NIRS XDS RapidContent 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 RapidContent 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.
Inhalt 1 2 3 4 5 6 7 Introduction to XDS™ Rapid Content 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 7.2.5 Low Flux Test ....................................................................................................... 61 Instrument Maintenance .............................................................................................. 64 8.1 Overview .................................................................................................... 64 8.2 Fan Filter Replacement............................................................................... 65 8.
1 Introduction to XDS™ Rapid Content Analyzer Thank you for selecting the XDS Rapid Content 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 Rapid Content Analyzer also offers variable spot size, to focus energy on small samples. This feature is standard on the Solids Module. 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.
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. There is no airflow drawn into the optics chamber instrument.
2 Site Readiness Like most precision instruments, the Rapid Content 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). Use the XDS Analyzer only in 10-90% relative humidity levels, non-condensing.
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 Rapid Content Analyzer dimensions are: Width: 18.0” (457 mm) Height: 15.25” (387 mm) Depth: 22.
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.
hacking or support of viruses is possible with XDS instruments. • 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.
can only be entered by an authorized user, using the “two-token” method of entry. (Unique User ID and password) 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.
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.
• 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”. Close all other boxes opened for this verification.
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.
assistance with these issues. First, verify the following: • The instrument is free-standing not connected to a network with DHCP server • There is only one network card in the computer • A crossover cable is used between the XDS instrument and the computer If these conditions are met, please proceed. Direct Connection Solution 1: If using a crossover cable, verify that the computer is communicating in the same IP range as the XDS instrument. The XDS instrument default IP address is 169.254.0.
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 Rapid Content Analyzer.
5 Rapid Content Module The XDS Rapid Content Analyzer is designed for sampling of many types of customer samples. This section covers use of the sample cell, use of the moving sampling mechanism, and spot size adjustment. 5.1 Sample Cell The sample cell operates in a horizontal orientation, to avoid spills of powder or pellets into the sampling chamber. The purpose of this cell is to expose a large amount of surface area (of the sample) to the instrument.
2. Do not pack, unpack, or open the sample cell in the sampling chamber. This could spread sample material into the sampling chamber, which may coat the sample window and affect the analysis. 3. The sample cell holds approximately 250ml (8-1/3oz.) of sample material, when completely filled. Exact volume of sample depends upon sample shape, packing density, and “settling” over time. 4.
A ball catch (one on each leg) is used to hold the sample cell in the correct position on the Sample Carrier. Be sure the sample cell is held by the ball catch at each end. Close the door of the sample chamber to exclude ambient light. The Data Collection Method (DCM) should be configured for a moving sample, as shown in the screen at right under “Cell:” This assures that the sample will be moved across the sampling window to accumulate as much spectral data as possible.
5.2 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. This is completely under control of the instrument, and requires no input from the user. The information to activate this feature is taken from the Data Collection method (DCM) when set up by the user.
self-cleaning, and requires no service of any kind. The lead screw is stainless steel, and needs no service. There are no user-serviceable parts in the mechanism. It has been aligned and set for quiet, stable operation. Please be gentle, and do not attempt to make any adjustments. Removal of Sample Carriage: The Sample Carrier may be removed when normal round sample cells are used. This is required for Reference Standardization and Instrument Calibration.
Installation of Iris Adapter: The Iris Adapter is used for round sample cups, beakers, vials, and other stationary samples. The Sample Carrier must be removed before installation of the Iris Adapter. Align the holes in the Iris Adapter with the pins on the sample platform, and carefully lower into place. The pins hold the Iris Adapter securely in position over the sample window. Use the adjustment to open the iris as needed.
The Rapid Content Analyzer may also be used for liquid analysis using the Reflectance Cell and Immersion Diffusers. These are often used for clear to semi-clear liquids such as alcohols and suitable fluids. Removal of the Iris Adapter and re-installation of the Rapid Content Analyzer Sample Carrier is quite straightforward. Simply remove the Iris Adapter Assembly, and re-install the Sample carrier onto the locating pins. Re-install the thumbscrew and tighten hand-tight.
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.
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. Install Vision on the computer to be used for instrument operations.
Vision asks if the default directory location is acceptable. Click on “Yes”. Vision creates a directory for the project as shown. Vision prompts the user to connect to the instrument. Be sure the instrument is turned on and is ready. Click on “Acquire New Data”. This screen sets up communication parameters for the instrument. The XDS instrument has a unique driver. Highlight this box and click on “Configure”.
A Data Collection Method (DCM) must be established to communicate with the instrument. There are no Data Collection Methods available upon initial connection. Click on “New”. The instrument “self-identifies” as an XDS system. Depending upon the configuration, the DCM will self-select as either a Rapid Solid Module or a Rapid Content Module, with or without spot size adjustment. Select the proper module for your type of system. The user should enter a logical name for the DCM.
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 Upon connection, Vision will prompt for the instrument configuration. This is used to establish a Diagnostic Database. It is important that the instrument be correctly identified, to prevent corruption of the database. If only one instrument is in use, accept the information and click “OK”.
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 for these diagnostics, as small round sample cells are used. See section 5.
Instrument matching (method transferability) requires that Reference Standardization and Instrument Calibration be selected, and that Certified Standards are used when required to maintain calibration. These calibrations should be run when indicated by Photometric Test (Reference Standardization) and Wavelength Certification (Instrument Calibration).
These peak positions are not meant to be traceable, as the wavelength calibration of the instrument is done on an external standard, traceable to NIST. The internal wavelength standards 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 ceramic reference. The results screen shown above is typical.
enhance model transferability between instruments. A photometric standard of known reflectivity (as measured on an absolute reflectance scale) is scanned on the instrument. The internal ceramic standard is scanned. The differences of the ceramic standard from 100% reflectivity are mapped, and a photometric correction is generated. This correction is then applied to every spectrum taken on the instrument, to make each spectrum appear as if taken with a reference of 100% reflectance.
Vision requests the “Standard File” for the Certified Wavelength Standard. Place the mini-CD into the CD drive, and select the standard file. Click “Open”. Vision requests that the Certified 80% Reflectance Reference Standard be placed in the sampling area. Place the standard as shown, with the identifying label parallel to the long axis of the tray. Close the cover, and click on “OK”. 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.
7.1.3 Instrument Calibration Instrument Calibration uses an 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 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.
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.
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 A: 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. Vision displays the wavelength regions for test.
Select the requested standard from the set. Labels on the back identify each standard. Note the mini-CD that contains the “Standards File”. This file is used only during IPV Setup. 7.2 Evaluation Diagnostics 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.
At the end of Performance Test, 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. Before clicking “Close All Reports”, the user is directed to the tabular display. To view the tabular display of results, place cursor over the tabular display and double-click twice. Vision enlarges the tabular portion of the screen. Now click on the OpQual tab, near the bottom of the screen.
Noise Summary 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.
When the reference scan is finished, insert the wavelength standard as directed. Always place the standard into the instrument in the same orientation, with the label parallel to the long axis of the mounting plate. Click “OK” when ready. After the test is complete, a spectrum of the standard is shown in the upper right quadrant of the screen. A tabular report is shown in the lower right quadrant, giving each peak, its nominal position and its measured position.
The 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. These peaks are used to set the “Instrument Wavelength Profile,” and one peak is used for bandwidth calculation.
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. Wavelength Certification is an excellent method to test whether Instrument Calibration needs to be re-run.
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 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”. Do not use the file on the standards mini-CD for Photometric Test, as it will cause Vision to return an error message. Vision requests a tolerance file.
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. When the 99% standard has been scanned, the result will be plotted as shown.
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. When Vision has completed the test, the tabulated results may be printed. They are also stored in the Diagnostic Database for later recall. When the test is complete, click “Close Window”.
The view above shows a fairly typical Rapid Content 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. In the Visible region (400-1100nm) the gains range from 1 to 80,000. 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 “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 over the sample window, and centered using the iris adapter.
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.
8 Instrument Maintenance Instrument maintenance is quite simple on the XDS Rapid Content 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. 8.1 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.
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.) 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. 8.5 Maintenance Log Vision provides a Maintenance Log in the Diagnostic Database to permit tracking of maintenance activity. This provides a convenient place to find information about tests, lamp changes, and 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. 8.6 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.
9 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.
9.1 Hardware Validation Tools 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.
• Meets CFR 21 requirements for instrument qualification. 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.
At over 2000 pages, this CD will satisfy your Internal Audit Staff and external regulators that Vision Software was designed from the first moment to be a fully code-validated, tested product for use in 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 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. 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.
10 Safety and Electrical Certification The XDS Rapid Content 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.
11 Troubleshooting The XDS Rapid Content 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 nonnetwork users. This requires a special cable. 2 No communication between Vision and the instrument. 3. Verify that the instrument is powered on. (See previous Observed Problem.) 4.
1. Verify that reference paddle is visible in Rapid Content Analyzer sample window when a reference scan is taken. 2. Temperature and/or humidity may be changing rapidly during the test. This can usually be observed as large spectral activity between 1300-1400nm and 1800-1900nm. If this is the case, the instrument should be tested in a more controlled setting to verify proper operation. 5 Instrument Fails Performance Test. 3.
1. Verify that air intake on side is not blocked by other equipment. Leave at least 3-4 inches (76-102mm) space by intake fins for proper airflow. 8 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.
13 Vision reports that there is no Reference Standardization or Instrument Calibration; suggests that these tests be run. 1. Usually caused by entering the test, then canceling, which leaves the instrument with no completed test constants. Do not cancel when these tests have been initiated. 2. May be caused by use of two network cards in PC. Data collisions are causing lost communication “packets”. Remove one NIC card, and use the connection method on page 4.
12 Lifting and transporting the Metrohm instrument: 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.
13 Index AC power switch ......................................... 83 Accessory Kit ......................................... 21, 27 air filter ............................................. 7, 82, 86 bias ............................................................. 49 CFR 21 ........................................ 6, 35, 77, 79 Crossover Cable ............................................ 8 Data Collection Method ...... 26, 28, 34, 37, 86 Database ................. 38, 56, 57, 60, 61, 63, 74 Default ......
