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Decomposition of Dithionates Dissertation

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Decomposition of Dithionates Dissertation DECOMPOSITION OF DITHIONATE S DISSE RTATI ON PRESEN TE D IN PA RTIAL F%LFI L LM EN T O F TH E REQ %IREM ENTS FO R THE D EG REE O F DO C TO R O F PHI LO SO PH Y IN THE G RA D%A TE S C H O O L O F THE O HIO STATE %N I%ERSITY BY JACOB CORNOG 1921 TABLE O F C ONTE NTS R eview of th e Lit er atur e P ertin ent t o th e Form ation and f t t po sition o Di hiona es . Aim s of th e Pr es ent Work on of B ar i um Dithionate a x e e t al of V riou s Dithionates (E p rim n . ) G en eral C on sider ation s an d Proc edur e T he D ecompo s ition of Barium Dithion at e of Some Other Dithionat es th e Lit eratur e P LYT H I O A T E I . T H E O N S H Dithionic acid , 2 8 2 0 6 , the first ember of this remarkable 1 - group of acids , was discovered in 9 by Welter and Gay Lus 1 5“ sacl H 1 842 Lan lo i s z ; trithionic acid , 2 S 3 0 6 , in , by g ; tetrathionic H 1 843 G elis 3 a acid , 2 8 4 0 6 , in , by Fordos and ; pent thionic acid , H 8 0 1 845 Wacken roder“ hexathi 2 5 6 , in , by ; finally potassium K 1 88 5 onate , Q S 6 , was discovered in 8 by D ebu s as a part of ’ roder his classic investigation of Wacken s solution . Dithionic acid was originally called hyp osulfu ri c acid (u n ters chw efelsau er in the German ) . The present nomenclature was suggested by ' 6 Fordos and Greli s in 1 847 to simplify the naming O f th e i n creas ing number of polythionic acids which were being discovered lfu ri oc about that time . However the name hyp osu c persists i o ll cas na y as late as 1 880. The Obviously outstanding feature of these acids is the piling ” up of sulfur atoms in the molecule , increasing in number one atom at a time , from dithionic acid with two to potassium hexa to thionate with six sulfur a ms to the molecule . This is a p rom ising field for investigation of valence and molecular structure . Indeed the molecular structure of the p olythi on ates has already f been the aim O much investigation , but apparently , thus far, results are more speculative than real . Without attempting a complete discussion of the results already attained in this field , O the following facts and bservations are mentioned . 5 ol hi on Debus experimentally found that all the p yt ates , save dithionate , are intermediate products between hydrogen sulfide and sulfur dioxide , on the one hand , and free sulfur and water o n the other , as represented by the equation 2 The sulfur in the sulfur dioxide represents a higher state of oxidation than does the sulfur in any of the polythi on ates save t O the dithiona e . S apparently the W hole series of p olythionates occurring between the first and last products of the above equa “ tion represents a running down proc ess in the degree of oxida tion of the sulfur . This opinion is in harmony with the findings 7 of Thomsen in the matter of heats of formation . He found for 5 kOle er 1 ol thi onates o the ew s i es 9 3p y , that the heats of formati n vary uniformly% and inversely as the number of sulfur atoms in e c o c s Of th respe tive m le ule . From the decreasing heats forma tion with increasing number of sulfur atoms in the molecule it would seem that there is an upp er limit to the number of sulfur I n atoms that may occur a single molecule , and further that the processes of formation and decomposition are not spontaneously reversible . A further characteristic action of the p olythi on ates occurs on their spontaneous decomposition in water solution under the influ ence of heat . Although in none of them is the sulfur found ' lf in a state of oxidation corresponding to that of su ates , yet all of them on spontaneous decomposition in water solution yield o n sulfates as e of the chief products , along with sulfur dioxide ol th i and in siome cases sulfur . This phenomenon in which a p y onate breaks down into products representing b oth a higher and a lower state of oxidation of the s ulfur th an is found in the “ parent substance is alluded to in the present work as autoxi da ” on e tion . Such in brief, in the opinion of the author, are or two o f the more salient aspects of the general subj ect of p olythi ol thi on ates on ates . Since the formation of one or more of the p y is a very frequent factor in actions involving sulfur dioxide and ’ in %iew of the wide importance of sulfur dioxide , it was thought desirable on the part of this l aboratory to attempt a series O f studies of this very interesting and important family of com pounds in the hope of amplifying present knowledge of the sub j ect and p erhaps ultimately formulating a rational theory of f mol ecular structure . In pursuit O this aim the following studies have been completed . l Z The Action of Sulfurous Acid on the S u fides of Iron , inc , and Manganese . C Henderson and Weiser . Journal of the American hemical 5 2 39 . Society . 3 , ’ Preparation and D ecomposition of Some Thiosulfates . Henderson and Hummel . (In Preparation . ) a Preparation and Decomposition of Tetrathion tes . Henderson and Scott . (In Preparation . ) The present work contemplates a study of the dithionates al ong lines indicated in the title . It is hoped that other papers will be forthcoming . 6 II I O F T H E LI T T TI T T O T H E . A REV EW E RA U RE PE R NE N F ORMA TI ON A N D D E C O M PO SI TI ON O F D I T H I ONA T E S . A survey of the literature shows that the preparation , analysis , crystallography , and determination of chemical and physical properties have been rather thoroughly though by no means exhaustively studied. Salts of nearly all the common and many of the rare metals have been prepared . Many double salts e O . are known though , singularly , no acid salts have be n bserved i d In the resume of the literature which follows , there are nclu ed , as being pertinent to the present work , only those citations which bear on the formation or decomposition of dithionates . An ex tensive bibliography covering the entire field of dithionates is to be found in the files o f the C hemistry Department of Ohio State bibli University . The reason for this exclusion is that the ography is large and much of it without significance in the - present work . Reference works such as Gmelin Kraut or ’ “ ” ’ “ ” Abegg s Handbuch or Hoffman s Lexikon con tain rather complete records of papers published on dithio nic acid and its various salts . The partly accidental discovery of dithionic acid was recorded 1 by Welter and Gay - Lussac as occurring in the following man ner . M . Welter , a manufacturer of bleach , in attempting to recover the manganese dioxide that h ad been used in making chlorine, treated the spent material with sulfur dioxide . As a “ ” result he Obtained a neutral bi sulfite which he b elieved to be a at the b se of manganese dioxide . At this point Welter con s ult - ed Gay Lussac , with the ultimate result that dithionic acid n and the manganese , barium , calcium , stro tium , and potassium ‘ salts were prepared and described . The mode of preparation , more fully discussed later , was by the passage of a stream of sulfur dioxide through a water suspension of manganese dioxide , whereby manganese dithionate , along with manganes e sulfat e , o was formed . Barium dithi nate was prepared by doubl e de composition between barium hydroxide and manganese dithi n i onate . Dithio ic acid was prepared by treating barium dith onate with an equivalent of sulfuric acid . After removal Of the resulting barium sulfate by filtration , the remaining Water s olu tion of dithionic acid was concentrated by evaporation under re duced pressure to a density of Attempts at further con centration resulted in the decomposition of dithionic acid into sulfuric acid and sulfu r dioxide . 8 In 1 82 6, H eeren published the results of a rather ext ensive work on dithionates . He found that high yields of manganese dithionate were promoted by the fineness of the m anganese di ox ide used in the suspension , the purity of the manganese dioxide used , and b y th e maintenance of a low temperature during the time in which the action occurred . Heeren prepared some i twenty salts , giving much attent on to crystalline structure . He Observed that dithionic acid an d many of its salts in water solu tion spontaneously decompose into sulfur dioxide and the cor responding sulfate . Jacquelain 9 learn ed that a water solution of sulfur dioxide in a tightly stoppered bottle after standing two years at room temperature contained sulfurous , sulfuric , and dithionic acids .
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