Use of a zinc spiral in the titrimetric determination of uranium

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Material Information

Title:
Use of a zinc spiral in the titrimetric determination of uranium
Series Title:
United States. Atomic Energy Commission. MDDC ;
Physical Description:
2 p. : ; 27 cm.
Language:
English
Creator:
McClure, John H
Banks, Charles V
Iowa State College
U.S. Atomic Energy Commission
Publisher:
Technical Information Division, Oak Ridge Directed Operations
Place of Publication:
Oak Ridge, Tenn
Publication Date:

Subjects

Subjects / Keywords:
Uranium -- Purification   ( lcsh )
Uranium oxides   ( lcsh )
Uranium compounds   ( lcsh )
Zinc   ( lcsh )
Genre:
federal government publication   ( marcgt )
bibliography   ( marcgt )
technical report   ( marcgt )
non-fiction   ( marcgt )

Notes

Bibliography:
Bibliography: p. 2.
Restriction:
"Date Declassified: June 17, 1947"
Statement of Responsibility:
by John H. McClure and Charles V. Banks.
General Note:
Manhattan District Declassified Code
General Note:
"Date of Manuscript: Unknown"

Record Information

Source Institution:
University of Florida
Rights Management:
All applicable rights reserved by the source institution and holding location.
Resource Identifier:
aleph - 005024228
oclc - 277772876
System ID:
AA00009299:00001


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MDDC 1044


UNITED STATES ATOMIC ENERGY COMMISSION









USE OF A ZINC SPIRAL IN THE TITRIMETRIC DETERMINATION OF URANIUM



by
John H. McClure
Charles V. Banks


Iowa State College










This document consists of 2 pages.
Date of Manuscript: Unknown
Date Declassified: June 17, 1947


This document is issued for official use.
Its issuance does not constitute authority
to declassify copies or versions of the
same or similar content and title
and by the same authorss.


Technical Information Division, Oak Ridge Directed Operations,


Oak Ridge, Tennessee


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USE OF A ZINC SPIRAL IN THE TITRIMETRIC DETERMINATION OF URANIUM


By John H. McClure and Charles V. Banks


A number of methods are reported in the literature for determining uranium titrimetrically by
reducing hexavalent uranium to the tetravalent state and titrating the latter by menas of standard
oxidizing agents.
Of these methods of reduction, probably the most common is the use of a Jones reductor using
amalgamated granular zinc as the packing material.: Silver,' lead,e or cadmium"' packing for the
reductor is also used. Other methods use aluminum',2,4 or copper7 spirals. All these methods are
reported as giving satisfactory results, but certain difficulties are encountered in each of them.
With the amalgamated zinc, the uranium has a tendency to be reduced to the trivalent state and
must then be oxidized to the tetravalent state by bubbling air through the solution for a few minutes.
Aluminum tends to give over reduction also, and after all the metal has dissolved, the solution
being hot, there is an appreciable amount of the tetravalent material oxidized unless air is excluded
during cooling. The use of a copper spiral requires the exclusion of air and long periods of boiling.
In the use of any reductor, a transfer of solutions is involved with the concomitant chances for error.

REAGENTS
Uranium Metal, U: Uranium metal of known purity was used.
Uranium Oxide, UsO,: Uranium oxide prepared by igniting ether-extracted uranyl nitrate was
used.
Zinc, Zn: High purity (99.99 per cent) zinc wire*, having a diameter of 0.125 inch, was used to
prepare the spirals. A piece of zinc wire about 700 mm long was wound on a cork borer 20 mm in
diameter. A length of the wire was left uncoiled, the end of which was bent into the form of a hook
to aid in the removal of the spiral from the flask.
All other reagents were of reagent-grade quality.

EXPERIMENTAL WORK

A tetrasulfatoceric acid solution was standardized against pure uranium oxide, U30,, by the
conventional method using the amalgamated zinc Jones reductors and also by using a zinc spiral.
The normality of the tetrasulfatoceric acid was found to be 0.1121 by the former method and 0.1123
by the latter method. These values represent the average of a series of determinations in each case.
The precision and accuracy of the proposed method was checked in the following manner.
Samples of uranium turnings were cleaned by placing them in dilute nitric acid until they were free


Zinc wire having these specifications can be obtained from the following sources:
Matthiessen and Hegller Zinc Co., La Salle, Illinois
Metallizing Company of America, Inc., 562 W. Washington Blvd., Chicago, Illinois.
The Platt Brothers and Company, Waterbury 90, Connecticut.


MDDC 1044









MDDC 1044


of any oxide coating. These turnings were then carefully washed and dried. Samples of the turnings
were analyzed according to the recommended procedure given below. The results of these experi-
ments are shown in Table 1.

Table 1. Titrimetric determination of uranium after
reduction with a zinc spiral.

U U Error
Taken Found U
(g) (g) Img)

0.5446 0.5448 -0.2
0.5625 0.5627 .0.2
0.5343 0.5338 -0.5
0.5716 0.5718 +0.2
0.5667 0.5669 +0.2
0.5160 0.5159 -0.1
0.5200 0.5200 0.0
0.5033 0.5027 -0.6
0.5293 0.5292 -0.1


It was found that if sulfuric acid was present, the rate of reduction was retarded and that the
boiling time must be increased from the usual 5 minutes to as much as 25 minutes to effect com--
plete reduction.

RECOMMENDED PROCEDURE
-i
Weigh into a 500 ml Erlenmeyer flask a sample containing about 0.5 to 0.6 g of uranium, and
treat with 30 ml of concentrated hydrochloric acid and 10 ml of 60 per cent perchloric acid. Heat
the mixture on a hot plate until all the uranium is in solution and fumes of perchloric acid are given
off. At this point the solution should be light yellow in color. Cool the solution and dilute with a
mixture of 250 ml of water and 10 ml of concentrated hydrochloric acid. Place a zinc spiral in the
flask and boil the solution vigorously for 5 minutes. Cool the flask under running water to room
temperature and remove the spiral. Wash the spiral with a stream of water from a wash bottle
while removing it from the flask. By leaving the spiral in the solution until it is cool, oxidation of
the tetravalent uranium by the atmosphere is prevented. After the spiral is removed, pass a -
current of air through the cool solution for 5 to 10 minutes. Add two drops of 0.025M 1, 10-phenan-
throline ferrous sulfate indicator and titrate the solution with 0.1 A' tetrasulfatoceric acid.


REFERENCES

(1) Birnbaum, M. and S. M. Edwards, Ind. Eng. Chem., Anal. Ed. 12: 155 (1940).
(2) Campbell, E. D. and C. E. Griffin, J. Ind. Eng. Chem. 1: 661-664 (1909).
(3) Furman, N. E. and I. C. Schoonover, J. Am. Chem. Soc. 53: 2561-2571 (1933).
(4) Griffin, C. E., Mining Eng. World, 37: 247-248 (1912).
(5) Karn, E. F., J. Am. Chem. Soc. 23: 685-726 (1901).
(6) Kohlic, 0., Chem. Listy 19: 1-3 (1925).
(7) Scagliarini, G. and P. Pratesi, Ann. chim. applicata. 19: 85-90 (1929).
(8) Treadwell, W. D., Helv. Chim. Acta, 5: 732-743 (1922).
(9) Treadwell, W. D., M. Luethy, and A. H. Rheiner, Helv. Chim. Acta, 4: 551-565 (1921)






























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