Apparatus for analyzing grain by infrared and fluorescence spectroscopy

Abstract

The apparatus (1) for spectroscopic analysis of grain samples includes a first module (200) for infrared analysis, a second module (300) for fluorescence analysis, a third module (400) for specific gravity analysis, and a processing module (500). Each of the first and second modules includes a measurement chamber for receiving at least a portion of the sample, an excitation submodule for emitting at least one generation of electromagnetic radiation in the direction of at least a portion of the sample, a measurement submodule for acquiring at least one electromagnetic spectrum of the sample, and an exhaust system for guiding the sample to the third module. The third analysis module includes a container for receiving the sample and a measurement submodule for measuring the specific gravity of the sample. The processing module includes a memory (510) for receiving data transmitted by a communication network (600), the data including the acquired electromagnetic spectrum and the measured specific gravity, and a processor (520) for combining the data received in the memory and establishing a quality indicator of the sample from the combined data. [Selection diagram] Figure 5

Description

[Technical Field]

[0001] The present invention relates to the field of spectroscopy, and in particular to an apparatus for measuring sample properties by fluorescence and infrared spectroscopy.

[0002] The invention may be applied in particular, but not exclusively, to the pharmaceutical, environmental or food industries, where industrial procedures require precise knowledge of the technological, nutritional and / or toxicological properties of the analyzed samples. In this context, the analysis of samples by spectroscopic techniques allows the extraction of parameters from the samples that are rich in physicochemical information. [Background technology]

[0003] Spectroscopic devices are known that rely on a variety of methods to measure these parameters accurately and in accordance with industry standards. In particular, for grain samples, fluorescence spectroscopy and infrared spectroscopy can separately measure various parameters of these samples.

[0004] However, a drawback of known devices is that they are designed to function in small spaces, such as silos or factory laboratories, with significantly reduced analysis times, i.e., only about 1-3 minutes per sample. Furthermore, measurements must be performed twice: on the one hand using a fluorescence spectrometer and on the other using an infrared spectrometer. Therefore, these separate devices require additional time, space, and acquisition costs, as each instrument is controlled by different processing means and software, making data management more complex, and monitoring the equipment and measurement location logistics more difficult. Furthermore, because these measurements are performed on different samples, the reliability and consistency of measurements performed using separate devices is significantly reduced.

[0005] Furthermore, another drawback is that the known devices significantly complicate the combination of measurements obtained from several different spectroscopic techniques, and are therefore often limited to determining sample parameters individually, but are not adapted to measure them in combination, for example via a combination of fluorescence spectroscopy in the ultraviolet range and infrared spectroscopy.

[0006] In known devices, the measurement and processing of the data obtained from these two types of spectroscopy are carried out in separate, uncoupled devices, which severely limits the commonality in data analysis and therefore the synergies that can be obtained. The lack of technical convergence between the two acquisition modes also makes the task more difficult and complex. Summary of the Invention

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

[0008] To this end, the present invention proposes a single device capable of carrying out measurements of the fluorescence spectrum, the infrared spectrum and the specific gravity of one and the same sample.

[0009] Accordingly, one aspect of the present invention relates to an apparatus for spectroscopic analysis of a grain sample, the apparatus comprising a first infrared analysis module, a second fluorescence analysis module, a third specific gravity analysis module, and a processing module, each of the first module and the second module comprising: a measurement chamber configured to receive at least a portion of the sample; an excitation submodule configured to emit at least one electromagnetic radiation toward at least a portion of the sample; a measurement submodule configured to acquire at least one electromagnetic spectrum of the sample; an ejection system configured to guide the sample towards the third module; Equipped with The third analysis module is a container configured to receive the sample; a measurement sub-module configured to measure the specific gravity of the sample; Equipped with The processing module is connected to each analysis module by a communication network; a memory configured to receive data transmitted by a communication network, the data including an acquired electromagnetic spectrum and a measured specific gravity; a processor configured to organize and combine the received data in the memory and determine a quality indicator of the specimen from the combined data; The present invention is characterized by comprising:

[0010] Various additional features of the device, which may be employed together or separately, include: the excitation sub-module of the first infrared analysis module is configured to emit at least one electromagnetic radiation at a wavelength comprised in the range of 600 to 2500 nanometers, and 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 having a wavelength comprised in the range of 200 to 800 nanometers, and the sub-module of the second fluorescence analysis module comprises a spectrometer configured to acquire at least one spectrum selected from front-on mode fluorescence spectra, i.e. conventional fluorescence spectra acquired at a right angle, acquired at an angle comprised in the range of 30° to 60° relative to the surface of the sample, and fluorescence spectra having a wavelength comprised in the range of 200 to 800 nanometers; the apparatus further comprises a funnel configured to guide at least a portion of the sample towards the first module and the second module; The quality indicators of the sample are selected from the group consisting of Hagberg falling number, mycotoxin contamination rate, acrylamide contamination rate, moisture rate, protein rate, sugar content, hardness, baking strength or other characteristics specific to flour, particle size, or specific gravity; - 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 for the sequential and / or simultaneous measurement of spectral and specific gravity data of a sample, which provides an information synergy that improves the performance of quality indicator predictions that are typically measured by either infrared or fluorescence techniques alone.

[0012] Advantageously, the presence of a measurement sub-module configured to measure the specific gravity of the sample provides a weighing means that makes it possible to determine a key criterion for 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 uniform spectral quality across a wider spectrum, thereby facilitating the pooling of spectrum for later use during fusion.

[0014] Advantageously, the device can be miniaturized, has a low volume and weight, and can be physically integrated into a system comprising multiple analytical modules.

[0015] Advantageously, the device is capable of processing large volumes of samples, which is particularly advantageous when the grain is highly heterogeneous, reducing the impact of sampling on the quality of the calibration and prediction.

[0016] Advantageously, two spectral effluents are generated in one analysis, reducing analysis time before calibration by a factor of two.

[0017] Advantageously, the cost of the device is reduced, thereby allowing the selling price of the device to be very significantly reduced relative to two or three separate devices that separately perform infrared spectroscopy, fluorescence spectroscopy, and specific gravity measurements.

[0018] In the following description, it will be understood that the specific gravity of a sample is the weight per unit volume of that sample, e.g., for grain, it is measured in kilograms per hectoliter. Note that the definition of specific gravity is specific to the measurement of whole grain and meets valid criteria, i.e., specific gravity is not exactly equal to the density of the sample, such as a fluid or solid. [Brief explanation of the drawings]

[0019] Other characteristics and advantages of the present invention will become apparent from the description that follows, without any limiting character, with reference to the accompanying drawings which illustrate examples of embodiments thereof.

[0020] [Figure 1a-1b] 1A and 1B respectively show a side view and a top view of a distribution funnel of an apparatus according to one embodiment of the present invention. [Figures 2a-2c] 2A-2C show a perspective view, a side view, and a top view, respectively, of a first analytical module of an apparatus according to one embodiment of the present invention. [Figure 3a-3b] 2A and 2B respectively show a perspective view and a top view of a second analytical module of an apparatus according to one embodiment of the present invention. [Figures 4a-4c] 1A-1C show a perspective view, a side view and a top view, respectively, of a third analytical module of an apparatus according to one embodiment of the present invention. [Figure 5] 1 illustrates a perspective view of an apparatus according to one embodiment of the present invention; [Figure 6] 1 illustrates a side view of an apparatus according to one embodiment of the present invention. [Figure 7] 1 illustrates, in flow chart form, steps of an analytical method according to an embodiment of the present invention.

[0021] Of course, those skilled in the art can apply modifications to the following description to meet their specific needs. Although different embodiments are mentioned, the present invention is not limited to these specific embodiments, and any modifications specific to the application field of the present invention can be considered as obvious to those skilled in the corresponding art. DETAILED DESCRIPTION OF THE INVENTION

[0022] 1a and 1b show a side view and a top view of a dispensing funnel 100 of an apparatus 1 according to the present invention. A sample, for example a grain sample, is poured onto the funnel 100, which then guides the sample towards other elements of the apparatus 1, as described below.

[0023] In a non-limiting manner, in the following description, the sample poured into the funnel 100 is considered to be a grain sample. In general, this sample may include any grain, flour and / or semolina type, such as barley, wheat, malt, corn, rye, rapeseed, oats, triticale, soybeans, sunflower, buckwheat, spelt, peas, fava beans, lentils, vetch and / or hemp seeds.

[0024] According to one embodiment of the present invention, funnel 100 has the shape of a funnel, for example, a rectangular funnel, with four faces 101, 102, 103, and 104. These four faces are inclined and adapted to guide the poured sample toward the bottom of funnel 100 under the influence of gravity. Each of faces 101, 102, 103, and 104 is connected to at least one of first outlet 120 and second outlet 130, each of which is located at the bottom of funnel 100.

[0025] According to one embodiment of the present invention, the two outlets 120 and 130 of the funnel 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 to separate and distribute the sample entering the funnel 100 into two volumes, the first volume being guided to the outside of the funnel 100 via the first outlet 120 and the second volume being guided to the outside of the funnel 100 via the second outlet 130. In general, the first and second volumes are different.

[0026] The surfaces of funnel 100 can be made of a single type of material or different types of materials, including, for example, metal, stainless steel, or plastic, and are designed to ensure continuous fluid flow and no loss of sample poured from the top of the funnel toward one of the two outlets 120 and 130.

[0027] The two outlets 120 and 130 of the funnel 100 are connected to at least one analytical module by transport guides, e.g., pipes, sliders or conveyors, configured to guide the sample towards at least one analytical module. To improve the guidance of the sample, dividing wheels 140 and 150 can be arranged between the outlets of the funnel and the transport guides to circulate the grain from the funnel towards the transport guides.

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

[0029] According to other, non-represented embodiments of the present invention, the funnel 100 has the shape of a circular funnel. In a non-limiting manner, the funnel 100 includes any number of faces, which can have various shapes, forming a tapered, cylindrical, or square funnel. The two outlets 110 and 120 and the wall 130 can be adapted to these different examples.

[0030] lb, a grain sample poured onto funnel 100 is guided towards first outlet 120 when flowing along surface 102 or along a portion of surface 103, and towards second outlet 130 when flowing along surface 104, along a portion of surface 103, or along a portion of surface 101. According to another not-represented example, a grain sample poured onto funnel 100 is guided towards first outlet 120 when flowing along surfaces 102 and 103 of the funnel, and towards second outlet 130 when flowing along surfaces 104 and 101.

[0031] According to one embodiment of the present invention, the wall 110 can be moved and / or oriented to allow for changing the manner in which the sample is separated into two volumes, thus defining specific values ​​for the first volume that is introduced outside the funnel 100 via the first outlet 120 and the second volume that is introduced outside the funnel 100 via the second outlet 130. For example, the wall 110 can be moved and / or oriented by a control device to change the arrangement or relative sizes of the first outlet 120 and the second outlet 130.

[0032] 2a, 2b and 2c show a perspective view, a side view and a top view of a first analysis module 200 of the device 1 according to one 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 near-infrared radiation from a sample, such as one or more absorbance and / or transmittance spectra. The infrared analysis module can also be configured to acquire one or more reflectance spectra.

[0034] In the framework of the principle 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 this sample. According to one embodiment of the present invention, the electromagnetic beam is emitted by a continuous broadband light source. In variants, other types of light sources can be used, for example, one or more monochromatic light sources.

[0035] A sample exposed to one or more infrared wavelength sources then emits a spectrum of electromagnetic radiation. Analysis of these electromagnetic radiation and the corresponding amounts of energy allows for the estimation of absorbance and / or transmittance spectra from the sample, which can then be used to measure parameters of the sample, such as moisture content, protein content, sugar content, hardness, or particle size.

[0036] The first analysis module 200 comprises a first measurement chamber 210 adapted to receive and accommodate a sample. According to an embodiment of the invention, the first chamber 210 comprises an inlet 211 for receiving this sample, in particular a first volume of the sample, which is guided to the outside of a funnel 100. Preferably, the inlet 211 comprises a funnel adapted to guide the sample towards the inside of the first chamber 210 and to fill it with sample without loss, either manually or automatically.

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

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

[0039] According to one embodiment of the present invention, part of wall 214 and wall 216 is provided with a transparent window, e.g., 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 in wall 216 is frosted so as to be partially or completely transparent to infrared electromagnetic radiation. Advantageously, the use of at least one frosted window in this way improves the quality of the measurable spectra of the sample and limits the dynamic range between these and a reference spectrum measured in the absence of the sample.

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

[0041] The first chamber 210 is provided with a third outlet 212 for discharging the sample outside of it and outside of the first analytical module 200 and directing it towards another element of the device 1 or towards the outside of the device 1. For example, the third outlet 212 can direct the sample towards the inlet of the second analytical module 300 or the third analytical module 400. The third outlet 212, which can be in either an open or closed position, is controlled manually or automatically.

[0042] According to one embodiment of the present invention, the control of the third outlet 212 of the first analysis module 200 is carried out by a first exhaust system 213, which comprises, for example, a motor that can be controlled to automatically open and close the third outlet 212.

[0043] According to one embodiment of the present invention, first wall 214 is a movable wall and second wall 216 is a fixed wall. In particular, wall 214 is movable along a major axis of first analysis module 200 by motor 240. Displacement of first wall 214 relative to wall 216 can increase or decrease the size of first chamber 210, and thus change the thickness or maximum volume of sample that can be contained in first chamber 210. Displacement of first wall 214 relative to wall 216, which can be automated, allows wall 214 to be positioned with an accuracy of less than 0.05 millimeters in a few seconds.

[0044] Due to the great variety of samples that can be analyzed by the device, for example, the size of the grains that make up the sample, the volume density of the sample contained in the first chamber 210 and the light diffusion properties of the sample can vary greatly in each case. For example, the spectral diffusion, absorption, and amplification properties of wheat, corn, and barley samples can vary greatly. Advantageously, adjusting the size of the first chamber 210 according to the sample makes it possible to optimize the quality of the measurements made by the first analysis module 200, when the first analysis module 200 is an infrared analysis module configured to acquire one or more infrared or near-infrared absorption or transmission spectra of the sample.

[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 present invention, when the first infrared analysis module 200 is configured to acquire one or more transmittance spectra, each of these two sub-modules is arranged on a respective side of the first chamber 210. In a variant, these two sub-modules can be arranged on the same side of one of the first chambers 210, for example to enable the acquisition of a reflectance spectrum.

[0046] The first excitation sub-module 220 is configured to emit electromagnetic radiation, particularly infrared radiation, which is emitted by the first excitation sub-module 220 in the direction of 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 that substantially defines a path of radiation emitted by the first excitation sub-module 220, which then passes through the first chamber 210 and is received by the second measurement sub-module 230.

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

[0048] For example, excitation sub-module 220 may comprise a quartz tungsten halogen (QTH) lamp that emits optical radiation from a heated tungsten filament. Preferably, the quartz tungsten halogen lamp is powered at between 25 watts and 50 watts and configured to emit radiation in the wavelength range between 240 and 2700 nanometers.

[0049] The first excitation sub-module 220 is preferably positioned such that radiation is emitted in the direction of the sample, which is then absorbed or scattered by the sample and detected by the second measurement sub-module 230, as described in more detail below. The second measurement sub-module 230 is configured to always transmit the acquired measurements to the processing module.

[0050] Absorption spectroscopy is based on the principle that a material exposed to incident radiation, e.g., infrared radiation, can reflect some of this radiation, absorb some of this radiation, or transmit some of this radiation. In particular, absorption of radiation by the sample causes the sample to produce one or more absorption and / or transmission spectra.

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

[0052] According to one embodiment of the present invention, the spectrometer of the second measurement submodule 230 is integrated in CMOS technology, for example on a silicon-on-insulator (SOI) wafer. According to another embodiment of the present invention, the spectrometer of the second measurement submodule 230 comprises a CCD-type sensor, for example a BI-CCD detector strip with a slot of about 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 comprised between 850 and 1100 nanometers.

[0053] The dynamic range of a spectrometer defines a detection range corresponding to the ratio between the intensity of the maximum signal and the intensity of the minimum signal measurable by the spectrometer. In particular, the spectrometer of the second measurement submodule 230 measures the minimum level of signal corresponding to a measurement made in the absence of a signal, and is characterized by a dynamic range equal to the maximum level of signal measurable by the spectrometer divided by the minimum level. Typically, measurements made in the absence of a signal can be performed by using one or more acquisitions of a spectrum in the absence of a signal, for example 25-50 acquisitions, and calculating the average, root mean square, and / or quadratic values ​​of these acquisitions to define the dynamic range of the spectrometer.

[0054] According to one embodiment of the present invention, the elements of the first analysis module 200 are arranged in a fixed manner so as to avoid any movement of the optical components apart from the first wall 214 when the first wall 214 is fixed. Furthermore, the spectrometer of the second measurement sub-module 230 can be fixed to the second measurement sub-module 230 by one or more mechanical supports. Advantageously, such an arrangement provides an optical chain that allows stable and accurate acquisition of transmittance spectra, especially in the near infrared.

[0055] According to one embodiment of the present invention, the first chamber 210 comprises diffusing elements 216. These diffusing elements 216 can be located at the inlet of the first chamber 210 near the wall 216 and the first excitation sub-module 220 and / or near the first 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 the sample, and a smaller portion of this radiation is transmitted in the direction of the second measurement sub-module 230. Generally, a sample illuminated with infrared radiation absorbs a significant portion of this radiation, which limits the intensity of the signal measured by the spectrometer.

[0056] Advantageously, the placement of a diffusing element, in particular an infrared element, at the inlet and / or outlet of the first chamber 210 can improve the quality of the transmittance spectrum measured by the second measurement sub-module 230 in the infrared and near-infrared ranges. In particular, the placement of a diffusing element reduces the dynamic range, allowing detection of at least an order of magnitude without significantly changing the time required to acquire the spectrum (of the order of 1% of the total measurement time).

[0057] According to one embodiment of the present invention, the diffusing element 216 comprises a diffusing surface made of one or more materials selected from silicon, silica, sapphire, or any type of material that allows increasing the transmission of electromagnetic radiation in the infrared and near-infrared wavelength range. For example, a diffusing element made of a silicon material is preferably transparent to infrared radiation but not to visible light radiation. Advantageously, the grain size of the diffusing element 216 can be varied and selected in combination to obtain the best compromise between reducing the dynamic range and limiting the loss of the measured signal.

[0058] To measure the signal and / or minimum level of the spectrum, the spectrometer of the second measurement submodule 230 includes a shutter 232, e.g., a plate or opaque element, connected to a rotating element 234, e.g., a motor, that moves the shutter. The shutter 232 can be moved manually or automatically between a position away from the inlet of the spectrometer and a position in front of the inlet of the spectrometer. When the shutter 232 is in the away position, the spectrometer is not concealed and receives all electromagnetic radiation emitted toward the spectrometer. When the shutter 232 is in front of the inlet of the spectrometer, the spectrometer is concealed and cannot measure electromagnetic radiation. This mechanism allows the spectrometer to capture the spectrum from the sample contained in the first chamber 210 when the spectrometer is not concealed and to obtain a minimum level of spectrum or noise when the spectrometer is concealed.

[0059] According to one embodiment of the present 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 for passing electromagnetic radiation. According to another embodiment of the present invention (not shown), there is no separating plate between the second measurement sub-module 230 and the first chamber 210.

[0060] 3a and 3b show a perspective view and a top view of a second analysis module 300 of the device 1 according to one 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 front-on fluorescence spectra.

[0062] In the principle of fluorescence spectroscopy, a sample is excited by light radiation of a given wavelength, for example in the visible or ultraviolet range. The fluorescence spectrum preferably spans the spectral range between 200 and 800 nanometers. Using these wavelengths in the framework of conventional or front-on fluorescence spectroscopy makes it possible to measure parameters such as the Hagberg falling number or the mycotoxin or acrylamide contamination rate. The Hagberg falling number allows for the measurement of α-amylase activity present in particular in wheat grains and / or the rapid detection of contaminated or damaged samples or the purity of varieties upon silage entry.

[0063] In response to this excitation, the sample emits radiation, the characteristics of which depend on the components contained in the sample. Based on the measurement of this luminescence radiation, it is possible to deduce the corresponding fluorescence spectrum / spectrum from the luminescence radiation. Processing these fluorescence spectra, preferably acquired in the spectral range of 200 to 800 nanometers, using preprocessing, decomposition, and modeling tools such as development, allows for the extraction of information such as the Hagberg falling number, mycotoxin contamination, and other parameters characterizing the degree of germination of grains contained in a given volume of sample.

[0064] The second analysis module 300 comprises a second measurement chamber 310 configured to receive and accommodate a sample. According to one embodiment of the invention, the second chamber 310 comprises an inlet 311 for receiving this sample, e.g. a second volume of the sample, which is guided to the outside of the funnel 100. Preferably, the inlet 311 comprises a funnel adapted to guide the sample towards the inside of the first chamber 310 in order to fill the first chamber 310 without losing any sample, either manually or automatically.

[0065] The second chamber 310 is provided with a fourth outlet 312 for discharging the sample and directing it outside the second analysis module 300 towards another element of the device 1, for example towards the inlet of the third analysis module 400. The fourth outlet 312, which can be in either an open or closed position, is controlled manually or automatically. In particular, the opening and closing of the fourth outlet 312 can be performed manually or automatically by a second discharge system 313, which can be motorized.

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

[0067] According to one embodiment of the present invention, the second chamber 310 further comprises a detection element, such as an optical, mechanical or electronic detector, for determining whether a sample is present in the second chamber 310 and preferably in what volume.

[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 being preferably such that they are positioned on the same side of one of the second measurement chambers 310 to enable measurement of the front fluorescence spectrum.

[0069] In a variant, other configurations can be considered to enable acquisition of conventional or front-on fluorescence spectra. For example, in a configuration provided for acquisition of front-on fluorescence spectra, the opening 314 of the second chamber 310 is located on the same side as the third excitation sub-module 320 and the fourth measurement sub-module 330. In a variant, the third excitation sub-module 320 and the fourth measurement sub-module 330 can be located on different sides of the second chamber 310 in other configurations.

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

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

[0072] In a non-limiting embodiment, the light sources of the opto-mechanical component 321 include monochromatic or polychromatic radiation sources. For example, these light sources include light emitting diodes or laser light sources. The third excitation sub-module 320 and / or the opto-mechanical component 321 can include other optical elements, such as focusing or diffusing elements, e.g., lenses. For example, the opto-mechanical component 321 includes a lens configured to focus or diffuse electromagnetic radiation passing therethrough.

[0073] According to one embodiment of the present invention, the optical-mechanical component 321 comprises an opening configured to allow electromagnetic radiation, in particular electromagnetic radiation emitted by a sample placed in the second chamber 310, to pass in the direction of the fourth measurement sub-module 330.

[0074] According to one embodiment of the present invention, the opto-mechanical component 321 is circular and includes a predetermined number of light sources, which number is between 1 and 20, and preferably between 1 and 10.

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

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

[0077] According to one embodiment of the present invention, the second chamber 310, the third excitation sub-module 320 and the fourth measurement sub-module 330 are arranged towards the fourth measurement sub-module 330 along an axis corresponding to the axis of the path of the electromagnetic radiation emitted by the sample in the second chamber 320. The fourth measurement sub-module 330 is arranged so as to be able to receive the electromagnetic radiation coming from the sample contained in the second chamber 310 after excitation of this sample. The fourth measurement sub-module 330 is configured to always transmit the acquired measurements to the processing module.

[0078] According to one embodiment of the present invention, the fourth measurement sub-module 330 is configured to measure one or more fluorescence spectra, e.g., ultraviolet and visible front-on fluorescence spectra, and includes a spectrometer compatible with wavelengths ranging from 200 to 800 nanometers. The spectrometer of the fourth measurement sub-module 330 is located on approximately the same side as the third excitation sub-module 320 to enable acquisition of front-on fluorescence spectra. Compared to other types of fluorescence spectra, acquisition of front-on fluorescence spectra avoids the generation of significant analytical errors related to the sample, its preparation, or external conditions such as temperature and pressure. Therefore, the results obtained are more accurate and can be determined more quickly.

[0079] As with the spectrometer of the second measurement sub-module 230, the spectrometer of the fourth measurement sub-module 330 is configured to further acquire a signal and / or minimum level spectrum, which can be performed without the need for a shutter by performing the measurement when the light source of the third excitation sub-module 320 is off.

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

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

[0082] According to one embodiment of the present invention, the second chamber 310, the third excitation sub-module 320, and the fourth measurement sub-module 330 are fixed to the second analysis module 330 by one or more mechanical supports. This configuration avoids movement of mechanical parts and provides an optical chain that allows stable and accurate acquisition of fluorescence spectra, especially front-on fluorescence spectra and / or other types of spectra. Advantageously, the second analysis module 300 is compact and does not integrate any moving optical components. This compactness and stability improve the sensitivity and reproducibility of measurements during acquisition of fluorescence spectra, while facilitating standardization of the instrument.

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

[0084] According to one embodiment of the present invention, the control of the fourth outlet 312 of the second analysis module 300 is carried out by a second exhaust system 313, which comprises, for example, a motor that can be controlled to open and close the fourth outlet 312.

[0085] 4a, 4b and 4c show a perspective view, a side view and a top view of a third analytical module 400 of the device 1 according to an embodiment of the present invention. According to an embodiment of the present invention, the third analytical module 400 is a module for measuring weight configured to measure the specific gravity of a sample.

[0086] The third analytical module 400 is connected to the rest of the device 1. According to one embodiment of the present invention, the third analytical 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 gravity of the same sample coming from the first analytical module 200 and the second analytical module 300. In a variant, the third analytical module 400 is connected to the first outlet 120 and / or the second outlet 130 of the funnel 100.

[0087] The third analytical module 400 includes 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 that stabilizes it and can have different sizes and shapes.

[0088] According to one embodiment of the present invention, the container 410 is a container having a cylindrical, parallelepiped or tapered shape, and has a filling volume comprised between 100 ml and 1000 ml, preferably 500 ml.

[0089] According to one embodiment of the present invention, the third analysis module 400 comprises a fifth measurement sub-module 430 disposed below 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 container 410 is empty or when it is partially or completely filled with sample.

[0090] According to one embodiment of the present invention, the third analytical module 400 comprises a detection element, for example an optical or mechanical detector, for determining whether a sample is present in the container 410 and preferably in what volume.

[0091] According to one embodiment of the present invention, the third measurement module 400 comprises a leveling element 415, such as a leveling strip or a leveling spring, configured to move on or within the container 410 in order to modify the sample contained in the container 410.

[0092] The displacement of the leveling element 415 is automated to ensure highly reproducible measurements of the weight of the sample contained in the container 410 .

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

[0094] The fifth measurement sub-module 430 is configured to constantly transmit the obtained measurements to the processing module and calculate the specific gravity of any sample contained in the container 410 from the measured weight and measured volume of this sample. Advantageously, the third analysis module 400 provides a compact and accurate means for measuring the specific gravity of grain samples with high precision, reproducibly at locations outside or inside the grain silo.

[0095] The container 410 comprises a fifth outlet 412 for discharging and directing the sample towards the outside of the container 410 and the outside of the third analysis module 400, e.g., the outside of the device 1. The fifth outlet 412, which can be in either an open or closed position, can be controlled manually or automatically. According to one embodiment of the invention, the control of the fifth outlet 412 of the third analysis module 400 is performed by a third outlet system 413, which comprises, for example, a motor that can be controlled to open and close the fifth outlet 412.

[0096] According to one embodiment of the present invention (not shown), the third analysis module 400 is equipped with a cleaning system configured to clean the platform 416 and / or the inside of the container 410 before or after ejection of the sample outside the container 410.

[0097] Thus, the third analytical module 400 allows for an accurate measurement of the specific gravity of the sample contained in the container 410, obtained from measuring the weight of the sample in the container. The third analytical module 400 further allows for the measurement of the tare weight, i.e., the weight of the container when it is empty. Thus, by subtracting the measured tare weight from the weight obtained in the presence of the sample and using a calibration formula, it is possible to accurately determine the specific gravity of the sample.

[0098] 5 and 6 show a perspective view and a side view, respectively, of an apparatus 1 according to the present invention, which comprises the above-mentioned funnel 100, the first analytical module 200, the second analytical module 300 and the third analytical module 400.

[0099] According to one embodiment of the present invention, the distribution funnel 100 and the third analytical module 400 are connected to the first analytical module 200 and the second analytical module 300, respectively, by guides to enable guiding the sample from the distribution funnel 100 towards the first analytical module 200 and the second analytical module 300, and then from each of the first and second analytical modules 200 and 300 towards the third analytical module 400, under the influence of gravity. The sample is then discharged below the third analytical module 400.

[0100] The device 1 further comprises a processing module 500. In Figures 5 and 6, the processing module 500 is represented as a laptop, but it can also be any type of electronic or computerized processing means, for example a processor, a desktop computer, a smartphone or any device similar to a terminal equipped with a control screen, a USB stick, a mobile memory card or 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 analytical modules of the device 1, by a communication network 600. The communication network 600 allows the processing module 500 to be connected to the analytical 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 an Ethernet network. In any case, the communication network 600 is configured to transmit information between the processing module 500 and each analytical module of the device 1.

[0102] According to one embodiment of the present 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 the inlets and outlets of the analytical modules 200, 300 and 400 and / or the funnel 100. Advantageously, the processing module 500 allows to manage the measurements made by the device 1 either manually or automatically, by following the method steps as described below with respect to FIG.

[0103] The processing module 500 comprises a memory 510 configured to receive data transmitted by the communication network 600. This data may include any type of information measured by the analytical modules, such as the wavelengths of radiation emitted by the sample in any of the analytical modules, the measured intensity of these radiations, the corresponding electromagnetic spectrum, or the tare weight and specific gravity measured by the third analytical module 400.

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

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

[0106] Processor 520 is configured to organize data and spectra, particularly fluorescence spectra, infrared spectra, and specific gravity spectra, acquired by analysis modules 200, 300, and 400, to perform digital, computerized processing of the data and spectra. For example, processor 520 organizes the fluorescence data into a three-dimensional table, with the three dimensions corresponding to the wavelength of the excitation electromagnetic radiation used, the wavelength of the sample's emission radiation measured by the spectrometer in response to this excitation, and the intensity of this emission radiation. Processor 520 organizes the infrared data into a separate table, e.g., two or three dimensions.

[0107] The processor 520 is configured to perform a combination of data and spectra, more specifically data organized in tables. For example, a first approach consists of concatenating the fluorescent data and infrared data tables into one and the same table. Advantageously, this first approach returns to juxtapose the spectra corresponding to this data across the entire wavelength range of the acquired spectrum. A second approach consists of creating a spectral image of the sample from the combination of the fluorescent spectrum and the infrared spectrum. Advantageously, this combination makes it possible to obtain a three-dimensional image that preserves the three-dimensional structure of the associated fluorescent data tables. A third approach consists of constructing a two-dimensional spectral image resulting from the combination of the first and second approaches.

[0108] To carry out the combination of spectroscopic data and determine quality indicators such as Hagberg falling number, mycotoxin contamination rate, acrylamide contamination rate, moisture rate, protein rate, sugar content, hardness, baking strength, flour-typical properties, particle size or specific gravity, one can refer to the reference "Infrared Spectroscopy and Its Analytical Applications" (2006) by D. Bertrand and E. Dufour for data from infrared spectra, and to the journal "Fluorescence Spectroscopy and Chemometrics in the Food Classification - A Review" by J. Sadecka and J. Tothova, Czech Journal of Food Sciences 25(4):159-173 (2007) for data from fluorescence spectra. For data fusion, you 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] Analysis of the pre- and post-fusion data is then performed by applying multivariate or multi-pass statistical models known in the art with a view to predicting one or more quality indicators. The weighting measures obtained from the third analysis module 400 allow the user or the processing module 500 to more accurately select a statistical model that corresponds to the type of sample being analyzed.

[0110] Furthermore, the processor 520 is configured to determine at least one indicator of the quality of the sample from the data and the spectrum combined by any of these techniques. According to one embodiment of the present invention, these quality indicators are selected from among the Hagberg falling number, mycotoxin contamination rate, acrylamide contamination rate, protein rate, sugar content, baking strength or other flour properties, hardness, particle size or specific gravity.

[0111] Advantageously, calculating the quality index of a sample from the combined data rather than from separately obtained data can improve the accuracy of the prediction of a quality index selected from moisture percentage, protein percentage, mycotoxin contamination percentage, Hagberg falling number or specific gravity. Knowledge of the specific gravity of the sample measured in the third analysis module 400 makes it possible to further improve the accuracy of this prediction through the selection of a statistical model fitted to the sample analyzed by the device 1.

[0112] According to one embodiment of the present invention, the maximum dimensions of device 1 are 75 centimeters high, 70 centimeters wide, and 55 centimeters deep. For example, device 1 has dimensions of approximately 71 centimeters high, 65 centimeters wide, and 45 centimeters deep. Preferably, device 1 has dimensions of approximately 60 centimeters high, 55 centimeters wide, and 50 centimeters deep.

[0113] According to one embodiment of the present invention, the device 1 and / or some of its elements are enclosed in a sealed casing to isolate them from external conditions such as, for example, the presence of dust, temperature fluctuations or effects related to the transport of the device.

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

[0115] According to one embodiment of the present invention, the second analysis step E200 performed by the first analysis module 200 aims to acquire an infrared or near-infrared spectrum of the sample and comprises the following steps: substep E210 of filling the first chamber 210 with the sample, substep E210b of detecting the filling of the first chamber 210 by the detection element of the first analysis module 200, substep E220 of exciting the sample by the first excitation submodule 220, substep E230 of acquiring at least one infrared or near-infrared spectrum by the first measurement module 230, substep E213 of ejecting the sample outside the first chamber 210 via the first exhaust system 213 towards the third analysis module 400, substep E240 of acquiring at least one spectrum blocked by the first module 230 when its spectrometer is shielded by the shutter 232, and substep E250 of transmitting the spectra acquired during step E200 towards the processing module 500.

[0116] According to one embodiment of the present invention, the filling substep E210 is preceded by a step of acquiring a reference spectrum, i.e. a spectrum step of the empty source. In a variant, this step of acquiring a reference spectrum can be followed directly by the substep E213 of ejecting the sample.

[0117] In a variant, the substep E213 of discharging the sample can be performed either after the substep E240 of acquiring at least one block spectrum and the transmitting substep E250. According to another variant, the substep E240 of acquiring at least one block spectrum can be performed before the substep E210 of filling the first chamber 210 with the sample. The filling substep E210 can further comprise a substep E210b of detecting the filling of the first chamber 210 by a detection element of the first analysis module 200.

[0118] According to one embodiment of the present invention, the third analysis step E300, performed by the second analysis module 300, aims to acquire at least one fluorescence spectrum and a block spectrum of the sample through the following substeps: substep E310 of filling the second chamber 310 with the sample, substep E320 of exciting the sample by the third excitation submodule 320, substep E330 of acquiring at least one fluorescence spectrum by the fourth measurement submodule 330, substep E313 of ejecting the sample outside the second chamber 310 via the second ejection system 313, substep E340 of acquiring at least one block spectrum by the fourth measurement submodule 330 when the light source of the third excitation submodule 320 is turned off, and substep E350 of transmitting the spectrum acquired during the third step E300 towards the processing module 500. In a variant, substep E313 of ejecting the sample can be performed after either substep E340 of acquiring at least one block spectrum or substep E350 of transmitting. The filling substep E310 may further comprise a substep E310b of detecting the filling of the second chamber 310 by means of a detection element of the second analysis module 300.

[0119] According to one embodiment of the present invention, the fourth analysis step E400, performed by the third analysis module 400, aims to determine at least one specific gravity and tare weight of the sample through the following substeps: substep E405 of measuring a tare weight corresponding to the empty weight of the container 410, substep E410 of filling the container with the sample, substep E415 of measuring the surface level of the sample by means of the leveling element 415, substep E420 of measuring the specific gravity of the sample contained in the container, substep E440 of discharging the sample out of the container 410 by means of the third discharge system 413, and substep E450 of transmitting the specific gravity and tare weight measurements to the processing module 500. The filling substep E410 may further comprise a substep E410b of detecting the filling of the container 410 with the sample by means of a detection element of the third analysis module 400.

[0120] According to one embodiment of the present invention, the fifth processing step E500 performed by the processing module 500 aims to determine a quality indicator of the sample through the following substeps: substep E510 of receiving data coming from the first analysis module 200, the second analysis module 300 and the third analysis module 400, substep E520 of combining this data, substep E530 of applying at least one multi-path statistical model, and substep E540 of predicting at least one quality indicator based on the previous substeps. The fifth processing step E500 may further include a substep E525 (not shown in FIG. 7 ) consisting of determining at least one multi-path statistical model according to the value of the specific gravity of the sample transmitted to the processing module 500 during substep E450, substep E525 being performed before substep E530 of applying at least one multi-path statistical model.

[0121] Of course, those skilled in the art can apply modifications of the foregoing description to meet their particular needs. 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 found in the field of application of the present invention will be apparent to those skilled in the art.

Claims

1. An apparatus (1) for spectroscopic analysis of a grain sample, said apparatus comprising a first infrared analysis module (200), a second fluorescence analysis module (300), a third specific gravity analysis module (400), and a processing module (500), wherein each of said first infrared analysis module (200) and second fluorescence analysis module (300) comprises: a measurement chamber (210, 310) configured to receive at least a portion of the sample; an excitation sub-module (220, 320) configured to emit at least one electromagnetic radiation towards at least a portion of the sample; a measurement sub-module (230, 330) configured to acquire at least one electromagnetic spectrum of said sample; an evacuation system (213, 313) configured to guide the sample towards the third density analysis module (400); Equipped with The third gravity analysis module (400) a container (410) configured to receive said sample; a measurement sub-module (430) configured to measure the specific gravity of said sample; Equipped with The processing module (500) is connected to each analysis module (200, 300, 400) by a communication network (600); a memory (510) configured to receive data transmitted by the communication network (600), the data including electromagnetic spectra acquired by the first infrared analysis module (200) and the second fluorescent analysis module (300) and specific gravity measured by the third specific gravity analysis module (400); a processor (520) configured to organize and combine the data received in said memory and determine a quality indicator of said sample from the combined data; Equipped with the measurement chamber (210) of the first infrared analysis module (200) comprises a first wall (214) at a first end and a second wall (216) at a second end, the first wall (214) and the second wall (216) comprising transparent windows, the window of the second wall (216) being frosted to partially or completely transmit infrared electromagnetic radiation; An apparatus characterized in that

2. 2. The apparatus of claim 1, wherein the excitation sub-module (220) of the first infrared analysis module (200) is configured to emit at least one electromagnetic radiation at a wavelength between 600 and 2500 nanometers, and 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. 3. The apparatus of claim 1, further comprising a funnel (100) configured to guide at least a portion of the sample toward the first infrared analysis module (200) and the second fluorescence analysis module (300).

4. 4. The apparatus according to claim 1, wherein the indicator of quality of the sample is selected from Hagberg falling number, mycotoxin contamination rate, acrylamide contamination rate, moisture rate, protein rate, sugar content, hardness, particle size, or specific gravity.

5. 5. The device according to any one of claims 1 to 4, wherein the height of the device (1) is less than 75 centimeters, the width of the device (1) is less than 70 centimeters, and the depth of the device (1) is less than 55 centimeters.

6. 6. The device of claim 5, wherein the height of the device (1) is less than 60 centimeters, the width of the device (1) is less than 55 centimeters, and the depth of the device (1) is less than 50 centimeters.

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