Optek Manual 1004 5003 02 Calibration Handbook VIS NIR US 2012-06-28

March 22, 2018 | Author: Gisa Ikawa | Category: Calibration, Spectrophotometry, Metrology, Absorption Spectroscopy, Measurement


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Calibration Handbook VIS-NIRoptek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28.pdf PN: 1004-5003-02 (-52) optek-Danulat GmbH Emscherbruchallee 2 45356 Essen Germany Telefon: +49-201-63409-0 Fax: +49-201-63409-999 E-Mail: [email protected] Internet: www.optek.com Preface This handbook is written to assist the user in proper procedures for trouble-free operation. It is explicitly pointed out that optek-Danulat GmbH assumes no responsibility for loss or damage caused due to improper use of this handbook or products described herein. This manual is protected by copyright. However, the user may produce copies and translations if required for correct operation of the products. On request, this manual is available in other languages as well as in digital format (Acrobat® Reader 7.0 required). Our products are being continuously improved. Technical data is subject to change without notice. Essen, June 2012 .............. Spectral Properties ..........1.............18 9........................................5 4.......................................................................................................1.1. Introduction ..................2.....................2 2.................. Calibration Devices......................................................... Overview.............................5 4.....................................1....................................................................1................................................. Calibration of optek VIS and NIR sensors................2........................... Handling and Storage...............3..............4 4.................................................................. Appendix...................................................................................................2............................................. Declaration of decontamination......................6 5....... Cleaning of optek Calibration Filters and Cuvettes ...........1...22 11.......2............................................. Traceability of optek calibration filters ........................ Spare parts ....7 5..............................................................................21 11..............................................1.................... Calibration Procedures ...................12 7................... Disposal.... General Procedure ...... Linearization Curves .................................................com .....................18 8.....................................Table of contents Preface 1...........................1..............................................22 11.................9 5.............1............................................................................................................ Overview................... Glossary.......................................................................1 1..1........................16 7........................26 ____________________________________________________________________________ -Ioptek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28......... General Procedure ................2......................11 6...................................................... Intended use................14 7.............................3..............1...................16 7....................................................................................................1................ Validity of the handbook ............................................................................................12 6...................................................pdf www..1........................................7 5.........1....................3.................... Contacts ...... Safety .................................................1........................................4.................................22 11.........3....3 3............................................... Traceability ................................................1..............2............................ Handling of Calibration Cuvettes...................1 1..11 6.... Calibration Certificate ..........................10 6...............................9 5. Example Calibration with FH03 Calibration Cuvette ............. Using the handbook ...........................................................................1....................14 7.................2..............................................................................................................9 5........16 8.......................2...........................13 7.............................. Handling and Storage of optek Calibration Filters..............optek..23 11.................5 4...............7 5..............................2.2................ Calibration with Calibration Filter......3.................3..........................13 7................................................2.................................. Sample certificate for VIS-L090 Calibration Filter .....14 7...................19 10.............. Pictograms and signal words ..........................1.......... Calibration with Calibration Cuvette ..... Calibration Device ....................... Photometric Accuracy and Linearity............................................................................2..........................................2... Overview......................................................................... Spectral properties ................................................................1.......7 5................................... Example Filter Calibration – Photometric Accuracy and Linearity .......................... Photometric accuracy and linearity ................. enhance its life cycle and avoid down times. If the calibration filters are not used according to this handbook. Follow this handbook for every operation. page 3 in combination with the inline sensors for VIS and NIR absorption indicated in chapter 4. page 5. To maintain reliability of the product.1. ____________________________________________________________________________ -1optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. Validity of the handbook This handbook is only valid for optek calibration filters described in chapter 2. follow the instructions given in this manual.pdf www.optek. please follow local accident prevention and environmental protection instructions.1. the function of the calibration filters and the measuring system to be checked may be affected. Using the handbook 1. as well as recognized technical regulations for safe and professional operation. Furthermore. Furthermore always observe the handbook of each measuring system to be checked.com . ____________________________________________________________________________ -2optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. Note! This pictogram indicates instructional or general advice.com .1. Danger! Electrical voltage. The text next to the symbol gives information on how to avoid bodily injuries.pdf www. This pictogram indicates danger due to electrical voltage. Caution! This pictogram indicates information on how to avoid material damage.optek. Pictograms and signal words Important information in this handbook is marked with the following pictograms: Danger! This pictogram indicates immediate danger to life and health of persons.2. 1 International vocabulary of metrology. The warranty for calibration filters as well as for corresponding certificates including product traceability expires in case of improper use. Intended use optek calibration filters and cuvettes shall only be used as a means for calibration of inline sensors for VIS and NIR absorption indicated in chapter 4. removal of the calibration filter from the filter holder. or modification of the labelling. Calibration with optek calibration means shall only be carried out by trained and qualified personnel.com .2.pdf www.Basic and general concepts and associated terms ed. Following this handbook is part of the intended use.optek. page 5. The term “calibration” is employed here in accordance with the definition of the “International vocabulary of metrology – Basic and general concepts and associated terms”1 Constructional changes as well as changes to and interference with the described procedures for using the calibration filter are prohibited. optek does not assume liability for loss or damage resulting from use of calibration filters. German Institute for Standardization nd 2 edition 1994 ____________________________________________________________________________ -3optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28.: DIN. This safety information is supplemented by the current national and local regulations on accident prevention and the recognized technical instructions for safe and professional operation. Report any damage immediately and do not commission the product until corrective actions have been taken. This especially applies to personnel who only occasionally carry out calibrations with calibration filters. Do not use calibration filters or cuvettes with visible damage to the filter glass or filter holder.3. Protect calibration filters and cuvettes from external influences which could affect proper function.com . Inspect the product for signs of physical damage. Read this handbook prior to initial commissioning.optek. Have such calibration means immediately checked by the manufacturer.pdf www. such as dust. ____________________________________________________________________________ -4optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. Safety Only use the calibration filter when free from defects and in accordance with the instructions provided in this handbook. Observe all safety and information labels on the product and keep them in readable condition. Spare parts must comply with technical requirements defined by optek. humidity or fingerprints. This is always guaranteed when using original spare parts. 3. AS16-F and AF26 sensors. Traceability 4.1.2. Overview The „International vocabulary of metrology – Basic and general concepts and associated terms” defines traceability as the “property of the result of a measurement or the value of a standard whereby it can be related to stated references. This test applies to the entire measuring chain consisting of converter. calibration certificate. ____________________________________________________________________________ -5optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. Determination of calibration frequencies is the user’s responsibility. usually national or international standards.1 page 7 and chapter 7. sensor and cable set.2 page 9 and chapter 7. cannot be NIST-traceable.4. explicitly described and documented series of comparisons that successively link the value and uncertainty of a result of measurement with the values and uncertainties of each of the intermediate reference standards and the highest reference standard to which traceability for the result of measurement is claimed. through an unbroken chain of comparisons all having stated uncertainties”. It can only be a calibrated spectrophotometer.pdf www. AF16-F.1 page 16) The available calibration filters are test devices traceable to NIST and used to calibrate VIS and NIR sensors at user-defined and applicationdependent frequencies. for example.com . optek offers VIS and NIR calibration means for the following tests: a) Calibration of photometric accuracy and linearity (chapter 5. Introduction This handbook is a description of optek’s VIS and NIR calibration filters and calibration cuvettes used to test the functionality of optek AF16-N. whose measurements are traceable to NIST.1 page 14) b) Calibration of spectral properties (chapter 5. These stated references can be standards developed and maintained by national or international metrological institutes. or transfer standards that are linked to other working standards. The “unbroken chain of comparisons” is referred to as a complete. or laboratory.1.1.optek. AS16-N. such as the „Deutsche Physikalisch-Technische Bundesanstalt“ (the national metrology institute in Germany) or the „National Institute of Standards and Technology“ (NIST) in the USA. A spectrophotometer. Traceability is thus a property of a measurement and not a property of a device. 4. In the center of the calibration laboratory is a spectro-photometer (Varian Cary 5000) which is subject to rigid inspection of measuring and test equipment in the course of which calibrations are carried out in permanently defined intervals using NIST Standard Reference Material (SRM).4.1.optek. Details regarding used reference materials and required indications are given in the respective optek calibration certificate. measurements at wavelengths above 800nm can’t be NIST traceable even if they were carried out with a spectrophotometer whose measurements are NIST traceable calibrated.2. optek is able to provide reliable and precisely calibrated calibration filters for optek NIR photometers. ____________________________________________________________________________ -6optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. Details regarding used reference materials and required indications with respect to the description of traceability are given in the respective optek calibration certificate. Just like the spectro-photometer are these SRMs also subject to a detailed determined inspection of measuring and test equipment and are recalibrated at regular intervals in a certified calibration laboratory. For that purpose optek uses reference calibration filters as transfer standards between an optek reference NIR photometer and the spectrophotometer of the optek calibration laboratory. Traceability of optek calibration filters Spectrophotometers and photometers are special with respect to traceability since they deliver dimensionless measuring results which can thus not be traced back to SI basic units. Certification of optek calibration filters is carried out in the optek calibration laboratory according to the recommendations of ISO 17025. Since the application range of NIST SRM is restricted to the UV-VIS wavelength range. Prior to the calibration of a reference calibration filter with the optek reference photometer the photometer was calibrated by using the double aperture method.com . The unbroken chain of comparisons in this case ends with measurements of a reference spectrophotometer in the „NIST Advanced Chemical Sciences Laboratory“(ACSL). Nevertheless.pdf www. may vary and. Since instrument specifications. for instance. Overview The goal of this test is to check the measuring chain. which brings the measurement values in a process photometer closer to those of a certified spectrophotometer. To minimize the influence of reflections on filter surfaces. with respect to photometric accuracy. sensor bodies. these filters are mounted in the holder in an angled position (see fig.pdf www. Calibration of optek VIS and NIR sensors 5.1. Insufficient photometric accuracy or linearity may be caused by the following effects: ƒ Non-linearity of used SI photodiodes. such as sensor types and designs.1.5. 0. This allows using the calibration filter for calibrating any type of optek VIS or NIR photometer specified in chapter 4. have a slight impact on the VIS-L and NIR-L filter readings.80 CU.1: FH03B filter holder with filter installed in an angled position ____________________________________________________________________________ -7optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28.1. Using calibration filters with different absorption levels tests linearity of the entire system. cable and converter. Offset & Slope. hence.2. Photometric accuracy and linearity 5.45 CU.com . due to component defects or humidity deposits on the diode bonding ƒ Hardware failure of the converter. it is necessary to discriminate between initial and subsequent calibration.optek.g. 1).90 CU and 1. Fig. These filters are almost wavelength-independent and therefore suitable for the specified wavelengths and wavelength ranges. When introduced into the light beam.1. or mA inputs affecting raw measuring values 5. Calibration Device optek offers calibration filters VIS-L045 through VIS-L180 and NIR-L045 through NIR-L180 with nominal absorption values of 0. e. Linearization Tables. such as Sensor Adaptation. consisting of sensor. Calibration filters cause a defined light attenuation at individual wavelengths and wavelength ranges. page 5. optical path length (OPL) and others. defective input cards ƒ Faulty wiring of sensor and converter ƒ Damaged cable plugs or termination on sensor and / or converter ƒ Wrong product definition due to selecting the wrong measuring function ƒ Unintentional or accidental activation of calibration functions. 03 CU 0.1.a.a.03 CU 0. n. page 7.01 CU 0. After constructional changes of the photometer.04 CU 0. n. n. Initial Subsequent AF16-N AS16-N VIS-L045 n. If the measuring system passes initial calibration.01 CU 0.065 CU 0.a.a. VIS-L090 n.03 CU 0.03 CU n.a ____________________________________________________________________________ -8optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28.a.01 CU 0.02 CU 0.03 CU 0. n.01 CU 0. The tolerance of the desired value is stated in the table 1 on page 8. n.015 CU 0. the initial value of a measuring system is recorded.com . Table 1: Tolerances for initial and subsequent calibration of optek photometers with optical path lengths up to 160mm.01 CU 0.a. They cannot be applied to any other photometer but are always required to be established for each photometer separately.a. n. Subsequent Calibration For subsequent calibrations.a.03 CU 0.015 CU NIR-L090 NIR-L180 AF16-F AS16-F AF26 0.015 CU 0. the initial value must be recorded again. n.a. For a subsequent calibration to pass.pdf www. n.a.optek. The exact tolerances for different filters and systems are listed in table 1 on page 8.a.a. n. caused by effects described in chapter 5.02 CU 0.a. n. n.03 CU 0. VIS-L180 n. NIR-L045 0.a.06 CU 0.015 CU 0.06 CU 0. Initial values as recorded only apply to the photometer tested. n.1. Constructional changes are: ƒ Change of interference filters or detector module ƒ Change of OPL ƒ Retrofit or change of sensor body b.01 CU 0. the initial value as recorded and documented during initial calibration serves as the desired (nominal) value of the individual photometer. the measured value must be within a certain tolerance of the initial value.a. Initial calibration During the initial calibration.a.06 CU 0.03 CU 0.02 CU 0.03 CU 0. it is very unlikely that the tested system exhibits insufficient photometric accuracy or limited linearity.015 CU 0. Spectral properties 5. By the same token. page 23) of this handbook.2. Calibration Certificate VIS-L and NIR-L Filters available from optek are delivered with a calibration certificate. and may vary within certain (tight) tolerances. page 14.com . optek has introduced the FH03 calibration cuvette. Instrument properties of a photometer are primarily defined by the installed optical filter. ____________________________________________________________________________ -9optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. A sample certificate is included in the appendix (chapter 11. the effective measuring wavelength is not only determined by instrument properties of the photometer but also by spectral characteristics of the compound to be analyzed. Resolution. In photometers.3. 5. however. calibration certificate and calibration filter are crossreferenced to each other ƒ Nominal absorption value of the filter ƒ Certified absorption value including expanded uncertainty for respective VIS and NIR wavelengths ƒ Measuring conditions. To this end.1. If and to what extend this may effect the measurement. The best. is not defined for instruments that are not adjustable in frequency (or wavelength). and Full Width at Half Maximum (FWHM).1. and probably the only calibration of a process photometer with respect to concentration as the measuring quantity is the use of the product to be analyzed or monitored by the photometer. Such calibrations using actual product may be carried out at defined frequencies and always prior to commissioning a VIS or NIR photometer.2. among other information.1. such as mean wavelength. The advantage of doing so is the direct applicability of test results to the process measurement. spectral accuracy of photometric systems cannot be determined by the location of transmission maxima. Each of these calibration certificates contains.5. Overview Evaluations of spectral properties are not straightforward and require a more detailed explanation. depends on the application itself. the following important information: ƒ ƒ Certificate number Calibration filter type with serial number Via serial number.1.3. which is characterized by parameters.2. at which absorption values were recorded ƒ Spectrophotometer used for certified measurements including reference standards used for calibration of the device ƒ Application of the calibration filter to optek VIS and NIR sensors An example is given in chapter 7. Spectrophotometers require calibration of spectral resolution and accuracy.optek.pdf www. which is also engraved on the filter holder of the calibration filter. the absorption spectrum of the compound to be measured also has an impact on the spectral response properties of the photometer. The most efficient way of testing spectral properties is.2. The exact procedure is described in chapter 7.5.2: Calibration Cuvette FH03 ____________________________________________________________________________ .optek.pdf www. Calibration Devices As already mentioned. using the FH03 Calibration Cuvette (see. Fig. Fig.3. 2) filled with the compound to be measured.2.10 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28.com . which is why testing of these properties must be performed with regard to the intended application. page 16. finger marks or scratches can damage the calibration filter and require recertification.optek. For protection. Handling and Storage 6.pdf www. Handling and Storage of optek Calibration Filters Since optek calibration filters serve as important calibration tools. streaks. Especially dust.1. Observe the following basic conditions: ƒ ƒ ƒ ƒ ƒ ƒ Do not remove the calibration filter from the mounting. Calibration filters should be stored in the filter storage boxes provided at ambient temperatures from 15°C to 30°C (59°F to 86°F) and a relative humidity not exceeding 70 %.com .6. Do not scratch the surface. Do not change the filter’s orientation inside the filter holder. The air should be free of corrosive vapor.11 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. ____________________________________________________________________________ . they require very careful handling so that their functionality is not affected by external influences. Storage temperature: 15°C to 30°C (59°F to 86°F) Air humidity: 0 % to 70 % Note! Store calibration filters in dry cabinets or other appropriate cabinets so that the filters are protected against variations in temperature and humidity. store calibration filters under exclusion of UV light in a dust-and oil-free place. After that. ____________________________________________________________________________ . rinse them with distilled water. Cleaning of optek Calibration Filters and Cuvettes Prior to use. chips.pdf www. cuvettes should be partly filled with solution. Handling of Calibration Cuvettes Please observe the following handling instructions for optek’s FH03 calibration cuvette: ƒ ƒ ƒ ƒ ƒ ƒ Prior to use.2.com . Note: Calibration filters should only be cleaned when required. Cuvettes should be stored in their corresponding boxes. through proper handling of calibration filters and cuvettes. Do not clean cuvettes in an autoclave or in ultrasonic baths since cuvettes could be damaged. 6. The solution should be discarded and the cuvette rinsed with water again. Always handle cuvettes with special care to keep inner and outer surfaces clean and to avoid scratches. and scratches and replaced if necessary. Before filling cuvettes with any solution. especially finger marks. shaken and turned upside down so that the solution wets the inner surface of the cuvettes. As a basic rule. Carefully remove any surface soiling capable of absorbing light or particles that might scatter incident radiation: ƒ ƒ Carefully remove surface particles using a soft lens brush that does not scratch the optical surface. Humidity and finger marks should be removed with lint-free paper or lens cleaning paper.g.6. it is recommended to avoid any soiling. Remove absorbing surface soilings with a solvent that is nonalkaline and free of surfactants (e.3.optek.12 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. calibration cuvettes should be checked for cracks. Isopropanol). visually inspect calibration filters and cuvettes for dust or other soiling such as finger marks or condensation and clean them if necessary. filter type. 2. Sensor Body and Zero Medium All procedures require a clean and empty sensor body or a sensor body completely filled with stable zero medium. Linearization. C4000 converters with software version C2 from December 11th. If several calibration functions are being used. such as Sensor Adaptation. Make sure detector assemblies are tightly screwed onto measuring cell. 3. page 7.optek. record the current measuring values. or later versions may use the Detector Monitor displaying raw measuring values. General Procedure 1. Sensor Identification Record serial numbers of sensor and converter as well as activated measurement input channels of the converter. 4.1. Remove Sealing Cover and Insert Filter • Loosen the 2 screws of the sealing cover of the detector adapter and remove sealing cover and screws.13 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. otherwise measurement results will be compromised. 2007. Zero Point Adjustment / Record Initial Value If possible. The described procedures only apply to optek VIS and NIR Sensors AF16-N. zero the instrument. date of calibration and nominal values. 6. AF16-F. record all relevant values. it is recommended creating your own Calibration ‘Product’ in the C4000 converter. Damping or mA inputs. Filter Identification Record serial number.the two pilot pins must be inserted in the alignment holes.com . 5. Also ensure that there is no condensation or soiling on the windows. For further information. please refer to the C4000 instruction manual. Record / Disable Additional Measurement Functions In case your measuring values are using calibration functions. please refer to the instruction manuals of the particular converters and sensors.pdf www. Allow analyzer at least 30 minutes to warm up. For further information on the product definition and the detector monitor.7. Clean it if necessary. 7. Calibration Procedures The following chapter deals with the calibration procedures using test devices introduced in chapter 5. 7. It is not necessary to remove the sensor body from the pipeline. ____________________________________________________________________________ . AS16-F and AF26. • Insert filter holder in the detector adapter. Preparation The system to be calibrated must be wired and fully operational. Otherwise. All calibration procedures are described in general. • Take filter holder out of storage box and visually inspect reference filter for dust or soiling. AS16-N. Tolerances are given in the calibration certificate on third page.2. 7. Evaluation of Measuring Result Take calibration functions into account that are activated.pdf www. then compare resulting value with certified nominal value on certification. The converter settings chosen for this example include sensor adaptation and processing a mA-input. ____________________________________________________________________________ . Nominal values for the photometric accuracy and linearity tests are the values given in the calibration certificate on first page. chapter ‘Instructions for use’. Make sure not to loose any screw.com . 7.1. 8.Fig.1.2.optek.2. 9.3: Insert Calibration Filter Note: The screws on the sealing cover are not secured against falling out. Record Measuring Result Record displayed measuring result. These settings must be taken into account when determining the measuring result.14 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. Example Filter Calibration – Photometric Accuracy and Linearity The following example documents a photometric accuracy test using an NIR-L090 calibration filter and sensor AF16-N. Calibration with Calibration Filter 7.1. as shown in this example. Photometric Accuracy and Linearity This test determines the accuracy and linearity of the photometer with respect to the certified nominal values. 9 10 Multiplication mA Input 1: yes 11 Value mA-Input: 50% 12 Measuring Result Zero Medium: 0.pdf www.889CU 05 Admissible Range: 0. 10.399 15 Compensate for Sensor Adaptation (No.895 ____________________________________________________________________________ . 09) * (1/0.03.443 16 Compensate for mA Input (No. this means: Admissible Range: 0. 12) 0.002=0.9)= 0.com .optek.5)=0.869 – 0.15 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28.877 – 0.909CU 06 Serial Number Sensor: 12345 07 Serial Number Converter: 12346 08 Measurement Input: A 09 Sensor Adaptation ABS-CU (A): 0.886 22 Calibration Value: 0.401CU-0.2010 04 Certified Value: 0.Table 2: Example Initial Filter Calibration. Description: Data: 01 Filter Type: NIR-L090 02 Filter ID: FH03B-11111-22 03 Calibration Date: 31.002 13 Measuring Result Calibration Filter: 0.886 CU 23 Evaluation: passed For a subsequent calibration. Photometric Accuracy and Linearity No.401 14 Measuring Result minus Offset Zero Point (No.11) * (1/0. 800 CU 0. such as a spectrophotometric measurement or the absolute mass of a test liquid.2.pdf www. The concentration of the calibration liquid in the cuvette should roughly represent the absorption of the working point. Table 4: Example Calibration with FH03 Calibration Cuvette Working Point 100 % Calibration Point 95 % 100 % 105 % Concentration Cuvette 380 mg/l 400 mg/l 420 mg/l Measured CU Value 0.860 CU ____________________________________________________________________________ .7. It is the user’s responsibility to choose the appropriate reference measurement. For this reason. calibration with the FH03 calibration cuvette filled with product or a specified calibration liquid has already been described as the best calibration method for photometers.1. Normally this procedure results in smallest deviations between cuvette and sensor body measurements. page 13.com .0 0.3. When choosing a calibration liquid. 7. it is recommended to establish a correlation between reference measurement and photometric measurement during initial calibration.3. possible differences in concentration between initial and subsequent calibration must be taken into account. and the absolute concentration of a product sample can also vary within certain limits. Example Calibration with FH03 Calibration Cuvette A concentration of 100 mg/l of a substance is to be measured in a sensor body with 10 mm OPL (m=4). differences in OPL between sensor body and cuvette must be corrected by a conversion factor m. Since preparation of a test liquid always involves some uncertainties. Therefore.4 2. Spectral Properties In chapter 5. In many cases. page 9. the product to be analyzed or any appropriate calibration liquid can be used. Calibration with Calibration Cuvette 7.5 1 5.0 2 10 4 20 8 40 16 For testing a photometer with the FH03 calibration cuvette.1.1. some additional aspects must be observed apart from the basic steps described in chapter 7. In these cases.2. A subsequent calibration with an FH03 calibration cuvette requires the test liquid be identical with that used for initial calibration. The accuracy of concentration is estimated to be approximately 2 %.16 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. it is important its spectrum matches the product spectrum as much as possible. It is most important to note that the correlation between absorption and concentration does not primarily depend on the concentration but on the reported absorption. This method also consists of initial and subsequent applications. When using the FH03 calibration cuvette.3. calibration points are chosen to be apart by ±5 % increments. Table 3: Conversion Factor m as a Function of Sensor Body OPL OPL [mm] Conversion Factor m 1. The weight concentration (mass) of this substance serves as a reference. For this reason. correlation was already established during the qualification process of the measuring system.optek. This procedure tests the photometer in one single test step. the characteristic curve for determining the actual concentration and the resulting nominal value should be used for calibration.740 CU 0. 006 CU Absorption In Value O.7 370 380 390 400 410 420 430 c [mg/l] Fig.? 0.75 0.006 CU tolerance range for the photometric measurement.9 0. which will be used in subsequent calibrations for determining the photometric nominal value. 4: Example of a Calibration Curve For a subsequent calibration.Thus. Fig.8 0. this means: Table 5: Subsequent Calibration Target Concentration Actual Concentration 400 mg/l 399 mg/l Absorption Out 0. it is important to note that the test will have passed if the photometric value is found to be within the uncertainties.optek. and concentration uncertainty is ±0.85 CU 0.K. slope is 0.796 ±0.17 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28.003 CU/mg/l (in the cuvette). However.79 6 0.795 CU yes Uncertainties including those of the sensor cannot be discussed here due to the large number of possible applications. 4 shows the correlation between reference measurement (concentration in [mg/l]) and photometric measurement.pdf www. ____________________________________________________________________________ .com . 0. corresponding to ± 0.5 % (here 2 mg/l). They can serve to convert measuring result to other unit scales (mostly concentrations). 4. make sure linearization tables that may previously have been activated are disabled.0 0. Linearization Curves Linearization Curves can be defined at select converters or in downstream signal processing. For example. the user may decide to increase number of calibration points in the linearization table. if deemed necessary. Depending on the OPL of the sensor body. Define the optical path length (OPL) of your sensor body. It is important to note that the correlation between absorption and concentration depends more on reported absorption than on concentration.18 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. In case mA input channels or sensor adaptations are active. In this case concentrations required for cuvette measurement are 0.5 mm OPL are as follows.com . For this reason.1. 6: Conversion Factor m as a Function of Sensor Body OPL OPL [mm] Conversion Factor m 1. Depending on measuring range and curve shape.1.5 1 5. some additional aspects must be observed as well. 8. double concentration does not necessarily mean double absorbance.4 2. determine to what extent they apply to the expected result and whether they affect measurement the same way as in the cuvette (such as temperature compensation). Prior to establishing a linearization curve. conversion factors m for a calibration cuvette with 2.optek. page 13).5*m* cPmax and m* cPmax. Especially for non-linear correlations between concentration and absorption. Table 7: Linearization Product Concentration cP in the process Product concentration cC in the cuvette 0 0 ½ * cPmax ½ *m* cPmax cPmax m*cPmax CU value measured with cuvette ↓ ↓ Output values in the Linearization table Input values in the Linearization table ____________________________________________________________________________ . Define maximum product concentration (cPmax) to be measured in the process.0 2 10 4 20 8 40 16 3. 2. use of linearization curves is recommended. It is recommended to establish a linearization curve using at least three calibration points. When using the FH03 calibration cuvette (apart from some basic steps described in chapter 7. 50 % and 100 %. General Procedure 1. differences in OPL between sensor body and cuvette must be corrected by a conversion factor m. Table.8.pdf www. including relative concentrations of 0 % (zero medium). such as adjusting an output value of a measuring system until its reading agrees with that of a reference standard. the relationship between values of quantities indicated by a measuring system and corresponding nominal values (calibration standards). USA NIST-traceable Measuring results tracing back to a chain of comparisons to standards approved by NIST are referred to as NIST-traceable. Mean wavelength Center wavelength between the two wavelengths. NIST National Institute of Standards and Technology. therefore with inherent minimal measurement uncertainties. No reference standard required here.19 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. T = % Transmission Calibration Operation of establishing. within which measurements can be confidently asserted to lie. under specified conditions. at which transmission values reach 50 % of the peak maximum.optek.com . Full Width at Half Maximum FWHM Distance between two wavelengths of a transmission curve of an interference filter. ____________________________________________________________________________ . OD can be calculated by dividing absorption by OPL in centimetres. Double aperture method Method to determine the linearity of a light measurement. AU Absorption Unit The dimensionless absorption value of log (1/T). Glossary Table 7: Glossary Term Explanation Adjustment Operation of bringing a measurement system into a state of performance suitable for its use. OD Optical Density Absorption value standardized to an optical path length (OPL) of 10 mm. Integration time Property of a spectrophotometric measurement. at which transmission values are equal to 50 % of the peak maximum of this curve.pdf www. T = % Transmission Deviation of linearity Deviation of the real measurement from the theoretical linear correlation.5 mm OPL) and inline sensor body in the process. CU Concentration Unit The dimensionless absorption value of log (1/T) measured with an optek filter photometer. whose absorption values are equivalent to those found in the process sensor body at a different OPL. a spectrophotometer looks at the incoming light to determine an average measurement value. Conversion Factor m Factor that accounts for the difference in OPL between calibration cuvette (2. Expanded uncertainty Standard uncertainty multiplied by coverage factor k to define interval about measurement result.9. Amount of time. corresponding to 95% of measurements being within the interval defined. Used to calculate the concentrations of calibration standards in the cuvette. Mostly k=2. pdf www. which measures at fix wavelength(s). Photometric accuracy Accuracy with which a measurement of two photocurrents and the calculation of it’s relationship with respect to it’s logarithm is carried out. Used directly in the process line. PTB “Physikalisch-Technische-Bundesanstalt”. Process photometer Measuring system for absorption / transmission. each contributing to the stated measurement uncertainty.Optical path length (OPL) Distance that light passes through a sample.com . SRM “Standard Reference Material ®” CRM issued under the NIST trademark. which is likely to enclose the true (‘correct’) value. Sensor adaptation Factor used to adjust measurement result of a measuring function. Traceability Property of a measurement result relating the result to a stated metrological reference through an unbroken chain of calibrations of a measuring system or comparisons. Tolerance / uncertainty Region about a measurement value.optek. Peak wavelength Wavelength. National metrology institute in Germany. Designed usually for laboratory use. Spectrophotometer / Spectrometer Apparatus measuring absorption / transmission values over a wavelength range of different wavelengths (simultaneously or successively). Spectral accuracy Accuracy with which the set wavelength of a spectrophotometer corresponds to the target wavelength. Slit width Property of a spectrophotometric measurement defining spectral resolution. at which transmission curve of an interference filter reaches its maximum.20 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. Braunschweig. ____________________________________________________________________________ . Function of optek C4000 converter. Slit height Property of a spectrophotometric measurement that affects geometry and intensity of the light beam. Spare parts Calibration filters and cuvettes VIS-L0.8 FH03 calibration cuvette Recertifications Recertification VIS-L Recertification NIR-L 1442-0025-0223-13 1442-0025-0223-23 1442-0025-0223-33 1442-0025-0213-13 1442-0025-0213-23 1442-0025-0213-33 1448-0102-0000-03 1452-0600-1000-03 1452-0500-1000-03 Accessories and spare parts Case for 7 filter boxes Set stoppers for calibration cuvette (10 pieces) O-Ring set 2.com .21 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28.00 Viton (20 pieces) O-Ring set 18.45 NIR-L0.9 VIS-L1.77 x 1.45 VIS-L0.8 NIR-L0.00 x 1.optek.9 NIR-L1.78 Viton (4 pieces) Screw set M3 x 10 DIN7985 (10 pieces) 1450-1000-0000-00 1206-0010-4840-86 1203-0020-0050-02 1203-0004-0013-02 1206-0010-0058-01 ____________________________________________________________________________ .10.pdf www. disassemble the system components and separate them according to different material groups. This signed declaration must be included with the shipping documents on the outside of the packaging. Declaration of decontamination For the safety of our employees and because of legal regulations we need a signed “declaration of decontamination” before your return can be handled.com . Appendix 11. Any returns which were exposed to hazardous substances and were not professionally decontaminated are not accepted and will be sent back on your cost. Dispose of materials according to national and local regulations.11. Disposal Special legal regulations apply to the return and disposal of industrial waste equipment. optek’s declaration of decontamination and contact information can be found on our website www. However.optek. products may be shipped to optek for disposal. manufacturer and user can contractually agree on which party is to fulfil these legal obligations.1.22 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28. ____________________________________________________________________________ . Observe current national disposal regulations.pdf www. 11.2. please separate materials into the following groups: • Paper / paperboard • Plastic For disposal. If no agreement has been made.optek. To dispose packaging material.com. 23 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28.optek.pdf www.11.com .3. Sample certificate for VIS-L090 Calibration Filter ____________________________________________________________________________ . ____________________________________________________________________________ .pdf www.optek.24 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28.com . pdf www.____________________________________________________________________________ .25 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28.optek.com . 26 optek-Manual--1004-5003-02--Calibration-Handbook-VIS-NIR-US-2012-06-28.com . www. Ltd.com USA optek-Danulat Inc.pdf www. N118 W18748 Bunsen Drive Germantown WI 53022 / USA Phone: +1 262 437 3600 Toll free call: +1 800 371 4288 Fax: +1 262 437 3699 E-Mail: [email protected] Please visit our website for contact details of our local distributors in other countries. 25 Int’l Business Park #02-09-f German Centre Singapore 609916 Phone: +65 6562 8292 Fax: +65 6562 8293 E-Mail: info@optek. China 201203 Phone: +86 21 2898 6326 Fax: +86 21 2898 6325 E-Mail: [email protected] Singapore optek-Danulat Pte. Contacts For further inquiry.com ____________________________________________________________________________ . 88 Keyuan Road Pudong Zhangjiang Shanghai. feel free to contact us or our distributing partners at any time: Germany optek-Danulat GmbH Emscherbruchallee 2 45356 Essen / Germany Phone: +49-(0)201-63409-0 Fax: +49-(0)201-63409-999 E-Mail: [email protected] China optek-Danulat Shanghai Co.optek.com 中国 优培德在线测量设备(上海) 有限公司 上海张江科苑路88 号德国中心718 室 邮编:201203 电话:+86-21-28986326 传真:+86-21-28986325 E-Mail: info@optek-danulat. Ltd Room 718 Building 1 No.optek.
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