Estimation of Boron bv a Modified Flame Test J

H. C. WEBER AND R. D. JACOBSON, 3lassachusetts Institute of Technology, Cambridge, Mass.

T HE flame test, in which concentrated sulfuric acid and

methyl alcohol produce a volatile boron compound, is
commonly used for the detection of boron in some labora-
equivalent of 0.02 to 0.10 mg. of boron in a test tube, evapo-
rating almost to dryness, adding a mixture of 6 cc. of methyl
alcohol and 1 cc. of sulfuric acid, and placing the test tube in
tories. The effects of the ratio of acid to alcohol, the tempera- the apparatus, a green color was imparted to the flame. The
ture of the solution, and the amount of water present are duration of the color was proportional to the amount of borate
presented by Stahl ( I ) , who has devised a quantitative present. The results showi in Table I n-ere obtained by
measurement of boron based on the intensity of the green these tests, the times to the end points being recorded on a
coloring in the flame u.ing a comparative standard. He stop watch, the dial of which had been covered.
claims i n accuracy of 15 per cent.
Using the apparat'us herein described, although the inten- T ~ B LI.E ESTIMATION
OF B O R O ~
sity of color in the flame diminishes a t a marked rate when .$Yerage Duration
Boron Present Observed Duration of of Flame
the amount of boron in the sample reaches 0.03 mg., the total -KQ Sec. Scc.
time of duration of color is almost a straight-line function 0.02 80, 82, 80, i 3 79
0.04 170, 140, 135 148
of the boron content up to about 0.1 mg. By successive 0.06 265, 2 5 5 260
dilution, a more concentrated sample of boron may be quickly 0.08 355, 275, 310, 330
390, 315, 340, 365, 360, 370, 410, 420, 366,
318
0.10 362
analyzed, using this method. 353, 360, 350, 325, 375, 330

SCREW CLAMP
AIR FLOW REGULATOR

PRESSURE FLOW SAMPLE IN

REGULATOR METER TEST TUBE

The figure shows the apparatus used. Air passes at a rate of
150 cc. per minute through a calcium chloride drying tube and
a into the bottom of a test tube, it bubbles
through the 7 cc. of liquid containing the boron sample. Lkmix-
ture of air, alcohol vapor, and methyl borate passes out the top
of the test tube, through the nozzle, and through the thin part
of a fan-shaped Bunsen flame, igniting and forming a small auxil-
iary flame at right angles to the other. It is this small flame that
is colored distinctly green as long as an appreciable amount
of methyl borate is present. The alcohol flame itself is blue-
green, but the green imparted to the flame by the boron is
enough different so that one has but little difficulty recognizing
an end point. Observation of the flame at intervals of a few
seconds is recommended rather than continuou3 observation.
That point when the constant blue-green of the alcohol flame is
noted at two successive observations is taken as the end point.
After a few trials this point. is readily determined.
T o check the accuracy of the method and its ease of ap-
plication, an apparat'us was assembled and operated by an
inexperienced observer. Two standard solutions x-ere macle
u p - o n e Rith 0.570 gram of boric acid, 2 g r a m of potassium
hydroxide, and distilled water to make 1 liter, and the other
by diluting 50 cc. of the first to 250 cc. One cubic centi-
meter of the first had an equivalent of 0.10 mg. of boron, and
1 cc. of the second, 0.02 mg. By placing a sample having the
273
The spread bet,ween the various tests is due in part to
difficulty in holding the Bunsen flime in a single position.
K i t h a little practice an accuracy better than one significant
figure may be obtained even for traces of boron, especially
if the tests be carried out in a some\That darkened room.
Difficultly soluble materials such as glasses are analyzed
by fusing the sample in a nickel crucible with potassium
carbonate, dissolring the fusion in distilled water, taking a
suitable aliquot, and elTaporat,ing almost to dryness. The
residue is acidified \Titil sulfuric acid and then analyzed as
out'lined above. Even ori glasses containing less than 1
per cent of boric oxide, checks of 10 per cent or better may be
expect,ed,
lcknowledgnient
The authors wish to thank W. T. Hall for his helpful
suggestions.
Literature Cited
(1) Stahl, W., 2. anal. Chem., 83, 268-88 (1930); 101, 342-7, 348-56
(1935).
RECEIYED
October 2 0 , 1937