Vapor Flow Calibration

Use to calibrate the type of vapor to be used when using the optional vapor generator. Associating the analysis data with a vapor generator calibration file allows the conversion of peak area data to volume data. The calibration can be performed either before or after performing the analysis. A single calibration file can be used with multiple analysis files.

  1. Go to File > Open > Sample information.
  2. Enter a calibration file name (.CAL).
  3. Click OK, then click Yes to confirm.
  4. Complete the remaining fields on the Sample Description window, as needed.
  If the window displays in Basic presentation, click Advanced in the view selector drop-down at the bottom of the window.
  1. Select the Analysis Conditions tab.
  2. Select AutoChem III  in the View conditions for drop-down list.
  3. Click Insert, then select Vapor Flow Calibration.

  1. Complete the dialog box according to this table:

Selections Description
Carrier Gas/Loop Gas [drop‑down box] Select the gases to be used for this step and enter the Flow rate.
Description [text box] Description for this calibration.
Flask Temperatures [group box] Enter a value between 20.0 and 120.0 degrees for the Minimum and Maximum.
Filament temperature [selection] Enter the temperature for the filament.
Number of steps [text box] Enter the number of steps (between 3 and 7) for this calibration.
Reflux Temperatures [group box] Enter a value between 20.0 and 100.0 degrees for the Minimum and Maximum.
Set external trigger [check box] If selected, the contact closure used to trigger an external mass spectrometer will be activated. If deselected, the contact closure will be deselected.
Temperature [group box] Enter a value between 20.0 and 150.0 degrees for the Valves and Detector block.
Vapor [drop‑down box] Select the vapor to be used.
  1. Click OK.
  2. Go to Unit [n] > Sample Analysis.
  3. Click Browse and select the sample file just created. Make edits as required.
  4. Click Start.
  5. Select an option from the View drop-down list to observe the progress of the analysis.
  6. When the analysis completes, close the Analysis window.
  7. When the displayed sample temperature reaches the ambient temperature, open the furnace. Use gloves and remove the sample tube. These fields do not require editing; the Reflux and Flask temperatures entered on the Vapor Calibration Experiment window are used.
  1. To edit the calibration file, go to Options > Signal Calibration > New.
 

Use the cotton gloves provided in the accessory kit when handling heated surfaces. These cotton gloves are not intended to protect hands when heated surfaces are above 60 °C.

  1. Select Load Calibration Data and select the sample file for this calibration. The data contained in the file are automatically loaded.
  2. Access the Calculations document on the Micromeritics web page (www.micromeritics.com) for information on calculating the volume of each vapor injection, then enter the values for each peak.
  3. Assess the plot, Goodness of Fit, and Coefficients to decide if the calibration file is acceptable. Use your laboratory’s standards to determine what level of linearity is acceptable. As a general guideline, use a calibration file with a very low value for Goodness of Fit (less than 1 to 2% of the signal), when 1st or 2nd Degree is specified.
  4. To delete any peaks that are outliers, highlight the peak data in the table and click Delete Peak.
  5. Evaluate the results when the degree is changed (select a different degree from the drop-down list).
  6. When satisfied with the calibration file, click Save then click Close.