result from application of plate voltage before the cathode has reached operating temperature. Center-zero type 50-0-50 ha. meters have been substituted for the 0-50 meters with their reversing switches. The above modifications can be made on existing instruments with a minimum amount of work and result in greatly improved performance and convenience of operation. The 5751 tubes last twice as long as the 6SC7’s and do not require selection. There is still some zero-point instability in the instrument, apparently due to line voltage fluctuations. This is almost completely eliminated by plugging the meter into a Sorenson Model 150-S vacuum-tube line voltage regulator or a Sola Model 30805 constant voltage
transformer. Soine sort of line voltage regulation thus seems t o be required. Replacement of the power transformer by a Sola-Type 7104 voltage regulating power transformer (which costs only about twice as much as the regular power transformer) eliminates nearly all of the zero drift. ’ A completely redesigned instrument n-as built (3). LITERATURE CITED
(1) Elmore, TV. C., tronics,” pp. 180-3, York, 1949. (2) Harwell, K. E., 616-19 (1954). (3) Proctdr, C. hl.,
Sands, M., “ElecMcGraw-Hill, New Ax.4~. CHEM. 26,
dissertation, Texaa A&M College, January 1958. (4) Rider, J. F., “Vacuum-Tube Volt-
meters,” 2nd ed., pp. 148-51, 216, John F. Rider Publishers, Kew York,
1951. (5) Tomer, R. B., Electronics 29, No. 9, 218-30 (1956). (6) Valley, G. E., Wallman, H., “Vacuum Tube Amplifiers,” pp. 419-21, McGrawHill, New York, 1948.
CHARLES 31.PROCTOR 4676 Columbia Parkway Cincinnati 26, Ohio
CONTRIBUTION 142, Department of Oceanogra hy and Meteorology, Agricultural and Gechanical College of Texas, College Station, Tex., based in part on investigations conducted for the Texas A&M Research Foundation through the sponsorship of the Office of Kava1 Research (Project NR083 036, N70nr-487, T.O. 2’1. This communication constitutes Technical Report 56-37T (10-9-56).
Separation of Uranium and Bismuth with Ion Exchange Papers SIR: Methods for the separation of uranium from large amounts of bismuth have been investigated because of interest in Brookhaven National Laborntory’s Liquid Metal Fueled Reactor (1, 4). One method for this separation utilizes ion exchange-impregnated papers to separate uranium from 250 times as much bismuth. Tuckerman ( 5 ) has reported the use of the cationic form of these papers for the separation of basic amino acids. Little work has been done on inorganic applications. EXPERIMENTAL
A solution of bismuth and uranium mas prepared that contained 10 grams of bismuth and 40 mg. of uranium (as EOn++)in 25 ml. of a 12N nitric acid solution. Another solution contained 250 mg. of bismuth and 250 mg. of uranium. The papers n-ere washed with distilled water by allowing the water to ascend through the papers, simulating a chromatoqraphic separation. They were used as received from Rohm and Haas, IR.4-400 (Cl-) and IR-45 (OH-). After drying, a 10-pl. sample of the test solution was applied and the paper was allowed to dry. It was developed bv nicending chromatography with distilled water as the s o l ~ e n t for 45 minutes. The paper was treated with a 3% potassium ferrocyanide solution to 10cate the uranium and a saturated basic sodium sulfide solution to locate the bismuth. The uranium appears as a broil-n 5eck and the bismuth as a black streak. The IRA-400 paper contained some impurity, probably iron, which appeared with the ferrocyanide reagent. Figures 1 and 2 show the separ a t‘ions.
The weakly basic (IR-45) paper will separate small quantities of the elements, but it is not so effective as IR4400 for large amounts of bismuth. In comparison with this rapid chromatographic method, conventional separations are incomplete after 10 hours of development. Separations were tried on Whatman 3MM paper using butanol saturated with 1N hydrochloric and
nitric acids. After 11.5 hours the h y drochloric acid solvent had not caused any separation, the bismuth running from 15 to 120 mm. and the uranium a t 45 mm. After 9.5 hours in the nitric acid solvent separation was only partial, the uranium being located from 53 to 60 mm. and the bismuth from 12 to 58 mm. from the point of application.
1-
SOLVENT FRONT
-
SOLVENT FRONT
1-
IMPURITY
URANIUM FRONT I
-
BISMUTH FRONT
r”\
I-
UOz FRONT (10
Y)
POINT OF APPLICATION
Figure 1 . Separation of 4 0 y of uranium from 10 mg. of bismuth on Am berlit e IRA-4 00-im p regnoted pap e r
Figure 2. Separation of 10 y of uranium from 10 y of bismuth on Amberlite IR-45-impregnated p a p e r VOL. 31, NO. 7, JULY 1959
1279
The liniitina factors involved in this separation a n i chemical detection of the separated elements are the capacity of the paper and the sensitivity of the reagents. According t o Feigl (2), as little as 0.92 y of uranium can be detected at a dilution of 1 t o 60,000 on paper by 3% potassium ferrocyanide. From 10 to 40 times as much uranium was employed here. This separation should lend itself to remote operation with the development of special paper-handling devices. Because of its speed and resolution. compared with the conventional paper,
it should have value in other inormnic separations. ACKNOWLEDGMENT
The author thanks the Rohm & Haas Co. and Robert Percival of the Resinous Products Division for sample6 of the ion exchange paper and helpful suggestions. At present the wet strength of the paper is poor and handling difficult; however, Rohm & Haas is putting a stronger paper into production (3).
Analysis of Butoxy Ethoxy Propyl Esters of 2,CDichlorophenoxyacetic Acid and 2,4,5-Trichlorophenoxyacetic Acid Mixtures F. J. WITMER, D. N. THOMAS, and J. B. VERNETTI Chipman Chemical Co., Inc., Portland, Ore.
CS-83 Slit
Component No./
1
I
Name
' 2 Achloro-W
Formula
1
X or
Accuracy
RTe%
1
I
6.1. Pis.
Y
~
C17H2405C120-100
~
1
-
,
chloro- I phenoxy-1 acetic acid butoxy ethoxy propyl ester
I
I
,
Range "(
1
2,4-DiC12H140&12 chlorophenoxyacetic acid butyl ester
13.67 0.400 100 0.038A 0.10
-1
'
0-100
Accurocy
70
! zk1.0
1 1
1
X or v 6.1. Pis.
(mm) AX or Av
Concn. mg/ml Lengfh mm
9.06 0.20 30 0.025j 0.545
zkl.0 112.54 0.50
30 0.047, 0.545
Instrument: Perkin-Elmer Model 1 1 2, NaCl prism Sample Phase: Solution in carbon disulfide
Instrument: Perkin-Elmer Model 1 12, NaCl prism Sample Phase: Solution in carbon disulfide Cell Windows: NaCl Absorbance Measuremenf: Calculotion:
Component Nome Formula
2,4-DiC I ~ H ~ ~ O IO-100 &I~ I chlorophenoxyacetic acid isopropyl ester
~
fl.O
CS-84 Slit
,
C I ~ H Z ~ O S C 0-100 I~
HAROLD T.PETERSON. JR. 999 DeWitt St. Valley Stream. N. Y.
jConcn.
( m m ) Img/ml A x or ,Length Av mm
phenoxy-/ I acetic acid butoxy ethoxy I propyl ester
2 12,4,5-Tri-
(1958).
F. J. WITMER, D. N. THOMAS, and J. B. VERNETTI Chipman Chemical Co., Inc., Portland, Ore.
12.55 0.400 100 0.039~0.10
kl.0
Banerjee, G Heyn, A. €1. A., A N A L . CHEX 30, 1795 (1958). ( 2 ) Feigl, F., "Spot Tests in Inorganic Analysis," 5th English ed., p. 265, Elsevier, Amsterdam, 1958. (3) Percival. R. W.. Rohm & Raas, . Philadelphia, Pa.,' private cornmu: nication. (4) Stoner, G. A., Finston, H. L., ANAL. CHEU. 29, 570 (1957). (5) Tuckerman, M. M., Ibid., 30, 231 (lj
Analysis of 2,4-Dichlorophenoxyacetic Acid Isopropyl Ester and 2,4-Dichlorophenoxyacetic Acid Butyl Ester Mixtures
~
I
LITERATURE CITED
Point
Cell Windows: NaCl Absorbance Measurement:
-X
Calculafion:
Inverse matri-
Point_-
Inverse matrix-)(
Relative Absorbances"-Analytical Matrix:
Relofive Absorbances'-Analytical Matrix: Component/X
1
2 Moterial Purity:
12.55 0.450 0.041
13.67 0.147 0.360
Reference compounds 99 +% pure
ComponentjX
8.06
1
1.814 0.709
2 Material Purity:
12.54 0.682 0.677
Reference compounds 99 +% pure
a Relative absorbances are given as the slope of the Beer's law concentration curves used expressed in terms o f absorbance per 100% of constituent.
Relative absorbances are given as the slope o f the Beer's law concentration curves used expressed in terms of absorbance per 100% o f constituent.
These data represent standard publication and submission is open to anyone in accordance with regulations of ANALYTICAL CHENISTRY. The Cohlents Society is acting only as an aid to t h e journal.
T o standardize procedure ANALYTICAL CHEMIsrRY requests that materid be s e n t in quintuplicate to (he chairman of the review committee: Robert C. Wilkerson, Celanese Corp. of America, Post O5ce Box 8, Clarkwood, Tex.
1280
ANALYTICAL CHEMISTRY
(I
