Micromeritics-Cirrus Interface

Micromeritics-Cirrus Interface

User’s Guide

292-42804-00July 2011

© Micromeritics Instrument Corporation 2011. All rights reserved. Printed in the U.S.A.

Micromeritics-Cirrus Interface Table of Contents

TABLE OF CONTENTS

Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

Documentation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

Conventions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

Starting the Software . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

Exiting the Software. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

Recipe Control Menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

Start Automatic Sequence . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

Push Buttons. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

Configuring an Automatic Sequence . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

Starting an Automatic Sequence . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8

Changing Axes and Legend Properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

Viewing Data with RGA Recall. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

Start Create/Edit Recipe. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

Creating or Editing a Recipe . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

Start Easyview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

Start Detector Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

Specifying Calibration Parameters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

Start Temperature Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22

Performing a Temperature Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22

Entering a Scaling Equation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

Start Manual Recipe. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26

Library . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

Turning Off the Cirrus Mass Spectrometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

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Micromeritics-Cirrus Interface User’s Guide Introduction

Introduction

The Micromeritics-Cirrus Interface Software is used with Micromeritics AutoChem 2920 and 2950 analyzers integrated with an MKS Cirrus Mass Spectrometer. This software runs within the MKS Process Eye Professional software.

The Micromeritics-Cirrus Interface software allows you to:

• automatically collect data with the Cirrus mass spectrometer via a trigger signal from the AutoChem

• customize Peak Jump recipes

• access standard operations, including Analog Scan, Barchart Scan, Peak Jump Scan, Leak Check, and data storage

• calibrate detectors

• scale the AutoChem sample thermocouple signal

The Interface Software enables you to control the analyzer via recipes. A recipe is a set of commands that are transmitted to and from the analyzer, acquiring and displaying data accord-ing to the parameters included in the recipe. Micromeritics has included preset parameters in the software, enabling you to create Peak Jump recipes with just a few keystrokes. Recipes can be saved for future use.

Documentation

This User’s guide provides a description of the commands included in the Micromeritics-Cirrus Interface and instructions on how to use them. It does not include descriptions for all commands related to the Cirrus software. Documentation for Cirrus-specific software, as well as this User’s Guide, can be accessed as follows:

1. Navigate to the directory into which the Micromeritics-MKS application was installed.

2. Open the subdirectory named Manuals and double-click on the desired manual.

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Conventions Micromeritics-Cirrus Interface User’s Guide

Conventions

This User’s guide uses the following conventions:

Starting the Software

To start the interface software:

• Double-click the Process Eye Professional software icon on your desktop, or • Use the Windows Start command to open the Process Eye Professional software.

Exiting the Software

To exit the interface software, click Recipe > Exit on the Process Eye Professional main menu.

Indicates important information pertinent to the subject matter.

Provides information that helps you prevent actions that may damage the analyzer or one of its components.

Blue words Indicate a link to additional information about the subject matter.

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Micromeritics-Cirrus Interface User’s Guide Recipe Control Menu

Recipe Control Menu

All functions for the Micromeritics-Cirrus Interface software are accessed via the Recipe Con-trol menu. This menu appears automatically when the Process Eye Professional software is started.

Start Automatic Sequence Allows you to collect data automatically via the AutoChem digital trigger.

Start Create/Edit Recipe Allows you to create Peak Jump recipes for the Automatic Sequence mode.

Start Easyview Allows you to access directly a number of operations including different scan modes and diagnostics.

Start Detector Calibration Allows you to calibrate the Faraday and SEM detectors.

Start Temperature Calibration Allows you to calculate the scaling equation for the AutoChem sample thermocouple signal.

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Recipe Control Menu Micromeritics-Cirrus Interface User’s Guide

Start Manual Recipe Allows you to quickly start and stop recipes created using the Recipe Wizard.

Library Allows you to view mass spectral data for a variety of compounds.

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Micromeritics-Cirrus Interface User’s Guide Start Automatic Sequence

Start Automatic Sequence

The Automatic Sequence command enables you to:

• automatically collect data via the AutoChem digital trigger.

• automatically export data files, which can be imported into the AutoChem analyzer application.

• control the filament for each recipe.

This window displays the current sequence configuration, which includes a list of recipes and their associated run conditions.

Push Buttons

The following push buttons are located on the Automatic Sequence dialog:

Begin Automatic Sequence Starts the sequence of recipes (refer to Starting an Automatic Sequence, page 8).

Abort Automatic Sequence Enabled when the Automatic Sequence is started. Clicking this button stops the sequence run.

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Start Automatic Sequence Micromeritics-Cirrus Interface User’s Guide

Save Automatic Sequence

Enabled when asequence is not running

Displays the Save Sequence dialog, allowing you to save the current sequence.

You may choose an existing file from the drop-down list (the file will be overwritten with the current data), or you can enter a name in the field provided.

Load Automatic Sequence

Enabled when asequence is not running

Displays the Load Sequence dialog, allowing you to load an existing sequence.

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Configuring an Automatic Sequence

You can make changes and additions to the current automatic sequence using the table in the window as described below.

1. Use the and buttons to add and remove recipes as desired.

2. Click the down arrow to the right of the Recipe Name if you wish to choose a different Recipe; a drop-down list containing all saved recipes is displayed.

3. Enter a name for each data Process Eye data file in the respective Save As column. If you do not specify a name, the data file will default to the Recipe Name.

A sequential 6-digit numerical tag is added to each file name. For example, Air will be saved as Air_000001.SI-d if no previous versions exist. The file is saved to the recipe-specific folder in the default Process Eye data directory.

Example: C:\Process Eye\Data\Air_000001.SI-d

4. Select the check box in the Export as Text ? column for each recipe you wish to export automatically to a text file. Text files are exported to the recipe-specific folder in the default Process Eye data directory, with the extension txt.

5. Select the check box in the Filament Enabled? column to have the filament turned on during recipe initialization.

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Starting an Automatic Sequence

After you have selected the recipes for the run, you are ready to start the sequence.

1. Click the Restart After Sequence Completion? option if you wish to have the sequence restart upon completion of the last recipe in the list.

2. Click Begin Automatic Sequence.

The first recipe is initialized and a tab with the recipe name is added to the Recipe Information window.

Waiting displays in the Status column until AutoChem Digital Trigger 1 is set to the high (1) state. The Trigger can be 1) preset in the analysis conditions portion of the AutoChem sample file, or 2) set manually using the AutoChem schematic when you start the automatic sequence.

Analysis conditions AutoChem sample file

Before the Start Recording step, insert a Set Outputs step; enable digital output D01 to be used as the trigger.

After the Stop Recording step, insert a Set Outputs step; disable digital output D01.

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3. After the trigger is enabled, the recipe is launched and data collection begins.

A message in the Recipe Information window states that data collection has started and displays the directory in which the data file is saved.

Two panes, one with atomic mass trends and one with the scaled AutoChem sample temperature, are opened. You can edit certain parameters of the mass spectra and temperature axes from these panes (refer to Changing Axes and Legend Properties, page 11).

AutoChem Instrument schematic at time of automatic sequence

Enable manual control and right-click in the Auxiliary I/O display window. Select Digital Output 1.

AutoChem Sample temperature

Atomic mass trendsPane 1

Pane 2

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When the AutoChem Digital Output 1 is set to low (0), the recipe stops running and closes the data file. The Trend View windows are closed and the Automatic Sequence window is displayed.

Completed is shown in the Status column for the recipe that finished. If there is more than one recipe in the sequence list as is shown here, the next recipe in the sequence is initialized. Waiting displays in the Status column for the current sequence. After the digital trigger is enabled, the recipe launches and data collection begins. (Refer to page 8 for information on enabling the digital trigger.)

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Changing Axes and Legend Properties

1. Select the graph in the pane in which you wish to make changes and right-click; the Trend Display Pane and Channel Properties dialog is displayed.

This dialog contains a list of the mass peaks that are associated with the current recipe. Use the check box to display or hide a mass; checked will display and unchecked will not.

You can also access this dialog by clicking in either graph area and choose the pane from the drop-down list.

• Choose Trend Pane 1 for the mass spectra

• Choose Trend Pane 2 for the AutoChem sample temperature

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2. Click Next; the Properties for Trend View Pane Y-axis dialog is displayed.

3. Edit the values in the Max value and Min value fields; this applies limits to the:

• partial pressure for the mass spectra (Pane 1) • temperature scale for the AutoChem (Pane 2)

4. Select the Log scale option to display the y-axis in logarithmic form; leave it unchecked to display the y-axis in linear form.

You can also edit other parameters in this dialog if desired. For example, you can edit the Title, display a grid, etc. Refer to the Process Eye Professional manual for additional information.

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5. Click Next; the Time Axis Display and Legend Properties dialog is displayed.

6. Select the Display elapsed time option to change the elapsed time displayed on the time axis (x-axis), then edit the fields as desired.

You can also adjust the span time; the default is 10 minutes.

7. Click the Save all the settings as a new or modified view definition option if you wish to have the modified settings be saved as the defaults.

8. Click Finish to save changes and return to the graph display.

You can also edit other parameters in this dialog if desired. For example, you can edit the time origin, the legend, etc. Refer to the Process Eye Professional manual for additional information.

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Viewing Data with RGA Recall

Only a limited amount of spectra and temperature data is stored in the data buffer used for the live display. Therefore, some data may appear truncated when viewing in ProcessEye. An aux-iliary program called RGA Recall has been included so that you can review the entire set of data. To access RGA Recall:

1. Using Windows explorer. navigate to the applicable data directory and locate the desired data file.

2. Right-click on the file and select Open with RGA Recall from the menu; the entire data set is displayed.

You can edit certain parameters of the mass spectra and temperature axes panes (refer to Changing Axes and Legend Properties, page 11).

If the file you attempt to open is currently running, the file will not open. An error message is displayed and allows you to open a copy, or you can wait until the file is inactive and try RGA Recall again.

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Micromeritics-Cirrus Interface User’s Guide Start Create/Edit Recipe

Start Create/Edit Recipe

This command enables you to create and configure Peak Jump Recipes (or edit existing ones) for the Automatic Sequence mode. A recipe specifies the actions that the Cirrus software is to take during data acquisition.

Creating or Editing a Recipe

1. Select an existing recipe or enter the name for a new one, then click OK; the Recipe Settings dialog is displayed.

Use the (plus) and (minus) buttons to the right of the Accuracy field to add or delete a mass to the Peak Jump scan.

Click the down arrow to choose

and edit an exiting recipe.

Enter a name to create and specify parameters for a new recipe.

The AutoChem sample thermocouple signal is included in each Peak Jump recipe you create.

Adds a mass below the selected one. The ID is added automatically; all fields contain program defaults (shown above as ID #3).

Deletes the selected mass.

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Start Create/Edit Recipe Micromeritics-Cirrus Interface User’s Guide

2. Select and edit the Mass field as desired. Refer to the Library if mass spectra info is needed.

3. Click the down-arrow to the right of the Detector field to choose the detector to be used for the selected Mass.

The detector options allow you to select the Faraday detector or any of the three gain configurations.

4. Select the Skip On Saturation? option (recommended). When this option is selected, masses that saturate the SEM detector (Mult1, Mult2, or Mult3) will be removed from the recipe after five consecutive saturated measurements.

5. Click the down arrow to the right of the Accuracy column and select the accuracy level.

This parameter controls the time for converting the signal in the analog to digital electronics. The range is 0 (shortest scan with the lowest noise filtering) to 8 (longest scan with the highest noise filtering).

6. Click OK to save changes and close the dialog. If you click Cancel, all changes will be discarded.

Scanning for concentrated species (>20% of mixture composition) on the Mult1, Mult2, or Mult3 detector is not recommended.

For recipes where a short cycle time is crucial, use only one detector (Faraday, Mult1, Mult2, or Mult3). Switching between detectors involves changing settings for internal electrical components, resulting in a high cycle time.

Saturating the SEM detector with a high concentration of ions may damage the detector.

For recipes where a short cycle time is crucial, choose the same accuracy level for all masses.

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Micromeritics-Cirrus Interface User’s Guide Start Easyview

Start Easyview

This button launches the EasyView suite, allowing you to access typical RGA operations.

When Easyview is activated, the name of the Start Easyview button changes to Stop Easyview; simply click this button when you wish to exit Easyview.

A brief description of the functions contained on this dialog are shown below. Refer to the Easy View and Process Eye User Manuals for details.

Analog scan mode is started (or stopped if running)

Bar chart scan mode is started (or stopped if running)

Leak Check scan mode is started (or stopped if running)

Peak Jump scan mode is started (or stopped if running)

When started, adds the Peak Settings button to the Easyview window

Visible when Peak Jump mode is activated; allows you to edit recipe parameters

Disk Store; allows saving of data

Filament status; turns active filament off (blue) and on (red)

Filament number; allows you to toggle between filaments

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Start Easyview Micromeritics-Cirrus Interface User’s Guide

Diagnostics; enables you to perform a diagnostic on the Cirrus electronics and associated sensor.

Returns the status window to the General Information page.

Displays the status of the turbo pump, manifold heater, and capillary heater.

Activates Tuning mode; enables you to adjust the tuning of the RGA (peak alignment and resolution).

Calibration mode; allows you to have a calibration factor calculated for converting the measured ion-current to the gas being used.

It is recommended that you use the Start Detector Calibration on the Recipe Control Menu for this calibration (explained on page 19).

Source Ion Source drop-down list; allows you to change the ion source.

Opens the Degas Settings page, allowing you to degas the ion source of selected MKS RGAs.

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Micromeritics-Cirrus Interface User’s Guide Start Detector Calibration

Start Detector Calibration

This option enables you to calibrate the Faraday and SEM detectors. Detector calibration is recommended at the beginning of each workday when the Cirrus analyzer is used on a daily basis.

A Faraday calibration compares the Faraday detector ion current associated with a particular mass against the known partial pressure of that mass. A Faraday calibration defines the basic ion source sensitivity in amps per pressure unit for a given set of ion source conditions.

A Multiplier calibration uses the basic ion source sensitivity to find a voltage that amplifies the ion source signal by a given gain setting.

The calibration may be performed with a variety of gas species, both pure and mixtures. The composition of the gas must be well known.

Specifying Calibration Parameters

1. Click the down-arrow to the right of the Select Gas field and choose the applicable gas.

2. Faraday Calibration:

a. Enter the inlet pressure (in Torr) in the Pressure field; typically 760 (atmospheric pressure). Table 1. Recommended Configuration Settings for Calibration, page 21 provides a list of recommended conditions for common gases when using an inlet pressure of 760 Torr.

b. Enter the mass in the Mass field. Typically, this is the mass of dominant species in the calibration gas.

For example: if using pure argon as the calibration gas, the entered mass would be 40. If using air as the calibration gas, the entered mass would be 28 for nitrogen.

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Start Detector Calibration Micromeritics-Cirrus Interface User’s Guide

c. In the Percentage field, enter the percentage contribution of the partial pressure of the selected mass to the inlet pressure entered above (step a).

For example: if using pure argon as the calibration gas, enter 100% for the contribution of mass 40. If using air as the calibration gas, enter 78% for the contribution of mass 28 (diatomic nitrogen).

3. Multiplier Calibrations:

a. Enter a mass that will not saturate the SEM detector. This is the mass used to perform a calibration against the comparative Faraday detector reading.

For example: if using pure argon as the calibration gas, enter mass 36 (mass 36 has a 0.337% contribution to the partial pressure of pure argon). If using air as the calibration gas, enter mass 29 (mass 29 has a 0.57% contribution to the partial pressure of air). Use the same mass for all three multiplier detectors.

b. The values in the Gain fields are appropriate in most cases and should remain as defaulted.

4. Click Run to begin calibration.

The Faraday calibration and SEM calibrations will run sequentially. Upon completion of all calibrations, you may be prompted to click Finish, at which time the Calibration window containing results for each calibration is displayed.

5. Click Save; the Save Confirmation dialog is displayed.

6. Click OK to overwrite the current calibration and close the dialog.

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Micromeritics-Cirrus Interface User’s Guide Start Detector Calibration

7. Click Stop Detector Calibration on the Recipe Control menu to close the calibration window.

Table 1. Recommended Configuration Settings for Calibration

Gas Pressure Faraday Mass Percentage Multiplier Mass

Air 760 28 78 29

Pure Nitrogen 760 28 100 29

Pure Argon 760 40 100 36

Pure Helium 760 4 100 8

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Start Temperature Calibration Micromeritics-Cirrus Interface User’s Guide

Start Temperature Calibration

This option enables you to calibrate the AutoChem sample thermocouple signal.

When using the standard AutoChem-MKS Cirrus interface cable, the AutoChem sample ther-mocouple signal is transmitted to the Cirrus on analog input channel 4. To collect temperature data, the analog input signal (in volts) must be scaled to temperature in degrees Celsius ( ºC).

Performing a Temperature Calibration

1. Ensure that the AutoChem furnace is closed and a sample tube is installed.

2. Start the AutoChem software. Open the Instrument Schematic and enable manual control.

3. Right-click on the furnace icon, then select Set Temperature.

a. Enter 100 in the Set point field.

b. Enter 20 in the Ramp rate field.

c. Click OK.

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Micromeritics-Cirrus Interface User’s Guide Start Temperature Calibration

4. Observe the Sample Temperature reading on the AutoChem instrument schematic. When the sample temperature reaches approximately 100 ºC and stabilizes:

a. Enter the AutoChem sample temperature in the Point 1: Temperature field on the Temperature Calibration window.

b. Click the Measure Voltage button for Point 1; the analog input voltage will be associated with the AutoChem sample temperature and the measured voltage displayed at the end of the row.

5. Right-click on the furnace icon, select Set Temperature.



c. Click OK.




Furnace icon

Observe this reading

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Start Temperature Calibration Micromeritics-Cirrus Interface User’s Guide

7. Right-click on the furnace icon, select Set Temperature.



c. Click OK.




9. Return the furnace to room temperature. Right-click on the furnace icon, select Set Temperature.



c. Click OK.

10. After all three temperatures have been entered and associated with input voltages, the Calibrate button is enabled; click Calibrate. A linear fit is applied to the collected points to determine a scaling equation. The temperatures, associated analog voltage values, and the Slope and Intercept results are displayed.



13. Click Stop Temperature Calibration on the Recipe Control menu to close the calibration window.

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Micromeritics-Cirrus Interface User’s Guide Start Temperature Calibration

Entering a Scaling Equation

As an alternative to fitting a line to three temperature and analog signal values, you can manu-ally enter a scaling equation for the thermocouple signal.

1. Where New Values is displayed, enter the desired values in the Slope and Intercept fields.

2. Click Re-Plot to display the new scaling function on the chart.



5. Click Stop Temperature Calibration on the Recipe Control menu to close the calibration window.

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Start Manual Recipe Micromeritics-Cirrus Interface User’s Guide

Start Manual Recipe

This option allows access to recipes created using the Recipe Wizard. For detailed instructions on using the Recipe Wizard, refer to the Recipe Wizard User Guide included with the Cirrus II documentation.

1. Click the down-arrow to the right of the field.

2. Select the desired recipe and click Run; the recipe is displayed in the window.

3. Click Stop Manual Recipe to close the window.

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Micromeritics-Cirrus Interface User’s Guide Library

Library

The Library allows you to access mass spectra for a variety of compounds.

1. In the File Name list, simply double-click on the desired compound to display mass spectral data.

2. Click the X in the upper right corner to close the dialog.

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Turning Off the Cirrus Mass Spectrometer Micromeritics-Cirrus Interface User’s Guide

Turning Off the Cirrus Mass Spectrometer

The Cirrus should be allowed to run continuously unless it will be unused for an extended period of time or needs to be shut down for maintenance.

Perform the following to properly turn off the mass spectrometer:

1. Switch off the Capillary and System heaters.

2. Switch off the filaments.

3. Wait 10 minutes to allow the filaments to cool.

4. Click the Pump button to stop the turbo, you should be able to hear the pumps stop and the vent valve open after a few minutes.

5. Wait 5 minutes for the system to cool further and come to a full stop.

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Micromeritics-Cirrus Interface