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submerge it in hot water beside the phosphorus specimen. Use a Mohr pipet fitted with a
pipet filler to transfer 5.75 mL (10.0 g) of molten specimen to the centrifuge tube, keep-
ing the end of the pipet under water while transferring the specimen. Remove the centri-
fuge tube containing the specimen and place it in a cold water bath for a minimum of 5
minutes to solidify the specimen. Apply pressure to one side of the specimen nugget with
a stirring rod to dislodge it from the tube. Pour about 250 mL of toluene into an extrac-
tion flask. Transfer the specimen nugget from the centrifuge tube to a beaker containing
enough acetone to remove water from the specimen surface. Transfer the specimen nug-
get from the acetone to a tared, medium porosity, 30-mL, high form, fritted glass cruci-
ble filled with toluene. Immediately place the crucible containing the specimen nugget in
the neck of the extraction flask and close the flask by placing the distillation trap in
position while introducing carbon dioxide into the opening to keep out all air (see figure
1). Place the stream of carbon dioxide in the top of the condenser and connect the ground
glass joint to the distillation trap. Remove the carbon dioxide from the top of the con-
denser, place a heat source under the flask, and heat until heated toluene vapors melt the
specimen in the crucible. Place the carbon dioxide stream in the top of the condenser,
remove the heat source, and let cool until the specimen filters through. Remove the car-
bon dioxide from the condenser. Place the heat source under the flask and boil gently
until all of the specimen is dissolved in the flask and no traces are left in the crucible.
Place the carbon dioxide stream in the top of the condenser, remove the heat source, and
cool to room temperature. (NOTE: A cold water bath may be placed under the flask if
desired.) Remove the condenser and trap from the extraction flask and place a gentle
stream of carbon dioxide in the neck of the flask. Remove the crucible from the flak,
place in a suction flask fitted with a crucible holder, and wash three times with fresh
toluene. Dry the crucible in the oven at 105C for about 20 minutes, cool to room tem-
perature in a desiccator, and weigh. Calculate the percent insoluble matter in toluene as
follows:
w h e r e : A = Weight of crucible and residue in grams
B = Weight of crucible in grams, and
W = Weight of specimen in grams.
5. PACKAGING
5.1 Packing. Packing shall be level A or C as specified (see 6.2).
5.1.1 Level A. One hundred 2-1/2-pound blocks of WP shall be packed under water
to nominal drum capacity in a 30-gallon capacity steel drum with fully removable head.
The drum shall conform to type III or IV of PPP-D-736. Packing shall also be in accor-
dance with Department of Transportation (DOT) regulations.
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