NIRS XDS MasterLab Analyzer Manual 8.921.
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 MasterLab Analyzer Manual 8.921.
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 address given above.
Table of contents 1 2 3 4 5 6 7 Introduction to XDS™ MasterLab Analyzer .................................................................... 5 Site Readiness ................................................................................................................ 8 2.1 Temperature and Humidity ........................................................................... 8 2.2 General Environment .................................................................................... 8 2.3 Vibration...
8 9 10 11 12 13 14 7.1.2 Reference Standardization, Tablet Transmission .................................................... 76 7.1.3 Instrument Calibration, Tablet Transmission .......................................................... 79 7.1.4 IPV Setup, Tablet Transmission (Instrument Performance Verification) ................... 83 7.2 Evaluation Diagnostics, Tablet Transmission .............................................. 87 7.2.1 Performance Test .................................................
1 Introduction to XDS™ MasterLab Analyzer Thank you for selecting the XDS MasterLab 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 sections on Reference Standardization. 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 of constituents, or for comparison to a library of known materials, providing identification and qualification of materials.
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. 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.
2 Site Readiness Like most precision instruments, the MasterLab 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 MasterLab Analyzer is designed to work in ambient air temperatures from 40-95°F (4.535°C). Use the XDS Analyzer only in 10-90% relative humidity levels, non-condensing.
standard RJ-45 type cable, such as CDW #074092, available from CDW Computer Centers, Inc. The 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 MasterLab Analyzer dimensions are: • Width: 18.
3 XDS Instrument Connection The XDS instrument may be connected to the host computer in one of two ways: If the XDS Instrument will be used as part of a network, use the Network Connection method shown immediately below. If there are not enough active network ports near the XDS instrument, a hub or router may be used. This section assumes use of Windows® 2000, XP, or later versions of Windows Operating Systems. For computers using Windows 95, 98, or NT 4.
• The XDS instrument appears just like a network printer (or other peripheral device) on the LAN system. It generates no signals, and only responds when commanded by an authorized user, logged into Vision software. • This is the easiest connection method for XDS instruments. 3.2 Direct Connection, in a free-standing manner with no network connection This method allows users to connect to the instrument when there is no network present. In such cases, a “crossover cable” (provided) is used.
3. 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” (Machine Access Code) to later re-assign that same IP address whenever the XDS instrument is on the LAN. 4. 4.
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”.) • On the “Exceptions” Tab, click “Add Program”. • Select Vision from the list of programs – click on it. (Vision must be installed to appear on the list.
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. These are often called “enterprises”.
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.
1. Vision cannot see any instrument on the connection path. Click on the “down arrow” at the right side of the empty field to see if instrument(s) are shown. Solution: By expanding the field, Vision can display the instruments shown. Note that only the top instrument, Serial #3010-0878, is “Available”. Highlight it and click “OK”. 2. Vision still sees no instrument(s) after expanding the field. This indicates connection or network issues. Verify Cable Type: Verify correct cable type for hookup.
• 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: Verify these settings: • Obtain an IP address automatically • Obtain DNS server address automatically When finished, click “OK”.
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 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.
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”. This command resets the communication port, and allows Vision to “find” the instrument, if connected properly.
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. It may be necessary to contact your IT department for assistance with these issues.
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.
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 scratches or damage.
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 in section 3.0. 7 Close the outer cover of the instrument. Push gently to the final closed position. It should latch securely.
9 Lift the release handle on the monochromator and engage the module “catches” to the locking togs on the monochromator. (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.
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 communication from Vision to the XDS instrument. This is detailed in Section 6.0, Vision Software. This completes assembly of the MasterLab Analyzer.
5 MasterLab Analyzer Overview The XDS MasterLab Analyzer is designed for several types of versatile analysis, from tablet sampling, to vials, and other types of samples. Several types are illustrated: Tablet Sampling in tray, Transmission • Detector Selection: Transmission • Wavelength Range: 800-1650 nm • Spot Size: 9.5 mm • Aperture: Installed • Iris Adapter: Removed Various tray configurations are available. Custom tray sizes may be ordered.
Large Sample Cell, Reflectance • Detector Selection: Reflectance • Wavelength Range: 400-2500 nm • Preferred Spot Size: 17.25 mm • Aperture: Removed • Iris Adapter: Removed This cell is optional, for large samples. Vial Sampling in Iris Adapter, Reflectance • Detector Selection: Reflectance • Wavelength Range: 400-2500 nm • Preferred Spot Size: 9.5 – 17.25 mm • Aperture: Removed • Iris Adapter: Installed A centering iris is used to position the vial or sample cell on the sample window.
Transmission Reflectance Use Tray Use Tray Use for multiple tablets, scanning in transmission. Use for multiple vials and tablets, in reflectance. The default spot size (9.5mm) is appropriate for all transmission analysis with this instrument. See section 5.3. Default spot size is 17.25mm; adjust as required for the given sample. See section 5.4. Use Boat Use this setting with the optional “boat” for large samples. Use spot size 17.25mm See section 5.4.
5.1 Introduction to Tablet Analysis The MasterLab Analyzer is designed to provide sampling for trays of tablets, like that shown at right. This provides for a great degree of automation, and permits the operator to perform sample loading and other duties while one tray is being scanned by the instrument. This extends the usefulness of the instrument into a routine analytical tool, since no operator input is required, once the sample information is entered and the tray is in place.
that in tablet transmission, some sample positions are not available because the reference standard takes up one or two tablet positions. Vision will not permit selection of these positions when the Transmission detector is selected in the Data Collection Method (DCM). The 15mm (4x5) vial diameter is shown as an example: The setup screen for sampling is straightforward and easy to use. An example is shown: Step by step instructions are given later in this manual. Please see Section 6.
5.2 Creation of a Custom Vial Size Most users will work with one of the standard vial sizes (or tablet layouts) 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 Configure, Tray. At the Select Tray Dialog box, note that four sizes (vial diameters) are already loaded in Vision. NOTE: The spot size (set in the Data Collection Method) should be no larger than 80% of the vial diameter.
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 Diameter. Click on “Number of Vials”. Vision calculates the maximum number of vials per tray. IN this case, 8 may fit on the tray. Vision fills in the number of vials per row and column. Click “More”.
These dimensions are the center of each vial opening in the tray. Vision uses these coordinates to position each vial during sampling. 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.
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: Minimum Sample Diameter.* Scanned Sample Area Diameter (mm) Diameter (in.) Square mm Sq. Inches 9.5 mm 11.9 mm 0.47 in. 70.9 sq. mm 0.11 sq. in. 10 mm 12.5 mm 0.49 in. 78.5 sq. mm 0.13 sq. in. 11 mm 13.8 mm 0.54 in. 95.0 sq. mm 0.15 sq. in. 12 mm 15.0 mm 0.59 in. 113.1 sq. mm 0.18 sq. in. 13 mm 16.3 mm 0.64 in. 132.7 sq. mm 0.
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 dimension to verify sample size. Set spot size in the Data Collection Method (DCM) under “Spot Size” as shown.
To insert the sample tray into the instrument, note the round guides on the sample carrier. They are shown in this photo – the pencil points to the one on the right. The sample tray must be positioned over these pins and gently pressed down to the stops. If crooked, the tray cannot be positioned correctly. Care must be used in placing the tray on the pins. The Select Tray Dialog box must have the correct selection made. Click on “Use Tray” as shown. This selection activates the x-axis and y-axis motion.
1. Remove the black covers from the adjustment post on the instrument, and the adjustment screw packed with the standards tray. 2. Thread the adjustment screw onto the adjustment post. Tighten only slightly, until it cannot be turned easily. You should feel slight contact as the screw reaches its full end point. You may even observe the machined end of the adjustment screw as it nears the ball-shaped end of the Do not force the adjustment screw beyond this initial contact. 3.
5. The vertical post of the adjustment is marked in 1mm (about 0.040”) increments. The rotary knob is marked in 50 increments. One marking on the knob equals 0.01mm in vertical position. It takes two full rotations of the knob per marking on the vertical post. Therefore, to move the height upward by one marking on the post, rotate the knob two full turns CCW. One mark on the post equals 0.5mm. Set the height to be approximately 0.5mm (0.020”) above the height of the thickest tablet.
Once set, the height will remain constant, even when the transmission detector is moved to the storage position as shown. When rotated back to the working position, the height will be correct. When rotating the transmission detector, do not “force” it at either end of travel. The detector is held in position magnetically, and will “snap” into position as the magnets attract the striker plate. Note that the aperture should be in place (as shown) when the tablet transmission detector is used.
5.6 Universal Tablet Tray Part Number 3013-243-01 The XDS MasterLab® Analyzer is shipped with one “Universal Tablet Tray” which may be used for feasibility studies and low-volume studies on round tablets. The tray may also be used for tablets which are approximately round, however some light leakage may occur. It is important to prevent light leakage around tablets. Therefore a “mask” is provided, to minimize leakage around the top surface of the tablet.
of the Universal Tablet Tray. (Remember that spectral intensity changes somewhat with detector height.) Bore sizes (diameter), for tablet sizes A-D, are as follows: Tablet Size Small Tablet Bore Bore Depth, Small Tablet Large Tablet Bore Bore Depth, Large Tablet Through Bore A .270” / 6.85 mm .095” / 2.41 mm .313” / 7.95 mm .062” / 1.57 mm .170” / 4.32 mm B .360” / 9.14 mm .095” / 2.41 mm .375” / 9.53 mm .062” / 1.57 mm .250” / 6.35 mm C .412” / 10.46 mm .095” / 2.41 mm .446” / 11.
5.7 Tablet Tray Unloader Because tablets fit snugly in the tray, and may be difficult to remove, a device has been designed to make unloading easier. The Tablet Tray Unloader has small projections at each tray position which lift the tablet slightly, so it can be removed using tweezers or a vacuum lifting device. A Tablet Tray is shown in the foreground, with two rows of tablets inserted. The tablets are nearly flush with the top of the tablet opening. Removal would be difficult.
The vacuum lifting device is easily controlled by blocking or releasing the hole on the wand. Cover the hole to pick up the tablet. To release the tablet, uncover the hole and the tablet may be set down. The height of the projections may be set for the tablet type in use. For thin tablets, the screws (4) on the bottom of the tablet unloading tray may need to be screwed inward, to provide more lift. There is a jam nut on each screw. This nut may require loosening before adjustment.
When using the Iris Adapter, Vision provides a command to move the sample carriage to a neutral position, as shown at right. First, remove the vial, tablet, or standards tray. (This can be difficult once the sample carriage has moved to the iris position.) Click on the menu item “Send Tray to Iris Position”. Vision requests that the Iris Adaptor be removed, if it is in place. This prevents a collision between the sample carriage and any other items in the path.
When ready, and all interfering items are removed, click “OK” in this dialog box. When scanning stationary objects, the “Use Iris” selection must be clicked. (Stationary objects need not be moved across the sample window for averaging.) When “Use Iris” is selected, any choice of tray is ignored. (The selections will “gray out” after a moment.) Use the Iris Adapter for centering.
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. Take a reference scan, the take a sample scan of the material. NOTE: If acquiring vial spectra that will later be used with a vial tray, be sure to perform the Reference Standardizations as described for both “Use Iris” and “Use Tray” positions. This assures consistent spectra.
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.
A new project must be created. The “project” is used to store data and calibrations for a given type of analysis. Multiple projects may be used, to keep spectra, calibrations and other data separate and wellorganized. Assign the project some meaningful name, to make it easy to remember. For our purposes, we simply called this “masterlab”. No spaces are allowed – use the “underscore” instead. Vision will assign a Location.
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 instrument. Before connection, we wish to figure the “Project Options”. Click on “View Spectra”. The user is returned to the main screen of Vision.
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 Tablet, 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.
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 details on setting up a custom vial size. Please continue to Acquire, Connect.) Select Acquire, Connect to initiate communication with the instrument.
The instrument “selfidentifies” as an XDS system with the Tablet 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 in reflectance. Normally the beam size should be set for 80% of the vial diameter. For the 15mm vial, use a 12mm spot size. In Tablet Transmission (covered in a later section) the default spot size is 9.5mm.
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. Note that when the instrument is set up for both reflectance and tablet transmission work, there will be two Data Collection Methods (DCM’s) shown in this selection box. Vision will connect with the instrument, and may display a message that a reference is being acquired to determine instrument stabilization.
If a Reference Standardization does not exist for the selected configuration, Vision will display this message. The user should perform both Reference Standardization and Instrument Calibration, to assure good method transfer. As explained in the section on Reference Standardization, Vision stores two reflectance references, based upon whether the sample is scanned directly on the sample window, or on the vial (or tablet) tray which is raised from the sample window to allow free motion.
instrument operation. Please proceed to the next step. In tablet transmission, Vision stores yet another Reference Standardization, for the transmission reference. This is addressed in the section covering Tablet Transmission. 6.2 Use of Vial Dialog Selection Menu The MasterLab Analyzer is designed for automated scanning of multiple tablets or vials. Vision Software supports this feature, and permits the user to set up the system for each sample to be collected.
Note that the Vial Dialog box is also called when either of these actions is performed: 1. The user clicks on the “Sample” Icon, or 2. The user selects Acquire, Sample from the File menu bar. It is not necessary to acquire a reference first with the MasterLab 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” column. This brings up the product selection menu. Highlight the desired product, and press “Enter”.
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 that represents the vial position. The circle turns yellow (It 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”.
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 verify or change the Product ID. To do this, double-click on the vial position below the center of the circle. This shows the available products, with the selected product highlighted. If the user wishes to save a given sample to a different product, it may be set using this screen.
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 the Sample ID names exist in an Excel spreadsheet, highlight those names in the spreadsheet as shown at the right. 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. Click “File, Copy”.
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.) 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.
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” field. Enter comments, if applicable. No entry is required; this 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.
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”. At the beginning of this section it was explained that a DCM for tablet transmission comes up with a slightly different layout for the Vial Dialog box. It is shown below: Please note the “grayed out” positions at the upper left corner.
below, this is automatic. At the bottom of the Vial Dialog screen is a checkbox marked “Use Order”. If this box is checked, the MasterLab Analyzer will start with the sample marked “1” in the “Order” column, and proceed numerically upward through the order designated in the “Order” column. If this box is left unchecked, the MasterLab Analyzer will proceed from vial position 1, to 2, to 3, in numerical order of the physical vial position in the tray. Vision will ignore the “Order” column.
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 position to be changed. 2. Re-click and that vial’s “order” will be sent to the end of the sequence. 3. Because this may be difficult to achieve by setting one vial at a time, click on all vial positions, to turn them white.
This setting defines the number of sample spectra to be taken per reference scan. With multiple samples, it is cumbersome to take a reference scan for each sample spectrum, and very timeconsuming. Because it is not necessary to take a reference spectrum for every sample scan, Vision may use the same reference scan for a number of sample spectra. The default is “10”, as shown above. This means that on a tray of 20 vials, Vision will take an initial reference scan, then scan the first ten vials.
Use Iris: If the 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 Tablet mechanism. Failure to remove the Vial Adapter will cause an error to be reported in Vision.
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” dialog box.) The user should remove the tray. Vision will position the tray mechanism out of the way, to allow the sample cell to be inserted. When finished, the sample cell should be removed, and the tray re-inserted into the Tablet mechanism. Failure to remove the Sample Cell may cause an error to be reported in Vision.
7 Instrument Diagnostics, Tablet Transmission Vision provides diagnostics for instrument setup. These diagnostics 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. Before proceeding with a full explanation, it is important to change the instrument settings from reflectance use to tablet transmission use. Follow these steps: 7.
This is a method to adjust the instrument wavelength profile to an external, traceable wavelength standard. This feature must be used to assure method transferability. Use Window Correction (XDS only): This feature is used only with XDS Process instruments that operate with Transmission Pair probes. Do not select.
A new DCM screen will be shown. The “Method” name will be blank, and the “Detector” may be marked as “Reflectance”. Proceed with these steps: 1. Select “Transmission” for the detector. (It is highlighted in the DCM above.) This automatically sets the “Range” to the correct setting, 800-1650nm. 2. Enter a “Method” name. In this case we entered “MasterLab Transmission”. Note that the “Spot Size” defaults to 9.5mm. You may hear the spot size motor running once you accept this DCM and initiate a scan.
To verify this connection, the user may click on Diagnostics, Instrument Configuration. Note that the Amplifier Type is listed as “Transmittance”. This is the correct setting for tablet transmission work. Click on “OK” to exit this screen. When scanning tablets in transmission, an aperture is required. This aperture is magnetically held on the sample deck, and is located with two short “pegs” that insert into openings machined in the deck. Clean the sample window if needed.
It is easier to install the aperture when the sample carriage is in the “Iris Position”. The unit may be in this position from previous work – if so, simply install the aperture. If needed, use this menu command to move the sample carriage to a backward position for easy insertion of the aperture. The tablet transmission reference is shown installed at right. It is attached to the frame of the sample carriage with a captive screw through the black frame. It must be used for tablet transmission work.
To re-install the tablet transmission reference, mount it onto the rail as shown, and screw down the captive thumbscrew about 4-5 turns. Do not over-tighten, or use any tools to tighten it. The thumb screw should only be hand-tight, and lightly so. The thumbscrew is machined to accept a #1 Phillips screwdriver. This is for removal only, if the thumb screw has been over-tightened. The tablet transmission detector must be moved to the correct position for tablet scanning.
The directions that follow include spectroscopic calibrations, which are used to “normalize” the instrument, to minimize differences between units of the same configuration. The programs are accessed from the Diagnostics menu bar, shown at right. The diagnostic steps are explained in the sections that follow. Vision uses a transmission instrument reference that is similar in absorbance to tablets of medium thickness.
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 Linearization from the Diagnostics menu. The instrument will scan the correct instrument reference. The results screen shown above is typical.
If Wavelength Linearization fails for any reason, check these items: • Tablet Transmission Detector in correct position • Tablet Transmission Reference in position on the sample carriage • Aperture in place • Instrument cover closed during scanning If any of these items needs correction, please set it properly and continue with the test. 7.1.
When Vision first communicates with the instrument (or after disconnection and re-connection) this screen is shown. Vision must 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. Click “OK to accept the instrument identification. Vision prompts the user to insert the Tablet Transmission Standards tray. Click “OK” to command Vision to position the instrument tablet transmission reference.
Vision plots the measured difference between the instrument tablet transmission reference and the certified standard in the Transmission Standard Set. This is plotted in light blue. This spectral difference is quite small. The small difference assures precise measurement of the instrument tablet transmission reference as compared to the calibrated reference in the Standards Set. Click on “OK”. Vision plots the spectrum of the calibrated standard in red.
Vision plots the spectrum of the final corrected reference spectrum in dark green. This spectrum should appear exactly the same as the calibrated standard spectrum (red) which was shown in the second screen. This view also shows the unused wavelength area on either side of that correction. Vision notes that Reference Standardization has been successfully performed. Click on “Print” or “Close Report”.
From the menu bar, click on Diagnostics, then Instrument Calibration. Vision requests that the aperture and Tablet Transmission Standard Tray be inserted, and that “Use Tray” be selected from the Configure, Tray menu. These items are reviewed below. Be sure to select “Tablet Transmission Standard” as the tray type. Click “Use Tray” and “Select”. If all items have been done, and the tablet transmission instrument reference is in place, please click “OK”.
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”. The file may be loaded into the C:\Vision directory, and recalled from that location. Vision acquires another instrument reference. Vision prompts the user to insert the Tablet Transmission Standard Tray into the instrument. Insert the tablet standards tray into the sample carriage when prompted. (If this was not already done.) Click “OK” to continue.
At the end of the test this dialog box is displayed. Print confirmation of test results if needed for a log book or other file. Click “Print” to document the successful completion of Instrument Calibration. This is the report from Vision to document completion. Click “OK” to exit Instrument Calibration. During Instrument Calibration, the wavelength response for each defined peak is adjusted, to assure precise wavelength registration between instruments.
to illustrate that the wavelength peaks of SRM-2035 remain constant, even when neutral density filters are added to increase absorbance level, as with the top spectrum. The SRM-2035 peaks are consistent even at higher absorbance levels. The XDS master instrument is verified as meeting NIST SRM-2035 nominals during Instrument Calibration, since these are the best known information for NIR transmission peak wavelengths.
under Configure, Options. That is, if the IPV Setup file is acquired with Reference Standardization switched on, and with Window Correction switched off, then Photometric Test should be performed using the same settings. The System Manager should pay particular attention to this. If options are not consistently applied, there will be a bias in the results of Photometric Test. The bias may be enough to cause test failure, depending upon selections.
Vision verifies the tray type – select the Tablet Transmission Standard, as highlighted. Verify “Use Tray”. Click on “Select”, then “Close”. Vision prompts the user to insert the Tablet Transmission Standard Tray into the instrument. Click on “OK”. Vision verifies the standards as shown in the Vial (Tablet) Dialog box shown. The active Tablet Transmission Standards are highlighted in yellow.
Vision takes an instrument reference. 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. Next, the T02 standard is displayed. Each standard spectrum will be displayed, until the test is complete. When the last standard is scanned. Vision indicates that IPV Setup has “Passed”. This verifies that the correct file has been written to the active Vision directory.
7.2 Evaluation Diagnostics, Tablet Transmission Evaluation Diagnostics are used to verify that the instrument is operating within allowable parameters. These tests should be run approximately once per week, or according to your company procedures. This information is meant to guide the user through the tests in an expeditious manner. A more complete description of these tests is given in the Vision Manual, in the Diagnostics section.
Because only the right two quadrants of the screen will be updated, many users “pull the screen over” to see better, as shown on the next page. This view shows the full width of the tabulated results, and expands the spectrum for better viewing. This test is not yet finished. It is on the 7th set of scans, out of ten.
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. 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.
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 nominals are arbitrary. The internal wavelength materials are a method to assure stable readings on the external wavelength standard, measured at the sample plane.
Vision asks the user to select the Standard File. This file is on the mini-CD, as shown. This file may be copied into the C:\Vision directory for convenience. The user is prompted to insert the Tablet Transmission Standard Tray. Place the tray in the instrument as shown, or verify that it is already in place. Close the cover and click “OK” to proceed. Vision begins a scan of the reference. When the reference scan is finished, Vision prompts for the wavelength standard. Click “OK”.
Double-click the lower right quadrant to see the full report. The first tab shows the Wavelength position, as found. Only one is used with this detector, which is very linear and predictable in response. The peak position is compared to the nominal peak position as identified on an instrument calibrated using NIST SRM-2035. The difference from nominal, and the repeatability of position are calculated. The acceptance specification is +/-1.0nm.
Note that the peak position is shown only to two digits after the decimal point. Any further digits are not considered significant, and are therefore not displayed. Wavelength Certification also tests certain “measured instrument profile” 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.
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. Verify that the instrument is fully warmed-up. If so, and this test still fails, re-run Instrument Calibration to set the peaks to proper positions.
Vision requests a “Standard File”. For Photometric Test, use the TSSVxxxx.da file stored in the Vision directory. This file was created during IPV Setup. Current photometric readings will be compared to that initial file. You may need to change the file type to display the file, as shown. Click on the TSSVxxxx.da file as shown. (The serial number will be different, of course.) Click “Open”. Do not use the file on the standards mini-CD for Photometric Test, as it will cause Vision to return an error message.
Vision displays the wavelength regions for test. For tablet transmission, these regions give a good overall picture of instrument performance and repeatability. The wavelength areas are chosen in flat parts of the standards spectra for stability. For Number of Replicates, the default setting is 1. Click on “OK”. Vision will begin to take an instrument reference scan. The red progress bar at the bottom of the screen indicates status.
Vision verifies the tray layout as shown. Click on “OK”. Vision acquires a reference scan. Next, the T02 is scanned. It is reported at right. Vision continues with each standard in the set. In the upper set of spectra, 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 in the middle (red on screen) is the current spectrum.
When all standards are scanned, results are posted as shown. When Vision has completed the test, the tabulated results may be printed. They are also stored in the Diagnostic Database for later recall. There is a tab marked “USP Test”. Click on this tab to see the USP-suggested plot and summary report. These are shown on the next page. (This test is not required as of 121-2008.) When the test is complete, click “Print Results” for a hard-copy report. Click “Close Window” when finished.
The four standards are plotted out in the USP format, showing repeatable response for each standard. The x-axis, A REF, is from the initial observation (during IPV Setup). The yaxis, A OBS, is the current observation. The slope must be 1.0, +/- 0.05. The zero intercept must be 0.0 +/_0.05. The box shows the results for this observation. Tabs allow the user to check at two wavelengths: 1200 and 1600nm. Click on the Photometric Linearity Test Results tab to return to the tabular information.
The view above shows Transmission gain on a typical MasterLab Analyzer. The gain program measures amplifier gain factor and voltage through the Tablet Transmission Reference. Gain is reported for NIR, since this detector does not provide separate voltages. While VIS gain is reported, it is a function of NIR gain and can be ignored. Gain Factor is a measure of signal amplification. Gain ranges from about 4000 to 400,000 in normal use. Gain Adjust can be helpful when troubleshooting an instrument.
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 “No” to use the internal 10% screen, combined with the 2 AU Reference. This is roughly 3 AU, or the overall absorbance of an average small tablet. Vision runs the Low Flux Test, which takes about 10 minutes. At the end, the results are displayed. Vision applies specifications for the T05 standard.
8 Instrument Diagnostics, Reflectance 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 for these diagnostics, as small round sample cells are used. See section 5.6 for instructions on how to install the Iris Adapter. 8.
Use Window Correction (XDS only): 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 on a regular basis to maintain calibration. These calibrations should be run when indicated by Photometric Test (Reference Standardization) or Wavelength Certification (Instrument Calibration.).
minutes, depending upon whether the instrument has been off, or if the transmission detector was used previously. Once Vision shows the instrument as stable, proceed with tests. 8.1.1 Wavelength Linearization, Reflectance Wavelength Linearization uses an internal wavelength material set to determine a set of internal, arbitrary peak positions that the instrument will use to maintain repeatability of wavelength response. The NIR wavelength positions of these peaks appear as shown.
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. Click “OK” to proceed. 8.1.
Reference Standardization. The benefit of this system is that only one calibration (or library) is required, and serves both sampling levels. (Without this system, two sets of calibrations (or libraries) would be required for operation.) Vision software stores the Reference Standardization files, which are downloaded to the instrument, and are applied as a correction to each spectrum. (Vision knows which file to use based upon selection of the “tray” in the Select Tray Dialog box.
When Vision first communicates with the instrument (or after disconnection and reconnection) this screen is shown. Vision must 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 plots a spectrum of the ceramic instrument reference, as shown. (The spectrum will be light blue 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.
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 as the Certified 80% Reflectance Standard. Click “Close Report” to continue. The correction is automatically downloaded, and is saved in the Diagnostic Data Base.
8.1.3 Reference Standardization, Reflectance, “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.
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. Vision requests that the Certified 80% Reflectance Reference Standard be placed in the sampling area.
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 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 as the Certified 80% Reflectance Standard. Click “Close Report” to continue. The correction is automatically downloaded, and is saved in the Diagnostic Data Base. The correction will be applied in real time to all spectra taken – in the “Use Iris” mode --with a DCM where “Reference Standardization” is checked.
8.1.4 Instrument Calibration, Reflectance Instrument Calibration uses a NISTtraceable, 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. Vision performs an algorithm to set the peak positions of the instrument to those of the standard.
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. Use the tray provided for this purpose. Insert the standard with the label parallel to the long axis of the tray. Click “OK” to continue. This test takes about 45 seconds.
Information about the reflectance wavelength standard: 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. This material has very sharp bands, which are found to be stable and repeatable.
8.1.5 IPV Setup, Reflectance (Instrument Performance Verification) IPV Setup is provided as a method to record initial instrument response to calibrated photometric reflectance standards. This is normally performed upon initial installation, immediately after Instrument Performance Certification (IPC), when a lamp has been changed, or when standards have been re-certified. When the standards are scanned during IPV Setup, a file is generated, and is stored in the Vision directory.
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”. The standard file is “NSAS File” format, which refers to an older software package. This format is used where it aids in file transfer. For Number of Replicates, retain the default setting of 1. Click on “OK”.
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. Insert the 40% standard, and click “OK”. Continue through all standards (99, 40, 20, 10 and 2%) as prompted by Vision. When the last standard is scanned.
8.2 Evaluation Diagnostics, Reflectance Evaluation Diagnostics are used to verify that the instrument is operating within allowable parameters. These tests should be run approximately once per week. This information is meant to guide the user through the tests in an expeditious manner. A more complete description of these tests is given in the Vision Manual, in the Diagnostics section. A discussion of the theory and interpretation of results is provided in the Vision manual. 8.2.
Because only the right two quadrants of the screen will be updated, many users “pull the screen over” to see better, as shown on the next page. 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.
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 • 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.
8.2.2 Wavelength Certification, Reflectance Wavelength 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. Click “OK” when ready.
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. The difference from nominal, and the repeatability of position are calculated. Wavelength Certification also tests certain “measured instrument profile” peaks in the wavelength standard.
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. Note that both tests use the wavelength standard at the sample plane, where actual sample measurement is done.
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.
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 exceed normal tolerance values, the instrument can be assumed to have changed in some manner, and may need service.
Vision displays the wavelength regions for test. For reflectance instruments, these regions give a good overall picture of instrument performance and repeatability. The wavelength areas are chosen in flat parts of the standards spectra for stability. For Number of Replicates, retain the default setting of 1. 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.
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 in the middle (red on screen) is the current spectrum.
The five standards are plotted out in the USP format, showing repeatable response for each standard. The x-axis, A REF, is from the initial observation (during IPV Setup). The y-axis, A OBS, is the current observation. The slope must be 1.0, +/- 0.05. The zero intercept must be 0.0 +/_0.05. The box shows the results for this observation. Tabs allow the user to check at three wavelengths: 1200, 1600, and 2000 nm. Click on the Photometric Linearity Test Results tab to see the tabular information.
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 MasterLab 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. In the NIR region (1100-2500nm) it occurs in steps of 1, 2, 4, 10, 20, 40 and 80.
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. The 10% reflectance standard should be positioned in the tray as shown. The label should be parallel to the long edge of the tray.
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” to complete the test.
9 Instrument Maintenance Instrument maintenance is quite simple on the XDS MasterLab Analyzer. The optical enclosure is sealed to prevent contamination of critical parts, which keeps maintenance to a minimum. A diagram of the internal parts is shown, primarily for user information. 9.1 Overview DO NOT attempt to open the optical enclosure. There are no user-serviceable parts inside. Damage is not covered under warranty. FANS Power Supply, Circuitry, Connectors, Etc.
9.2 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.) We recommend that instrument power be turned off before changing the filter. The filter is changed as follows: Turn off power at the power switch located on the back panel. The power cord may be removed for easier access to the filter, if desired.
Using the new filter material, gently insert it into the filter cover. It should fit easily in any direction, as it is symmetrical. Be sure the filter material is positioned correctly, and is not wrinkled or folded. There should be no gaps at the edges. Starting at the top, snap the frame into place. When all four snaps are in place, the face of the filter frame should be parallel to the back plate of the instrument. When finished, re-install the power cord if removed earlier.
Turn off power at the power switch located on the back panel. Unplug the power cord. While this is not essential, it makes access easier. Remove the communications cable too. Loosen the six (6) captive screws which hold the back cover in place. These should only be handtight. If the screws are too tight, use a Phillipshead or flat-bladed screwdriver to loosen them. Back the screws out as far as they will go, to release the back plate. Do not attempt to remove the captive screws from the back plate.
This orientation photo shows the area inside the back cover. The lamp box is at the lower left. The fan and heat sinks, shown to the right of the lamp box, are used to cool the instrument. No maintenance or adjustment should be done on these items. If the lamp is still warm, give it several minutes to cool. It may be hot enough to cause burns – this should be avoided. The lamp box contains the lamp terminals at the upper right, and the lamp itself, held in a quickrelease holder.
Gently grasp the corners of the lamp mounting plate. Push in about 1mm, then rotate clock-wise (to the right) about 5 mm. The lamp mounting plate should then be pulled outward from the mounting studs. When the lamp mounting plate is free of the studs, lift the lamp and plate assembly out of the lamp box as shown. As a precaution, the lamp may be held by the wires at this point, to avoid the hot lamp housing and reflector. Lift the lamp mounting plate up over the ends of the lamp wires and remove it.
Position the lamp with the black arrow up as shown. Gently insert the lamp and mounting plate into the lamp housing as shown. Engage the holes over the studs. When all three are in place, rotate the mounting plate counterclockwise (to the left) until they all lock in position. Verify that the black arrow on the lamp is aligned with the machined groove in the lamp housing. If not, gently rotate the lamp to get it into alignment. This is required for proper operation of the instrument.
Carefully re-install the back cover, lining up the captive screws with the mating threaded holes. Tighten gently by hand. Do not over-tighten as the screws tend to become tighter over time. Do not use a screwdriver, as this will make the screws very difficult to remove at a later date. When finished, re-install the power cord if removed earlier. Re-install the communications cable as well. Instrument power may be turned on. Turn the power switch to the ON position.
Perform tests as specified in the prior sections of this manual. These normally include the following: • Wavelength Linearization • Performance Test • Reference Standardization (if applicable to this model) • Instrument Calibration The spare lamp may come with generic instructions for instrument testing. Use the instructions in this manual to test the instrument, as this manual overrides all instructions packed with the lamp. Immediately contact your Metrohm distributor to order a new spare lamp.
Remove the power cord for access to the fuse. Use a tool (such as an Allen wrench) to pull the housing open. There is a small slot, underneath the fuse door and in the center, where the tool can be inserted to pry the door gently open. 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 The new fuses clip into the plastic holder, and should be positioned at the center of the holder. Close the fuse door fully.
When finished, re-install the power cord. Turn on AC power and re-establish instrument communication. 9.5 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 userentered comments. To access the Maintenance Log, click on Diagnostics, Maintenance Log, then the correct selection. Maintenance Log tracks all instrument tests, as shown in the screen below.
This screen shows entries, sorted by record number. To re-sort by another parameter, click on the column heading. 9.6 Window Cleaning The sample window should be inspected and cleaned frequently. Dirt, dust and sample carry-over on the window can affect analytical results. Cleaning may be performed at any time, even when the instrument is operating, and between samples if needed.
After cleaning, allow any residual alcohol to evaporate off. Then use the sample brush from the accessory kit to gently brush away any lint or dust from the sample window. Repeat this as often as needed to keep the window free of dust and contaminants.
10 Validation Tools Validation is an overriding concern in the pharmaceutical marketplace. In the United States, manufacturers must follow Title 21 of the Code of Federal Regulations, also known as CFR 21. Each country has its own regulations or has adopted a set from another source; therefore, the requirement for validation is worldwide. The requirements are very detailed, and will not be recounted here.
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. Test results are included for each module or configuration ordered. These test results are included in an informative brochure that explains the tests, what they measure, and how they relate to instrument performance.
Independent assessment, not performed by instrument user • Meets independent test requirements of CFR 21 and most auditing methods. Full documentation of all tests, adjustments and findings • Serves as Instrument Log, with valuable records of ongoing performance. Metrohm NIRSystems Master Instrument Program In support of our worldwide base of instruments, Metrohm maintains a Near-Infrared Master Reflectance Instrument.
the pharmaceutical industry. Documents were selected (from the enormous quantity of records in our logs) based upon the patterns set during the many customer audits of our software development process. Documents may be printed using Adobe Acrobat®, which is included on the CD for download. This CD is the most comprehensive, informative record of software validation anywhere in the industry today.
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 in Vision, 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.
11 Safety and Electrical Certification The XDS MasterLab Analyzer and all associated components have been tested for CE (Communite European) certification. An independent, accredited laboratory is used for this testing. CE certification is a comprehensive set of requirements that encompass user safety, immunity from electrical interference, and low radiated electrical emissions. The requirements overlap with UL and CSA requirements in nearly all areas.
12 Troubleshooting The XDS MasterLab Analyzer is a dependable, trouble-free instrument, designed for many years of service in your laboratory. In spite of the rugged design, problems may arise that require attention. This guide is intended as a means of diagnosing minor problems. There are no user-serviceable parts inside the instrument enclosure. Because of this design, we emphasize that under no circumstances should the user attempt to open the instrument cabinet and service any part.
1. Verify that the RJ-45 cable is plugged in at both the instrument and at the network wall jack. 2. Verify that the RJ-45 cable is plugged in at both the computer and at the network wall jack. (NOTE: Direct connection is explained in section 3.0 for non-network users. This requires a “crossover” cable as supplied. 2 No communication between Vision and the instrument. 3. Verify that the instrument is powered on. (See previous Observed Problem.) Note front-panel LED indicators. 4.
1. Upon successful connection, the instrument “lost track” of which amplifier was last in use. This may happen when changing computers, or under conditions of improper disconnection. (This is being investigated and addressed.) 3 If in a transmission DCM, switch to a reflectance DCM, then back to the transmission DCM. If in a reflectance DCM, switch to a transmission DCM, then back to a reflectance DCM.
1. Instrument Reference is not in correct position. Verify that reference paddle is visible in MasterLab Analyzer sample window when a reflectance reference scan is taken. 5 Instrument fails Wavelength Linearization 2. MasterLab, transmission: The tablet transmission reference may not be in position, the detector may not be in the “lowered” position, or the instrument beam may be blocked. Correct these conditions and re-try. 3.
1. Verify that the Wavelength Standard is properly positioned in the holder when prompted by software. 7 Instrument fails Instrument Calibration. 2. Verify that the Windows or WINNT directory (on the C:\ dive) contains a file named “Sys3.ini”. This file contains parameters needed in Instrument Calibration. If this file is not located in the directory, Vision may not operate correctly in Instrument Calibration. The installer and user must have proper permission to this directory when Vision is installed.
1. Verify that air intake on side is not blocked by other equipment. Leave at least 3-4 inches (76102mm) space by intake fins for proper airflow. 9 Instrument cooling fans are operating at maximum rate. 2. Verify that air filter is clean. If not, clean or replace filter. If fan speeds dropped shortly after opening fan filter door, this is a sign of a blocked filter. 3. Verify that the fan exhaust area is not blocked, restricting the fan outflow.
12 X-Y Sampling Mechanism crashes into Iris Adapter, causing Limit Switch Error Remove Iris Adapter. Click “Use Iris” in Vial Dialog box. Vision will re-acquire the home position of the X-Y mechanism, and will be ready to operate. Re-install the Iris Adapter. 13 Sampling Mechanism does not move when using large sample cell Click “Use Boat” in Vial Dialog box. 1. Instrument may not be warmed up. Fans do not operate until the instrument is near operating temperature.
Auto Linearization is a program to maintain correct wavelength position of the instrument. When this error is reported, it may be due to one of the following reasons: Vision reports “Auto Linearization failed” 16 17 1. In tablet transmission, the beam may be blocked. 2. The tablet transmission reference may not be in place. 3.
13 Lifting and transporting 1 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. The monochromator is the heavier component. Instructions follow. 2 When lifting the monochromator, place arms on either side of unit as shown. Lift with the knees, not with the back! Lift unit up, move to a cart, and lower gently.
13.1 Instructions for MasterLab® Shipping Position When shipping the MasterLab 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 MasterLab project, and communication established between Vision and the MasterLab instrument.
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.
14 Index Accessory Kit 21 Aperture 26, 27, 76 Assembly 21, 46 Auto-Linearization 50, 68, 102, 155, 160 Bias 89, 122 Boat 28, 50, 66, 159 Cell 27, 67, 115 CFR 21 6, 47, 147, 148, 149 Comments 61, 65, 67 Configure 14, 15, 31, 48, 49, 50, 52, 66, 67, 68, 72, 73, 80, 84, 102, 117, 151, 154, 155, 158, 159, 160, 162 Connect 16, 20, 27, 51, 69, 103, 155 Crossover Cable 8 Custom Vial Size 31, 51 Data Collection Method 30, 31, 33, 35, 51, 69 Database 53, 77, 93, 94, 98, 100, 101, 107, 126, 129, 131, 133, 144 Detecto
Vibration 8 Voltage 160 Wavelength Certification 69, 83, 90, 93, 94, 103, 116, 118, 123, 124, 125, 148 Wavelength Linearization 74, 75, 76, 80, 104, 114, 156 Wavelength Standard 81, 82, 115, 116, 157 Weight 9 Width 9 Window 69, 84, 98, 103, 117, 129 Windows Operating Systems 10 â–Şâ–Şâ–Şâ–Şâ–Şâ–Şâ–Ş 165
