Precision of a Simple Flame Photometer

JOHN U. WHITE
The White Development Corp., Stamford, Conn.

To improve the ease and accuracy of sodium and
potassium determinations in biological samples, a
simple flame photometer has been built employing
glass and interference filters, photovoltaic cells, and
a galvanometer. Its air-gas flame is completely
enclosed to prevent atmospheric contamination.
With well-regulated gas and compressed air supplies,
average departures from the average of thirty suc-
cessive readings of ±1% were measured for direct
intensities and ±0.3% for internal standard read-
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ful air pressure regulation, the average departure for
the internal standard measurements increased to
±0.5%. The readings were least affected by gas
pressure changes with a large flame burning rela-
tively little primary air. Their stability with respect
to air pressure changes was constant over a wide
range of conditions. The accuracy obtainable per-
mits the measurement of the small changes in con-
centration that are significant when the normal
range is only a small fraction of the amount present,

ings. With unregulated gas pressure and less care- as in the case of sodium in serum.
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most useful applications of flame photometry are in de- The glass atomizer, .1, is held in the center of a large glass
THE
terminations of the alkali metals, which are easiest by this chamber, C. Sample S is introduced through the funnel in the
top of the atomizer and compressed air through the inlet, CA.
method and most difficult by chemical procedures. Photoelec- The atomizer uses about 2.5 cubic feet per minute of compressed
tric flame photometers suitable for such analyses have been de- air at 9 pounds per square inch and consumes 4 cc. of sample per
scribed by Barnes et al. (1), Berry et al. (2), Bowman and Ber- minute under these conditions. Its sample tube is 0.3 mm. in in-
liner (4), Fox (5), Gilbert et al. (6), Schuhknecht (8), Weichsel- side diameter with no constriction anywhere along its length.
The absence of a constriction is important in avoiding plugging of
baum and Varney (9), and others. A number of these instru- the capillary by dirt and dust. In addition, the capillary is
ments are now commercially obtainable. The instrumentation straight, so that any dirt lodging there is readily pushed through.
has been developed to the point where flame photometry is suit- The atomized sample blows down through a chamber 1.62
able for use in many chemical as well as spectrographic laborato- inches in inside diameter and 5 inches long. At the bottom the
fine fog is separated from the larger drops of liquid in a loop of 0.5
ries. However, for medical applications there is still need for inch tubing. The fog goes out to the burner, and the unused
greater simplicity, so that reliable analyses may be made by rela- liquid goes through a liquid trap, T, to the drain, D. There is an
tively unskilled operators. In addition, the accuracy required in opening in the tubing following the liquid trap to avoid siphoning
determinations such as sodium in blood serum is sometimes not the liquid out of the trap.
The burner is a standard Fisher Type 3-900 for burning city
attainable. In the instrument described the range is restricted
gas, modified for some of the experiments to take various fixed-
to sodium, potassium, and, in some cases, calcium, which permits diameter gas jets instead of its original variable orifice. Its
the use of such simple designs and controls that accidental errors throat area is 0.31 square inch, its grid area, 0.57 square inch, and
are greatly reduced.
The accuracy of the flame photometric
method has been reported in a number of
papers, the most comprehensive being those of
Berry, Parks et al. (7), Bills et al. (3), and Fox.
They have reported accuracies of ± 1 % of the
amount present in the determination of sodium
and potassium, using instruments in which the
atomizer is separate from the burner. Weichsel-
baum and Gilbert have reported accuracies of a
few tenths of 1% when the sample is atomized
directly into the flame. This paper describes a
very simple instrument of the former type and
discusses its stability and precision.
The only factors affecting stability that are
considered are air pressure, gas pressure, and
burner adjustment, the ones that affect the re-
producibility of repeat measurements of the same
sample. These set a limit to the analytical ac-
curacy obtainable from the instrument. By the
use of suitable precautions and calibrations, this
accuracy may be approached but not exceeded.
The effects of such variations as viscosity, pH,
surface tension, etc., are not considered. They
are reported in the references above along with
a summary of the literature on the accuracy of
flame photometry.

ATOMIZER AND BURNER

The atomizer and the burner system are

shown schematically in Figure 1.
394
VOLUME 2 4, NO. 2, FEBRUARY 1952 395

its maximum air inlet area, 0.94 square inch. The fixed gas jets
used had diameters of 0.052, 0.070, 0.082, and 0.100 inch. The
burner is surrounded by a 2-inch glass chimney, CH, 12 inches long.
Air containing atomized sample enters past a baffle into the space
inside the chimney. As there is no opening to the atmosphere at
the base of the chimney, all the air supply to the burner is ob-
tained from the atomizer, and there is no possi-
bility that smoky or dust-bearing room air will
get into the flame. Sample is introduced into
the flame both in the primary air drawn in at the
bottom of the burner and in the secondary air at
the top.
The chimney also reduces heat conduction and
convection from the flame to the body of the
instrument. To reduce heating still further, a
bright aluminum reflector, R, keeps most of the
radiant energy out of the instrument. Two
openings provide paths for the light beams to
reach the photocells. The photocells look through
them and the flame into a black light trap, B.
The trap becomes hot and must be insulated from
the reflector.
For the most stable operation the air supply to
the atomizer was regulated by two diaphragm
regulators connected into the line in series. The
gas supply had a normal pressure of about 9
inches of water and a fuel value of 528 B.t.u.
per cubic foot. It was regulated by passing
through an adjustable constriction to the burner
and to another tube immersed an adjustable dis-
tance below a water surface, thus stabilizing the
pressure at the burner whenever part of the flow
escaped through the bubbler tube.

OPTICAL SYSTEM

The optical system is shown in Figure 2.

Two beams of light are taken from the flame just

above the top of the burner. Each light path has
two condensing lenses, L, of 2-inch diameter and
Figure 2. Optical System 3-inch focal length, which focus images of the
lower part of the flame, F, on the photocells, P.
The filters for isolating different emission lines
are located between the lenses. The lithium
filter, Li, is positioned in the internal standard
beam, while the other filters, Na, are held on a
rotating plate so arranged that any other filter
may be inserted into the other beam. For meas-
urements of lithium concentrations, the lithium
photocell is switched into the part of the circuit
normally occupied by the other photocell.

The combinations of filters selected for the de-

termination of the different elements are given
in Table I. Those marked I are simple filters
for general use. Those marked II are more com-
plicated and expensive filters for the determina-
tion of small amounts of unknowns in the pres-
ence of large amounts of interfering elements.

ELECTRICAL SYSTEM

The schematic wiring diagram in Figure 3

shows a simple potentiometer
_
circuit with a single sensitivity
control and one switch to
Table I. Filter Data shift from internal standard
For each filter are given the components, transmittance to the desired radiation, minimum detectable concentration to lithium and to direct in-
in parts per million, and the interference factors expressed as the relative gravimetric concentrations of the inter-
fering and desired elements needed to produce the same signal. tensity measurement of other
Filter K Na I Li I Ca I Na II Li II Ca II elements.
Components C-2600 C-3480 C-2403 C-5120 C-3480 C-2403 C-2412
C-9780 B-6708 C-2412 C-9788 B-6708 C-5120 The internal standard po-
CB-ON20 B-5893 B-6708 B-6240 tentiometer for balancing the
CB-ON20 CB-ON20 amount of unknown light
Transmittance, % 75 18 55 25 18 35 15
Minimum detectable 0.05 0.05 0.3 1 0.05 0.5 2 against the lithium light is a
Interference factor 10,000-ohm Beckman helipot.
K 3000 40 4 3000 2000 10 With a ten-turn duodial, it
Na 9000 3000 100 3000 200
Li 9000 3000 1 3000 30 gives an internal standard scale
Ca 9000 100 400 600 1000 1000 divisions long. The
C. Glass filter from Corning Glass Works, Corning, N. Y. photocells are of the self-gen-
B. Dielectric interference filter from Baird Associates, Inc., Cambridge, Mass. erating type (Vickers Electric
CB. Glass filter from Chance Brothers, Ltd., Glass Works, Smethwick 40, Birmingham, England. Division, Vickers, Inc., 1815
Locust St., St. Louis. Mo.).
 396
The galvanometer is a General Electric (General Electric Co.,
Schenectady, N. Y.) high-sensitivity portable Type 32C-246G13.
Its characteristics are: sensitivity, 0.0007 microampere per mm.;
resistance, 1900 ohms; external critical damping resistance,
42,000 ohms; period, 4 seconds. It is used with less than its
critical damping resistance to increase the current output from
the photocell and hence to increase the deflection for a given con-
centration of unknown. The speed of response of the complete
flame photometer is limited by the time needed to flush out the
atomizer chamber, which is about 20 seconds. The increase in the
galvanometer’s response time by overdamping is not important,
so long as it is much smaller than this.
Figure 4. Flame Photometer
Figure 4 is a photograph of the flame photometer.
The main housing is an aluminum casting. The atomizer and
atomizer chamber project out of the front right-hand corner. The
burner is diagonally opposite in the back, hidden from view by the
reflector. The optical system is just below the top with the lith-
ium photocell behind the atomizer and the other to the left of it.
The control panel on the front includes the three electrical con-
trols. The remaining operating control is the element selector
wheel, which projects through the top and has different filters
mounted on it.
PERFORMANCE
The flame photometer has been set up and operated in several
laboratories over a period of 8 months. It has shown unusual
stability and freedom from atmospheric contamination. Accu-
rate determinations of sodium and potassium are possible in
smoky or dusty rooms. The atomizer seldom clogs. For low
concentrations the noise level is less than half a galvanometer divi-
sion. However, because this is about the limit of readability, it
is arbitrarily assumed to be the minimum detectable signal. The
corresponding minimum detectable concentrations given in Table
I were calculated from the deflections measured for four solutions
containing 200 p.p.m. of calcium, and 10 p.p.m. of sodium, potas-
sium, and lithium, respectively.
Figure 5 shows direct and internal standard calibration curves
for sodium; Figure 6, an internal standard curve for potassium.
The internal standard curve for sodium was measured independ-
ently in three laboratories with three different sets of standards.
In the figure, the group of points from each laboratory has been
adjusted to correct for differences in the sensitivity that was used
in each laboratory. Each point in this curve is the average of
ANALYTICAL CHEMISTRY
three or five measurements. Each point on the other curves
represents a single measurement.
Interference. The filters should meet two requirements, high
transmittance at the desired wave length and low transmittance
at other wave lengths. In general, these are mutually dependent,
so that a compromise must be made to obtain reasonably high
sensitivity without excessive interference from the transmittance
of unwanted light. The amount of interference between the dif-
ferent elements depends on the spectral response curve of the
photocells and the natural emissivities of the different elements as
well as on the properties of the filters. The composite effect of
these has been measured as the concentration of each desired ele-
ment which gives the same deflection as a high concentration of
each interfering element. For example, a solution containing
1000 p.p.m. of sodium gave a deflection of 0.5 division through the
potassium filter; 10 p.p.m. of potassium through the same filter
gave a deflection of 45, so that Vs p.p.m. of potassium would have
given a deflection of 0.5. The interference factor was 1 in 9000.
The interference factors of all the filters are given in Table I.
Figure 5. Direct and Internal Standard Calibration
Curves for Sodium
The measurement of interference factors for the sodium filters
was limited by the presence of sodium in the potassium, lithium,
and calcium available for test solutions. In all cases the D lines
were clearly visible in the flame with a spectroscope. When the
emission from the concentrated calcium, lithium, or potassium
solution was measured through sodium filter II, the insertion of
Corning filter 2412, which removed the sodium light but trans-
mitted the calcium, lithium, and potassium light, reduced the de-
flection by more than 80%. The principal parts of the deflections
measured for the lithium and potassium solutions through sodium
filter I were also due to the sodium impurity. These interference
factors for the sodium filters would probably have been several
times larger if measured with pure materials. For calcium inter-
ference, the impurity was not significant with sodium filter I.
Calcium filter I is suitable for the determination of relatively
large amounts of calcium, but a correction must be applied if lith-
ium or much potassium or sodium is present. In serum analysis
VOLUME 2 4, NO. 2, FEBRUARY 1952 397

nal standard, these are reduced to 39 and 26%. The improve-

Table II. Approximate Calculation of Errors Due to ment with the I filters by internal standard is fortuitous, as it is
Interference Factors caused by cancellation of two errors arising from different inter-
Sample contained 10 p.p.m. of sodium, 1000 p.p.m. of calcium, and 10,000 fering elements. In the analysis of sampleslikethis, filter combina-
p.p.m. of potassium, with 500 p.p.m. of lithium added as internal standard.
tions I might be expected to give errors up to about 100%, filter
Apparent. Concentration of Sodium and
Lithium Due to Different Components, combinations II up to about 30%. Both of these could be re-
P.P.M.
Na Li Na Li
duced by adding comparable amounts of the interfering elements
Component
filter filter filter filter to the standards or by correcting for known interferences.
I I II II
10 p.p.m. Na +500 Li 10 500 10 500
1000 p.p.m. Ca 10 2.5 1.7 1

10,000 p.p.m. K 1 250 1 5

Total 21 752.5 12.7 506
Concentration by internal standard
21 X =
P'P*111, ^or I combination
7-2%
Concentration by internal standard
12.7 X = 12.6 p.p.m. for filter II combination

these corrections require that the standards be made up with

concentrations of sodium and potassium proportional to those of
normal serum. Calcium filter II has more favorable interference
factors and is useful for measurements with lithium as an internal
standard.
The significance of the interferences is shown by an example of
a low-sodium food sample containing 10 p.p.m. of sodium, 1000

p.p.m. of calcium, and 10,000 p.p.m. of potassium. When 500

p.p.m. of lithium have been added as an internal standard, the er-
rors calculated approximately in Table II should result. An in-
terference factor of 1 in 10,000 instead of 3000 is assumed for po-
tassium through the sodium filters, as this makes a reasonable al-
lowance for the contamination of the potassium sample mentioned
above. Figure 7. Effect of Change in Air Pressure
A. Direct intensity
By direct intensity measurements the calculated errors are 110 B. Internal standard* 144 me. per liter (1000 p.p.m.) of lithium
and 27% for the I and II pairs of filters, respectively. By inter- C. Internal standard* 72 me. per liter (500 p.p.m.) of lithium

In this’calculation nonlinearity at the high potassium concen-

tration would reduce its interference from that above. This cal-
culation considers only optical interference due to incomplete
spectral isolation. There may be other interatomic effects in the
flame that contribute equal or larger errors.
Stability. To test the stability and reproducibility, sodium
was selected as the element to be measured) since many analyses
call for the greatest accuracy in its determination. Its concen-
tration in the samples used for tests was kept in or near the
range below 2.5 me. per liter (59 p.p.m.), where the intensity of
the 1) lines emitted was linearly proportional to the sodium con-
tent of the sample. For direct intensities, 1.09 and 2.18 me. per
liter (25 and 50 p.p.m.) were used, and for the internal standard
ones the same with 72 and 144 me. per liter (500 and 1000 p.p.m.)
of lithium added. In some cases a wetting agent was also added,
though it did not prove to have any effect on the readings.
The effect of changing the air pressure on the direct intensity
reading was measured under different conditions to test its inde-
pendence of the burner adjustments. When all other variables
were held constant, the rate of change of intensity with air pres-
sure was the same for three different gas pressures, for four dif-
ferent air inlet settings, and for three different sizes of gas jet.
The range of the variables covered the range through which the
burner operated well. Changing the air pressure appeared to af-
fect only the amount of sample going into the flame without inter-
related effects between it and the size or kind of flame.
A number of factors besides pressure affect the atomizer’s per-
formance. The principal ones are the size and orientation of the
atomizer jets, the size and shape of the atomizer chamber, the
position of the atomizer in it, and the pressure drop in the lines
leading to and from the atomizer and chamber. Changing them
Figure 6. Internal Standard Calibration Curve for changes the deflection but does not have much effect on its rate of
Potassium change with air pressure.
398
Figure 7 shows in curve A the effect of air pressure change on di-
rect intensity. A given percentage change in air pressure pro-
duces half as great a percentage change in direct intensity reading
at high pressures, with larger changes at low' pressures, as found
by Berry. The internal standard readings using 144 me. per liter
(1000 p.p.m.) of lithium show'n in curve B are only about a fourth
as much affected as the direct ones. With 72 me. per liter (500
p.p.m.) of lithium, curve C shows that the dependence on air pres-
sure is reduced almost to zero, as found by Fox. The reading
passes through a minimum around 10 pounds. The difference
between these and the reduction by 2.5 found by Berry W'ith 144
me. per liter of lithium may well be due to the faster flow of his
atomizer, which made the concentration of both the lithium and
sodium atoms in his flame higher. At the concentrations used,
there is practical!}' no reabsorption of sodium light in the flame,
but there is enough reabsorption of lithium light to make a pro-
portional increase in the concentration of both elements appear as
a relative increase in the amount of sodium.
Figure 8. Effect of Changing Gas Pressure
0.100-inch jet and different air inlet openings
gas
The effect of changing gas pressure W'as measured at constant
air pressure for different air inlet settings and for different gas jet
sizes. Figures 8, 9, and 10 show' how the direct intensity and in-
ternal standard readings varied with gas pressure. In each figure
air inlet areas are expressed in square inches. The curves for the
0.052-inch jet are not given, as they were too erratic to be useful.
The data show that the minimum intensity wras about the same for
each jet at the smallest gas pressure and air inlet setting atw'hich
the burner wrnuld operate. The intensity increased w'ith gas pres-
sure and w'ith the amount of primary air. The rate of increase
was greatest for the smallest jet and smallest for the largest one.
The percentage change in the readings for a given percentage
change in gas pressure is proportional to the slope of the curves,
w'hich varies from 0.3 to 0.9 for different jet sizes and air inlet
settings. The least slopes are about the same for each jet and oc-
ANALYTICAL CHEMISTRY
cur with the minimum amount of primary air. They always in-
crease as the air inlets are opened, but do so more rapidly for small
jets than for large ones.
The internal standard curves are considerably less steep than
those of the direct intensities. The improvement in stabiliza-
tion varies from a factor of 10 in the most favorable conditions to
5 in the less favorable but usable ones.
GAS PRESSURE IN INCHES
Figure 9. Effect of Changing Gas Pressure
0.082-inch gas jet and different air inlet openings
Reproducibility. The reproducibility of the flame as a source
of radiation was measured by making a series of approximately
30 readings in 7.5 minutes and calculating for each series the
average departure from the mean. These average differences are
called the average noise level when expressed as percentages of
the mean readings.
The noise level was found to be independent of air pressure over
a wide range, so long as the air flow was below a critical rate.
Above this rate, drops wrere picked up from the walls of the
atomizer chamber and blown into the atomizing jet and into the
base of the burner. From 6 to 12 pounds’ air pressure, the noise
level averaged 1.2% by direct intensities; at 14 pounds, it was
4.3%. Using 144 me. per liter (1000 p.p.m.) of lithium as an in-
ternal standard, the noise level was 0.5%. It decreased as the air
pressure was reduced. When the lithium concentration in the
sample W'as reduced to 72 me. per liter (500 p.p.m.) values of 0.3
to 0.4% were obtained.
Other series of measurements showed that the noise level was
the same W'ith sodium concentrations of 25 and 50 p.p.m., both
by the direct and by the internal standard methods; the blue
light emitted by the flame in the absence of sample was about
tw'ice as steady as the sodium series under the same conditions;
and the stabilities of direct measurements of lithium and potas-
sium were essentially the same as those of sodium.
The fact that both the observed noise level and the rate of
change of internal standard reading with air pressure went down
when the lithium concentration W'as reduced suggests that the re-
sidual noise level W'as associated with the air supply and atomizer.
It may have been affected by variations in atomizer performance,
caused either by small changes in air pressure or by turbulence
and other conditions around the atomizer.
VOLUME 2 4, NO. 2, FEBRUARY 1952
The noise level was also measured as a function of gas pressure
and burner adjustments, using both the direct and internal stand-
ard methods. When the conditions were well stabilized, the
noise was about the same for all direct intensity readings, with
perhaps slightly better performance at the smallest usable air in-
let openings. The fluctuations in the internal standard readings
also were almost independent of conditions but slightly less than
half as large as those for direct intensity. The range of measure-
ments included gas jet diameters of 0.070 and 0.100 inch, gas pres-
sures from 1 to 6 inches, and air inlet openings from 0.29 to 0.94
square inch.
Several series of internal standard measurements were made in
which the sensitivity of the instrument was adjusted by standard-
izing on a reference solution before each reading. All were made
with 9 pounds’ air pressure, 4 inches’ gas pressure, gas jet diam-
eter 0.070 inch, and air inlet opening 0.15 square inch. Some se-
ries used 144 me. per liter (lOOOp.p.m.) of lithium and sodium con-
centrations of 2.18 and 3.27 me. per liter (50 and 75 p.p.m.);
others, 72 me. per liter (500 p.p.m.) of lithium and sodium con-
centrations of 1.09 and 1.74 me. per liter (25 and 40 p.p.m.).
Neither showed the slow variations of the other series, their read-
ings appearing to have only random fluctuations. The average
difference from the mean was only ±0.3% for each. As this
short-time reproducibility is representative of the operating pro-
cedure actually used in analyzing an unknown sample, this is the
amount of fluctuation that might be achieved under well-stabil-
ized conditions.
Figure 10. Effect of Changing Gas Pressure
0.070-inch gas jet and different air inlet openings
If the gas and air pressures vary, their effects are additional to
this. The percentage change in either of them that would con-
tribute an equal amount of variation with favorable instrument
settings is ±10% for gas pressure, ±2% for air pressure with 144 me.
per liter of lithium, and considerably more for air pressure with 72
me. per liter of lithium. These are variations that might be ex-
399
pected to occur under normal conditions where the gas supply is
not regulated and a single regulator is used on the air supply.
When the variations are larger than these, they contribute the
principal part of the noise. The mean noise level was measured
under such conditions and found to be ±0.5%. This may be ex-
pected to vary from time to time depending on the loads on the
supply lines.
DISCUSSION
The results above indicate the most favorable operating condi-
tions for the flame photometer burning this gas. The best air
pressure is the highest that does not cause an increase in the noise
level. The best gas jet and air inlet openings can be picked out of
the figures as those that give the highest intensity and least
slope at the available gas pressure. However, if the heat content
of the gas is different, compensating adjustments must be made to
keep the same actual conditions in the flame.
It has been the author’s experience that the appearance of the
flame is a reliable guide to its proper adjustment. In general, in-
creasing the size of the gas jet with constant gas pressure increases
the size of the flame and the intensity of the light emitted. If the
gas pressure is low, the jet should be large; if it is very high, it
may be advantageous to reduce it by putting a fixed constriction
in the line so that a larger jet may be used. The air inlets control
the amount of primary air in the flame. At very small openings,
the flame lifts off the top of the burner. At larger ones it burns
directly over the grid in little green cones. Next, the cones turn
blue. Finally, at very large openings the cones lose their tops
and give the flame a fuzzy appearance. With the largest jet, the
flame did not get enough air to turn blue even with the air inlets
wide open. If the gas has a higher heat content, more air is
needed to burn it, and a smaller gas jet must be used to get equiv-
alent flame conditions. •
The color and appearance of the flame are indicated in Figures
8, 9, and 10. The solid lines indicate that the flame had green
cones, the dashed ones that it had blue cones, and the dotted ones
that it appeared fuzzy.
To get high sensitivity, high intensity is needed. This is best
combined with relatively noncritical conditions at large jets and
moderate gas pressure giving the largest flames that do not cause
overheating. The conditions of a small jet and high gas pres-
sure, where the curves might appear to indicate invariance, are
not favorable, as the readings are very dependent on air inlet
opening and tend to vary erratically.
ACKNOWLEDGMENT
The author wishes to thank John W. Berry of the Amer-
ican Cyanamid Co., Howard Eder of the Cornell Medical
School, Charles L. Fox, Jr., of the College of Physicians and
Surgeons, Columbia University, and B. C. Wiggin of Baird
Associates, Inc., for their help and advice in planning and testing
this instrument.
LITERATURE CITED
(1) Barnes, R. B., Richardson, D., Berry, J. W., and Hood, R. L.,
Ind. Eng. Chem., Anal. Ed., 17, 605 (1945).
(2) Berry, J. W., Chappell, D. G., and Barnes, R. B., Ibid., 18, 19
(1946).
(3) Bills, C. E., McDonald, F. G., Niedermier, W., and Schwartz,
M. C., Anal. Chem., 21,1076 (1949).
(4) Bowman, R. L., and Berliner, R. W., Federation Proc., 8, 14
(1949)
.
(5) Fox, C. L., Jr., Anal. Chem., 23, 137 (1951).
(6) Gilbert, P. T., Hawes, R. C., and Beckman, A. O., Ibid., 22, 772
(1950).
(7) Parks, T. D,, Johnson, H. O., and Lykken, L., Ibid., 20, 822
(1948).
(8) Schuhknecht, W., Angew. Chem.., 50, 299 (1937).
(9) Weichselbaum, T. E., and Varney, P. L., Proc. Soc. Exptl. Biol.
Med., 71,470 (1949).
Received May 28, 1951.