8'3O CAX"\'ADIAK JOURK;\L O F CI-IEMISTKY. VOL.

37, 1059

the racemic acid (1). The hydrochloride of the methyl betaine which was recrystallizecl
by adding hot ethyl acetate to a boiling solution of the coinpouncl in absolute ethanol
had m.p. 217-218' (gas evolution) and [a]: - 13.0" (27, in ethanol). The infrared
spectrum and the X-ray powder diagram of the synthetic (-)-homostachydrine hydro-
chloride were identical in all respects with those of the hydrochloride of the natural
material. Similarly, the synthetic and natural sainples were chromatographically pure,
and indistinguishable from each other, having RF 0.58 in n-butanol -concentrated
hydrochloric acicl - water (100 :20 :39) and R p 0.33 in 95% ethanol -concentrated aqueous
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ammonia (95 :5).

We thanlr. Dr. Maria Przybylslta and Mr. R. Lauzon of these laboratories for the
X-ray powder diagrams and for the infrared absorption spectra, respectively.

1. WIEHLER,G. and MARIOS, L. Can. J. Chcnl. 36, 338 (1958).

2. KING,F. E., KING,1'. J., and WARWICK, A. I. J. Chem. Soc. 3500 (1950).
3. SCHWEET,R. S., HOLDES,J. T., and LO'IVY, P. H. J. Biol. Chem. 211, 517 (1954).
4. LEITIE,W. Ber. 65, 927 (1932).
5. HARRIS,G. and POLLOCK, J. R. A. Chem. & Ind. 462 (1953).
Can. J. Chem. 1959.37:830-831.

SEPARATION O F NICKEL AND COBALT B Y PAPER CHROMATOGRAPHY*

T h e R, values of Xi and Co have been cletermined for 1,-tributyl phosphate (TBP)

adjusted with concentrated hydrochloric acid of various concentrations. T B P is as
suitable for the separation of Ni and Co by paper chromatography as other solvents
mentionecl in the literature (1, 2, 3). Before use the reagent was shaken with nitric acicl
to remove mono- and di-butyl phosphate (4), then distilled and adjusted with HCI of
different molarities. Afterwards the organic phase was separated and mixed with methanol
in the ratio 2:l and I:1.
PROCEDCRE
The chromatograms were developed by ascending chromatography. The paper ~lsecl
was Schleicher and Schiill No. 40233 (LVhatman No. I). Solutioiis of Ni- and Co-chloricles
each in quantities of 207 were put on the paper. The process ran 4 hours a t a temperature
of 22" C. The flow of Co was easily identified by its blue color. On the following pictures
Co was marked with a-nitroso-P-naphthol. Ni n7as identified with an alcoholic solution
of dimethyl glyoxime.
RESULTS
The RF values of Co recorded i l l Table I show a close dependence on increasing con-
centration of HCI ~isedto eq~iilibratethe T B P . Ascencling concentration of HCI reduces
the distance of Co from the liquid front, i.e. the K p va1~1esincrease. When working with
*Prioate conlribzrtion.
 Can. J. Chem. 1959.37:830-831.
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 Can. J. Chem. 1959.37:830-831.
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 NOTES 83 1

highly concentrated HC1, Co will allnost reach the liquid front. I n this case Co does
not flow as a spot any more, but has a long diffuse tail (see Fig. I ) . Similar results are
obtained when chromatographing CO using T B P as a solvent without admixture of
methanol (see Fig. 2).

TABLE I
RF of CO ~ ~ s i an gTBP/methanol mixture in the ratio 2:l
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T B P adjusted with
N HCI 5.5 6 . 5 7 . 5 8 . 5 9 . 0 9 . 5 10 10.5 11 11.5 12 12.5
RF of CO 0.16 0 . 2 3 0 . 2 8 0.34 0 . 3 8 0.43 0.46 0.48 0.52 0.59 0.66 0.74

As Table I1 shows, the RF values resulting thereof are considerably higher than those
obtained sing TBP/methanol mixtures.

'I'ABLE I1
RF values of Co

Ratio TBP/nrethanol
T B P adjusted
with N HCI 1 :1 2:l T B P pure
Can. J. Chem. 1959.37:830-831.

Previous tests have shown that Ni is not extracted by T B P from an aqueous solution.
This effect is apparent in the chromatogram. Figure 2 shows that, when using pure
HC1 equilibrated T B P , Ni is immobile; and in TBP/methanol mixtures the flow rate
is roughly proportioilal to the quantity of methanol present.

Sharp chromatographing separations of Ni and Co can be obtained using HCI -

equilibrated T B P . I t is recommended that the T B P be treated with 9 to 10 molar
HCl, and mixed with methanol in the proportion 2:l.

1. F. H., DAVIES,G. R., LINSTEAD,R. P., and WELLS, R. A. J. Chem. Soc. 516 (1950).
BURSTALL,
2. BURSTALL,F. H. et al. J. Chem. Soc. 1497 (1952).
3. LEDERER,E. Chromatography. Elsevier Publishing Company, Xew York. 1954.
4. BURGER,L. L. and MCCLANAHAN, E. D. I/EC 50, 153 (1958).

QUENCHING AND VIBRATIONAL-ENERGY TRANSFER

OF EXCITED IODINE MOLECULES

From their investigation of the effect of foreign gases on the emissiorl spectrum of I2
"11 (v' = 2 6 ) , Arilot and McDowell ( I ) obtain collisioilal transfer coefficients which are