WO2001023868A1 - Pcb measurement in pork fat with nir - Google Patents
Pcb measurement in pork fat with nir Download PDFInfo
- Publication number
- WO2001023868A1 WO2001023868A1 PCT/EP2000/009476 EP0009476W WO0123868A1 WO 2001023868 A1 WO2001023868 A1 WO 2001023868A1 EP 0009476 W EP0009476 W EP 0009476W WO 0123868 A1 WO0123868 A1 WO 0123868A1
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- WO
- WIPO (PCT)
- Prior art keywords
- samples
- calibration
- fat
- pcb
- process according
- Prior art date
Links
- 238000005259 measurement Methods 0.000 title description 30
- 235000015277 pork Nutrition 0.000 title description 10
- 238000000034 method Methods 0.000 claims abstract description 45
- 230000008569 process Effects 0.000 claims abstract description 36
- 230000003595 spectral effect Effects 0.000 claims abstract description 19
- 150000001875 compounds Chemical class 0.000 claims abstract description 8
- 150000002896 organic halogen compounds Chemical class 0.000 claims abstract description 7
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 4
- 238000005375 photometry Methods 0.000 claims abstract description 4
- 150000003071 polychlorinated biphenyls Chemical class 0.000 claims abstract description 4
- 239000000523 sample Substances 0.000 claims description 39
- 238000001514 detection method Methods 0.000 claims description 11
- 238000002835 absorbance Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000007621 cluster analysis Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000002790 cross-validation Methods 0.000 claims description 6
- HGUFODBRKLSHSI-UHFFFAOYSA-N 2,3,7,8-tetrachloro-dibenzo-p-dioxin Chemical compound O1C2=CC(Cl)=C(Cl)C=C2OC2=C1C=C(Cl)C(Cl)=C2 HGUFODBRKLSHSI-UHFFFAOYSA-N 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- 238000010238 partial least squares regression Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000012417 linear regression Methods 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000012472 biological sample Substances 0.000 claims description 3
- XCAUINMIESBTBL-UHFFFAOYSA-N lead(ii) sulfide Chemical compound [Pb]=S XCAUINMIESBTBL-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 2
- 238000009795 derivation Methods 0.000 claims description 2
- 238000006911 enzymatic reaction Methods 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 238000000611 regression analysis Methods 0.000 claims description 2
- 238000004611 spectroscopical analysis Methods 0.000 claims 1
- 239000003925 fat Substances 0.000 description 46
- 238000001228 spectrum Methods 0.000 description 46
- 235000019197 fats Nutrition 0.000 description 44
- 230000000875 corresponding effect Effects 0.000 description 13
- 238000004458 analytical method Methods 0.000 description 10
- 235000003434 Sesamum indicum Nutrition 0.000 description 9
- 238000004817 gas chromatography Methods 0.000 description 9
- 238000004364 calculation method Methods 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 7
- 238000004422 calculation algorithm Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 210000001519 tissue Anatomy 0.000 description 5
- 101100327917 Caenorhabditis elegans chup-1 gene Proteins 0.000 description 4
- 238000004497 NIR spectroscopy Methods 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- 238000012896 Statistical algorithm Methods 0.000 description 2
- 238000000692 Student's t-test Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 238000013450 outlier detection Methods 0.000 description 2
- 238000000513 principal component analysis Methods 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000009897 systematic effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 101100004286 Caenorhabditis elegans best-5 gene Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 description 1
- 239000004367 Lipase Substances 0.000 description 1
- 102000004882 Lipase Human genes 0.000 description 1
- 108090001060 Lipase Proteins 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 102000035195 Peptidases Human genes 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
- 239000004365 Protease Substances 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 210000000577 adipose tissue Anatomy 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 150000004074 biphenyls Chemical class 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 description 1
- 239000010791 domestic waste Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005264 electron capture Effects 0.000 description 1
- 238000000556 factor analysis Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 235000019421 lipase Nutrition 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- -1 moisture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 235000021003 saturated fats Nutrition 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 235000021081 unsaturated fats Nutrition 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 238000012800 visualization Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
Definitions
- the present invention is related to a process for determination of halogenated organic compounds, especially PCBs, that means polychlonnated biphenyls, m at least partially hydrophobic samples like fat, using photometry.
- PCB' s In meat fat a build-up of PCB' s and dioxms from the environment has been observed.
- the principal ways by which PCB' s are coming into the environment are: vaporisation from plasticisers, combustion of industrials and domestic waste, transformers and capacitors cooling liquids (according to data of the World Health Organisation) .
- the nature and dynamics of the distribution persistence, chemical inertness, spreading m the atmosphere due to fairly high vapour pressure and capacity for diffusion in the soil and surface waters combined with lipophilicity promote the bioaccumulation of PCB' s m the fatty tissues of man and animals m amounts considered to be dangerous for vital activity.
- PCB' s is correlated to the dioxm level and is a way to measure the dioxm level indirectly.
- GC Gas Chromatography
- Gas chromatography is a separation technique, the samples are separated m different fractions. The different components coming out of a chromatography column are detected. Different detection techniques can be used. Like mass spectroscopy (MS) or electron capture detector (ECD) . In the latter gas chromatography detection technique is used, because halogens are very well detected by this technique and PCB' s contain a lot of chlorinated bondings. For PCB a family of 7 congenating piques, each pique of approximately 20 ppb level for the 200 ppb level samples, can be detected and defined as the PCB concentration level. The standard deviation read-out is approximately 20%.
- the object of the present invention is to provide a process having a superior combination of good sensitivity and easy handling with respect to prior art.
- NIR-spectroscopy is an analytical method. Results are calculated from reference data, e.g. obtained from different analytical procedures like gas chromatography, using statistical algorithms.
- NIR ranges from about 750 nm to 2500 nm.
- At least one chemometric calibration model is calculated using factor analysis and/or regression techniques are used and later on used to predict unknown samples.
- Calibration results are calculated from reference data obtained from different analytical procedures, e.g. gas chromatography, using statistical algorithms. This is called the calibration process.
- the unusualness of this invention is the use of NIR for the detection of components in ppb (parts per billion) level. This means for PCB in pork fat a level of approximately 200 nanogram per 100 gram fat. This is extremely low and thought to be beyond the NIR detection limits.
- the spectral data are recorded advantageously within a wavelength range between 1100 and 2500 nm, where characteristic near-infrared signals, e.g. of PCB are found and where standard near- infrared spectrometers can be used.
- the selection of calibration sample concentrations comprises usefully increasing differences of successive samples with increasing concentrations, especially with a concentration range extending up to more than 10-fold of the minimum detection level of the process to provide good calibrations in the lower concentration level of the calibration samples and/or in order to have much variance represented by the calibration samples.
- the selection of samples Preferably have a concentration range extending up to more than 10-fold of the minimum detection level.
- mixtures of 0, 140, 280, 1400 and 2800 ppb PCB per 100 gram blank fat are used as calibration samples, m particular m combination with real fat samples comprising PCB concentrations within this range.
- Transmission and/or reflectance data and/or absorbance and/or the first and/or the corresponding first or higher derivation of these data may be recorded m the process according to the present invention for the measurements. This can be done by conversion of the measured data according to known techniques, as well.
- An advantageous embodiment of the process of the present invention comprises a selection of preferred wavelengths is used for recording spectral data, especially the combination of at least three wavelengths, preferably containing 173015, 1740+5 and 2260 ⁇ 5nm, or 173015, 174015 and 2264 ⁇ 5nm, or 1730+5, 174015 and 2258 ⁇ 5nm, or 137615, 1384+5 and 2184+5nm, or 1376+5, 138415 and 2180 ⁇ 5nm in order to reduce measurement time and/or to obtain a good accuracy.
- a subrange of NIR including a number of selected wavelengths, is used.
- the selection algorithms implemented m the SESAME software, commercialised by Bran+Luebbe GmbH, can be used for this purpose.
- the chemomet ⁇ c model used is multiple linear regression (MLR) and/or partial least squares regression (PLSR) and/or principal components regression or cluster analysis.
- MLR multiple linear regression
- PLSR partial least squares regression
- principal components regression or cluster analysis are for example provided with the SESAME software, commercialised by Bran+Luebbe GmbH, and described m the corresponding manual .
- the determination of the calibration factors comprises a cross validation of calibration samples and/or wavelengths.
- the best calibration samples will be selected by subsequent removal of calibration data of a few defined calibration samples and verification of the corresponding calibration results.
- This can be carried out by using the corresponding functions of the SESAME software, commercialised by Bran+Luebbe GmbH.
- the calculations and/or the selections are performed at by a software, comprising operations controlling a spectrometer used m the process, wherein calibration data are saved on a computer, possibly via downloading from a data network connected to said computer.
- any suitable combination of standard computers like a personal computer and software products like the SESAME software, commercialised by Bran+Luebbe GmbH and possibly internet software tools can be used.
- calibration data then have to be recorded and calculated only once for several experiments or recording of them may be completely omitted by simply downloading them, e.g. from a data-network link to the manufacturer of the spectrometer used m the process of the present invention, especially via Internet.
- Common suitable data transfer techniques may be used for this purpose.
- the samples are liquefied via melting, especially by heating n a microwave and/or chemical reactions and/or enzymatic reactions.
- a microwave and/or chemical reactions and/or enzymatic reactions Especially fat tissue samples, available in solid and measurable in liquid state will be treated this way.
- Any suitable enzyme for degradation of biological samples like lipases, proteases may be employed m this process.
- the sample is an extraction from an initial sample with organic solvents.
- This extraction from an initial sample with organic solvents enables analysis of various initial samples and decreases the content of moisture and corresponding near-mfrared signals m the samples to be measured. Also water samples can be analysed with this process. Any kind of suitable extraction like Soxhlet or shaking an aqueous liquid with organic solvent can be employed for this purpose.
- mixtures of 0, 140, 280, 1400 and 2800 ppb PCB per 100 gram blank, that means PCB-free, pork fat are used as calibration samples, in particular m combination with real fat samples comprising PCB concentrations within this range.
- a reflectance recording spectrometer is used for a process according to the present invention, which comprises at least one lead sulphide detector for sensitive signal detection and preferably at least one diffusely gold-plated reflector disposed on the bottom of a sample cup, preferably comprising an electric resistor under the bottom of a sample cup, especially m a cavity within the bottom of a sample cup, preferably m combination with a temperature sensor, preferably a Peltier element directly fitted under the sample cup and connected to a heat controller which is further connected to the resistor for temperature control.
- the Bran + Luebbe InfraAlyzer 500 can be used as such kind of spectrometer. This device enables, e.g. to maintain the liquid state of a melted fat sample and/or good temperature control.
- An advantageous application of a process and/or spectrometer according to the present invention is detecting PCB m fat on a level between 200 and 1000 ppb per lOOg fat, e.g. for surveillance of food quality in accordance with proposed or prescribed limits for PCB contaminatio .
- Another advantageous application of a process and/or spectrometer is detecting halogenated organic compounds m biological samples like food stuffs or in liquefied polymers, petrol or other organic liquids like gasoline and nafta based products, the combustion of which generates extremely toxic substances when halogenated organic compounds are present, or in water like fresh water supplies.
- a further advantageous application of a process and/or spectrometer is detecting dioxin indirectly since PCB measurements provide an indirect measure for dioxin as described above.
- Figure 1 shows a cross section through a sample bearing connected to a temperature controller, all used in a spectrometer according to the present invention.
- the sample bearing m Figure 1 comprises a sample cup 1 namely a Bran+Luebbe Transflectance Cup (type Dutch cup) , which has a diffusely gold plated reflector 2 as a bottom and a path length of 0.2 mm + 0.01mm. A hole is drilled under the reflector 2, until just 1 mm under the gold plated surface and a PT100 resistor 5 (type DM503) with a positive temperature coefficient of 100 ⁇ at 20°C is mounted m this drilled hole and fixed with a specific temperature paste: heat sink compound (type 340 Dow Corning) .
- a sample cup 1 namely a Bran+Luebbe Transflectance Cup (type Dutch cup)
- a diffusely gold plated reflector 2 as a bottom and a path length of 0.2 mm + 0.01mm.
- a hole is drilled under the reflector 2, until just 1 mm under the gold plated surface and a PT100 resistor 5 (type DM503) with a positive temperature coefficient of 100 ⁇ at 20
- the resistor is connected to a temperature controller 6 with cables 7 (type: 17-8811-46342300, from Bartec) , outside the cup, which is then further connected with cables 7 to a Peltier element 3 (Thermoelectric Module type DT6-6LS, from Marlow Industries) , glued under the sample cup 1.
- the temperature controller 6 is connected to a outside power supply (type EA-3003 S-Current, 2.5 A, not shown) .
- the sample cup 1 is covered with a quartz window 3 covering the sample space 4 and the sample cup 1 is placed m the Solid Drawer of a Bran+Luebbe InfraAlyzer 500 spectrometer (not shown), during the complete measurement. Only the quartz window is opened to apply the sample.
- the NIR Analyser used for this experiment is a Bran+Luebbe InfraAlyzer 500 ⁇ , equipped with the Standard Solid Drawer.
- the wavelength range is 1100 to 2500 nm, selected with a holographic grating.
- the selected step size was 2 nm for this experiment to give 701 steps for each spectrum.
- the used detectors are a pair of lead sulphide detectors and a diffusely gold-plated integrating sphere is used to collect the reflected light by the sample.
- the temperature can be adjusted by the temperature controller and has been fixed at 50°C +/- 1°C, the optimal temperature for fat measurement, so that fats were m a liquid phase, without crystallisation, at this temperature .
- a selection of 8 pork fat samples is used, the concentrations of which, between 70 and 2695 ppb PCB per 100 g sample, have been determined by gas chromatography detection.
- the samples were heated in a microwave for 4 minutes, and the fat substance coming out of the pork tissue, is collected, approximately 5 ml .
- a sample without PCB (bianco) and a PCB standard sample of 20.000 microgram per ml in iso-octane solution, is then used for making a concentration gradient of five samples, with different PCB concentrations.
- the standard has first been diluted to a solution of 1 picogram m hexane, and used to spike the bianco sample.
- the pork tissue samples have been heated m a dish, one after the other m a common household microwave until melted, for 4 minutes.
- the collected fat m the dish has been used for the measurement.
- these samples were also heated m the microwave.
- a second heating in the microwave took place.
- the collected melt fat was poured into a small lab beaker. This microwave heating was also applied to be sure that less water is remained in the samples.
- the melted samples were applied on the gold reflector of the sample cup 5, by a pipette.
- the samples have been carefully sucked in a pipette, avoiding solid particles and air bubbles. Approximately 4 drops were sufficient to apply a layer of 0.2 mm on the reflector.
- the cup is then closed with the Quartz window. Some time is needed to be sure that the sample has reached the temperature of 50 °C in the cup. An additional time period of 30 sec. is used to be sure the temperature is not varying. Then the measurement (scanning) is started. After the measurement the cup is opened and cleaned with a paper tissue.
- spiked samples have been measured in duple. Then the other real samples have been measured also in duple. All these samples were measured in random order like shown in table 1, to avoid false correlations with temperature, etc.. After this measurement cycle some samples, spiked and not spiked samples, have been measured a third time, to be sure no other changes during this experiment took place.
- the invention may also be used for analysing solid samples.
- ppb PCB in fat level of PCB per 100 gram fat
- Example 1 cluster analysis
- SESAME software version 3.1 commercialised by Bran+Luebbe GmbH was used in this example.
- a conversion from reflectance data to first derivative data has been applied and the as qualitative analysis approach of cluster analysis was used as calibration calculation.
- Two of the spectra were determined to have excessive deviations and were deselected by the software from the set of calibration data.
- the selected calibration spectra were divided into two classes, one of which for 22 spectra from samples with more than 200 ppb PCB per lOOg fat and another one for 8 spectra from samples with more than 200 ppb PCB per lOOg fat.
- the algorithm of the software which is based on a principal component analysis (vectorial) calibration factors have been calculated which describe the properties of the two classes of spectral data. From these calibration factors the so called scores factor 2 generated by the software has been selected.
- Figure 2 shows a plot of the scores factor 2 against itself for better visualization, resulting in the representation of each of the selected calibration spectra factors as circles in this plot.
- Two clusters of scores factor 2 values were clearly distinguishable observable as two clusters of overlapping circles in figure 2.
- the cluster in the upper right area of the plot corresponds to spectra from samples below 200 ppb PCB per lOOg fat and the other cluster extending to the left edge of the plot corresponds to spectra from samples over 200 ppb PCB per lOOg fat. This indicates that the differences between the samples are obvious.
- reconstructions of the initial spectra were calculated from the corresponding concentration values, the deviation of which is represented by residual values. The data are given in table 2.
- Test set 0 series, 0 spectra 1 '
- T student's t test carried out for each spectrum representing the residual error, i.e. how closely the reference value matches the predicted value.
- S spectral reconstruction error, which is obtained by trying to recalculate the original spectrum from the selected factors. (A spectrum is suspected to be an S outlier if the
- PCB Property range 0 to 2800 (*) wavelength range 1100..2500nm, 701, 2 nm steps Transformation: Absorbance
- T student's t test carried out for each spectrum representing the residual error, i.e. how closely the reference value matches the predicted value.
- the present invention enables to predict the PCB content in pork fat samples via NIR measurement and can also be used to screen pork fat samples for the PCB level e.g. if they contain above 200 ppb or less than 200 ppb PCB per 100 gram fat in a few seconds, which is a major improvement compared to prior art and to gas chromatography analysis.
Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP00971294A EP1232386A1 (en) | 1999-09-28 | 2000-09-28 | Pcb measurement in pork fat with nir |
JP2001527205A JP2003510601A (en) | 1999-09-28 | 2000-09-28 | Measurement of PCB in pork fat by NIR |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EPPCT/EP99/07174 | 1999-09-28 | ||
EP9907174 | 1999-09-28 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2001023868A1 true WO2001023868A1 (en) | 2001-04-05 |
Family
ID=8167450
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2000/009476 WO2001023868A1 (en) | 1999-09-28 | 2000-09-28 | Pcb measurement in pork fat with nir |
Country Status (2)
Country | Link |
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JP (1) | JP2003510601A (en) |
WO (1) | WO2001023868A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8530844B2 (en) | 2005-06-27 | 2013-09-10 | Sfk Technology A/S | Recording of position-specific wavelength absorption spectra |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP5233549B2 (en) | 2008-09-22 | 2013-07-10 | 住友電気工業株式会社 | Food quality inspection device, food component inspection device, foreign substance component inspection device, taste inspection device, and transition state inspection device |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0614079A2 (en) * | 1993-03-03 | 1994-09-07 | W.R. Grace & Co.-Conn. | A method of directly monitoring the concentrations of microbiocides in aqueous systems |
WO1996011399A1 (en) * | 1994-10-07 | 1996-04-18 | Bp Chemicals Limited | Property determination |
EP0757243A1 (en) * | 1995-07-31 | 1997-02-05 | Instrumentation Metrics, Inc. | Liquid correlation spectometry |
US5830132A (en) * | 1993-08-24 | 1998-11-03 | Robinson; Mark R. | Robust accurate non-invasive analyte monitor |
WO1999009395A1 (en) * | 1997-08-14 | 1999-02-25 | Instrumentation Metrics, Inc. | Method and apparatus for generating basis sets for use in spectroscopic analysis |
WO1999024815A1 (en) * | 1997-11-12 | 1999-05-20 | Kvaerner Canada Inc. | Determination of anionic species concentration by near infrared spectroscopy |
-
2000
- 2000-09-28 WO PCT/EP2000/009476 patent/WO2001023868A1/en not_active Application Discontinuation
- 2000-09-28 JP JP2001527205A patent/JP2003510601A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0614079A2 (en) * | 1993-03-03 | 1994-09-07 | W.R. Grace & Co.-Conn. | A method of directly monitoring the concentrations of microbiocides in aqueous systems |
US5830132A (en) * | 1993-08-24 | 1998-11-03 | Robinson; Mark R. | Robust accurate non-invasive analyte monitor |
WO1996011399A1 (en) * | 1994-10-07 | 1996-04-18 | Bp Chemicals Limited | Property determination |
EP0757243A1 (en) * | 1995-07-31 | 1997-02-05 | Instrumentation Metrics, Inc. | Liquid correlation spectometry |
WO1999009395A1 (en) * | 1997-08-14 | 1999-02-25 | Instrumentation Metrics, Inc. | Method and apparatus for generating basis sets for use in spectroscopic analysis |
WO1999024815A1 (en) * | 1997-11-12 | 1999-05-20 | Kvaerner Canada Inc. | Determination of anionic species concentration by near infrared spectroscopy |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8530844B2 (en) | 2005-06-27 | 2013-09-10 | Sfk Technology A/S | Recording of position-specific wavelength absorption spectra |
Also Published As
Publication number | Publication date |
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JP2003510601A (en) | 2003-03-18 |
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