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Unclassified Unclassified UNCLASSIFIED ANL-4265 Photostat Price $ ff 3o Microfilm Price $ Jf­ b> O MINUTES OF CONFERENCE ON THE CHEMISTRY Available from the Office of Technical Services OF RUTHENIUM, DECEMBER 13 AND 14, 1948 Department of Commerce Washington 25, D. C. By H. Baxman, E. Turk, and L. Deutsch < ) f CLASSIFICATION CANCELLED I DATE FEB 14 1957 QJg E S e For The Atomic Energy Commission ~ o Z sE s*­ « E . E _* o v> *­ O 01 J a> jr c a) C o <­> •- g — x a Chief, Declassification Branch * o III "> o ; £ °- 8> " ""S S- c 12 'I o .2 .2 E o = "= "P Dec. 16, 1955 Ex a o ~ Q­ .E S E p _2 "° .E J ­g | ^ X <­> *• .E E O O J) J2 x £ c *o .2 ■£ ~ c Argonne National Lab. 0> V 4. O £ o o Q. X s 1! Lemont, 111. o 2 X O j s a f> o o * E ■I e Z "" .0 |£ Q. o 2 o> i o < « "8 u o 9­ 2 ™ .2 •> .2 c ■£ o c O .2 e a Ul c jo "o c E ° c Q. » S .9 > 3 -I 2 i £ S S ° ­o .a o "5 s i ; o> 8. j x"S s. i c 3 8­» UNITED STATES ATOMIC ENERGY COMMISSION £ U E 5 1 £ 8 .2 I w Technical Information Service, Oak Ridge, Tennessee V. c» tj p £• E 6 * I o £ ~ e «• £ i2 ­£• « Ti o 1 8 8. 8 .E £ P i. ■* P §1 TJ O S w ­C o i 8 3 'x 3 P 5 J o T; * * * E i\ 'c 3 S £ If. D £ ­2 a. a. UNCLASSIFIED \ • ^ }■ *$#-/ \ " DISCLAIMER This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency Thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof. DISCLAIMER Portions of this document may be illegible in electronic image products. Images are produced from the best available original document. »­ tCMEllENllAC 4 ANL­4265 Chemistry­General, Chemistry Separations Processes. for_Pu. ARGONNE NATIONAL LABORATORY r P. Oo Box 520? Chicago 80, Illinois MINUTES OF CONFERENCE ON THE CHEMISTRY OF RUTHENIUM December 13 and 14, 19^8 Report Compiled "by H» Baxman, E0 Turk, and Le Deutsch PRESENT H0 R0 Baxman ­ Chem„ Eng. Div. ­ Argonne M„ Beederman ­ Chem. Eng. Div. ­ Argonne S8 T0 Benton ­ Lab. Div. ­ K­25, Oak Ridge Co F. Callis ­ Tech. Div., GD E. ­ Hanford Jo B. Cameron ­ Chem. Div. ­ Argonne 'L0 Deutsch ­ Chem, Eng. Div. ­ Argonne Ho L„ Farrar ­ Lab. Div. ­ K­25, Oak Ridge H„ M. Feder ­ Chera. Eng. Dive ­ Argonne S0 Gaarder ­ AEC ­ Chicago Wo Hardwick ­ NRC Chenu Div. ­ Chalk River K. M. Harmon ­ Tech. Div., G„ E0 ­ Hanford 0. Fo Hill ­ Tech. Div., G. B0 ­ Hanford J, C„ Hindman ­ Chem. Div. ­ Argonne H. H. Hyman ­ Chem. Eng. Div. ­ Argonne J„ J. Katz ­ Chem. Div. ­ Argonne B„ Kaplan ­ Chem. Eng. Div. ­ Argonne L« Kaplan ­ Chem. Div. ­ Argonne M. Kilpatrick ­ Chem. Dept. ­ Illinois Institute of Technology So Lawroski ­ Chem. Eng. Div. ­ Argonne M. Lewis ­ Tech. Div0, G„ ED ­ Hanford L. Wo Niedrach ­ Chem. Div. ­ KAPL T. C. Runion ­ Tech„ Div„ ­ Oak Ridge R9 W. Stoughton ­ Chem„ Div. ­ Oak Ridge E0 Ho Turk ­ Chem. Eng. Div. ­ Argonne R0 C„ Vogel ­ Chem. Dept„ ­ Illinois Institute of Technology S. Vogler ­ Chem. Eng. Div. ­ Argonne R0 Wagner ­ Chem8 Eng„ Div. ­ Argonne P0 Wehner ­ Chem. Div. ­ Argonne CHEMICAL ENGINEERING DIVISION S. Lawroski, Division Director C. E0 Stevenson, Assoc. Division Director Operated by the University of Chicago under Contract W­31­109­eng=38 2-9?- V CONFIDENTIAL; ­2­ • V \ . • ■ >•« • -if . _V <•* " -~i.' ~L r (? ~ > 1 I TCONffDENTIACtJ;I TABLE OF CONTENTS '""" Page List of Tables . O o o o o O0OO00O0O0*90»00O*O0 4 List of Figures . OO099900O09OO99 5 U« ADSTfJTcLCTr OOOO0O09O000 • 0 0 9 O O 6 I. Analytical Methods for Ruthenium Ao Gravimetric ...'..... o o e » e e o 7 Bo Colorimetric Methods 0O0OO0O0 OOOOO00O 9 Co Valence State Analyses .. O0OO0000O0O00OO0O 11 D. Radiochemical Methods of Analysis 0 O 0 O O O O 12 E. Preparation of Standards . 000000009­0 0000 12 II. Pure Compounds A. Ruthenium Pentafluoride 14 III. Solution Chemistry Ao. Spectrophotometry Data . 0000000000000 15 Bo Polarography O0O00000000O00O0000O000 25 IVo Ruthenium in Solvent Extraction 00 0 0 0*000 O O « o 28 V. Special Problems and Techniques Ao Decontamination by Volatilization . 0000000000 32 sir •'• i ■ ir J­1M <2#f■- 5U. { 1 1 CONFIDENTIAL! '■} LIST OF TABLES Table Page I. Per Cent Error in Ruthenium Analysis 9 II. The Absorption Spectra of Ruthenium (IV) in Hydrochloric Ac xo, ooxuixxons 00000000 0000000*0000000 xy III. The Absorption Spectra of Unknovm Forms of Ruthenium in Hydrochloric Acid ............. ......o.. 21 IV. The Absorption Spectra of Ruthenium in Nitric Acid ooxuuxons 0000o00O0»0o«o**0O0«000 #00 £j V. The Absorption Spectra of Ruthenium in Sulfuric Acid O OXllU XOH.S 0000000000*000 O0O00000OO00 *~i+ VI. Summary of Polarographic Data on Various Ruthenium OOXUlvXOIlS O00OO O 090 OO 00 000*0 00 000O00 ^O VII. Polarographic Reduction of Ruthenium (IV) in 1 N i©rcnxorxc ACXCL 00000000000000000000000 *~ ( VIII. Extraction and Scrub of Ruthenium Tracer With and Without Interchange ...­«....».. ..».....». 29 IX. The Effect of Hydrochloric Acid on the Extraction and Scrubbing of Ruthenium Tracer ................ 30 X. Per Cent Extraction of Platinum Metals 31 XI. Ozonization from Dilute Acid Solutions ............. 34 XII. Ozonization from UNH Solutions .. .......... 35 XIII. Ozonization from Dissolver Solutions ...... 36 t t 4i COFIDENTIALI './ "LIST OF FIGURES Figure Page 1 Absorption Curve of Ruthenium (IV) Chloride :(D . 37 2 Absorption Curve of Ruthenium (IV) Chloride (>al ) . 38 3 Absorption Curve of Ruthenium (IF) Chloride >bl( ) . 39 4 Absorption Curve of Ruthenium (IV) Chloride (cl ) . 40 5 Absorption Curve of Ruthenium (IV) Chloride (,dl ) . 41 6 Absorption Curve of Ruthenium (IV) Chloride :*i) 0 0 0 0 0 0 . 42 7 Absorption Curve of Ruthenium (IV) Chloride (,gl ) . 43 8 Absorption Curve of Ruthenium (IV) Chloride '[hi ) . 44 9 Absorption Curve of Ruthenium (IV) Chloride- :JD o « 45> 10 Absorption Curve of Ruthenium (IV) Chloride ;ki( ) 00*00000 46 11 Absorption Curve of Ruthenium (IV) Chloride :n( ) . 47 12. Absorption Curve of Ruthenium (IV) Chloride (.ml ) 0 A * 0 O 0 O 48 13 Absorption Curve of Ruthenium (IV) Chloride >nl( ) O O 0 O 0 O 0 49 14 Absorption Curve of Ruthenium (IV) Chloride (.ol ) O O 0 O 0 0 . 50 15 The Effect of Saturation with Chlorine on the Absorption of a Ruthenium (IV) Chloride Solution „ OO0 00000 51 16 The Absorption Spectra of Ruthenium Tetroxide in 2 N Nitric Acid and 2 N Hydrochloric Acid Solutions 9" "O O * O O 0 . 52 17 The Absorption Spectra of Two Ruthenium Tetroxide - Nitric Acid Solutions Reduced with (1) Sulfuric Acid and (2) Hydrogen Peroxide 00O0OOOO0O 53 0. ABSTRACT ' The conferees discussed gravimetric, colorimetric, and radiochemical techniques for ruthenium analysis. Acceptable procedures were reported using each of these techniques. The determination of valence states was in a less satisfactory state. Ruthenium tetroxide and ammonium hexachloro-^ ruthenate were suggested as primary standards. The absorption spectrum of ruthenium in a wide variety of solutions has been investigated and some peaks identified as characteristic of a particular ruthenium structure in different solutions. The effects of complexing ions, acidity and valence states have all been studied by this technique. Polarographic data of a preliminary nature was presented for various solutions. The difficulty of analyzing typical solvent extraction data on the behavior of ruthenium was emphasized. The possibility of radiocolloid forma• tion as an explanation was mentioned. It was pointed out that other platinum metals showed similar irreproducibility in extraction into hexone from dis• similar aqueous solutionsB The behavior of ruthenium tetroxide in solvent extraction was discussed as well as the production and volatilization of this form of the element. Its use as a special decontamination procedure was emphasizedo i^n CONFIDENTIAL 2-?£ < CONFIDENTIAL ANALYTICAL METHODS FOR RUTHENIUM A. Gravimetric The three methods of gravimetric analyses principally investigated at the various sites were the magnesium precipitation(l). the thionalid method of Rogers and Beamish^), and the Gilchrist procedure^). The magnesium precipitation method was standardized at Argonne by means of the standard ammonium hexachlororuthenate, (NH, )2RuCl^*o The precipita• tion, when carried out in 6 M hydrochloric acid, agreed within f 1% with the calculated value after adding a 6% empirical correction factoro In 3 M hydrochloric acid the results were erratic. When the acid concentrations were as low as 0»5 M, the results were 20 to 30% above the calculated value. The thionalid procedure reported by Rogers and Beamish has been tested both at Argonne and Chalk River. The method consists of a sodium bromate-sulfuric acid distilla• tion of ruthenium tetroxide (sample should contain 8-10 mg. ruthenium) into a cold 3% hydrogen peroxide absorbing solution. This is followed by boiling to eliminate the hydrogen peroxide and to concentrate the solution. The acidity is then adjusted to 0.2 to 0.5 M hydrogen ion concentration with hydrochloric acid and the thionalid added.
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