MIL-DTL-98B
FIGURE 1. Solidification point apparatus.
4.2.1.3 Procedure. Transfer the dried sample to the inner test tube and melt it. Place the
tube in the apparatus and adjust the thermometer so that the bulb is in the center of the
diphenylamine. Stir the molten material vigorously by means of a hand stirrer and carefully note
the point where the temperature begins to rise when solidification begins. Observe the
temperature every 15 seconds until the maximum reading is obtained. Observe the maximum
reading as the setting point of the diphenylamine.
4.2.2 Purity by gas chromatography (alternate for setting point). A DPA control standard
is analyzed every day by gas chromatography fitted with a split/splitless capillary inlet, flame
ionization detector, and a non-polar capillary column. The % Purity analysis for the DPA control
standard is plotted on an individuals/range statistical process control chart. The standard analysis
must be in control prior to evaluating production samples. Out-of-control conditions are
indicated by any one analysis exceeding the upper or lower control limits or a sequence of eight
consecutive analyses on one side of the mean. An out of control data point would invoke a
corrective action plan according to established trouble shooting guidelines.
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