DEVICE FOR ANALYSIS OF CEREAL USING FLUORESCENCE AND INFRARED SPECTROSCOPY

Description

[0001] The invention relates to the field of spectroscopic analysis. In particular, the invention relates to a device for measuring the properties of a sample by fluorescence spectroscopy and infrared spectroscopy. Background of the invention

[0002] The invention can be applied in particular, but not exclusively, to the pharmaceutical industry, the environmental industry or the food industry. In the food industry, industrial procedures require precise knowledge of the technological, nutritional and / or toxicological properties of the samples analyzed. In this context, the analysis of samples using spectroscopic techniques makes it possible to extract parameters with a high physicochemical information content.

[0003] To measure these parameters accurately and in accordance with industrial standards, spectroscopy devices are known that use different methods. In particular, in the case of grain samples, fluorescence spectroscopy and infrared spectroscopy make it possible to separately measure different parameters of these samples. Document EP 2 148 185 A2 describes a device for spectroscopic analysis of a grain sample comprising a module for infrared analysis of the sample and a module for analyzing the specific weight of the sample.Documents WO 2017 / 134050 A1 and EP 1 850 117 A1 disclose devices for spectroscopic analysis of grains comprising a module for acquiring infrared spectra of the sample, a module for analyzing fluorescence of the sample and a processing module configured to couple the data acquired by said modules and to determine a grain quality indicator from the coupled data.

[0004] However, a disadvantage of known devices is that they are only designed to operate in small spaces, for example in silo or factory laboratories, with a very short analysis time, approximately 1 to 3 minutes per sample. However, the measurement must be performed twice: firstly by means of a fluorescence spectroscopic device and secondly by means of an infrared spectroscopic device. Such separate devices therefore involve higher acquisition time, space and cost, more complex data management because each instrument is controlled by different processing means and software, and more cumbersome logistics for monitoring the devices and measurement sites. In addition, the reliability and consistency of measurements made by separate devices is significantly reduced since these measurements are carried out on different samples.

[0005] Furthermore, another disadvantage is that known devices significantly complicate the joint processing of measurements obtained from several different spectroscopic technologies. Thus, known devices are often limited to determining the parameters of a sample separately and are not suitable for measuring them in a combined manner, for example via joint processing of fluorescence spectroscopy measurements in the ultraviolet range and infrared spectroscopy measurements.

[0006] In known devices, the measurement and processing of data from these two types of spectroscopy are carried out within separate and uncoupled devices, which severely limits their joint use and therefore the resulting synergies in data analysis. The lack of technical convergence between the two acquisition modes also makes the task more cumbersome and complex. Subject matter and summary of the invention

[0007] The invention aims to overcome at least one of the aforementioned drawbacks.

[0008] For this purpose, the present invention proposes a unique device capable of carrying out a measurement of fluorescence spectra, infrared spectra and specific weight on the same sample.

[0009] One aspect of the invention thus relates to a device for spectroscopic analysis of a grain sample, said device comprising a first infrared analysis module, a second fluorescence analysis module, a third specific weight analysis module, a processing module and a communication network, each of said first module and second module comprising a measuring chamber configured to accommodate at least a portion of the sample; an excitation sub-module configured to emit at least one electromagnetic radiation towards said at least one portion of the sample; a measuring sub-module configured to acquire at least one electromagnetic spectrum of the sample; a draining system configured to guide the sample towards said third module; the third analysis module including a container configured to receive the sample; a measuring sub-module configured to measure a specific weight of the sample; said processing module being connected to each of the analysis modules by the communication network and comprising a memory configured to receive data transmitted by said communication network, said data comprising acquired electromagnetic spectra and measured specific weights; and a processor configured to organize and couple the data received in the memory and to determine a sample quality indicator from the coupled data.

[0010] According to various additional characteristics of said device which may be taken together or separately: the excitation sub-module of the first infrared analysis module is configured to emit at least one electromagnetic radiation with a wavelength between 600 and 2500 nanometers, and in which the measurement sub-module of the first infrared analysis module comprises a spectrometer configured to acquire at least one absorbance and / or transmittance spectrum;the excitation sub-module of the second fluorescence analysis module is configured to emit at least one electromagnetic radiation with a wavelength between 200 and 800 nanometers and the sub-module of the second fluorescence analysis module comprises a spectrometer configured to acquire at least one spectrum selected from: a fluorescence spectrum in frontal mode, acquired at an angle between 30 and 60° relative to the surface of the sample, or a conventional fluorescence spectrum, acquired at a right angle, a wavelength of said at least one spectrum being between 200 nanometers and 800 nanometers; ; said device further comprises a hopper configured to guide at least a portion of the sample to the first module and the second module; said sample quality indicator is chosen from: a Hagberg falling index, a mycotoxin contamination rate, an acrylamide contamination rate, a moisture content, a protein content, a sugar content, a hardness, a baking strength or other typical characteristic of flours, a particle size or a specific weight; the height of the device is less than 75 centimeters, preferably less than 60 centimeters, the width of the device is less than 70 centimeters, preferably less than 55 centimeters, and the depth of the device is less than 55 centimeters, preferably less than 50 centimeters.

[0011] Advantageously, the device allows successive and / or simultaneous measurement of spectral data and specific weight data of a sample, which provides a synergy of information improving the performance of the prediction of quality indicators usually measured by only one of the infrared or fluorescence technologies.

[0012] Advantageously, the presence of a measuring sub-module configured to measure a specific weight of a sample provides a weighing means which makes it possible to determine a major criterion of the quality of the grains, for example with a view to determining the price and subsequent use of these grains.

[0013] Advantageously, the device also makes it possible to ensure homogeneous spectral quality over a wider spectrum, which facilitates the pooling of spectra for their subsequent exploitation during a merger.

[0014] Advantageously, the device is miniaturizable and physically integrable into a system comprising several analysis modules with reduced volume and weight.

[0015] Advantageously, the device is able to process a large volume of sample, which is particularly interesting when the grains are very heterogeneous, in order to reduce the impact of sampling on the quality of calibration and prediction.

[0016] Advantageously, the analysis time before calibration is reduced by half, since a single analysis generates both spectral outputs.

[0017] Advantageously, the cost of the device is reduced, which makes it possible to significantly lower its transfer price compared to two or even three separate devices separately implementing an infrared spectroscopic measurement, a fluorescence spectroscopic measurement and a specific weight measurement.

[0018] In the following description, it will be understood that the specific weight of a sample is the weight per unit volume of this sample, and measured in kilograms per hectoliter, for example of grains. It will be noted that the definition of specific weight is specific to measurement on whole grains and meets the standards in force: the specific weight is not exactly equal to the volume weight of a sample such as a fluid or a solid. Brief description of the drawings

[0019] Other characteristics and advantages of the present invention will emerge from the description given below, with reference to the appended drawings which illustrate exemplary embodiments thereof which are not limiting in nature.

[0020] In the figures: THE Figures 1a and 1b represent, respectively, a side view and a top view of a distribution hopper of a device according to an embodiment of the invention; the Figures 2a, 2b and 2crepresent, respectively, a perspective view, a side view and a top view of a first analysis module of a device according to an embodiment of the invention; the Figures 3a and 3b represent, respectively, a perspective view and a top view of a second analysis module of a device according to an embodiment of the invention; the Figures 4a, 4b and 4c represent, respectively, a perspective view, a side view and a top view of a third analysis module of a device according to an embodiment of the invention; the Figure 5 represents a perspective view of a device according to an embodiment of the invention; the figure 6 represents a side view of a device according to one embodiment of the invention; and the figure 7 represents, in the form of a flowchart, steps of an analysis method according to one embodiment of the invention.

[0021] Naturally, to meet specific needs, a person skilled in the art may apply modifications in the following description. Although it refers to different embodiments, the present invention is not limited to these specific embodiments, and any modifications specific to the scope of the present invention may be considered obvious to a person skilled in the relevant art. Detailed description of an embodiment

[0022] THE Figures 1a and 1b show a side view and a top view of a distribution hopper 100 of a device 1 according to the invention. A sample, for example a grain sample, is poured above the hopper 100 which subsequently guides it towards other elements of the device 1, as described below.

[0023] In a non-limiting manner, it will be considered in the remainder of the description that the sample poured into the hopper 100 is a grain sample. In general, this sample may also include any type of seeds, flours and / or semolina, for example barley, wheat, malt, corn, rye, rapeseed, oats, triticale, soybeans, sunflowers, buckwheat, spelt, peas, field beans, lentils, vetches and / or hempseed.

[0024] According to one embodiment of the invention, the hopper 100 has the shape of a funnel, for example a rectangular funnel comprising four faces 101, 102, 103 and 104. These four faces are inclined and adapted to guide the sample poured towards the lower part of the hopper 100 under the effect of gravity. Each of the faces 101, 102, 103 and 104 is connected to at least one outlet among a first outlet 120 and a second outlet 130, each of these two outlets being located in the lower part of the hopper 100.

[0025] According to one embodiment of the invention, the two outlets 120 and 130 of the hopper 100 are separated from each other by at least one wall 110, for example a vertical wall, comprising two faces 112 and 114. The two faces 112 and 114 are arranged so as to separate and distribute the sample flowing into the hopper 100 into two volumes, a first volume being guided out of the hopper 100 via the first outlet 120 and a second volume being guided out of the hopper 100 via the second outlet 130. In general, the first volume and the second volume are different.

[0026] The faces of the hopper 100 may be made of a single type of material or of different types of materials, including for example metal, stainless steel or plastic, and are designed to allow a smooth, continuous and loss-free flow of the sample poured from the upper part of the hopper towards one of the two outlets 120 and 130.

[0027] The two outlets 120 and 130 of the hopper 100 are connected to at least one analysis module by means of a conveying guide, for example a pipe, a slide or a conveyor belt, which is configured to guide the sample to this or these analysis modules. To improve the guidance of the sample, segmented wheels 140 and 150 can be arranged between the outlets of the hopper and the conveying guide to circulate the grains from the hopper to the conveying guide.

[0028] According to one embodiment of the invention, the first output 120 and the second output 130 are distribution wheels. Preferably, the first output 120 is connected to a first analysis module 200, and the second output 130 is connected to a second analysis module 300. Alternatively, the first output 120 and the second output 130 are further connected to a third analysis module 400.

[0029] According to other embodiments of the present invention, not shown, the hopper 100 has the shape of a circular funnel. In a non-limiting manner, the hopper 100 has any number of faces, said faces being able to have various shapes, and which form a conical, cylindrical or square funnel. The two outlets 110 and 120 as well as the wall 130 can be adapted to these different examples.

[0030] In reference to the Figure 1b, a sample of grains poured above the hopper 100 is guided towards the first outlet 120 when it flows along the face 102 or along a portion of the face 103 and towards the second outlet 130 when it flows along the face 104, along a portion of the face 103 or along a portion of the face 101. According to another example not shown, a sample of grains poured above the hopper 100 is guided towards the first outlet 120 when it flows along the face 102 and along the face 103 of the hopper, and towards the second outlet 130 when it flows along the face 104 and along the face 101.

[0031] According to one embodiment of the invention, the wall 110 can be moved and / or oriented in order to modify the manner in which the sample is separated into two volumes, and thus to define specific values ​​of the first volume guided out of the hopper 100 via the first outlet 120 and of the second volume guided out of the hopper 100 via the second outlet 130. For example, the wall 110 can be moved and / or oriented by a control device in order to modify the arrangement or the relative size of the first outlet 120 and the second outlet 130.

[0032] THE Figures 2a, 2b and 2c show a perspective view, a side view and a top view of a first analysis module 200 of a device 1 according to an embodiment of the present invention.

[0033] In particular, the first analysis module 200 is an infrared analysis module configured to acquire one or more spectra of a sample in the near infrared, for example one or more absorbance and / or transmittance spectra. Said infrared analysis module may also be configured to acquire one or more reflectance spectra.

[0034] Under the principles of infrared spectroscopy, the infrared or near-infrared spectrum of a sample is established by passing an electromagnetic beam with a wavelength between 600 and 2500 nanometers through the sample. According to one embodiment of the invention, the electromagnetic beam is emitted by a broadband continuous source. Alternatively, other types of sources may be used, for example, one or more monochromatic sources.

[0035] The sample subjected to one or more sources of infrared wavelengths then emits a spectrum of electromagnetic radiation. The analysis of this electromagnetic radiation and the corresponding quantity of energy makes it possible to deduce the absorbance and / or transmittance spectra of the sample and, subsequently, to measure parameters such as the humidity level, the protein level, the sugar content, the hardness or even the particle size of a sample.

[0036] The first analysis module 200 comprises a first measurement chamber 210 configured to receive and contain a sample. According to one embodiment of the invention, the first chamber 210 comprises an inlet 211 for receiving this sample, in particular the first volume of the sample guided out of the hopper 100. Preferably, the inlet 211 comprises a funnel adapted to guide the sample towards the interior of the first chamber 210 and to fill it without losses, manually or automatically.

[0037] According to one embodiment of the invention, the first chamber 210 comprises detection elements, for example optical, mechanical or electronic detectors, configured to determine and indicate whether a sample is present in the first chamber 210, and preferably what volume of this sample. These detection elements comprise, for example, a detection sensor combining an infrared emitter and a photodiode to enable detection of the presence of a sample in the first chamber 210, and to deduce therefrom whether the latter is completely, partially or not at all filled.

[0038] According to one embodiment of the invention, the first chamber 210 comprises at a first end a first wall 214 and at a second end a second wall 216.

[0039] According to one embodiment of the invention, a portion of the wall 214 and the wall 216 comprises a transparent window, for example a glass or plastic window. At least one of the two walls 214 and 216 is partially or completely transparent to electromagnetic radiation. Preferably, the window of the wall 216 is frosted so as to be partially or completely transparent to infrared electromagnetic radiation. Advantageously, the use of at least one window thus frosted improves the quality of the measurable spectra of the sample, and limits the dynamic range between these and reference spectra measured in the absence of the sample.

[0040] On the Figures 2a, 2b and 2c , the wall 216 is arranged on the side of a first excitation sub-module 220 and the wall 214 is arranged on the side of the measurement sub-module 230. Equivalently, the first excitation sub-module 220 is an illumination sub-module.

[0041] The first chamber 210 includes a third outlet 212 for discharging and guiding the sample therefrom and out of the first analysis module 200 to another element of the device 1, or out of the device 1. For example, the third outlet 212 may guide the sample to an inlet of the second analysis module 300 or the third analysis module 400. The third outlet 212, which may be either in the open position or in the closed position, is controlled manually or automatically.

[0042] According to one embodiment of the invention, control of the third output 212 of the first analysis module 200 is carried out by means of a first drainage system 213, this first drainage system 213 comprising for example a motor which can be controlled to automatically open and close the third output 212.

[0043] According to one embodiment of the invention, the first wall 214 is a movable wall and the second wall 216 is a fixed wall. In particular, the wall 214 is movable along the main axis of the first analysis module 200 by means of a motor 240. The movement of the wall 214 relative to the wall 216 makes it possible to increase or decrease the size of the first chamber 210, and thus to modify the maximum thickness or volume of a sample that can be contained in the first chamber 210. The movement of the wall 214 relative to the wall 216, which can be automated, makes it possible to position the latter with an accuracy of less than 0.05 millimeters in a few seconds.

[0044] Due to the great diversity of samples that can be analyzed by the present device, for example due to the size of the grains that make up this sample, the volume density of the sample contained in the first chamber 210 and the optical scattering properties of this sample can vary greatly from one case to another. For example, the scattering, absorption and spectral amplification properties of samples of wheat, corn and barley can be very different. Advantageously, an adjustment of the size of the first chamber 210 as a function of the sample present makes it possible to optimize the quality of the measurements carried out by the first analysis module 200 when the latter is an infrared analysis module configured to acquire one or more absorption or transmission spectra of a sample in the infrared or near infrared.

[0045] The first analysis module 200 further comprises a first excitation sub-module 220 and a second measurement sub-module 230. According to one embodiment of the invention, and when the first infrared analysis module 200 is configured to acquire one or more transmittance spectra, each of these two sub-modules being arranged on either side of the first chamber 210. As a variant, these two sub-modules can be placed on the same side of the first chamber 210, for example to allow the acquisition of reflectance spectra.

[0046] The first excitation sub-module 220 is configured to emit electromagnetic radiation, in particular electromagnetic radiation whose wavelength is in the infrared. This radiation is emitted by the first excitation sub-module 220 towards the first chamber 210 and the second measurement sub-module 230. The first sub-module 220, the first chamber 210 and the second sub-module 230 are aligned along an axis substantially defining the trajectory of the radiation emitted by the first excitation sub-module 220, then passing through the first chamber 210 and received by the second measurement sub-module 230.

[0047] According to one embodiment of the invention, the first excitation sub-module 220 comprises a broadband continuous light source, said light source being configured to emit electromagnetic radiation whose wavelength is between 600 and 2500 nanometers.

[0048] For example, the excitation sub-module 220 includes a quartz-tungsten-halogen (QTH) lamp, which emits light radiation from a heated tungsten filament. Preferably, said quartz-tungsten-halogen lamp is configured to be underpowered with a power of between 25 Watts and 50 Watts, and to emit radiation in a wavelength range of between 240 and 2700 nanometers.

[0049] The first excitation sub-module 220 is preferably arranged so that the radiation is emitted towards the sample. This radiation is then absorbed by the sample, or scattered by the sample and detected by the second measurement sub-module 230, as detailed below. The second measurement sub-module 230 is configured to transmit the measurements made at any time to a processing module.

[0050] Absorption spectroscopy is based on the principle that any material subjected to incident radiation, for example infrared radiation, can either reflect part of this radiation, absorb part of this radiation, or transmit part of this radiation. In particular, the absorption of radiation by the sample causes it to generate one or more absorption and / or transmission spectrum(s).

[0051] The second measurement sub-module 230 is arranged and configured to receive electromagnetic radiation emitted by the first excitation sub-module 220 and electromagnetic radiation coming from the first chamber 210 and / or from a sample contained in this first chamber 210. According to one embodiment of the invention, the second measurement sub-module 230 comprises a high-sensitivity spectrometer which is configured to acquire one or more spectra, for example in the near infrared.

[0052] According to one embodiment of the invention, a spectrometer of the second measurement sub-module 230 is integrated in CMOS technology, for example on a silicon-on-insulator (SOI) wafer. According to another embodiment of the invention, the spectrometer of the second measurement sub-module 230 comprises a CCD type sensor, for example a BI-CCD detection strip with a slit of the order of 200 micrometers. Advantageously, such a spectrometer is sensitive to infrared electromagnetic radiation emitted by a wide range of samples, in particular in the wavelength range between 850 and 1100 nanometers.

[0053] The dynamic range of a spectrometer defines its detection range, corresponding to the ratio of the intensity of the largest signal and the intensity of the smallest signal measurable by this spectrometer. In particular, a spectrometer of the second measurement sub-module 230 is characterized by a dynamic range equal to the maximum level divided by the minimum level of a signal measurable by this spectrometer, the measurement of a minimum level signal corresponding to a measurement carried out in the absence of a signal. Generally, a measurement carried out in the absence of a signal can be implemented using one or more acquisitions of spectra in the absence of a signal, for example 25 to 50 acquisitions, and by calculating the average, the effective value and / or the quadratic value of these acquisitions to define the dynamic range of the spectrometer.

[0054] According to one embodiment of the invention, the elements of the first analysis module 200 are arranged in a fixed manner to avoid any movement of the optical part, with the exception of the wall 214 if the latter is fixed. In addition, a spectrometer of the second measurement sub-module 230 can be fixed thereto by one or more mechanical supports. Advantageously, such a configuration provides an optical chain which allows stable and precise acquisition of transmittance spectra, in particular in the near infrared.

[0055] According to one embodiment of the invention, the first chamber 210 comprises diffuser elements. These diffuser elements can be placed at the inlet of the first chamber 210 near the wall 216 and the first excitation sub-module 220 and / or near the wall 214 and the second measurement sub-module 230. When a sample is present in the first chamber 210, a large portion of the electromagnetic radiation emitted by the first excitation sub-module 220 is absorbed by it and a smaller portion of this radiation is transmitted towards the second measurement sub-module 230. In general, a sample illuminated by infrared radiation absorbs a significant fraction of this radiation, which limits the intensity of the signal measured by a spectrometer.

[0056] Advantageously, the placement of diffuser elements, and in particular infrared diffusers, at the input and / or output of the first chamber 210 makes it possible to improve the quality of the transmittance spectra measured by the second measurement sub-module 230 in the infrared and near infrared range. In particular, the placement of diffuser elements reduces the dynamic range to be detected by at least one order of magnitude without significantly modifying the time required for the acquisition of the spectra, of the order of 1% of the total measurement time.

[0057] According to one embodiment of the invention, the diffusing elements comprise diffusing surfaces made of one or more materials chosen from silicon, silica, sapphire or any type of material allowing high transmission of electromagnetic radiation in the infrared and near infrared wavelength ranges. For example, diffusing elements made of a silicon material preferably transmit infrared radiation, but not visible light radiation. Advantageously, the granularity of the diffusing elements can be varied and selected with a view to combining several of them to obtain the best compromise between reduction of the dynamic range and limitation of the loss of the measured signal.

[0058] To measure a minimum level signal and / or spectrum, the spectrometer of the second measurement sub-module 230 comprises a shutter 232, for example a plate or an opaque element, which is connected to a rotation element 234, for example a motor, to move the shutter. The shutter 232 is manually or automatically movable between a position remote from the spectrometer inlet and a position located in front of the spectrometer inlet. When the shutter 232 is in a remote position, the spectrometer is not obscured and receives all electromagnetic radiation emitted towards it; when the shutter 232 is in front of the spectrometer inlet, the spectrometer is obscured and no electromagnetic radiation can be measured by it.This mechanism allows the spectrometer to acquire a spectrum from a sample contained in the first chamber 210 when the spectrometer is not occluded and a minimum level, or noise, spectrum when the spectrometer is occluded.

[0059] According to one embodiment of the invention, the first analysis module 200 further comprises a plate 250 for separating and isolating the second measurement sub-module 230 from the first chamber 210. The plate 250 comprises an opening that allows electromagnetic radiation to pass through. According to another embodiment of the invention (not shown), no separation plate is present between the second measurement sub-module 230 and the first chamber 210.

[0060] THE Figures 3a and 3b show a perspective view and a top view of a second analysis module 300 of a device 1 according to an embodiment of the present invention.

[0061] In particular, the second analysis module 300 is a fluorescence analysis module configured to acquire one or more fluorescence spectra of a sample, for example one or more frontal fluorescence spectra.

[0062] Under the principles of fluorescence spectroscopy, a sample is excited by light radiation of a specific wavelength, for example in the visible or ultraviolet range. Fluorescence spectra preferably extend over a spectral range between 200 nanometers and 800 nanometers. The use of these wavelengths in conventional or frontal fluorescence spectroscopy methods makes it possible to measure parameters such as the Hagberg falling number or the contamination rate of mycotoxins, acrylamide, etc. The Hagberg falling number makes it possible to measure the activity of alpha-amylase present in wheat grains, in particular, and / or to quickly detect contaminated or damaged samples, or even varietal purity, upon entry into the silo.

[0063] In response to this excitation, the sample emits radiation whose properties depend on the components contained in this sample. Based on the measurement of this emission radiation, it is then possible to deduce the corresponding fluorescence spectrum(s). The processing of these fluorescence spectra, preferably acquired over a spectral range between 200 nanometers and 800 nanometers, using pre-processing, decomposition and modeling tools by learning or other means, makes it possible to extract information such as the Hagberg falling number, mycotoxin contamination or other parameters characterizing the degree of germination of the seeds contained in a volume of the sample.

[0064] The second analysis module 300 comprises a second measurement chamber 310 configured to receive and contain a sample. According to one embodiment of the invention, the second chamber 310 comprises an inlet 311 for receiving this sample, for example the second volume of the sample guided out of the hopper 100. Preferably, the inlet 311 comprises a funnel adapted to guide the sample towards the interior of the first chamber 310 to fill it without loss manually or automatically.

[0065] The second chamber 310 comprises a fourth outlet 312 for evacuating and guiding the sample out of the second analysis module 300 to another element of the device 1, for example to an inlet of a third analysis module 400. The fourth outlet 312, which can be either in the open position or in the closed position, is controlled manually or automatically. In particular, the opening and / or closing of the fourth outlet 312 can be carried out manually or automatically by means of a second emptying system 313, which can be motorized.

[0066] The second analysis module 300 is connected to the device 1. In particular, the fourth output 312 is connected to at least one analysis module, by means of a guide. Preferably, the fourth output 312 is connected to a third analysis module 400.

[0067] According to one embodiment of the invention, the second chamber 310 further comprises detection elements, for example optical, mechanical or electronic detectors, for determining whether a sample is present in the second chamber 310, and preferably, what volume of this sample is present.

[0068] The second analysis module 300 further comprises a third excitation sub-module 320 and a fourth measurement sub-module 330, the configuration of each of these two sub-modules preferably being such that they are arranged on the same side of the second measurement chamber 310 to allow measurement of frontal fluorescence spectra.

[0069] Alternatively, other configurations are conceivable to enable the acquisition of conventional or frontal fluorescence spectra. For example, in the case of a configuration intended for the acquisition of frontal fluorescence spectra, the opening 314 of the second chamber 310 is arranged on the same side as the third excitation sub-module 320 and the fourth measurement sub-module 330. Alternatively, the third excitation sub-module 320 and the fourth measurement sub-module 330 may be placed on a different side of the second chamber 310 for the case of other configurations.

[0070] The third excitation sub-module 320 is configured to generate and emit at least one electromagnetic radiation towards the second chamber 310, in particular visible or ultraviolet electromagnetic radiation with a wavelength between 200 and 800 nanometers.

[0071] The third excitation sub-module 320 is stably fixed in the second analysis module 300 and comprises an optomechanical part 321. This optomechanical part 321 comprises one or more light sources configured to emit electromagnetic radiation at predetermined illumination wavelengths. Preferably, the or each of the light sources emits monochromatic radiation at a given wavelength towards the sample contained in the second chamber 320. Depending on the number of light sources, these electromagnetic radiations can roughly sample (several tens of wavelengths) or finely sample (several hundreds of wavelengths) a spectral range, for example a spectral range covering the visible and ultraviolet domains.

[0072] In a non-limiting manner, the light sources of the optomechanical part 321 comprise a monochromatic radiation source or a polychromatic radiation source. For example, these light sources comprise a light-emitting diode or a laser source. The third excitation sub-module 320 and / or the optomechanical part 321 may comprise other optical elements such as focusing elements or diffusion elements, for example lenses. For example, the optomechanical part 321 comprises a lens configured to focus or diffuse the electromagnetic radiation passing therethrough.

[0073] According to one embodiment of the invention, the optomechanical part 321 comprises an opening configured to allow the passage of electromagnetic radiation, in particular the electromagnetic radiation emitted by the sample located in the second chamber 310, towards the fourth measurement sub-module 330.

[0074] According to one embodiment of the invention, the optomechanical part 321 is circular in shape and comprises a given number of light sources, this number being between one and twenty, and preferably between one and ten.

[0075] On the Figures 3a and 3b, the third excitation sub-module 320 comprises six light-emitting diodes arranged along the circumference of the circular optomechanical part 321. The six light-emitting diodes 322 to 327, comprise four diodes 322, 323, 324 and 325 configured to emit ultraviolet radiation with a central wavelength equal to 275 + / - 5 nanometers, a diode 326 configured to emit ultraviolet radiation with a central wavelength equal to 338 + / - 3 nanometers, a diode 327 configured to emit ultraviolet radiation with a central wavelength equal to 385 + / - 3 nanometers. Generally, each diode can be configured to provide a power of between 5 milliwatts and 1 watt. The third excitation sub-module 320 may also include a seventh diode configured to emit ultraviolet radiation with a central wavelength equal to 420 + / - 5 nanometers.

[0076] When it reaches the sample contained in the second chamber 320, electromagnetic radiation emitted by one of the light sources of the optomechanical part 321 causes excitation of the sample. When this sample de-excites, it emits a complete fluorescence spectrum in all directions, and in particular in the direction of the fourth measurement sub-module 330.

[0077] According to one embodiment of the invention, the second chamber 310, the third excitation sub-module 320 and the fourth measurement sub-module 330 are aligned along an axis corresponding to the axis of the trajectory of the electromagnetic radiation emitted by the sample in the second chamber 320 towards the fourth measurement sub-module 330. The fourth measurement sub-module 330 is positioned so as to be able to receive the electromagnetic radiation coming from the sample contained in the second chamber 310 after the excitation of this sample. The fourth measurement sub-module 330 is configured to transmit the measurements carried out at any time to a processing module

[0078] According to one embodiment of the invention, the fourth measurement sub-module 330 comprises a spectrometer configured to measure one or more fluorescence spectra, for example a frontal fluorescence spectrum in the ultraviolet and visible range, and corresponding to wavelengths between 200 and 800 nanometers. The spectrometer of the fourth measurement sub-module 330 is arranged substantially on the same side as the third excitation sub-module 320 to enable the acquisition of frontal fluorescence spectra. Compared to other types of fluorescence spectra, the acquisition of frontal fluorescence spectra makes it possible to avoid generating excessively large analytical errors linked to the sample, its preparation or external conditions such as temperature or pressure; the results obtained are therefore more precise and determined more quickly.

[0079] Just as for the spectrometer of the second measurement sub-module 230, the spectrometer of the fourth measurement sub-module 330 is configured to further acquire a minimum level signal and / or spectrum. This acquisition can be implemented without requiring a shutter, by performing a measurement when the light source(s) of the third excitation sub-module 320 are switched off.

[0080] According to one embodiment of the invention, the spectrometer of the fourth measurement sub-module 330 comprises a CCD type sensor with a slit of the order of 500 micrometers and a resolution of approximately 10 nanometers.

[0081] According to other embodiments not shown, the third excitation sub-module 320 may be arranged in different positions and orientations in the second analysis module 300. For example, the third excitation sub-module 320 may be arranged along an axis substantially perpendicular to another axis passing through the second chamber 310 and through the second measurement sub-module 330, in order to acquire fluorescence spectra at right angles.

[0082] According to one embodiment of the invention, the second chamber 310, the third excitation sub-module 320 and the fourth measurement sub-module 330 are fixed in the second analysis module 300 by one or more mechanical supports. This configuration avoids any movement of mechanical parts, and provides an optical chain allowing stable and precise acquisition of fluorescence spectra, in particular frontal fluorescence spectra and or other types of spectra. Advantageously, the second analysis module 300 is compact and does not integrate moving optical parts. This compactness and stability improve the sensitivity and repeatability of measurements during the acquisition of fluorescence spectra while facilitating instrumental standardization.

[0083] According to one embodiment of the invention, the filling of the second chamber 310, the excitation of the sample by the excitation sub-module 320 and the acquisition of fluorescence spectra by the second measurement sub-module 330 are automated mechanically and electronically.

[0084] According to one embodiment of the invention, control of the fourth output 312 of the second analysis module 300 is carried out by means of a second drainage system 313, this second drainage system 313 comprising for example a motor which can be controlled to open and close the fourth output 312.

[0085] THE Figures 4a, 4b and 4cshow a perspective view, a side view and a top view of a third analysis module 400 of a device 1 according to an embodiment of the present invention. According to an embodiment of the invention, the third analysis module 400 is a weight measurement module configured to measure the specific gravity of a sample

[0086] The third analysis module 400 is connected to the rest of the device 1. According to one embodiment of the invention, the third analysis module 400 is connected to the third outlet 212 of the first chamber 210 and to the fourth outlet 312 of the second chamber 310 in order to measure the specific weight of the same sample as that from the first analysis module 200 and the second analysis module 300. Alternatively, the third analysis module 400 is connected to the first outlet 120 and / or to the second outlet 130 of the hopper 100.

[0087] The third analysis module 400 comprises a container 410 configured to receive and contain a portion of the sample. The base of the container 410 is supported by a platform 416 which stabilizes it and which can have different dimensions and geometries.

[0088] According to one embodiment of the invention, the container 410 is a container which has a cylindrical, parallelepiped, or even conical shape. This container comprises a filling volume of between 100 milliliters and 1000 milliliters, preferably 500 milliliters.

[0089] According to one embodiment of the invention, the third analysis module 400 comprises a fifth measurement sub-module 430 arranged under the container 410. The fifth measurement sub-module 430 comprises one or more weight sensors configured to measure the weight of the container 410 when the latter is empty or filled with a sample, partially or completely.

[0090] According to one embodiment of the invention, the third analysis module 400 comprises detection elements, for example optical or mechanical detectors, to determine whether a sample is present in the container 410, and preferably, what volume of this sample.

[0091] According to one embodiment of the invention, the third measuring module 400 comprises a leveling element 415, for example a leveling blade or a leveling spring, configured to move above the container 410, or in this container 410, in order to level a sample contained in the container 410.

[0092] The movement of the leveling element 415 is automated, and guarantees a measurement of the weight of the sample contained in the container 410 which presents excellent repeatability.

[0093] According to one embodiment of the invention (not shown), the leveling element 415 comprises a cleaning and / or resetting element.

[0094] The fifth measurement sub-module 430 is configured to transmit the measurements made at any time to a processing module, to calculate the specific weight of any sample contained in the container 410 from the measured weight and the measured volume of this sample. Advantageously, the third analysis module 400 provides a compact and precise means for measuring with high precision the specific weight of a grain sample in a reproducible manner on an outdoor site or inside a grain silo.

[0095] The container 410 comprises a fifth outlet 412 for discharging and guiding the sample out of it and out of the third analysis module 400, for example to the outside of the device 1. The fifth outlet 412, which can be either in the open position or in the closed position, can be controlled manually or automatically. According to one embodiment of the invention, control of the fifth outlet 412 of the third analysis module 400 is carried out by means of a third emptying system 413, this third emptying system 413 comprising for example a motor which can be controlled to open and close the fifth outlet 412.

[0096] According to one embodiment of the invention (not shown), the third analysis module 400 comprises a cleaning system, which is configured to clean the platform 416 and / or the interior of the container 410 before or after evacuation of the sample from the container 410.

[0097] The third analysis module 400 therefore allows an accurate measurement of the specific weight of a sample contained in the container 410 can be obtained from the measurement of the weight of the sample in the container. The third analysis module 400 further allows a measurement of the tare, that is to say the weight of the container when it is empty. By subtracting the measured tare from the weight obtained in the presence of the sample and using a calibration equation, it is thus possible to accurately determine the specific weight of the sample.

[0098] THE figures 5 And 6 show, respectively, a perspective view and a side view of a device 1 according to the invention, the device 1 comprising the hopper 100, the first analysis module 200, the second analysis module 300 and the third analysis module 400 previously described.

[0099] According to one embodiment of the invention, the distribution hopper 100 and the third analysis module 400 are each connected to the first analysis module 200 and to the second analysis module 300 by means of guides in order to allow guidance of a sample from the distribution hopper 100 to the first analysis module 200 and to the second analysis module 300, then from each of the first and second analysis modules 200 and 300 to the third analysis module 400, under the effect of gravity. The sample is then evacuated from below the third analysis module 400.

[0100] The device 1 further comprises a processing module 500. On the figures 5 And 6, the processing module 500 is represented as a laptop but which can also be any type of electronic or computer processing means, for example a processor, a desktop computer, a smartphone or any device similar to a terminal with a control screen, a USB key, a mobile memory card or any other similar technology. Preferably, the processing module 500 is an embedded PC.

[0101] The processing module 500 is connected to the device 1, in particular to one or more analysis modules of the device 1, by means of a communication network 600. The communication network 600 makes it possible to connect the processing module 500 to the analysis modules 200, 300 and 400. For example, the communication network 600 is a local network such as a wired network, a Bluetooth network, a Wi-Fi network or even an Ethernet network. In all cases, the communication network 600 is configured to transmit information between the processing module 500 and each analysis module of the device 1.

[0102] According to one embodiment of the invention, the processing module 500 is configured to control the circulation of the sample in the different elements of the device 1, for example via the control of inputs and outputs of the analysis modules 200, 300 and 400 and / or of the hopper 100. Advantageously, the processing module 500 makes it possible to manage either manually or automatically the measurements made by the device 1 by following process steps as described below in relation to the figure 7 .

[0103] The processing module 500 comprises a memory 510 which is configured to receive data transmitted by the communication network 600. This data may comprise any type of information measured by the analysis modules such as wavelengths of the radiation emitted by the sample in any one of the analysis modules, measured intensities of this radiation, corresponding electromagnetic spectra or even tares and specific weights measured by the third analysis module 400.

[0104] On the figures 5 And 6, the broken arrows represent the direction of data transmission by the communication network 600, from a first element to a second element. For example, the communication network 600 transmits an infrared spectrum acquired by the first analysis module 200 to the processing module 500, a fluorescence spectrum acquired by the second analysis module 300 to the processing module 500 or a specific weight measured by the third analysis module 400 to the processing module 500.

[0105] The processing module 500 further comprises a processor 520 which is configured to perform operations on the data contained in the memory 510. Different software installed on the processor 520 can be used to perform these operations. In particular, the processor 520 is configured to perform a coupling of spectra, for example a coupling of an infrared spectrum from the first analysis module 200 and a fluorescence spectrum from the second analysis module 300, to produce a mixed spectrum. Furthermore, the processor 520 of the processing module 500 is configured to determine at least one quality indicator of the sample from this data or these spectra.

[0106] The processor 520 is configured to organize the data and the spectra in order to carry out digital and computer processing thereof, in particular the fluorescence spectra, the infrared spectra and the specific weights acquired by the analysis modules 200, 300 and 400. For example, the processor 520 organizes the fluorescence data into three-dimensional mathematical tables, these three dimensions corresponding respectively to the wavelength of the excitation electromagnetic radiation used, to the wavelength of the emission radiation of the sample measured in response to this excitation by a spectrometer, and to the intensity of this emission radiation. The processor 520 organizes the infrared data into separate mathematical tables, for example two- or three-dimensional.

[0107] The processor 520 is configured to perform a coupling of the data and the spectra, and more particularly of the data organized in mathematical tables. For example, a first technique consists of concatenating the mathematical tables of the fluorescence data and the infrared data in the same mathematical table. Advantageously, this first technique amounts to juxtaposing the spectra corresponding to these data over the entire wavelength range of the acquired spectra. A second technique consists of constructing a spectral image of the sample from the combination of fluorescence spectra and infrared spectra. Advantageously, this combination makes it possible to obtain a 3-dimensional image which preserves the three-dimensional structure of the mathematical table of the associated fluorescence data.A third technique is to construct a two-dimensional spectral image resulting from the combination of the first technique and the second technique.

[0108] To perform spectroscopic data couplings and determine quality indicators such as Hagberg falling number, mycotoxin contamination rate, acrylamide contamination rate, moisture content, protein content, sugar content, hardness, baking strength or other typical flour characteristics, particle size or specific weight, one can refer to the reference work by D. Bertrand and E. Dufour, “Infrared spectroscopy and its analytical applications” (2006) for the case of data from infrared spectra and to the review by J. Sadecka and J. Tothova, “Fluorescence Spectroscopy and Chemometrics in the Food Classification - A Review”, Czech Journal of Food Sciences 25(4):159-173 (2007) for the case of data from fluorescence spectra.For data fusion, we can refer to the different methods mentioned in the journal “Data fusion methodologies for food and beverage authentication and quality assessment - A review”, Analytica Chimica Acta 2015, 891, 1-14.

[0109] A decomposition of the data before or after fusion is then implemented by applying multivariate or multi-way statistical models known in the technical field, with a view to predicting one or more quality indicators. The specific weight measurements from the third analysis module 400 allow a user or the processing module 500 to choose more precisely the statistical models corresponding to the type of sample analyzed.

[0110] Furthermore, the processor 520 is configured to determine at least one quality indicator of the sample from the data and spectra coupled by one or other of these techniques. According to one embodiment of the invention, these quality indicators are chosen from: a Hagberg falling index, a mycotoxin contamination rate, an acrylamide contamination rate, a humidity rate, a protein rate, a sugar content, a baking strength or other characteristic of the flours, a hardness, a particle size or even a specific weight.

[0111] Advantageously, the calculation of quality indicators of a sample from coupled data rather than from data obtained separately makes it possible to improve the accuracy of the prediction of quality indicators selected from the humidity level, the protein level, the mycotoxin contamination level, the Hagberg falling number or the specific weight. Knowledge of the specific weight of the sample measured in the third analysis module 400 makes it possible to further improve the accuracy of this prediction, via a choice of statistical models adapted to the sample analyzed by the device 1.

[0112] According to one embodiment of the invention, the maximum dimensions of the device 1 are 75 centimeters in height, 70 centimeters in width and 55 centimeters in depth. For example, the dimensions of the device 1 are of the order of 71 centimeters in height, 65 centimeters in width and 45 centimeters in depth. Preferably the dimensions of the device 1 are of the order of 60 centimeters in height, 55 centimeters in width and 50 centimeters in depth.

[0113] According to one embodiment of the invention, the device 1 and / or some of its elements are contained in a sealed housing in order to isolate them from external conditions such as, for example, the presence of dust, temperature fluctuations or even shocks linked to the transport of the device.

[0114] There figure 7shows in the form of a flowchart the steps of a method for analyzing a sample according to one embodiment of the invention. According to one embodiment of the invention, the method comprises a first separation step E100 during which a sample poured into the hopper 100 of the device 1 is separated and guided to a first analysis module 200 and to a second analysis module 300. A second analysis step E200 and a third analysis step E300 are then carried out, either successively or simultaneously.

[0115] According to one embodiment of the invention, the second analysis step E200 implemented by the first analysis module 200 aims to acquire an infrared or near-infrared spectrum of the sample and comprises the following steps: a sub-step E210 of filling the first chamber 210 with a sample, a sub-step E210b of detecting the filling of the first chamber 210 by the detection elements of the first analysis module 200, a sub-step E220 of excitation of the sample by the first excitation sub-module 220, a sub-step E230 of acquisition by the first module 230 of acquisition of at least one infrared or near-infrared spectrum by the first measurement module 230, a sub-step E213 of evacuating the sample from the first chamber 210 and towards the third analysis module 400 via the first emptying system 213,a sub-step E240 of acquiring at least one spectrum in darkness by the first module 230 when the spectrometer of the first module 230 is closed by the shutter 232 and a sub-step E250 of transmitting the spectra acquired during the step E200 to the processing module 500.,

[0116] According to one embodiment of the invention, a reference spectrum taking step, i.e. a vacuum source spectrum step, precedes the filling sub-step E210. Alternatively, this reference spectrum taking step may directly follow the sample removal sub-step E213.

[0117] Alternatively, the sub-step E213 of removing the sample may be implemented after either the sub-step E240 of acquiring at least one dark spectrum and the sub-step E250 of transmitting. According to another variant, the sub-step E240 of acquiring at least one dark spectrum may be implemented before the sub-step E210 of filling the first chamber 210 with a sample. The sub-step E210 of filling may further comprise a sub-step E210b of detecting the filling of the first chamber 210 by detection elements of the first analysis module 200.

[0118] According to one embodiment of the invention, the third analysis step E300 implemented by the second analysis module 300 aims to acquire at least one fluorescence spectrum of the sample and a dark spectrum via the following sub-steps: a sub-step E310 of filling the second chamber 310 with a sample, a sub-step E320 of excitation of the sample by the third excitation sub-module 320, a sub-step E330 of acquisition by the fourth sub-module 330 of measurement of at least one fluorescence spectrum, a sub-step E313 of evacuation of the sample from the second chamber 310 via the second emptying system 313,a sub-step E340 of acquiring at least one spectrum in the dark by the fourth measurement sub-module 330 when the light sources of the third excitation sub-module 320 are switched off and a sub-step E350 of transmitting the spectra acquired during the third step E300 to the processing module 500. Alternatively, the sub-step E313 of removing the sample may be implemented after either of the sub-step E340 of acquiring at least one spectrum in the dark and the sub-step E350 of transmitting. The sub-step E310 of filling may further comprise a sub-step E310b of detecting the filling of the second chamber 310 by detection elements of the second analysis module 300.,

[0119] According to one embodiment of the invention, the fourth analysis step E400 implemented by the third analysis module 400 aims to measure at least one specific weight of the sample and a tare weight via the following sub-steps: a sub-step E405 of measuring the tare weight corresponding to the empty weight of the container 410, a sub-step E410 of filling the container with a sample, a sub-step E415 of leveling the surface of the sample by the leveling element 415, a sub-step E420 of measuring the specific weight of the sample contained in the container, a sub-step E440 of evacuating the sample from the container 410 by the third emptying system 413, and a sub-step E450 of transmitting the measurements made of the specific weight and the tare weight to the processing module 500.The filling sub-step E410 may further comprise a sub-step E410b of detecting the filling of the container 410 with a sample, by means of the detection elements of the third analysis module 400.

[0120] According to one embodiment of the invention, the fifth processing step E500 implemented by the processing module 500 aims to determine a quality indicator of the sample via the following sub-steps: a sub-step E510 of receiving the data from the first analysis module 200, the second analysis module 300 and the third analysis module 400, a sub-step E520 of coupling these data, a sub-step E530 of applying at least one multi-channel statistical model and a sub-step E540 of predicting at least one quality indicator on the basis of the preceding sub-steps. The fifth processing step E500 may further include a sub-step E525 not shown in the figure 7consisting of determining at least one multi-channel statistical model as a function of the value of the specific weight of the sample transmitted to the processing module 500 during sub-step E450, said sub-step E525 being implemented before sub-step E530 of applying at least one multi-channel statistical model.

[0121] Naturally, to meet specific needs, a person skilled in the art of the invention may apply modifications in the foregoing description. Although the present invention has been described above with reference to specific embodiments, the present invention is not limited to the specific embodiments, and modifications that fall within the scope of the present invention will be obvious to a person skilled in the art. The invention is defined by the following claims.

Claims

1. Device (1) for spectroscopically analysing a grain sample, said device comprising a first infrared analysis module (200), a second fluorescence analysis module (300), a third specific weight analysis module (400), a processing module (500) and a communication network (600), each of said first module (200) and second module (300) comprising • a measurement chamber (210, 310) configured to receive at least a portion of the sample; • an excitation submodule (220, 320) configured to emit at least one electromagnetic radiation towards said at least a portion of the sample; • a measurement submodule (230, 330) configured to acquire at least one electromagnetic spectrum of the sample; • a draining system (213, 313) configured to guide the sample towards said third module (400); the third analysis module (400) comprising • a container (410) configured to receive the sample; • a measurement sub-module (430) configured to measure a specific weight of the sample; said processing module (500) being connected to each of the analysis modules (200, 300, 400) by said communication network (600) and comprising • a memory (510) configured to receive data transmitted by said communication network (600), said data comprising electromagnetic spectra acquired by said first module (200) and said second module (300) and specific weights measured by said third analysis module (400) ; and • a processor (520) configured to organise and couple the data received in the memory and to determine an indicator of quality of the sample from the coupled data.

2. Device according to claim 1, wherein the excitation submodule (220) of the first infrared analysis module (200) is configured to emit at least one electromagnetic radiation of wavelength comprised between 600 and 2500 nanometres, and wherein the measurement sub-module (230) of the first infrared analysis module (200) comprises a spectrometer configured to acquire at least one absorbance and / or transmittance spectrum.

3. Device according to claim 1 or 2, wherein the excitation submodule (320) of the second fluorescence analysis module (300) is configured to emit at least one electromagnetic radiation of wavelength comprised between 200 and 800 nanometres and the sub-module (330) of the second fluorescence analysis module (300) comprises a spectrometer configured to acquire at least one spectrum selected from among: a fluorescence spectrum in frontal mode, acquired at an angle comprised between 30 and 60° with respect to the surface of the sample, that is a conventional fluorescence spectrum, acquired at a right angle, a wavelength of said at least one spectrum being comprised between 200 nanometres and 800 nanometres.

4. Device according to any one of the preceding claims, wherein said device further comprises a funnel (100) configured to guide at least a portion of the sample towards the first module (200) and the second module (300).

5. Device according to any one of the preceding claims, wherein said indicator of quality of the sample is selected from among: a Hagberg falling number, a mycotoxin contamination rate, an acrylamide contamination rate, a humidity rate, a protein rate, a sugar content, a hardness, a particle size or also a specific weight.

6. Device according to any one of the preceding claims, wherein the height of the device (1) is less than 75 centimetres, preferably less than 60 centimetres, the width of the device (1) is less than 70 centimetres, preferably less than 55 centimetres, and the depth of the device (1) is less than 55 centimetres, preferably less than 50 centimetres.