thermo scientific Nicolet Summit X HTRN Spectrometer User Guide

Nicolet Summit X HTRN
Quick Start Guide

Nicolet Summit X HTRN Spectrometer

This guide demonstrates how to set up the Thermo Scientific™ Affirma™Horizontal Transmission Lubricant Analysis System for the Nicolet™ Summit™ X Fourier transform infrared (FT-IR) spectrometer and perform a basic analysis.
The system consists of a Pearl Horizontal Transmission (HTRN) accessory and baseplate that fit in the spectrometer sample compartment.
Our OMNIC Paradigm software and customized workflows step you through each sample analysis.

Figure 1-1: Nicolet Summit X HTRN Lubricant Analysis System

Unpack the Pearl HTRN Accessory

To prevent condensation, which can damage internal optics, leave the Pearl HTRN accessory and components in their plastic shipping bags for 4 hours after delivery to allow them to slowly adjust to room temperature. Save the packing materials for storing or transporting the accessory.

❖ To unpack the Pearl HTRN accessory

1. Remove all components from their shipping boxes.
2. Wait 4 hours and then remove any components from their plastic shipping bags.
3. Verify the order is complete (compare against packing list).

Prepare the Nicolet Summit X Spectrometer

Before you install the Pearl HTRN accessory, follow these steps to prepare the Nicolet Summit X spectrometer.

❖ To prepare the spectrometer

1. Set up and install the Nicolet Summit X spectrometer and its associated computer according to the provided instructions. Skip this step if you are using a Nicolet Summit X spectrometer that is already installed.

2. Remove any existing accessory from the spectrometer.
   Grasp the front and back of the accessory and lift it straight up and off the spectrometer.

3. If the spectrometer is not powered on, turn it on by pressing the power button on the back panel.

Note If you powered on the spectrometer in step 3 above, wait 4 to 6 hours for the spectrometer to warm up before acquiring data with the Affirma Lubricant Analysis System.

Install the Pearl HTRN Accessory

The Lubricant Analysis System includes a Pearl HTRN accessory and its custom baseplate designed to fit in the sample compartment of a Nicolet Summit X spectrometer. The baseplate fits over two alignment pins in the spectrometer sample compartment and is held in place by strong magnets. Once the accessory is mounted on the baseplate, you can install and remove them as a unit.

❖ To install the Pearl HTRN Accessory

1. If the baseplate is not attached to the Pearl HTRN accessory, orient the baseplate as in the image below (small thumbscrew pillar faces front) and then lower the baseplate onto the  spectrometer.
   Figure 1-1: Baseplate orientation Once the two alignment holes in the baseplate line up with the alignment pins in the spectrometer sample compartment, the baseplate seats itself.

2. Grasp the Pearl HTRN accessory by its side handles and lower the accessory onto the baseplate.

3. Tighten the thumbscrew into the middle front pillar.
   Figure 1-2: Tightening HATR accessory thumbscrew Note To remove the accessory, grasp the accessory by its side handles and lift the accessory and the baseplate straight up and off the spectrometer. Store the accessory in a clean, dust-free environment such as its shipping box or a cabinet.

Install the sample windows

The Pearl HTRN accessory comes with a set of zinc selenide (ZnSe) transmission windows that provide a 100 micron (0.10 mm) sample pathlength. The windows are a matched set. They are marked with the window material, serial number and sample pathlength, followed by a “W” (i.e., “wedged”) which means the bottom window is set at an slight angle. The angled bottom window optimizes the resulting sample spectra for both qualitative and quantitative measurements.

NOTICE

• Wear recommended gloves to install sample windows.
• Handle sample windows gently and do not touch the window material with your bare hands.

Materials needed:

• Powder-free nitrile gloves
• Top window housing (provided)
• ZnSe top and bottom window assemblies (provided)
• 1.5 mm hex (or Allen) key ball driver (provided)

❖ To install the transmission sample windows

1. Gently pull out the accessory sample tray and make sure the tray is free of obstructions. If necessary, use a small, clean laboratory brush to remove any dust or debris.
   Figure 1-1: HTRN accessory sample tray

2. Install the bottom window assembly.
   The bottom window assembly fits in the recessed area. Hold the bottom window assembly right side up (see image below) and gently lower it into the recessed area.
   Figure 1-2: Bottom window assembly installation

3. Carefully rotate the window assembly until its alignment hole (the larger of the two holes) fits over the alignment pin on the sample tray.
   Figure 1-3: Alignment hole and pin fit together

4. Install the top window assembly:
   The top window assembly fits into the underside of the top window housing and is held in place by a set screw.
   a. Use the 1.5 mm hex key ball driver to loosen the set screw so that it doesn’t protrude into the recessed area (you don’t need to remove the set screw).
   Figure 1-4: Recessed area and set screw access b. While holding the top window assembly right side up, line up the groove along the edge of the top window assembly with the alignment pin in the top window housing and gently lower the window assembly into the housing.
   Figure 1-5: Groove and alignment pin c. Use the 1.5 mm hex ball driver to gently tighten the set screw.
   NOTICE
   Do not overtighten the set screw or you may cause distortions in your acquired date.

5. For safekeeping, place the top window housing in the sampling position on the sample tray and close the tray. See the next section for details.

Top window housing – sampling and load position
The top window housing must be in the sampling position for data acquisition. Move the housing to the load position when you are ready to clean the sample windows or load a sample.

❖ To place the top window housing in the sampling position

1. Hold the top window housing right side up (see image below) and place it on the left side of the sample tray, lining up the alignment hole with the central alignment pin on the sample tray.

Figure 1-6: Top window housing in sampling position

❖ To place the top window housing in the load position

1. Lift the top window housing off the sample tray.
2. Turn the top window housing upside down and place it on the right side of the sample tray, lining up the alignment hole with the central alignment pin.
   Figure 1-7: HTRN top window housing in load position

Install the software and Affirma workflow package

Follow the steps below to install the Affirma workflow packages.

❖ To install the Affirma workflow package

1. Run the Setup.exe file to install the corresponding Affirma package for your accessory, then reboot your computer. Each accessory has its own file.

2. Start OMNIC Paradigm software.

3. Connect to your instrument. To do so, go to Configure > Connectivity > Nicolet Summit.

4. Go to Configure > View > Operator. This will put the software in Operator mode.

5. In the upper left-hand corner, select the triple bar button, then choose Administrator and enter the password.

6. Select Open in the upper right-hand side of the screen and select the following path: \
   C:\Users\Public\ Documents\Thermo Scientific\OMNIC Paradigm\Factory Packages
   Figure 1-1: Open folder icon in OMNIC Paradigm software Operator mode

7. Select the .rdep file for your accessory and select Open.
   Note The .rdep file will only appear if you have followed these steps in order and installed the appropriate Setup.exe file.

8. In the upper left-hand corner, select the triple bar button, then select Home to exit Operator mode.
   The Affirma workflows for your accessory are now available in Operator mode.
   Figure 1-3: OMNIC Paradigm software home screen with Affirma workflows

Perform a background measurement

The system requires a background spectrum for making measurements with the Affirma Horizontal Transmission Lubricant Analysis System. The background should be updated after 2 hours of continuous use.

❖ To perform a background measurement

1. Install the Pearl HTRN accessory in the spectrometer sample compartment.
2. Open the sample tray.
3. In OMNIC Paradigm software Operator mode, select the HTRN Setup category and then select the Background HTRN workflow.
4. Follow the instructions in the workflow to complete the background measurement.

When the background measurement is completed, follow the instructions in the next section to run the calibration check.

Run the Affirma calibration check

After you complete the background measurement, run the calibration check with the Pearl HTRN accessory installed to verify sample pathlength.

Materials required:

• FT-IR Squalane Liquid Calibration Kit (includes high purity squalane and dropper bottle)
• Clean, non-abrasive laboratory wipes (unscented and lotion-free; paper napkins work well)
• Powder-free nitrile gloves

CAUTION
Avoid chemical exposure. Squalene is a chemical irritant. When handling squalene:

• avoid contact with skin and eyes
• avoid inhaling vapor or mist
• wear gloves that provide adequate protection

Note Use only high grade (>95%) squalane. Do not sample squalane directly from its original container. Pour it into another clean, labeled container for routine use.

❖ To run the calibration check

1. Make sure the Pearl HTRN accessory is installed in the spectrometer sample compartment.

2. Clean the sample windows. See Clean the sample windows for instructions.

3. Make sure the appropriate Background workflow has been performed. See Perform a background measurement. If a message indicates that a new background measurement is needed, follow the instructions in that section and restart the calibration workflow.

4. In OMNIC Paradigm software Operator mode, select the HTRN Setup category and then select the Calibrate Cell HTRN workflow. The workflow shows its historical results, if any exist.

5. Follow on-screen prompts to continue.

6. When the workflow asks you to load squalene, open the sample tray, move the top window housing to the load position and add three drops of high grade squalane to the sample cup in the bottom window assembly.
   Figure 1-2: Sample cup in load position

7. Place the top window housing in the sampling position and close the sample tray.

8. Click to start the measurement.
   Do not touch the sample tray until all measurements are completed. When the measurements
   are completed, the report is displayed.
   If all the results are within the specified limit(s), click to continue.

9. Clean the sample windows and click to complete the workflow.

See Clean the sample windows for details.

Note If one or more calibration test results are outside the specified limit(s), rerun the calibration test. If the system fails again, contact us.
The system is now ready for you to perform a sample analysis. Before you do that, review the remaining sections in this document which describe the software, explain the safety and operating precautions, and provide tips for running samples as well as cleaning  and maintaining the system.

About OMNIC Paradigm software

Use OMNIC Paradigm software Operator mode to operate the Lubricant Analysis System. The main window provides features for installing and running customized workflows to operate the instrument and instrument diagnostics.
There are two categories of workflows in this package:

• Pearl HTRN Setup workflows
• Pearl HTRN In-Service Lubricant workflows

Pearl HTRN setup workflows

• Run Background. Performs a background measurement with the instrument. The background should be measured every 2 hours during continuous use.

• Calibrate Cell. Measures known material (squalane) to determine sample pathlength. Calculates pathlength and offset values used in sample measurements.
  Note To ensure accurate analysis results, we recommend that you run the Calibrate Cell workflow at least once each week of instrument use.

• Collect Reference. Measures a reference oil sample. Uses the stored reference for sample measurements taken with a “differential” sample workflow.

• Clean Check. Performs a sample measurement through the cell windows without a sample in place to determine if the windows have been properly cleaned.

HTRN in-service lubricant workflows

• ASTM E2412 Direct Petroleum. Intended for petroleum-based sample oils to be measured using the ASTM E2412 standard practice.
• ASTM E2412 Direct Hydraulic. Intended for hydraulic sample oils to be measured using the ASTM E2412 standard practice.
• ASTM E2412 Direct Synthetic. Intended for synthetic sample oils to be measured using the ASTM E2412 standard practice.
• ASTM E2412 Subtract Petroleum. Intended for petroleum-based sample oils that have a matching pure reference oil, where the reference measurement is subtracted from the sample measurement. Use the Collect Reference workflow to measure and  archive the reference oil.
• ASTM D7418 Direct. Intended for any sample oil to be measured using the ASTM D7418 standard practice.
• ASTM D7418 Differential. Intended for any sample oil that has a matching pure reference oil, where the sample measurement is divided by the reference measurement. Use the Collect Reference workflow to measure and archive the reference oil.

system.
| Workflows that measure sample oil content directly (without a reference oil). Direct sample workflows can be based on the ASTM E2412 or D7418 method.
| Workflows that use a pure reference oil measurement to determine sample oil content.

Safety and operating precautions

WARNING
Prevent fire and explosion. If using volatile solvents, provide an active venting system that is free of spark and other ignition sources and prevents flammable vapors from collecting in the atmosphere surrounding the instrument.
To prolong the life of your system, follow these precautions:

• Protect sample windows from thermal and mechanical shock
• Do not leave solvent on the sample windows for longer than 2 minutes.
• Do not attempt to measure materials that are strong acids (pH less than 4), strong bases (pH greater than 11) or strong oxidizing agents
• Do not use chlorinated solvents or materials that may produce HCl or HF vapors with or near the system
• Do not block the vents at the back of the spectrometer

NOTICE
Read the safety guide that came with the spectrometer before operating the spectrometer with the Affirma Lubricant Analysis System installed.

Sampling tips

For optimal sampling with the Affirma Lubricant Analysis System, follow these guidelines:

• A background measurement is required at predefined intervals during continuous use. The workflows display a message when a background is needed. Use the Run Background workflow in the HTRN Setup category to acquire a background spectrum. The background is measured with nothing in the sample beam (pull out the sample tray). We recommend that the time between background collections does not exceed 2 hours.

• The Affirma Lubricant Analysis System can be used to measure aqueous and organic liquids as well as viscous materials such as gels, oils and greases.

• Use one of the sample workflows in the HTRN In-Service Lubricant group to run a sample analysis.
  Note Sample workflows based on a differential (or subtraction) require a new oil reference spectrum. Use the Collect Reference workflow in the HTRN Setup category to acquire a spectrum from your reference material.

• To apply a sample for measurement, open the sample tray and move the top window housing to the load position. Use a disposable pipette to apply two to three drops of sample to the sample cup. (Fill the cup about two-thirds full.)
  Place the top window housing in the sampling position, close the sample tray and start the measurement.
  Do not touch the sample tray until the measurement has completed.
  Tip You can tilt the top window slightly while lowering it into position to help dispel any bubbles. View the sample through the top window to check for bubbles.

• Always clean the sample windows immediately after you finish the analysis. See below for instructions.

Clean the sample windows

Make sure the sample windows are clean before and after taking sample measurements with the Affirma Lubricant Analysis system.

Materials required:

• Small volume of heptane or isooctane
• Clean dropper bottle for cleaning solvent (provided)
• Clean, non-abrasive laboratory wipes (unscented and lotion-free; paper napkins work well)
• Powder-free nitrile gloves

CAUTION
Avoid chemical exposure. Isooctane and heptane are chemical irritants. When handling isooctane or heptane:

• do not ingest
• avoid contact with skin and eyes
• avoid inhaling vapor or mist
• wear gloves that provide adequate protection
• properly dispose of soiled containers, wipes, gloves, etc.

NOTICE
When cleaning the sample windows, avoid using excessive force or you may damage the crystal.

❖ To clean the sample windows

1. Open the sample tray, raise the top window housing a small amount, place a clean, nonabrasive laboratory wipe between the two windows and then lower the housing to soak up most of the material.
2. Move the top window housing to the load position and use a new wipe to gently clean the  upper and lower sample windows and surrounding areas.
3. Place a few drops of cleaning solvent onto a new wipe and use it to thoroughly clean both windows and the area around them.
4. To protect the sampling surfaces, place the top window housing in the sampling position and close the sample tray.

Purge the Accessory

When using the Affirma Lubricant Analysis System to measure volatile materials or materials dissolved in volatile solvents (or if a persistent message tells you the background measurement has artifacts due to unknown materials inside the instrument), follow the steps below to purge the accessory.

Materials required: Puffer device (provided)

❖ To purge the accessory

1. Open the sample tray and inspect the sample windows for residual sample.
   If necessary, clean the sample windows again.
   See Clean the sample windows for details.
   When finished, leave the sample tray open.

2. Insert the provided Puffer device into the purge port on the front of the accessory.

3. Squeeze the Puffer five times to expel any vapors from inside the unit.

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