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It is recommended that the user tare no less frequently than six hours, but certainly if the user suspects anything may have changed on either balance. 
Figure 12. Taring the paired balances at 300 measurements.
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Once the tare is complete, place the sample container on the unknown balance and close the sliding door. Place counterweights from the standard box as close to the mass of the unknown as possible and close the reference balance door. It may be useful to look at the balance LCD screens; the circle shows the rough load on the balance and masses can be roughly equalized by using them. It is important to get the masses within 5 grams. If the red and green traces are more than 5 grams apart after the measurement is started, then press the "Stop" button, add or subtract reference masses, and start the measurement over.
The "Reference Mass" field should be filled with the total mass of the reference masses before the measurement is started. Figure 13 shows the Reference Mass (circled in blue) and the traces of the two balances and their corrected result mass. Note that the reference mass balance began at a value of just under 19 grams and the unknown balance started close to 21 grams; the difference between them is ≤5 grams, so this measurement could be allowed to continue.
Figure 13. Mass measurement on a sample.
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Once the empty cell has been measured the specified number of times, the unit will prompt the user to add the standard(s) to the cell; the "SPHERE_10" standards are found in the wooden box shown in Figure 23. Open the pycnometer cell and place the standard ball(s) into the cell, then close securely. Clicking "Done" will trigger the above analytical steps, including purges, for the standard ball(s). After the replicate measurements on the steel ball(s) are done, the system will prompt the user to remove the standards from the cell. Pressing done at this point shows the expansion (red circle) and analytical cell (black circle) volumes determined by the calibration experiment as shown in Figure 24.
Figure 23. Six sets of steel balls are kept in this box along with the wire tool to extract them from the cells. Do not touch the spheres with bare fingers! Fingerprints don't significantly affect the volume measurement, but will cause the spheres to begin corroding. Wipe them thoroughly off with a Kim-Wipe if it is necessary to do so.
Figure 2324. Final calibration screen for the pycnometer cell.
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After calibration is complete, the user can begin analyzing samples and one standard per six runs as noted above. Double-click on the Volume Dry (cm3) portion of the main screen next to the sample to be studied; normally the SPHERE_10 standards are also listed for the one cell in six to be dedicated for a standard measurement. A window will appear as shown in Figure 24 25 prompting the user to select a cell and to set the number of replicates. It is recommended to use the same number of replicates as the calibration.
Figure 2425. Pycnometer measurement window.
Ensure that the sample is correct and select the cell to be used and the number of replicate measurements to be performed.
Once the user has selected the cell and number of cycles, click the "Measure" button, which will open the pycnometer cell control window (Figure 2526). Place the sample in the cell, seal it, and then click "Done" followed by clicking the "Start" button (circled in blue). Unlike the calibration measurement, the experiment will not start until the "Start" button is clicked.
Figure 2526. Starting a pycnometer measurement on a sample.
The pycnometer will step through the same purge and measurement steps described in the calibration section and when it is finished, will show the screen shown in Figure 2627.
Figure 2627. Sample completed indicator for pycnometer.
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The result should be in the appropriate field, but in case the user double-clicked the wrong volume measurement, MADMax provides the capability to switch the volume measurement from "wet" to "dry" and vice-versa. As shown in Figure 2728, right-click the mass cell and select the "Send this result to the Volume Wet (cm3)" option. If two volumes are already present, this option will instead state "Swap Volume Wet (cm3) to Volume Dry (cm3)."
Figure 2728. Right-click options for the volume measurement.
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If the user wishes, they can also look at a detail of the mass results as shown in Figure 2829. This is a summary of all of the parameters used to determine the volume with the parameters labeled by their database names.
Figure 2829. Review dry volume results window.
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Volume determination by caliper is best used on consolidated, high-porosity samples (e.g., coral or vesicular basalt) as part of Method D. It is not likely to give accurate results when used on soft sediments (Method A).
Double-click on the "Caliper Volume (cm3)" column in the field adjacent to the sample to be analyzed. This will invoke the caliper measurement window as shown in Figure 2930. The user should select cube or cylinder depending on the sample to be measured with the precision caliper.
Figure 2930. Caliper measurement entry screens.
Ensure that the sample being measured is the correct one and click either the "Cube" or "Cylinder" radio button. Make the measurements using the precision caliper (Figure 3031). Enter the measurements for each dimension in centimeters. Once the measurements have been entered, click "Ok" and the result will be transferred to the main screen.
Figure 3031. Digital caliper used for volume measurements.
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The MADMax software will calculate all of the other MAD parameters once any three of four measurements are completed: wet mass, dry mass, dry volume, and wet volume. Once the three measurements related to the chosen method (e.g., Method C: wet mass, dry mass, dry volume) are completed, double-click on the "Methods Completed" field on the line of the sample in question. This will invoke the MAD calculation window as shown in Figure 3132.
Figure 3132. Run MAD Calc window. Ensure the proper sample is shown.
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After the MAD calculation is run, the user may wish to clean up the main screen list of samples. This is done by clicking in the "Done" boxes as shown in Figure 3233. Once the samples to be removed are checked, click the "Refresh Sample List" button and the checked samples will disappear. (Any new samples will also appear.)
Note: Until this step is completed, two (and rarely three) lines will appear in the LIMS reports. Once this step is completed, the extra lines will be canceled.
Figure 3233. Using the "Done" check boxes to clean up completed samples.
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