Metrohm FOSS NIRS XDS MultiVial Analyzer Manual
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Metrohm FOSS NIRS XDS MultiVial Analyzer Manual

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NIRS
XDS MultiVial Analyzer
Manual
8.921.8002EN

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Summary of Contents for Metrohm FOSS NIRS XDS MultiVial Analyzer

  • Page 1 NIRS XDS MultiVial Analyzer Manual 8.921.8002EN...
  • 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 Teachware Metrohm AG CH-9100 Herisau teachware@metrohm.com This documentation 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...
  • Page 5 Change Control (initiated with version 1.0): Version Date Summary of Changes April 15, Initial Release of Manual. 2005 Replaced photos in section 5.4 on Iris Adapter, replaced photos in August 4, 1.01 section 5.5, revised text to clarify correct software settings for use 2005 with cells.

  • Page 6: Table Of Contents

    Table of contents Introduction ........................6 Site Readiness ........................ 9 Temperature and Humidity ................9 General Environment ..................9 Vibration ...................... 9 Electrical Power ................... 9 Instrument Communication ................9 Instrument Dimensions and Weight ............10 XDS Instrument Connection ..................11 Network Connection, connected to an active network port as shown ..
  • Page 7 Vision Certificate of Validation ................105 9.2.3 21 CFR Part 11 Compliance ................. 106 Safety and Electrical Certification ............. 108 11.0 Troubleshooting ................109 Lifting and transporting the Metrohm instrument: ........113 12.1 Instructions for MultiVial® Shipping Position ........... 114 12.1.1 Instructions follow ....................114 Index ......................

  • Page 8: Introduction

    1 Introduction Thank you for selecting the XDS MultiVial Analyzer, manufactured by FOSS. This instrument is the third generation in a series of instruments designed for precision NIR measurement, characterization of organic materials, and qualification of known materials to allowable quality parameters. The XDS MultiVial Analyzer is designed for stable operation in typical laboratory environments, while providing the precision and accuracy users have come to expect of FOSS near-infrared (NIR) instruments.
  • Page 9 two sets of optical (“reference”) calibrations are stored in the instrument. It is important to Reference Standardize on the correct level, as prompted by Vision Software. This aids in method transfer, and is explained in the section on Reference Standardization. This instrument uses near-infrared (NIR) spectral energy to illuminate the sample.
  • Page 10 This IP address may be permanently installed, if required for network purposes. RJ-45 connection also permits remote interrogation and diagnostics checks of the instrument, if necessary and authorized. The instrument enclosure is completely sealed to prevent contamination by dust or other substances. The cooling fans operate outside the main enclosure, and are thermally linked to internal fans that maintain a constant temperature inside the instrument enclosure.

  • Page 11: Site Readiness

    2 Site Readiness Like most precision instruments, the MultiVial Analyzer (RCA) is sensitive to environmental conditions that can affect its performance and useful life. Observe the following guidelines when selecting a site and installing the instrument: 2.1 Temperature and Humidity The XDS Analyzer is designed to work in ambient air temperatures from 40-95°F (4.5-35°C).

  • Page 12: Instrument Dimensions And Weight

    instrument detects network capability and optimizes communication speed. The computer that operates the instrument must have clear access through the network, and be configured to communicate properly. This communication is the responsibility of your on-site network personnel. Full instructions are given in section 3.0. 2.6 Instrument Dimensions and Weight The XDS MultiVial Analyzer dimensions are: •...

  • Page 13: Xds Instrument Connection

    For computers using Windows 95, 98, or NT 4.0, we recommend upgrade of the computer and operating system to current specifications. CAUTION: METROHM NIRSystems does not recommend the use of two network cards under any circumstances. Do not use Direct Connection to the instrument along with a network connection to the company network.

  • Page 14: Direct Connection, In A Free-Standing Manner With No Network Connection

    This method of hookup should not be used when the computer is also connected to a network. Such connection 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.

  • Page 15: Flowchart Diagram Of Xds Communication Protocol

    3. Upon being powered up on a LAN, the XDS instrument requests a “dynamic” IP address from the DHCP server which controls the LAN. This IP address is normally granted promptly (typically in 5-10 seconds) so the instrument can function on the LAN. Most DHCP servers track the XDS instrument by the “MAC”...

  • Page 16: Microsoft Windows Firewalls

    3.4.1 Microsoft Windows Firewalls The Microsoft Windows® Firewall on the PC may interfere with Vision communication. To assure communication, follow these steps: • Enter Control Panel, Security Center. • On the “General” Tab, be sure that “exceptions” are allowed. (Un-click “Don’t allow exceptions”.) •...

  • Page 17: Connection In Vision

    Internet Protocol (IP) and it is the first version of the protocol to be widely deployed. Together with IPv6, it is at the core of standards-based internetworking methods of the Internet and is still by far the most widely deployed Internet Layer protocol. XDS Instruments use IPv4. LAN: A local area network (LAN) is a computer network covering a small physical area, like a home, office, or small group of buildings, such as a corporate site, a university, or an airport.

  • Page 18: Troubleshooting Connection Problems

    2. Highlight “NIRSystems XDS- series Instrument Driver” as shown, then click on “Configure”. Information: At this point, Vision requests any XDS instrument on the local area network (LAN) to report connection status. This may take a few moments. If the instrument is not on a LAN, and instead is connected with a crossover cable, this will take a minute or more.

  • Page 19: Network Troubleshooting Overview

    If your computer uses Windows 95, 98, or NT 4.0 for the operating system, we strongly recommend upgrade to Windows XP for easiest connectivity. This may require a full computer upgrade, as older computers may not have the processor speed, memory, or connectivity required to run Windows XP with full Ethernet compatibility.
  • Page 20 Check Internet Protocol (TCP/IP) Properties. (You may need to contact your IT department to follow these steps.) • Click on Start, then Control Panel • Double-click on Network Connections • Double-click on Local Area Connection • Click on Local Area Connection Properties •...
  • Page 21 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.
  • Page 22 Network Solution 3: The IT department at your company can verify if the network offers full Ipv4 compatibility. If the network has migrated to Verify network has full IPv4 Ipv6 operation, a “compatibility pack” may need to be compatibility. loaded to support Ipv4-enabled devices. Some networks have moved to Ipv6 (Internet Protocol version 6) which uses different address...

  • Page 23: Direct Connection Troubleshooting Overview

    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. 3.6.2 Direct Connection Troubleshooting Overview If no XDS instrument shows as “available”, the computer may need to be configured for the IP address range of the XDS instrument.
  • Page 24 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 for this amount of time, or communication may be interrupted. Direct Connection Solution 3: Click on “Try Direct Connect...

  • Page 25: Assembly Of The Instrument

    4 Assembly of the Instrument The XDS Analyzer will be assembled and installed by a trained representative of Metrohm. This person will perform a full suite of diagnostics to verify correct operation, and will explain basic operating points. Assembly information is given as a guide for the user, should re-assembly ever be required due to an instrument move or for other reasons.
  • Page 26 DO NOT OPERATE OR TROUBLESHOOT WITH THE LID OPEN. SUNLIGHT MAY CONFUSE THE OPTICAL INTERRUPTERS USED TO POSITION THE SAMPLE CARRIAGE. THIS MAY CAUSE AN “X-Y POSITIONING ERROR” TO BE REPORTED. Follow the assembly sequence that begins on the next page: Load Vision Spectral Analysis Software onto the computer designated to operate the XDS instrument.
  • Page 27 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 close fully.
  • Page 28 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 the final position. The latches are used to lock the module in position.
  • Page 29 If using a network, use a non-crossover type cable as listed in section 3.0. Plug the RJ-45 network connector into a functional network port. If this requires approval from a network administrator, it should be properly approved for hookup. For “Direct Connection” the gray cable from the instrument plugs directly to the computer network jack.

  • Page 30: Xds Multivial Module

    The XDS MultiVial Analyzer is primarily designed for vial sampling, which is the focus of this manual. Optional sampling devices are available, and are also described following the vial information. For optional sampling accessories, please contact your Metrohm NIRSystems distributor. 5.1 Introduction to Vial Analysis...

  • Page 31: Creation Of A Custom Vial Size

    Step by step instructions are given later in this manual. Please see Section 6.2 for full information. It is important that the “spot size” adjustment be set up properly for a given vial size. This is also covered 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.
  • Page 32 At the Select Tray Dialog box, note that four sizes (vial diameters) are already loaded in Vision. (Other sizes may be added over time.) NOTE: The spot size (set in the Data Collection Method) should be no larger than 80% of the vial diameter.

  • Page 33: Spot Size Adjustment

    Note that there are other important dimensions, including the vial “support ledge”, and the flatness of the final tray. Because the fabrication is critical to repeatability, Metrohm NIRSystems does not recommend local machining. Please contact your Metrohm NIRSystems Distributor for ordering information.
  • Page 34 • 19mm vial: 15mm spot size • 25mm vial: 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 The adjustment ranges from 9.5mm to 17.25mm, in adjustment steps of 0.25mm. The effective scanned sample areas at various spot sizes are as follows: Spot Size Minimum Sample Scanned Sample Area Diameter.* Diameter Diameter Square mm Sq. Inches (mm) (in.) 9.5 mm 11.9 mm 0.47 in.

  • Page 36: Iris Adapter

    NOTE: Perform Reference Standardization immediately after changing the spot size, to have the proper reference correction loaded in the instrument. 5.4 Iris Adapter When scanning stationary objects, the “Use Iris” selection must be clicked. (Stationary objects need not be moved across the sample window for averaging.) Use the Iris Adapter for centering.
  • Page 37 Use the iris to center samples in the window area. Push the handle to the right to center the sample, then to the left to move the iris from the sample window area. Close the door of the sample chamber to exclude ambient light.

  • Page 38: Use Of The Sample Transport Mechanism

    5.5 Use of the Sample Transport Mechanism The sample transport uses a small motor and lead screw to position the cell over the sampling window of the module, as shown in the photo at right. In normal operation, the mechanism will move the cell to one of 8 sample positions, for maximum sampling area exposure.

  • Page 39: Use Of The Iris Adapter

    The sample transport mechanism is quite rugged, and requires no service by the user. Please observe these cautions: • Never attempt to move the mechanism manually. This will cause a “Limit Switch Error” in Vision. The user must then disconnect, cycle power, and re-connect to the instrument to reset the mechanism.

  • Page 40: Vision Software: Connection To The Instrument

    6 Vision Software: Connection to the Instrument This section describes communication between the computer (with Vision Software loaded) and the XDS instrument. Please follow these steps to establish communication. The instrument may be “direct connected” as explained in section 3.0 of this manual. Alternatively, the instrument and computer must both be plugged into a live RJ-45 communication jack, on an active network.
  • Page 41 Vision asks if the default directory location is acceptable. Click on “Yes”. Vision creates a directory for the project as shown. This screen sets up communication parameters for the instrument. The XDS instrument has a unique driver. Highlight this box and click on “Configure”.
  • Page 42 Select Configure, Options from the menu bar. Verify that these selections are clicked: • Instrument must stabilize before data acquisition • Use Auto-Linearization • Reference Standardization • 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.
  • Page 43 Vision has four “default” trays built in, for ease of use. These are common trays, and should serve many users. Check the vial diameter you plan to use, and highlight it on this list, if shown. (15mm_4x5 is selected for this example.) For a vial diameter not shown, click on “New”.
  • Page 44 Vision requests that a Data Collection Method (DCM) be selected for communication with the instrument. The DCM sets important parameters for how the data is taken, and assures consistent methods. There are no Data Collection Methods available because this is a new project. Click “New” to establish a new Data Collection Method.
  • Page 45 Use 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 done rapidly. Click “OK” when finished.

  • Page 46: Use Of Vial Dialog Selection Menu

    Upon connection, Vision may prompt for the instrument configuration. This is used to establish a Diagnostic Database. (Under some circumstances this screen may not appear.) 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 47 From the menu bar, go to Acquire, Select Channel. Vision prompts for the Product ID using this dialog box. Enter the correct product name in the Product ID field. NOTE: If multiple products exist, click the arrow to see all products, then highlight and select the desired Product ID.

  • Page 48: Sample Id Entry

    2. The user selects Acquire, Sample from the File menu bar. It is not necessary to acquire a reference first with the MultiVial Analyzer, since it is programmed to take a reference as part of the scan sequence. To change the Product ID, right-click over the “Product ID”...
  • Page 49 is shown with a circle here, for clarity in “black and white”.) The “Edit” box appears as shown. Click on “Edit”, then type the sample name into the vial position. Press “Enter”. The Sample ID will also be shown in the table at right, as shown below: Vision fills in the “Order”...
  • Page 50 the column at the right. Note that the Product must exist (that is, it must have been created within the Project) to be used in this manner. In the example shown, there are two “mgstearate” products shown. One has a suffix “1” that is not shown due to window size.
  • Page 51 Click on the vial positions to be entered, so they are yellow and active. (This may be done after 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.
  • Page 52 The Sample ID names are pasted into the column, as shown. In this case only five names were pasted, for clarity. The entire column may be pasted, up to the limit 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.
  • Page 53 There is a field for comments beside each sample. To see this field, click the small arrow at the bottom right, and the field will be visible. Alternatively, use the “Tab” key. Start on the Sample ID, Product ID, or Order, and tab over to the “Comments”...

  • Page 54: Order Of Sampling

    To delete multiple Sample ID names, highlight those fields, and use the “Delete” key on the PC keyboard. Vision will ask for confirmation, as shown. If the fields are to be cleared, click “Yes”. Otherwise click “No”. 6.2.2 Order of Sampling There are multiple ways to set the order of vial sampling.
  • Page 55 At the bottom of the Vial Dialog screen is a checkbox marked “Use Order”. If this box is checked, the MultiVial Analyzer will start with the sample marked “1” in the “Order” column, and proceed numerically upward through the order designated in the “Order”...

  • Page 56: Additional Vial Dialog Functions

    column to the proper sequence. 4. Click on “Use Order” to have Vision follow the designated order. 6.2.3 Additional Vial Dialog Functions There are several other important functions to be set or used in the Vial Dialog box. They are shown below, and described in the text that follows.
  • Page 57 highlighted area of the table. Print: This prints the table containing the Sample ID, Product ID, Order, and Comments, as shown at right. The full length of the table will be printed – it is cut off here for clarity. Print in “portrait” mode. Use Iris: If the user needs to scan a sample using the Iris Adapter, this box should be clicked.
  • Page 58 To reset the mechanism for MultiVial trays, select Configure, Tray to return to the Select Tray dialog box, and re-select “Use Tray”. Use Boat: If the user needs to scan a sample using the large Sample Cell (boat), this box should be clicked. (This resets the choice made in the “Select Tray”...
  • Page 59 The “Clear” button removes all data from the dialog box. The user should clear the box before entry of information on a 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.

  • Page 60: Instrument Diagnostics

    7 Instrument Diagnostics Vision provides diagnostics for instrument setup, which must be performed before use of the instrument for analysis. Following these diagnostics, another set of diagnostics is provided to evaluate the ongoing performance of the instrument. These are explained in the sections that follow. The instrument must be set up with the Iris Adapter or Reference Tray for these diagnostics, as small round sample cells are used.

  • Page 61: Wavelength Linearization

    This feature is used only with XDS Process instruments that operate with Transmission Pair probes. Do not select. Instrument matching (method transferability) requires that Reference Standardization and Instrument Calibration be selected, and that Certified Standards are used when required to maintain calibration.
  • Page 62 The “visible” portion of the spectrum is similar. A linearization is applied to this portion of the spectrum. Minor artifacts appear in these raw spectra due to detector crossover and other spectroscopic reasons. After linearization these artifacts are minimal or not evident, some being beyond the usable range of the instrument.

  • Page 63: Reference Standardization, "Use Tray" Position

    The results screen shown above is typical. 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, this message confirms the transfer.
  • Page 64 Standardization using the Iris Adapter, without spacers. Reference Standardization may be performed in this order, or “Use Iris” first, and “Use Tray” second. Select Diagnostics, Reference Standard, Create Reference Standard. Vision prompts for the instrument reference. The XDS MultiVial Analyzer has an internal instrument ceramic reference which is positioned automatically.
  • Page 65 Place the standard as shown, with the identifying label parallel to the long axis of the tray. Close the cover, and click on “OK”. Vision plots a spectrum of the ceramic instrument reference, as shown. (The spectrum will be light blue on the screen –...
  • Page 66 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. A final spectrum (green when plotted on-screen) is plotted to verify that the corrected spectrum produces the same results...

  • Page 67: Reference Standardization, "Use Iris" Position

    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.
  • Page 68 If Vision displays the Instrument Configuration screen again, click “OK to accept the instrument identification. Vision briefly displays a dialog box which indicates that the instrument reference is being placed into position. In reflectance, this is automatic. No user action is required. The status bar indicates scan progress.
  • Page 69 Vision performs the same operations as done on the previous Reference Standardization. Click “OK”. The Certified 80% Reflectance Standard 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...
  • Page 70 A final spectrum (green when plotted on-screen) is plotted to verify that the corrected spectrum produces the same results as the Certified 80% Reflectance Standard. Click “Close Report” to continue. The correction is automatically downloaded, and is saved in the Diagnostic Data Base.

  • Page 71: Instrument Calibration

    7.1.4 Instrument Calibration Instrument Calibration uses an NIST- traceable, stable, standard, of known wavelength response, as a method to establish wavelength scale response of the instrument. The instrument is set to scan the standard, and the nominal peak positions for each major absorption are determined.
  • Page 72 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 prompts the user to insert the WSR10xxx standard into the instrument. Insert the WSR10Xxx Wavelength Standard Cell when prompted.
  • Page 73 The wavelength standard used is directly traceable to NIST SRM-1920a, through direct comparison on the Metrohm master reflectance instrument, and in chemical formulation. In addition to the prescribed formulation, one additional ingredient is added, in a small amount, to provide peaks beyond those normally found in SRM-1920a.

  • Page 74: Ipv Setup (Instrument Performance Verification)

    NOTE: The response of the WSR Wavelength Standard may vary slightly with temperature. This is typically in the range a few hundredths of a nanometer for small temperature variations. While this effect is small, it may cause some variation when running Wavelength Certification. We suggest that the WSR standard be stored in the standards box, rather than inside the instrument.
  • Page 75 Vision requests a “Standard File”. This is provided on a mini-CD, packed in the wooden box with the standards. Insert this mini-CD into the CD drive, select that drive in the dialog box, and click on the RSS1xxxx.da file as shown. (The serial number will be different, of course.) Click “Open”.

  • Page 76: Evaluation Diagnostics

    Place the 99% standard into the tray. The label edge should be parallel to the long edge of the tray. This enhances repeatability. Once the 99% standard has been scanned, it is shown on screen. Note that the header identifies the standard just scanned. The dialog box prompts for the 40% standard to be scanned next.

  • Page 77: Performance Test

    discussion of the theory and interpretation of results is provided in the Vision manual. 7.2.1 Performance Test Performance Test is a comprehensive test of instrumental performance, and is the final assurance that the instrument is ready to run samples. The key items verified during this test are: •...
  • Page 78 This view shows the fill width of the tabulated results, and expands the spectrum for better viewing. When Performance Test is finished, a message box is displayed to indicate test completion and status. All measured values are compared with acceptance criteria stored in Vision. If all results meet acceptance criteria, the test is successful and this dialog box is displayed.
  • Page 79 Noise Summary displayed using the OpQual tab. The OpQual tab brings up the display shown. This shows results of the Noise Test for each of the four wavelength regions. These regions are: • 400-700nm • 700-1100nm • 1100-1700nm • 1700-2500nm For each region, results are given for •...

  • Page 80: Wavelength Certification

    The XDS instrument contains internal wavelength reference materials, which are used as a means 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.
  • Page 81 screen. A tabular report is shown in the lower right quadrant, giving each peak, its nominal position and its measured position. A typical screen is shown: Double-click the lower 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.
  • Page 82 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 the peaks are in correct positions, and that the peak positions are consistent over time.
  • Page 83 The wavelength peaks used here are not the NIST peak positions, though they are within +/- 1.0nm of the NIST peaks. The peaks used in Instrument Calibration are the peak positions used to assure transferability of the XDS instrument, and are defined based upon tests of many XDS instruments. Note that Performance Test measures peak positions of internal reference materials, and these positions are used as a preliminary method to maintain wavelength measurement.

  • Page 84: Photometric Test

    In some cases the user may see the message shown. This indicates that the instrument has passed Wavelength Certification on the NIST-defined peaks, but has not passed on the tighter, FOSS-defined wavelength positions. This is not considered a failure, as the instrument still passes Wavelength Certification on NIST-defined peaks.
  • Page 85 Vision requests a “Standard File”. For Photometric Test, use the RSSVxxxx.da file stored in the Vision directory. This file was created during IPV Setup. Current photometric readings will be compared to that initial file. Click on the RSSVxxxx.da file as shown. (The serial number will be different, of course.) Click “Open”.
  • Page 86 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 the reflectance value.
  • Page 87 After each standard is run, Vision plots the comparison for each wavelength area 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.

  • Page 88: Gain Test

    This shows tabulated results, at each of the three wavelengths. USP dropped this test requirement from General Chapter <1119> as of December 1, 2008. Metrohm does not recommend that this 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.

  • Page 89: Low Flux Test

    To start Gain Adjust, click on Diagnostics, then Gain Adjust. The instrument is connected and in communication for this to function. The view above shows a fairly typical MultiVial Analyzer. The gain program sets the internal reference paddle over the sample opening, and takes gain readings for both NIR and Visible regions. Gain Factor is a measure of signal amplification.
  • Page 90 From the Diagnostics menu bar, select Low Flux Test. Vision asks if the user wishes to use an external sample (standard) for the test. Click “Yes” to use an external 10% reflectance standard. XC-1010 Reflectance Standards contain a 10% reflectance standard (R101xxxx) which may be used for this test.
  • Page 91 Click on the tab marked “Summary” to see the summarized 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”...

  • Page 92: Instrument Maintenance

    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.

  • Page 93: Fan Filter Replacement

    8.2 Fan Filter Replacement The fan filter should be inspected at least monthly. (If installed in a dusty or dirty environment, it should be checked weekly or twice-weekly.) The filter is changed as follows: Open the door of the filter compartment. Grasp the upper fin as shown and gently pull.
  • Page 94 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: Lamp Replacement

    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 to rise from established values. Follow this procedure: Turn off Instrument power and unplug AC power cord from AC receptacle or supply.
  • Page 96 Grasp the lamp retaining ring as shown. Push inward slightly, and rotate clockwise (the top to the right; the bottom to the left) 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...
  • Page 97 7. With the lamp wires straight, lift the lamp retaining ring upward and off the lamp as shown. Discard this lamp immediately. Order a new lamp from your Metrohm distributor to keep for the next lamp change. Always keep a spare lamp in stock, to avoid last-minute emergencies.
  • Page 98 10. 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. 11. Orient the arrow upward as shown before locking the lamp retaining ring in place.
  • Page 99 13. When the lamp is properly locked, the assembly will appear as shown. Note the shoulder screws holding the lamp retaining ring. Verify that the arrow is in the “upward” position. 14. Install the wire terminals to the terminal strip as shown. There is no polarity. Place one wire to each terminal.
  • Page 100 Always keep a spare lamp in stock, to avoid last-minute emergencies. If you do not 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.
  • Page 101 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: Fuse Replacement

    8.4 Fuse Replacement Fuse Replacement is an unusual event, and usually is caused by some electrical fault. The electrical fault should always be investigated and repaired before fuse replacement. Once the fault is found and corrected, this procedure should be followed: Turn off power and unplug the instrument from AC power.

  • Page 103: Maintenance Log

    Remove old fuses from holder and discard. Install the new fuses as shown. Fuse Ratings: 5A 250 VAC, 5 x 20mm Slo-Blo (2) Required They clip in to the plastic holder, and should be positioned at the center of the holder. Close the fuse door fully.
  • Page 104 Maintenance Log tracks all instrument tests, 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: Validation Tools

    · User Application (Customer samples, limits detection, range of calibration set, calibration precision, and other factors.) Users have requested specific tools and techniques to achieve validation. Metrohm has provided the following tools to assist and expedite the task. Each item is described.

  • Page 106: Hardware Validation Tools

    9.1.1 Factory Instrument Test Guide and Results Every Metrohm instrument is factory-tested, using the same battery of tests provided for ongoing customer testing. Included with your instrument are results from Instrument Noise, Bandwidth, Wavelength Accuracy, Photometric Certification, and Wavelength Certification. These factory tests are performed under controlled, ideal conditions, and serve as an important baseline for all subsequent testing.

  • Page 107: Metrohm Nirsystems Master Instrument Program

    (yet complementary) techniques to assure consistency and accurate response. Full records of testing and calibration are logged and maintained on an ongoing basis. By maintaining a Master Instrument, Metrohm is able to track long-term response of field instruments, verify ongoing operational improvements to manufactured systems, and provide yearly re-calibration of NIRStandards used in Instrument Performance Certification.

  • Page 108: Cfr Part 11 Compliance

    Vision Spectral Analysis Software design process, per software “life cycle” requirements. The Part Number is AP- 0007, and is available for purchase through your Metrohm Distributor. Documentation begins with the original Functional Requirement Specification, Software Requirement Specification,...
  • Page 109 operational instruction This screen shows many of the setup items to be set by the System Manager for 21 CFR Part 11 Compliance. To access this screen, click on Configure, Account Policy. A 21 CFR Verification Document is available for users who wish to verify key features.

  • Page 110: Safety And Electrical Certification

    In the unlikely event of problems, contact Metrohm service or your local authorized Distributor. This equipment is to be used only for the purpose specified. If used for any other purpose, the protection provided by the equipment may be impaired.

  • Page 111: 11.0 Troubleshooting

    Recommendations are listed in logical order of occurrence wherever possible. When all recommendations 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.
  • Page 112 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. Instrument Fails Performance 1. Verify that reference paddle is visible in MultiVial Test.
  • Page 113 another part of the laboratory, or place it on isolated supports away from the XDS Analyzer. 4. Increasing noise in Performance Test may indicate a gradually failing lamp. Performance Test is very sensitive to any optical changes in the instrument, including noise caused by lamp issues.
  • Page 114 To check fan operation, cycle the Power Switch. Note if the fans come on for a short burst, approximately 25 seconds after power, the fans are operating properly. If these measures do not correct the problem, please contact Metrohm service. ▪▪▪▪▪▪▪...

  • Page 115: Lifting And Transporting The Metrohm Instrument

    12 Lifting and transporting the Metrohm instrument: Always separate the module from the monochromator (shown) before lifting or transporting the instrument. When the module is attached, raise this handle to separate the module from the monochromator. Slide the module away from the monochromator.

  • Page 116: Instructions For Multivial® Shipping Position

    12.1 Instructions for MultiVial® Shipping Position When shipping the MultiVial Analyzer, it is vital to set the sample carriage to the “shipping” position. The shipping foam should be installed. The movement to “Shipping Position” (formerly “Park Position”) must be done with the instrument “On”, Vision in the MultiVial project, and communication established between Vision and the XDS MultiVial instrument.
  • Page 117 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: Index

    13 Index Operating Systems ........11 Accessory Kit ..........23 Park Position ..........114 Bias ............. 77 Boat ........36, 41, 56, 112 Password ........15, 38, 106 Cell ..........35, 56, 70 Peak-to-Peak Noise ........77 CFR 21 ........7, 38, 103, 105 Performance Test 9, 58, 75, 76, 78, 81, 87, 93, Comments ........

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