NIRS Analyzer PRO 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 Analyzer PRO Manual 8.928.8004EN 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 Change control on this document is as follows: Version Date Summary of Changes 1.0 Dec.
Table of contents 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 Introduction ................................................................................................................... 5 1.1 Information Disclaimer ................................................................................. 7 Hardware Familiarization .............................................................................................. 8 2.1 Lamp Housing ........................................................................
1 Introduction Analyzer PRO is a rugged, compact Near-Infrared Process Instrument, designed for the wavelength range from 1100-1650 nanometers. This is an excellent region for process analysis, containing many second and third overtones of molecular vibrations which can be measured. The instrument is based upon high-resolution diode array technology. The InGaAs diode array, with spectral dispersion of 1.1 nm/pixel, is a stable, intrinsically accurate method of NIR absorbance measurement.
The Analyzer PRO vides non-destructive analysis of chemical and pharmaceutical products directly in the process line, without use of a bypass loop. Because most materials can be measured directly, with no need for sample dilution or preparation, the material can be measured as produced, with no loss of end product. Operation of the Analyzer PRO is through Metrohm Vision™ software, which is robust, powerful, and easy to use.
1.1 Information Disclaimer This manual and the information herein are correct as of the time of publication, based upon the best information available at the time. Configuration, options, and software information may change over time, in keeping with the corporate philosophy of continuous improvement. Metrohm NIRSystems and its distributors cannot be liable for changes to the customer process based upon information contained in this manual which is subject to revision and update.
2 Hardware Familiarization Analyzer PRO is built into a rugged, sealed stainless steel housing which is designed to withstand the harsh production environment, including washdown. Fiber optics are used with the Reflectance Probe design, and should always be protected from damage and abuse. In particular, fiber bend radius should never be less than 6” (150mm). It is strongly recommended that fibers be mounted in enclosed cable trays to minimize handling, movement, and possible accidents.
wavelength range from 1100-1650 nm. (The optical switch may be heard moving when instrument scans are taken, if the ambient noise level is low enough.) 2.3 Diode Array Spectrometer The diode-array spectrometer is composed of 512 discrete InGAs detector diodes. It has no moving parts. The wavelength accuracy is intrinsically stable, and requires no adjustment. Temperature is maintained internally to assure consistent and accurate response.
Block Diagram The internal light paths of the Analyzer PRO are shown. The sample is illuminated with white light. The resulting signal is sent back (through the optical switch) to the Diode Array Spectrometer for analysis. Both dark and light reference signals are used to set the scale of absorbance. Vision uses the resulting information to produce sample spectra.
3 Specifications Overall Analyzer PRO instrument specifications are as follows: Item Specification Ambient Temperature 23 to 104° F (-5 to 40° C) With Air Cooling: 23 to 149° F (-5 to 65° C) Ambient Humidity 10-90% Relative Humidity, non-condensing Electrical Supply 100-240 VAC, 50-60 Hz, 2.0 A, 150 W Protection IP69k according to IEC 60529 and DIN 40050 part 9, NT ELEC 023 Dimensions Width: 17.0” (42 cm) Height: 17.0” (42 cm) Depth: 5.0” (13 cm) Weight 33.
3.1 Window Reflectance In-line analysis of paste, granulates, slurry, powdered products and similar materials in pipes or fluid transport systems can be performed without need for bypass streams. The sample material must pass over the sample interface window. The window reflection interface may easily be installed into the production line using standard GEA Tuchenhagen flowcell mountings, or by welding an interface flange into the wall of the pipe/transport system.
3.3 Direct Light In-line analysis of products where direct contact with the product is not technically feasible, such as product transported on a conveyor belt or similar means of movement. Lens: Sapphire; diameter 45 mm (1.8”), thickness 12 mm (0.5”), with EPDM O-ring seal for reliable, temperature resistant sealing Distance: 100-250 mm to sample surface (4 to 10”) Scanning Area: 20 - 85 mm (0.8 to 3.
4 Mounting Information Analyzer PRO is provided with an innovative, rugged integral flange-mounting system that permits easy installation and service. There are two mounting flanges, top and bottom, to which are mounted “blind plates” using a rugged, industry-standard tri-clamping mechanism. This approach eliminates bolt holes or other entry points for contaminants. The mounting flanges are sized to attach directly to 3” (76.
2. Fabricate the mounting frame as shown. It may be larger if required. In this installation we purchased pre-cut channel from McMaster Carr. We used four (4) lengths of Steel Strut Channel, Slotted, 1-5/8” x 1-5/8”, zinc-plated, 2 foot length, part number 3310T53. The brackets each measure 24” (610 mm) in length. The upright brackets are bolted so the centerline of the slotted holes is 17.25” (about 439 mm) apart. Use 3/8” (or 10mm) bolts.
4. Adjust height with the lab jacks, so the U-Bolts align properly with the frame slots. Adjust each side equally, to keep the Analyzer PRO aligned with the bracket. 5. When the height is correct, push the U-Bolt through the slots. Do this on both sides of the Analyzer PRO instrument, in preparation for securing with washers and nuts. 6. Install large washers, lock washers, and nuts on the ends of the U-Bolts. Do not tighten until all four sets of washers and nuts are in place.
7. The Analyzer PRO instrument is now securely mounted to the fabricated frame. It is ready to be mounted to the final process location. Verify that all hardware is secure. Protect the fiber (if so equipped) as well as the power and communications cables. Carefully move the Analyzer PRO instrument and mounting frame to the final location. 8. Mounting studs should be placed in the correct positions to hold the frame in place. We installed 3/8” studs in the mounting area as shown. These are 21.
10. Install a large washer, a lock washer, and a hex nut onto each stud. Do not tighten until all four sets of hardware are in place. Continue to protect the fiber optic cable, as shown here. 11. When all four sets of washers and nuts are threaded on, begin tightening each set. Do not damage or distort the mounting frame. If nylon-insert nuts are preferred, those may be used in place of standard hex nuts. 12. When all hardware is tight, the lab jacks may be lowered and removed.
4.2 Mounting by straps to blind plates The blind plates are 15mm stainless steel, and are equipped with a special gasket to properly affix the blind plate to the flange on the instrument. The blind plates may be welded or machined in any way to properly affix and support the instrument in the desired position. Do not distort or weaken the blind plates, as they support the full weight of the Analyzer PRO. Weight is 33 pounds, or 15 Kg. The mounting flange of the instrument is shown at the top.
This photo shows one installation on a process pipe. The Analyzer PRO instrument is supported by metal straps from a support above the instrument, using the mounting flanges. In this case the blind plates were drilled to accept the mounting bolt. Because the mounting flange openings are sealed, there is no risk of contaminants getting inside the Analyzer PRO enclosure. This photo was taken before the cables were secured with tie wraps.
This photo shows an installation on a chute, where the product falls by gravity onto the sample window, thus providing a suitable measurement. The Weld Flange is bolted to a plate which mounts in the duct. The plate may be removed if needed, and replaced with a blank plate. This allows cleaning and minor maintenance, without stopping the line for more than a brief interval. Note that the Analyzer PRO is supported by straps on each side, which support the weight.
5 Mounting Dimensions The Analyzer PRO dimensions are as shown. Note that the dimensions are in “hard Metric”. The inch conversions are very close, but will be less exact. This view shows the distance to the viewing window, as measured from the side. Note the mounting flanges shown on either side of the drawing – these are detailed below. The front view shows overall dimensions, as well as the height to each flange.
6 Electrical Connection The Analyzer PRO is shipped with a temporary AC mains electrical cable in place, suitable for initial testing. Cord length is just over two meters. The installer need only terminate the AC mains power cable as required to meet local codes and installation requirements. For permanent installation, a suitable cable must be installed. This cable should be three-conductor, round cross-section, 3.
mains cable is replaced, the same type of cross-section of cable must be used to assure a good seal. The cables are carefully routed to prevent interference with operation of the Analyzer PRO. When replacing the temporary AC mains cable, follow this procedure: 1. Remove power from the instrument. Both poles must be broken. Use safety lock-out procedures if applicable. 2. Unplug or disconnect existing, temporary AC mains cable. 3. Remove the 32 screws holding the cover in place on the instrument.
4. Press each tab above the wire to be removed, and pull the wire directly outward. NOTE: Verify that power is off before performing this operation. 5. Gently loosen the cable gland over the existing AC mains cable. Use a 22 mm (approx 7/8”) open-end wrench. NOTE: This nut is easy to loosen before removal of Tri-clamp. Do not fully remove the nut at this point. 6. Remove the Tri-clamp holding the cable input header. Save clamp for re-use. 7.
8. Slide the gland nut and sealing ferrule back from the threaded area. 9. Prepare a “fish” line which will be used to pull the new cable into the enclosure. This line will be used to pull the new cable back into the correct position. 10. Gently pull the old cable out of the threaded header, guiding the fish line as needed. Do not pull the line all the way out – the far end should remain where it can be used to pull the new line into the instrument enclosure. This view shows the fish line after pulling.
12. Install the parts as shown on the new cable. This cable is a “North American” type of cable, with white, black and green conductors. 13. Secure the new cable to the fish line, and prepare to gently pull the new cable into the instrument. 14. Pull the fish line inside the instrument, while feeding the new cable gently through the threaded opening, and up through the corner of the instrument cabinet. 15. Run the new cable to the AC power block.
16. Be sure the black o-ring is installed into the groove on the sealing ring as shown. 17. Thread the gland nut and hand-tighten. 18. Using the same 22 mm wrench, tighten the gland nut to compress the seal properly. Do not crush the cable. When tight, the cable should not “give” when tugged slightly. 19. Tie-wrap the new cable to the Ethernet cable internally, to secure it from moving under vibration. Cut off the loose end.
20. If not using a “fish”, the wire can be fed directly. Note that the cable is fed through a corner of the mounting enclosure, and is easier to feed in one direction than the other. We recommend feeding the new AC mains cable through the triangular corner opening – and then into the large round opening -- where it can easily be located and pulled through. The AC Mains connection point is shown, with European color coding. Always follow all applicable local codes to assure safe, reliable connection.
7 Air Cooling Connection Kit Compressed Air Cooling Kit (60038416), installation The optional air cooling kit for high ambient temperatures over 45 °C includes quick-connect fittings that are placed in the two plugged holes. Tubing is also supplied, along with an air filter set with regulator to remove water and oil from the compressed air supply. Adjust the air supply volume until the temperature is below this value This kit includes three Air Fittings, a 30 cm (11.
13. Pull the knob on the regulator and turn it fully counter clockwise in order to set the pressure to zero. 14. Connect the factory air to the water separator. 15. Slowly increase the pressure until a smooth flow is felt from the exhaust tube. Normally a setting of app. 0.02 MPa (0.2 bar) is about right. The objective is to keep the temperature somewhat below 65 °C.
8 Air Purge Connection (Used with “Spoon Probe”) Air purge may be used with the MicroBundle “Spoon Probe’ which uses air purging to remove accumulated sample from the window area, under control of the software. Part number 60039031 must be used. Install the kit as explained above. The Analyzer PRO MicroBundle Fiber version comes with the solenoid air control valve and fittings already mounted. Connect the output from the regulator to the air input on the instrument.
This photo shows a typical accumulation of sample on the face of the spoon probe. This photo was taken in a fluid bed dryer, in between purge cycles. As sample accumulates, the instrument will take a sample scan and produce sample spectra for analysis. The scan timing must sometimes be adjusted to the flow rate, to assure that enough sample has accumulated. When the purge air system is activated, the pressure through the purge holes “blasts” the sample from the face of the probe.
9 Fiber Optic Probe Mounting The MicroBundle fiber optic probe will come installed to the Analyzer PRO. It will be tested in the final configuration, to assure good operation. It is very important to protect the fiber optic cable, to prevent damage. While the cable can be replaced, this is quite expensive and should be avoided. Careful mounting and handling are important. Never let a fiber optic cable hang where it can be snagged by equipment, crushed, or otherwise damaged.
10 Ethernet Connection The Analyzer PRO is shipped with a two-meter length of Ethernet communication cable, wired into the instrument and tie-wrapped in place. Do not remove the tie wraps or attempt to change the cable. The cable should last the life of the Analyzer PRO Instrument. The cable type is as follows: • Category 5e, SF/UTP Patch 4P • IEC 61156-6 LSHT (or equivalent) The exposed end of the Ethernet cable has an RJ-45 plug like that shown in the photo at right.
Crossover Cable: When held with both ends as shown, conductors up, the wire patterns are different. Note the left plug – the order of solid wires is orange, blue, green, and brown. On the right plug, the order of solid wires is green, brown, orange, and blue. On a crossover cable, the pairs are designed to “cross over” the signal when devices are hooked directly to each other, instead of through a network switch.
11 Safety and Power-up The Analyzer PRO is designed for safe operation in a process environment, and is well-sealed against dust, dirt, and wash-down. Do not open the housing or loosen any cable glands, as this may compromise the sealing of the unit. It is allowable to release the mounting clamps which secure the unit, as the housing is sealed behind where the clamps mount. If removing the clamps, always use adequate safety precautions to prevent personal injury, or damage to the Analyzer PRO instrument.
12 Connection to Vision Software Analyzer PRO is designed to operate with Vision software. Vision requires a User ID and password for entry as a security measure. Each user must operate within a “Project” inside Vision. The procedure for creating a Project will be shown. Inside the Project, Vision uses a Data Collection Method (DCM) to communicate with the Analyzer PRO. Please follow this procedure to connect: 1. Click on the Start icon, then click on Vision in the menu as shown.
4. Vision asks to create a Project database as shown. If this location is acceptable, click “OK”. As a rule it is best to use the default location, unless there is an over-riding reason to use another location. 5. Vision opens a screen for configuration of data sources. This enables communication with the instrument through Vision. Highlight “NIRSystems DDA Analyzer PRO Instrument Driver” and click “Configure”. 6. Select and highlight the instrument with the correct chassis ID number.
8. The Analyzer PRO instrument runs an automatic selfchecking routine, which appears as shown. No operator input is required. 9. When finished, the screen indicates successful testing. Click on “Close” to proceed. 10. Vision requests a valid Data Collection Method (DCM) in this screen. Since no DCM has been created yet, click on “New”.
11. The Profess Analyzer sends its configuration to the Data Collection Method – this is a “Window Reflection” system, as shown in the Sampling system “Module” box. The wavelength range is 1100-1650 nanometers. Reference Standardization is a default for this model, and the box is checked. The “Method” name is empty when the DCM is displayed. Enter a name for the method. The name used here is “Window Refl”. Spaces are allowed in the DCM name. Click “OK” when finished. 12.
14. Vision displays the instrument configuration, so the user may confirm that this is the correct instrument. This information is used to create a path in the Diagnostic Database. 15. When the system is ready to run, the Diagnostics menu will become active. Please proceed to the section on Analyzer PRO Diagnostics.
13 Diagnostics Diagnostics are provided to assure ongoing performance of the Analyzer PRO instrument. Upon each connection to the instrument, Self-Test is performed automatically. The instrument monitors itself, and will alert the operator in the event of malfunction. It is wise to institute ongoing testing to monitor instrument performance and operation.
1. Click on “Analyzer PRO Setup/Diagnostic”, then “Run Performance Test”. 2. Vision displays the Instrument Configuration box. This information is used to set up the Diagnostic Database entries for this instrument. If correct, click on “OK”. This box is shown upon each initial connection, and is not shown on subsequent diagnostic tests, as long as the instrument has remained connected to Vision. 3. Vision asks which fiber should be used for the test. The test defaults to the Sample fiber.
5. When the test is finished, the split-screen display will appear as shown. (The test normally takes 9-10 minutes in this configuration.) Double-click in the lower right quadrant to see the tabulated results. 6. The tabulated results show these items: • Scan: 10 is the default value • EOC: Errors on communication this will be “0” nearly all the time.
7. The “OpQual” tab gives acceptance specifications, along with actual results and a “Yes/No” indicator to test status. 8. If a printed copy is needed, click on “Print Report”. A copy is automatically saved to the Vision Diagnostic Database. Click on “Close Report” when finished. NOTE: We advise removing the standards from the sample window when not in use. The intense light beam can warm the standards considerably, which will change their photometric response.
2. Vision shows this selection box, marked “Select ERC Correction File”. The term “ERC” stands for “External Reference Correction”, which is another term for Reference Standardization. Essentially, this is a method to mathematically correct the instrument reference to the equivalent of 100% reflectance. From the CD or DVD drive, highlight the RSS1xxxx file, then click “Open”. 3. Vision prompts the user to place the 80% reflectance standard (R801xxxx) from the XC-1000 set over the sample window. 4.
6. Vision shows the spectrum of the certified 80% Reflectance Standard spectrum, plotted from 1100-1650nm. Chick “OK” to plot the spectrum of the correction. 7. Vision plots the correction spectrum in dark green. This correction spectrum will be applied to the internal reference. Click “OK” to apply the correction. 8. Vision applies the correction, shown in purple. Click “Yes” to save the ERC to the Diagnostic Database. 9.
10. Vision loads the ERC (Reference Standardization) file to the instrument. Click “Print Report” if verification is needed. Click “Close Report” when finished. 11. This enlarged plot shows the full Reference Standardization. Further explanation may help the user understand what is taking place. The magenta plot at the top is a raw absorbance spectrum of the R80 standard, as measured though the instrument fiber paths. The absorbance level is too high, due to fiber absorbance.
13.1.3 Wavelength Certification This test verifies that the wavelength scale of the Analyzer PRO meets parameters specified by the U.S. National Institute of Standards and Technology (N.I.S.T.) for NIR wavelength response using rareearth standards. 1. Click on “Analyzer PRO Setup/Diagnostic”, then “Run Wavelength Certification”. 2. The default number of scans is 10. The default selection is “Wavelength Standard Analyzer PRO”. Click “OK”. 3.
7. This test runs in about two minutes. Splitscreen results appear as shown. Double-click on the lower right quadrant to see full tabulated results. 8. There are four wavelength peaks used, which serve to characterize the full wavelength scale of the instrument. N.I.S.T. uncertainty is applied for rare-earth-type wavelength standards, shown as a tolerance of +/-1.0 nm. The Pass result is shown at the bottom of this report for each wavelength peak tested. 9.
13.2 MicroBundle Fiber Optic Sensing First, verify that the Data Collection Method is correctly set up. 1. Please verify that the Sampling System appears as shown below, in the area marked by the box. Note that the drop-down menu shows three different types of probes which may be used. We will use the Interactance Reflectance Probe with Purge. This probe is normally configured with a “Purge” time and a “Settle” time set in the DCM.
1. Click on “Analyzer PRO Setup/Diagnostic”, then “Run Performance Test”. 2. Vision displays the Instrument Configuration box. This information is used to set up the Diagnostic Database entries for this instrument. If correct, click on “OK”. This box is shown upon each initial connection, and is not shown on subsequent diagnostic tests, as long as the instrument has remained connected to Vision. 3. Vision asks which fiber should be used for the test. The test defaults to the Sample fiber.
5. When the test is finished, the split-screen display will appear as shown. (The test normally takes 9-10 minutes in this configuration.) Double-click in the lower right quadrant to see the tabulated results. 6. The tabulated results show these items: • Scan: 10 is the default value. • EOC: Errors on communication – this will be “0” nearly all the time.
6. If a printed copy is needed, click on “Print Report”. A copy is automatically saved to the Vision Diagnostic Database. Click on “Close Report” when finished. NOTE: We advise removing the standards from the sample window when not in use. The intense light beam can warm the standards considerably, which will change their photometric response. Please place the standards on the window only for current testing, and remove them promptly when finished. 13.2.
3. Vision takes a scan of the internal instrument reference path. Click “OK” to have Vision plot the file spectrum of the Certified 99% Reflectance Reference standard, from the CD. 4. Vision plots the stored file of the Certified 99% Reflectance Reference standard. Position the Certified 99% Reflectance Reference on the probe end, and click “OK”. 5. Vision prepares to scan the Certified 99% Reflectance Reference. Click “OK”. This may take several minutes to complete.
6. Vision plots the spectrum of the internal instrument reference in magenta. Note that the wavelength scale is that of the instrument, 11001650nm. This is normal. The overall plot is scaled from 400-2500 nm, the useful range of the Certified 99% Reflectance Standard. Click on “OK” to proceed. 7. Vision calculates the correction needed to adjust the instrument reference as required. This is shown in green. Click “OK” to apply the correction. 8.
9. Vision asks to upload the ERC to the instrument for use when taking spectra. Click “OK”. 10. When finished, Vision indicates that the correction was properly loaded to the instrument. If a printed copy is needed, click on “Print Report”. The plots on this diagram bear further explanation to help the user understand what is taking place. The magenta plot at the bottom is a raw absorbance spectrum of the internal reference fiber of the instrument.
the 100% reflectance level, though this is not shown on the correction plot. By applying this mathematical correction, sample spectra appear as if taken using an ideal 100% reflective background reference. When correcting the reference, there will always be slight correction differences due to fiber position, placement of the standard, temperature, dust, and other factors. Normally the correction will be good to within several hundredths of an absorbance unit, as illustrated above.
5. Verify that the serial number of the standard is the same as that shown in the Vision prompt box. (A tie wrap may be present to hold the cup in place.) Click “OK” when ready. Vision will start the test. 6. This test runs in about two minutes. Tabular results appear as shown. There are four wavelength peaks used, which serve to characterize the full wavelength scale of the instrument. 7. If a printed copy is needed, click on “Print Report”. A copy is automatically saved to the Vision Diagnostic Database.
1. Please verify that the Sampling System appears as shown below, in the area marked by the box. There is no need to set “Cell” or Detector” as these selections default to the proper settings. 2. Verify that the instrument is correctly shown, and that the Sample Module Type is “Direct Light”. Click “OK”. 13.3.1 Performance Test Follow these steps to run Performance Test: 1. Click on “Analyzer PRO Setup/Diagnostic”, then “Run Performance Test”.
2. Vision displays the Instrument Configuration box. This information is used to set up the Diagnostic Database entries for this instrument. If correct, click on “OK”. This box is shown upon each initial connection, and is not shown on subsequent diagnostic tests, as long as the instrument has remained connected to Vision. 3. Vision asks which fiber should be used for the test. The test defaults to the Sample fiber. (Do not click yet.) The Direct Light system should be tested in the “Reference” position.
4. 4. When the test is finished, the split-screen display will appear as shown. (The test normally takes about 5 minutes in this configuration, on the Reference Channel.) Double-click in the lower right quadrant to see the tabulated results. 5. This is a typical set of Performance Test results for the Reference Channel. The tabulated results show these items: • Scan: 10 is the default value. • EOC: Errors on communication – this will be “0” nearly all the time.
6. To see the test results and acceptance specifications, click on the “OpQual” tab at the bottom of the screen. This is a typical result. 7. If a printed copy is needed, click on “Print Report”. A copy is automatically saved to the Vision Diagnostic Database. Click on “Close Report” when finished. 13.3.2 Reference Standardization (External Reference Correction) Reference Standardization is a method to set the photometric scale of the instrument to a known, repeatable level.
14 Sampling Once Vision Diagnostics have been performed, the user may take reference and sample spectra. In Data Acquisition, these actions are performed. First, click on the Reference icon, which is a white cuvette. When the Reference spectrum is finished, continue below. Next, click on the Sample icon, which is a green cuvette. When the Sample spectrum is shown on screen, it may be saved. To save the sample spectrum, click on the blue diskette icon.
15 Standards and Approvals The Analyzer PRO™ instrument is CE labeled and complies with the following directives: • EMC Directive (2004/108/EC) • Low Voltage Directive (LVD) (2006/95/EC) • RoHS Directive (2002/95/EC) (Restriction of Hazardous Substances) • Packaging and packing and waste Directive (94/62/EC) • WEEE Directive (2002/96/EC) (Waste Electrical and Electronic Equipment) • ATEX Directive, (94/9/EC), Zone 20 (EN 61241-1-2004 – Explosion safety for DUST-Protection by enclosure tD) • IEC
