Foss XDS OptiProbe Manual Download Page 95

 

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93 

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Index 

Accessory Kit ............................................... 21 
Bias ............................................................. 58 
CFR 21 .................................. 7, 37, 81, 82, 83 
Crossover Cable ............................................ 8 
Data Collection Method .................. 27, 29, 40 
Depth............................................................ 9 
Diagnostics  42, 43, 44, 46, 53, 55, 56, 58, 62, 

66, 67, 79 

Dimensions ................................................... 9 
Direct Connection ... 10, 15, 16, 19, 20, 23, 24 
Electrical Power ............................................. 8 
Fan Filter ..................................................... 70 
Firewall ................................................. 12, 19 
Fuse Replacement ....................................... 77 
Gain Adjust ........................................... 66, 67 
Gain Factor ................................................. 67 
Hardware Validation ................................... 81 
Height ........................................................... 9 
Humidity ....................................................... 8 
HVAC ............................................................ 8 
Input ..................................................... 14, 88 
Installation Qualification ........................ 82, 83 
Instrument Calibration .... 3, 28, 31, 42, 43, 44, 

49, 50, 52, 59, 61, 62, 77, 90, 91 

Instrument Diagnostics ................................ 42 
Interactance Immersion . 26, 29, 30, 31, 40, 50 
Interactance Reflectance  3, 26, 27, 30, 36, 40, 

50, 67, 89, 90 

IP Address ....................................... 15, 18, 39 
IPV Setup ............................ 53, 55, 62, 63, 65 
Lamp ................................ 3, 7, 21, 72, 77, 88 
Low Flux Test ........................................ 67, 68 
Maintenance ................................... 70, 79, 80 
Method ................................................. 32, 42 
Module ............................... 21, 24, 26, 40, 46 
Monochromator .......................................... 21 

Network Connection ............................... 3, 10 
NIRStandards ........................................ 82, 83 
Noise .............................................. 56, 57, 58 
Operating Qualification ......................... 82, 83 
Options ................................. 3, 31, 38, 42, 53 
Password ........................................ 14, 37, 84 
Performance Test 8, 28, 31, 35, 42, 56, 57, 58, 

62, 67, 72, 77, 82, 89 

Photometric Test ............. 3, 53, 55, 62, 63, 66 
Power Switch .............................................. 91 
Project ............................................ 31, 38, 42 
Q9000 ........................................................ 81 
Reference3, 29, 31, 36, 40, 42, 43, 46, 47, 48, 

49, 53, 54, 56, 63, 64, 66, 77, 90, 91 

Reflectance Standards ................................. 68 
RJ-45 ..................... 7, 8, 23, 24, 25, 37, 79, 88 
Safety ........................................ 21, 31, 86, 92 
Software . 7, 21, 22, 25, 37, 42, 81, 82, 83, 91 
Spacers ....................................................... 30 
Standardization .. 3, 29, 31, 36, 42, 43, 46, 47, 

49, 53, 66, 77, 90, 91 

Temperature ..................................... 8, 53, 89 
Troubleshooting .................... 3, 15, 16, 19, 87 
User Application .......................................... 81 
User ID ...................................... 11, 14, 37, 84 
Validation.................................... 3, 81, 83, 84 
Vibration ....................................................... 8 
Wavelength Certification 3, 52, 53, 58, 61, 62, 

82 

Wavelength Linearization 3, 28, 31, 43, 44, 45, 

51, 89 

Wavelength Standard .... 29, 51, 52, 53, 89, 90 
Weight .......................................................... 9 
Width ............................................................ 9 
Window ................................................ 42, 65 
Windows Operating Systems ....................... 10 

 

Summary of Contents for XDS OptiProbe

Page 1: ...NIRS XDS Interactance OptiProbe Analyzer Manual 8 921 8006EN ...

Page 2: ......

Page 3: ...Metrohm AG CH 9100 Herisau Switzerland Phone 41 71 353 85 85 Fax 41 71 353 89 01 info metrohm com www metrohm com NIRS XDS Interactance OptiProbe Analyzer Manual 8 921 8006EN 03 2013 fpe ...

Page 4: ...mentation is protected by copyright All rights reserved Although all the information given in this documentation has been checked with great care errors cannot be entirely excluded Should you notice any mistakes please send us your comments using the address given above ...

Page 5: ...8 Added notes about possible failure of Photometric Test and corrective action Corrected wrong instruction in Gain Test Reflectance probe is normally used in Gain Changed photo in Lamp Replacement now showing arrow on lamp Corrected reference to Lamp Replacement in Troubleshooting to section 8 3 Updated Vision opening screen removed copyright date for publication Updated Configure Options screen a...

Page 6: ...lems 15 3 2 7 Network Troubleshooting Overview 16 3 2 8 Direct Connection Troubleshooting Overview 19 4 Assembly of the Instrument 21 5 OptiProbe Module 26 5 1 Interactance Reflectance Configuration 27 5 2 Interactance Immersion Configuration 29 5 2 1 Cleaning the Probe End 32 5 3 Cleaning of internal reflectance reference 32 6 Vision Software Connection to the Instrument 37 7 Instrument Diagnosti...

Page 7: ...trument Performance Verification 82 9 1 4 Instrument Performance Certification 82 9 1 5 Metrohm Master Instrument Program 83 9 2 Software Validation Tools 83 9 2 1 Installation and Operating Qualification Documents 83 9 2 2 Vision Certificate of Validation 83 9 2 3 Vision Validation Document Package 83 9 2 4 21 CFR Part 11 Compliance 84 10 Safety and Electrical Certification 86 11 Troubleshooting ...

Page 8: ...that might influence performance The XDS uses various patented algorithms to provide superior accuracy and transferability between like instruments This instrument uses near infrared NIR spectral energy to illuminate the sample By measuring the energy reflected off or passing through the sample chemical information and composition may be determined This information may be used for quantification o...

Page 9: ...ngths beyond 2000 nm These additional wavelengths have been independently measured on calibrated instrumentation to ascertain the wavelength positions used Instrument communication is through RJ 45 network connections which eliminates issues involved with long runs of RS 232 cable An Internet Protocol IP address is dynamically requested upon connection This address may be permanently installed if ...

Page 10: ...If dust has accumulated on the fans carefully wipe them clean with a moist soft cloth Do not distort or damage the fan blades or fins as this will impede cooling Do not place the instrument directly near any HVAC duct The direct flow of heating or cooling air will cause the instrument to exhibit high noise during the Performance Test 2 3 Electrical Power Power should be a single separate stable tr...

Page 11: ...trument Dimensions and Weight XDS OptiProbe Analyzer dimensions are Width 18 0 457 mm Leave about 6 152mm on the right side for access to standards door Height 15 0 381 mm Height with Probe 17 5 445mm Depth 22 5 572 mm front to back Depth with Probe 32 812mm Leave a minimum of 3 76mm around the back and left side for airflow and access space Leave at least 6 152mm on the right side and in front fo...

Page 12: ...annot be responsible for software and instrument problems resulting from the use of two network cards in the host computer This information is correct as of the time of original publication Changes to computers operating systems and network protocols may require revision of this information without notice 3 1 Network Connection connected to an active network port as shown This is the preferred met...

Page 13: ... may result in lost commands lost data and unsatisfactory software operation Metrohm cannot be responsible for software and instrument problems resulting from the use of two network cards in the host computer For IT personnel it may be helpful to understand the sequence of events used by the XDS instrument and Vision software when establishing an electronic connection These are explained 3 2 1 Ove...

Page 14: ...local free standing communication only In such cases a crossover cable or a hub with two patch cables should be used to connect the computer and the XDS instrument 5 Upon the next power down and subsequent power up of the XDS instrument it will again request an IP address of the DHCP server It will go through the same cycle eventually reverting to the stored default IP address This is intentional ...

Page 15: ...es we recommend minimal tampering with computer settings This can cause instability and may be prohibited by company policies At this time we recommend Microsoft Windows XP as the easiest operating system by which to establish network communication We strongly recommend that Windows 95 98 and NT 4 0 be avoided as they require considerable expertise in network configuration 3 2 4 Quick Glossary of ...

Page 16: ...d reduce packet collisions within the network To accomplish subnetting Subnet Masks may be applied to separate one section of the network from another A subnet mask typically takes the form 255 255 255 0 or something similar This scheme is becoming obsolete as new network management methods are being implemented TCP IP Transmission Control Protocol Internet Protocol is the basic communication lang...

Page 17: ...with the XDS Serial number The instrument is shown as Available on port 2083 Highlight the instrument and click OK 4 If the IP Address field is empty the user should consult Troubleshooting Connection Problems 3 2 6 Troubleshooting Connection Problems Many connection problems are easily solved especially with Windows XP operating systems Windows XP is currently the preferred operating system and h...

Page 18: ...t back up Wait 120 seconds for the XDS instrument to fully reset its communication If an instrument is shown proceed to Acquire Connect in Vision If this does not resolve the problem continue to the next section 3 2 7 Network Troubleshooting Overview If no XDS instrument shows as available there may be a setting which should be changed It may be necessary to contact your IT department for assistan...

Page 19: ...orward to Internet Protocol TCP IP Properties is shown Verify these settings Obtain an IP address automatically Obtain DNS server address automatically When finished click OK Close all other boxes opened for this verification If the settings were not set properly it may be necessary to exit Windows XP then re enter XP to have the correct settings take effect If in doubt do this and try XDS instrum...

Page 20: ...d it may be necessary to verify that the XDS instrument is installed within the IP address range of the computer Network Solution 3 Verify network has full IPv4 compatibility Some networks have moved to Ipv6 Internet Protocol version 6 which uses different address formats The IT department at your company can verify if the network offers full Ipv4 compatibility If the network has migrated to Ipv6 ...

Page 21: ...sets the communication port and allows Vision to find the instrument if connected properly Network Retry Windows 2000 Windows 2000 users should click on Retry Reset This command resets the communication port and also resets Windows 2000 to the proper state to connect using a dynamic IP address in the XDS instrument 3 2 8 Direct Connection Troubleshooting Overview If no XDS instrument shows as avai...

Page 22: ...ulator gives the allowable computer IP address range as 169 254 0 1 through 169 254 2 254 DO NOT use 169 254 0 2 in the computer Set the computer IP address to either 169 254 0 1 or 169 254 0 3 Direct Connection Solution 2 Power down the XDS Instrument then power it back up Wait 120 seconds for the instrument to determine the correct method of Ethernet communication Please do not click anything fo...

Page 23: ...sion Spectral Analysis Software Spare Lamp in Accessory Kit Accessory Kit containing cords cables and other required items Safety Manual for CE certification Instrument Test Results Packet Note Packaging may vary from that shown The serial number of the instrument and module are located on serial plates on the left side when facing the instrument These serial numbers should match the serial number...

Page 24: ...nel opens to about a 45 degree angle for access to connectors and for filter inspection Avoid scratches or damage 4 Gently thread the AC power cable and network cable through the lower right corner of the instrument access area as shown The cables should snap into the black holder The innermost position is large to fit the power cord If the power cord is in the wrong location the door may not clos...

Page 25: ... it is a UTP crossover cable and will not work with a network Use a network cable as described in section 3 0 7 Close the outer cover of the instrument Push gently to the final closed position It should latch securely 8 Position the sampling module directly in front of the monochromator This photo shows the mating connection plates prior to final alignment and assembly The locating pins help find ...

Page 26: ...t Carefully wind the fiber bundle clockwise around the saddle The 2 meter probe shown takes one wrap The 3 meter probe takes 2 wraps The final assembly is as shown 11 Plug the AC power cord into a grounded AC outlet A surge protector or Uninterruptible Power Supply UPS is recommended for best operation 12 For Direct Connection the gray cable from the instrument plugs directly to the computer netwo...

Page 27: ...ve assembly is finished turn on the power switch on the monochromator It is located on the lower surface on the right hand side as shown The monochromator performs some initialization tests which take a moment Some noises will be heard as items find their initial positions This is normal 15 Prepare to establish communication from Vision to the XDS instrument This is detailed in Section 6 0 Vision ...

Page 28: ...5 2 Always be sure the barrel is screwed down fully before sampling The black O Ring should not be visible when fully assembled Failure to tighten the probe barrel will cause the instrument to fail diagnostic tests and will cause spectral distortion The fiber optic bundle while well protected should always be handled with care The individual fibers are quite thin and can be broken by rough handlin...

Page 29: ...elect the proper Tip type in the Data Collection Method DCM in Vision See section 6 0 for full information The reference scan is taken with the Interactance Reflectance Tip located in the uppermost aperture on the front of the instrument as shown Position the probe fully into the aperture Click on the reference icon in Vision With the Interactance Reflectance probe barrel mounted the operator may ...

Page 30: ...t or material carried on the probe barrel may soil or damage the instrument reference This should be avoided When finished sampling the probe should be stored in the reference position This is the proper position for Performance Test Gain Test and Wavelength Linearization Instrument Calibration makes use of an external wavelength reference The reference mounts in a cup holder on the side of the in...

Page 31: ...door and the holder will open Pull as far as it will come out then insert the cup window side toward the probe Close door and insert the probe into the middle aperture against the sample cup 5 2 Interactance Immersion Configuration This is the Interactance Immersion Liquid Tip used to sampling liquids such as alcohols and other clear to semi clear liquids The path length of the tip is set by use o...

Page 32: ...reference scan is taken with the Interactance Immersion Tip located in the lowest aperture on the front of the instrument as shown Click on the reference icon in Vision Position the probe fully into the aperture to block external sources of light When placing the Interactance Immersion Liquid Tip into the sample angle it slightly to avoid trapped bubbles between the mirror end and the sample windo...

Page 33: ... in the Reflectance mode After mounting the Interactance Immersion tip run Wavelength Linearization if Auto Linearization is selected under Project Options Always follow these guidelines when handling sample materials 1 Always use appropriate safety equipment with hazardous materials to prevent injury This equipment may include safety glasses gloves lab apron and fume hood Always check the MSDS Ma...

Page 34: ...e and dry Pharmaceutical applications may require a Cleaning validation which describes each step of the cleaning process solvents to be used and specific verification tests to determine whether cleanliness levels have been reached Because a cleaning validation is sample specific Metrohm cannot recommend detailed cleaning methods for such samples The OptiProbe is shown here sampling a liquid in a ...

Page 35: ...he internal reflectance reference follow these steps 1 Remove the OptiProbe from the reference position and place it in a secure place where it will not fall or be damaged 2 Lift the release handle then remove the OptiProbe module from the monochromator 3 Gently lift the module onto its left side with the blue housing upward 4 Gently pry the large black cap off the back of the module as shown 5 Li...

Page 36: ...d the screwdriver blade horizontal as shown to lift the threaded plug out of the unit 7 Remove the plug 8 The white object inside the opening is the reflectance standard 9 Reach in with a tissue then press the reflectance standard out from the other side insert the OptiProbe gently into the reference position The standard should pop out into the tissue 10 Gently wipe the surface with a laboratory ...

Page 37: ... 12 When the reflectance standard is clean re insert it into the instrument opening Handle by the edges to avoid deposition of oils onto the surface 13 Re install the threaded plug and snug down 14 Slide the sample drawer back to the normal position 15 Install the OptiProbe module back onto the monochromator and tighten the release handle 16 Place the OptiProbe into the reference position 17 Warm ...

Page 38: ...rotective case between uses Avoid any introduction of dirt or contaminants into the surface of the Reference Standard Dirt and sample carryover will change the optical characteristics of the standard which will then affect how the instrument reads samples The quality of the instrument spectra depend upon proper Reference Standardization This Reference Standard has been calibrated on a Master OptiP...

Page 39: ...pears on the opening screen Enter the default User ID NIRS It is not case sensitive Tab or mouse to the Password box and enter the default password NIRS Note that you should set up specific User ID and passwords for each authorized user Do not operate on the default User ID or you may be in violation of CFR 21 Part 11 To begin a new project must be created The project is used to store data and cal...

Page 40: ...Be sure the instrument is turned on and is ready Click on Use Existing Data to postpone instrument connection The Project Options must be verified before connecting Click on Configure Options to set Project Options Project Options should be set as shown If they are not this way click on the checkbox to select or de select as needed When the Project Options are as shown click on OK ...

Page 41: ...iver Highlight NIRSystems XDS series Instrument Driver and click on Configure This box allows the user to select the instrument by serial number The IP Internet Protocol address is also shown Use the drop down arrow of the IP Address box and select the correct instrument The instrument must show Available Port 2083 to be selected Click OK to exit the dialog box ...

Page 42: ... enter a logical name for the DCM such as that shown above Use the default of 32 scans for Sample and 32 scans for Reference The instrument scans on each forward swing and each backward swing of the grating unlike previous Metrohm instruments Thus 32 scans are accomplished on only 16 grating cycles and are very rapid Click OK when finished The user will hear a slight ticking sound from the interna...

Page 43: ...Communication LED is lit on the instrument Upon connection Vision will prompt for the instrument configuration This is used to establish a Diagnostic Database It is important that the instrument be correctly identified to prevent corruption of the database If only one instrument is in use accept the information and click OK ...

Page 44: ...ta acquisition This prevents the user from taking data on a non functional instrument Run performance test after wavelength linearization Forces user to run test sequentially This is not necessary with XDS Use Auto Linearization Maintains correct wavelength registration automatically using internal wavelength materials to keep instrument in precise adjustment over time Reference Standardization Us...

Page 45: ... the same configuration The correction programs are accessed from the Diagnostics menu bar shown at right The diagnostic steps are explained in the sections that follow 7 1 1 Wavelength Linearization Wavelength Linearization uses an internal wavelength standard set to determine a set of internal arbitrary peak positions that the instrument will use to maintain repeatability of wavelength response ...

Page 46: ...t meant to be traceable as the wavelength calibration of the instrument is done on an external standard traceable to NIST The internal wavelength materials are used to maintain the wavelength registration of the instrument This is done by software Final tighter adjustments are later performed in Instrument Calibration Select Wavelength Linearization from the Diagnostics menu The instrument will sc...

Page 47: ...s finished with this screen a result screen will be displayed A typical result screen is shown Peak positions for the reference materials are located using a peak finding algorithm These found peaks are compared to the nominals Differences should be no more than 0 4nm for any peak Click Yes to send the linearization to the instrument After the linearization is successfully sent to the instrument t...

Page 48: ...00 reflectance This assures that bright samples do not saturate the instrument or produce negative absorbance values Vision software stores the Reflectance Standard file which is downloaded to the instrument and is applied as a correction to each spectrum Follow these steps to create a reference standard Select Diagnostics Reference Standard Create Reference Standard When Vision first communicates...

Page 49: ...ference Standardization with a standard from the XC 1010 set The XDS OptiProbe must be calibrated with the XC 1200 only Vision prompts the user to rotate the Certified 99 Reflectance Reference This is done to minimize the directional effects of the standard and provide best consistency Note the label on the standard and rotate 90 degrees at each prompt A total of four positions will be used Vision...

Page 50: ...ment reference as shown Click OK to plot a spectrum of the Certified Reflectance Reference The Certified 99 Reflectance Reference is shown with the spectrum of the instrument reference Click OK to plot a correction spectrum The correction spectrum represents the amount of spectral correction required to provide a virtual 100 reflectance reference at each data point ...

Page 51: ...tra taken with a DCM where Reference Standardization is checked Note that cleanliness of the probe window is very important when this program is run If the window is not extremely clean the character of the window contamination will be imparted to the reference correction Therefore maintain a clean window at all times If a Reference Standardization does not exist for the selected configuration Vis...

Page 52: ...nt to those of the standard These wavelength positions are applied at the sample plane where samples are measured or read These adjustments are saved and are applied on each subsequent scan of the instrument yielding a correct spectrum This adjustment is performed in reflectance using the Interactance Reflectance Probe tip Once done this calibration applies to Interactance Reflectance and Interact...

Page 53: ...ent Insert the WSR10xxx Wavelength Standard Cell when prompted Insert the cell in a consistent rotational position for repeatability The probe must be in the center position as shown and the WSR standard must be in the drawer on the side of the instrument Close the drawer first then gently lower the OptiProbe into light contact with the standard window The drawer is shown open for illustration pur...

Page 54: ... at above 2200nm These additional peaks are used to set the wavelength scale of the instrument to aid in instrument matching This is one important step in calibration transfer The Foss WSR Wavelength Standard exhibits slightly different absorbance and baseline levels due to the reflectivity of the added ingredient The peaks however are in the same wavelength positions and are similar in shape to S...

Page 55: ...but a V is placed into the fourth character of the file name This indicates that it is a verification file For example if the standards set has the serial number RSS10301 the IPV Setup file is named RSSV10301 With the IPV Setup file stored the user can run Photometric Test to check the repeatability of instrument performance This is detailed later in this manual in Evaluation Diagnostics Photometr...

Page 56: ...is used where it aids in file transfer For Number of Replicates enter 4 Because the OptiProbe has a small sampling window the replicates assure better consistency Click on OK Vision will begin to take an instrument reference scan if the instrument is operating in Reference Standardized mode The red progress bar at the bottom of the screen indicates status If operating in Reference Standardized mod...

Page 57: ...els on the back identify each standard Note the mini CD that contains the Standards File This file is used during IPV Setup but not during Photometric Test Photometric Test uses the file that is created during IPV Setup The newly created file is stored in the Vision directory 7 2 Evaluation Diagnostics Evaluation Diagnostics are used to verify that the instrument is operating within allowable para...

Page 58: ...ormance wavelength positions on non traceable internal reference materials Internal Wavelength Precision Repeatability NIR Gain Visible Gain The test is initiated as follows Select Performance Test from the Diagnostics menu Click on Run Performance Test Verify that the OptiProbe is inserted into the Reference position as shown As the test runs a screen like that shown on the next page is displayed...

Page 59: ...ialog box is displayed Before clicking Close All Reports the user is directed to the tabular display To view the tabular display of results place cursor over the tabular display and double click twice Vision enlarges the tabular portion of the screen Now click on the OpQual tab near the bottom of the screen Noise summary results are shown Noise Summary displayed using the OpQual tab ...

Page 60: ...ns to maintain monochromator wavelength measurement These internal wavelength materials are protected and are moved by software command transparent to the user When Performance Test is run the relative wavelength positions and repeatability of these wavelength materials are monitored and reported Note that these internal wavelength materials need not be precisely on the assigned nominals These nom...

Page 61: ...ion for this instrument Please verify that it is correct Click OK when ready Vision requests that the user place the instrument reference into position Verify that the probe is in the position shown Click OK When the reference scan is finished insert the wavelength standard as directed Always place the standard into the instrument in the same orientation In this case the user has marked the standa...

Page 62: ...ay damage the surface When the test is complete a spectrum of the standard is shown in the upper right quadrant of the screen A tabular report is shown in the lower right quadrant giving each peak its nominal position and its measured position The difference from nominal and the repeatability of wavelength peak positions are calculated ...

Page 63: ...ertification also tests certain peaks in the wavelength standard These peaks are used to set the Instrument Wavelength Profile and one peak is used for bandwidth calculation The wavelengths used for the instrument wavelength profile are well defined stable peaks in the wavelength standard These are the same peaks used during Instrument Calibration Wavelength Certification is a verification that th...

Page 64: ...to other causes Re run Instrument Calibration then run Wavelength Certification again to verify that it has passed 7 2 3 Photometric Test Photometric Test provides a method to verify ongoing photometric performance of the instrument This is a requirement for pharmaceutical users Test results are stored in the Diagnostic Database and may be accessed at any time Control charts are plotted after seve...

Page 65: ...r Photometric Test are numbered The digits 04 refer to the fourth version of this tolerance file When new XDS instruments are added the tolerance file number is incremented Tolerances for a given instrument do not change within the file however The file IPVXDS01 xda will provide the same test tolerances as IPVXDS04 xda Vision displays the wavelength regions for test For reflectance instruments the...

Page 66: ...tivity Therefore it is very important not to allow dirt to contact the reference If operating in Reference Standardized mode Vision requests the 99 standard from the set If not operating in Reference Standardized mode Vision requests the 80 standard which is used in place of the internal instrument reference Select the requested standard from the set Labels on the back of each standard identify th...

Page 67: ...rea as shown Tolerances are automatically applied and a Pass or Fail indication is given Continue to follow the on screen prompts for each standard Vision requests the 40 20 10 and 2 standards When Vision has completed the test the tabulated results may be printed They are also stored in the Diagnostic Database for later recall When the test is complete click Close Window A tab on this display als...

Page 68: ...mbination of the above The user should verify proper test methods cleanliness and Reference Standardization If the Spectralon reference is quite dirty it may require replacement and subsequent re Reference Standardization 7 2 4 Gain Test The Gain Adjust feature can be a useful diagnostic tool though it is not required for normal operation Technically gain is never adjusted on the XDS OptiProbe Ana...

Page 69: ...se This permits the user to see if the gain factor has changed significantly over time 7 2 5 Low Flux Test Low Flux Test is included for users who must run this test in support of regulatory requirements Low Flux Test uses a nominal 10 reflectance standard in the sample position A noise test is run using this standard Because the reflectivity is less than the instrument standard the test is consid...

Page 70: ... on the side of the instrument with the reflectance probe inserted into the middle opening for this test Follow Vision screen instructions for testing If the user clicks No to the external standard then Vision will automatically trigger the 10 internal screen for this test In this case the reflectance probe should be in the upper opening against the internal instrument standard Vision runs the Low...

Page 71: ...mmarized results as compared to acceptance specifications Vision reports a pass or fail based upon successful test completion Results are stored in the Diagnostic Database for later recall The user may print results or click Close to complete the test ...

Page 72: ...ce personnel The instrument should be kept clean at all times If it becomes dusty or dirty wipe it with a damp soft cloth to restore the finish The sampling window should be kept clean to prevent loss of signal This is especially important with high absorbance samples Clean with a dampened soft non linting tissue Remove all surface deposits and dust Do not scratch the Smart Probe window Scratches ...

Page 73: ...hould release allowing the door to open as shown Lower the door as shown to expose the filter material Using a 1 4 nut driver remove the four 4 40 nuts that hold the filter frame in place Lift the filter frame off and carefully set it aside for re use with the new filter material Do not lose the nuts ...

Page 74: ...l the filter frame Install the 4 40 nuts and tighten hand tight as shown Gently close the instrument door Order new filter material from your Metrohm authorized distributor immediately 8 3 Lamp Replacement The lamp may need to be changed after several thousand hours of use Generally the instrument will exhibit high noise during Performance Test or when wavelength precision repeatability has begun ...

Page 75: ...nt to cool for about 15 20 minutes before attempting to change the lamp 2 On the back side of the instrument loosen the eight 8 captive thumbscrews that secure the lamp cover in place 3 Loosen the screws holding the wire terminals onto the terminal strip Do not remove these screws One or two turns counter clockwise is sufficient Pull the wire connectors out from under the screws ...

Page 76: ... to release the retaining ring from the shoulder screws 5 This photo shows the lamp retaining ring in the removal position The spring will tend it push the retaining ring outwards when the shoulder screws line up with the openings Do not drop the lamp or retaining ring 6 Pull the lamp and ring outward from the instrument as shown ...

Page 77: ... next lamp change Always keep a spare lamp in stock to avoid last minute emergencies 8 Unpack the new lamp from the protective box Place the new lamp carefully onto the bench and place the lamp retaining ring over the wires as shown 9 Gently place the lamp and retaining ring into the lamp box in the instrument The outer edge of the lamp should fit into the machined inset in the lamp plate ...

Page 78: ... appear as shown Note the shoulder screws holding the lamp retaining ring The rectangular base of the lamp may be in any orientation We have placed it horizontally for appearance purposes only 12 Install the wire terminals to the terminal strip as shown There is no polarity Place one wire to each terminal Tighten securely 13 Place the lamp door over the lamp box and tighten the eight 8 thumbscrews...

Page 79: ...t have a spare lamp after changing this lamp order one from your Metrohm distributor immediately NOTE The lamp is a very special assembly and should never be replaced with any substitutes Special features of the lamp include but are not limited to the following Hand selected for high energy filament placement Coated internally and externally for maximum NIR performance Welded wire connectors to mi...

Page 80: ...t from AC power Open the side cover Remove the AC power plug from the AC power block of the instrument Use a tool such as an Allen wrench to pull the housing open There is a small slot where the tool can be inserted to pry the door gently open ...

Page 81: ...ug the AC power cord in Plug the RJ 45 cable in if it was removed Turn on AC power and re establish instrument communication 8 5 Maintenance Log Vision provides a Maintenance Log in the Diagnostic Database to permit tracking of maintenance activity This provides a convenient place to find information about tests lamp changes and user entered comments To access the Maintenance Log click on Diagnost...

Page 82: ...s shown in the screen below In addition the user may enter text comments which are saved as part of the log Enter the text then click on OK This screen shows entries sorted by record number To re sort by another parameter click on the column heading ...

Page 83: ...ormly enforced with analytical instrumentation There are many reasons for this including assessor familiarity with NIR instrumentation However the enforcement is beginning to be applied more commonly In summary validation is or will be the concern of every analytical instrument user sooner or later Validation is generally broken down into three categories Hardware Analyzer and sampling accessories...

Page 84: ...ontinuing stability of photometric and wavelength response These reflectance standards include Metrohm IPV Software It records first use instrument response and permits regular verification of subsequent response to the original measurements NIRStandards are designed for easy use with all Metrohm reflectance instruments used in the pharmaceutical industry and most instruments used in other industr...

Page 85: ...lation Qualification IQ and Operating Qualification OQ Documents are included as part of the Vision Spectral Analysis Software package These documents are presented in checklist fashion guiding the user through each step in setting up and qualifying the instrument The software OQ is a pre built project model using actual spectra It is imported for quantitative and qualitative analysis and output r...

Page 86: ...ce Vision meets the strict requirements of 21 CFR Code of Federal Regulations Part 11 covering Electronic Records and Signatures Key compliance features include Validation of system software and instrument connection Blocking of invalid or altered records Generates accurate and complete copies of records in human readable and electronic form Records protected and retrievable throughout their reten...

Page 87: ...screen click on Configure Account Policy A 21 CFR Verification Document is available for users who wish to verify key features This document is included with Vision installation materials on the same CD starting with Vision 3 50 SP1 Please contact your local distributor for information or if you cannot locate this document ...

Page 88: ...rmal energy have been evaluated The instrument design is meant to dissipate any thermal energy A circuit interlock is provided as a backup to primary thermal controls The instrument has been tested at maximum operating temperature with all functions active as a means of verifying thermal dissipation under worst case conditions Normal care should be exercised by the user to avoid conditions which m...

Page 89: ...ction For minor problems this guide should be consulted While some recommendations are quite basic some of the suggestions may be helpful in avoiding oversights or problems Follow the recommendations and eliminate any possible causes listed Recommendations are listed in logical order of occurrence wherever possible When all recommendations have been checked and if the instrument is not operating p...

Page 90: ...nt This serial number should be visible in Vision in Configure Input 6 Verify that the connector ends of the RJ 45 cable are not damaged crushed or distorted in any way Wires should be firmly clinched by the connectors 3 Lamp does not come on when instrument is connected 1 Verify communication with instrument Click on Acquire Disconnect then Acquire Connect Select DCM to verify proper connection I...

Page 91: ...or humidity may be changing rapidly during the test This can usually be observed as large spectral activity between 1300 1400nm and 1800 1900nm If this is the case the instrument should be tested in a more controlled setting to verify proper operation 3 Instrument may be located on a bench with grinders stirrers or other laboratory equipment which produces vibration or mechanical disturbance This ...

Page 92: ...in Test 1 NIR Gain should always be less than 100 on the reference unless extreme lengths of fiber are used If gain is high verify that the Interactance Reflectance probe is positioned in the top opening against the internal reflectance reference 2 Verify that lamp is lit see above 8 Instrument cooling fans are operating at maximum rate 1 Verify that air intake on side is not blocked by other equi...

Page 93: ...sed by use of two network cards in PC Data collisions are causing lost communication packets Remove one NIC card and use the connection method on page 4 11 Vision reports that there is no Reference Standardization or Instrument Calibration suggests that these tests be run 1 Usually caused by entering the test then canceling which leaves the instrument with no completed test constants Do not cancel...

Page 94: ...knees not with the back Lift unit up move to a cart and lower gently Do not lift from below waist level as the unit may be awkward to control Ask for assistance when lifting from lower levels to bench height 3 Always use a cart when moving the instrument from one location to another The monochromator weighs 21 kilograms 46 2 lb and should never be carried except when moving from a bench to a cart ...

Page 95: ...intenance 70 79 80 Method 32 42 Module 21 24 26 40 46 Monochromator 21 Network Connection 3 10 NIRStandards 82 83 Noise 56 57 58 Operating Qualification 82 83 Options 3 31 38 42 53 Password 14 37 84 Performance Test8 28 31 35 42 56 57 58 62 67 72 77 82 89 Photometric Test 3 53 55 62 63 66 Power Switch 91 Project 31 38 42 Q9000 81 Reference3 29 31 36 40 42 43 46 47 48 49 53 54 56 63 64 66 77 90 91 ...

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