample UCM to be analyzed, A step of assigning a two-dimensional coordinate near each maximum intensity point on the UCM to a Gaussian function to generate a graph to be analyzed with respect to each of the analyzed UCMs to be analyzed; And calculating the area ratio between the two areas.
Before calculating the area ratio between the analyzed UCMs to be analyzed, the process of determining the type of analyte to be analyzed constituting the sample to be analyzed is compared with the maximum intensity point in time of the UCM analyzing target UCM and the maximum intensity point of the standard UCM And the like.
The apparatus for analyzing mixing ratio of mixed oil using UCM information of gas chromatography according to the present invention comprises a DB block for storing standard UCM information and standard UCM area ratio information; (UCM) for each analytical target species constituting the sample to be analyzed is generated by extracting the two-dimensional coordinates of the UCM to be analyzed and substituting the two-dimensional coordinates of the UCM to be analyzed into the Gaussian function, A Gaussian function conversion module for calculating an area ratio between target UCMs; The area ratio between the analysis target UCMs generated by the Gaussian function conversion module is matched with the area ratio information between the standard UCMs according to the mixing ratio of the standard species stored in the DB block, A matching module for determining a blending ratio of the analyte to be analyzed; The Gaussian function conversion module and the matching module are controlled to store the standard UCM information and the standard UCM area ratio information, to convert the analysis target sample into the Gaussian function graph, to determine analysis target species constituting the analysis target sample, And a dissimilar analysis server control device for controlling the determination of the mixing ratio of the analysis target species constituting the sample.
In addition, the matching module determines the type of analyzer to be analyzed by comparing the maximum intensity point of time of the analyzing target UCM generated by the Gaussian function converting module with the maximum intensity point of time of the standard UCM stored in the DB block .
The DB block is composed of a standard UCM DB and a standard UCM area ratio DB. The standard UCM DB stores all kinds of UCM information. The UCM information includes maximum strength point and maximum width information The standard UCM area ratio DB stores the area ratio between the standard UCM and the standard UCM according to the mixing ratio of the standard samples mixed with different standard types.
The method and apparatus for analyzing mixing ratio of mixed oil using UCM information of gas chromatography according to the present invention have the following effects.
For the oil pollutants mixed with plural kinds of oil pollutants, the UCM of oil pollutants and the UCM of each kind constituting the oil pollutants are secured, and the area ratio of UCM of each oil type is set to < standard It is possible to easily measure the mixing ratio of each oil species constituting the oil pollutant by comparing the area ratio of the UCM with the oil species.
1 is a reference view showing an example of a chromatogram including UCM.
FIG. 2 is a flow chart for explaining a method of analyzing mixing ratios of mixed oil using UCM information of gas chromatography according to an embodiment of the present invention.
FIG. 3 is a block diagram of an apparatus for analyzing mixing ratio of mixed oil using UCM information of gas chromatography according to an embodiment of the present invention. FIG.
Fig. 4 shows a standard sample UCM and a standard UCM when kerosene and diesel are mixed at a ratio of 4: 1.
FIG. 5 shows a standard sample UCM and a standard UCM when kerosene and diesel are mixed at 2: 1, 1: 1, 1: 4, and 1: 9, respectively.
6 shows a standard sample UCM and a standard UCM when kerosene and lubricant are mixed at 9: 1, 4: 1, 1: 1, 1: 4, and 1: 9, respectively.
FIG. 7 shows a standard sample UCM and a standard UCM when the light oil and the lubricating oil are mixed at 9: 1, 4: 1, 1: 1, 1: 2 and 1: 4, respectively.
FIG. 8A shows the area ratio between UCMs of each standard type (light oil and kerosene) according to the mixing ratio of the standard oil based on the result of FIG.
FIG. 8B shows the area ratio between each standard oil (lubricating oil and light oil) UCM according to the mixing ratio of standard oil based on the result of FIG. 6.
FIG. 8C shows the area ratio between each standard oil (light oil and lubricating oil) UCM according to the mixing ratio of standard oil based on the result of FIG.
The present invention provides a technique for checking the mixing ratio of a plurality of oil species and oil species contained in oil pollutants by using UCM (unresolved complex mixture) information of a chromatogram.
In the gas chromatographic analysis, the sample to be analyzed is separated into individual components in a separation column, and each separated component is converted into an electrical signal (peak) at a detector. At this time, the electric signal (peak) for each component is continuously generated with time, and each component is represented by a peak change over time. The change in peak of each component with time is usually referred to as a chromatogram.
An unresolved complex mixture (UCM) refers to a hump-shaped or bell-shaped region located at the bottom of a peak on a chromatogram showing the peak change over time of each component. UCM is an aggregate of organic compounds that are not peptized into peaks that can be analyzed by gas chromatographic analysis. For example, the UCM type of kerosene differs from the UCM type of diesel. Depending on the sample to be analyzed, UCM may not be present, but in the case of oils consisting of thousands of hydrocarbon compounds, most UCMs exist in gas chromatographic analysis.
The UCM having a unique shape according to the type of oil can be converted into a Gaussian function graph, and the maximum intensity point and the maximum intensity can be specified through the converted Gaussian function graph. That is, each UCM has its own maximum intensity time point and maximum width. Here, the maximum intensity viewpoint refers to the time point at which the UCM shows the maximum intensity on the chromatogram, and the maximum width means the maximum width of the UCM.
When the oil pollutants are composed of a single oil species, the discrimination process for the corresponding oil species is relatively easy as the oil species having the maximum maximum intensity time point and maximum specific intensity. The comparison of the UCM (maximum intensity point and maximum width) and the UCM (maximum intensity point and maximum width) of the sample to be analyzed can determine the species of the sample to be analyzed.
On the other hand, when the oil pollutants are composed of a plurality of oil types, the UCM does not form a symmetrical shape but has a number of peaks corresponding to the number of oil species. That is, the UCM of the oil contamination mixed with the plurality of types of oil is overlapped with the UCM of each oil species, and each peak means the maximum intensity point in each UCM of each kind.
When the oil pollutants are composed of a plurality of oil species, the maximum intensity time point of each oil species is not changed, but the maximum width of each oil species is variable according to the mixing ratio of oil species. Therefore, when the oil pollutant to be analyzed is composed of a plurality of oil species, a plurality of peaks (maximum intensity point) are shown in the corresponding UCM, and a point where each peak is located The UCM can determine the type of each species included in the corresponding UCM.
The present invention provides a technique for determining the mixing ratio of a plurality of oil species in addition to discriminating the oil species contained in the sample to be analyzed when the sample to be analyzed is composed of a plurality of oil types. The blending ratio of the plural kinds of oil species can be confirmed by the ratio of the area formed by each kind of UCM. That is, the mixing ratio of the oil species has a correlation with the area ratio of each kind of UCM.
In the standardized area ratio of each kind of UCM according to the mixture ratio of the species, the plurality of species are identified through the UCM of the sample to be analyzed, the area ratio of each kind of UCM is calculated, and the area ratio Is compared with the area ratio of each standardized UCM, it is possible to confirm the mixing ratio of the species contained in the sample to be analyzed.
Hereinafter, a method and an apparatus for analyzing mixing ratio and mixture ratio of mixed oil using UCM information of gas chromatography according to an embodiment of the present invention will be described in detail with reference to the drawings.
First, standard area ratio of standard UCM according to the mixing ratio of oil species is standardized.
Specifically, as shown in FIG. 2, a standard specimen is prepared by mixing different kinds of pure specimens (hereinafter referred to as "standard specimens") at a predetermined ratio (S201), and a gas chromatographic analysis To generate a chromatogram for the standard sample, and a UCM on the standard sample chromatogram, that is, a standard sample UCM is secured (S202).
Next, the standard sample UCM is converted into a Gaussian function graph.
As described above, the UCM of a single type of UCM forms a bilateral symmetrical bell, but the UCM of a mixture of a plurality of types of the same kind of standard sample has a number of peaks corresponding to the number of the species.
The conversion of the standard sample UCM into the Gaussian function graph proceeds as follows. The standard sample UCM is expressed in two-dimensional coordinates of time (x-axis) and intensity (y-axis). A Gaussian function graph (hereinafter referred to as a "standard type graph") for each standard type constituting the standard sample is substituted for the two-dimensional coordinates near each peak (maximum strength point) into the Gaussian function (S203). The standard graph is the UCM for each standard type that constitutes the standard sample.
(expression)
(x is the time of UCM, y is the intensity of UCM, y 0 is the y-axis background value of UCM, x c is the median value constant of Gaussian function graph, A is the area of UCM and w is the half width of Gaussian function graph)
Through the conversion of the standard sample UCM to the Gaussian function graph, the standard sample UCM can be divided into a plurality of standard UCMs, and each standard UCM stands for each standard standard graph.
In this state, an area value of each standard UCM constituting the standard sample UCM is integrated and calculated, and an area ratio of each standard UCM is calculated (S204).
The process of calculating the area ratio of the standard UCM according to the mixing ratio of the above-mentioned species will be described as follows. When a standard sample is composed of two standard oils (kerosene and light oil) and kerosene and light oil are mixed at a ratio of 4: 1 (volume ratio), the standard sample UCM is produced as shown in FIGS. (FIG. 4 (b) is an enlarged view of FIG. 4 (a)). Then, the two-dimensional coordinates around each peak are substituted into the Gaussian functions in the generated standard sample UCM, (See " D " in FIG. 4 (c)) of the standard UCM. Then calculate the area for each standard kerosene UCM (standard kerosene graph) and kerosene standard kerosene UCM (standard kerosene graph), and calculate the area ratio of standard kerosene UCM of kerosene and standard kerosene UCM of light oil. Through this process, it is possible to calculate the standard UCM area ratio of a standard sample mixed with kerosene and diesel at a ratio of 4: 1.
By repeating the calculation process of the area ratio of the standard UCM according to the mixing ratio of the different kinds by applying different mixing ratios, it is possible to calculate the standard UCM area ratio of the standard UCM to the standard sample of various mixing ratios. In addition, the standard ratio of standard UCM to standard UCM according to the mixing ratio of nitrogen species is calculated by applying different kinds of standard species constituting the standard sample. . ≪ / RTI > FIG. 5 shows a standard sample UCM and a standard UCM when kerosene and diesel were mixed at 2: 1, 1: 1, 1: 4 and 1: 9, 4: 1, 1: 1, 1: 4, 1: 1, 1: 4 and 1: 9, , 1: 2, and 1: 4, respectively. FIG. 8A is a graph showing the area ratio between UCM and standard UCM according to the mixing ratio of the standard oil based on the results of FIG. 5, and FIG. And FIG. 8C shows an area ratio between UCM (standard oil) and UCM (standard oil) based on the mixing ratio of standard oil based on the result of FIG. 7 . FIGS. 5 to 7 and FIGS. 8A to 8C illustrate an embodiment. It is needless to say that the area ratio of standard UCM and standard UCM can be calculated for all types of kerosene, diesel oil, lubricating oil, and the like.
Through the above procedure, the process of discriminating the species of the sample to be analyzed and the mixing ratio of the sample to be analyzed is performed in a state where the standard ratio of the standard UCM according to the mixing ratio of the seeds is normalized.
First, gas chromatography analysis is performed on the sample to be analyzed to obtain UCM (sample to be analyzed UCM) for the sample to be analyzed (S205). At this time, the analysis target sample means a mixture of a plurality of species and a plurality of peaks (maximum intensity point) exist in the sample UCM to be analyzed as a mixture of a plurality of species.
The two-dimensional coordinates of the sample UCM to be analyzed are extracted, and then the two-dimensional coordinates near each peak (maximum intensity point) are substituted into the Gaussian function to obtain a Gaussian function graph (hereinafter, Analysis object type graph) (S206). The graph to be analyzed can be said to be the UCM (UCM to be analyzed) for each analyte species constituting the sample to be analyzed.
In other words, the type of the analyzing object oil included in the analysis sample UCM is checked in comparison with the maximum intensity time point of the standard UCM (S207).
The process of confirming the blending ratio of the analyte to be analyzed is carried out while the kind of analyte constituting the sample to be analyzed is confirmed through the maximum intensity point (plural peaks) of the sample UCM to be analyzed. Specifically, the area of each kind of UCM to be analyzed constituting the sample UCM to be analyzed is calculated, and then the area ratio of each UCM to be analyzed is calculated (S208).
The area ratio of the analyzed UCM to be analyzed is compared with the area ratio of the standard UCM to determine the area ratio of the analyzed UCM to be the area ratio of the specific standard UCM within the predetermined error range, The mixing ratio of the raw materials corresponding to the area ratio of UCM is checked (S209). Through this process, it is possible to confirm the mixing ratio of the analyte species contained in the sample to be analyzed based on the area ratio of the UCM to be analyzed.
Hereinabove, the method of analyzing mixing ratio and mixture ratio of mixed oil using UCM information of gas chromatography according to one embodiment of the present invention has been described. Meanwhile, the method of analyzing mixing ratio and mixture ratio of mixed oil using UCM information of gas chromatography according to an embodiment of the present invention can be implemented as a computerized apparatus and can be implemented by the following analyzing apparatus.
Referring to FIG. 3, an apparatus for analyzing mixing ratio of mixed oil using UCM information of gas chromatography according to an embodiment of the present invention includes a
The
The Gaussian
The
The dissimilarity analysis
310: Variety analysis server control device 320: Gaussian function conversion module
330: matching module 340: DB block
341: Standard UCM DB 342: Standard UCM area ratio DB
350: interface module 360: client
Claims (7)
A gas chromatographic analysis is performed on a sample to be analyzed which contains a plurality of analyte species to be analyzed to obtain a sample UCM to be analyzed and an area of each analyzing UCM constituting the sample UCM to be analyzed and an area between the analyzing UCM Area ratio >
Determining a ratio of the UCM area ratio between the species to be analyzed and the UCM area ratio among the species to be analyzed in comparison with the ratio of the UCM area ratio between the species to be analyzed and the standard UCM area ratio according to the species mixing ratio. A method for analyzing mixing ratio and mixing ratio of mixed oil using UCM information of gas chromatography.
Performing a gas chromatographic analysis on a standard sample in which a plurality of standard specimens are mixed at a specific mixing ratio to produce a standard sample UCM,
Generating standardized graphs for each standard UCM by substituting the two-dimensional coordinates near each maximum intensity point on the standard sample UCM into a Gaussian function;
Calculating the area ratio between the standard UCMs of each standard UCM and the area ratio between the standard UCMs and calculating the standard UCM area ratio based on the mixing ratio of the different kinds of UCMs. A Method of Mixing Ratio Analysis of Mixed Oil.
Performing a gas chromatography analysis on a sample to be analyzed in which a plurality of analytical target species are mixed to generate a sample UCM to be analyzed,
A step of assigning a two-dimensional coordinate near each maximum intensity point on the UCM to be analyzed to a Gaussian function to generate a general graph to be analyzed for each UCM to be analyzed;
And calculating the area ratio between the analyzed UCMs and the area ratio between the analyzed UCMs to be analyzed. The method of analyzing mixing ratio of mixed oil using UCM information of gas chromatography.
Determining the type of analyte to be analyzed constituting the sample to be analyzed, in comparison with the maximum intensity point in time of the standard UCM and the maximum intensity point in time of the standard UCM, A Method of Mixing Ratio Analysis of Mixed Oil Using Information.
(UCM) for each analytical target species constituting the sample to be analyzed is generated by extracting the two-dimensional coordinates of the UCM to be analyzed and substituting the two-dimensional coordinates of the UCM to be analyzed into the Gaussian function, A Gaussian function conversion module for calculating an area ratio between target UCMs;
The area ratio between the analysis target UCMs generated by the Gaussian function conversion module is matched with the area ratio information between the standard UCMs according to the mixing ratio of the standard species stored in the DB block, A matching module for determining a blending ratio of the analyte to be analyzed;
The Gaussian function conversion module and the matching module are controlled to store the standard UCM information and the standard UCM area ratio information, to convert the analysis target sample into the Gaussian function graph, to determine analysis target species constituting the analysis target sample, And an analysis server control device for controlling the determination of the mixing ratio of the analysis target species constituting the sample. The apparatus for analyzing mixing type and mixing ratio of mixed oil using UCM information of gas chromatography.
The standard UCM DB stores all kinds of UCM information, and the UCM information includes the maximum intensity time point and the maximum width information of the standard type,
Wherein the standard UCM area ratio DB stores the area ratio between the standard UCMs according to the mixing ratio of the standard samples mixed with the different standard UCMs. Analysis device.
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CN106770796A (en) * | 2017-01-25 | 2017-05-31 | 青岛市食品药品检验研究院 | The method that static headspace-GC-MS combination determines ready-mixed oil harmonic proportion |
CN111929398A (en) * | 2019-05-13 | 2020-11-13 | 中国石油化工股份有限公司 | Method for identifying mixed source oil |
KR20200140977A (en) * | 2019-06-07 | 2020-12-17 | 켐아이넷(주) | Toxicity data processing integrated platform GC/MS and LC/MS based |
KR20220112113A (en) * | 2021-02-03 | 2022-08-10 | 한국과학기술연구원 | Method and apparatus for analyzing oil type using Unresolved Complex Mixture of gas chromatography |
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