1670 ANALYTICAL CHEMISTRY

Operation of this control unit may be seen from the wiring dia- immiscible with water and its flow is regulated with the separator
gram (Figure 2). With the thermoswitch closed, closing of the stopcock, usually to a rate of about 5 ml. per minute. The ex-
line switch causes the pilot light to go on. Depressing the push- tract is collected in an Erlenmeyer flask. When ether is used as
button actuates the relay (&, 110-volt, 60-cycle, normally open), extracting solvent, a drying tube containing anhydrous sodium
starting the clock and delivering current to the heating coil as sulfate is attached to the side arm.
well as to the Variac output. Should the temperature of the After completion of the extraction, the solvent temaining in the
water rise above the preset value the thermoswitch will open. apparatus is displaced by careful addition of water through the
Should water flow be interrupted, the temperature of the sta- funnel until the water level reaches the side arm. With the ex-
tionary water in the chamber will promptly rise because of the ce tion of ether, which first must be evaporated and the' residue
effect of the heating coil, and again the circuit will be opened. tagen up in another organic solvent, the extract may be titrated
directly in the organic solvent (1,2 ) , or assayed in the conven-
tional manner after evaporation to dryness.
PS

Advantages. The apparatus has certain advantages over the
previous model.
In I
dl2-5 STD.
p..-i1~,,,~,------6,60CKET JOINT

Figure 2. Wiring Diagram
AC. 60-cycle 110-volt input C. Clock
LS. Line switch V. Variac output
FS. Fenwal switch HC. Heating coil
PS. Pushbutton switch Ri. Relay
P. Pilot lamp' R2. Rheostat

The speed with which this latter effect ensues can be adjusted
by the setting of the rheostat (Rg, 1000-ohm, 50-watt), and in
practice it has been found possible to have output power turned
off 10 seconds after the water supply is discontinued. If the
pushbutton, PSI is locked down, the flow of current will be re-
sumed should the temperature of water in the chamber fall to 125 m l .
or below the preset level. If the pushbutton is not locked down,
manual resetting is required, and this is sometimes a desirable
feature. In either event, the clock will record the accumulated Elimination of the lower side arm and the baffle plate results
time during which current flows, a quantity often essential in a more durable construction. The solvent enters a t the center
to know when continuous extraction or heating procedures are
involved. of the vortex instead of a t its side, thus permitting improved dis-
ACKNOWLEDGMENT
persion and extraction. The flask can be easily connected to a
reflux condenser for hydrolysis or saponification reactions, fol-
It is a pleasure to acknowledge the encouragement that DeWitt lowed by replacement with the separator column. This technique
Stetten, Jr., has shown to the authors in the conduct of this proj- permits all reactions to be carried out without manual transfer.
ect. Yale J. Topper carried out preliminary runs with this in-
strument and has made helpful suggestions. ACKNOWLEDGMENT

The authors are indebted to Lloyd C. Miller, director of revi-
sion, United States Pharmacopoeia, who suggested the design of
Modification of the Schmall Extractor. Morton Schmall, Charles
the apparatus, to E. G. E. Shafer for his helpful advice, and to
W. Pifer, and Ernest G. Wollish, Products Control Laboratory, J. W. Wilkenfeldt for drawing the blueprint.
Hoffmann-La Roche Inc., Nutley, N. J.
extractor (2) for solvents lighter than water has
TbeenSchmall
HE LITERATURE CITED
modified and improved. (1) Pifer, C. W.,Wollish, E. G., and Schmall, M., J. Am. Pharm.
The apparatus consists of an elongated Erlenmeyer flask with Assoc., Sci. Ed., 42, 509 (1953).
f female ground joint which has a capacity of 50 or 125 ml. and (2) Schmall, hl., Pifer, C. W., and Wollish, E. G., ANAL.CHEX.,24,
a separator column having a side arm and a T male ground joint 1446 (1952).
which connects to the Erlenmeyer flask. A drying tube can be
attached to the separator column by means of a ground joint.
A 250-ml. separator, used as solvent reservoir, and a funnel are Determination of Potentiometric Titration Inflection Point by
fitted to a Y-tube which is connected by means of a socket joint the Concentric Arcs Method. Charles F. Tubbs, Color Print
($1. and Processing, Eastman Kodak Co., Rochester, N. Y.
0 eration. The sample or aliquot of a solution-for example,
a sa& from which the base is to be extracted-is weighed or meas-
ured into the Erlenmeyer flask. A magnetic stirring bar is placed ERTAIN automatic titrating instruments produce a continuous
in the flask, which is mounted on top of a magnetic stirrer. The
separator column is inserted and attached to the reservoir by
C record of potential milliliters of titrant added. The tech-
us.
nique described has proved useful in determining the inflection
means of a Y-tube a t the ball joint. Water is added through the
funnel, so as to bring the volume in the flask to the tip of the point of such a curve or one produced by connecting individual
delivery tube, and the stirrer is set in motion. The desired quan- measurements.
tity of alkali or mineral acid is added through the funnel i n order
to liberate the corresponding free organic base or acid. The reser- Prepare a template by scribing and inking concentric arcs on a
voir is filled with 150 to 200 ml. of a solvent lighter than and sheet of semirigid transparent sheeting. Place the template