Fluorescent anti-forgery ink luminescence effect characterization and quality control method
By using a standard solution of fluorescent corrector and a fluorescence spectrometer to detect fluorescent ink samples and construct quality control charts, the problem of accurate detection of the luminescence effect of fluorescent anti-counterfeiting inks was solved, and quantitative evaluation and stable quality control were achieved.
Patent Information
- Application Number
- CN202511771715.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-28
- Publication Date
- 2026-01-23
AI Technical Summary
Existing technologies cannot accurately detect and evaluate the fluorescence color and intensity of fluorescent anti-counterfeiting inks under ultraviolet light excitation using data-driven methods. The results are greatly affected by human factors and light intensity, leading to inaccurate test results.
Fluorescence spectroscopy was performed using a standard solution of a fluorescence corrector. Fluorescence peaks of the ink samples were corrected using a fluorescence spectrometer. A quality control chart was constructed to achieve quality control, including the preparation of color development samples and solvent dispersion samples. The fluorescence spectrum of the samples was corrected using the response value of the fluorescence corrector.
This study enabled the quantitative evaluation of the luminescence effect of fluorescent anti-counterfeiting inks, reduced the influence of human factors and light, improved the accuracy and stability of detection, and established a method suitable for quality control of fluorescence intensity.
Smart Images
Figure CN121384904A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the technical field of packaging printing material detection, and particularly relates to a fluorescent anti-counterfeiting ink light-emitting effect characterization and quality control method. BACKGROUND
[0002] As a key component of anti-counterfeiting technology, anti-counterfeiting printing ink plays an important role in the field of packaging anti-counterfeiting. Among them, fluorescent ink is prepared by adding connecting material and additives on the basis of organic fluorescent dye or rare earth metal complex pigment, and is widely used in packaging printing. The fluorescent effect of the fluorescent ink under ultraviolet excitation is crucial for product anti-counterfeiting and color effect presentation.
[0003] In terms of fluorescent anti-counterfeiting ink light-emitting effect characterization, fluorescence is photoluminescence, which is difficult to detect and analyze by color difference instrument and other equipment. At present, the fluorescent color and intensity of the fluorescent ink used in packaging under ultraviolet excitation are mainly detected by visual observation method. This method is simple and intuitive, but is greatly affected by human factors, and the detection is also seriously affected by light brightness. Therefore, it is difficult to dataize the results, which brings great difficulty to the evaluation and improvement verification of the fluorescent effect of this kind of ink.
[0004] Therefore, in order to support the analysis of such problems and consolidate the control level of raw material industry chain, it is necessary to develop a data detection method for fluorescent anti-counterfeiting ink light-emitting effect characterization, and to explore the establishment of a quality control chart to support the application of this kind of anti-counterfeiting technology. SUMMARY
[0005] In view of the above-mentioned shortcomings of the prior art, the purpose of the present application is to provide a fluorescent anti-counterfeiting ink light-emitting effect characterization and quality control method to solve the problems in the prior art.
[0006] To achieve the above-mentioned purpose and other related purposes, the present application adopts the following technical scheme:
[0007] A fluorescent anti-counterfeiting ink light-emitting effect characterization and quality control method, comprising the following steps:
[0008] 1) Preparing a fluorescent correction agent standard solution: adding a fluorescent correction agent into a solvent and then making up to volume to prepare a standard solution.
[0009] 2) Preparing a fluorescent anti-counterfeiting ink sample: coating the ink onto the surface of paper or dispersing it into a solvent to prepare a color development sample or a solvent dispersion sample.
[0010] 3) Detecting the sample: using a fluorescence spectrometer to detect and analyze the ink sample and the fluorescent correction agent standard solution respectively, correcting the fluorescence spectrum peak of the ink sample based on the response of the fluorescent correction agent, and obtaining a sample corrected spectrum graph.
[0011] 4) Constructing quality control chart: taking the fluorescence response of the series of ink samples as data points, constructing the quality control interval of the fluorescence response of the ink samples, and evaluating the quality of the subsequent to-be-tested samples.
[0012] Preferably, in step 1), the fluorescence correction agent is rhodamine B.
[0013] Preferably, in step 1), the solvent is ethanol.
[0014] Preferably, in step 1), the concentration of the fluorescence correction agent is 0.005-0.5 mg / L.
[0015] Preferably, in step 2), when preparing the color development sample, the amount of ink used is 0.1-0.125 mL.
[0016] Preferably, in step 2), when preparing the color development sample, the coated paper used is white cardboard.
[0017] More preferably, in step 2), the basis weight of the coated white cardboard used is 170-250 g / m 2 .
[0018] Preferably, in step 2), when preparing the color development sample, a color development instrument is used for coating.
[0019] More preferably, in step 2), the color development instrument corresponds to the type of ink: offset ink uses an offset color development instrument, gravure ink uses a gravure color development instrument, and screen printing ink uses a screen printing sample.
[0020] Preferably, in step 2), when preparing the color development sample, the ink is UV ink or non-UV ink; the UV ink is treated by ultraviolet light irradiation to form a dry and cured state, and the non-UV ink is naturally placed for 0.5-24 h to form a dry and cured state.
[0021] Preferably, in step 2), when preparing the solvent dispersion sample, the amount of ink used is 10-20 mg.
[0022] Preferably, in step 2), when preparing the solvent dispersion sample, the solvent used is ethyl acetate.
[0023] Preferably, in step 3), when detecting the fluorescence correction agent solution, the excitation wavelength is 540-548 nm, the emission wavelength is 550-800 nm, the excitation light slit width is 5 nm, the emission light slit width is 5-10 nm, and the PMT voltage is 500-600 V.
[0024] Preferably, in step 3), when detecting the ink color development sample, the excitation wavelength is 350-370 nm, the emission wavelength is 400-800 nm, the excitation light slit width is 5 nm, the emission light slit width is 2.5-5 nm, and the PMT voltage is 550-600 V.
[0025] Preferably, in step 3), when the ink solvent dispersion sample is detected, the excitation wavelength is 350-370 nm, the emission wavelength is 400-800 nm, the excitation light slit width is 5 nm, the emission light slit width is 5-10 nm, and the PMT voltage is 550-600 V.
[0026] Preferably, in step 3), the fluorescence response of the first fluorescence correction agent is taken as a reference value, and when the subsequent sample is measured, the fluorescence spectrum of the ink sample is corrected by taking the fluorescence correction agent response value / reference value as a coefficient.
[0027] Preferably, in step 4), the quality control interval of the fluorescence response of the ink sample is constructed by calculating the average value and the standard deviation of a series of corrected spectrum fluorescence response results, and constructing the quality control interval with 2 times the standard deviation (2STD, confidence 95.5%) or 3 times the standard deviation (3STD, confidence 99.7%) as the limit value.
[0028] As described above, the present application has the following beneficial effects:
[0029] 1. The present application first proposes a sample preparation, correction and quality control method for the fluorescence anti-counterfeiting ink light emitting effect characterization system, which provides a quantitative evaluation method for fluorescence anti-counterfeiting and solves the problems of poor accuracy and large subjective influence of visual observation.
[0030] 2. The present application carries out fluorescence spectrum detection after preparing the ink sample by color development or solvent dispersion, and establishes two detection methods. The precision of the solution dispersion method is higher and is suitable for fluorescence intensity quality control. The color development method is more similar to the actual printed product form and is suitable for analysis of the influencing factors of the ink fluorescence effect.
[0031] 3. The present application adds a fluorescence correction agent, which can reduce the influence of instrument response fluctuation on the fluorescence intensity of the measured object. BRIEF DESCRIPTION OF DRAWINGS
[0032] Figure 1 A trend graph showing the fluorescence intensity of the ink sample of the present application example 1 and example 2 over time;
[0033] Figure 2 The fluorescence intensity of the ink sample of the present application example 1 and example 2 is shown;
[0034] Figure 3 The influence of the glazing oil on the fluorescence intensity of the ink sample of example 2 is shown;
[0035] Figure 4 The ink fluorescence intensity quality control graph of the present application example 3 is shown. DETAILED DESCRIPTION
[0036] The technical solutions of the present application will be described clearly and completely in connection with the embodiments. Obviously, the described embodiments are only some of the embodiments of the present application, but not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work are within the scope of protection of the present application.
[0037] Embodiment 1
[0038] The embodiment provides a fluorescent anti-counterfeiting ink light-emitting effect characterization method, which is specifically as follows:
[0039] 1. Instruments, standards and reagents
[0040] Main instruments: Cary Eclipse fluorescence spectrometer (Agilent, USA), XPE204 electronic balance (Mettler, Switzerland).
[0041] Standard and reagent: Rhodamine B (100 mg / L), ethanol, ethyl acetate (HPLC grade, Shanghai Anpu Experimental Technology Co., Ltd.).
[0042] 2. Preparation of fluorescence correction agent
[0043] Accurately take 100 μL of Rhodamine B (100 mg / L) into a 10 mL volumetric flask, and prepare a stock solution with a concentration of 1 mg / L by using ethanol as a solvent. Take 200 μL of the stock solution into a 10 mL volumetric flask, and prepare a fluorescence correction agent with a concentration of 0.02 mg / L by using ethanol as a solvent.
[0044] 3. Instrument conditions
[0045] 3.1 Ink solution dispersion sample
[0046] Excitation wavelength: 365 nm, emission wavelength: 400-800 nm, excitation light slit width: 5 nm, emission light slit width: 10 nm, PMT voltage: 580 V.
[0047] 3.2 Fluorescence correction agent
[0048] Excitation wavelength: 544 nm, emission wavelength: 550-800 nm, excitation light slit width: 5 nm, emission light slit width: 10 nm, PMT voltage: 580 V.
[0049] 4. Experimental method
[0050] Take 15 mg of fluorescent ink into a 50 mL centrifuge tube, and add 30 mL of ethyl acetate. After shaking until the ink is completely dispersed, take 3 mL of the solution into a colorimetric cell with a stopper. Place the colorimetric cell on a liquid cell support, and collect the signal by using a fluorescence spectrometer.
[0051] Example 2
[0052] The present embodiment provides a fluorescent anti-counterfeiting ink light emitting effect characterization method, which is as follows:
[0053] 1. Instruments, standards and reagents
[0054] Main instruments: Cary Eclipse fluorescence spectrometer (Agilent, USA), XPE204 electronic balance (Mettler, Switzerland), NB229T full-automatic offset ink color developing instrument (Zhongshan Nobon Color Equipment Co., Ltd.).
[0055] Standards and reagents: Rhodamine B (100 mg / L), ethanol (HPLC grade, Shanghai Anpu Experimental Technology Co., Ltd.).
[0056] 2. Preparation of fluorescence correction agent
[0057] Accurately pipette 100 μL of Rhodamine B (100 mg / L) into a 10 mL volumetric flask, and prepare a stock solution with a concentration of 1 mg / L using ethanol as the solvent. Take 200 μL of the stock solution into a 10 mL volumetric flask, and prepare a fluorescence correction agent with a concentration of 0.02 mg / L using ethanol as the solvent.
[0058] 3. Instrument conditions
[0059] 3.1 Ink color developing sample
[0060] Excitation wavelength: 365 nm, emission wavelength: 400-800 nm, excitation light slit width: 5 nm, emission light slit width: 2.5 nm, PMT voltage: 585 V.
[0061] 3.2 Fluorescence correction agent
[0062] Excitation wavelength: 544 nm, emission wavelength: 550-800 nm, excitation light slit width: 5 nm, emission light slit width: 10 nm, PMT voltage: 580 V.
[0063] 4. Experimental method
[0064] Quantitatively pipette 0.1 mL of ink onto the rubber roller of the offset ink color developing instrument, and evenly spread the ink for 2-3 min. Place the 225 g / m 2 White card is fixed on the impression cylinder of the ink color developing instrument, and the color developing instrument is started to make the color developing sample. Place the color developing sample on the solid sample holder, and use the fluorescence spectrometer to collect the signal.
[0065] Results analysis:
[0066] (1) Evaluation of the time stability of the fluorescence intensity of the ink sample
[0067] The stability of the fluorescence intensity of the ink solvent dispersion sample of Example 1 and the color development sample of Example 2 at different storage times was investigated, and the spectral signal of the sample was collected every half hour. The results are shown in Figure 1 From the figure, it can be seen that the RSD of the change in the fluorescence intensity of the ink solvent dispersion sample was 2.62% within 28 hours; after the ink color development sample was dried, the RSD of the change in the fluorescence intensity was 1.08%, indicating that the fluorescence fluctuation of the ink sample was less than 3% at a certain storage time under the two sample preparation methods, and the detection stability was good.
[0068] (2) Consistency evaluation of detection results of two sample preparation methods
[0069] Eleven batches of ink solvent dispersion samples prepared by the method of Example 1 and eleven batches of color development samples prepared by the method of Example 2 were detected, and the results are shown in Figure 2 From the figure, it can be seen that the change trend of the fluorescence intensity of the ink solvent dispersion sample and the color development sample of different batches was basically the same.
[0070] (3) Inter-person comparison experiment
[0071] For the samples prepared by the methods of Example 1 and Example 2, the influence of different personnel operations was investigated, and the relative standard deviation (RSD) was used to represent the dispersion degree of the data relative to the mean value. The results are shown in Table 1. From the table, it can be seen that when the ink sample was prepared by the solvent dispersion method, the intra-person RSD was 0.53%-1.94%, and the inter-person RSD was 1.41%. When the ink sample was prepared by the color development method, the intra-person RSD was 0.27%-3.33%, and the inter-person RSD was 1.66%. The results showed that the repeatability of different personnel operations was good (RSD was less than 2%) under the two sample preparation methods; compared with the color development method, the precision of the solution dispersion method was higher, so the subsequent fluorescence intensity quality control mainly used the solution dispersion method. In addition, the ink color development sample was closer to the actual printed product in form, and was suitable for analyzing the influencing factors of the fluorescence effect of the ink (such as the coverage of the surface varnish of the ink and the light irradiation of the ink).
[0072] Table 1 Results of inter-person comparison experiment
[0073] (4) Influence of surface varnish coverage
[0074] The ink color development sample prepared in Example 2 was coated with a varnish corresponding to the product on the surface of the ink color development sample, and the influence of the varnish on the fluorescence intensity of the ink was investigated. The results are shown in Figure 3 From the results, it can be seen that after the surface layer of the ink was varnished, the fluorescence intensity decreased by 13.8%, indicating that the varnish had a certain influence on the fluorescence intensity of the ink.
[0075] Example 3
[0076] The present embodiment provides a fluorescent anti-counterfeiting ink quality control chart construction method, which is specifically as follows:
[0077] 1. Instruments, standards and reagents
[0078] Main instruments: Cary Eclipse fluorescence spectrometer (Agilent, USA), XPE204 electronic balance (Mettler, Switzerland).
[0079] Standards and reagents: Rhodamine B (100 mg / L), ethanol, ethyl acetate (HPLC grade, Shanghai Anpu Experimental Technology Co., Ltd.).
[0080] 2. Preparation of fluorescence correction agent
[0081] Accurately pipette 100 μL of Rhodamine B (100 mg / L) into a 10 mL volumetric flask, and prepare a stock solution with a concentration of 1 mg / L using ethanol as the solvent. Take 200 μL of the stock solution into a 10 mL volumetric flask, and prepare a fluorescence correction agent with a concentration of 0.02 mg / L using ethanol as the solvent.
[0082] 3. Instrument conditions
[0083] 3.1 Ink solution dispersion sample
[0084] Excitation wavelength: 365 nm, emission wavelength: 400-800 nm, excitation light slit width: 5 nm, emission light slit width: 10 nm, PMT voltage: 580 V.
[0085] 3.2 Fluorescence correction agent
[0086] Excitation wavelength: 544 nm, emission wavelength: 550-800 nm, excitation light slit width: 5 nm, emission light slit width: 10 nm, PMT voltage: 580 V.
[0087] 4. Experimental method
[0088] 4.1 Prepare several batches of fluorescent ink; weigh 15 mg of fluorescent ink into a 50 mL centrifuge tube, add 30 mL of ethyl acetate, shake until the ink is completely dispersed, take 3 mL of the solution into a stoppered cuvette, place the cuvette on the liquid cell holder, and use the fluorescence spectrometer to collect the signal. Take the fluorescent correction agent as the reference value, which is 293.7 (a.u.), and correct the response of the ink solvent dispersion sample to obtain the fluorescence intensity data of the several batches of ink as shown in Table 1. Figure 4
[0089] 4.2 Take the data of 2024011902~2024092402 as the basis of the construction of the quality control chart, get the average value of the response intensity of the five batches of ink, and take three standard deviations (3STD, confidence 99.7%) as the evaluation criterion, get the fluorescence correction agent reference value 293.7 (a.u.), and realize the construction of the quality control chart.
[0090] 4.3 The target fluorescent ink to be tested is processed by the method shown in step 4.1, and the fluorescence intensity data of the target fluorescent ink is compared with the quality control chart, that is, whether the target ink meets the quality control standard can be evaluated.
[0091] Finally, it should be pointed out that: the above only for the preferred embodiments of the present application, and is not used to limit the present application, although the foregoing embodiments of the present application are described in detail, for those skilled in the art, it still can be modified to the technical scheme recorded in the foregoing embodiments, or equivalent replacement of part of the technical features, any modification, equivalent replacement, improvement, etc. within the spirit and principles of the present application, should be included in the protection scope of the present application.
Claims
1. A method for characterizing and quality controlling the luminescent effect of fluorescent security ink, characterized in that, The method comprises the following steps: 1) preparing a fluorescent correction agent standard solution: adding the fluorescent correction agent into a solvent to prepare a standard solution; 2) preparing a fluorescent anti-counterfeiting ink sample: applying the ink to the surface of paper or dispersing the ink in a solvent to prepare a color developing sample or a solvent dispersion sample; 3) detecting the sample: using a fluorescence spectrometer to detect and analyze the ink sample and the fluorescent correction agent standard solution, respectively, correcting the fluorescence spectrum peak of the ink sample based on the response of the fluorescent correction agent, and obtaining a corrected spectrum of the sample; 4) constructing a quality control chart: taking the fluorescence response of a series of ink sample corrected spectrum as data points to construct a quality control interval of the fluorescence response of the ink sample, and evaluating the quality of a subsequent sample to be detected.
2. The method according to claim 1, characterized in that: In step 1), the fluorescent correction agent is rhodamine B, and the solvent is ethanol.
3. The method according to claim 1, characterized in that: In step 1), the concentration of the fluorescent correction agent is 0.005-0.5 mg / L.
4. The method according to claim 1, characterized in that: In Step 2), the ink was taken in an amount of 0.1-0.125 mL and the coated paper had a weight of 170-250 g / m 2 when the color sample was prepared, and the ink was taken in an amount of 10-20 mg and ethyl acetate was used as the solvent when the solvent dispersion sample was prepared.
5. The fluorescent anti-counterfeiting ink luminescence effect characterization and quality control method according to claim 1, characterized in that: In step 2), when the color developing sample is prepared, the ink is UV ink or non-UV ink; the UV ink is treated by ultraviolet irradiation to form a dry and cured state, and the non-UV ink is naturally placed for 0.5-24 h to form a dry and cured state.
6. The fluorescent anti-counterfeiting ink luminescence effect characterization and quality control method according to claim 1, characterized in that: In step 3), when the fluorescent correction agent solution is detected, the excitation wavelength is 540-548 nm, the emission wavelength is 550-800 nm, the excitation light slit width is 5 nm, the emission light slit width is 5-10 nm, and the PMT voltage is 500-600 V.
7. The method according to claim 1, wherein the method is characterized by: In step 3), when the color developing sample of the ink is detected, the excitation wavelength is 350-370 nm, the emission wavelength is 400-800 nm, the excitation light slit width is 5 nm, the emission light slit width is 2.5-5 nm, and the PMT voltage is 550-600 V.
8. The method according to claim 1, characterized in that: In step 3), when the solvent dispersion sample of the ink is detected, the excitation wavelength is 350-370 nm, the emission wavelength is 400-800 nm, the excitation light slit width is 5 nm, the emission light slit width is 5-10 nm, and the PMT voltage is 550-600 V.
9. The fluorescent anti-counterfeiting ink luminescence effect characterization and quality control method according to claim 1, characterized in that: In step 3), taking the fluorescence response of the first fluorescent correction agent as a reference value, and taking the response value of the fluorescent correction agent / reference value as a coefficient to correct the fluorescence spectrum of the ink sample when the subsequent sample is measured.
10. The method according to claim 1, characterized in that: In step 4), the quality control interval of the fluorescence response of the ink sample comprises: calculating the average value and the standard deviation based on a series of fluorescence response results of the corrected spectrum, and constructing the quality control interval with 2 times the standard deviation (2STD, confidence of 95.5%) or 3 times the standard deviation (3STD, confidence of 99.7%) as the limit value.