OVP PhEur 2.2.40
Contents
1. IT 1 Sample Compartment Test Channel Configuration Source NIR v Beamsplitter Quartz Measurement Channel 5 ample Compartment d z Detector AEAEE Make sure the measurement channel is prepared for the L WN Hier calibration before you start the measurement Instrument Configuration Sample Compartment Ami Accessory Title for new configuration Load Image Add new configuration Clear current Configuration caret Ho Figure 3 Setup OVP Bitmap of instrument type Bruker Optik GmbH OVP for PhEur 2 2 40 7 Test Setup If you click on the OVP Test Setup tab the following dialog opens M MEM I LI m m Figure 4 OVP Test Setup tab The line on the very top shows the test channel selected on the OVP Test Channel Setup tab If you activate the Run check box on the OVP Test Setup tab the following line will be displayed 8 OVP for PhEur 2 2 40 Bruker Optik GmbH Setting up OVP for PhEur 2 2 40 OVP Test Channel Setup OVP Test Setup IT 1 Sample Compartment with NIR Quartz TE InGads Internal Test Selection Run PO Test every 24 Hours Run OO Test every 12 Months IV Run PHEUR2240 as Figure 5 Configuring PhEur 2 2 40 test N sow Select PhEur 2 2 40 from the first drop down list and the OQ test category from the second If the OQ test has not been setup make sure that the e2. 10 SRS 10 010 standard This measures system performance at reduced light level Noise from the source detector optics and electronics make significant contributions at this level PhEur 5 2 2 40 Test Protocol E xl Wavelength Uncertainty Reproducibility Photometric Linearity TestSetup Photometric Noise A Requires Labsphere 99 Reflectance Standard SRS 99 010 Perform High Light Flux Measurement B m Labsphere 10 Reflectance Standard SRS 10 010 Perform Low Light Flux Measurement lm Measurement Range 8300 cm 1 4500 cm 1 Cancel Apply Help Figure 9 PhEur 2 2 40 Test Protocol Photometric Noise tab Bruker Optik GmbH OVP for PhEur 2 2 40 13 Test Setup Ae Use Water Vapor A Activate this check box if you want to perform the High Flux Noise measurement B Activate this check box if you want to select the Low Flux Noise measurement C The measurement range used for the specified channel The range is recommended by PhEur 2 2 40 but may be different if the instrument does not support this range 2 3 3 Wavelength Uncertainty Test In case of the wavelength uncertainty test you can choose between two test methods The recommended method measures a specific peak of water vapor This has the advantage of not requiring a reflectance standard and also grants a much higher precision The appendix describes the advantages of using water vapor for thi
3. ISSUE DATE AUTHOR Description File name REVISION 1 10 09 2002 Andrea Giehl Wavelength uncer Wavelength tainty test for Bruker accuracy doc FT NIR spectrometer 4 3 4 4 4 5 Introduction Wavelength uncertainty test is part of the instrumental tests needed for the qualification of an NIR spectrometer in accordance with e USP Pharmacopoeia Forum lt 1119 gt 26 2000 237 247 Ph Eur III 2 2 40 Near Infrared Spectrometry 43 44 This test is to ensure that the measured wavelengths are accurate and remain accurate for measurements in diffuse reflectance or transmittance mode Purpose The purpose of this document is to provide detailed information on the use of water vapor absorbance bands for the calibration and validation of Fourier Transform NIR spectrometers Measuring the water vapor absorbance band at a single wavenumber shall replace the wavelength uncertainty test of Michelson type FT NIR spectrometers required by USP for both diffuse reflection and transmission measurements NOTE wavenumber 1 wavelength USP Requirements In 1 the regulations are set for the Instrument Operational Qualification with regards to Wavelength Uncertainty They are as follows Wavelength Uncertainty Note The method used in developing wavelength uncertainty values is based on the NIST Center of Gravity algorithm Potential problems with internal calibration schemes are avoided by
4. OPUS Spectroscopy Software User Manual OVP PhEur 2 2 40 gt lt BRUKER LL 2006 BRUKER OPTIK GmbH Rudolf Plank StraBe 27 D 76275 Ettlingen www brukeroptics com All rights reserved No part of this manual may be reproduced or transmitted in any form or by any means including printing photocopying microfilm electronic systems etc without our prior written permission Brand names registered trademarks etc used in this manual even if not explicitly marked as such are not to be considered unprotected by trademarks law They are the property of their respective owner The following publication has been worked out with utmost care However Bruker Optik GmbH does not accept any liability for the correctness of the information Bruker Optik GmbH reserves the right to make changes to the products described in this manual without notice This manual is the original documentation for the OPUS spectroscopic software Table of Contents 1 Introduction 1354 arenae ue bod ek Reaw saw wesw SAN eee 1 1 1 PhEUr 2 2 40 T8S US os aac oa qu eat Se Senn a Du teta ee ew ae 1 2 Test Setup o s ceed ses ss Gade me eee ee S SCR Rua RU SEND CILE E AA CR S ce 3 2 1 Reference AIC ANS ds du S Ades CS ese X ue abdo cb AM osa opt 3 23 Setting up OVP Tor PhBut 2 2 40 c ousuesex Si awn eho oi rte qne RN 5 2 3 Reflection Measurement Mode 00 cc ccc cee eee 10 2 3 1 Photometric Linearity Test cedi ees ARE Heute tas eS 10
5. Ten sample measurements are performed and the band location of the specified band is evaluated for all ten spectra Based on the band location of these 10 single measurements the average is calculated The maximum deviation determined from this average The deviation must not exceed a specified limit which depends on the type of standard used The table below shows the evaluated band and maximum deviation of a few standards Standard Band used cm Maximum Deviation cm Water vapor 7306 736 0 05 NIST SRM 2036 10245 0 1 Ch5Cl 6064 0 1 16 OVP for PhEur 2 2 40 Bruker Optik GmbH Transmission Measurement Mode 2 4 Transmission Measurement Mode Pheur Setup i x Photometric Noise Wavelength Uncertainty Reproducibility TestSetup Photometric Linearity Photometric Linearity European Pharmacopoeia 5 Section C Reflection Measurement Transmission Measurement Measurement Channel z Test Selection Last Test Date Time v Photometric Linearity IV Photometric Noise rs IV Wavelength Uncertainty IV Wavelength Reproducibility Figure 12 PhEur 2 2 40 Test Protocol TestSetup for transmission The test setup for the transmission mode is very similar to the one for reflection mode Initially all tests are selected The Test Selection group field contains all tests available for transmission measurement To perform all four tests select all th
6. for water vapor to determine the wavelength accuracy test is sufficient for a Michelson type FT instrument The wavelength in an FT instrument is calibrated by an internal He Ne laser with a wavelength of 633nm The value of the He Ne wavenumber is entered in the control software of the instrument and slightly adjusted so that this specific water line is accurately registered in wavenumber and hence wavelength by taking the reciprocal Theoretically for an FT instrument all wavelengths across the entire spectrum will be accurately determined from this single setting Repeated measurements of the water vapor line with a calibrated FT instrument will show residual fluctuations due to spectrometer noise These shifts however are extremely small and can be neglected The residual fluctuations at all other wavelengths will be of a similar negligible amount Bruker Optik GmbH OVP for PhEur 2 2 40 35 Appendix Wavelength Uncertainty Test using Water Vapor 4 7 Reference for Water Vapor Absorbance Spectrometer calibration for H O bands Resolution 25 cm Single channel spectra Target 7 306 74 cm 7800 7600 7400 7200 7000 6800 6600 Wavenumber cm 1 Figure 23 Spectrometer calibration using the water vapor band at 7 306 74cm There is no certification needed for water vapor as it represents a natural constant and is always the same substance present in the ambient air It can be used for both transmittance and d
7. the instrument can be considered as being qualified in the region from 10300cm 971nm to 5130cm 1949nm Spectra of this standard are shown in figure 20 and figure 21 in wavenumbers For the NIST SRM 2035 transmittance standard the maximum allowed deviations specified in the certificate depend on the investigated absorbance band and the applied resolution The NIST certificate 3 applies to the COG of 7 wavelength bands certified in nm and cm Examples for an FT instrument with a resolution of 4cnr 5138 45cm 6804 65cm 7313 46cmr 8178 58cm 8681 56cm 9293 38cm 10245 43cm 1 Holmium oxide solution NIST SRM 2034 wavelength standard from 240 to 650nm may be used cur rently in the 650 to 1100nm region although bands are not certified in this region 2 A rare earth oxide in glass transmission wavelength standard SRM 2035 has been certified recently by NIST This standard may be used in transflectance mode but is not currently certified for such use Bruker Optik GmbH OVP for PhEur 2 2 40 33 Appendix Wavelength Uncertainty Test using Water Vapor The NIST certificate provides the uncertainty on the measurements which are said to be about equivalent to a 95 confidence interval The actual limits for the allowed deviations are however not defined in the certificate or the USP guideline When determining the band position the same center of algorithm COG has to be used as the algorithm a
8. Measurement OK Cancel Apply Help ea Figure 15 PhEur 2 2 40 Test Protocol Photometric Noise tab A Activate this check box if you want to perform the High Flux Noise measurement B Activate this check box if you want to perform the Low Flux Noise measurement C The measurement range used for the specified channel The range is recommended by PhEur 2 2 40 but may be different if the instrument channel does not support this range 2 4 5 Wavelength Uncertainty Test In case of the wavelength uncertainty test you can choose between two test methods The method recommended by Bruker measures a specific peak of water vapor This has the advantage of not requiring a transmission standard and also grants a much higher precision The appendix describes the advantages of using water vapor for this test 20 OVP for PhEur 2 2 40 Bruker Optik GmbH Transmission Measurement Mode A E Use Water Vapor MEME PhEur 5 2 2 40 Test Protocol i al xj TestSetup Photometric Noise Wavelength Uncertainty Reproducibility Photometric Linearity Select Standard C Use Internal Reference Standard BRM 2065 C Use extemal certified Reference Standard Transmission Recommended Water Band 7306 735 cm 1 Use Water Band at 7306 736 Cancel Apply Help Figure 16 PhEur 2 2 40 Test Protocol Wavelength Uncertainty test A Activating the Use Water Vapor option butt
9. REPORTS directory and can automatically be displayed and or printed To have the report displayed and printed you require the Adobe Acrobat Reader which is available on the OPUS installation CD 30 OVP for PhEur 2 2 40 Bruker Optik GmbH References 4 Appendix Wavelength Uncertainty Test using Water Vapor 4 1 References 1 Second Supplement USP NF lt 1119 gt Near Infrared Spectrophotometry 2 H20 vapor calibration engl doc Dr Axel Keens 31 May 2001 3 2035 pdf National Institute of Standards amp Technology Certificate Standard Reference Materiali 2035 4 C Kradjel U Grummisch R Rachlis in Making Light Work Advantages in Near Infrared Spectroscopy Developed from the 4th International Conference on Near Infrared Spectroscopy Aberdeen Scotland August 19 23 1991 edited by I Murray and I A Cowe VCH Weinheim 1992 Page 470 5 H G nzler H M Heise IR Spektroskopie Eine Einf hrung 3 Auflage VCH Weinheim 1996 Seite 84 6 J Gronholz W Herres Understanding FT IR Data Processing I amp C Dr Alfred Huethig Publishers 1984 Page 2 7 H Gremlich Infrared and Raman Spectroscopy 82 1 UlImann s Encyclopedia of Industrial Chemistry 1994 VCH 8 P Griffiths Fourier Transform Infrared Spectrometry 81 VII 1986 Wiley ISBN 0 471 09902 3 Bruker Optik GmbH OVP for PhEur 2 2 40 31 Appendix Wavelength Uncertainty Test using Water Vapor 4 2 Document History
10. a set of certified reflectance standards with known reflectance values PhEur 2 2 40 requires one standard 99 for reference and at least four standards for the test itself 80 40 20 and 10 When measuring samples of low reflectance an additional low reflecting standard 5 is required Enter the data for the certification table These data are listed in tables in the calibration certificate or are provided in digital form on a CD or diskette Click on the Photometric Linearity tab to open the following dialog PhEur 5 2 2 40 Test Protocol E x Photometric Noise Wavelength Uncertainty Reproducibility TestSetup Photometric Linearity B MERE tandards Set A ne amp 216 v Report Number 41666 2 16 Read Calibration I of Calibration October 11 2005 Data D a Ts Use 4 Standards Use 5 Standards C Use 7 Standards E SRAS 99 010 SAS 80 010 SRS 40 010 SRS 20 010 SRS 10 011 1100nm 0 990 0 824 0 428 0 214 0 114 F 1150nm 0 990 0 826 0 432 0 218 0 118 1200nm 0 989 0 827 0 433 0 221 0 119 A 1250nm 0 987 0 827 0 434 0 222 0 122 1300nm 0 987 0 828 0 435 0 223 0 120 1500nm 0 986 0 830 0 440 0 228 0 125 1550nm 0 988 0 833 0 443 0 229 0 125 1ANN nm fn aaa naw N 443 nan n1 5 or 4 b v Use Straylight Correction Cancel Apply Help Figure 7 PhEur 2 2 40 Test Protocol Photometric Linearity tab Bruker Optik GmbH OVP for PhEur 2 2 40 11 Test Setup A If you click on this button a
11. for new configuration entry field to specify the current setup by a descriptive text 1 Short term test which evaluates the spectrometer performance and proper spectrometer functioning Bruker Optik GmbH OVP for PhEur 2 2 40 5 Test Setup Click on the Add new configuration button Now all the other selection fields will no longer be hidden and can be filled in Setup O P x A OVP Test Channel Setup A OVP Test Setup A Current Test Channel BB o 1 Sample Compartment m m Test Channel Configuration p TEE Source NIR Beamsplitter Quartz Measurement Channel S ample Compartment hd Detector TERROR Tene C Make sure the measurement channel is prepared for the L wN Measure COE calibration before you start the measurement LWN D Instrument Configuration m Accessory Title for new configuration r E Load Image G Add new configuration F Clear current Configuration H Figure 2 Setup OVP Activated drop down lists A The drop down list shows the test channel used by OVP B For each spectrometer test channel you have to assign a measurement configuration to be used during actual validation measurement This is a valid combination of source beam splitter measurement channel and detector As soon as you have selected all components the appropriate instrument configuration C and the bitmap E specified for the measurement chan
12. instructions and insert the standard using whatever method is appropriate for the instrument configuration you are using Note The measurement requires specialized holders for the reference standards After the reference measurement has completed you will be prompted for each of the reflectance standards selected in the PhEur Setup dialog Insert each standard as requested and follow the instructions to perform the measurements If each of the standards has been measured the final results will be computed 3 1 2 Transmission Measurement Prerequisites The Photometric Linearity test for transmission measurements uses the glass filters mounted on the IVU Internal Validation Unit The test itself runs fully automatically and needs no user interaction For instruments with only two glass filters on the IVU an external NG 11 glass filter is required Bruker Optik GmbH OVP for PhEur 2 2 40 27 Run OVP Tests 3 2 Photometric Noise Test 3 2 4 Reflection Measurement Prerequisites The Photometric High Light Flux Noise test for reflection measure ments requires the Labsphere 99 reflectance standard SRS 99 010 The Photometric Low Light Flux Noise test for reflectance measure ments requires the Labsphere 10 reflectance standard SRS 10 010 Foran integrating sphere an 8 degree sample holder must be used Follow the wizard instructions and insert the standard using whatever method is appropriate for th
13. spectra and the frequencies used for evaluation are shown in figure 14 Filter NG9 Fosorbance Units 11000 10000 9000 8000 7000 6000 5000 4000 Wavenumber cm 1 Figure 14 Typical filter spectra 2 4 2 Photometric Noise Test The photometric noise test involves measuring spectra using the open channel and one of the glass filters on the IVU as low transmission material The analysis is performed by tabulating the Peak to Peak PP noise level in successive 100nm 300cm spectral segments between 1200 and 2200nm 8300 and 4500cmr and the average of these values Depending on the measurement channel a different frequency range may be used The High Flux Noise measurement uses the open channel The Low Flux Noise measurement uses the glass filter NG9 or the internal Spectralon This measures system performance at reduced light levels Noise from the source detector optics and electronics make significant contributions at this level If one of the tests is not available for a certain instrument configuration this test will be disabled Bruker Optik GmbH OVP for PhEur 2 2 40 19 Test Setup A B C ERN Measurement Range 8300 cm 1 4500 cm 1 PhEur 5 2 2 40 Test Protocol amp xj Wavelength Uncertainty Reproducibility Photometric Linearity TestSetup Photometric Noise Uses an empty channel measurement v Perform High Light Flux Measurement Uses internal Filter v Perform Low Light Flux
14. 2 16 Date of Calibration October 11 2665 SRS 99 616 888 8 986 858 8 987 988 8 987 958 8 990 1888 8 989 18058 8 989 1108 8 990 1158 8 990 1208 8 989 1258 8 987 1308 8 987 1358 8 986 1400 8 986 1456 8 986 1508 8 986 1558 8 988 1600 8 988 1650 8 986 1700 8 983 1750 8 986 1866 6 984 1858 8 988 1988 8 988 1958 8 977 2808 8 972 2858 8 959 2108 8 952 2158 8 9549 2208 8 965 2258 8 967 2308 8 959 2358 8 958 24568 6 943 2508 8 953 SRS 88 018 808 8 815 858 8 817 onn A RIR Figure 8 Text file example for data input 12 OVP for PhEur 2 2 40 Bruker Optik GmbH Reflection Measurement Mode You do not need to add factors for every column of reflection stan dard only enter the data for standards you will be using You have to enter a value for every frequency in the table You have to navigate by using the mouse as the Zab and Enter keys cannot be used 2 3 2 Photometric Noise Test The photometric noise test involves measuring spectra of high and low light throughput which is achieved by using high and low reflectance material The analysis is performed by measuring the peak to peak noise level in successive 100nm 300cmr spectral segments between 1200 and 2200nm 8300 and 4500cm Depending on the measurement channel a different frequency range may be used The High Light Flux measurement uses the Labsphere 99 SRS 99 010 standard The Low Light Flux measurement uses the Labsphere
15. 2 3 2 1 Photometric Noise Test daos ne edens Kew onan Danner ed 13 2 3 3 Wavelength Uncertainty Test ies ev rU S eas 14 2 3 4 Wavelength Reproducibility Test 0005 16 2 4 Transmission Measurement Mode 0 0000 e cece eee eee 17 2 4 1 Photometric Linearity Test eso ance yo we Pene ed d 17 242 Photometric Noise Test duse eee FRAN ueste aas 19 24 3 Wavelength Uncertainty Test seed a x Pne e S ada 20 2 4 4 Wavelength Reproducibility Test 0 0 00 00008 23 3 Rum OVP Tests esse zVwRx Ix CR Sag RO Wie weal AUR 25 3 1 Photometric Linearity Test ose od sa e oce a eta inn ne ceto s 27 3 1 1 Reflection Measurements 252i Lee Road eee res dda ha IS 27 3 1 2 Transmission Measurement 0 0000 cece eee eee 27 3 2 Photometric Nose st sd re weet Sad ae ew a uus 28 3 2 1 Reflection Measurement uova oe aoa ba us epa ous 28 3 2 2 Transmission Measurement 2 ones du afe ea E EX PES 28 3 3 Wavelength Uncertainty Reproducibility Test 29 3 3 1 Reflection Measnrenielito ius ele had ee Shae E nO RN Pew US 29 3 3 2 Transmission Measurement llle 29 3 4 P inting Reports 4 445005 tase Dor Sar eae aon hor eee as 30 4 Appendix Wavelength Uncertainty Test using Water Vapor 31 4 1 References a osa Pad eod A leta aes qos eh oe Bes 31 4 2 Document History Coeur icc at irt tc aci n te gw es e ce le Fg nd 32 4 3 IrittOQUCct IOILa 16e 5 53 Shes hid CERES
16. 2240 OQ Test expires in 359 days 23 Hours 40 Minutes Figure 19 OVP test status As soon as you have activated the check box for the respective test protocol you can see which test s will be performed by the browser like display next to the bitmap All measurement results are stored in a report PDF file and in the UserData database To append a comment to the current test protocol entry write a comment into the User Comment entry field Click on the Run selected Tests button to start the respective tests If you do not want to perform any test click on the Cancel button 26 OVP for PhEur 2 2 40 Bruker Optik GmbH Photometric Linearity Test 3 1 Photometric Linearity Test 3 1 4 Reflection Measurement Prerequisites The photometric linearity test for reflection measurements requires the use of the 99 reflectance standard SRS 99 010 for refer ence background measurement For an integrating sphere the straylight correction spectra must have been measured using a Bruker certified gold standard with the certified reflection factor entered to measure the straylight correction spectra Foran integrating sphere the straylight correction check box in the PhEur setup has to be set and the proper channel selected Foran integrating sphere an 8 degree sample holder has to be used For a fiber solid probe the straylight correction must not be used Instead use an appropriate sample holder Follow the wizard
17. 99 for reference VECTOR 22 N measurement SRM 1920a or KTA 1920x or SRM 2036 or CH Cl Suspension in TiO gt MPA with BRM 2065 Transmission BRM 2065 SRM 2065 or and Glass filters SRM 2035 or NG4 NG9 and NG11 BRM 2065 or CH Cl MPA MATRIX Transmission None SRM 2065 or VECTOR 22 N with SRM 2035 or Polystyrene and BRM 2065 or Glass filter NG4 and CHCl OVP for PhEur 2 2 40 Bruker Optik GmbH Setting up OVP for PhEur 2 2 40 2 2 Setting up OVP for PhEur 2 2 40 If you have already set up OVP for OQ and or PQ Performance Qualification you can skip this chapter Before you can use OVP for PhEur 2 2 40 you have to set up the corresponding PhEur 2 2 40 parameters and define the OVP test channels and OVP tests Select the OVP Setup command from the Validation menu to open the following dialog x A OVP Test Channel Setup AN OVP Test Setup Current Test Channel Es 7 Test Channel Configuration Source as Beamsplitter e 3 Y Measurement Channel PUE ev Detector EE Make sure the measurement channel is prepared for the LWN calibration before you start the measurement Instrument Configuration Y Accessory Z Title for new configuration m Load Image Add new configuratian Gear current Configuration Save and Exit Cancel Help Figure 1 Setup OVP Enter a title for the current configuration into the Title
18. CLE EEG su SUP SS So Dres 32 4 4 Purpose 25 04 grote amea Ves TAS eb DIM d ey Te ms VER SAT 32 4 5 HSP Requimemenis 2142 2 reae RERO C RN S RO ee 32 4 6 Spectra Comparison of SRM 2035 and Water Vapor 33 4 7 Reference for Water Vapor Absorbance 00000 c esee 36 4 8 Connes Advantage of Fourier Transform Interferometry 38 4 9 Conclusion fx Suse cv ba ln a SSO pol itera kite Prato ess Sate 38 iii PhEur 2 2 40 Tests 1 Introduction This manual describes the OPUS Validation Program OVP for spectrometer qualification according to the guidelines set forth by the European Pharmacopoeia 5 PhEur OVP for PhEur 2 2 40 is an integral part of the OPUS spectroscopic software The tests and test criteria intend to check the Bruker line of spectrometers and modules according to the PhEur regulations They are designed to follow the guidelines outlined in section 2 2 40 Near Infrared Spectrophotometry by the European Pharmacopoeia 5 The OQ Operational Qualification test protocol checks the instrument performance and compares this performance to the instrument specifications OQ tests should normally run after installation maintenance or major repair exchange of optical components which may influence the instrument performance on a regular yearly or semi yearly basis The PhEur 2 2 40 test protocol is intended to be run as part of the OQ test 1 4 PhEur 2 2 40 Tests e Photometric Lin
19. ard can be used If both tests are run a reference is only measured once Follow the wizard instructions and insert the standard using whatever method is appropriate for the instrument configuration you are using You will be prompted for each of the standards Note This may require specialized holders for the reference standard At the end of the test the final results will be computed 3 3 2 Transmission Measurement Prerequisites In case of transmission measurements the reference background measurement for the wavelength uncertainty test is run with the open channel Unless water vapor is used for this test either an external certified reference standard see table in chapter 2 1 or the internal refer ence standard BRM 2065 on the IVU with certificate is required for the sample measurement You will be prompted for the standard to be inserted only if an external reference standard has been selected Note This may require specialized holders for the reference standard If the internal BRM 2065 standard or water vapor has been selected the test will run without any further user interaction Bruker Optik GmbH OVP for PhEur 2 2 40 29 Run OVP Tests 3 4 Printing Reports The results of test measurements are stored in a report PDF format The test report contains a summarized test result page and subsequent pages for each test with all the test spectra displayed Reports are stored in the separate VALIDATION
20. ated after replacement of optical components or major repair NOTE In case of instruments without the internal NG11 glass filter you will be asked during the reference measurement to insert the external NG11 standard which is available at Bruker PhEur 5 2 2 40 Test Protocol E x TestSetup Photometric Noise A Wavelength Uncertainty Reproducibility Photometric Linearity Filter Settings 9400 00 cm 1 5000 00 cm 1 4200 00 cm 1 Open Channel Open 0 D n Filter 1 Filter NG11 0 Filter 2 Filter NG 4 0 Filter 3 Filter NGS 0 0 0 0 0 0 0 BERNER Measure Reference Spectra Last reference measured Not yet measured Reference Measurement required DK Cancel Apply Help _ Cancel e Figure 13 PhEur 2 2 40 Test Protocol Photometric Linearity tab A The Filter Setting column shows the filters used for testing The filters are automatically determined by the program B The values for the reference measurement are displayed in the table C Click on this button to measure the reference spectra D These lines show if and when the last reference has been measured In the latter case the date and time of the measurement is also displayed These lines also show whether a reference measurement is in progress 18 OVP for PhEur 2 2 40 Bruker Optik GmbH Transmission Measurement Mode The transmission values are retrieved from the spectra and filled in the grid Typical filter
21. e instrument configuration you are using You will be prompted for each of the standards Note The measurement requires specialized holders for the reference standards For each test High or Low Light Flux a reference and sample measurement are made using the reflectance standard At the end of the test the final results are computed 3 2 2 Transmission Measurement Prerequisites None The photometric noise test for transmission measurements is performed by using the open channel and a filter on the IVU The test itself runs fully automatically and needs no user interaction 28 OVP for PhEur 2 2 40 Bruker Optik GmbH Wavelength Uncertainty Reproducibility Test 3 3 Wavelength Uncertainty Reproducibility Test 3 3 4 Reflection Measurement Prerequisites The wavelength uncertainty and wavelength reproducibility test for reflection measurements require the use of either the 99 reflec tance standard SRS 99 010 or a gold standard for the reference background measurement Unless water vapor is used for these tests an external certified refer ence standard see table in chapter 2 1 is required for the sample measurement The reference measurement for these tests can be performed using the standard method used for your spectrometer and configuration e g gold standard for integrating sphere reference position for fiber optics solid probe etc Instead of the gold standard the 99 Labsphere Reference stand
22. e test options There is a separate page for each test selected Note that at least one test has to be selected 2 4 4 Photometric Linearity Test The photometric linearity test is performed using the open channel and three different glass filters which are mounted on the internal validation unit IVU of your spectrometer Currently no external certified transmission standards with known transmission values are available Similar to the reflectance measurements the evaluation uses three different frequencies over the measurement range The frequencies have been selected with respect to the filter material which does not provide a linear transmission Bruker Optik GmbH OVP for PhEur 2 2 40 17 Test Setup over the full range The open channel and three filters have to be measured to cover an as large as possible range of transmission values According to PhEur 2 2 40 the measurements are not possible to establish an absolute calibration for a given instrument However as long as the standards have the same physical description the same reference background is used and the target instrument measures each under identical settings the reproducibility of the photometric scale will be established over the range of standards used Subsequent measurements give information on long term stability To set up a photometric linearity test you have to measure reference values before you can run the test Reference measurements should only be repe
23. earity e Photometric Noise high light flux and low light flux e Wavelength Uncertainty Wavelength Reproducibility For additional information on the different testing methods refer to European Pharmacopoeia 5 section 2 2 40 For further general information on OVP refer to the OPUS Reference Manual Bruker Optik GmbH OVP for PhEur 2 2 40 1 Introduction 2 OVP for PhEur 2 2 40 Bruker Optik GmbH Reference Standards 2 Test Setup OVP PhEur 2 2 40 supports reflectance channels as well as transmittance channels Depending on the specified measurement channel OVP PhEur 2 2 40 detects the proper configuration automatically If you select a reflectance channel only the tests for reflectance measurements will be activated If you select a transmission channel only the test for the transmission measurement will be activated In case of fiber optic ports you can select between reflectance and transmission mode depending on the type of probe connected to the fiber port Once selected the mode cannot be changed later Depending on the spectrometer type and test mode additional external reference standards may be required The following table shows instrument types test modes and standards which are used for the different tests Before setting up the tests make sure that the required standards are available 2 4 Reference Standards Photometric Linearity Test Instrument Type Test Mode Internal Standard Exte
24. hotometric Linearity 10 11 17 27 Photometric Noise 13 19 28 R Reference Standards 3 Reflection Measurement 10 Report 26 Reports 30 Run Tests 25 T Test Setup 3 Transmission Measurement 17 U USP Requirements 32 W Water Vapor Absorbance 36 Wavelength 35 Wavelength Reproducibilit 16 Wavelength Reproducibility 4 23 Wavelength Uncertainty 4 14 20 29 31
25. icking on the status light and using the nstrument Status dialog For details on the letter case refer to the OPUS Reference Manual chapter 13 To start running the tests click on the Run OVP Tests command in the Validation menu The following dialog opens Run OVP Tests E xj OVP Run Tests MPA Sample Compartment with NIR Quartz TE InGaAs Internal IT1 Probenraum v IV PHEUR2240 OQ Test not yet run e Photometric Linearity Test High Flux Noise Test Low Flux Noise Test e Wavelength Uncertainty Test User Comment Print Report automatically IV Show Report automatically Run selected Tests Cancel Help Figure 18 Run OVP Tests Bruker Optik GmbH OVP for PhEur 2 2 40 25 Run OVP Tests The T n drop down list allows to select the appropriate IT test channel The lines below show the tests set up for the IT test channel selected as well as the test status Tests which have expired or which have not yet been performed are automatically activated for measurement Tests which interval has not yet expired are not activated and their remaining time is indicated as a reminder If a test has not expired but the interval has only e g 2 hours left you can activate the check box for that test and run the test earlier If a test has expired but you are not prepared to perform that test external standards required you can deactivate the check box for the corresponding test IV PHEUR
26. iffuse reflectance measurements Details on the reference values of the water vapor absorbance peaks are given below 2 Ref Reference values for the calibration of Bruker FT NIR spectrometers with reference to the water band at 7 306 74cm The data is obtained data source is from the HITRAN 1992 database published by Air Force Phillips Laboratory 29 Randolph Road Hanscom AFB MA 01731 3010 Dr Laurence Rothman PL GPOS 36 OVP for PhEur 2 2 40 Bruker Optik GmbH Reference for Water Vapor Absorbance M I wn cm 1 S E v v Q Q HO 1 7299 44900 1 300E 20 42 372 000 101 211 110 HO 7303 23140 6 889E 22 95 176 000 200 322 211 HO l 7305 08049 3 149E 22 326 625 000 200 606 515 HO 7306 73600 2 000E 20 79 496 000 101 313 212 HO 1 7306 74700 1 000E 21 325 348 000 200 616 505 HO l 7308 81782 6 179E 22 136 762 000 101 322 303 HO l 7310 34759 1 949E 22 326 625 000 101 514 515 HO l 7310 67785 5 959E 21 134 902 000 101 322 0221 HO l 7312 27100 7 400E 21 70 091 000 101 303 202 M Molecule I Isotope 1 lg 160 H wn Vacuum wavenumber fom S Intensity cm Molecule 2 cm at 296K E Energy ofthe lower state cm v Global Quantum numbers of the lower state v Global Quantum numbers of the upper state Q Local Quantum numbers of the upper state Q Local Quantum numbers of the lower state The reference band is the one with the largest intensity S row 4 The wavenumbe
27. interferometer the position of the mirror can be determined to an accuracy better than 0 005nm This means that the wavenumbers of an FT NIR spectrum can be determined with high accuracy 0 01cm In other words FT IR spectrometers have a built in wavenumber calibration of high precision This advantage is known as Connes advantage see 7 Due to the Connes advantage there is no distortion of the frequency in the spectrum and the x axis may be calibrated exactly by a single frequency Conclusion We believe that for Michelson type FT instruments e g Bruker MATRIX series Bruker VECTOR series Bomem BM160 series Nicolet Antaris series Perkin Elmer IdentiCheck series using water vapor for the wavelength uncertainty test is the most optimal solution available for both diffuse reflection and transmission measurements Due to the Connes advantage only a single absorption peak is required for the test The water vapor absorbance bands are very sharp and allow determination of the position to a very high accuracy For a Bruker MATRIX spectrometer for example the wavelength uncertainty test is specified with a maximum deviation of 0 1cmr A higher deviation would be regarded as failing the test This limit is much tighter than the requirements by USP tolerances of 4cm 38 OVP for PhEur 2 2 40 Bruker Optik GmbH Index C Connes Advantage 38 H High Flux Noise 4 I IVU 27 L Low Flux Noise 4 P P
28. ion of 4cm l PhEur 5 2 2 40 Test Protocol E x TestSetup Photometric Linearity Photometric Noise Wavelength Uncertainty Reproducibility Select Standard Use extemal certified Reference Standard Reflection C Use Water Vapor a gt Booo ge Standard used SAM 1920a c IEE Use Band close to 7923 00 5943 00 5073 00 De Certified Values cm 1 E BE 2 Input in wavenumbers C Input in nm Cancel Apply Help Figure 11 PhEur 2 2 40 Test Protocol Wavelength Uncertainty test A Select the standard to be used for the test When using water vapor B to E will not be visible B Select the standard to be used from the drop down list C This line shows the recommended frequencies to be used for evaluation Select bands from the certificate which are close to these frequencies D The three entry fields allow to enter the bands as provided in the Certificate of Analysis E Depending on the standard the frequencies in the certificate can be listed in nanometers or wavenumbers Thus the values can either be entered in nanometers or as wavenumbers Select the required units by activating the respective option button Bruker Optik GmbH OVP for PhEur 2 2 40 15 Test Setup 2 3 4 Wavelength Reproducibility Test This test uses the parameters settings and standards as specified for the wavelength uncertainty test except that only a single band is used for evaluation
29. load dialog opens Load the calibration data file which allows to read the certificate values from a text file which is normally delivered with the set provided the set was purchased from Bruker Table F and the drop down lists B and C correlate to the file data B Enter the report number to identify a set of standards The report number is listed in the certificate C Enter the date of calibration to identify a set of standards The date of calibration is listed in the certificate If you click on the arrow key a small calendar view pops up D Select the number of standards to be measured for the test excluding the 99 reference standard E Depending on the number of standard selected the table displays only those columns for which an entry is required F You have to enter both the values for the three specified frequencies and two values left and two values right from these frequencies G Activate this check box if a stray light correction has to be done prior to the evaluation of test spectra If you measure by using an integrating sphere it is essential to use the stray light correction for this test For details about the stray light correction and how to record the correction spectra refer to the OPUS Reference Manual Some hints for data entry We highly recommend to use a text file for data input If such a file has not been supplied generate such a file For details see chapter 4 Spectralon Standards Report Number 41666
30. nel will automatically be displayed C In general the instrument configuration is automatically displayed as soon as you have selected all components D Depending on the test channel the drop down list contains appropriate accessories E Depending on the measurement channel selected a configuration specific bitmap will be displayed F Use the Load Image button to load further instrument images available in OPUS The bitmaps are stored in the OPUS VALIDATION Bitmaps directory Select the Thumbnail option from the pop up menu when clicking on the EHr button to be able to see at once which bitmap belongs to which file name For details on the bitmaps refer to the OPUS Reference Manual chapter 13 You can also make your own photo with a size of 90 x 90 and store it into the bitmap directory using the Tnn bmp file name nn is a consecutive number 6 OVP for PhEur 2 2 40 Bruker Optik GmbH Setting up OVP for PhEur 2 2 40 G To delete the current configuration click on this button Once deleted the settings cannot be reloaded If you have accidentally deleted a channel you have to repeat the complete setup again OVP configurations are stored in the OPUS VALIDATION Data base lt Instrument gt directory H To save the configuration click on the Save and Exit button I Click on this button to interrupt the setup without saving Setup O P i X A OVP Test Channel Setup IN OVP Test Setup Current Test Channel
31. nter any data into the entry fields Additionally a temperature control of the band position is automatically performed in the subsequent test 22 OVP for PhEur 2 2 40 Bruker Optik GmbH Transmission Measurement Mode 2 4 4 Wavelength Reproducibility Test This test uses the same parameters settings and standards as specified for the wavelength uncertainty test If a reference standard is selected for the wavelength reproducibility test the frequency specified in the first entry field is used D in figure 17 A reference measurement is only required if the wavelength uncertainty test had not been run before Ten sample measurements are performed and the band location of the specified band is evaluated for all ten spectra Based on the band location of these 10 single measurements the average is calculated The maximum deviation determined from this average The deviation must not exceed a specified limit which depends on the type of standard used The table below shows the evaluated band and maximum deviation of a few standards Standard Band used cm Maximum Deviation cm Water vapor 7306 736 0 05 NIST SRM 2036 10245 0 1 Ch5Cl 6064 0 1 Bruker Optik GmbH OVP for PhEur 2 2 40 23 Test Setup 24 OVP for PhEur 2 2 40 Bruker Optik GmbH Run OVP Tests There are two possibilities to run OVP tests Either by selecting the Run OVP Tests command in the Validation menu or by cl
32. on measures a water vapor peak using the standard peak picking algorithm B Two water bands are suited for this test Select either the band at 7306 736cm recommended or the band at 7299 449cm External standards like NIST SRM 2065 SRM 2035 or CH Cl can be purchased and used as well Bruker offers a traceable BRM 2065 reference standard which is mounted on the IVU and which allows to run all tests fully automatically A certificate for this standard is available Note For instruments without the internal BRM 2065 an external transmission standard BRM 2065 or SRM 2065 is required if you want to use a standard This standard is available from Bruker First a background measurement is performed Then the standard is measured The specific frequency peaks for the reflectance standards are measured with their values determined using the center of gravity algorithm This test also provides information for long term system stability The band frequencies are listed in the Certificate of Analysis provided with the reference standard Make sure that you select the frequency values from the column with the specified resolution of 4cm Recommended band frequencies vary for different standards and are shown on the Wavelength Uncertainty page Bruker Optik GmbH OVP for PhEur 2 2 40 21 Test Setup Thus before entering the reference values from the certificate make sure the proper reference standard has been selected from the standa
33. pplied by NIST 15000 14000 13000 12000 11000 10000 8000 8000 7000 8000 5000 Figure 20 SRM 2035 spectrum transmission wavelength standard mixture of rare earth oxides A resolution 2em 0 150 10450 10425 10400 10375 10350 10325 10300 10275 10250 10225 10200 10175 10150 10125 10100 10075 10050 10025 Figure 21 The sharpest absorption band in the SRM 2035 spectrum 34 OVP for PhEur 2 2 40 Bruker Optik GmbH Spectra Comparison of SRM 2035 and Water Vapor 0 500 0 450 0 350 0 300 SRM 2035 0 200 0 250 0 150 AA NUN ak Water vapor T T T T T T T T T T T T T T T 1 7600 7400 7200 7000 6800 6600 6400 6200 8000 5800 5600 5400 5200 5000 4800 4800 Figure 22 Comparing SRM 2035 and water vapor at a resolution of 2cm The measurement of water vapor can be used to check the wavelength accuracy for Michelson type FT instruments The water vapor absorbance peak at e g 7306 74cm measured with a high resolution can be applied Water vapor has the advantage of having an extremely narrow band and the wavelength position can be measured to a very high degree of accuracy This gives a more precise measurement of the wavelength accuracy than would be in case of NIST SRM 2035 standard see figure 22 The NIST SRM 2035 standard itself is calibrated against the water vapor band see 3 In addition using only one point e g 7306 74cmr
34. r is usually regarded as a constant as it is independent of the refractive index of the surrounding medium A Fourier Transform Spectrometer FTS however measures wavelengths and thus depends on the refractive index of the medium The wavenumber 1 2 is calculated from the wavelength by FFT Fast Fourier Transformation As the refractive index of the air is subject to a dispersion at 15800cm it is higher than at 7300cm the wavenumber range becomes distorted in a non linear way the effect however is extremely small Therefore it is possible to exactly calibrate an FTS under standard pressure only over a small range The spectra which are calibrated in this way are indicated in vacuum wavenumbers When converting vacuum wavenumbers into wavelengths you have to divide by the refractive index of the air This index amounts to 1 0002735 for dry standard atmosphere at 7300cm Bruker Optik GmbH OVP for PhEur 2 2 40 37 Appendix Wavelength Uncertainty Test using Water Vapor 4 8 4 9 Connes Advantage of Fourier Transform Interferometry The fact that only one point e g 7306 74cm for water vapor is required for the wavelength accuracy test is due to the Connes advantage of the Fourier Transform Infrared technique see 4 to 8 In an FT spectrum the accuracy of each wavenumber is coupled to the accuracy with which the position of the moving mirror is determined by using an additional HeNe laser
35. rds drop down list PhEur 5 2 2 40 Test Protocol amp xi TestSetup Photometric Noise Wavelength Uncertainty Reproducibility Photometric Linearity Select Standard Use Internal Reference Standard BRM 2065 Use extemal certified Reference Standard Transmission C Use Water Vapor B oi Standard used SAM 2035 c BEL S Use Band close to 10245 00 8173 00 6806 00 D j Cette Values cm 1 E eee Input in wavenumbers C Input in nm Cancel Apply Help Figure 17 PhEur 2 2 40 Test Protocol Wavelength Uncertainty test A Select the standard to be used for the test When selecting the internal or external reference standard using water vapor B to E will not be visible B Select the standard to be used from the drop down list C This line shows the recommended peaks to be used for evaluation First select the standard as described in A D Three entry fields are provided to enter the peak frequencies as provided in the Certificate of Analysis E Depending on the standard the frequencies in the certificate can be listed in nanometers or wavenumbers The values can thus either be entered in nanometers or as wavenumbers Select the required units by activating the respective option button If you use an internal standard and in case of instruments previously designed the standard data are read from the instrument and entered automatically In this case you cannot e
36. reference position e g Sphere Background for the MPA In this case the Measurement Channel drop down list allows selecting the channel which shall be used for the linearity measurements To perform all four tests make sure that all test options are selected There is a separate page for each test selected Note that at least one test has to be selected 2 3 1 Photometric Linearity Test The photometric linearity test is performed using a set of reflectance standards of known relative reflectance This test has been optimized for use with the Labsphere brand of NIR reflectance standards 10 OVP for PhEur 2 2 40 Bruker Optik GmbH Reflection Measurement Mode According to PhEur 2 2 40 the spectra obtained from reflectance standards are subject to variability due to the difference between the experiment conditions under which they are factory calibrated and those under which they are subsequently used Hence the percent reflectance values supplied with the calibration certificate may not be useful to establish an absolute calibration for a given instrument However as long as the standards have the same physical description the same reference background is used and the target instrument measures each under identical settings the reproducibility of the photometric scale will be established over the range of standards used Subsequent measurements give information on long term stability The photometric linearity test requires
37. rnal Standard MPA Reflection None Gold Standard for stray MATRIX light correction spectra VECTOR 22 N only Labsphere Standard Set with 99 Reference 80 40 20 10 optional 5 MPA with BRM 2065 Transmission Filter NG4 None and Glass filters Filter NG9 NGA NG9 and NG11 Filter NG11 MPA MATRIX Transmission Filter NG4 Filter NG11 VECTOR 22 N with Filter NG9 Polystyrene and Glass filter NG4 and NG9 Bruker Optik GmbH OVP for PhEur 2 2 40 3 Test Setup High Flux and Low Flux Noise Test Polystyrene and Glass filter NG4 and NG9 Instrument Type Test Mode Internal Standard External Standard MPA Reflection None Labsphere Standards MATRIX 99 and 10 VECTOR 22 N MPA with BRM 2065 Transmission Filter NG9 None and Glass filters NG4 NG9 and NG11 MPA MATRIX Transmission Filter NG9 None VECTOR 22 N with Wavelength Uncertainty and Wavelength Reproducibility Test Note This test requires only a single standard if standards are listed in both the internal and external standard column you can either use the internal or external standard Alternatively you can use water vapor instead of reference standards for both reflection and transmission mode Details are given in attachment 1 NG9 Instrument Type Test Mode Internal Standard External Standard MPA Reflection None Gold Standard or Lab MATRIX sphere
38. s test PhEur 5 2 2 40 Test Protocol E x TestSetup Photometric Noise Wavelength Uncertainty Reproducibility Select Standard C Use extemal certified Reference Standard Reflection Recommended Water Band 7306 736 cm 1 Use Water Band at 7306 736 Ub 736 7299 449 OK Cancel Apply Help ok Figure 10 PhEur 2 2 40 Test Protocol Wavelength Uncertainty test A Activating the Use Water Vapor option button measures a water vapor peak using the standard peak picking algorithm B According to PhEur 2 2 40 two water bands are suited for this test Select either the band at 7306 736cm recommended or the band at 7299 449cem The alternative method requires the use of a certified reference standard like NIST 1920a NIST SRM 2065 KTA 1920x or CHCl TiO suspension A standard background measurement is performed and then the standard is measured The specific peaks for the reflectance standards are measured with their values determined using the center of gravity algorithm This test also provides information for long term system stability 14 OVP for PhEur 2 2 40 Bruker Optik GmbH Reflection Measurement Mode The band frequencies are listed in the Certificate of Analysis provided with the reference standard Some certificates list frequencies for a different resolution Make sure that you choose the frequency values from the column with the specified resolut
39. specifying appropriate independent external wavelength standards For the reflectance mode the NIST SRM 1920a reflectance standard is preferred Standards containing dysprosium or holmium oxide are available The nature and type of 32 OVP for PhEur 2 2 40 Bruker Optik GmbH Spectra Comparison of SRM 2035 and Water Vapor background reference standard must also be specified In transmittance measurements the corresponding rare earth solution or glass standards can be used Solid or sealed solutions can be maintained similarly to a set of calibration weights to provide information on long term stability Table 1 Recommended Near Infrared Instrument specifications SRM 1920a peaks occur at 1261 1681 and 1935nm Wavelength Uncertainty Tolerances 1nm at 1200nm or 8cm at 8300cm 1nm at 1600nm or 4cm at 6250cm 1 5nm at 2000nm or Hem at 5000cm a A maximum nominal instrument resolution of 10nm at 2500nm or 16cm at 4000cm is appropriate for most applications b The nominal 1935nm peak depends on the instrument resolution Use the wavelength value from the SRM 1920a certificate which comes close to the resolution used 4 6 Spectra Comparison of SRM 2035 and Water Vapor The NIST SRM 2035 transmittance standard is recommended by USP to be used to determine the wavelength accuracy for transmission measurements Using the Center of Gravity COG of the absorbance peaks instead of the peak maximum
40. xpiration time for the test is properly defined in the OQ line Type the interval period into the entry field and select the units from the drop down list Available units are hours days or months Click on the Setup button to open the PAEur 2 2 40 Test Protocol dialog If all tests have been set up and you click on the OK button the setup status is indicated by a green check mark IV Run PHEUR 2240 o 00 Test Setup Bruker Optik GmbH OVP for PhEur 2 2 40 9 Test Setup 2 3 Reflection Measurement Mode PhEur 5 2 2 40 Test Protocol i x Photometric Noise Wavelength Uncertainty Reproducibility TestSetup Photometric Linearity European Pharmacopoeia 5 Section 2 2 40 Reflection Measurement C Transmission Measurement Measurement Channel Sphere Macrosample M m Test Selection Last Test Date Time IV Photometric Linearity v Photometric Noise Testnotyetun IV Wavelength Uncertainty IV Wavelength Reproducibility Cancel Apply Help Figure 6 PhEur 2 2 40 Test Protocol TestSetup for reflection First define the correct type of measurement i e either reflection or transmission Activate the corresponding option button Figure 6 shows the setup dialog for reflection measurement Initially all tests are selected in the Test Selection group field When using a configuration with an integrating sphere the test channel for OVP will normally be set up with the internal
Download Pdf Manuals
Related Search