Thermo Fisher SCIENTIFIC X HATR Lubricant Analysis System User Guide

Thermo Fisher SCIENTIFIC X HATR Lubricant Analysis System

Product Information

The Nicolet Summit X HATR Quick Start Guide provides instructions for setting up and using the Nicolet Summit X HATR Accessory with the Nicolet Summit X Spectrometer. The product is manufactured by Thermo Fisher Scientific and is designed for spectroscopic analysis.

Product Usage Instructions

Unpacking the Pike HATR Accessory

To prevent condensation, which can damage internal optics, leave the Pike HATR 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.

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 by comparing against the packing list.

Preparing the Nicolet Summit X Spectrometer

Before installing the Pike HATR accessory, follow these steps to prepare the Nicolet Summit X spectrometer:

1. Set up and install the Nicolet Summit X spectrometer and its associated computer according to the provided instructions.

Installing the Pike HATR Accessory

The Lubricant Analysis System includes a Pike HATR 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.

1. Orient the Pike HATR baseplate with the Pike label facing front and then lower the baseplate onto the spectrometer. Ensure that the two alignment holes in the baseplate line up with the alignment pins in the spectrometer sample compartment, allowing the baseplate to seat itself.
2. Grasp the Pike HATR sampling plate by the edges and set it on top of the baseplate. Make sure the alignment holes on the underside are at the back of the accessory baseplate.

Installing the software and Affirma workflow package

Follow the steps below to install the Affirma workflow packages:

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 by going to Configure > Connectivity > Nicolet Summit.
4. Go to Configure > View > Operator. This will put the software in Operator mode.

Unpack the Pike HATR Accessory

To prevent condensation, which can damage internal optics, leave the Pike HATR 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 Pike HATR 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 thePike HATR accessory, follow these steps to prepare the Nicolet Summit X spectrometer.

To prepare the spectrometer 1.

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.
2. Remove any existing accessory from the spectrometer.
3. Grasp the front and back of the accessory and lift it straight up and off the spectrometer. 3.
4. 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 Pike HATR Accessory

The Lubricant Analysis System includes a Pike HATR 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 Pike HATR accessory

1. Orient the Pike HATR baseplate with the Pike label facing front and then lower the baseplate onto the spectrometer.
   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 Pike HATR sampling plate by the edges and set it on top of the baseplate. Make sure the alignment holes on the underside are at the back of the accessory baseplate.

Note
To remove the HATR accessory, grasp the baseplate by the front and back edges and lift the baseplate and the sampling plate 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 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 OMINC 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.

4. Nicolet Summit X HATR Quick Start Guide Install the software and Affirma workflow package

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
   Figure 1-2: OMNIC Paradigm software Operator mode Factory Packages location .

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.

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 .

Perform a background measurement

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

To perform a background measurement 1.

1. Install the Pike HATR accessory (sampling plate and baseplate) in the spectrometer sample compartment. 2.
2. Make sure the sampling plate and ATR crystal are clean and dry. See “Clean the ATR Crystal” in this document for instructions.
3. In OMNIC Paradigm software Operator mode, select the HATR Setup category and then select the Background HATR workflow. 4.
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 on the Pike HATR accessory 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. Squalane is a chemical irritant. When handling squalane:

• 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 Pike HATR accessory (sampling plate and baseplate) is installed in the spectrometer sample compartment.

2. Make sure the ATR crystal is clean and dry. See Clean the ATR crystal.

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 HATR Setup category and then select the Calibrate Cell HATR 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 squalane, add just enough high grade squalane to cover the ATR crystal completely.
   Figure 1-2: HATR accessory: add squalane

7. Click to start the measurement.
   Do not touch the spectrometer 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.

8. Clean the ATR crystal and click to complete the workflow. See Clean the ATR crystal.
   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:

• Pike HATR Setup workflows
• Pike HATR In-Service Lubricant workflows

Pike HATR 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 day of instrument use and if you use a different HATR accessory or crystal.

• 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 ATR crystal without a sample in place to determine if the windows have been properly cleaned.

HATR 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 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 Petroleum. Intended for any sample oil to be measured using the ASTM D7418 standard practice.
• ASTM D7418 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.

Safety and operating precautions

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 the ATR crystal from thermal and mechanical shock
• Do not leave solvent on the ATR crystal 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 HATR Setup category to acquire a background spectrum. The background is measured through the ATR crystal (make sure it is clean). 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 HATR 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 HATR Setup category to acquire a spectrum from your reference material.

• To apply a sample for measurement, use a disposable pipette to add just enough sample to cover the ATR crystal completely and then start the measurement.
  Figure 1-1: Application of sample using pipette
  Do not touch the spectrometer until the measurement has completed.

• Always clean the crystal immediately after you finish the analysis. See “Clean the ATR Crystal” for instructions.

Clean the ATR crystal

Make sure the ATR crystal is clean before and after taking sample and background 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

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 ATR crystal, avoid using excessive force or you may damage the crystal. ❖

To clean the ATR crystal

1. Use a clean, non-abrasive laboratory wipe to soak up most of the sample material. Figure 1-1:
   Wiping off sample material with non-abrasive cloth

2. Use a new wipe to gently clean the ATR crystal and surrounding area.

3. Place a few drops of cleaning solvent onto a new wipe and use it to thoroughly clean the crystal and the area around it.

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