CN112986175A - Method for rapidly detecting adulteration of melamine tableware by utilizing infrared spectrum - Google Patents
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- 229920000877 Melamine resin Polymers 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 29
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002329 infrared spectrum Methods 0.000 title claims abstract description 13
- 229920001807 Urea-formaldehyde Polymers 0.000 claims abstract description 41
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 claims abstract description 38
- 239000004640 Melamine resin Substances 0.000 claims abstract description 33
- HANVTCGOAROXMV-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine;urea Chemical compound O=C.NC(N)=O.NC1=NC(N)=NC(N)=N1 HANVTCGOAROXMV-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000000465 moulding Methods 0.000 claims abstract description 24
- 238000004458 analytical method Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000001514 detection method Methods 0.000 claims abstract description 6
- 238000012937 correction Methods 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 11
- 238000004566 IR spectroscopy Methods 0.000 claims description 8
- 238000001228 spectrum Methods 0.000 claims description 8
- 238000004364 calculation method Methods 0.000 claims description 6
- 238000012795 verification Methods 0.000 claims description 6
- 238000010586 diagram Methods 0.000 claims description 4
- 238000002790 cross-validation Methods 0.000 claims description 3
- 230000003595 spectral effect Effects 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 238000007781 pre-processing Methods 0.000 abstract description 10
- 235000003166 Opuntia robusta Nutrition 0.000 abstract description 7
- 244000218514 Opuntia robusta Species 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005102 attenuated total reflection Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004451 qualitative analysis Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000010239 partial least squares discriminant analysis Methods 0.000 description 1
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012764 semi-quantitative analysis Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
- G01N2021/3572—Preparation of samples, e.g. salt matrices
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Abstract
The invention discloses a method for rapidly detecting adulteration of melamine tableware by utilizing infrared spectrum, which comprises the steps of manufacturing a standard melamine resin dinner plate, a urea-formaldehyde resin dinner plate and a melamine urea-formaldehyde blending molding dinner plate, carrying out infrared spectrum detection on the dinner plate to obtain an infrared spectrogram, carrying out data preprocessing on the infrared spectrogram by using a multivariate scattering correction data preprocessing mode, respectively establishing a qualitative model and a quantitative model by adopting an orthogonal partial least square method-discriminant analysis method and a partial least square method, checking the models, and finally introducing the infrared spectrogram of the tableware to be detected to obtain an analysis report of the tableware to be detected. The method utilizes the model to identify the samples purchased in the market and the adulterated samples, has simple operation and reliable technology, and can realize nondestructive, quick and direct judgment of whether the melamine tableware is adulterated or not.
Description
Technical Field
The invention relates to the technical field of detection, in particular to a method for rapidly detecting adulteration of melamine tableware by utilizing infrared spectrum.
Background
Melamine tableware is produced by compression molding melamine-formaldehyde resin as base material and alpha cellulose as stuffing melamine molding powder as material, and is widely used in daily life. The melamine tableware has the defects of stain resistance, humidity resistance and formaldehyde and melamine migration in the quality and safety indexes of melamine tableware. Some melamine dishware mixed with urea-formaldehyde resin in the market is easy to cause the quality safety problem, and especially, excessive formaldehyde migration is an important index influencing the use safety of the dishware.
The adulteration of melamine tableware is mainly classified into three types: the first type is urea-formaldehyde resin molded articles; the second type is urea-formaldehyde resin surface melamine-coated molded products; melamine and urea formaldehyde blend moldings of the third type. At present, the domestic research on melamine tableware mainly focuses on material identification, particularly distinguishing urea resin molded products. The main methods are nuclear magnetic resonance, infrared spectroscopy, thermogravimetry and thermogravimetry-mass spectrometry.
At present, infrared spectroscopy mainly utilizes two types of KBr tabletting technology and attenuated total reflection technology, and the attenuated total reflection method is superior to the KBr tabletting method in the aspect of pretreatment of a sample. The infrared spectroscopy is used by Sunweber, Changxiao, Gaoxia and the like to identify the material quality and adulteration of melamine tableware, and whether the urea-formaldehyde resin is doped into the melamine tableware can be judged by directly observing the infrared spectrogram and analyzing the infrared spectrogram, but the blending molding dinner plate with the addition amount of the urea-formaldehyde resin being below 30 percent cannot be distinguished.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for rapidly detecting adulteration of melamine tableware by utilizing infrared spectroscopy, which solves the problem that the blending molding dinner plate with the urea-formaldehyde resin addition amount of less than 30 percent cannot be distinguished in the prior art.
(II) technical scheme
In order to achieve the purpose, the invention adopts the following specific technical scheme:
a method for rapidly detecting adulteration of melamine tableware by utilizing infrared spectroscopy comprises the following steps:
(1) preparing tableware: manufacturing standard melamine resin tableware, urea-formaldehyde resin tableware and melamine urea-formaldehyde blended molding tableware;
(2) detecting a spectrum: detecting the infrared spectrogram of the manufactured standard melamine resin tableware, urea-formaldehyde resin tableware and melamine urea-formaldehyde blended molding tableware;
(3) establishing a model: introducing the obtained infrared spectrogram of standard melamine resin tableware, urea-formaldehyde resin tableware and melamine urea-formaldehyde blend molding tableware into TQ analysis spectral analysis software, randomly selecting 75% of the infrared spectrogram as a correction set to establish a model, and using the remaining 25% of the infrared spectrogram as a verification set to verify the stability of the model;
(4) qualitative modeling: establishing a model file in TQ analysis spectral analysis software, selecting DA as a modeling function, respectively defining the names of standard melamine resin tableware, urea-formaldehyde resin tableware and melamine urea-formaldehyde blend molding tableware, and establishing a qualitative model of the infrared spectrogram through DA to obtain a calculation result and a classification distribution diagram;
(5) quantitative modeling: establishing a model file in TQ analysis spectral analysis software, selecting PLS as a modeling algorithm, selecting a constant light path, respectively defining the names of standard melamine resin tableware, urea-formaldehyde resin tableware and melamine urea-formaldehyde blend molding tableware, carrying out feasibility test, adding the infrared spectrogram, carrying out spectrum pretreatment by using MSC, selecting a spectrum range, and storing a quantitative model to obtain a calculation result of the quantitative model;
(6) detection and identification: the method comprises the steps of obtaining an infrared spectrogram of unknown tableware to be tested, opening a built qualitative model or quantitative model in TQ analysis spectral analysis software, selecting and introducing one or more infrared spectrograms of the tableware to be tested by using Multiple Quantify options in a Diagnostics menu to obtain an analysis report of the tableware to be tested, wherein in the qualitative identification, the infrared spectrogram of the tableware to be tested falls on the side surface of a PC3 axis and is unadulterated standard melamine resin tableware, the infrared spectrogram falls on the side surface of a PC1 axis and is urea-formaldehyde resin tableware, and the infrared spectrogram falls in the middle of the two side surfaces and is melamine-urea-formaldehyde blending molding tableware.
Preferably, in the step (1), the melamine urea formaldehyde blended molded tableware is prepared by mixing the following components in a mass ratio of melamine resin to urea formaldehyde resin: 1:9, 2:8, 3:7, 4:6, 5:5, 6:5, 7:3, 8:2, 9: 1.
Preferably, the step (4) introduces the infrared spectrogram of the tableware concentrated by the verification in the step (3) into a qualitative model to obtain a prediction classification, and compares the prediction classification with an actual classification to calculate the accuracy.
Preferably, the spectral range in the step (5) is 600-4000 cm-1。
Preferably, step (5) utilizes a cross-validation method to validate the quantitative model, and the correlation coefficient R and the prediction mean square error RMSEP between the NIR predicted value and the actual value of the tableware in the validation set in step (3) are used for evaluating the performance of the quantitative model.
(III) advantageous effects
The invention provides a method for rapidly detecting adulteration of melamine tableware by utilizing infrared spectroscopy. The method has the following beneficial effects:
(1) urea-formaldehyde resin powder and melamine resin powder are collected, urea-formaldehyde resin powder with different proportions (10 percent, 20 percent to 90 percent) is added into the melamine resin powder, the mixture is processed into a finished tableware product, and infrared spectrum detection is carried out by using a melamine-urea-formaldehyde blending model dinner plate to obtain an infrared spectrogram.
(2) The invention carries out data preprocessing on the original spectrogram through more than ten data preprocessing modes such as Multivariate Scattering Correction (MSC), Standard Normal Variation (SNV) and combination thereof, and finds that the MSC has the best data preprocessing effect.
(3) The invention adopts an orthogonal partial least squares-discriminant analysis (OPLS-DA) method and a partial least squares method (PLS) method to establish a qualitative model and a quantitative model, and verifies the models. And finally, identifying the market purchase sample and the adulteration sample by using a model, wherein when the adulteration amount reaches more than 10%, the identification accuracy rate reaches 100%. The method is simple to operate and reliable in technology, and can realize nondestructive, rapid and direct judgment of whether the melamine tableware is adulterated or not.
Drawings
FIG. 1 is a classification distribution diagram of qualitative models of infrared spectra of standard melamine resin tableware (A5), urea formaldehyde resin tableware (A1) and melamine urea formaldehyde blend molded tableware (A1-A5) according to the present invention;
FIG. 2 is a graph for evaluating the performance of quantitative models of infrared spectra of standard melamine resin tableware (A5), urea resin tableware (A1) and melamine urea formaldehyde blend molded tableware (A1-A5) according to the present invention
Detailed Description
For further understanding of the present invention, the following examples are provided to illustrate a method for rapidly detecting adulteration of melamine tableware by using infrared spectroscopy, and the scope of the present invention is not limited by the following examples.
Example 1:
(1) preparing tableware: the urea-formaldehyde resin powder and the melamine resin powder are used for manufacturing standard melamine resin tableware (A5), urea-formaldehyde resin tableware (A1) and melamine urea-formaldehyde blend molding tableware (A1-A5). Wherein, the melamine urea formaldehyde blending molding tableware (A1-A5) is manufactured according to the mass ratio of melamine resin to urea formaldehyde resin of 1:9, 2:8, 3:7, 4:6, 5:5, 6:5, 7:3, 8:2 and 9: 1.
(2) Detecting a spectrum: the infrared spectra of standard melamine resin tableware (A5), urea-formaldehyde resin tableware (A1) and melamine urea-formaldehyde blend molded tableware (A1-A5) were examined.
(3) Establishing a model: and (3) importing the obtained infrared spectrograms of the standard melamine resin tableware (A5), urea-formaldehyde resin tableware (A1) and melamine urea-formaldehyde blend molding tableware (A1-A5) into TQ analysis spectral analysis software, randomly selecting 75% of the infrared spectrograms of the three types of tableware as a correction set to establish a model, and using the remaining 25% of the infrared spectrograms of the three types of tableware as a verification set to verify the stability of the model.
Example 2:
qualitative modeling:
(1) a model file is established in TQ analysis spectral analysis software, DA is selected as a modeling function, names of standard melamine resin tableware, urea-formaldehyde resin tableware and melamine urea-formaldehyde blend molding tableware are respectively defined, a qualitative model of infrared spectrograms of the standard melamine resin tableware, urea-formaldehyde resin tableware and melamine urea-formaldehyde blend molding tableware is established through the DA, a calculation result and a classification distribution diagram are obtained, and as shown in figure 1, the infrared spectrograms of three types of tableware are well separated and basically have no overlap.
In FIG. 1, the tableware placed on one side with the PC3 axis was unadulterated standard melamine resin tableware, the tableware placed on one side with the PC1 axis was urea-formaldehyde resin tableware, and the tableware placed in the middle of both sides was melamine urea-formaldehyde blend molded tableware.
(2) And (3) introducing the infrared spectrogram of the tableware with three concentrated verification classes into a qualitative model to obtain a prediction classification, comparing the prediction classification with an actual class, and calculating the accuracy, wherein the result shows that the identification accuracy of the established DA qualitative model can reach 100 percent as shown in Table 1.
Table 1: accuracy rate of qualitative analysis model identification obtained by preprocessing different data
Example 3:
quantitative modeling:
(1) establishing a model file in TQ analysis spectral analysis software, selecting PLS as a modeling algorithm, selecting a constant light path, respectively defining the names of standard melamine resin tableware, urea-formaldehyde resin tableware and melamine urea-formaldehyde blended molded tableware, carrying out feasibility test, adding infrared spectrograms of three types of tableware, carrying out spectrum pretreatment by using MSC, selecting 600-4000 cm-1And (5) in the spectral range, storing the quantitative model and obtaining a calculation result of the quantitative model.
(2) And verifying the quantitative model by using a cross-validation method, and evaluating the performance of the quantitative model by verifying the correlation coefficient R and the prediction mean square error RMSEP between the NIR predicted value and the actual value of the infrared spectrogram of the concentrated three types of tableware, as shown in Table 2.
Table 2: accuracy rate of semi-quantitative analysis model identification obtained by preprocessing different data
Example 4:
identifying and detecting unknown tableware to be detected:
(1) the method comprises the steps of obtaining an infrared spectrogram of unknown tableware to be tested, opening a built qualitative model in TQ analysis spectral analysis software, selecting and introducing one or more infrared spectrograms of the tableware to be tested by using Multiple Quantify options in a Diagnostics menu to obtain a qualitative analysis report of the tableware to be tested, wherein the infrared spectrogram of the tableware to be tested falls on the side surface of a PC3 axis and is unadulterated standard melamine resin tableware, the infrared spectrogram of the tableware falls on the side surface of a PC1 axis and is urea-formaldehyde resin tableware, and the infrared spectrogram of the tableware falls in the middle of the two side surfaces and is melamine urea-formaldehyde blending molding tableware.
(2) And obtaining an infrared spectrogram of unknown tableware to be detected, opening a built quantitative model in TQ analysis spectral analysis software, and selectively importing the infrared spectrogram of one or more tableware to be detected by using Multiple Quantify options in a Diagnostics menu to obtain a quantitative analysis report of the tableware to be detected.
In conclusion, the method uses urea-formaldehyde resin powder and melamine resin powder to manufacture standard melamine resin tableware, urea-formaldehyde resin tableware and melamine urea-formaldehyde blending molding tableware and carries out infrared spectrum detection to obtain an infrared spectrogram; then, data preprocessing is carried out on the original infrared spectrogram through more than ten data preprocessing modes such as MSC, SNV and combination thereof, and the MSC finds that the data preprocessing effect is optimal; then, establishing a qualitative model and a quantitative model by adopting OPLS-DA and PLS, and verifying the models; and finally, identifying the tableware to be detected purchased in the market by using the model, wherein when the adulteration amount reaches over 10 percent, the identification accuracy rate reaches 100 percent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A method for rapidly detecting adulteration of melamine tableware by utilizing infrared spectrum is characterized by comprising the following steps:
(1) preparing tableware: the urea-formaldehyde resin powder and the melamine resin powder are used for manufacturing standard melamine resin tableware, urea-formaldehyde resin tableware and melamine urea-formaldehyde blending molding tableware;
(2) detecting a spectrum: detecting the infrared spectrogram of the manufactured standard melamine resin tableware, urea-formaldehyde resin tableware and melamine urea-formaldehyde blended molding tableware;
(3) establishing a model: introducing the obtained infrared spectrogram of standard melamine resin tableware, urea-formaldehyde resin tableware and melamine urea-formaldehyde blend molding tableware into TQ analysis spectral analysis software, randomly selecting 75% of the infrared spectrogram as a correction set to establish a model, and using the remaining 25% of the infrared spectrogram as a verification set to verify the stability of the model;
(4) qualitative modeling: establishing a model file in TQ analysis spectral analysis software, selecting DA as a modeling function, respectively defining the names of standard melamine resin tableware, urea-formaldehyde resin tableware and melamine urea-formaldehyde blend molding tableware, and establishing a qualitative model of the infrared spectrogram through DA to obtain a calculation result and a classification distribution diagram;
(5) quantitative modeling: establishing a model file in TQ analysis spectral analysis software, selecting PLS as a modeling algorithm, selecting a constant light path, respectively defining the names of standard melamine resin tableware, urea-formaldehyde resin tableware and melamine urea-formaldehyde blend molding tableware, carrying out feasibility test, adding the infrared spectrogram, carrying out spectrum pretreatment by using MSC, selecting a spectrum range, and storing a quantitative model to obtain a calculation result of the quantitative model;
(6) detection and identification: acquiring an infrared spectrogram of unknown tableware to be detected, opening a built qualitative model or quantitative model in TQ analysis spectral analysis software, and selectively importing the infrared spectrogram of one or more tableware to be detected by using Multiple Quantify options in a Diagnostics menu to obtain an analysis report of the tableware to be detected; in the qualitative identification, the infrared spectrogram of the tableware to be detected falls on the side surface of the PC3 axis and is the unadulterated standard melamine resin tableware, the infrared spectrogram of the tableware falls on the side surface of the PC1 axis and is the urea-formaldehyde resin tableware, and the infrared spectrogram of the tableware falls in the middle of the two side surfaces and is the melamine-urea-formaldehyde blending molding tableware.
2. The method for rapidly detecting adulteration of melamine tableware by using infrared spectrum as claimed in claim 1, wherein in the step (1), the melamine urea formaldehyde blended molded tableware is prepared by mixing melamine resin and urea formaldehyde resin according to the mass ratio of melamine resin to urea formaldehyde resin: 1:9, 2:8, 3:7, 4:6, 5:5, 6:5, 7:3, 8:2, 9: 1.
3. The method as claimed in claim 1, wherein the step (4) of introducing the infrared spectrogram of the tableware collected in the step (3) into the qualitative model to obtain the predicted classification, and comparing the predicted classification with the actual classification to calculate the accuracy.
4. The method for rapidly detecting adulteration of melamine tableware by using infrared spectrum as claimed in claim 1, wherein the spectral range in the step (5) is 600-4000 cm-1。
5. The method for rapidly detecting adulteration of melamine tableware by using infrared spectroscopy as claimed in claim 1, wherein the step (5) is to verify the quantitative model by using a cross-validation method, and the correlation coefficient R and the prediction mean square error RMSEP between the NIR predicted values and the actual values of the tableware in the verification set in the step (3) are used for evaluating the performance of the quantitative model.
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