WO2000064242A1 - Tete de mesure pour dispositif servant a analyser des produits - Google Patents

Tete de mesure pour dispositif servant a analyser des produits Download PDF

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Publication number
WO2000064242A1
WO2000064242A1 PCT/NL2000/000273 NL0000273W WO0064242A1 WO 2000064242 A1 WO2000064242 A1 WO 2000064242A1 NL 0000273 W NL0000273 W NL 0000273W WO 0064242 A1 WO0064242 A1 WO 0064242A1
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WO
WIPO (PCT)
Prior art keywords
sensor
source
radiation
light
milk
Prior art date
Application number
PCT/NL2000/000273
Other languages
English (en)
Dutch (nl)
Inventor
Johannes Dommerholt
Johannes Bernardus Maria Wilmink
Petrus Cornelus Franciscus Borsboom
Original Assignee
Coöperatie Rundveeverbetering Delta U.A.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from NL1011905A external-priority patent/NL1011905C2/nl
Application filed by Coöperatie Rundveeverbetering Delta U.A. filed Critical Coöperatie Rundveeverbetering Delta U.A.
Priority to AU46246/00A priority Critical patent/AU4624600A/en
Publication of WO2000064242A1 publication Critical patent/WO2000064242A1/fr

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84Systems specially adapted for particular applications
    • G01N21/85Investigating moving fluids or granular solids
    • G01N21/8507Probe photometers, i.e. with optical measuring part dipped into fluid sample

Definitions

  • the invention lies in the field of measuring heads for analysis of products, for instance raw milk, faeces, manure, soil, urine, fruit (slices) , potatoes, (slabs of) tooth material etc., hereinafter regularly referred to for the sake of brevity as "products”.
  • products for instance raw milk, faeces, manure, soil, urine, fruit (slices) , potatoes, (slabs of) tooth material etc., hereinafter regularly referred to for the sake of brevity as "products”.
  • the invention provides a measuring head for a device for direct analysis of products, such as milk given by lactating animals, for instance raw milk, processed milk such as fermented milk, yoghurt and the like, faeces, manure, urine, fruit slices, potatoes, slabs of tooth material etc., such that the value of at least one parameter is measured or detected, for instance the total quantity of milk from one milking session, the milk flow rate during milking, the structure, the fat content, the fatty acid composition, the protein content, the protein composition, the number of somatic cells optionally specified per type, urea content, ketone body content, determining of ketone body details, hormone levels, lactose content, blood content, beestings characteristics, which device comprises: a spectrophotometer with: a source of electromagnetic radiation with at least one chosen spectral component in the wavelength range of about 300-2500 nm; a photosensor which is sensitive to at least the first, second and third, and optionally the fourth harmonics or
  • a separate light-conducting assembly such as is used for connection to the carrier for the source or the sensor, it is possible to test the light-conducting assembly in advance, prior to assembly with the carrier, for the desired light transmission characteristics. This results in an optimization of the optical path for each of the measuring heads produced in this manner.
  • the carrier with the source or the sensor thereon can also be separately tested before being connected to the light-conducting assembly. Such a connection can be effected by integral moulding of both elements.
  • the source will usually comprise a number of elements, for instance a lens, each having its own frequency characteristic. The assembly of sources on the carrier can thus be tested, if required even in combination with a local variation in the transmission characteristics of the light-conducting assembly as a function of the different frequency characteristics of the source elements.
  • measuring head By dividing production of the measuring head into a light-conducting assembly and a carrier for sources or sensors a simplification of the production process is achieved, more reliable measuring heads can be provided, which measuring heads can also be simpler and easier to produce, and so on.
  • Calibration of the indirect measurement by means of the device according to the invention can take place via a chemical and/or physical analysis of a series of samples.
  • sensitivity In order to monitor the operation of the analysis device according to the invention a distinction can be made in respect of testing inter alia the following relevant properties: sensitivity, dark current noise, contamination, temperature characteristics, wear, ageing.
  • calibration standards usually comprising a diffuse white or a black reflector or neutral grey filters which is or are placed at a distance from or in a measuring head.
  • the monitoring measurement is carried out daily, weekly or monthly.
  • the application of a white or fluorescent reference liquid can be envisaged.
  • the above overview relates to all monitoring of functions of the physical system.
  • Another component of the calibration relates to the deriving of spectral information, on which the device according to the invention is after all based, as to the composition of the product for analysis.
  • Diverse “conversion methods” are available for this purpose. All calculations are however based on, and therefore dependent on, so-called wet chemical analysis or physical analysis of the composition.
  • the problems here are sensitivity, reproducibility, error margins of the reagents used and reactions, and so on.
  • Standard software can be used for derivation, for instance Unscramble from the company Camo, ' or similar calculations based on multivariation analysis, or applying neural networks.
  • 300-2500 nm is based on typical, and partly overlapping optical absorption bands of C-H, O-H or N-H bonds of chemical type. Spectroscopy in the range 300-2500 nm has the advantage compared to other per se known measuring methods such as FTIR, Raman and NMR of a low production and purchase price and simple operation.
  • the NIR spectral range which lies roughly in the order of 700- 2500 nm, comprises the range within which the harmonics of molecule vibrations are relevant.
  • the first resonance frequency or second harmonic relates for instance to the range of 1400-1800 nm; the third harmonic to about 950- 1200 nm and the fourth harmonic to 700-925 nm.
  • the optical characteristics of the object for measuring are the optical characteristics of the object for measuring, particularly the wavelength-dependent absorption and scattering coefficients. These properties determine to a considerable extent the conditions for an optimal measurement geometry and the associated sensitivity, accuracy and reproducibility of the measuring method. It has been found from absorption measurements on water that the absorption coefficient increases sharply as a function of the wavelength. This relates to the absorption of H 2 0 (O-H band) .
  • the fourth harmonic lies in the order of 745 nm, third harmonic in the order of 975 nm and the second harmonic at about 1485 nm and the first harmonic at 1940 nm.
  • the scattering characteristics are determined inter alia by the form of the particles, particle sizes, the distribution of the particle sizes, the distribution of the particles, variation of the refractive index (wavelength-dependent functions) .
  • the scattering characteristics can often be directly derived as to the structure of specific components.
  • Material with scattering cores with dimensions smaller than the wavelengths used display scattering characteristics differing from scattering cores larger than the wavelengths used.
  • the characteristics are considerably more complex in the case of a combination of multiple types of scattering cores, such as is the case with milk (dimensions micelles about 80 nm, fat particles on average about 1000 nm and somatic cells around 15 ⁇ m) and many other materials, whether or not they are biological.
  • the scattering coefficient generally decreases in the visual and the NIR range as wavelength increases.
  • the decrease in the scattering coefficient and the increase in the absorption coefficient in the range 300-2500 nm results in a practically applicable window for measuring techniques based on transmission and/or volume reflection with a relatively long optical path.
  • the anisotropic scattering characteristics dependent on wavelength and particle size the measuring result in the case of transmission will depend mainly on the forward scatter effect.
  • volume reflection the measuring result will depend mainly on backward scattering effects.
  • the choice for transmission measurement or volume reflection measurement, or a combined transmission and volume reflection measurement in one measuring device is also determined by a desired sensitivity for particular particle structures. Form and position of the window in the relevant spectral range depend on the optical properties of the object for measuring.
  • the ideal measurement geometry depends not only on the optical properties of the object but also on practical conditions, such as (potential and possibly progressive) contamination of measuring window, foam formation, flow, separation and so on. It is found in practice that measurement in the largest possible measurement volume is desirable in respect of possible intra-variation in the object and a smaller influence of possibly contaminating or contaminated measuring windows.
  • a long optical path through the object for measuring provides more reliable information than a short optical path.
  • the maximal optical path is however limited by the minimum permissible signal/noise ratio.
  • volume reflection measurement For milk and other light-scattering materials into which the light can penetrate deeply over a distance of many millimetres, a volume reflection measurement (measurement wherein in the measuring surface there is some distance between the source surface and the sensor surface and the radiation is thus forced to cover a certain distance in the milk, also referred to as forced minimal optical path) is strongly recommended over a reflection measurement (wherein depending on the scattering characteristics of the light-scattering materials the optical path can be very short) .
  • volume reflection wherein the adverse effects of surface reflection are precluded
  • the back-scattering characteristics resulting from the internal material structure are applied and optical path lengths of 10 mm and more can be realized.
  • An objective measure for a correct measuring device and wavelength range relating to a specific object for measuring is the contrast for the wavelength-dependent absorption and scattering characteristics in an obtained spectrum.
  • Various aspects can be tested with a model to be manufactured from suspensions on a basis of commercially obtainable latex particles of different relevant dimensions and the addition of different commercially obtainable absorbers .
  • For transmission and volume reflection measurements use can be made in the wavelength range of about 300- 2000 nm of relatively inexpensive, commercially obtainable detectors, at this moment for instance InGaAs, Si and Ge detectors or combinations thereof.
  • An LED or a polymer LED can optionally be provided with a transmission interference filter to reduce the band width of the emitted electromagnetic radiation from for instance 50-100 nm to about 10-20 nm.
  • the wavelength range can be subdivided into a number of bands. For the relevant range use can for instance be made according to the invention of a subdivision into ten to twenty spectral bands. If it is desired to perform a larger or smaller number of parameter value measurements, this number can optionally be further increased or decreased. In the case of in-line milk analysis very good results have been achieved with a test arrangement.
  • the wavelengths of not only the detector (s) but also of the light source or light sources can be selected such that the spectral analysis according to the invention can produce measurement results which correspond with the values of desired parameters as stated above, for instance fat content, fatty acid composition, protein content and so on. It has been found that wavelength-dependent measurements can show which wavelengths produce the best analysis results for the different parameters and parameter groups to be tested.
  • These wavelengths can also be implemented in an embodiment of the device according to the invention wherein LEDs are applied as radiation sources, and a plurality of sources can be applied which are each tuned to a spectral range associated with one parameter.
  • the device according to the invention could prove useful on the basis of, among others, the following considerations which relate to direct control in the short term, these considerations relating to the field of application of this invention stated as example, i.e. dairy farming:
  • the device according to the invention is important for a dairy plant since during the qualitative separation of milk at the farm a distinction can already be made between various raw main component categories, whereby an extra added value and possibly lower processing cost-price can be realized
  • the devices according to the invention are also important for suppliers of data transmission systems and providers of telecommunications facilities. Central use of information or data-mining is also possible. In this way a statistical analysis of measurement data can for instance take place, deeper analysis of the data can take place to obtain information about individual lactating animals and, for instance on the basis of an interactive system, report-back to the dairy farm can be realized
  • fat ca . D *o protein ca . s lactose ca. 2.5 % cell number 0-150,000 ca. 10 % cell number 150,000-1,000,000 ca. 30 % blood detection for presence suffices beesting characteristics detection for characteristics suffices
  • the total accuracy to be realized per parameter corresponds with the given relative accuracy for each individual measurement as according to the above table divided by the root of the number of measurements. It will be apparent that with an increase in the number of measurements the effective measurement accuracy can be substantially improved.
  • dairy farming a minimum of 1,000,000 measurements, 1,000 cows, 10 farms with identical measuring systems, more extensive and better calibration information can be obtained relating to inter alia diverse types of milk abnormalities, general health of the lactating animals, feed conversion, oestrus, genetic properties and so on.
  • the invention provides the option in the field of application of dairy farming mentioned as example of analysing the composition of the milk per cow and during the milking session, and in particular of monitoring the milk cycle integrally and of achieving an added value for the whole cycle.
  • the measurement results on the basis of the invention enable a monitoring in respect of inter alia:
  • the milk quality such as: fat, protein, lactose (possibly including determining of details, for instance fatty acid composition and protein components)
  • the measurement results and/or monitoring results can be used for immediate control (destination of the milk and other actions during milking) as well as for aspects typified by a longer (permitted) response time, including matters concerning:
  • the automatic process input parameters include (see for instance figure 12):
  • the milk-monitoring information system to be set up on the basis of the invention can provide and/or monitor control tasks wholly independently, in combination with reporting to a central data processing system.
  • control at the farm can be envisaged specific feed, separate destination for the milk, individual adjustment of the milking installation, a change in the accommodation of the cow and so on.
  • the diary farmer may have to perform manual operations at an alarm signal.
  • the other process information which can be recorded during milking and which can optionally be input manually into the device according to the invention, relates to udder damage and other physiological evaluation and empirical data identifiable by the farmer.
  • Data to be input before or after milking relates inter alia to:
  • the criteria of the milk-monitoring information system therefore include objective measurement results, experience, physiological timing, results of internal and external measurements, monitoring, control, statistical evaluations and other aspects.
  • Such a system can be deemed a continuous learning and management system in which the dairy farmer, as a trained professional, can play an essential part and with which he can increase his skills.
  • the software embodiment of a system according to the invention can develop into an expert system on the basis of for instance neural networks, multivariation analysis and other forms of data-warehousing and data- mining.
  • Use can be made of a white source with monochromator of known type. Use can also be made of sources and detectors which individually or in combination define diverse spectral measurement windows. Use can for instance be made of a number of light conductors to guide the light from a source (for instance from a monochromator) to the measurement window of the source.
  • the practical implementation of the device according to the invention will be based on the use of a signal processing unit into which data can be entered manually on the one hand and in which data originates from the sensor on the other.
  • the signal processing unit can be coupled to other such signal processing units or pass its data to a central signal processing unit, for instance via a date transmission line, such as a telephone line, or the like.
  • dairies control on the basis of quality, lower cost-price, higher quality of the half-product and the end product
  • suction means comprise a ring of holes connecting onto a suction pump around the active outer surface of the source and/or the sensor.
  • the device can be provided in a particular embodiment with a grey filter, for instance with the attenuation of 1 decade, for moving optionally in and out of the radiation path.
  • the distance between the active end surfaces of the source and of the sensor is adjustable.
  • the sample for measuring will have a layer thickness which is adjustable to correspond with a desired thickness.
  • the volume reflection or the transmission is thus determined by a well-defined layer of the sample.
  • the thickness of the applied plastic foil material of the plastic bag will be small in proportion to the layer thickness of the sample for measuring, or can be compensated by pre-measurement .
  • the sample holder must be positioned and filled such that the liquid or the solid of the object for measuring is separated by the force of gravity from the air or the gas in the sample holder such that the object for measuring is situated between the measuring surfaces .
  • Essential for a high sensitivity of the analysis device is the largest possible optical path through the sample/object for measuring. The maximum length of the optical path is determined by the permissible signal/noise ratio. In a transmission measuring device this can be adjusted by adjusting the distance between the source and the sensor; there is no possibility of adjustment in volume reflection measurements, but the distance is determined by the distance between the concentric lighting source and the sensor surface. The distance is further determined by the optical properties, the scattering properties and the absorption properties of the sample.
  • an optically neutral density filter with known transmission characteristics can be arranged in the optical path. This can be used in determining a dynamic measurement range.
  • the diameter of the light beam in the transmission measuring arrangement can be adapted to the geometry of the object for measuring, or dimensioned, in particular be so small, such that position-dependent variations in the composition of the object can be scanned by positioning the object relative to the radiation beam.
  • figure 1 shows a broken-away perspective view of a mould in which a number of elements are received for manufacture of a sensor according to the invention
  • figure 2 shows the finished sensor removed from the mould of figure 1 and without a source and a photosensor
  • figure 3 shows an exploded view of a volume reflection spectrophotometer measuring head with LEDs and sensor chip
  • figure 4 shows a transparent perspective view of the finished measuring head of figure 3
  • figure 5 is a broken-away perspective view of a possible arrangement of a transmission spectrophotometer
  • figure 6 is a view corresponding with figure 5 of a volume reflection variant
  • figure 7 is a perspective view of another variant
  • figure 8 shows a partly transparent side view of a following variant
  • figure 9 is a partly broken-away perspective view of yet another variant
  • figure 10 is a partly broken-away perspective view of a reflection variant with a transparent measuring window
  • figure 11 is a partly broken-away perspective view of the so-called milk collector of a milking
  • Figures 1, 2, 3 and 4 show the manner in which a particular embodiment of an integrated source and photosensor with associated optical structure can be manufactured.
  • Placed centrally in a round cup-shaped mould 1 is a perspex cone 2 and a perspex cylinder 3 placed co-axially therewith.
  • the spaces between respectively cone 2 and cylinder 3 and cylinder 3 and the standing wall of mould 1 are then filled with a plastic mass curing to an opaque ring respectively 4, 5.
  • plastic rings 4,5 After curing of plastic rings 4,5 the thus integrally formed unit 2, 3, 4, 5 is removed from the mould. This is the stage shown in figure 2.
  • Figure 3 shows positioning of a disc-like ring 6 which bears a ring of light-emitting diodes as LEDs 7.
  • This ring 6 also fulfils the function of printed circuit board to which LEDs 7 are soldered, which printed circuit board also carries an electronic circuit for controlling the LEDs and processing the signal from chip 8. The nature of these LEDs 7 will be further discussed below. LEDs 7 are placed such that they can emit their electromagnetic radiation via cylinder 3. A photosensor chip 8 is arranged on the upper surface 9 of cone 2.
  • a curing plastic mass 11 is subsequently also placed in the manner shown in figure 4 between the upper surface 10 of unit 3, 4, 5 and the lower surface of ring 6 such that all described components form an integrated unit 12.
  • this unit or head 12 comprises a source of electromagnetic radiation in the wavelength range of 300-2500 nm consisting of the LEDs and perspex cylinder 3.
  • the effective radiation- generating source is formed essentially by the annular lower surface 13 of cylinder 3.
  • the lower surface 14 of cone 2 forms together with chip 8 a photosensor with entrance window 14.
  • the surface 14 can receive electromagnetic radiation generated via surface 13.
  • Head 12 is based on the volume reflection principle, wherein both said surfaces 13, 14 are situated in or close to the milk for analysis.
  • the LEDs 7 can be built up of mutually adjacent cyclic groups of LEDs which emit any radiation in a specific wavelength band.
  • the LEDs can be controlled by electronic provisions such that all LEDs of a specific wavelength band are for instance energized in cyclic alternation. Through gating, synchronous detection and other signal processing an electronic signal processing unit to which sensor 8 is connected can then determine which radiant intensity always corresponds with a given wavelength range.
  • temperature sensors are integrated with the LEDs and the detector.
  • the central processing unit or CPU can thus carry out a temperature-dependent correction and thus eliminate the temperature dependence. After this correction a "clean" signal not dependent on temperature is obtained. Attention is drawn to the fact that for the operation of the head 12 it is in principle irrelevant whether the concentric surfaces 14 and 13 act as source or as receiver.
  • the optimal configuration is determined by optimal detection possibilities in relation to radiant intensity and cost-price.
  • Figure 5 shows a tube 15 in which are situated a schematically represented source 16 and a likewise schematically represented photosensor 17. It will be apparent from the shown configuration, in which source and sensor are located diagonally opposite each other, that this configuration is not based on volume reflection but on transmission through the milk situated in the tube.
  • Figure 6 shows a tube 18 in which a single source 16 and photosensor 17 are located adjacently of each other. This variant is based on volume reflection.
  • Figure 7 shows a tube 18 with a bend. In this configuration two sources 19,20 are placed on either side of sensor 17. This variant is based on volume reflection.
  • Figure 8 shows a conduit 21 with a source 16 and a photosensor 17 which are directed toward each other in the bend of conduit 21.
  • This variant is based on transmission.
  • source 16 and photosensor 17 are accommodated in a cavity 23 connecting onto a tube 22.
  • the variant of figure 9 is based on transmission.
  • sources 19,20 are directed away from photosensor 17.
  • This variant is based on reflection in the milk.
  • Such a per se known measurement is referred to as "reflection measurement”.
  • a window 110 is present in the embodiment of figure 10 which is transparent for radiation in the used wavelength range, for instance a window of glass, quartz or perspex/PMMA. Attention is drawn to the fact that the configuration has to be such that sensor 17 cannot sense the mirror images of sources 19,20 via reflection through window 110.
  • FIG 11 shows a part of a milking apparatus 24.
  • This apparatus comprises a housing 25, milk hoses 26, vacuum hoses 27, a head 12 received in a housing, a temperature sensor 28, level sensors 29,30, a linear actuator 31 which carries a valve 85, and a drain conduit 32.
  • Valve 85 which is shown in figure 11 in its lowest position, can co-act sealingly with the annular bottom edge 86 of a rotation-symmetrical inner jacket 87 which, together with the closed valve 85, bounds a space 88 in which the milk flowing in as according to arrows 89 is collected.
  • the signals coming from the level sensors are passed to a CPU 33 (see figure 12) .
  • the signals coming from temperature sensor 28 are also passed to CPU 33.
  • the CPU controls actuator 31 to take up its shown opened position. The milk can then move downward as according to arrows 90 to be drained via conduit 32 for further processing.
  • the active underside of head 12 is immersed for a time in the milk situated in space 88.
  • FIG 12 shows that via a central processing unit or CPU 33, which is controlled by a personal computer 34, information exchange takes place with feed dosing unit 35 which connects onto a trough 36, a cow identification receiver 37 which co-acts with a transponder 38 worn round the neck of cow 39, with milking apparatus 24 and a display and operating unit 40.
  • CPU 33 is further connected to a personal computer 41 with memory 42.
  • Via respective key units 43,44,45,46 information coming from CPU 33 can be transmitted to a signal processing and presentation unit 47, a processing unit 48 and processing unit 49 and a processing unit 50.
  • the signal processing unit and presentation unit 47 serves to present to the farmer the data relevant to him relating to the milk given by cow 39. This is for instance the total amount of milk from one milking session, fatty acid content, protein content and other important parameters.
  • Via signal processing unit 48 selected medically significant data can optionally be transmitted via a telephone modem 51 to a veterinary surgeon.
  • Via signal processing unit 49 data which if desired is selected in other manner can be transmitted to national institutes, while signal processing unit 50 can transmit data in analogous manner via modem 51.
  • FIG. 13 shows that the milk carried via conduit 32 to a tank 52 passes head 12 which is accommodated in a unit 53 shown in figure 15 with a reciprocally driven piston 54 which periodically drains the milk entering via conduit 32 (arrow 55) to a conduit 56 (arrow 57) .
  • FIG. 14 shows an analysis device 57 according to the invention.
  • a substantially "white” radiation source 58 is used in device 57 which via a known monochromator generates in periodic variation with time electromagnetic radiation with wavelength changing periodically in time to a bundle 62 of glass-fibres 63 via an exit slit 61 present in a plate 60.
  • Use is made for this purpose of a number of fixed mirrors 93,94,95,96 extending the path length of the radiation beam 92 and a reflection grating 98 driven for periodic pivoting as according to arrow 97.
  • the drive for grating 98 is not drawn.
  • the respective glass-fibres 63 serve as radiation conductors and debouch on a cylinder 64 manufactured from PMMA
  • a head 65 (perspex) , glass or quartz which forms part of a head 65.
  • the end surfaces 66 serve as effective radiation sources.
  • a PMMA cone/cylinder 67 is placed centrally with end surface 68 serving as effective receiver.
  • chip 8 Placed on the top is chip 8 which via an amplifier 69 transmits its signals corresponding with the detected radiant intensity to a signal processing unit 70, which is connected to monochromator 59 for information exchange and can thus control a presentation unit 71 such that for instance a graphic representation 72 is formed in which the measured radiant intensity or a value of a quantity associated therewith is presented as a function of the frequency or wavelength.
  • the head shown as well as other components in figure 12 makes use of a number of LEDs as sources for electromagnetic radiation in the frequency bands to be applied.
  • a LED can produce a high radiant intensity in a comparatively narrow frequency band.
  • the use of monochromator 59 can have the drawback in some circumstances that the ratio of the energy of a transmitted effective band and the energy in the total band generated by light source 58 is small, so that little energy is available in the band in question.
  • a LED has an effective band width in the order of magnitude of for instance 50-100 nm. Should it be wished to decrease the band width to for instance 10-20 nm for the purpose of a greater resolution, an interference transmission filter can then be added to each relevant LED. A greater resolution may be required particularly in the spectral analysis in the range above 1000 nm. In that case an interference transmission filter can be added to each individual LED in for instance the structure according to figure 4.
  • Figure 15 shows the detail XV of figure 13.
  • the structure of figure 15 is adapted for a proportional determination of the quantity of milk allowed through.
  • Use is made for this purpose of not shown means (electric, pneumatic) , the vacuum of the milking apparatus 24 or the like for reciprocal movement according to arrow 99.
  • the effective volume of chamber 100 can amount for instance to 100 ml.
  • Extending in flush-mounted position on the front surface of the head are conductance-determining electrodes 101,102 which serve to determine the presence of milk at the level of the front surface of head 12.
  • Temperature sensors 103,104 are placed on the inner surface of the plastic housing 105.
  • Figure 16 shows a practical arrangement.
  • a head 12 is immersed in a conduit 73 via a connecting tube stub
  • Tube stub 74 into which head 12 fits sealingly.
  • Tube stub 74 bears a flange 75 for coupling head 12 via a support ring 76.
  • Both the unit 53 according to figure 15 and the unit shown in figure 16 can be added to an existing milking installation.
  • Figure 16 does not show that for this purpose an existing conduit can be interrupted for incorporation therein of conduit 73.
  • the flange is connected sealingly to a respective flange 108,75.
  • the sealing is ensured by means of an O-ring 109.
  • FIG 17A shows a source 77 and a receiver 78.
  • the source comprises a number of LEDs 7 which can emit their radiation via a PMMA cylinder 79.
  • Via an interspace 80 sensor 8 can receive radiation via cone/cylinder 67.
  • the paths of photons are symbolically represented with irregular lines 106. This shows symbolically that the radiation emitted by cylinder 79 reaches cone/cylinder 67 via erratic paths and then only to a small extent. Some photons are intercepted and will therefore never reach said cone/cylinder 67. This interception is represented symbolically with the black spots 107 symbolizing absorption.
  • Figure 17B shows an end view of receiver 78.
  • Figure 17C shows that the ten LEDs 7 are grouped in a ring.
  • Figure 18 shows a head 81 in which source and sensor are likewise integrated.
  • the head comprises an opaque cured plastic mass 82 in which a PMMA insert 83 is received.
  • Connecting onto insert 83 is a ring of LEDs 7 which have an axial direction of about 45° relative to the rotation axis 84 of head 81.
  • only one transparent perspex or PMMA element 83 is applied in head 81 both for guiding outside the radiation generated by LEDs 7 and for guiding inside via surface 84 to sensor 7 the radiation coming from outside.
  • Figure 19 shows a measuring arrangement which makes use of a source 77 and a receiver 78 of the type shown in figure 17.
  • the arrangement according to figure 17A is based on transmission.
  • the arrangement according to figure 19 is based on volume reflection.
  • Figure 20 shows an arrangement which provides measuring facilities based on volume reflection as well as measuring facilities based on transmission.
  • the source head 77 is identical to the relevant head according to figure 17, while source/sensor head 85 is identical to the head shown in figure 14.
  • the transparent cylinder 64 can act as source.
  • the transparent cylinder 79 can act as source.
  • the cone/cylinder 67 acts as receiver.
  • the arrangement shown in figure 20 provides the possibility of improving the reliability of the measurements .
  • head 65 can also be replaced by a head with a number of LEDs, such as head 12 according to figure 4.
  • the LEDs can herein be tuned or tunable separately or in groups to a frequency range associated with a parameter in order to enable simultaneous determining and/or detection of diverse parameters.
  • Figures 21-23 show a part of a device according to the invention.
  • the device comprises a frame 122 with two vertical supports 123, 124 in which respective tubes 125, 126 are accommodated for displacement in longitudinal direction.
  • Source 77 is arranged in tube 126; receiver or sensor 78 is arranged in tube 125.
  • Suction chambers 127, 128 Around the active end surfaces of respectively receiver 78 and source 77 are arranged respective suction chambers 127, 128 which are provided with respective mutually facing flat parallel surfaces 128, 129 which are each provided with a pattern of perforations 130 which act as suction apertures. Suction chambers 127, 128 enclose respectively receiver 78 and source 77 in substantially sealing manner such that the apertures 130 can effectively serve as suction apertures. Connected for this purpose to suction chambers 127, 140 are flexible conduits 131, 132 which are connected to a suction pump 133 drawn schematically in figure 23.
  • the substance 138 for measuring which is arranged beforehand in a plastic bag, is placed between the surfaces 128, 129. Tubes 125, 126 are then displaced until surfaces 128, 129 have the desired mutual spacing. Suction pump 133 ensures that via holes 130 the walls of bag 137 are sucked against surfaces 128, 129, whereby they come to lie tautly against the windows of respectively source 77 and sensor 78. Measurement inaccuracies and uncertainties are hereby effectively avoided.
  • Figure 23 in particular shows the manner in which bag 137 is placed in relation to suction chambers 127, 140 during performing of the measurement in which the source and the sensor are active and are controlled and transmit signals to a central signal processing unit in the above described manner.
  • the sample holder which can be embodied in practice as a plastic bag, can be manufactured in practical manner from a foil material which is flexible, optically homogeneous and transparent to the applied wavelengths such that the sample for measuring is closed off to a sufficient extent from its surroundings, can be transported in the holder and can also be stored at low temperatures.
  • the choice of material for the foil bag must be made such that mechanically or manually or in other manner the bag enables operations such as dilution, mixing, homogenizing and other pre-treatments .
  • packaging and sample holder must be such that it can be received in the analysis device cheaply and simply without the necessity of pre- treatment or modification and is also suitable, with possibly small modifications, to be arranged in process installations relevant to the object for measuring, for instance a milking installation.
  • a second storage bag can if necessary be applied, into which the sample holder is placed.
  • Feed hoses and discharge hoses can if desired be connected to the holder for the purpose of dilution or the addition of reagents.
  • the chosen foil material can if necessary withstand centrifugal forces which occur in centrifuges in the case of a centrifugal separation in the sample.
  • Figure 24 shows results of wavelength-variable measurements on 100 different human faeces samples, using a slightly modified setup relative to that shown in figure 23. These were samples from patients with a great variation in diet, including patients with disorders of the digestive system. The absorptivity is plotted along the vertical axis against the wavelength in nm along the horizontal axis. The dark current is represented by the spectrum indicated with numeral 141. Absorption peaks can clearly be identified in figure 24, such as at position 142. The absorption peaks are associated with the composition of faeces and the peaks thereof to be tested in the analysis according to the invention.
  • Figure 24 comprises a plurality of absorption peaks. It will be apparent that the quality of the diagnostic evaluation can possibly be improved considerably if more absorption peaks are involved in the analysis.
  • the quality of the analysis, and therewith the quality of the diagnosis is improved.
  • Figure 25 thus shows the regression spectrum based on analysis of all spectra shown in figure 24 after multivariation analysis making use of the commercially obtainable multivariation analysis software program "Unscramble" from Camo of Norway.
  • the peak 142 of figure 24 can be clearly discerned as well as peaks which are not immediately discerned upon cursory visual inspection of figure 24. These are for instance peaks 145, 147, 142, 144 and 146 and other peaks.
  • the weighting factor is plotted vertically as a percentage against the horizontal wavelength in nm.

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Abstract

La présente invention concerne une tête de mesure destinée à un dispositif de mesure qui comprend : un spectromètre composé d'une source de rayonnement électromagnétique dont au moins une composante spectrale est choisie dans la plage de longueur d'onde comprise entre environ 300 et 2500 nm ; un photodétecteur qui est sensible au moins à la première, la deuxième, la troisième et facultativement la quatrième harmoniques ou à des composantes spectrales, qui appartiennent à la région de longueur d'onde utilisée, plus particulièrement comprise entre 300 et 2500 nm ; le photodétecteur étant placé par rapport au produit à analyser de telle sorte que le détecteur reçoive le rayonnement diffusé par le produit par transmission, réflexion et/ou réflexion du volume ; et une unité d'analyse du signal qui est reliée au détecteur ; et un volume prévu pour contenir les produits à analyser dans lequel sont exposées les surfaces actives de la source et du détecteur.
PCT/NL2000/000273 1999-04-27 2000-04-27 Tete de mesure pour dispositif servant a analyser des produits WO2000064242A1 (fr)

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AU46246/00A AU4624600A (en) 1999-04-27 2000-04-27 Measuring head for a device for analysing products

Applications Claiming Priority (4)

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NL1011905A NL1011905C2 (nl) 1999-04-27 1999-04-27 Inrichting voor het analyseren van melk en daarvoor bestemde sensor.
NL1011905 1999-04-27
NL1013805A NL1013805C2 (nl) 1999-04-27 1999-12-09 Inrichting voor het analyseren van producten en daarvoor bestemde sensor.
NL1013805 1999-12-09

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DE10124917A1 (de) * 2001-05-28 2002-12-12 Vinorica S L Verfahren zur Klassifizierung von Wein und Kaffee
WO2003040704A1 (fr) * 2001-11-08 2003-05-15 S.A.E. Afikim Computerized Dairy Management System Analyseur spectroscopique de fluide
DE10318942A1 (de) * 2003-04-26 2004-11-18 Zunhammer, Sebastian, Dipl.-Ing. (FH) Verfahren und Fahrzeug zur Ausbringung von Gülle
WO2007010530A1 (fr) * 2005-07-20 2007-01-25 Yissum Research Development Company Procédé et dispositif pour déterminer la qualité du lait
US7270543B2 (en) 2004-06-29 2007-09-18 Therametric Technologies, Inc. Handpiece for caries detection
WO2008043502A1 (fr) 2006-10-11 2008-04-17 Sebastian Zunhammer Procédé et véhicule pour l'épandage de lisier
DE102008005650A1 (de) 2008-01-23 2009-07-30 Zunhammer, Sebastian, Dipl.-Ing. (FH) Verfahren und Vorrichtung zur Ausbringung von Gülle
ES2324589A1 (es) * 2008-02-07 2009-08-10 Universidad De Oviedo Metodo y sistema de obtencion de leche fresca de caracteristicas diferenciadas basado en la separacion durante el ordeño.
US7997228B2 (en) 2001-06-12 2011-08-16 Delaval Holding Ab Milk measurement and milk collection
US8360771B2 (en) 2006-12-28 2013-01-29 Therametric Technologies, Inc. Handpiece for detection of dental demineralization
CN103134940A (zh) * 2013-01-23 2013-06-05 北京三元食品股份有限公司 生奶生产全自动监测与采样系统
US9204593B2 (en) 2008-01-23 2015-12-08 Sebastian Zunhammer Device for spreading liquid manure
FR3074636A1 (fr) * 2017-12-12 2019-06-14 Mauguin Citagri Tonne equipee d'un dispositif de determination de la concentration d'un compose chimique d'un effluent d'elevage contenu dans la tonne et procede correspondant
US10357634B2 (en) 2016-07-28 2019-07-23 Cook Medical Technologies Llc Steerable catheter with wire-tensioning mechanism
EP2646800B1 (fr) * 2010-12-03 2019-11-27 FOSS Analytical A/S Analyse spectrale de l'infrarouge central d'un matériau hétérogène en écoulement
GB2602666A (en) * 2021-01-12 2022-07-13 Palintest Ltd Spectrophotometric instrument
US11566999B2 (en) 2018-04-24 2023-01-31 Union College Spectral analysis of gasses emitted during roasting food

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Cited By (28)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10124917B4 (de) * 2001-05-28 2007-03-22 Bionorica Ag Verfahren zur Klassifizierung von Wein und Kaffee
DE10124917A1 (de) * 2001-05-28 2002-12-12 Vinorica S L Verfahren zur Klassifizierung von Wein und Kaffee
US7244902B2 (en) 2001-05-28 2007-07-17 Bionorica Ag Method for classifying wine and coffee
US7997228B2 (en) 2001-06-12 2011-08-16 Delaval Holding Ab Milk measurement and milk collection
CN100458405C (zh) * 2001-11-08 2009-02-04 S.A.E.埃菲金计算机化乳业管理系统 光谱流体分析器
US7236237B2 (en) * 2001-11-08 2007-06-26 S.A.E. Afikim Computerized Dairy Management System Spectroscopic fluid analyzer
WO2003040704A1 (fr) * 2001-11-08 2003-05-15 S.A.E. Afikim Computerized Dairy Management System Analyseur spectroscopique de fluide
DE10318942B4 (de) * 2003-04-26 2007-05-24 Zunhammer, Sebastian, Dipl.-Ing. (FH) Verfahren und Fahrzeug zur Ausbringung von Gülle
DE10318942A1 (de) * 2003-04-26 2004-11-18 Zunhammer, Sebastian, Dipl.-Ing. (FH) Verfahren und Fahrzeug zur Ausbringung von Gülle
US7270543B2 (en) 2004-06-29 2007-09-18 Therametric Technologies, Inc. Handpiece for caries detection
WO2007010530A1 (fr) * 2005-07-20 2007-01-25 Yissum Research Development Company Procédé et dispositif pour déterminer la qualité du lait
WO2008043502A1 (fr) 2006-10-11 2008-04-17 Sebastian Zunhammer Procédé et véhicule pour l'épandage de lisier
US9241439B2 (en) 2006-10-11 2016-01-26 Sebastian Zunhammer Method and vehicle for distributing manure
US8360771B2 (en) 2006-12-28 2013-01-29 Therametric Technologies, Inc. Handpiece for detection of dental demineralization
DE102008005650A1 (de) 2008-01-23 2009-07-30 Zunhammer, Sebastian, Dipl.-Ing. (FH) Verfahren und Vorrichtung zur Ausbringung von Gülle
DE102008005650B4 (de) 2008-01-23 2023-04-06 Sebastian Zunhammer Verfahren und Vorrichtungen zur Ausbringung von Gülle
US9204593B2 (en) 2008-01-23 2015-12-08 Sebastian Zunhammer Device for spreading liquid manure
ES2324589A1 (es) * 2008-02-07 2009-08-10 Universidad De Oviedo Metodo y sistema de obtencion de leche fresca de caracteristicas diferenciadas basado en la separacion durante el ordeño.
WO2009098339A1 (fr) * 2008-02-07 2009-08-13 Universidad De Oviedo Procédé et système d'obtention de lait frais à propriétés différenciées, se fondant sur la séparation pendant la traite
EP2646800B1 (fr) * 2010-12-03 2019-11-27 FOSS Analytical A/S Analyse spectrale de l'infrarouge central d'un matériau hétérogène en écoulement
CN103134940A (zh) * 2013-01-23 2013-06-05 北京三元食品股份有限公司 生奶生产全自动监测与采样系统
CN103134940B (zh) * 2013-01-23 2013-10-30 北京三元食品股份有限公司 生奶生产全自动监测与采样系统
US10357634B2 (en) 2016-07-28 2019-07-23 Cook Medical Technologies Llc Steerable catheter with wire-tensioning mechanism
EP3498069A1 (fr) * 2017-12-12 2019-06-19 Mauguin Citagri Tonne équipée d'un dispositif de détermination de la concentration d'un composé chimique d'un effluent d'élevage contenu dans la tonne et procédé correspondant
FR3074636A1 (fr) * 2017-12-12 2019-06-14 Mauguin Citagri Tonne equipee d'un dispositif de determination de la concentration d'un compose chimique d'un effluent d'elevage contenu dans la tonne et procede correspondant
US11566999B2 (en) 2018-04-24 2023-01-31 Union College Spectral analysis of gasses emitted during roasting food
GB2602666A (en) * 2021-01-12 2022-07-13 Palintest Ltd Spectrophotometric instrument
GB2602666B (en) * 2021-01-12 2023-08-23 Palintest Ltd Spectrophotometric instrument

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