CHEMISTRY 
 
 OF URANIUM 
 
 NET 
 
 H. BREARLE 
 
LIBRARY 
 
 OF THE 
 
 UNIVERSITY OF CALIFORNIA. 
 
 ClMS 
 
THE ANALYTICAL CHEMISTRY 
 OF URANIUM 
 
With 85 Illustrations. 8v0, 14^. net 
 
 THE ANALYSIS OF STEEL-WORKS 
 MATERIALS 
 
 By HARRY BREARLEY 
 
 AND 
 
 FRED IBBOTSON, B.Sc. (Lond.) 
 
 Demonstrator of Micrographic Analysis, U niversity College, 
 Sheffield 
 
 LONGMANS, GREEN, AND CO. 
 
 LONDON, NEW YORK AND BOMBAY 
 
THE 
 
 ANALYTICAL CHEMISTRY 
 OF URANIUM 
 
 BY 
 
 HARRY BREARLEY 
 
 JOINT AUTHOR OF "THE ANALYSIS OF STEEL-WORKS MATERIALS 1 
 
 LONGMANS, GREEN, AND CO. 
 
 39 PATERNOSTER ROW, LONDON 
 
 NEW YORK AND BOMBAY 
 
 1903 
 
 All r/gJ'ts reserved 
 

PREFACE 
 
 ANY ONE desirous of mastering the practical 
 determination of any metal in its ores and in the 
 commercial products whose value it influences, 
 perhaps could do no better, if immediate results 
 were of no consequence, than to choose a gravi- 
 metric and a volumetric process which worked 
 well with pure solutions of the metal's salts, and 
 then to set about observing the influence exerted 
 by variations in the mode of operating and by 
 the presence of other metallic salts. Such a 
 procedure, at any rate, usually gives ultimate satis- 
 faction and confidence, and makes valuable addi- 
 tions to one's permanent knowledge of chemical 
 facts, as well as, now and again, eliminates some 
 fictions. 
 
 Some years ago the author was invited to 
 familiarize himself with the assay of some metals 
 of which he had no special knowledge with 
 the view of taking charge of an analytical practice 
 in which these metals were to be largely dealt 
 
 57 
 
vi PREFACE. 
 
 with. As far as time permitted, his mode of 
 doing so was that just indicated. In a few 
 instances the outlines then accumulated have been 
 filled in, and an orderly arrangement of the 
 material made, so that it might be as useful as 
 possible in the laboratory. 
 
 If each element were dealt with in such a 
 manner, the accumulated result would save much 
 vexation and laborious search. This, in time, 
 some industrious person, free from the necessity of 
 earning a living, may do. Meanwhile this booklet, 
 by the manner in which it is received, may assist 
 one to decide whether more of a like kind are 
 desirable, or whether the author is mistaken in 
 the general usefulness of the plan. 
 
CONTENTS 
 
 PAGE 
 
 INTRODUCTORY NOTE i 
 
 I. MODES OF DETERMINING URANIUM 3 
 
 II. THE DETERMINATION OF URANIUM AS PHOSPHATE 7 
 
 III. THE SEPARATION OF URANIUM 
 
 FROM IRON . 13 
 
 FROM NICKEL, COBALT, AND ZINC 20 
 
 FROM MANGANESE 21 
 
 FROM ALKALIS AND ALKALINE EARTHS ... 22 
 
 FROM COPPER AND OTHER METALS PRECIPI- 
 TATED BY SULPHURETTED HYDROGEN ... 24 
 
 FROM SILICA 25 
 
 FROM MOLYBDENUM 26 
 
 FROM TUNGSTEN 28 
 
 FROM CHROMIUM 29 
 
 FROM VANADIUM 30 
 
 FROM TITANIUM 33 
 
 FROM ALUMINIUM 34 
 
 IV. THE ANALYSIS OF URANIUM ORES 
 
 PITCHBLENDE 38 
 
 CARNOTITE 42 
 
 METALS AND ALLOYS 43 
 
**r N 
 
 UNr 
 
 THE ANALYTICAL CHEMISTRY 
 OF URANIUM 
 
 INTRODUCTORY NOTE. 
 
 URANIUM was discovered by Klaproth in 1789, 
 but the actual metal was isolated by Peligot in 
 1842 ; what had previously been regarded as 
 the metal was really its lower oxide (UO 2 ). 
 
 The ore occurs in Saxony, Cornwall, and 
 America, but the deposits are generally of a 
 very sparing character. The Cornish mine at 
 St. Stephen's, where ore (mostly uranic phosphate) 
 is said to occur in a continuous lode from 3 to 
 5 feet thick, is exceptional. 
 
 Uranium is closely related (chemically) with 
 chromium, molybdenum, and tungsten. These 
 latter metals have each an acid-forming trioxide ; 
 the trioxide of uranium, however, acts both as an 
 acid (sodium uranate) and a base (uranyl nitrate). 
 Early papers on the chemistry of uranium are 
 unintelligible unless one bears in mind, not only 
 that the protoxide was mistaken for the metal, 
 
2 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 but also that the atomic weight of the metal has 
 been doubled in recent times. 
 
 Uranous oxide is formed by heating U 3 O X 
 in hydrogen. It is the base from which the 
 unstable uranous salts are derived, e.g. U(SO 4 ) 2 . 
 
 Uranic oxide unites with strong bases to 
 form uranates which have a composition analo- 
 gous to dichromates, e.g. Na 2 U 2 O 7 (sodium ura- 
 nate). But it also acts as a base in the formation 
 of uranyl salts ; eg. UO 2 SO 4 and UO 2 (NO 3 ) 2 . 
 
 Uranoso=uranic oxide occurs in nature as 
 pitchblende, and may be prepared artificially by- 
 heating any oxide in air or oxygen. When 
 digested with nitric acid it dissolves to UO^NQ*)* 
 and this salt by limited ignition is converted^ to 
 the trioxide, of which it is a derivative. When 
 U 3 O 8 is very strongly ignited it loses oxygen, and 
 passes to U 2 O 5 ; this, it is surmised, i^fthe change 
 
 which takes place with the formation "of an 
 
 V *? "** 
 intense black colour when porcelain painted 
 
 with the uranic glaze is fired. 
 
 Higher oxides, which give rise to perura- 
 nates, are formed by adding hydrogen peroxide 
 to uranyl solutions. These, have been investi- 
 gated by Fairley and others, and made use of 
 to a limited extent in the analysis of uranium 
 compounds. 
 
I. 
 
 MODES OF DETERMINING URANIUM. 
 
 Qravimetrically, the determination of uranium 
 depends on its precipitation as alkaline uranate, 
 which is weighed as such or ignited to oxide ; as 
 protoxide by means of ammonium sulphide ; or 
 as phosphate. 
 
 The yellow precipitate formed when caustic 
 soda -is added to a solution of uranyl nitrate is a 
 hydrated diuranate, which loses water merely on 
 ignition, and may be weighed as Na 2 U 2 O 7 . When 
 ammonia is used instead of soda, the analogous 
 precipitate is decomposed on ignition, and yields 
 "a compound approximating more or less to U 3 O 8 , 
 according to circumstances. If only moderately 
 heated the ammonium uranate does not ignite 
 uniformly to the dark green colour of U 3 O 8 ; it 
 contains visible streaks and patches of a yellow 
 or brown colour. 1 At higher temperatures, how- 
 ever, the oxide becomes practically black (though 
 
 1 These are said to be formed when traces only of alkaline 
 earths are present. 
 
4 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 it gives a green streak), and loses slightly in 
 weight. According to Zimmermann, pure U 3 O 8 
 is formed only when heated and cooled in a 
 current of oxygen ; if heated in air and cooled 
 quickly a small amount of oxygen is lost, and in 
 an indifferent gas the loss is still greater : never- 
 theless, the elaboration of a current of oxygen 
 may be omitted in technical assays, as the error 
 is comparatively trifling. 
 
 The precipitation of uranium by means of 
 ammonium sulphide is accurate, and lends itself 
 to a number of important separations ; but great 
 care must be taken to exclude carbonates from 
 the solution and the reagent, as they prevent a 
 complete precipitation. The precipitate thus 
 formed may be ignited in hydrogen and weighed 
 as UO 2 , or ignited in air to U 3 O 8 . Kern found 
 that (NH 4 ) 2 U 2 O 7 could be readily converted to 
 UO 2 by ignition in hydrogen, but that a previously 
 ignited precipitate could not be so reduced and 
 reweighed for purposes of control, particularly if the 
 operation was carried on in a porcelain crucible. 
 
 The precipitate of UO 2 HPO 4 , which is formed 
 when sodium phosphate is added to an acetic acid 
 solution containing uranium, is gelatinous, and 
 washes badly worse than ammonium uranate 
 even, and is to be desired only on account of 
 
MODES OF DETERMINING URANIUM. 5 
 
 the lower factor needed to convert the weight of 
 the ignited precipitate to metallic uranium. This 
 difficulty can be partly met, as Kern points out, 
 by the careful use of dihydrogen ammonium 
 phosphate instead of the sodium salt ; the most 
 satisfactory procedure, however, is that noticed 
 in the next section. 
 
 Attempts to weigh the dried precipitate as 
 ammonium uranyl phosphate (UO 2 NH 4 PO 4 ) have 
 not met with much success ; it is customary, 
 therefore, to ignite it apart from the paper, and 
 weigh as pyrophosphate (UO 2 ) 2 P 2 O 7 . If ignited 
 at low redness the precipitate has a pure yellow 
 colour, but at higher temperatures it is partly 
 reduced and becomes green. It is feasible, of 
 course, to ignite precipitate and paper together, 
 and then treat the green residue with nitric acid, 
 evaporate, and ignite to low redness, so as to 
 restore the characteristic yellow colour. 
 
 Uranium may be electro-deposited from acetate 
 solutions, and ignited to U 3 O 8 . Separations from 
 barium, calcium, magnesium, and zinc have been 
 based on this reaction, but it is interfered with by 
 many of the common metals, particularly those 
 of the iron group. 
 
 Volumetric processes for the determination 
 
6 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 of uranium have attracted little attention, and 
 failed to inspire much confidence. The titration 
 with a standard solution of microcosmic salt, using- 
 ferrocyanide as a spot indicator, is known rather 
 as the inverse of a common way of titrating phos- 
 phoric acid than as a widely usable means of esti- 
 mating uranium. Guyard's process depends on 
 the precipitation of a triple ammonium-uranium- 
 manganese phosphate when a solution of man- 
 ganic metaphosphate is added to an acetate 
 solution of uranium. The process is only suitable 
 for the estimation of large amounts of uranium. 
 
 The volumetric method most in vogue depends 
 on the reduction of UO 3 to UO 2 in acid solutions 
 by means of zinc, aluminium, or magnesium, 
 followed by titration with permanganate in the 
 usual manner, contact with air being prevented 
 as much as possible. There are no decisive 
 colour changes to indicate complete reduction, so 
 that an abundance of the metallic reducing agent 
 must be used, and a time limit, depending on the 
 amount of uranium dealt with, must be adhered 
 to. Under the most favourable circumstances 
 this limit exceeds the time needed to perform a 
 gravimetric estimation, so that the usefulness of 
 volumetric processes generally are confined to 
 special cases. 
 
II. 
 
 THE DETERMINATION OF URANIUM AS 
 PHOSPHATE. 
 
 ABOUT ten times as much microcosmic salt as 
 there is judged to be uranium present is added to 
 the boiling solution ; then dilute ammonia, until a 
 small precipitate is formed ; then just as much nitric 
 acid as clears the solution, but no more ; and, 
 finally, sodium thiosulphate equivalent to about 
 10 grams of the crystallized salt. The solution 
 becomes intensely yellow, and almost immediately 
 deposits a voluminous precipitate. After boiling- 
 for ten or fifteen minutes, this precipitate con- 
 tains all the uranium, and is so dense that it 
 settles immediately, and may be easily washed by 
 decantation and collected on the filter. The pre- 
 cipitate is transferred to a porcelain crucible, 
 ignited, the green residue weighed, just moistened 
 with nitric acid and gently heated. It dissolves 
 to a yellow solution with slight effervescence, and 
 is then dried, ignited at low redness, and the yellow 
 
8 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 residue weighed. ( (UO 2 ) 2 P 2 O 7 x o'668i = U.) 
 Pure pyrophosphate dissolves entirely when 
 heated with nitric acid ; in practice an insoluble 
 residue, weighing a milligram or so, may be 
 found. 
 
 If a series of weighings of the green and 
 yellow residues be scrutinized, a fairly uniform 
 relation is seen to exist between them, and, for 
 many technical purposes, it is unnecessary to take 
 the extra trouble of converting the former to the 
 latter. This is illustrated by the following table, 
 which also justifies the above mode of operating. 
 In each case the solution was diluted to about 
 300 c.c. before precipitating. 
 
 
 Green Residue. 
 
 Yellow Residue. 
 
 U. taken. 
 
 
 
 
 Weighed. 
 
 x 0-6855. 
 
 Weighed. 
 
 X 0.6681. 
 
 0*2220 
 
 0-3233 
 
 O'22l6 
 
 0-3322 
 
 0-22I9 
 
 0*I226 
 
 
 
 
 
 o- 1 840 
 
 0-I229 
 
 O'HIO 
 
 0*l6l7 
 
 0'iioS 
 
 0-1663 
 
 O'lIII 
 
 0-0666 
 
 0-0972 
 
 0*0666 
 
 
 
 
 
 O*O444 
 
 0-0660 
 
 0-0452 
 
 0-0675 
 
 0*0448 
 
 0*0220 
 
 0*0320 
 
 0-0219 
 
 0-0340 
 
 0*0227 
 
 O'OI 1 1 
 
 o'oi 70 
 
 0*01 16 
 
 0*0170 
 
 OOII4 
 
 The green precipitate is decidedly less hygro- 
 scopic than the yellow pyrophosphate, and may be 
 easily brushed from the crucible even after strong 
 ignition : it, however, is too hygroscopic to make 
 
DETERMINATION OF URANIUM AS PHOSPHATE. 9 
 
 the practice of brushing from the crucible a com- 
 mendable one. Fresenius' statement, that the 
 yellow salt is not hygroscopic, is contrary to all 
 my experience ; in fact, a good dessicator and 
 quick weighing are imperative if its weight is to 
 be depended on. The residue disintegrates and 
 leaves the sides of the crucible after absorbing 
 moisture from the air. 
 
 In each of the following experiments 30 c.c. of 
 a standard solution of uranyl nitrate, containing 
 0*2045 gram uranium, was used, and the volume 
 of the solution precipitated was about 300 c.c. 
 The figures in brackets represent the amount of 
 uranium obtained when calculated from the green 
 residue by the factor already used (0*6855.) The 
 agreement of the two sets of figures confirms the 
 statement already made, that its composition is 
 sufficiently constant to warrant its weight being 
 used in calculating the percentage of uranium for 
 technical purposes. 
 
 Acetic Acid. The operation is in no way 
 affected by moderate amounts of this acid. 
 
 Acetic acid (c.c.) o 10 30 50 
 
 U obtained (gr.) 0*2045 0*2042 0*2047 0*2049 
 Green precipitate (0*2046) (0*2053) (0*2048) 
 
 Time of Boiling. When large amounts of 
 
io THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 uranium are being handled, it is sometimes a 
 difficult and dangerous operation to boil the solu- 
 tion from ten to fifteen minutes on account of the 
 vigorous bumping. Nearly all the uranium is 
 down after boiling for a minute or two, but this 
 can hardly be depended on. The danger may be 
 avoided after adding the thiosulphate, by heating 
 only as long as is necessary to liberate a consider- 
 able amount of sulphur and form a precipitate, 
 which settles readily. Then, if 5 c.c. strong 
 ammonium acetate are added to destroy any free 
 mineral acid and complete the precipitation, little 
 or no further boiling is necessary. A small 
 amount of acetate may be added after long- 
 boiling, if further assurance of a complete pre- 
 cipitation is desired. The added acetate is harm- 
 less, as the following tests show : 
 
 Acetate (c.c.) 5 30 50 
 
 U obtained (gr.) 0*2046 0-2045 0*2044 
 
 (0*2051) (0-2049) 
 
 Ammonium Nitrate (20 grams). 
 0*2048 (0*2050) instead of 0*2045 gram uranium. 
 
 Ammonium Chloride (20 grams). 
 0*2042 (0*2046) instead of 0*2045 gram uranium. 
 
 Ammonium Sulphate (20 grams). 
 0*2038 (0*2046) instead of 0*2045 gram uranium. 
 
DE TERMINA TION OF URA NIUM A S PHOSPHA TE. 1 1 
 
 The precipitated uranyl phosphate, formed on 
 neutralizing, clears up less readily on adding nitric 
 acid than when ammonium sulphate is absent. 
 The same observation applies to the added sodium 
 sulphate. 
 
 Sodium Nitrate (20 grams). 
 
 0*2047 (0*2043) instead of 0*2045. 
 Sodium Chloride (20 grams). 
 
 0*2049 (0*2043) instead of 0*2045. 
 Sodium Sulphate (20 grams). 
 
 0*2035 (0*2036) instead of 0*2045. 
 
 Potassium Nitrate (20 grams). 
 
 Potassium salts are carried down. The weight 
 of the ignited pyrophosphate was equivalent to 
 0*2200 gram uranium, but, on dissolving and 
 reprecipitating a residue corresponding to the 
 correct weight of uranium is obtained, i.e. 0*2040 
 gram. 
 
 Microcosm ic Salt. Varying excesses of 
 this reagent may be used without detriment, but 
 more than the theoretical amount is necessary. 
 For example, the author, when using 5 grams 
 instead of the usual 2 grams, of microcosmic salt, 
 obtained a precipitate having a weight equiva- 
 lent to 0*2042 gram uranium. On dissolving 
 this and reprecipitating, without adding any more 
 
12 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 microcosmic salt, the resulting precipitate was 
 equivalent to 0*1988 gram; on again dissolving, 
 adding microcosmic salt, and again precipitating, 
 the weight of the residue was equivalent to 0*2030 
 gram. This shows that the second precipitate, 
 which contained nearly all the uranium, was a 
 basic compound. 
 
 Properties of the Precipitate. - The 
 ignited pyrophosphate is more readily soluble in 
 nitric than in sulphuric or hydrochloric acid ; con- 
 tamination with ferric oxide greatly decreases the 
 solubility. It is easily attacked by fused sodium 
 carbonate or caustic soda, but on extracting 
 with water the yellow residue contains only 
 about 90 per cent, of the uranium operated with. 
 The portion in the filtrate is at once detected 
 by the yellow colour which carbonated alkali 
 solutions give with hydrogen peroxide. 
 
III. 
 
 THE SEPARATION OF URANIUM. 
 
 SEPARATIONS FROM IRON. 
 
 By Acetates. The separation of uranium from 
 iron, by precipitating the latter as basic acetate, 
 was referred to in a general way by Gibbs, 1 
 but no particulars were given. Some phases of 
 the process were studied by Rheineck, 2 who 
 suggested that the operation was a delicate one, 
 and observed that a crystalline precipitate is 
 formed at once in concentrated, and, after some 
 time, in more dilute solutions, when sodium acetate 
 is added to any salt of the oxide of uranium. 
 
 The following experiments were made with 
 the object of determining in which direction the 
 weakness of the separation lay, rather than with 
 the idea of improving it for regular service. Five 
 grams of bar iron were dissolved in hydrochloric, 
 and oxidized with nitric acid, 25 grams ammonium 
 chloride and 150 c.c. standard uranium solution 
 
 1 Chemical News, xi. 102. 2 Chemical News^ xxiii. 233. 
 
1 4 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 added, and the mixture then neutralized and 
 divided into five equal portions. 
 
 (a) Was diluted to 300 c.c., and boiled. The 
 iron was almost entirely precipitated, and no 
 acetate whatever was added : 0*2055 gram 
 uranium was found in the filtrate, instead of 
 0*2045 gram. 
 
 (b) Five cubic centimetres strong ammonium 
 acetate were added, which precipitated the iron 
 immediately in the cold. The solution was then 
 boiled three or four minutes. The filtrate con- 
 tained only 0*0853 gram uranium. 
 
 (c) Treated like (b), but 10 c.c. acetic acid 
 were added before the acetate. A precipitate 
 formed after very little heating. The filtrate 
 contained 0*1994 gram uranium. 
 
 (d) Treated as (a), but added 0*5 c.c. acetate 
 to the boiling solution, to completely pre- 
 cipitate the iron 0*2000 gram uranium in the 
 filtrate. 
 
 (e) Treated as (a), but added 5 c.c. acetic acid 
 to the cold solution, and i c.c. ammonium acetate 
 to the boiling solution. The precipitation of the 
 iron was complete ; in fact, less acetate might 
 have been used. The filtrate contained 0*2048 
 gram uranium. 
 
 There is no doubt that when phosphoric acid 
 
THE SEPARATION OF URANIUM. 15 
 
 is absent, and the proportion of uranium is large 
 enough to yield a sufficient amount in the filtrate, 
 without having to deal with unwieldy precipitates 
 of basic ferric acetate, this separation is a reliable 
 one. The neutralized solution, however, should 
 contain i or 2 per cent, of free acetic acid, 
 and no more acetate should be used than will 
 comfortably precipitate all the iron. With these 
 precautions the separation appears to be quite as 
 easy as that of iron and nickel by the same 
 process. It is probable, also, that others of 
 the alkaline salts which have the power of 
 precipitating neutralized ferric solutions might 
 advantageously be substituted for ammonium 
 acetate. 
 
 By Alkalis. When ammonium carbonate is 
 added to a solution containing iron and uranium, 
 the former is precipitated, but may or may not be 
 free from the latter. A separation, which is practi- 
 cally perfect, can be made by pouring a solution 
 containing as much as 2 grams of iron into a 
 solution, which is kept agitated, of ammonium or 
 sodium carbonate or sodium bicarbonate. A little 
 iron, however, is apt to remain in solution, and it 
 is customary, if its presence is objectionable, to 
 allow it to settle out after prolonged standing 
 or to precipitate it with ammonium sulphide. 
 
i5 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 Separations made in this way gave the following 
 results : l 
 
 Am. carb. 
 Sod. carb. 
 Sod. bicarb. 
 
 U present. 
 
 U found. 
 
 0^0621 
 
 0*062 1 
 0-062I 
 
 00623 
 0'0622 
 
 o'o6 1 9 
 
 Caustic alkalis, of course, precipitate the ura- 
 nium along with the iron, but, according to Walker, 
 it remains in solution if hydrogen peroxide is also 
 present. 2 This separation appears to be quite 
 successful only when the proportion of iron is not 
 large and the total weight of the metals dealt 
 with is small. 
 
 By Ether, etc. Kern's valuable contribu- 
 tion to the quantitative separation and determina- 
 tion of uranium 3 deals particularly with the 
 separation of iron. His experimental work is 
 confined to the ether-extraction process, which 
 in other directions is already well known, and 
 he finds that the most complete separations are 
 obtained by using hydrochloric acid of no 
 specific gravity. More than one extraction is 
 
 1 I am indebted to my friend, Fred Ibbotson, B.Sc., for these 
 results. 
 
 2 Jour. Amer. Chem. Soc.,xx. 513. 
 
 3 Jour. Amer. Chem. Soc., xxiii., and Chemical News, vol. Ixxxiv. 
 
THE SEPARATION OF URANIUM. 
 
 necessary, and it is doubtful whether the process 
 is a desirable one unless ether extractions in other 
 directions are being regularly carried out. 
 
 A separation described by Rose depends on 
 the precipitation of the two oxides by ammonia, 
 ignition in a stream of hydrogen, and extraction 
 of the metallic iron with hydrochloric acid. Or 
 the iron may be volatilized from the mixture by 
 heating it in an atmosphere of the gaseous 
 acid. 
 
 The electro-deposition of iron from oxalate 
 solutions is said to lead to a perfect separation. 
 
 The separation by means of alkaline acetates 
 is trustworthy and convenient within the limita- 
 tions already referred to. Its value and accuracy 
 is further attested by the following results ; never- 
 theless, some other alkaline salt instead of acetates 
 could probably be used with advantage : 
 
 Fe present. 
 
 % U present. 
 
 % U found. 
 
 5 grams 
 
 0-8,7 
 
 0-836 
 
 3 
 
 3"i8 
 
 3' 1 S 
 
 2 
 
 473 | 477 
 
 1 
 
 20-45 
 
 20-40 
 
 2 
 
 I0'22 
 
 10-15 
 
 When a minor constituent of any mixture is 
 required to be estimated, it is generally best to 
 
 c 
 
i8 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 separate it by direct precipitation. This can be 
 accomplished with a mixture of uranium and iron- 
 by applying, under suitable circumstances, the 
 method already described for determining uranium 
 in pure solutions. The operations are similar 
 to those used for separating small amounts of 
 aluminium and chromium from steel as phos- 
 phate. The separation can, of course, be used 
 equally well when the proportion of uranium is 
 great. 
 
 The iron being in the ferrous state, and 
 preferably as chloride, heat the solution nearly to 
 boiling, add microcosmic salt in the proportion 
 already indicated, and then dilute ammonia until 
 the precipitated flocks of ferrous hydrate are no 
 longer quite redissolved. Clear with the smallest 
 possible excess of hydrochloric acid, add 10 
 grams of sodium thiosulphate and 20 c.c. acetic 
 acid, and boil for ten to fifteen minutes. Allow 
 the precipitate to settle, filter as quickly as pos- 
 sible, and wash with hot water containing a few 
 cubic centimetres per litre of acetic acid and am- 
 monium acetate. 
 
 The residue, after redissolving from the filter 
 and the accompanying sulphur, may be reprecipi- 
 tated to separate the remaining portion of iron, 
 which, when the operation is properly performed, 
 
THE SEPARATION OF URANIUM. 19 
 
 is rarely greater and often much less than the 
 amount of uranium. Or, instead, the residue may 
 be ignited, fused with sodium carbonate, dissolved 
 in hydrochloric acid, filtered after evaporation to 
 remove any such insoluble body as silica, and 
 reprecipitated as before. The ignited precipitate 
 has the characteristic green colour, and may, if 
 desired, be converted to the yellow pyrophosphate. 
 Not more than a negligible trace of ferric oxide, 
 carried down by the sulphur in the final precipita- 
 tion, should be present. The following results 
 were obtained in this way : 
 
 Iron Used. 
 
 % U present. 
 
 % U found. 
 
 5 grams 
 
 0-136 
 
 0-136 
 
 5 
 
 0'273 
 
 0-280 
 
 5 
 
 0546 
 
 o'555 
 
 10 
 
 0'068 
 
 0*070 
 
 5 
 
 0'8l9 0*836 
 
 i 
 
 The addition of ammonium acetate to complete 
 the precipitation and shorten the boiling is not 
 commendable when much iron has to be separated. 
 In order to avoid violent bumping, I have found 
 the following plan to work well : Slide a small 
 widely perforated filter-plate into the solution, 
 and limit its movement along the bottom of the 
 beaker by putting the drawn-out end of a glass 
 
20 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 stirring-rod through one of the holes. A similar 
 plate, allowed to move freely, breaks the steam 
 envelopes in a haphazard way, and may cause 
 the liquid to boil over. 
 
 SEPARATIONS FROM NICKEL, COBALT, AND 
 ZINC. 
 
 These metals are usually separated from 
 uranium by passing a stream of sulphuretted 
 hydrogen through a boiling solution of the ace- 
 tates (Gibbs). Zinc only may be separated by 
 means of ammonium carbonate (Rammelsberg). 
 Nickel and cobalt, on the other hand, remain in 
 solution when an emulsion of barium carbonate 
 is added to a mixture of the metals containing a 
 small amount of free acid and some ammonium 
 chloride. Uranium is precipitated, but must, 
 subsequently, be separated from the excess of 
 barium carbonate. The electro-deposition of the 
 uranium as hydrated oxide from an acetate solu- 
 tion is not interfered with by the presence of zinc. 
 
 The presence of either nickel, cobalt, or zinc 
 in no way interferes with the estimation of 
 uranium by the method already given for pure 
 solutions. The following are results of test 
 analyses : 
 
THE SEPAR 
 
 F URANIUM. 
 
 21 
 
 Metal present. 
 (o'io grams.) 
 
 Acetic Acid (c.c.)- 
 
 U present. 
 
 U found. 
 
 Zinc . . . 
 
 
 
 0-2045 
 
 0-2056 
 
 Zinc . . . 
 
 50 
 
 0-2045 
 
 02056 
 
 Nickel . . 
 
 O 
 
 0*2045 
 
 0*2053 
 
 Nickel . . 
 
 50 
 
 0-2045 
 
 0*2049 
 
 Cobalt . . 
 
 
 
 0-2045 
 
 0-2046 
 
 Cobalt . . 
 
 50 
 
 0-2045 
 
 0-2049 
 
 The respective filtrates can be used conve- 
 niently for determining the separated metal ; 
 those containing zinc or cobalt (after boiling with 
 nitric acid to destroy the thiosulphate) by pre- 
 cipitating as the double ammonium phosphate, 
 and those containing nickel by making alkaline 
 and titrating with potassium cyanide and silver 
 iodide. 
 
 SEPARATIONS FROM MANGANESE. 
 
 The separation of manganese from uranium 
 does not appear to have been much studied. It 
 can be separated, according to Rammelsberg, with 
 ammonium carbonate alone, but the separation 
 generally described is that applicable to other 
 members of its group, viz. precipitation with 
 sulphuretted hydrogen from a solution containing 
 alkaline carbonates. 
 
 When uranium is precipitated as phosphate in 
 
22 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 the manner described above, it carries down a 
 small portion of any manganese present in the 
 solution. A series of separations of 0*10 gram 
 Mn from 0*2045 gram uranium were made in 
 solutions containing amounts of acetic acid, vary- 
 ing from o to 50 c.c. The manganese associated 
 with the uranyl pyrophosphate varied from 0*0013 
 to 0*0006 gram. 1 When the Mn 2 P 2 O 7 equiva- 
 lents of these figures were deducted from the 
 total weights, the remainders calculated to amounts 
 of uranium varying between 0*2030 and 0*2050 
 gram. 
 
 SEPARATIONS FROM ALKALIS AND ALKALINE 
 EARTHS. 
 
 The separation of alkalis from uranium is of 
 technical importance, as potash is a very con- 
 siderable constituent of an industrial ore car- 
 notite. Alkalis, alkaline earths, and magnesia 
 can be separated by precipitating the uranium 
 several times with ammonia in the presence of 
 ammonium chloride ; but, considering how badly 
 ammonium uranate filters, this separation is an 
 
 1 The amount is easily determined by dissolving in nitric acid 
 oxidising with sodium bismuthate, and titrating the permanganate 
 formed with ferrous sulphate. 
 
THE SEPARATION OF URANIUM. 23 
 
 undesirable one. It is much better to precipitate 
 the uranium from acetic solutions with ammonium 
 phosphate, which, according to Fresenius, effects 
 a complete separation from alkalis and alkaline 
 earths. Potash is the most difficult element to 
 separate, and if present in large amounts a second 
 precipitation may be necessary. 
 
 The separation of calcium as oxalate from 
 ammonium carbonate solutions has been strongly 
 disparaged by Alibigoff. He effects the separa- 
 tion also from alkalis and strontium, but not 
 barium by boiling the solution, containing 
 ammonium chloride or nitrate, with an emulsion 
 of mercuric oxide. 
 
 The separation of barium with sulphuric acid 
 is accurate and convenient. The separation of 
 calcium and strontium, in the same way, from 
 alcoholic solutions is practised, but for small 
 amounts is much less satisfactory. 
 
 The precipitation of uranium as phosphate by 
 boiling acetic acid solutions with thiosulphate 
 effects a complete separation from calcium. If 
 no acetic acid is present a portion of the calcium 
 is precipitated as phosphate. The following 
 tests were made on solutions (300 c.c.) con- 
 taining 0*10 gram of calcium and 0*2045 gram 
 uranium : 
 
24 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 Acetic Acid (c.c.). 
 
 U found. 
 
 o 
 5 
 
 10 
 
 0-2536 
 0-2063 
 02056 
 
 20 o'2o47 
 
 5o 
 
 0*2043 
 
 The lime in the filtrate can be determined 
 simply by adding an excess of ammonium oxa- 
 late, allowing the solution to cool, filtering, ignit- 
 ing the residual oxide, transforming it to sulphate, 
 and weighing. The weight of the oxide cannot 
 be relied upon, as it may contain sulphuric acid. 
 
 Magnesium does not interfere with the pre- 
 cipitation of uranium. 
 
 Acetic acid (c.c.) . o 5 
 
 U obtained (gr.) . 0-2046 0*2051 
 
 SEPARATION FROM COPPER AND OTHER METALS 
 PRECIPITATED BY SULPHURETTED HYDROGEN. 
 
 The presence of metals whose sulphides 
 are insoluble in very dilute acid solutions would 
 interfere with the chosen method of precipitat- 
 ing uranium. When any single member of this 
 group which includes lead, cadmium, mercury, 
 bismuth, copper, silver, tin, antimony, and arsenic 
 
THE SEPARATION OF URANIUM. 25 
 
 has to be separated, its precipitation with sul- 
 phuretted hydrogen, from a suitably acidified 
 solution, can be arranged. But if it is desired to 
 detect and separate any (unknown) one of them, 
 the acidity must be slight enough to permit the 
 complete precipitation of the one whose sulphide 
 is most easily dissociated, viz. lead. A complete 
 precipitation of lead as sulphide can be made from 
 solutions containing 2 per cent, of concentrated 
 hydrochloric acid. When 2\ per cent, of concen- 
 trated acid is present the precipitation is incomplete. 
 This is the conclusion arrived at by Kern, after 
 making a series of quantitative separations under 
 varying conditions of acidity and temperature. 
 
 SEPARATION FROM SILICA. 
 
 The ignited pyrophosphate always contains 
 silica when the precipitation has been made from 
 a solution containing a soluble silicate. Thus, 
 from a solution containing sodium silicate equal 
 to 0*184 gram silica, 0*2045 gram uranium 
 carried down in the two cases 0*0 10 and 0*006 
 gram silica respectively. 
 
 If the silica is not removed by evaporation 
 with acids prior to the precipitation, it remains 
 insoluble on digesting the pyrophosphate with 
 
26 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 nitric acid, and can be filtered off, weighed, and 
 approximately allowed for, or the uranium may 
 be reprecipitated from the filtrate. 
 
 Uranyl pyrophosphate loses weight when 
 treated with hydrofluoric acid alone. With a 
 mixture of hydrofluoric and nitric acid no loss 
 occurs ; but it is necessary to evaporate a second 
 time with nitric acid only, in order to secure the 
 yellow pyrophosphate free from fluorides. A 
 mixture of hydrofluoric and sulphuric acids may 
 also be used if the weight of the green residue is 
 being depended upon ; but in that case a very 
 strong ignition is needed in order to drive off all 
 the sulphuric acid. 
 
 SEPARATION FROM MOLYBDENUM. 
 
 Molybdenum is partly precipitated as sulphide 
 when an acid solution containing it is boiled with 
 thiosulphate. The means of precipitating uranium 
 previously adhered to cannot therefore be used in 
 the presence of this element ; but a very satis- 
 factory determination can be made by raising the 
 clear acid solution of the two metals to boiling 
 point, and adding at once the required amount 
 of phosphate mixed with as much hot ammonium 
 acetate as will destroy all the free mineral acid. 
 
THE SEPARATION OF URANIUM. 27 
 
 The precipitate is then washed well by decanta- 
 tion, and collected on the filter. The washing 
 is somewhat facilitated by adding a small quantity 
 of floured sulphur during the decantation. 
 
 Mo present . 0*0000 cviooo 0*2000 gram 
 U obtained . 0-2045 0-2046 0*2046 
 
 The estimation of the molybdenum in the 
 filtrate, at least so far as its precipitation as lead 
 molybdate is concerned, is complicated by the 
 presence of phosphoric acid ; it may therefore be 
 remarked, that molybdenum can be estimated on 
 a separate portion in the following manner, with- 
 out previously removing the uranium : 
 
 To the hot solution containing a few cubic 
 centimetres hydrochloric acid in excess, add enough 
 lead acetate to combine with all the molybdenum 
 present, and then sufficient ammonium acetate to 
 destroy the free hydrochloric acid. The precipi- 
 tated lead molybdate, which is very granular and 
 easily washed, is ignited and weighed. The 
 traces of uranium which the precipitate may 
 contain can be recovered, if desired, by pouring 
 the hydrochloric acid solution of it into caustic 
 soda ; the error which they introduce is, however, 
 quite insignificant. The uranium in the original 
 filtrate may be estimated as phosphate only after 
 
28 THE ANALYTICAL CHEMISTRY OF URANIUM, 
 
 separating the lead either by passing sulphuretted 
 hydrogen or evaporating with sulphuric acid. 
 
 SEPARATION FROM TUNGSTEN. 
 
 Tungsten may be completely precipitated from 
 neutral solutions by uranyl nitrate or chloride (but 
 not acetate, according to Hitchcock) in the form 
 of uranyl tungstate. This fact, and the marked 
 tendency of tungstic acid to precipitate spontane- 
 ously from acidified solutions, prevent uranium 
 from being determined as phosphate in a mixture 
 of the two metals. Evaporation to dryness on 
 the water-bath with a good excess of hydrochloric 
 acid is a very satisfactory means of making the 
 separation, because, after boiling with dilute 
 hydrochloric acid (i in 5), all the tungsten is left 
 in the residue, and requires to be merely ignited 
 and weighed as tungstic oxide ; and all the 
 uranium is in the filtrate ready to be estimated 
 in the usual manner. From a synthetic mixture 
 of 0*1992 gram tungsten and 0*2045 gram 
 uranium there were obtained 0*1989 and 0*2040 
 gram respectively. 
 
THE SEPARATION OF URANIUM 29 
 
 SEPARATION FROM CHROMIUM. 
 
 The separation from this element can be made 
 most easily when it exists as chromic acid ; as 
 chromic oxide it is completely precipitated along 
 with the uranyl phosphate. The chromium can 
 be conveniently oxidized with sodium peroxide, 
 but it is almost impossible in the presence of 
 uranium to entirely decompose the excess of 
 peroxide by boiling. It is therefore necessary to 
 proceed as follows : 
 
 Neutralize most of the free acid with sodium 
 carbonate, and then add sodium peroxide until the 
 solution becomes strongly alkaline. Both metals 
 are precipitated and again dissolved, the chromium 
 being entirely in the higher state of oxidation. 
 Boil the solution well, then acidify, and add a 
 small volume of decinormal permanganate (10 
 c.c. should be ample), and boil for about ten 
 minutes. If the permanganate decomposes at all 
 (thus showing that a portion of the chromic acid 
 was reduced by the residual hydrogen peroxide 
 in the acid solution) then filter off the manganic 
 oxide through asbestos fibre, and destroy any 
 unused permanganate with a few drops of hydro- 
 chloric acid. The acid liquor is now made slightly 
 alkaline with ammonia, decidedly acid with acetic, 
 
30 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 and when it boils briskly an excess of microcosmic 
 salt is added, and the filtration proceeded with as in 
 the separation from molybdenum. The chromium 
 in the filtrate is estimated volumetrically. 
 
 Uranium could probably be precipitated from 
 an acetic solution of chromic acid as uranyl vana- 
 date ; the converse of this is Klecki's method 
 for separating vanadium from chromium. The 
 uranium may also be precipitated with caustic 
 soda, or the chromium may be thrown down with 
 mercurous nitrate. Other means of making the 
 separation are those of electro-deposition, and 
 that depending on ignition of the oxides in a 
 current of hydrogen and extraction of the uranium 
 with nitric acid. 
 
 SEPARATION FROM VANADIUM. 
 
 Vanadium is an essential constituent of Car- 
 notite, and occurs also in small amounts in other 
 uranium ores. Artificial compounds of uranium 
 and vanadium do not occur in commerce, and 
 therefore the separations to be found in the litera- 
 ture of the subject refer almost exclusively to 
 the analysis of particular ores, and may not be 
 generally applied. For instance, such amounts of 
 
THE SEPARATION OF URANIUM. 31 
 
 vanadium as occur in pitchblende are separated 
 (Lallemand) by pouring the filtered nitric acid 
 solution of the mineral into sodium carbonate, 
 which causes the vanadium to go down with the 
 iron and the uranium to pass into solution. 
 Fritchle, on the other hand, precipitates the dis- 
 solved carnotite with a mixture of sodic hydrate 
 and carbonate, which throws out iron and^ uranium, 
 and leaves vanadium, in solution. The separa- 
 tion with mercurous nitrate and mercuric oxide 
 (Langmuir), and the extraction of uranium with 
 ammonium nitrate after evaporating the mixture 
 to dry ness with nitric acid are both more widely 
 useful. 
 
 The analysis of a complex ore may often be 
 completed without any separation of uranium and 
 vanadium being made. This is accomplished by 
 determining vanadium volumetrically with ferrous 
 sulphate and permanganate, or colorimetrically 
 with hydrogen peroxide, according to its amount, 
 and making the necessary correction in the weight 
 of the precipitated compound used for the estima- 
 tion of the uranium. The varied uses of devices 
 of this kind cannot be explicitly stated, but it may 
 generally be assumed that, when precipitated with 
 ammonia, the uranium will carry down all the 
 vanadium, and the weighed U 3 O. S will be too 
 
32 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 heavy by the V 2 O 5 equivalent of the amount of 
 vanadium already determined. Also, when ura- 
 nium is precipitated as phosphate in the ordinary 
 manner, any vanadic acid carried down merely 
 replaces its equivalent of phosphoric acid, and the 
 error introduced may be too trifling for considera- 
 tion, although the exact amount of it can be 
 arrived at by determining the vanadium in the 
 ignited uranyl pyrophosphate. 
 
 An accurate separation can be made by pour- 
 ing a faintly acid and heated solution of the two 
 metals into a heated mixture of microcosm ic salt 
 and 5 or 10 c.c. ammonium acetate. The 
 latter solution is kept violently agitated, while the 
 former is added through a funnel with a stem so 
 constricted that only a thin column passes out of 
 it. The precipitate is washed by decantation and 
 weighed as usual ; the combined washings are 
 evaporated to a convenient bulk, and titrated with 
 ferrous sulphate and permanganate. The follow- 
 ing results were obtained : 
 
 V present. 
 
 U present. V found. 
 
 U found. 
 
 0-0503 
 0-06I5 
 
 o - 1 205 
 
 0-I552 
 
 o 1 704 
 
 0-2045 
 
 0-0503 
 
 0*06 1 5 
 
 0' 1 208 
 
 0-1554 
 O-IJOO 
 0-2043 
 
THE SEPARATION OF URANIUM. 
 
 SEPARATION FROM TITANIUM. 
 
 Titanium is precipitated entirely with the 
 uranyl phosphate in a form very closely approxi- 
 mating to TiO 2 . P 2 O 5 . It occurs so sparingly in 
 ores that a colorimetric estimation satisfies most 
 requirements. In larger amounts it can be 
 separated by adding 30 to 50 c.c. acetic acid to 
 the hot solution, and then sufficient ammonium 
 acetate to destroy the free mineral acid. A 
 large excess of ammonium acetate is to be 
 avoided. (See " Separation of Iron.") 
 
 Titanium is completely precipitated by boiling 
 its acid solution with an excess of thiosulphate in 
 the presence of much free acetic acid ; uranium 
 is not at all precipitated under these conditions, 
 providing phosphoric acid is absent, but quantita- 
 tive separations on this principle from synthetic 
 mixtures have not been attempted. When phos- 
 phates are present uranium and titanium must be 
 precipitated together, ignited, fused with sodium 
 carbonate, extracted with water, and the residue 
 (consisting of all the titanium and most of the 
 uranium) dissolved in acid, and separated as 
 above. 
 
34 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 SEPARATION FROM ALUMINIUM. 
 
 Since the introduction of alumino-thermic 
 reductions, experimental metallurgy often requires 
 rapid assays to be made by such means as are 
 not interfered with by aluminium, and it is there- 
 fore to be regretted that one's choice of means of 
 separating this element from uranium are so 
 limited. Of the methods proposed for the separa- 
 tion of iron and uranium only two are applicable 
 to the separation of uranium and aluminium, 
 and these with no great measure of success. 
 
 The separation of aluminium as basic acetate 
 is never very satisfactory unless preponderating 
 amounts of iron are also present. Its separation 
 as hydroxide with ammonium carbonate is less 
 successful than usual when applied to a mixture 
 containing uranium. Uranium passes entirely 
 into solution when a hot and slightly acid mixture 
 of the two metals is poured in a thin stream into 
 an agitated solution of ammonium carbonate, but 
 much of the aluminium also goes into solution, 
 and it cannot with certainty be assumed that all 
 this will again separate even if allowed to stand 
 twelve or fourteen hours in a warm place, and a 
 small amount of aluminium left unprecipitated has 
 an important influence on the estimation of the 
 
THE SEPARATION OF URANIUM. 35 
 
 uranium on account of its comparatively low com- 
 bining weight. Boiling, of course, cannot be 
 resorted to, for fear of precipitating uranium. 
 
 All the aluminium passes into solution when 
 a mixture of the two metals is poured into aqueous 
 caustic soda, but much uranium also goes into 
 solution, and no amount of boiling causes it to 
 separate again. Uranium is precipitated from 
 acetic acid solutions with nitroso-/3-naphthol, 
 and aluminium is not ; but persistently reliable 
 results were not obtained with this reagent, which 
 is to be regretted, because the uranyl naphtholate 
 filters and washes much better than most other 
 precipitated compounds of uranium. 
 
 Generally in the course of analysis aluminium 
 and uranium are obtained together as phosphates. 
 In this form the separation with ammonium carbo- 
 nate is much more successful ; in fact, it is entirely 
 successful if the phosphates are dissolved in nitric 
 acid, most of the acid neutralized, 1 and the clear 
 heated solution poured into the agitated alkaline 
 liquid. If filtered at once a few milligrams of 
 
 1 A pale yellow crystalline precipitate forms on adding am- 
 monia, and not an amorphous cloud such as when solutions of 
 either aluminium or uranium phosphate are neutralized. The 
 former precipitate does not redissolve so quickly in hydrochloric 
 acid as the latter, and more care must therefore be taken over the 
 neutralization. I do not know the composition of the lemon-coloured 
 crystalline precipitate. 
 
36 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 aluminium phosphate remain in solution, and 
 possibly also traces of uranyl phosphate remain 
 in the precipitate. Standing for an hour or two 
 in a warm place minimizes both these errors. 
 
 A modification of this separation, which is 
 sometimes to be preferred, is to pour the dissolved 
 metallic phosphates into an excess of sodium 
 carbonate. The clear or merely opalescent liquid 
 is then heated to boiling, but not boiled, removed 
 from the flame, and ammonium chloride (in 
 amount more than equivalent to the excess of 
 sodium carbonate) added. This solution also, 
 if filtered at once, contains a few milligrams of 
 aluminium phosphate ; but it is an easy matter 
 to dissolve the uranyl pyrophosphate subsequently 
 obtained (and weighed) in nitric acid, pour the 
 solution into ammonium carbonate, collect the 
 precipitate, and weigh it. The following results 
 were obtained after separating from a gram of 
 aluminium : 
 
 Ammon. Carb. .... 
 Sod. Carb. and Am. Chlor. 
 
 U present. 
 
 U found. 
 
 0-2I32 
 O-2I32 
 
 0*2122 
 0-2132 
 
 The behaviour of the ignited pyrophosphate 
 when fused with sodium carbonate is referred to 
 
THE SEPARATION OF URANIUM. 37 
 
 on page 12. It might be imagined that a separa- 
 tion of practical utility could be based on this 
 reaction if supplemented by a colorimetric esti- 
 mation of the small fraction of uranium extracted 
 by digesting with water. Experiment, however, 
 shows that the amount of uranium passing into 
 solution is very much greater when the fused 
 pyrophosphate contains aluminium. But this 
 opportunity may be taken to say that small 
 amounts of uranium, either alone or associated 
 with other metals, may often be conveniently 
 estimated by adding an excess of potassium car- 
 bonate and half a gram or so of sodium peroxide, 
 and then matching the colour formed by running 
 a standard uranyl solution into an equal volume 
 of distilled water in which are dissolved similar 
 amounts of potassium carbonate and sodium per- 
 oxide. A milligram of uranium can be detected 
 in 60 to 100 c.c. of solution by these means, and 
 the indication is more characteristic than that 
 given with potassium ferrocyanide. 
 
IV. 
 
 THE ANALYSIS OF URANIUM ORES 
 AND ALLOYS. 
 
 Pitchblende. Pitchblende is the best-known 
 ore of uranium ; it is an impure U 3 O 8 , containing 
 from 40 to 95 per cent, of that oxide, but not 
 always exactly in the proportion of UO 2 : 2UO 3 . 
 The following elements have been found asso- 
 ciated with it : sulphur, selenium, phosphorus, 
 calcium, magnesium, aluminium, silicon, vana- 
 dium, manganese, arsenic, bismuth, antimony, 
 tin, zinc, lead, iron, cobalt, nickel, copper, and 
 silver. Many of these occur in such small 
 amounts, that their presence is negligible so far 
 as commercial analyses are concerned. Nitrogen 
 and a number of rare earths are also to be found 
 in uraninite from some localities (vide " On the 
 Occurrence of Nitrogen in Uraninite, and on the 
 Composition of Uraninite in General," Hillebrand, 
 U. S. Geological Survey Bulletin, No. 78, and 
 Chemical News, vol. Ixiv., p. 221, etc.). The 
 following outline method of analysis meets most 
 
ANALYSIS OF URANIUM ORES AND ALLOYS. 39 
 
 industrial demands. The particular form in which 
 the results are expressed is a matter of ex- 
 pediency. 
 
 Digest 4 grams of the finely powdered ore 
 with 20 c.c. (1*42) nitric acid, boil down to low 
 bulk, and filter off the siliceous residue. This 
 residue very rarely contains uranium ; besides 
 silica, alumina, and ferric oxide, it may contain 
 small amounts of vanadium, tin, and antimony. 
 A further analysis is made, or not, according to 
 circumstances. 
 
 The soluble portion is evaporated with hydro- 
 chloric acid, diluted, any silica or silver chloride 
 filtered off, and a current of sulphuretted hydrogen 
 passed. The precipitated sulphides of antimony, 
 arsenic, tin, lead, copper, and bismuth, are 
 separated in the usual manner into two groups 
 with sodium sulphide, and the separate determina- 
 tions made as usual. 1 A separate determination 
 of the arsenic may be desirable, as a portion is 
 probably volatilized from the main portion during 
 the evaporation with hydrochloric acid. 
 
 The main filtrate is boiled to expel sulphuretted 
 hydrogen, and nitric acid added to oxidize the 
 
 1 It is hardly feasible to give details of these separate de- 
 terminations, but the general procedure followed by the author is 
 dealt with, in relation to the analysis of white-metal alloys, in " The 
 Analysis of Steelworks Materials" (Longmans, Green & Co.). 
 
40 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 iron. It is then made up to 250 c.c. ; 100 c.c., 
 or some other volume well suited to the supposed 
 amount of the impurities to be determined, is 
 measured into a flask containing a few crystals 
 of ammonium phosphate, then nearly neutralized, 
 and poured into an excess of aqueous sodium 
 carbonate. The mixture is raised to boiling, and 
 at least as much ammonium chloride added as 
 will destroy the free soda. After standing a few 
 hours the precipitated phosphates are filtered off. 
 Uranium is determined in a portion of the filtrate 
 after acidifying and boiling free from CO 2 . The 
 residue is dissolved in sulphuric acid. A portion 
 of this acid solution is reduced with sulphur 
 dioxide, and the iron titrated with permanganate, 
 care being taken to make allowance for any vana- 
 dium which may be present. The vanadium may 
 also be estimated, colorimetrically, on this portion 
 if its amount is small compared with the alumina 
 and ferric oxide. The remaining portion of the 
 sulphuric acid solution is boiled with sodium 
 phosphate and thiosulphate to obtain a precipi- 
 tate from which alumina and titantic oxide may 
 be determined ; any uranium not having passed 
 into the ammonic carbonate solution would be 
 found here. 
 
 To another fraction (100 c.c.) of the main 
 
ANALYSIS OF URANIUM ORES AND ALLOYS. 41 
 
 solution, an excess of microcosmic salt is added, 
 then an excess of ammonium acetate to ensure 
 the complete precipitation of uranium, iron, 
 aluminium, etc., from a strongly acetic acid solu- 
 tion. A fraction of this solution is filtered, most 
 of its free acetic acid neutralized, and the lime 
 precipitated as oxalate, and the magnesia subse- 
 quently as phosphate. There is generally not 
 sufficient manganese in these ores to interfere 
 with this procedure. 
 
 The remaining portion (50 c.c.) of the main 
 filtrate is used for the determination of phosphoric 
 acid via the molybdate precipitation ; or a sepa- 
 rate portion may be prepared by digesting the ore 
 with nitric acid in case no appreciable amount of 
 tin is present. 
 
 Separate determinations may be made of 
 manganese by digesting i gram of the ore with 
 nitric acid, oxidizing the solution with sodium 
 bismuthate, and titrating the permanganate 
 formed ; of vanadium, by fusing i gram with 
 sodium carbonate, extracting with water, and 
 determining colorimetrically with hydrogen per- 
 oxide, or otherwise ; of nickel, cobalt, and zinc, 
 by precipitating uranium, aluminium, iron, etc , as 
 phosphates from strongly acetic acid solutions, 
 and applying the usual processes to the filtrate. 
 
42 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 The sulphur and moisture are determined as in 
 samples of pyrites. 
 
 Carnotite. This ore, which has attained 
 commercial importance, is found chiefly in 
 Western Colorado. It is a canary yellow com- 
 pound associated with a fragile sandstone bearing 
 some resemblance to Roscoelite. The analysis is 
 comparatively easy. 
 
 Digest 3 grams of the ore with nitric acid, 
 and filter. The ignited siliceous residue may be 
 reported as such, or fused with sodium carbonate, 
 evaporated with hydrochloric acid, etc. Uranium 
 is usually entirely absent from the residue, but 
 vanadium (V 2 O 3 ) and barium sulphate are fre- 
 quently present along with the usual constituents 
 of silicates. 
 
 The filtrate is evaporated with hydrochloric 
 acid, the trifling amount of silica collected, and a 
 few drops of sulphuric acid added to precipitate 
 any barium. If no barium is indicated, sul- 
 phuretted hydrogen is passed to separate copper, 
 and, in rare cases, other metals of this group. The 
 filtrate is boiled, oxidized with nitric acid, and 
 made up to 300 c.c. From this point the analysis 
 proceeds on similar lines to that of pitchblende. 
 Vanadium is estimated on a separate portion by 
 titration with ferrous sulphate or otherwise, 
 
ANALYSIS OF URANIUM ORES AND ALLOYS. 43 
 
 Carbon dioxide must also be separately deter- 
 mined. The following analyses are of commercial 
 
 ores :- 
 
 PITCHBLENDE. 
 
 CARNOTITE. 
 
 
 Cornwall. 
 
 Joachim- 
 sthal. 
 
 
 Insoluble. 
 
 Soluble. 
 
 U 3 8 
 
 43 '47 
 
 49'95 
 
 uo s 
 
 
 
 I9-22 
 
 Si0 2 
 
 25'3i 
 
 I8'54 
 
 SiO, 
 
 62-85 
 
 0*20 
 
 Fe 2 3 
 
 0-44 
 
 I-I4 
 
 Fe 2 3 
 
 0-48 
 
 0-50 
 
 A1 2 3 
 
 2-25 
 
 3^5 
 
 A1 2 3 
 
 I -0 9 
 
 0-68 
 
 MnO 
 
 0*20 
 
 O'll 
 
 CaO 
 
 0-17 
 
 1-17 
 
 CaO 
 
 i '34 
 
 2-52 
 
 MgO 
 
 0-18 
 
 0*90 
 
 MgO 
 
 0-25 
 
 0-38 
 
 BaO 
 
 
 
 
 
 V 2 5 
 
 0-25 
 
 0'02 
 
 V 2 5 
 
 O'lO 
 
 2-90 
 
 TiO 2 
 
 traces 
 
 
 
 TiO 2 
 
 o'og 
 
 
 
 ZnO 
 
 
 
 1-09 
 
 P 2 0, 
 
 
 
 traces 
 
 P 2 5 
 
 3-28 
 
 o*33 
 
 S0 3 
 
 
 
 1-03 
 
 S 
 
 8-25 
 
 5-08 
 
 C0 2 
 
 
 
 2-70 
 
 Ag 
 
 0-075 
 
 0*03 
 
 H 2 
 
 
 
 3'95 
 
 Sn 
 
 
 
 
 
 K 2 O " and 
 
 
 
 Sb 
 
 0*62 
 
 
 traces of 
 
 
 
 As 
 
 I '00 
 
 0-44 
 
 other me- 
 
 
 
 Pb 
 
 2'O2 
 
 175 
 
 tals 
 
 
 
 179 
 
 Bi 
 
 0*015 
 
 0-24 
 
 
 
 
 Cu 
 
 1-32 
 
 0-89 
 
 
 
 
 Fe 
 
 7-14 
 
 8-04 
 
 
 
 
 H 2 
 
 1-50 
 
 0-67 
 
 
 
 
 C0 2 
 
 
 
 5-02 
 
 
 
 
 Oxygen 
 
 
 
 
 
 
 combined 
 
 
 
 
 
 
 with Fenot 
 
 
 
 
 
 
 existing as 
 
 
 
 
 
 
 FeS 2 , etc. 
 
 1-27 
 
 o'53 
 
 
 
 
 
 lOO'OO 
 
 1 00 '00 
 
 
 64-96 
 
 35 '04 
 
 Metal and Alloys. Metallic uranium was 
 
44 THE ANALYTICAL CHEMISTRY OF URANIUM. 
 
 prepared originally by reducing the chloride 
 with potassium, and this process, or some modi- 
 fication of it, was the only one available until 
 a few years ago. Moissan prepared "cast 
 uranium " by submitting an intimate mixture 
 of the oxide and sugar charcoal, contained in 
 a coke crucible, to the electric current. He 
 isolated a crystallized carbide (C 3 U 2 ) whose melt- 
 ing point is much higher than that of platinum, 
 and he prepared samples of the metal containing 
 less than i per cent, of impurities. On this latter 
 metal and other samples prepared by the electro- 
 lysis of the double uranium-sodium chloride 
 (UC1 4 . 2NaCl) he determined some of its pro- 
 perties. Ferro-uranium alloys are formed by the 
 last-mentioned process when iron electrodes are 
 used. The metal and some of its alloys have 
 been prepared by various modified forms of the 
 alumino-thermic process : the author, however, 
 found this method to yield poor and very uncer- 
 tain results. 
 
 Pure uranium is a white non-magnetic metal, 
 and can be easily filed ; it does not scratch glass, 
 is easily carbonized, and may be tempered. Its 
 specific gravity is said to be about 187, but the 
 carbonized metal usually met with has a specific 
 gravity of about 12 only. When in fine powder 
 
ANALYSIS OF URANIUM ORES AND ALLOYS. 45 
 
 the metal burns at a comparatively low tempera 
 ture (170 in pure oxygen), and also very readily 
 combines with nitrogen. It tarnishes on exposure 
 to air, and also decomposes water to some extent, 
 particularly if heated. 
 
 Metallic uranium is decomposed by dilute 
 hydrochloric acid, but black flocks of carbide 
 persist until a few drops of nitric acid have been 
 added. With ferro-uranium alloys or uranium 
 steels it is advisable to filter off this black residue, 
 ignite, fuse it with sodium carbonate, dissolve the 
 melt in hydrochloric acid, and add it to the main 
 solution. The simultaneous precipitation of ura- 
 nium and separation of iron is made in the manner 
 already described. Carbon in metallic uranium 
 is determined by simple ignition in a stream of 
 oxygen, the resulting carbon dioxide being col- 
 lected and weighed. The determination of the 
 remaining impurities which affect the value of the 
 metal or alloy for steel-making purposes is made 
 by the usual processes, with which uranium does 
 not interfere. 
 
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