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tion to boiling, and slowly add 10 ml. of a 10-
reached. Make the electrical connections,
percent solution of barium chloride to the
place the bomb in a bucket of cold water, and
ignite the sample. After 10 minutes remove
boiling solution. Continue boiling for 15 min-
utes, and then allow to stand for 2 hours at
the bomb from the water and release the
a temperature just below the boiling point.
pressure at a uniform rate, so that the oper-
ation requires a t least 1 minute. Open the
Filter the barium sulfate precipiate through
bomb, and examine the contents for traces
a tared filtering crucible and wash thoroughly
of unburned sample. If any traces are found
with hot distilled water. Dry the crucible and
the determination shall be discarded and an-
its contents in an oven, and then ignite at a
other test performed.
temperature of 850 50C. Cool in a desic-
cator and weigh. Calculate the increase in Dissolution, precipitation, and cal-
weight of the crucible to percent sulfur con-
culation. --The dissolution and precipitation
tent of the sample, as follows:
of the material shall be carried out as speci-
fied in 4.4.2. The calculation of percent sulfur
content shall be performed as specified in
where: A = weight of barium sulfate pre-
cipitate, grams.
4.4.9 Ether-extractable matter. --Transfer
W = weight of sample, grams.
an accurately weighed sample of approxi-
mately 4 grams of the lump-free material to Alternative method. --The sulfur
an extraction thimble, and extract with ether
content may also be determined with a Parr-
using a tared extraction flask and a Soxhlet
type oxygen bomb, using oxygen from an
extractor, or equivalent. Use a hot-water bath
external source.
or a steam plate as the source of heat, adjust-
ing the applied heat so that ether drips from Apparatus.
the reflux condenser at the rate of 2 to 3 drops Bomb. -- Self-sealing oxygen
per second. Continue the extraction for at
combustion bomb equipped with a double
least 8 hours. Remove the extraction flask
valve (see 6.3),
and evaporate the ether by heating on a steam
bath until approximately 26 ml, of the ether Cup. --Stainless steel cup of a
solution remains. Complete the evaporation
capacity of 6.5 ml.
to dryness by blowing a slow current of dry
air over the solution, Dry the flask to constant Firing wire. --Iron-nickel-chro-
weight in a vacuum desiccator containing sul-
mium alloy wire of 0.0063-inch nominal di-
furic acid, Calculate the gain in weight of the
flask to percent ether-extractable matter. Ignition --The firing wire shall
4.4.4 Volatile matter.
be clean and so arranged that it will touch Apparatus.
the sample when the cup is placed in position
in the bomb. Place 5 ml. of distilled water in Crucible. -- A platinum crucible
the bomb to saturate the oxygen used for
with a capacity of approximately 20 ml. (ap-
combustion with water" vapor. Place an ac-
proximately 25 mm. in diameter and 35 mm.
curately weighed portion of approximately
deep), and equipped with a closely fitting
0.4 gm. of the sample in the cup. Place the
platinum cover.
cup in the bomb, and close the bomb. Tighten Burner. --A Mekker-type burner
the bomb cover firmly to avoid blowing the
having a top approximately 42mm. in diame-
sample from the cup, and allow the oxygen
ter, and giving a flame approximately 16 cm.
to flow into the bomb. Cease the addition of
high (see 6.4). The temperature of the flame
oxygen after a pressure of 40 atmospheres is

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