NIRS XDS Process Analyzer MicroBundle Manual 8.928.
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 Process Analyzer MicroBundle Manual 8.928.8001EN 03.
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.
Change Control Version Date Summary of Changes Initiation of Change Control on this manual Updated company address to 7703 Montpelier Road, Laurel, MD 20723 FOSS NIRSystems, Inc. added to page footers. 1.11 Updated Wavelength Linearization spectrum on page 49, 60, and 73 December 16, with correct graphic. 2004 Updated Wavelength Linearization screen on page 50 with correct graphic. Updated section 10.4.3, page 77, to reflect use of calibrated XC-1300 Wavelength Standard used in transmission measurement.
Table of contents 1 2 3 4 5 6 7 8 Introduction ................................................................................................................... 6 1.1 Enclosure Styles ........................................................................................... 6 1.2 Fiber Optic Probe Ends ................................................................................. 8 1.3 MicroBundle Fiber Information .................................................................... 9 1.
9 Temperature Controller Set-up ..................................................................................... 47 10 Vision Software Operation.......................................................................... 49 10.1 Configure Options....................................................................................... 56 10.2 Interactance Reflectance Tests ................................................................... 58 10.2.1 Wavelength Linearization, Interactance Reflectance .......
1 Introduction The XDS Process Analytics Microbundle Multiplexer Instrument uses Near Infrared (NIR) energy to determine chemical and physical characteristics of the sample. The sample is illuminated with white light, and the signal returning is broken down into visible and NIR wavelengths for spectroscopic analysis. Vision Software® is used for this analysis. Vision® has a complete suite of analysis methods for both quantitative measurement, and for qualitative analysis.
The “X-Purge” unit comes in either the air-conditioned enclosure (shown) or the Vortec-cooled version. This Vortec-cooled system may be used in Div. 1 areas as defined under NEC 500 standards, and in Zone 1 areas as defined by IEC/CENELEC and NEC 505 requirements. The air-conditioned unit is limited to Div. 2 areas. The BEBCO system supplies clean instrument air or inert gas to remove flammable vapors, and to prevent accumulation of ignitable dust within the protected XDS Process enclosure.
1.2 Fiber Optic Probe Ends Interactance Reflectance Probes are used for processes where the medium is somewhat turbid and will provide a good reflectance signal back to the instrument. This includes fermentation products and other materials with high solids content. The fiber optic bundle has two channels. One carries the light to the probe, and the other channel carries the reflected signal back to the detector for analysis. This probe requires only one pressure port in a reactor.
1.3 MicroBundle Fiber Information “Micro-bundle” fiber is normally 40 fibers per source channel, and 40 fibers per receiving channel. This is shown at right, compared to single fiber. The dark spot at the center of the SMA connector is the fiber in each type. Because the Micro-bundle has more fibers, it has greater light-carrying capacity, and is therefore capable of measurements on denser samples.
Temperature probes are available, which offer the option of monitoring process temperature. This is especially useful in liquid streams. Spectra may change slightly with temperature. The data from the probes may be used to adjust the calibration for temperature effects, for more consistent results.
2 Purged System for Hazardous Environments The XDS Process Analytics Instrument offers the option of a BEBCO purging system for hazardous environment use. This compact purging system is designed to meet European approvals as well as North American standards. The system permits use of the XDS Process Analytics Instrument in Div. 1 areas as defined under NEC 500 standards, and in Zone 1 areas as defined by IEC/CENELEC and NEC 505 requirements.
As strictly defined by NFPA 496, this method is a start-up process of Class I area pressurizing which removes flammable vapors from a protected enclosure. This is accomplished by exchanging a known volume of protective gas, while maintaining a minimum positive enclosure pressure of 0.10 inches of water. 2.2 Class, Group and Division Ratings The 1993 edition of NFPA 496 recommends 4 volume exchanges for all enclosures and 10 volume exchanges for all motors.
2.3 Display / Interface Module: The Display Interface Module is located on the Electronic Power Control Unit (EPCU). Status of power-up may be monitored using this display. The Display/Interface Module gives information about the purge control. Each LED indicates status of a specific function.
The flapper valve allows controlled air to escape from the XDS Process Analytics Instrument enclosure. The air exits through a spark arrestor, as shown. With the cover in place, this serves as a safe exit for purge gases. Do not disassemble the vent housing except as specifically instructed. This is not a user-serviceable item. Any alteration to the vent assembly will void the protection provided by the purging system. 2.4 Power-up Instructions: These are the instructions provided on the BEBCO panel.
This shows the positions for the key used in steps 4, 5, and 6 above. The upper position is used to set enclosure pressure. The lower position is the locking position described in step 6. A Sequencing Diagram with LED operation is shown in the following pages, continuing through to system Fault Conditions. This sequencing diagram is provided by BEBCO Industries, Inc., to explain the operations sequence and LED status during purge operation. A graphic description is provided in the following pages.
Operations Sequence and Flow Diagram BEBCO Industries, Inc.
Sequence 4: Safe Pressure Achieved Apply air to achieve Safe Pressure SERIES 4000 ELECTRONIC POWER CONTROL UNIT ENCLOSURE POWER DISENGAGED PRESSURE LOSS ALARM SAFE ENCLOSURE PRESSURE SYSTEM CONTROL BYPASSED RAPID EXCHANGE FLOW POWER SHUTDOWN DELAY RAPID EXCHANGE TIMER EMERGENCY POWER SHUTDOWN HIGH ENCLOSURE PRESSURE RAPID EXCHANGE OVERRIDE ENCLOSURE POWER ENGAGED EPCU POWER ENGAGED HEP SDT RET When Safe Pressure Setpoint is achieved, Safe Enclosure Pressure LED is ON.
FAULT CONDITIONS Each of these conditions is considered abnormal.
face. HEP High Enclosure Pressure. When activated, the Rapid Exchange Solenoid Valve is disabled and the alarm relay is energized. IEC International Electrotechnical Commission. The IEC issues international standards for all areas of electrical, electronic and related technologies. ISA Instrument Society of America. ISA is an industry organization representing the interests of quality, safety, and productivity of measurement and control systems and equipment.
3 Instrument Specifications The XDS Process Analytics Instrument uses Near Infrared (NIR) energy to determine chemical and physical characteristics of the sample. The sample is illuminated with white light through a fiber optic bundle. The light is returned through a separate fiber bundle path, and the returning signal is broken down into visible and NIR wavelengths for spectroscopic analysis. The spectroscopic data is processed using a PC, and results are output in real time.
3.3 Weight System Type Pounds Kilograms Basic System: 93 lbs 41.9 With Vortec Cooler: 106 lbs 47.7 With Purge Control and Air Conditioning: 135 lbs 60.8 3.4 Operating Temperature Range System Type Fahrenheit Centigrade Basic System: 32-95 0-35 With Vortec Cooler: 32-104 0-40 With Purge Control and Air Conditioning: 32-125 0-51 With Air Conditioning 32-125 0-51 3.5 Operating Humidity Range System Type % Relative Humidity All Systems: 10-90 % non-condensing 3.
Safe Pressure Flow Rate (both System Types) US: 0.31 to 11 SCFH Metric: 0.15 to 5.2 NL/Minute ¼” FPT NOTE: Large supply lines are recommended to permit adequate airflow. Some loss will occur due to internal friction. Use ½-inch to 1-inch (12mm to 25mm) supply lines. 3.6.1 Terminology • SCFM: The term SCFM stands for Standard Cubic Feet per Minute, referenced to a pre-specified pressure, temperature, and relative humidity. In most cases, SCFM is referenced to 14.
• 20 MHz – Module Control Board 3.11 Power Supply Voltages • 15VDC, 250W Maximum • 12 VDC, 40W Maximum 3.12 Resistive Heater in Basic System and Vortec Cooled Systems • Two (2) 150W, 240VAC resistive heaters, operated at half power. 3.13 Air Conditioner Type • TECA 500 BTU, Solid State with Resistive Heaters. 3.14 Lamp Source in XDS Process Analytics Instrument • 42 Watt Tungsten Halogen Reflector Lamp This lamp is specially processed to enhance NIR energy output and assure stable illumination.
4 Site Requirements The XDS Process Analytics Instrument specifications are given in section 3.0. These specifications include weight, AC Power (Mains) requirements, air supply, temperature, and humidity conditions. This section includes dimensional drawings and recommended space for service access. VENT FOR PURGE SYSTEM Optional Purge System 1.5" (38.1mm) 0.75" (19.05mm) Heat Sink, Fan 16" (406.5mm) 17.5" (444.5mm) 19" (482.6mm) 24" (609.6mm) 24.75" (628.65mm) 25.5" (647.7mm) 31" (787.5mm) 24" (609.
SYSTEM Left Side Right Side Basic Unit, Fancooled 12” (305mm) Vortec Cooled Top Bottom Front Access 18” (457mm) 18” (457mm) Flush Mount 48” (1220mm) 12” (305mm) 18” (457mm) 18” (457mm) Flush Mount 48” (1220mm) Purged System, Vortec Cooled 12” (305mm) 18” (457mm) 18” (457mm) Flush Mount 48” (1220mm) Purged System, Air Conditioned 12” (305mm) 18” (457mm) 18” (457mm) Flush Mount 48” (1220mm) The mounting bolts must be 3/8” (10mm) in size.
5 Installation of Process Enclosure The basic types are shown here, for familiarization. Installation instructions follow. 5.1 Basic NEMA 4X Process Analytics Instrument The basic NEMA 4X, fancooled instrument is shown. Note the fiber mounting plugs at the top right. This is where the fiber optics are routed into the instrument. The window in the door permits the user to view the LED indicators and the temperature controller. The heat sink and fan chassis are shown on the right side.
This shows the Basic Unit with Vortec Cooler on the right side. The left side of the basic XDS Process Analytics Instrument shows the AC cable entrance and RJ-45 connection, indicated by arrows. The XDS Process Analytics Instrument is shipped with an AC cable for testing and lab use only, since many instruments are operated in a laboratory setting prior to implementation on the process line.
5.2 Vortec Cooled XDS Process Analytics Instrument The Vortec cooled instrument has a Vortec assembly on the right side, attached to the heat sink. An air curtain (inside the horizontal housing) directs the cooling flow over the full width of the heat sink. This instrument also has the vent for the purge system, mounted on top of the cabinet. Vent Housing Actuation Valve Vortec Cooler Filter This photo shows the inside of the Vortec cooler, where the air curtain is released.
5.3 Purged Enclosure for Hazardous Environments Vent Assembly LED Indicators Catastrophic Shutoff BEBCO Purge Unit Monochromator Fiber Housing Lamp Housing Vortec Cooler AC Power Block RJ-45 Communications fibers enter the purged system where shown in the photo, near the filter unit. The instrument air input to the filter is shown. AC Power enters the purged enclosure via the cable entrance at lower right in this photo.
5.4 Mounting of XDS Process Enclosure These steps explain physical mounting of the XDS Process Enclosure. Note that the enclosure may weigh as much as 135 pounds (60.8kg). It is imperative that the installers take precautions to avoid injury during installation. 1. Select a mounting area with a minimum of transmitted vibration which could affect the instrument. 2. Verify that the mounting area is able to support the full weight of the instrument, including options.
4. Mounting dimensions for the enclosure feet are as shown on the following page. The mounting bolts must be 3/8” (10mm) in size. The environment may require stainless steel due to industry or washdown requirements. 5. Lift the instrument onto the mounting bolts, seating both upper mounting brackets first. VENT FOR PURGE SYSTEM Optional Purge System 1.5" (38.1mm) 0.75" (19.05mm) Heat Sink, Fan 16" (406.5mm) 17.5" (444.5mm) 19" (482.6mm) 24" (609.6mm) 24.75" (628.65mm) 25.5" (647.7mm) 31" (787.
6. These photos show a mounting with 3/8” mounting studs, welded to a heavy backing plate. The mounting may also be a sturdy frame, or other method suitable to support the full weight of the instrument. Use extreme caution with the fiber optic cables when mounting the instrument. If possible, the cables should be coiled up and secured to the unit to avoid damage. Radius of coiled fibers should never be less than 6” (153mm). Diameter should be at least 12” (305mm).
5.5 Removal of Shipping Restraints The monochromator enclosure is mounted on wire rope shock absorbers to minimize the effect of vibration in the ambient environment. The monochromator is locked down for shipment, to prevent shipping movement from jostling the shock mounts beyond their normal range of motion. Release the shipping restraints as shown. The shipping restraints are three (3) captive screws, circled in the photo at right. Two are at the front of the monochromator box, and one is at the rear.
6 Installation of Fiber Optics Fiber optic cables are quite rugged, and are jacketed to protect the delicate optical fibers within. While protected, the fiber bundles are still somewhat fragile when not handled correctly. Always use care when routing and installing fibers. The fibers are installed on the instrument, and are shipped in a coiled position in the shipping container. Handle very gently when moving and lifting, to avoid damage. Follow these guidelines: 1.
A suitable wrench is the NC-100 with 5/16” (about 8mm) head, made by Seekonk Manufacturing Co., Seekonk, MA 02771, USA. Remove caps from unused channels to facilitate access, then replace caps. The head on the NC-100 is large, and may be hard to turn if caps are not removed before use. Manual section 14.0 explains disassembly of lens barrel from the fiber bundles. In many cases the lens barrel is mounted first, then the fiber is inserted, to minimize stress on the fiber bundle assembly.
7 Electrical Connection The XDS Process Analytics Instrument is shipped with an AC line cord, which is used for initial checkout testing only. When installed in a permanent location, the instrument is to be connected with a dedicated conduit drop, following all applicable electrical codes. AC Mains wiring is as follows: Power Requirements: • 100/240 VAC Selectable • 50/60 Hz • 2A / 1.5A With Air Conditioning (optional) 5A / 2.7A 7.
2. When the green cast cover is removed, the Control Module Assembly will be exposed as shown. Using a #1 Phillips screwdriver, remove both screws holding the Display Interface Module face in place. 3. Gently lift the Display Interface Module face plate off. Put in safe place. 4. Unplug both wired headers, as shown, from the Encapsulated Intrinsic Safety Module (EISM). 5. Use a small flat-bladed screwdriver to loosen both screws holding the Encapsulated Intrinsic Safety Module (EISM) in place.
6. Using proper anti-static (ESD) protection, pull the Encapsulated Intrinsic Safety Module (EISM) straight outward. Set the Encapsulated Intrinsic Safety Module (EISM) aside on a static-protected mat. Note the installer’s ESD Wrist Strap. 7. Note the connector at center right. This is Main Power Wiring Header P1. A close-up is shown below. Pull straight outward to separate from PC card. 8. The Main Power Wiring Header is turned around in this view, so the terminals are in ascending numbered sequence.
L1, Neutral L2, HOT Ground Intl: Blue Intl: Brown Intl: Green/Yellow US: White US: Black US: Green 12. Attach Grounds to the Ground Lug inside the Base Unit of the EPCU. 13. The wiring diagram on page 13 of the BEBCO Industries Series 4000 manual is shown for reference. Refer to the actual diagram for complete wiring particulars. Follow the actual wiring diagram in the BEBCO manual. 14. Verify that all wires are secure and that the clamping screws are tight. 15.
19. Install the face plate onto the Display Interface Module. Install the two Phillips-head screws that hold it in place. 20. Re-install the round green cover over the Display Interface Module. Rotate about 8-10 turns clockwise, until almost snug. Red label should be in the “up” position. 21. Use a 1/16” Allen wrench to tighten the set screw on the cover to prevent removal or unintended rotation. 7.3 AC Power Switch Settings There are two switches that must be set for the supplied operating voltage.
This photo shows the switch prior to air conditioner installation at the factory. This is included to help the installer understand the switch location and positions.
8 RJ-45 Network Connection RJ-45 Cable Connection applies to the non-purged instrument, and is detailed below. For the purged unit, fiber optic modems are provided, to meet hazardous location requirements. 8.1 Basic Process Instrument RJ-45 Connection The Basic XDS Process Analytics Instrument (nonPurged) has an RJ-45 cable entrance on the left side of the box, toward the bottom. It is shown, with cable connected. The plug shown is a water-tight, dust-tight connector with O-ring seals.
Install the O-ring onto the cable connector housing as shown. Do not damage or distort the O-ring during installation. Slide the cable connector housing onto the RJ-45 cable as shown. Using the correct type of crimping tool, crimp the RJ-45 connector jack onto the cable. Be sure the conductors are arranged in the proper order and are in the designated positions for crimping. Push the RJ-45 jack fully into the connector housing. Install the locking clip as shown to hold the jack to the connector housing.
Slide the knurled collar up onto the connector housing. The final assembly is shown. To attach to the instrument, insert the connector jack (tab down) into the plug on the side of the instrument. Push until it “clicks” into place. Thread the knurled collar onto the threaded portion of the mating assembly. Tighten handtight. Be sure the knurled collar is tightened enough to compress the O-ring, to seal out contaminants.
The purge enclosure uses a 100BaseTX-FX Media Converter for safety and clean communications in a factory environment. A 30-meter fiber optic pair is supplied. Longer lengths are available by special order. Maximum cable distance is 2 kilometers. This is a fullduplex system. The fibers must be fed into the enclosure using a proper fitting, as shown at right. The modem is shown with the correct fitting for purge systems. The connections ends are shown, with protective covers in place.
Modem Location Modem Inside Process Instrument Modem External to Instrument “Black” Fiber Cable To “TX” (left port) To “RX” (right port) “Red” Fiber Cable To “RX” (right port) To “TX” (left port) Button Position Button out: “X” position Button in: “I” position The above settings apply as long as the PC connection to the external model is “Direct Connect” and uses the UTP Crossover cable supplied in the Process Analytics Accessory Kit.
9 Temperature Controller Set-up The XDS Process Analytics Instrument contains a temperature controller to maintain internal temperature of the enclosure. This is normally set to 38.0 degrees C (100.4 degrees F). Temperature is read in degrees C. A temperature-sensing device is embedded in the instrument cabinet, and this is used as a method to control the internal temperature.
The enclosure temperature is displayed in the Status Bar of Vision, as shown. This is not adjustable from Vision. In this case, the instrument temperature had not yet reached the set point of 38 degrees C. It is shown for operator information.
10 Vision Software Operation This section describes the steps required to establish communication with the XDS Process Analytics Instrument. It explains how to run set-up diagnostics, and run routine instrument assessment diagnostics. The Vision Software Manual provides information on quantitative and qualitative operation. Communication between the computer (with Vision Software loaded) and the XDS instrument may be handled in one of several ways.
3. To begin, 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 well-organized. Assign the project some meaningful name, to make it easy to remember. For our purposes, we simply called this “project7”. Please use a more descriptive name. Vision will assign a Location; leave this blank. 4. Vision asks if the default directory location is acceptable.
7. This screen sets up communication parameters for the instrument. The XDS instrument has a unique driver. Highlight this box and click on “Configure”. 8. This box allows the user to select the instrument identified by the instrument serial number. The number in front of the instrument S/N is the IP (Internet Protocol) address assigned to the XDS instrument. Use the drop-down arrow of the IP Address box, and select the correct instrument. The instrument must show “Available” to be selected. 9.
11. Select Options as shown at right. Reference Standardization and Use Instrument Calibration are essential for method transfer between similar instruments. Check both boxes, then click on “OK”. This screen is discussed in more detail in section 10.1 of this manual. 12. Click on Acquire, Connect.
13. A Data Collection Method (DCM) selection box will appear. It is empty, so no selection is available. Click on the “New” button. A blank DCM screen will be displayed. An example of a DCM for this instrument is shown on the next page. 14. When this DCM screen is shown, the Method is blank. Fill in the name with a meaningful description. In this case we will name the method “Multiplexer 1Ch,” for the type of instrument, and the sample channel used. The Multiplexer has a Range of 800-2200nm.
15. This screen is used to set up the multiplexer channels. Selections include tip Type, Fiber Count, and Fiber Length. Click on Channel 1. Click on “Used” to indicate that it will be used for sampling. 16. Click on the drop-down arrow beside the Tip Type box. This shows supported types of probe configurations. In this case, select Interactance Reflectance Probe.
17. Click on the drop-down arrow next to Fiber Count. Supported types are Regular Bundle, Micro Bundle, and Single Fiber. In this case select Micro Bundle. Fiber Length depends on the fibers used in the system. The default is 0-3 Meters. Scans defaults to 32 scans for a spectrum. This is normally not changed unless there is a sampling reason that requires fewer or more scans. 18. Now click on Channel 2. By default, Channels 2-9 are marked “Not Used”.
22. This manual now describes various software tests used to set up and test the instrument. These tests must be run on each sample channel marked as “Used” in the Mux Table. First select the channel. From the menu bar, click on Acquire, then Select Channel. Use the spinner to select the channel. Start with Channel 1, and continue with all “Used” channels. 10.1 Configure Options Before tests are run, the Options must be set.
2. The menu shown at right is the set of selections. A brief explanation follows: Instrument must stabilize before data acquisition: This prevents spectral acquisition if the instrument is cold. Performance Test must pass before data acquisition: This prevents the user from taking data on a non-functional instrument. Run performance test after wavelength linearization: Forces user to run test sequentially. This is not necessary with XDS.
This screen is normally displayed, with serial numbers for the system in use. If this configuration is correct, click on “OK” to proceed with tests. 10.2 Interactance Reflectance Tests The tests in this section apply specifically to Interactance Reflectance Probes. Do not use the same procedures on other styles of probe. See the proper section for each style of probe used. 10.2.1 Wavelength Linearization, Interactance Reflectance The first test to be run is Wavelength Linearization.
The wavelength positions of these peaks appear as shown. The scale of this display is marked in encoder pulses, which do not relate to nanometers directly. From the peaks, a linearization is performed, which allows assignment of nanometer values. (Actual spectral shape depends on fiber configuration.) The spectrum shown above does not exhibit any noise effect from fiber attenuation.
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. This is done twice, one for each direction of the grating motion. After the linearization is successfully sent to the instrument, this message confirms the transfer. Click “OK” to proceed. 10.2.
Note that Reference Standardization must have been selected under Configure, Options, for this to take effect. Once selected, a new Data Collection Method (DCM) must be created for Reference Standardization to be checked in the DCM box. It is not applied to a DCM retroactively. When Reference Standardization is selected under Configure, Options, a Reference Standard must be created for every sample channel that is “Used” even if the probe style is not Interactance Reflectance.
Place the Certified 99% Reflectance Reference onto the Reflectance Probe, hold in place, and click on “OK”. Note the orientation of the standard. Vision prompts the user to rotate the Certified 99% Reflectance Reference. Rotate in 90-degree increments, for a total of four scans, at the prompts. The four spectra are averaged, and the averaged spectrum is used for Reference Standardization. This minimizes the directional effects of the standard, to provide best consistency.
The Certified 99% Reflectance Reference is shown with the sample channel spectrum, acquired against the internal instrument reference fiber. (Plot color is red.) The wavelength scale is now wider, because the Certified 99% Reflectance Reference has a spectrum from 4002500nm. The sample fiber spectrum (top) is still plotted 800-2100nm. After Reference Standardization, the upper spectrum will be corrected to look like the lower spectrum. Click “OK” to plot a correction spectrum.
When finished, this box is shown with the final correction spectrum. The correction is downloaded to the instrument for the proper channel, and will be applied whenever a “Reference Standardized” DCM is used. Note that the DCM must be created with “Reference Standardization” checked in the “Project Options” box. If the DCM was created prior to selection of “Reference Standardization”, then it was checked, the DCM will not apply Reference Standardization. Click “Print Report” to print the corrected spectrum.
Instrument Calibration uses a traceable, stable, standard, of known wavelength response, as a method to establish wavelength scale response of the instrument. The instrument is set to scan the standard, and the nominal peak positions for each major absorption are determined. Vision performs an algorithm to set the peak positions of the instrument to those of the standard. These adjustments are saved, and are applied on each subsequent scan of the instrument, yielding a correct spectrum.
Wavelength Linearization is performed in two sections, each of which takes about 15 seconds. Following Wavelength Linearization, the user is asked to select a standard file. This is provided on the diskette in the Certified Standard box. It may be manually copied on the computer in the Vision directory, as shown. Select this file and click on “Open”. Vision prompts the user to position the WSR103xx standard on the probe. When prompted, position the WSR103xx Wavelength Standard Cell on the probe as shown.
At the end of the test this dialog box is displayed. If hard copy is desired, click on “Print”. Click “OK” to exit Instrument Calibration. Select the next channel, if used. From the menu bar, click on Acquire, then Select Channel. Use the spinner to select the correct channel, then click on “OK”. This must be performed for each channel. Always verify the channel before proceeding with the test.
In Instrument Calibration, the XDS instrument is set to nominals which provide excellent instrument transfer, and which meet published NIST wavelengths when tested in Wavelength Certification. Peaks for the additional ingredient are set to peak nominals determined by measurement on several different types of research instrumentation. In Wavelength Certification, the NIST-stated uncertainty of 1.0nm is applied.
Vision provides a split-screen display that details instrument performance. The lower right quadrant shows tabulated data. Double-click to enlarge this screen to full size. When the test is complete, tabs shows results. 10.3 Interactance Immersion Tests The Interactance Immersion Probe is quite similar to the Interactance Reflectance Probe. It uses the same type of fiber bundle with concentric light paths. The only difference is the “lens barrel” which directs the light in a different geometry.
The NIR wavelength positions of these peaks appear as shown. The scale of this display is marked in encoder pulses, which do not relate to nanometers directly. From the peaks, a linearization is performed, which allows assignment of nanometer values. (Actual spectral shape depends on fiber configuration.) The spectrum shown above does not exhibit any noise effect from fiber attenuation.
high-quality spectrum on each instrument, and to enhance transferability between instruments. When using the Interactance Immersion Probe, Reference Standardization is performed using an Interactance Reflectance barrel. Following all calibration steps, the Interactance Reflectance barrel is removed, and the Interactance Immersion barrel is installed. A final “Window Correction” is performed, which adjusts the optical response to the Interactance Immersion configuration.
Vision requests that the Certified Reflectance Reference be scanned. The Certified 99% Reflectance Reference is shown. It comes with a diskette, which must be used during Reference Standardization on Interactance Reflectance channels. The set is named RSSPxxxx, which includes the R99Pxxxx Certified Reflectance Standard, and the “Standards” diskette. The Standards diskette contains a certified NIR spectrum, taken on the Metrohm NIRSystems master instrument.
Vision requests the Standard File for the Certified 99% Reflectance Reference. This file is on the diskette (or Mini-CD) packed with the standard, and may be copied to the Vision directory for ease of use. It is shown here on the D: drive, on a MiniCD. The file is named “RSSPxxxx.da”. Click on the file, then click “Open”. This is a plot of the un-calibrated sample fiber in the instrument. (The plot color is cyan, which is made darker and “heavier” here for readability.
The correction spectrum represents the amount of spectral correction required to provide a virtual 100% reflectance reference at each data point. (The correction is plotted in violet.) This is calculated in Vision. The difference between the sample fiber and the Certified 99% Reflectance Reference, plus the stored spectrum on the diskette or Mini-CD, permits calculation of the true response of the sample fiber, on a scale of absolute absorbance.
Typically the user will complete a full set of tests on one multiplexer channel before proceeding to the next. If this is the case, proceed to Instrument Calibration. The Interactance Reflectance Probe Barrel should be left in place for Instrument Calibration. It is helpful to keep a checklist of what tests were performed on each channel, to be sure no tests are omitted. If proceeding to Reference Standardization on the next channel, it must be selected.
This adjustment is performed using the Interactance Reflectance probe barrel supplied, and applies to both Interactance Reflectance and Interactance Immersion. (The DCM for Interactance Immersion may be used for this operation.) Vision takes an instrument reference, using the internal reference fiber. This takes about 20 seconds. This dialog box is displayed. Next a scan is taken (on the reference) and this box is displayed. This takes about 20-30 seconds.
Vision prompts the user to position the WSR103xx standard on the probe. When prompted, position the WSR103xx Wavelength Standard Cell on the probe as shown. The label should always be in a consistent position. In this case, the bottom of the label is parallel with the holder. Click “OK” to continue. This test takes about 45 seconds. The wavelength response for each defined peak is adjusted, to assure precise wavelength registration between instruments.
peaks beyond those normally found in SRM-1920a. This material has very sharp bands, which are found to be stable and repeatable. Spectra of each are as described: The darker spectrum, which has no discernible peaks beyond about 2150nm, is SRM-1920a. The FOSS WSR Wavelength Standard is the lighter spectrum, and has clear peaks visible at above 2200nm. These additional peaks are used to set the wavelength scale of the instrument to aid in instrument matching.
This window correction method offers a large advantage to users running with a probe barrel permanently installed in a reactor or other vessel. At initial set-up, the window difference is measured and stored in the instrument by channel. At periodic maintenance intervals, the fiber optic bundle can be removed from the barrel, which is now permanently installed.
The TSSZERO file is shown as a spectral plot. The spectrum is a flat line at 0 AU. Vision takes a reference using the fiber optic probe. This spectrum is plotted (not shown here.) When this message appears, click on “OK”. Vision plots the TSSZERO.da file on screen. Click on “OK”. The correction file is plotted. Click “OK” to see the final correction, overlaid onto the certified TSSZERO spectrum. The two spectra should overlay perfectly. Click on “OK”. When finished, the user may print the report.
1. Select Performance Test from the Diagnostics menu bar. 2. Select the channel to be used for the test. In this case, we select “SAMPLE”. The end of the Interactance Immersion probe should be protected from stray light for this test. This tests the sample channel, and provides a comprehensive test of instrument performance. Vision provides a split-screen display that details instrument performance. The lower right quadrant shows tabulated data. Double-click to enlarge this screen to full size.
10.4 Transmission Probe Tests The Transmission Probes require special methods of calibration. One fiber bundle carries “white light” from the instrument to the sample. The other fiber bundle is used to return light to the instrument, to be broken down in the monochromator to individual wavelengths, then measured for spectral response. Absorbance of the sample is then determined. 10.4.1 Wavelength Linearization, Transmission Probes The first test to be run is Wavelength Linearization.
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.
2. Tighten the thumbscrew gently on the probe. 3. With both probes in position, cover the center area shown in the photo to prevent stray light from affecting the Reference Standardization. Do not insert the WST3Wxxx standard. Nothing is to be placed between the fiber bundle ends during Reference Standardization. 4. Select the channel. From the menu bar, click on Acquire, then Select Channel. Use the spinner to select the correct channel, then click on “OK”. This must be performed for each channel.
6. Vision requests that the correction file be located. It is in the C:\Vision directory. Highlight the file “TSSZERO.da” and click “Open.” 7. Once the file is selected, Vision applies the correction to sample spectra taken with this channel. This method enhances transferability of samples from one channel (of a given probe geometry) to another. Click “Close Report” to proceed. 8. Select the next channel, if used. From the menu bar, click on Acquire, then Select Channel.
Instrument Calibration uses a traceable, stable, standard, of known wavelength response, as a method to establish wavelength scale response of the instrument. The instrument is set to scan the standard, and the nominal peak positions for each major absorption are determined. Vision performs an algorithm to set the peak positions of the instrument to those of the standard. These adjustments are saved, and are applied on each subsequent scan of the instrument, yielding a correct spectrum.
Next a scan is taken (on the reference) and this box is displayed. This takes about 20-30 seconds. Wavelength Linearization is performed in two sections, each of which takes about 15 seconds. Following Wavelength Linearization, the user is asked to select a standard file. This is located on the computer in the Vision directory, as shown. Select the file “TSS3Wxxx” and click on “Open”. Vision prompts the user to position the probes in the fixture as shown.
At the end of the test this dialog box is displayed. Click “OK” to exit Instrument Calibration. Information about the WST3Wxxx Transmission Wavelength Calibration Standard: The transmission wavelength standard used is traceable to NIST SRM-2035, through direct comparison on the Metrohm Master Transmission Instrument. The optical materials used in the WST3Wxxx Calibration Standard have very sharp bands, which are found to be stable and repeatable.
This window correction method offers a large advantage to users running with probe barrels permanently installed in a reactor or other vessel. At initial set-up, the window difference is measured and stored in Vision. At periodic maintenance intervals, the fiber optic bundles can be removed from the barrels, which are now permanently installed. The instrument and fiber optics can be calibrated for wavelength and Reference Standardized response, without using the Transmission Probe barrels.
The TSSZERO file is shown as a spectral plot. The spectrum is a flat line at 0 AU. Vision takes a reference using the fiber optic probes. This spectrum is plotted (not shown here.) When this message appears, click on “OK”. Vision plots the TSSZERO.da file on screen. Click on “OK”. The correction file is plotted. Click “OK” to see the final correction, overlaid onto the certified TSSZERO spectrum. The two spectra should overlay perfectly. Click on “OK”. When finished, the user may print the report.
1. Select Performance Test from the Diagnostics menu bar. 2. Select the channel to be used for the test. In this case, we select “SAMPLE”. The end of the Interactance Immersion probe should be protected from stray light for this test. This tests the sample channel, and provides a comprehensive test of instrument performance. Vision provides a split-screen display that details instrument performance. The lower right quadrant shows tabulated data. Double-click to enlarge this screen to full size.
11 Maintenance of the XDS Process Instrument The XDS Process Analytics Instrument is designed to be trouble-free, with a minimum of maintenance. These guidelines should always be followed: 1. Keep the outer enclosure as clean as possible, to maintain heat transfer characteristics. 2. Do not allow dirt buildup in the heat sink fins. These should be blown clear of any dirt or obstructions on a regular basis. 3. Be extremely careful of the fiber optic bundles.
The monochromator is mounted on wire rope shock mountings to absorb vibration and assure a low noise instrument. One of these wire rope shock mounts is shown at right. The instrument must be operated in the upright position to take advantage of the shock mounting. The thumbscrew to the left of this wire rope mount is a shipping lockdown. It should be locked down when transporting the instrument. It must be released when operating.
The multiplexer is shown in close-up. The channels are marked, but are quite hard to read. This diagram shows the channel numbers where the “return” fibers attach. The fiber at the #10 position connects to the #10 position on the lamp box. The fiber at the center is the internal reference channel, and runs to the monochromator box. The instrument contains a catastrophic shutdown temperature control, shown at right. This instrument is set at 120 degrees F.
Fiber Optic Cables connect at the top of the enclosure as shown. This instrument has only one channel, mounted at the rear-most entrance. Stainless-steel plugs seal the unused entrances. Up to nine channels may be used, when the multiplexer is installed. When optional temperature probes are used, the number of fiber optic channels may be reduced, as the temperature probes exit using these openings. A fiber optic modem is available for the XDS Process Analytics Instrument.
11.2 Lamp Replacement Lamp replacement is quite simple with the XDS Process Analytics Instrument. Lamp replacement should normally be scheduled at factory shutdown intervals, to avoid unexpected downtime during peak production. Lamp instructions are as follows: 1. Shut off AC Power to the instrument. If the location has a “Lockout Policy” it must be followed. 2. Using a large, flat-bladed screwdriver, open the door latches. Turn counterclockwise to open. When open, the slot is vertically-oriented.
3. The lamp may be very warm. Give it at least 15-20 minutes to cool down before attempting replacement. The lamp housing is the stainless steel cover at in the lower part of this photo. Note the four (4) captive thumbscrews. When the housing is cool to the touch, loosen the four thumbscrews. 4. Carefully lift the cover off as shown. The lamp is now visible. 5. Loosen the two lamp screw terminals. Slide the lugs out from under the screws. Do not remove the screws from the terminal strip.
6. Twist the lamp retaining ring to the right, and lower it from the heads of the shoulder screws. Remove the lamp assembly from the instrument. 7. Carefully remove the ring from the lamp wires. This ring will be re-used with the new lamp.
8. Place the new lamp retaining ring over the new lamp assembly. The wires must run through the center hole of the bracket as shown. 9. Carefully lift the lamp upward into the lamp bracket. Place the lamp retaining ring over the heads of the shoulder screws, then rotate to the left to lock in place. Be sure all three shoulder screws are securely seated on the lamp retaining plate. There is no rotary orientation of the lamp. It may be installed in any orientation.
11. Install the lamp cover back onto the lamp housing. The widest part faces the user. Do not try to install in the wrong orientation. 12. Tighten the four (4) captive thumbscrews on the lamp cover. Do not use tools to tighten these screws, as the heat cycling of the instrument may make them hard to remove. Hand-tight is sufficient. 13. Close the instrument. Apply power to warm up the instrument. 14. Enter Vision Software and connect to the instrument. 15. Run Wavelength Linearization. 16.
1. Turn off electrical power and follow any required lockout policy. 2. Using a large, flat-bladed screwdriver, open the door latches. Turn counterclockwise to open. When open, the slot is vertically-oriented. A coin may be used if a large screwdriver is not available. 3. The AC (Mains) Fuses are located in the AC Power Block. Poles 1 and 2 contain the fuses for each side of the line.
4. Gently lift the tab to open each fuse position. Spare fuses are included in the instrument Accessory Kit. Fuse Ratings: • 250 VAC, 5 x 20mm, Slo-Blo (2) Required • Non-Air Conditioned: 3.15A • Air-Conditioned: 6.3A Order spare fuses immediately, to have on hand. 5. Remove each fuse from the clip. It may help to push the fuse, using a pencil eraser, from the side shown, and then grasp the fuse to fully remove. Inspection of the blown fuses may provide some information about the type of fault.
7. Push down the fuse door firmly until it snaps into place. Be sure this has been performed for both fuses. 8. Close and latch the door of the XDS Process Analytics Instrument. 9. Restore power to the instrument. 10. Connect to the instrument from Vision. Allow time for Purge System activation (if so equipped) plus about 20 minutes for temperature stabilization. 11. Run Performance Test to verify instrument operation. Because no optical components were changed, there is no requirement to run other tests.
12 Safety Information SAFETY NOTICE A separate electrical shutoff is required for this instrument for safety purposes. The shutoff must break both sides of the line (“All-pole”) and be electrically grounded. The shutoff box must be adjacent to the unit for ease of shutoff for maintenance or emergency purposes. If your plant codes require “lockouts” on electrical equipment, the shutoff should accommodate the lockout devices to prevent inadvertent power-up.
All major electrical components used in the instrument meet UL, CE, CSA, or TUV certification. Usage is as defined by the manufacturer, to assure safe performance. Wire sizes, colors, and terminations meet CE requirements. All connectors meet CE safety standards. Shielding is provided to avoid user contact with hazardous voltages during use of the instrument. Additional safeguards have been taken to avoid defeating these shields and interlocks.
13 Troubleshooting The XDS Process Analytics Instrument is a dependable, trouble-free instrument, designed for many years of service in your facility. 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, except for the lamp. Because of this design, we emphasize that under no circumstances should the user attempt to service any part other than the lamp.
1. Verify that the RJ-45 cable is plugged in at both the instrument interface, and at the network jack. 2. Verify that the RJ-45 cable is plugged in at both the computer and at the network jack. (NOTE: Direct connection is explained in a separate document for non-network users. This requires a special “UTP Crossover” cable. 2 No communication between Vision and the instrument. 3. Verify that the instrument is powered on. (See previous Observed Problem.) 4.
1. Temperature and/or humidity may be changing rapidly during the test. This can usually be observed as large spectral activity between 13001400nm and 1800-1900nm. Be sure the instrument enclosure is closed and locked. Allow to stabilize. 5 Instrument Fails Performance Test. 2. Instrument may be located near grinders, stirrers, or other equipment which produces vibration or mechanical disturbance. This shows up as spectral activity in various areas, depending upon the transmitted frequency of the motion.
14 Probe Disassembly It may be necessary to remove the outer lens barrel from the fiber optic bundle for mounting. Follow these instructions. (Instructions apply only to the probe type shown.) 1. Note the knurled collar. To remove the lens barrel, unscrew the knurled collar. 2. As the knurled collar is loosened, be sure to support the lens barrel. Do not let it drop. 3. When the knurled collar is disengaged from the lens barrel, slide the lens barrel off over the fiber optic bundle end.
5. Probes are generally mounted in pressure vessels (and other locations) using Swagelok™ fittings such as that shown. Nominal inside diameter is 1.00”. Always follow Swagelok recommendations for proper pressure sealing. Any deviation from instructions may result in leaking. 6. A “probe purge port” is provided on each lens barrel. This may be used to introduce a vacuum on the inside of the lens barrel of the probe.
15 Appendix: Typical Probe Drawings As mentioned in section 4.0, these probe drawings are of the standard probe types, and are provided as a guide. Because probes vary, and are subject to updates, DO NOT USE THESE DRAWINGS without verifying current dimensions, fittings and materials with Metrohm NIRSystems, Inc. Metrohm NIRSystems is not responsible for use of these drawings for probe installation. Always request current probe drawings before finalizing installation.
Typical Interactance Immersion Probe Style Typical Transmission Probe Style with threaded spacer 112 ▪▪▪▪▪▪▪
