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Studies in the Application of Extraction Methods to Analytical Chemistry. Jack Kenneth Carlton Louisiana State University and Agricultural & Mechanical College

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Studies in the Application of Extraction Methods to Analytical Chemistry. Jack Kenneth Carlton Louisiana State University and Agricultural & Mechanical College Louisiana State University LSU Digital Commons LSU Historical Dissertations and Theses Graduate School 1950 Studies in the Application of Extraction Methods to Analytical Chemistry. Jack Kenneth Carlton Louisiana State University and Agricultural & Mechanical College Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_disstheses Part of the Chemistry Commons Recommended Citation Carlton, Jack Kenneth, "Studies in the Application of Extraction Methods to Analytical Chemistry." (1950). LSU Historical Dissertations and Theses. 7974. https://digitalcommons.lsu.edu/gradschool_disstheses/7974 This Dissertation is brought to you for free and open access by the Graduate School at LSU Digital Commons. It has been accepted for inclusion in LSU Historical Dissertations and Theses by an authorized administrator of LSU Digital Commons. For more information, please contact [email protected]. stu d ie s on the AmxoAixcnf o? Bxxtwmas mmom to «m O A I- 0imi.3TRY A Dissertation Submitted to the Grad.us.te Faculty o f the Louisiana State University and Agricultural and I'eohanieal College in partial fulfillment of the requirements for the degree of Doctor of Philosophy in The Department of Chemistry by Jack Kenneth Carlton B.3,# Centenary College, I9^2 !i*%, Louisiana State University, 1949 June, 1951 UMI Number: DP69352 All rights reserved INFORMATION TO ALL USERS The quality of this reproduction is dependent upon the quality of the copy submitted. In the unlikely event that the author did not send a complete manuscript and there are missing pages, these will be noted. Also, if material had to be removed, a note will indicate the deletion. UMI' Dissertation Publishing UMI DP69352 Published by ProQuest LLC (2015). Copyright in the Dissertation held by the Author. Microform Edition © ProQuest LLC. All rights reserved. This work is protected against unauthorized copying under Title 17, United States Code ProQuestQue ProQuest LLC. 789 East Eisenhower Parkway P.O. Box 1346 Ann Arbor, Ml 48106- 1346 MANUSCRIPT THESES Unpublished theses submitted for the master^ and doctor*s degrees and deposited in the Louisiana State University Library are available for inspection* Use of any thesis is limited by the rights of the author* Bibliographical references may be noted, but passages may not be copied unless the author has given permission. Credit must be given in subsequent written or published work* A library which borrows this thesis for use by its clientele is expected to make sure that the borrower is aware of the above restrictions. LOUISIAMl STATE UNIVERSITY LIBRARY AOimowL^Dam’W 13*o author wishes to express his sincere appreciation to Hr* Philip W. West for his advice and assistance as director of this research* Ho is very grateful to Or. J* L* !£., Erickson, Dr* Max Goodrich and Dr-. Gunther Siohorn for th eir helpful suggestions in the prepar­ ation of this manuscript* So wishes to acknowledge the financial Sid provided by the Office of Naval Research. Ho also wishes to acknowledge the encouragement of his w ife, Mary 3&len9 to whom he la especially grateful for typing the dissert- ation* He would Ilk© to take this opportunity to express his deepest appreciation to hia mother, Mrs* J* K. Oarlton, for her help and inspiration. table of ©ohtmps CHAPTER PAOS X * Introduction X II* An Experimental Survey of the Extractiono f Metallic Complexes with Organic Solvents 7 Experimental 8 Discussion of Results and Conclusions 12 Bibliography 26 XIX, The Extraction of head Iodide with Methyl Isopropyl Ketone ^2 IV, Specific Spot Test for Gold IMploying Par&roa&ni lino Hydrochloride y*> V, Extraction Pi pot for Spot Teat Analysis *>4 VI, Summary ?5 V II, V ita ?6 i l l U3T OF TABLES $A8&E PACE X. Solvents Uaed in the Extraction itudy 15 IX* Conditioning Agents Used in the Extraction Study 16 XXX. Metal Ions Included in the Extraction Study 11 IV. Extractions Bnploying Potassium Iodide as Conditioning Agent V. Extractions Sftploying Assnonium Thlooyanate ae Conditioning Agent m vx. Extractions HJaploying Hydrochloric Acid as Conditioning Agent 23 VII. Extractions Employing pyridine as Condition­ in g Agent 25 iv ABSTRACT? A Bystem&tio investigation has boon mads of the extraction, of metal­ l i c s a lts and complex®© by organic solvents* The conditioning agents employed in this survey included athylonedi a nine, ©thylcnodiaminet©tra&c©tia s o ld , rcanr&tol, hydrochloric acid, potassium iodid©, ammonium thiecyamt®, p y rid in s, perchloric acid, a c etic acid and malonio acid* Th© solvents used were n-butyl chloride, petroleum ether, benaene, n~arnyl alcohol, chloro­ form, methyl isopropylkotano, isopropyl ether, butyraldehyd©, carbon tetra­ c h lo rid e and e th y l ao etate* .Methyl iso p ro p y l koton© and butyr&ldehyd© were found to be vory good solvents for the extraction of metallic complexes. Only those solvents used which contained oxygen were found to extract the complexes included in this study* Several extract!one war© discovered which hold promise for application in qualitative and quantitative analysis* The extraction of load iodide with methyl isopropyl fcoton© has boon thoroughly investigated as a part of those studio©* It has boon found that when lead solutions are treated with a large excess of potassium iodide and adjusted to the proper acidity, lead iodide can bo extracted with methyl isopropyl ketone * The extraction performed in this manner was 91% complete in a single pace* Interferences wore kept at a minimum through the use of a preliminary extraction which was applied after treat­ ing the aqueous solution with ammonium tin.ocyanato and hydrochloric acid. Hie perarosanilino hydrochloride teat for gold was rendered specific for that metal by extracting an acidic aqueous solution of auric chloride with ethyl acetate* In this manner, gold was separated from the platinum metals, a group which constituted tho principal intorfaranc© in the v detection of gold* After the separation of phases the organ!o layer was evaporated* taken up with a few drops of water and applied to the reagent on Spot test paper* The teat was found to be sensitive to [3 ge^maa of gold* A device was needed for the rapid extr&otlon of small volumes of aqueous solutions with only a few drops of organic solvent. An extraction pi pet was designed and prepared and hao carved quit© well in this capacity. nrrRODUOTXon The use o f e x tra c t!o n techniques as a moans of e ffe c tin g a n a ly tic a l separations has for many years provided the chemist with a very useful tool, and especially in recent years have these techniques become general­ ly popular* The increased interest in this field can be attributed in part to the appearance of a considerable number of extraction devices, suchm the countercurrent extractors discussed annually In the review articles o f O rsig (6 , 7 , 8 ) f and the development of numerous colorimetric proced­ ures based on the extraction of organic-metallic complexes15 (, 35# 24, 27, 52)* The extraction of inorganic complexes also holds many interest­ ing possibilities, and the applications of those extractions to analytical separations, as well as to colorimetric procedures, are to be found throughout the literature. It is with the extraction of inorganic complexes that this investigation is primarily concerned. Before embarking upon a discussion of the experimental work and the results of this investigation It night be well to discuss the various classes of extractions and tho uses to which they have been put* Generally, extractions can be classified according to the follow ing categories* liquid-liquid, liquid-solid, 11quid -gas and s o lid -gas* Be­ cause this study was Gonflnod to liq u id -11quid systems only brief mention w ill be mado of tho other claosiflcntions. Probably the most familiar type of liquid-liquid extraction being employed In analytical chemistry is tin t in whioh a particular component of an aqueous mixture is extracted into an organic solvent with tho form­ ation of a highly colored organic phase which la then readily adapted to (« (2) ft photometric analysis. In auoh ft iaann®r cobalt can bo rioter mined, after treating I t with a.mmonium thiooyanata and extracting it with arsyl alcohol (18, 19, 38)* the blu© color of the thlooyanatc complex is sufficiently intense to provide an excellent means of do to raining cobalt colorimetric** ally. Similarly, iron can be extracted as the thiooyanato complex by a mixture of amyl alcohol and ethyl ether55 (> 55) I th e blood red co lo r of the organic phase ie then measured photometrically after the separation o f phases, The tMooy&nate o f molybdenum can be e x tra c te d by normal butyl acetate with the formation of& redd!sh-brovm color* A colorimetric do* torrid.nation of molybdenum based on this extraction has boon reported by James (15)* Oolorimotrio procedures have been developed for the dotorn&n- ation of bismuth, both as the thioeyanato complex5 ^)( and as the iodide complex (12), In the former procedure amyl alcohol was employed as solvent, and in the latter a 5*1 mixture of amyl alcohol and ethyl acetatew m used. One of the more outstanding examples of the use of extraction techniques in colorimetric procedures is the determination of chromium by extract* ing the blue per chromic acid and Treasuring the intensity of the blue extract. Amyl acetate has been used in a procedure reported by Bishop and Dwyer (1)• There are two principal advantages of employing an extraction procedure in colorimetric analyses. First, in many oases tho desired component
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