Perform a Reference Material Analysis

 

In 21CFR11 environments, users are required to login to the Confirm application to start an analysis. Once the analysis window is opened, manual control is disabled until the analysis has completed. During analysis, pausing and resuming is allowed, however, steps cannot be skipped.

A reference material analysis is used to verify the analyzer is operating properly and producing optimum results. These methods provide specifications for critical report quantities and reporting of whether quantities are in or out of specification.

When running a reference material analysis, use the appropriate reference material provided in the accessories kit to perform this analysis. The results should match those shown on the label of the reference material bottle, within the tolerance level.

  Ensure the analyzer safety shield is closed before beginning an analysis. If the analyzer is operated at an excessive pressure, the sample or balance tube could become dislodged from its port, possibly causing personal injury or damage to the equipment.
  1. Go to File > New Sample > [.SMP] to create a new sample file.
  2. Click Replace All. Locate and select the file Carbon.smp. Click Load. This file contains the appropriate conditions for analyzing the carbon reference material. All values will be copied into the new sample file. Edit fields as needed.
  3. Click Save As, enter a new file name if necessary, click Save, then click Close.
  4. Clean and label a sample tube. If installing a new balance tube, clean and label it also.
  5. Determine the sample mass.
  6. Degas the sample using a degassing unit.
  7. Install the sample tube with degassed sample on the sample port.
  8. Install the balance tube (if not installed) on the balance port.
  9. Fill the Dewar with liquid nitrogen to about 5 cm (2 in.) from the top. Allow the Dewar to equilibrate to ambient conditions (approximately 30 minutes).
  10. Close the sample compartment door.
  1. Go to Unit [n] > Start Analysis.

  1. Click Browse. Locate and select the sample file created previously for this analysis. Click Open.
  1. Click Report After Analysis.
  2. Select Report after analysis and Preview as the destination. Click OK.
  1. Click Start.
  2. Compare the BET Surface Area in the report with the BET Surface Area on the reference material bottle.
    • If results are within tolerance, the analyzer is operating properly.
    • If results are not within tolerance, refer to the following table for possible causes and actions. After performing the action, perform the reference material analysis again.
    CauseAction
    The sample was not degassed properly.Degas the sample again.
    The gas lines are not clean.Clean and verify the gas lines.
    The measured free space is too high. This indicates the helium may not be pure enough.Helium must be 99.995% pure.