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Metrohm FOSS NIRS XDS MultiVial Analyzer Manual Download Page 67

 

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65 

7.1.3

 

 Reference Standardization, “Use Iris” Position 

Next we will perform Reference Standardization in the “Use Iris” mode. 

First, verify that “Use Iris” is selected in the 
Select Tray Dialog box. 

 

Vision will advise the user to insert the Iris 
Adapter after the sample carriage mechanism is 
reset. Do not insert the Iris Adapter until the 
message is given by Vision. 

 

Click “OK” and insert the Iris Adaptor as 
shown. 

 

Select Diagnostics, Reference 
Standard,  
Create Reference Standard. 

Vision prompts for the 
instrument reference. The 
XDS MasterLab Analyzer has 
an internal instrument 
ceramic reference (reflectance 
only) which is positioned 
automatically. 

 

Summary of Contents for FOSS NIRS XDS MultiVial Analyzer

Page 1: ...NIRS XDS MultiVial Analyzer Manual 8 921 8002EN ...

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 MultiVial Analyzer Manual 8 921 8002EN 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: ...ting Instrument Calibration that Reference Standardization must be performed Removed discussion of sample spacers in section 5 4 Spacers are not necessary with this unit The slight optical difference in height between Use Iris mode and Use Tray mode is handled by having a separate Reference Standardization for each mode Changes were made in Reference Standardization to clarify this issue It was pr...

Page 6: ...5 3 6 Troubleshooting Connection Problems 16 3 6 1 Network Troubleshooting Overview 17 3 6 2 Direct Connection Troubleshooting Overview 21 4 Assembly of the Instrument 23 5 XDS MultiVial Module 28 5 1 Introduction to Vial Analysis 28 5 2 Creation of a Custom Vial Size 29 5 3 Spot Size Adjustment 31 5 4 Iris Adapter 34 5 4 1 Installation of Iris Adapter 34 5 5 Use of the Sample Transport Mechanism ...

Page 7: ...ctory Instrument Test Guide and Results 104 9 1 2 Installation and Operating Qualification Documents 104 9 1 3 NIRStandards for Instrument Performance Verification 104 9 1 4 Instrument Performance Certification 104 9 1 5 Metrohm NIRSystems Master Instrument Program 105 9 2 Software Validation Tools 105 9 2 1 Installation and Operating Qualification Documents 105 9 2 2 Vision Certificate of Validat...

Page 8: ...accuracy and transferability between like instruments These software algorithms must be used to assure method transfer between instruments See section 7 1 for full details The versatile sampling mechanism of the MultiVial Analyzer offers a movable sampling platform suitable for handling multiple vials or other samples The software supports acquisition of spectra in an unattended mode freeing the o...

Page 9: ...results tracked over time The menu driven validated Vision Software package meets all requirements of CFR 21 Part 11 covering Electronic Records and Signatures Vision comes with a full manual for operation and theory of operation with complete instructions for analytical development The XDS Analyzer provides 0 5nm data points and uses several innovative methods to assure wavelength accuracy and re...

Page 10: ...mperature inside the instrument enclosure There is no airflow drawn into the optics chamber instrument An external fan cooling loop is provided in the side chassis with thermal conduction from the inside of the optics chamber This avoids contamination of the instrument in dusty environments An air filter is built into the door of this chamber For cool environments heaters are embedded in the therm...

Page 11: ... the filter 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 Vibration Install the XDS Analyzer where it will...

Page 12: ...rk personnel Full instructions are given in section 3 0 2 6 Instrument Dimensions and Weight The XDS MultiVial Analyzer dimensions are Width 18 0 457 mm Height 15 25 387 mm Depth 22 5 572 mm front to back Leave a minimum of 3 76mm around the instrument sides and back for airflow and access space Leave as much space as possible in front for sample handling Weight 68 7 pounds 31 25 kg Follow lifting...

Page 13: ... cannot 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 m...

Page 14: ...on 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 3 Ove...

Page 15: ... an internally stored default IP address This address 169 254 0 2 is used for 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 cy...

Page 16: ...ons are followed In the rest of the cases there may be network issues corporate restrictions or other issues which inhibit easy connection The troubleshooting section covers some of the most common problems In all cases 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 eas...

Page 17: ...called enterprises Subnet Mask Subnetting is used to break a large network into smaller sections This can enhance efficiency raise speeds and 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...

Page 18: ...onnection using a crossover cable 3 When Vision finds the instrument on the LAN it will be shown The dynamic IP address assigned by the server is shown along 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 6 Troubleshooting Connection P...

Page 19: ... indicates connection or network issues Verify Cable Type Verify correct cable type for hookup Most networks use patch cables Free standing systems use a crossover cable Power down the XDS instrument then power it 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 conti...

Page 20: ... steps Click on Start then Control Panel Double click on Network Connections Double click on Local Area Connection Click on Local Area Connection Properties Click on Internet Protocol TCP IP Click on Properties The full path from Network Properties forward to Internet Protocol TCP IP Properties is shown ...

Page 21: ...ngs take effect If in doubt do this and try XDS instrument communications again after this takes effect Network Solution 2 Returning to the Local Area Connection Status dialog box note these items for the computer Address Type should be assigned by DHCP IP Address Write this address down for the next step Subnet Mask Write this down for the next step If connection cannot be achieved it may be nece...

Page 22: ... compatibility pack may need to be loaded to support Ipv4 enabled devices Network Solution 4 Verify that the Firewall on the computer has Vision loaded as an exception This is located under Control Panel Windows Firewall If this is not enabled click Add Program and select Vision from the list When finished click OK Network Retry XP and Vista Windows XP and Vista users should click on Retry Only Th...

Page 23: ...issues First verify the following The instrument is free standing not connected to a network with DHCP server There is only one network card in the computer A crossover cable is used between the XDS instrument and the computer If these conditions are met please proceed Direct Connection Solution 1 If using a crossover cable verify that the computer is communicating in the same IP range as the XDS ...

Page 24: ...t communication Please do not click anything for this amount of time or communication may be interrupted Direct Connection Solution 3 Click on Try Direct Connect with Default IP This searches for the default IP address stored in the instrument When the instrument is found click OK This should resolve the connection issue Proceed to Acquire and Connect in Vision ...

Page 25: ... Spectral Analysis Software Vision Manual is on CD Spare Lamp Accessory Kit containing cords cables standard tray and other required items Safety Manual for CE certification Instrument Test Results Packet Packaging of items 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 mat...

Page 26: ...uence that begins on the next page 1 Load Vision Spectral Analysis Software onto the computer designated to operate the XDS instrument 2 Place the monochromator on the lab bench in the position shown 3 Open the right hand panel of the instrument Pull it gently by a fin until the catch releases This panel opens to about a 45 degree angle for access to connectors and for filter inspection Avoid scra...

Page 27: ...o into either of the other two locations 5 Insert the AC power cable into the AC power block as shown 6 Attach the RJ 45 cable to the network connector on the instrument If using Direct Connection use the gray cable from the instrument accessory kit If using network connection do not use the gray cable as it is a UTP crossover cable and will not work with a network Use a network cable as described...

Page 28: ...onochromator Module not shown to allow a good view of handle Push monochromator and module together firmly with handle up then lower the release handle 10 When the catches are fully engaged to the locking togs push the release handle down all the way This automatically engages the electrical connector and fiber optic interface and maintains proper alignment of the module to the instrument The fina...

Page 29: ...network jack Use the cable supplied with the instrument 13 When all the above 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 14 Prepare to establish communicatio...

Page 30: ...ral information for each vial is acquired and stored and the calibration or library identification is automatically applied Partial racks may be run and the order of scanning determined by the user Vision provides easy graphical tools to make setup easy and accurate No special software skill is required to set up the instrument for routine analysis once the calibration is in place Because the Mult...

Page 31: ...ed in the section on Vision Normally spot size should be no larger than 80 of vial size However this is not pre set as users may wish to scan a smaller area 5 2 Creation of a Custom Vial Size Most users will work with one of the standard vial sizes offered However for setup of custom sizes this information is provided To create a custom vial diameter follow these steps From the menu bar select Con...

Page 32: ...ize If your vial diameter is not shown ignore the default sizes Click New This brings up the Tray Configuration Dialog box shown below A Tray ID must be assigned The normal convention is to use the diameter then the number of vials in a row and a column You may use your own naming method of course The shortcut to this screen is shown below In this case the vial diameter is 22mm Enter 22 for Vial D...

Page 33: ...be machined to these specifications A charge applies for each custom tray supplied 5 3 Spot Size Adjustment The MultiVial Analyzer offers spot size adjustment which permits the user to set the relative size of the illumination beam that strikes the sample This is useful for small objects such as 15mm vials about 5ml volume tablets and other small diameter materials The instrument energy is focused...

Page 34: ...l 17 5mm spot size 29mm vial 17 5mm spot size As a rule a large spot size is preferable for large samples This provides as much sample viewing area as possible for a good cross sectional area of the sample The default spot size is 17 25mm ...

Page 35: ...sizes in between those listed Areas are rounded to the digits shown When using the default spot size of 17 25mm the sample diameter should be at least 21 6mm 0 85 inch as represented by the gray circle in this diagram At the minimum spot size of 9 5mm the sample diameter should be at least 11 9mm 47 inch as represented by the gray circle in this diagram Diagrams may not be actual size check dimens...

Page 36: ...entering Close the aperture around the object to center it then open the aperture to avoid reflecting light back from the aperture itself 5 4 1 Installation of Iris Adapter The Iris Adapter is used for round sample cups beakers vials and other stationary samples NOTE Set the Select Tray dialog box to Use Iris Align the holes in the Iris Adapter with the pins on the sample platform and carefully lo...

Page 37: ... analysis using the Reflectance Cell and Immersion Diffusers These cells are often used for clear to semi clear liquids such as alcohols and suitable fluids When using vial trays in the normal mode the vials are slightly elevated from the sampling window A separate Reference Standardization is performed in the Use Tray mode to account for the slight photometric difference between the Use Iris mode...

Page 38: ...d guides on the sample carrier They are shown in this photo the pencil points to the one on the right The sample cell must be positioned over these pins and gently pressed down to the stops If crooked the cell cannot be positioned correctly Care must be used in placing the cell on the pins The Select Tray Dialog box must have the correct selection made Click on Use Boat as shown This selection de ...

Page 39: ...Adapter When using the Iris Adapter select the Use Iris setting in the Select Tray dialog Box This positions the sample carrier to a central position and permits the user to install the Iris Adapter The Iris Adapter is shown in the next photo NOTE Failure to set the Use Iris setting may result in damage to the instrument which is not covered by instrument warranty When set to Use Iris Vision ignor...

Page 40: ...creen 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 will be in violation of CFR 21 Part 11 A new project must be created The project is used to store data and calibrations for a given type of ...

Page 41: ...top left and the module LED lower right should be illuminated as shown This box directs the user to select the instrument IP Internet Protocol address Use the drop down arrow of the IP Address box and select the correct instrument The instrument must show Available to be selected Click OK to exit the dialog box then OK again to exit Configure Data Sources Vision prompts the user to connect to the ...

Page 42: ...ndardization Use Instrument Calibration These selections are explained in more detail further in this manual Because some selections do not apply to the MultiVial they are not selected Reference Standardization and Instrument Calibration must be selected for transferability between similar instruments Click OK to exit the dialog box Select Configure Tray from the menu bar ...

Page 43: ... to use vials so we keep the Use Tray setting Click on Select to save these settings and exit this dialog box If the user clicks on Modify View from the Select Tray Dialog box this screen is shown If New is clicked all fields are blank for entry of vial information Click OK to save and exit In this example the 15mm vial will be used See section 5 2 on Creation of a Custom Vial Size creation for de...

Page 44: ...ause this is a new project Click New to establish a new Data Collection Method The instrument self identifies as an XDS system with the MultiVial Module The user should enter a logical name for the DCM Spaces are OK Note that the Spot Size should be adjusted if the vial used is smaller than 21 56mm diameter The default spot size is 17 25mm Normally the beam size should be set for 80 of the vial di...

Page 45: ...ference Standardization is checked If it is not the user should return to Configure Options and select Reference Standardization on that menu before establishing a DCM Click OK to exit the dialog box The DCM information will be saved Next select this DCM from the selection box Click OK to connect to the instrument Once connected verify that the amber Communication LED is lit on the instrument Visi...

Page 46: ...mple is scanned directly on the sample window or on the vial tray which is raised from the sample window to allow free motion By storing two separate reference files Vision can compensate for the optical difference between the two methods This allows use of one library or calibration which is applied to either sampling method If the user does not see this message Vision has the required Reference ...

Page 47: ...roducts then highlight and select the desired Product ID The Sample ID Prefix is not entered in this box that is done in the next screen Click OK when finished Vision displays this screen which corresponds to the vial tray Note that the Product ID is entered this came from the previous dialog box Note that the Vial Dialog box is also called when either of these actions is performed 1 The user clic...

Page 48: ...roduct ID column This brings up the product selection menu Highlight the desired product and press Enter This sets the product for the highlighted rows Also note that 20 vials are shown in a 4 x 5 configuration This came from the Select Tray Dialog box It is shown at right as a reminder 6 2 1 Sample ID Entry There are several ways to enter the Sample ID Entry Method 1 Right click on the circle tha...

Page 49: ...hen active and the sampling order is incremented in the Order column Do not click on the vial position and turn it white that removes it from the Order column and de activates sampling on that vial Entry Method 2 Double click on the upper part of the vial position which brings up the box shown The Sample ID may be typed into this box Press Enter when finished While entering Sample IDs the user may...

Page 50: ...o Entry Method 3 Click on the cell in the Sample ID column and type the sample name directly into the cell Be sure to click the vial position to turn it yellow to make the vial position active The cell entry method is shown above highlighted by the red border The user may type a Sample ID then press Enter to move down to the next row This speeds entry of a column of sample names Entry Method 4 If ...

Page 51: ...er pasting Sample ID instead Hint To select quickly click on the first cell hold the Shift key and click on the last cell All cells in between will also be highlighted Highlight the Sample ID fields to be pasted as shown above Click on the Paste button in the dialog box It is outlined in red below ...

Page 52: ...imit of the vial positions Entry Method 5 The user may use the right click copy and paste method as illustrated below This uses the Windows convention for pasting Highlight the information to be copied right click and select Copy Move the cursor to the destination field right click and select Paste The information will be pasted into the field as desired ...

Page 53: ...his field is optional The field is shown here To remove all entries from the Vial Dialog screen click on the Clear button at the lower left corner of the screen This will clear the entire Sample ID column Click OK to close If this button was clicked and was a mistake click the Cancel button The Vial Dialog screen will close Select Acquire Select Channel verify the product and the original screen w...

Page 54: ...be cleared click Yes Otherwise click No 6 2 2 Order of Sampling There are multiple ways to set the order of vial sampling As a rule it is faster to sample in the sequence of the Order column since this involves less movement of the MultiVial sampling mechanism This saves positioning time If the Sample ID for each sample is entered in order as below this is automatic ...

Page 55: ...e Order it is important to set the order correctly Fortunately there is a method to set order easily without losing Sample ID information In the example above the order is out of sequence for samples 7 9 and 16 If Use Order is left unchecked Vision proceeds in order of Sample Number No action is needed However if the user wishes to set the sequence the procedure is as follows 1 Click on each vial ...

Page 56: ...ill take an initial reference scan then scan the first ten vials Then Vision will take another reference scan and go on to scan the last 20 vials If the tray has fewer than 10 vials Vision will scan up to ten vials if the setting is 10 If the setting is another number other than 10 Vision will use that setting as the maximum number of vials to be scanned per reference A 0 may be entered in this fi...

Page 57: ...he user needs to scan a sample using the Iris Adapter this box should be clicked This resets the choice made in the Select Tray dialog box The user should remove the tray Vision will position the tray mechanism out of the way to allow the Iris Adapter to be inserted When finished the Iris Adapter should be removed and the tray re inserted into the MultiVial mechanism Failure to remove the Vial Ada...

Page 58: ...way to allow the sample cell to be inserted When finished the sample cell should be removed and the tray re inserted into the MultiVial mechanism Failure to remove the Sample Cell may cause an error to be reported in Vision To reset the mechanism for MultiVial trays select Configure Tray to return to the Select Tray dialog box and re select Use Tray This was illustrated in the section immediately ...

Page 59: ... new tray Note that this clears the Sample ID Order and Comments It does not clear the Product ID column To edit the Product ID double click on that row and the selection list is shown Cancel This cancels all actions performed while the dialog box has been open The box is closed and remains as it was before it was opened ...

Page 60: ... must pass before data 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 Referenc...

Page 61: ...sed to apply corrections to the instrument to minimize differences between units of 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 material set to determine a set of internal arbitrary peak posit...

Page 62: ...some being beyond the usable range of the instrument These peak positions are not meant to be traceable as the true wavelength calibration of the instrument is done on an external standard traceable to NIST The internal wavelength materials are used to maintain the external wavelength registration by use of software adjustment for any external effects on the instrument Select Wavelength Linearizat...

Page 63: ... not saturate the instrument or produce negative absorbance values The MultiVial Analyzer requires two reference standardizations one for each sampling level The first level is with a vial directly on the sample window in Use Iris mode with the Iris Adapter The second level involves the MultiVial tray in Use Tray mode where the vial tray is slightly above the sample window Vision applies the corre...

Page 64: ...st establish the configuration and have it verified by the user This assures that test data is sent to the correct location in the Diagnostic Database If the Sample Module Serial Number field is empty locate the sample module serial number on the side of the module Record the serial number and enter it in this field Click OK to accept the instrument identification Vision briefly displays a dialog ...

Page 65: ...lue on the screen it is plotted in a darker color here for readability Next Vision takes a spectrum of the Certified 80 Reflectance Standard as indicated by the status bar on screen Click OK to plot a spectrum of the Certified 80 Reflectance Standard in the next window The Certified 80 Reflectance Standard is shown with the spectrum of the ceramic instrument reference Click OK to plot a correction...

Page 66: ...dization is checked and a tray is used Next perform a Reference Standardization in the Use Iris position Be sure to select Use Iris in the tray menu Follow instructions for removal of tray and insertion of the Iris Adapter Repeat steps given on pages 45 47 in the Use Iris position The Reference Standardization will be stored for use when scanning sample in the Use Iris mode NOTE Perform Reference ...

Page 67: ...r to insert the Iris Adapter after the sample carriage mechanism is reset Do not insert the Iris Adapter until the message is given by Vision Click OK and insert the Iris Adaptor as shown Select Diagnostics Reference Standard Create Reference Standard Vision prompts for the instrument reference The XDS MasterLab Analyzer has an internal instrument ceramic reference reflectance only which is positi...

Page 68: ... automatic No user action is required The status bar indicates scan progress Vision requests the Standard File for the Certified Wavelength Standard Place the mini CD into the CD drive and select the standard file Click Open Vision requests that the Certified 80 Reflectance Reference Standard be placed in the sampling area Place the standard as shown with the identifying label parallel to the long...

Page 69: ...andard is shown with the spectrum of the ceramic instrument reference Click OK to plot a correction spectrum in the next window The correction spectrum represents the amount of spectral correction required to provide a virtual 100 reflectance reference at each data point Click OK to plot the correction spectrum in the next window ...

Page 70: ... taken in the Use Iris mode with a DCM where Reference Standardization is checked When finished remove the Iris Adapter and return to the Use Tray mode NOTE Perform Reference Standardization immediately after changing the spot size to have the proper reference correction loaded in the instrument In the event that Vision does not find a Reference Standardization where it is needed it will prompt fo...

Page 71: ...to those of the standard These adjustments are saved and are applied on each subsequent scan of the instrument yielding a correct spectrum Vision takes an instrument reference which takes about 20 seconds This dialog box is displayed Vision determines the detector time constants using a patented algorithm and sets the proper correction for this parameter Wavelength Linearization is performed in tw...

Page 72: ... end of the test this dialog box is displayed Print confirmation of test results if needed for a log book or other file Click OK to exit Instrument Calibration Hint This file may be manually copied on the computer in the Vision directory if desired During Instrument Calibration the wavelength response for each defined peak is adjusted to assure precise wavelength registration between instruments A...

Page 73: ...hese additional peaks are used to set the wavelength scale of the instrument to aid in instrument matching This is one important step in method 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 SRM 1920a The XDS instru...

Page 74: ...rification 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 Photometric Test compares the current performance of the instrument to the file stored during IPV Se...

Page 75: ...nce 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 mode Vision requests the 99 standard from the set The reference spectrum is shown in red Note that Reference Standardization is not shown as applied to this spectrum it is displayed in raw form If not operating in Reference ...

Page 76: ...o the active Vision directory During IPV Setup Vision writes a special file that is subsequently used in Photometric Certification This new file is named RSSVxxxx The V indicates that this file is to be used for long term Verification of the photometric scale of the instrument This file is written to the C Vision directory or whatever directory from which Vision is operating 7 2 Evaluation Diagnos...

Page 77: ...h regions Internal Wavelength Performance 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 As the test runs a screen like that shown below is displayed This shows the first of ten sets of scans from the ...

Page 78: ...ed in Vision If all results meet acceptance criteria the test is successful and this dialog box is displayed Click Print Report for a hard copy of results Before clicking Close Report 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 OpQua...

Page 79: ... These regions are 400 700nm 700 1100nm 1100 1700nm 1700 2500nm For each region results are given for Peak to Peak Noise P P Root Mean Square Noise RMS Bias A measure of baseline energy changes Each of these parameters is described in more detail in the Diagnostics Section of the Vision Manual If the test is reported as Passed the user may proceed with sample analysis ...

Page 80: ...velength Certification is used to confirm the peak positions of the instrument to a defined external wavelength standard Click on Diagnostics Wavelength Certification Run Wavelength Certification The Number of Samples should be 10 as shown The wavelength standard for reflectance is the SRM 1920 plus talc which refers to the WSR1xxxx standard This is the same cell used for Instrument Calibration Cl...

Page 81: ...wer right quadrant to see the full report The first tab shows the Wavelength positions as found They are compared to the NIST nominal peak positions or the empirically determined positions for talc peaks The difference from nominal and the repeatability of position are calculated Wavelength Certification also tests certain measured instrument profile peaks in the wavelength ...

Page 82: ...tion that the peaks are in correct positions and that the peak positions are consistent over time Note that both tests use the wavelength standard at the sample plane where actual sample measurement is done Wavelength Certification is an excellent method to test whether Instrument Calibration needs to be re run If the original settings in Instrument Calibration have drifted a message will be displ...

Page 83: ...preliminary method to maintain wavelength measurement The final measurement is made at the sample plane using the external standard As discussed under Performance Test the internal reference materials are not traceable and are only used as an internal method of maintaining correct wavelength measurement prior to measurement of the external wavelength standard If the test has passed the user should...

Page 84: ...his 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 several tests have been stored to provide an ongoing record of performance The test uses the same standards used in IPV Setup Photometric Test compares current spectra of each standard to those stored during IPV setup If any differences e...

Page 85: ...is file may have a higher number This merely indicates that additional XDS instruments are now supported by the same file This is transparent to the user Tolerances for this instrument remain the same throughout different tolerance file releases Select this file and click Open Vision displays the wavelength regions for test For reflectance instruments these regions give a good overall picture of i...

Page 86: ...y the reflectance value Insert the 99 standard into the tray as shown with the label parallel to the long axis of the tray When the 99 standard has been scanned the result will be plotted as shown In this picture the upper and lower spectra are tolerances from the initial IPV Setup spectrum The IPV Setup spectrum is the dark spectrum in the middle displayed in black on screen The lighter spectrum ...

Page 87: ...to see the USP recommend plot and summary report These are shown on the next page Note that this test is de emphasized as of December 1 2008 When the test is complete click Print Results for a hard copy report Click Close Window when finished If the photometric scale of the instrument has drifted or if the instrument is not fully warmed up the user may see this message Photometric Test is a good c...

Page 88: ...his test be run unless company policies require it The user should be aware that USP tolerances for Photometric Linearity are quite relaxed compared to FOSS NIRSystems specifications for IPV testing Therefore there may be times when the USP test passes and IPV does not meet manufacturer s specifications This may be due to instrument changes such as dirty windows failing lamp or placement errors In...

Page 89: ...ed in Performance Test and can be called up from the Diagnostic Database This permits the user to see if the gain factor has changed significantly over time 7 2 5 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 Beca...

Page 90: ...andard R101xxxx which may be used for this test The 10 reflectance standard should be positioned in the tray as shown The label should be parallel to the long edge of the tray If the user clicks No to the external standard then Vision will automatically trigger the 10 internal screen for this test No user action is required Vision runs the Low Flux Test which takes about 10 minutes At the end the ...

Page 91: ...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 92: ...nstrument showing the relative location of major components Do not attempt to open the instrument enclosure unless directed to do so by trained Metrohm service 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 wit...

Page 93: ...lows Open the door of the filter compartment Grasp the upper fin as shown and gently pull The snaps should 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 nu...

Page 94: ...er material carefully over the screws as shown The screws should penetrate the filter material fully Install 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 ...

Page 95: ...trument power and unplug AC power cord from AC receptacle or supply The O position is OFF Allow the instrument 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...

Page 96: ... 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 97: ...t lamp change Always keep a spare lamp in stock to avoid last minute emergencies The part number is XA 3000 8 Notice the black arrow on the new lamp This arrow must be upward when the lamp is installed into the instrument This will be shown later 9 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 ...

Page 98: ...locking the lamp retaining ring in place This photo shows the lamp retaining ring locked after proper orientation of the lamp Proper positioning helps assure consistent instrument performance 12 Place the lamp retaining ring over the shoulder screws and rotate counter clockwise top side to left bottom to right to lock the lamp retaining ring into place This photo shows the ring being rotated into ...

Page 99: ...ard position 14 Install the wire terminals to the terminal strip as shown There is no polarity Place one wire to each terminal Tighten securely 15 Place the lamp door over the lamp box and tighten the eight 8 thumbscrews to hold the door in place Do not use any tools to tighten the thumbscrews 16 Plug the instrument back in to AC power Turn the AC power switch to ON ...

Page 100: ...are 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 minimize resi...

Page 101: ... 99 We suggest that you click on Add Lamp Change Entry in the Maintenance Log This provides a record in the maintenance log for the instrument ...

Page 102: ...fore fuse replacement Once the fault is found and corrected this procedure should be followed Turn off power and unplug the instrument 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 103: ...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 104: ...as 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 105: ...s ISO9000 This regulation is similar in scope and intent to CFR 21 but has not been uniformly 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 i...

Page 106: ...e user through each step of instrument set up and qualification 9 1 3 NIRStandards for Instrument Performance Verification Various regulatory bodies recommend regular testing of NIR reflectance instrumentation to verify continuing stability of photometric and wavelength response These reflectance standards include Metrohm IPV Software It records first use instrument response and permits regular ve...

Page 107: ...rify ongoing operational improvements to manufactured systems and provide yearly re calibration of NIRStandards used in Instrument Performance Certification This long term stable Master Instrument assures our users of consistent measurement methodology between instruments and for a given instrument over time 9 2 Software Validation Tools 9 2 1 Installation and Operating Qualification Documents Sof...

Page 108: ...ware audits Upon agreed notice and terms to those customers wishing deeper information FOSS will host software audits by the FDA or other recognized regulatory bodies upon customer request Normal audit terms and scheduling policies will apply Escrow agreements for source code are available 9 2 3 21 CFR Part 11 Compliance Vision meets the strict requirements of 21 CFR Code of Federal Regulations Pa...

Page 109: ... access this 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 110: ...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 111: ...mmendations have been checked and if the instrument is not operating please contact Metrohm Service Department or your local authorized distributor if the problem is not solved Observed Problem Recommendations 1 Instrument does not power up 1 Verify that AC power cord is plugged in to AC power source 2 Verify that the AC power cord is plugged into the instrument AC power block 3 Verify that the AC...

Page 112: ...fore subsequent operation Service may be required 4 Instrument fails Wavelength Linearization 1 Instrument Reference not in correct position Verify that reference paddle is visible in MultiVial Analyzer sample window when a reference scan is taken 2 Instrumental problems contact Metrohm service or your authorized distributor 5 Instrument Fails Performance Test 1 Verify that reference paddle is vis...

Page 113: ...verify that reference paddle is in place on most modules 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 equipment Leave at least 3 4 inches 76 102mm space by intake fins for proper airflow 2 Verify that air filter is clean If not clean or replace filter If fan speeds dropped shortly after opening ...

Page 114: ...ism does not move when using vial tray Click Use Tray in Select Tray Dialog box 12 X Y Sampling Mechanism crashes into Iris Adapter causing Limit Switch Error Click Use Iris in Vial Dialog box 13 Instrument Cooling Fans do not operate 1 Instrument may not be warmed up Fans do not operate until the instrument is near operating temperature 2 Ambient temperature may not require fan cooling This is co...

Page 115: ... 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 116: ...tion The sample carriage will move to the Shipping Position This protects the mechanism from damage during shipment should the container be subjected to excessive bumps and jolts The shipping position is shown Disconnect and turn the instrument OFF This was called Parking Position in some versions of Vision It was re named Shipping Position so that customers did not feel compelled to move the samp...

Page 117: ... 115 When re entering the project to run the instrument be sure to select the correct Use Tray or Use Iris setting in Vision This assures that the instrument will operate correctly ...

Page 118: ... 62 78 86 87 90 108 109 110 114 Network Connection 11 Operating Qualification 104 105 Operating Systems 11 Park Position 114 Password 15 38 106 Peak to Peak Noise 77 Performance Test9 58 75 76 78 81 87 93 98 110 Photometric Linearity 3 86 Photometric Test 59 72 82 83 85 Power Switch 112 Product ID 45 46 47 48 51 55 57 Project 39 48 58 Q9000 103 Reference 3 7 34 35 40 43 44 54 58 59 61 62 64 65 66 ...

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