1980-09-25 – MDNR – West Lake Landfill – Source of Contamination in Area 2 is unknown at this time

i1 f^- MEMORANDUM * ^*wt SEP 2 5 1980 SOLID Date: September 25, 1980 To: Robert J. Schreiber. through... View Document

Post

1948-11-01 – AEC – SLAPS – Uranium contamination at Airport Storage Area, St Louis MO

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YTOn•IUM CONTAMINALOTUI~~ ATM IASSIROPUORRI T S’l’ORAGE AREA VL\1\ll sr. •
BY
PAv.T~T.Yo B• KLEVIN
·~~;/ a~C; #~ ~~wJ.(__,
T/,r C’-1””” a/ ~0., ~-/
s Atomic Energy ComOnfifsisc1eon u. • I k: Operations
New or 1 Di vi;:i on
November 1 • 1948
Medica
. ,; _-_·-·c(\_.M,·EfJJ.£NfiAt.,.- ~-~~ _ V.tiY
I
M?TRACT
A study of pollution o£ Cold ‘?later Creek and content of
uranium that may be .found in the earth at the Airport .
Storage Area, st. Louis, Uissouri revealed the followinga
1. Creek water samples were well within the limits
of tole ranee.
2. M.ld samples adjacent to the area ranged in value ·
from nil to 190 times that of normal uranium
content in soil.
H~rever, no final conclusion should be drawn from these
samples.
Ad~itional samples both under normal and adverse weather
conditions need to be taken so that the evaluation o!
hazards presented by erosion and drainage both into the
Creek and adjacent area can be more soundly determined.
‘~ •
Egrpose of Raoo~
During the period z~~rch 23 to March 28, 1948 mud and l’later samples were
taken by Paul B. Klavin in the a raas adjacent to t.lJ.e air:9ort storage area,
Robertson, !o:;issouri. This sampling survey nas planned in order to study
(1} the pollution of Cold ~1ater Creek by materials stored or dun?ed at the
ai rport a rea, and (2) the content of uranium that might have soaked into the
soil.
~thod of _s.t u9z
Seventeen water samples werG collected in 500 cc bottles fr~ the various
drainage ditches and streams alongside and adjacent to the storage area. In
addition, samples were collected from the main stream, cold 7’fater Creek.
Samples of water ware obtained from various hiehway bridges frO!ll its oriein
to its mouth.
Fifty mud samples ”are tal(en in 250 cc bottles at both surface and subsurface
levels 01•-.3″ and .3″ to 7″ raspectively; the latter procu.Nd to indicate
pene·tr ation. Using a two inch di.a.metar pi-pe to obtain a 211 x 3″ cylinder
of mud, the sub~urface and surface mud was sampled throughout tht3 area west
of the property, where the most noticeable drainage from. the storage area
occurs. Thera lVere 20 sampling stations along a north-eouth line follotdng the
wast fence appro:x:i.:nately 25 – 30 feet apart. ‘Ihe remaining staticns were wast
of the fenced area along the drainage ditches and a9pr~ll~tely 100 feet apart.
In addition to these samples four control mud samples were taken at distances
of one and five miles from the area.
Soil and liquid samples were· analyzed by the University of Ro<'~he ster for uranium content. A soil analysis result of o.o signifies no uranitun detect ed. If present, the uranium concentration is less than 0.1 micrograms l;.ranium per gram of soil. The sensitivity of the water analysis is 0.0004 micrograms uranium per cc of water. ~scriotion of TeiTain aqjoining...MQ...E!:OJ29rlY at J:!obertson..a J:j. ss~t1 Just prior to the period of mud and water sampling t here had boen gena r-a.l and frequent rains causi ng sluage and residue to be washed onto the adjoining property wast of the area. The area nearest tha west fence was swampy and boggy with many small drainage ditches emanating .from the area itself. In the central portion of the adjoini..l'lg area there is a swampy stretch running northsouth for 250 feet and east"""'f9st f'or 125 feat. 'l'liElnty to thirty feet south of asphalt cover ed Brawn Road which borders the area on the nortn., there was a pool of l'fater 50 feet in length. Due wast of t his pool thora was a.nother swampy stretch 125 feet in length originating or terminating at the swampy section desc1~bed above. All of the ground west of the Sl'Bmp area leading to Cold Vlater C:reek was firm terr ain. Two IDAi."l ditchew originati.ng near the fence area were avident1 one 25 feet directly south of and parallel to Brown Road and the other, a larger one originates in ~~a residue area and runs due west for 500 fest into the creek. -1- . As previously m3ntioned, the rainy weather conditions prior to the' sa:npling period were unusually severe and caused the appearance t)f many ephe;aeral ditches in the area. Cold ilater Creek was swollen and turbulent along its entire course to the Missouri River. Discussion The results of the mud analysis showed conclusively that s01no3 residue from the area had been washed "estward towards the creek. It should b1~ recognized that the weather conditions at the time the samples W9re taken af~ects the amounts of uranium obtained par sample. 1.he uranium tolerance value has been given by K. z. ~~rgan a:s: 60 micrograms uranium per milliliter of water. All values from the seventeen water samples taken are well within the limits of tolerance, ths highest,.lO micrograms uranium per milliliter of water being 17% of the recommended laval. Fieure 1 shows the fall-off of intensity in Jlg/ml w.i th respect to distance. It can be noted here that although the path or the creek south of the area ~1s not been plotted, the concentration throughout was nil. The figure generally accepted for normal uranium in soil is 4 x 10-6 grams per gram. Of the 50 soil samples analyzed, the values range from nil to 190 tin:es this figure. Figures 2 and 3 show the number of samples takEn at surface and sub-ourface levels and their multiples of normal. Figura 4 contains plots of both surface and sub-ourface soil concentrations west of the fenced area, showing once again, the sharp drop in inte.nsity with distance. Conclusion '!he study revealed the followinit~ 1. The creek vrater samples ware well within the limits of tolel"ance. 2. }.fud samples adjacent to the area ranged in value from nil to 190 times that of normal uranium content in soil. It is felt that a sound conclusion cannot be drawn from the s~9les shown hera because of the unusual conditions that prevailed at the tillB of sampling. Because of the excessive rains, two divergent forces would tend to affect the results. There would be a tendency to a higher result because of tho increased erosion; while the increased quantity of water would tend to dilute 1;be concentration. With comprehensive data the evaluation of hazards presanted by erosion and drainage both into the creek and adjacent area can be more soundly determined. It is thersfore recommended that subsequent soil and liquid samples be taken during essentially dr.y conditions. -2- ------------------- . • '0 t z 3 • ~ ' 1 a O'- 2 l " ~ 6 7 a 9 o 34567891 ~±Tr-: f -:: - ·~ ,: _ + --~-ttt~ -. ~ --- 8 -- • ·. ~ . :!' . .... --~~ ... -.. .• • 1. - : • •. • t . ,;;;. ..: ·, J,.~,·. Figure .3 ,, ...... --- · -"·-~ ·· ___ ...,.. -.~ ....... ._..... _ . ....,._,..... ____ ~ ·-·------·----·-----'"--·--··! , ...... ~ ............... . " ·--· · ···-···.··--·-~ . 'i / -·--·' . ---.. , ·, ., ......... ... -.l Figun 2. ~j."· l.. .t. .· .k i:··":· ... ·- ,· • • • ANAJ,ISE.S Or' Water Samples Taken at Airport Area & Cold ·,rater Creak Robertson, ~ssouri Hlltiples Sample Ur!'niUI!l of pmf. No. Operation Date Description W.crogrami/ml !$vel 1 Airport Area 'J/23/48 Main stream 150 ft. from fence area 4.0 O.O? 2 ,, II " JUnction of stream and Cold ~ter Creek 0.45 o.oos .3 II It II Cold water Creek & Brown Rd . Approx. 250 it. "l from fence 6 . 0 0. 1 ., ... 4 II " II stream near Brown Rd. 10 i't. fran area .3. 5 o.o6 'J 5 II u Stream near Br01!1l Rd. {juncti on with Cold Water Creek) 10.0 0 .17 tt.r:' " I. . 6 II " • 10 ft. from area main stream leading into Cold ~~ Water Creek 7 .0 o.u 7 " " II 100 ft. from area . Stream near Br~tn Rd. 3. 5 o.o6 8 " II It Cold ','l'ater creek at Taylor Rd. Approx. 1 lllile t:: .:. ~., . J down tile creek 0. 015 O. OOOJ 1""' . ~ · 9 n It n Byp&ss 6? - Highl'lay l40 - ~zel'I'IOOd al. o.ooos o.oooo1 t 10 " It 11 Cold uater Creek - t mile N of New Halls Ferry Rd. o.oo10 0.00002 11 II II II Cold Water Creek - Ol d Ferry Ri. 0.0026 0. 00004 l2 II! n II Cold water Creek - Old Jamestown Rd. 0. 0010 . 00002 13 .. n .. Cold water Creek - Junction of Mo. 99 & Highway 67 0. 0020 . 0000.3 14 " II It Cold Water Creek-1m Halls Ferry Rd. & Patterson Rd. o.oo:w . 0000.3 15 " II It Cold water Creek at N• tural Bridge Rd. o.ooos . oooo1 • 16 II " It Cold Water Creek - St. Charles Rd. o.oooo 0 • • 5alnple No. Operation Date l? 18 A.irport. Area J/23/48 " II II aNALYSES OF Water S&mples Taken at Airport Al'aa & Cold Water Creek Robertson, ~s5ouri Description Cold ~t er Creek - ~dland Blvd. M.lltiples Ui~n.1:wn o.i" Pttti • Alicrograms/ml laval o.oooo 0 c:ra'Wfish picked up on area {Ash weight 3.0 grams} 12. )1/gram of ash .. · •r . ..:t I ~ -- ·-- • ANALYSES OF Soil Samples Taken at Airport Area, Robertson, Mo:. l!llti ples Sanple Uranium of nonaal No1 Q.Eeration Date Il!P'th ~ription micrograms tEE,aJn soil Con9_t 1 Airport Area 3/2E/4S Surface l.'ud 6r from S end of area drainage ditch 0 to 311 near railroad o.o 0 2 II II II Mld. .3" to 6tl 6r fran s end of area drainage ditch balOl'l surface near railroad o.o 0 3 11 II Surface mud 201 N of S and of fence 101 W of fence o.o 0 0 to 311 deep 4 !.Ud Jll to 6U 201 N of Send of fence 10' 'IV of fence o.o 0 r. ·.· II It n • deep ,~. · " 5 II II Surface mud .35' N of s end of f ence 101 W of fence o.o 0 ~ : o to 311 ~; . , .. 6 II II " l!l.d .3n to 6n .35 1 N of S end of fence lO' \1 of fence o.o 0 ~:· :"' deep ,. . f ? n 11 Surface mud 60• N from S eoo of fence lO• \'i of fence 3.2 .so 0 t o .311 a q II II MUd 311 to 7u 601 N from B end of fence 10 r 1'l of fence 3.3 .8,3 deep 9 II .. II Surface mud 95' .from S end of Fence 10' ',f of fence 760. 0 to 4" in ditch 190 10 II II II Surface mud 1251 N of SW end of fence 10' W of fence 19. 4.5 0 to 311 ll II II II }Jld 311 to 611 deep 1251 N of ~ end of fence 101 11 of fence 17. 4.3 12 II II II Surface mud 150' N of SW end of fence 10' W of fence l6. 4.0 • 0 to .3" deep • Sample Uranium !Jlltiples o:f no :rmal No. Operation Depth Description micrograms/gram soU Cone. 1;3 Airport Area J/28/48 llud ~~~ to 6" 1501 N of Sli end of .fence 101 Wo! .fenee 17. 4.;3 14 II II II &lrface mud 1801 N of 5W end t:.>£ renee 101 W of
0 to 3″ fence 8.1 2.0
15 n II .. l!ld 3u to 6•- 1801 N of S5. end of fence lOt Wo! o.o 0
fence
16 II II Surface I!Dld 2201 N of SW end of fence 5′ ii of n. 2.8
0 to 3″ fence
17 11 II ” l’!Wi 3″ to 6n 2201 N of SN end of fence 5′ w or o.o 0
beneath surface fence
l8 II ” It lbd 0 to 511 250• N of SW end or fence 101 W of 9 • .3 2.7
deep fence
19 II II Surface mud 10′ N of NW end of fence o.o 0
0 to 4″ deep
..0
20 II It II Surface mud 310′ N of Sif end of fence 101 \’l of o.o 0 I
0 to 411 fence
21 II II Surface md 201 s of Bl’own Rd. 1001 W of fence 12. 3
0 to 311 towards Cold ·,vater Creek
22 1:11 It .. )u to sin deep 100′ W of fenee towards Cold Water 2.1 o.s
Creek 201 S of Brown Rd.
2J II … It 0 to ,311 deep 2001 W of fence towards Cold ·:1ater 1.2 o3
Creek 201 5 of Brown Rd.
24 II II II Ml.d depth 311 2001 W o! fence towards Cold \'{ater o.o 0
to 611 Creek 5′ S ot Brown Rd.
25 II II II Surface I!Dld 275′ :’i o! fence towards Cold Water u. 2.8
0 to .)11 Creek 5′ S of Brown Rd. (Ditch) • 26 •• II It 3″ to 611 deep 275• w of fence towards Cola water
Creek 51 S of Brown Rd. (Ditch)
12. .3
·. – – —· -·- –·
.. – – • MJ.ltiples
$ample Uranium of normal
No . Operation DaUI Depth Desca-iption Mi.crogramB/gram soil cone.
27 Airport Area 3/’)13/413 l.ll.d 0 to Jitt 4501 ll” of fence near Col d Water Creek 5. 0 1. 25
101 from Brown Rd. (Ditch)
;cs II ” ” Surface mud 500′ r f of ~Ff end of fence junction 1. 5 .38
0 to 3 11 deep of ditch and Cold water Creek 10′ N
of Rl.ilroad tra cks
!%
29 l l 11 n 3n to 7 11 deep 500′ \Y of SY: end of fence j unction o.o 0
ot ditch and·. Cold Water Creek 10′ N of Railroad tracks ·J.
30 II It II Surface mud 4001 Vf of Sl'( corner of fence 75′ N 4 – 5 1 .1 :!’
0 to 4″ deep of RR tracks (drainage ditch} : ~~– f:
31 ll II II 411 to 7″ be- 4001 W af S’:l corner of fence 751 N 2.2 .7
neath surface of RR tracks (drainage. ditch) ,.
32 ll II Surface mud 300′ ‘\’:” of S\7 end of fence (drainage 6 .0 1.5 ~ :.
0 to~~
·-·· : ditch) and 591 N of RR t racks . …,
3!11 to 6in 300′ ‘\’f of SW end of fence (drainage 6.
V ‘
33 •• 11 •• .24. I .
deep ditch) 50 1 N of RR tracks
34 II ” • Surface mud 200• W of s’• end oi f ence 751 N of n. 2.7
0 to 3″ 4eep RR tracks (drainage ditch)
35 II ll ” 311 to 6n 200• ‘II oi S’,f end of fence 75′ N of .3·4 .8.5
RR tracks (drainage ditch)
36 n It II 0 to 3″ deep 100′ W of’ SW end a! fence 50′ N o! 50. 12.5
Surface mud RR tracks (s1’lB.Illpy section)
Yl • • Ju to 6!n 1001 W of sn· end of f ence 50• N of ?.9 .2
RR tracks (Sllalllpy section)
38 II II II 0 to 2ttt sur- 1001 7( of srr and of fence 100′ N of 31. s.o
face mud RR tracks (swampy section)
. 39 n It 2~’ to 6~” 100′ w of S1f end of fence 1001 N o! 4. 0 1.0
If deep RR tracks (swampy section)
• MuJ:t.iples
&unple Urani\llll of normal
No. Oper14tion Date Depth Descri;etion :t.:~ crogramsLrz.a.m. soil Cone .
40 Airport ANa 3/2I3/JJ3 0..311 deep sur- 251 W of w fence towards Cold so. 12.5
face !!!.’J.d ~i’il.tar Creak, 200′ H or RR track
(swamp)
41 II 11 II 0…311 deep 201 w of 11 fence towards Cold ·t~ater 65. 16.2
surface mu.d C~ek 1001 1-1 of RR tra.cka (swamp) w: ~-·
42 II It J• to 6- deep 20• W of “f1 fence tor.oards Cold Water ?.1 1.8
Creak 100• N of RR tr&cks (swamp)
43 11 II 11 Surface mud 20• N of SVT end of fence .251 ‘!T of ?! 3.8 .95
0- 2~1 fence towards cold Water Creek
(drainage ditch)
44 II • • 2!11 to stu 201 N of Si’l end of fence 251 vr of Y o.o 0
deep fence t.ONards Cold ‘Nater Creek
(drainage ditch)
45 II 11 0 – 311 deep 110’ s of NW end of fence 251 7f or 38. 9.5
fence towards Cold :rater Creek ··:Sh-‘
Jn to 5~’
– ~
46 II 11 It u o• s of Nlf end of tenoe 251 w of 25. 6.2 ‘ .
deep fence tO”//&.rds Cold !’later Creek
47 ,, It II Surface mud Control Natural Bridge Rli. &. Air- o.o 0
0- .3″ deep port ~. 1 mile fran area
48 • • II 3″-Qn·daep Control Na.turs.l Bridge Rd . P~ Air- o.o 0
port Rd. 1 mile from area
49 11 • tt 9-3” daep sur- Control – 5 miles from Airport o.o 0
face 1111d Area city limits
50 II .. Jn-Ott deep Control – 5 miles fran J..irport o.o 0
Area city l:imits •
.\
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r KHOol cK£MtCAl WOR I
lfo4ALL.PtC ‘lor ·~ -~–··

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Post

1944-11-28 – Manhattan Project – Security Lapses at Mallinckrodt Chemical Works

IN REPLY
REFER TO
,f.1100.00S’. &~J8 ….
This docm~en’ consists Of. •••.~ • ••.p ages(,.;/ ‘.•
No ~ A~ __ I-__ ~ of. ~ _ CGY:·o;::. ::~-::.!,j.e3. __ y.,.~-·~
ARMY SERVICE FORCES
MANHATTAN ENGIN!’:ER DISTRICT
INTELLIGENCE AND SECURITY DIVISION
CHICAGO BRANCH OFFICE
iJNCLASSII=/ED
P. O. Box 6770·A
CHICAGO 80, ILLINOIS EIDM CIP-l
BEGlSTERED MAIL . /rm
28 November 1944 “ill > ill
r< z Q SUBJECT: ~ « Safeguarding Military Information, Mallinckrodt Chern ~ Works, St. Louis, Missouri. ~ TO: The Area Engineer P. O. Box 42, Station F New York, New York « ~ u ill o >.
C)
5H>~”‘ct;;:””””—c-4QI z
ill
Through: Lt. D. S. Teeple, P. O. Box 42, Station F, ~
New York, New York. s- ill .”…
‘«”
1. In accordance with request from your office, special, 8:;
attention was given to the safeguarding of military informatiou·_””-‘—‘-;.-=-:.:.-..:.-:;:….::,
during a recent Security Survey of Subject facility by b~. G. W.
Wheaton of this office.
2. It was learned that onl9 October 1944, the former St~ Louis
Area Engineer sent to the contractor a request that the guards make a
nightly inspection of all desk surfaces for exposed classifiedinformation
end of all files and safes to determine that the;v had been
properly locked. .
3. This proposal was rejected by the contractor on 7 November
1944, as it was not desired to have guards inspeot papers on desks
because most of the people interested in the M.E.D. work also are
engaged in other Mallinckrodt acthities. At the same time a bulletin
was sent to all key personnel on the project that all classified information
must be securely locked up at night.
4. A night inspection was made by Mr. Wheaton with Intelligence
Agent, M. F. Game of the main offices of the project in Building No. 25
and of the office in Plant No.4. It was found that all safes and
filing cabinets were properly locked where locka were provided.
5. However, in Building No. 25, inspection of the contents of
four,. desks which were not locked revealed such secret manuals as:
./
~’ ‘. a. Tube Alloy Process Report
j b. Control Tests for Special Products
l” ” /c. Ether Extraction Studies
~(0 ‘\ .~( . -1-,; d. Ignition Temperature of Green Salt-Magnesium
~ “‘,”<... rb Mixtures and Related Subjects. \~\ ~ . .' ~\~. ...,. \" , ~; ,sr~:r0\~'r-!l. ¢' [ \~C\.\. JI"\S S\FlED .. ~ ~-~ ~-t , ' ~r jOq /'30 EIDM CIP-l 28 November 1944 SUBJECT: Safeguarding Military Information, MallincY..rodt Chemical Works, St. Louis, Missouri. 6. Also, in these desks was found material which was not classified, but which properly should have been, such as: a. Shipping Schedules for Chemioals 306 and 264. b. New Procedures for North and South Extractors o. Control Tests fqr Manufaoturing Tube Alloy . . 7. While the office in Building 25 is visited hourly by a patrolling guard, it is readily adcessible to personnel working nights in the Mallinckrodt Chemical Works; but who have no oonnection with the M.E.D. projeot. 8. In the office of Plant No.4, considerable classified material and muoh that should have been olassified was found on top of desks, in open desks, and in a file oabinet not equipped with a look. This material comprised various operating prooedures used in Plant No. 4 and also Daily Reports and Tally Sheets showing the exact daily production of shippable ingots. 9. This offioe is in the well-guarded Plant No.4, accessible on+Y to cleared employees, but at night it is not regularly oooupied, and personnel not authorized to have classified information would be able to obtain it without any restriotion. 10. A conference was held 21 November i944, attended by Lt. E. M. Velten, Area Engineer; Mr. J. Fistere, Jr. Projeot Direotor; Mr. H. E. Thayer, Assistant Projeot Direotor and Seourity Agent; Dr. Harrington, Manager, Plant No.4; Mr. Game and Mr. Wheaton. . 11. It was learned that the management had felt that the storage of olassified material in locked desks provided satisfactory seourity and that suoh material in Plant No. 4 did not need any speoial seourity because of the guard proteotion. It was also brought out that there had never been any established prooedure for olassifying data on production figures and operation methods unless prepared for mailing or as a formal report or manual. 12. After a thorough discussion, it was agreed that a survey would be made by Mr. Thayer and an assistant, Mr. S. Anonsen, to determine if additional locked file oabinets are needed and every effort will be' made to store olassified information in accordance with . Intelligence Bulletin No. ;. 13. A bulletin will be issued by Mr. Thayer to all personnel advising that any and all notes, reports, letters, production records, drawings. eto. should be properly classified where furnishing a true pioture ;f the daily produotion of various materials, quality beir~ produced and desoriptions of processes and operating procedures. C:[~ ~nk..1 , " EIDM CIP-l SUBJECT: Safeguarding Military Information, Works, st. Louis, Missouri. 28 November 1944 Mallinokrodt Chemioal 14. Mr. Thayer am Mr. Anonsen will regularly review with all personnel affeoted, the proper olasSifioation am storage of material for which they are responsible. 15. It was also agreed to adopt a system whereby a speoifioally designated employee in each offioe will be responsible to see that safes am files are properly locked each night am that all olassified information is removed from desks. 16. It is expected that the management of this projeot will oooperate in every way possible to oorreot the oonditions disoussed at this oonferenoe. 17. The next morning Mr. Thayer made a careful study of comitions in Plant No.4. A locked vault is to be provided adjoining the guardls headqu81-ters on the first floor for all information ofa olassified nature which is no longer regularly used, and that kept in the office is to be stored in seourely looked cabinets. Material will be properly ol~qsified in the future in this office, it was promised. 18. Mr. Game made another night inspection 24 November 1944, am found tangible evidence that improvements are already in progress. In the Projeot Offioe in Building No. 25, no classified material was found in the desks where readily acoessible earlier in the week. However, Mr. Yeager, who has been one <:if the leading offenders was foundto have olassified material in his desk whioh was looked but easily opened. Seourity Agent Thayer gave positive instruotions to Mr. Yeager the next day that he absolutely must make use of the looked filing oabinets provided in this office. 19. In the office in Plant No.4, two filing cabinets were found to have been provided with bars and padlocks. A similar secure looking arrangement had been provided on the right hand drawers of one of the desks in this office. No classified information was found on or in open desks. The production tally sheets are now locked in a filing cabinet at night. 20. The filing cabinet in the Engineering Department where classified drawings are kept is now equipped with a substantial bar am padlock device. . 21. Personnel in the various office sections have already been given seourity talks by Mr. Thayer am he am Mr. Anonsen will continue to check that security regulations are being enforced. -3- ~t:~ i j. j . I,. . r EIDM CIP-1 28 November 1944 SUBJECT: Safeguarding Military Information, Mallinckrodt ChemicaJ. Works, st. Louis, Missouri. 22. The Security Survey covering Subject facility is being forwarded this date to the St. Louis Area Engineervdth an extra copy for Mr. Th~er, who has agreed to follow all of the recomniendations therein, relating to Safeguarding Military Information. 23. It has been quite difficult because of an inadequate description to' locate a reported Mallinckrodt employee who is said to have made the statement to an informant that he worked "in the Uranium Plant", but Intelligence Agent Game will continue to work on this case and when fovxrl, caution the violator against loose talk. '24.' Such instanees of loose talk among 'employees at this project have been rare during the past few months. The security education program at this facility consists of a large number of well-chosen pOsters displ~ed throughout the project areas, and reminders are issued each month on payday on the importance of Safeguarding Military Information. ' 25. Intelligence Agent Game will continue to report everywo weeks on progress being made at this facility. Now that a definite program has been established by the contractor, a material improvement in security conditions ia anticipated. • I. Officer cc: Lt. Col. W. B. Parsons, P. O. Box E, Oak Ridge, Tenn. cc: Mr. M. Frank Game, P. O. Box 36, Bremen Station, St. Louis, Mo.

Post

1967-08-15 – AEC – Historical Review of the Mallinckrodt Airport Cake

— PVILIC II’O• ta NiO
TIWfSPOt(T A T10H
ICII:NCI oUID nCAAOLOGY
REPOSITORY–~~ ….. .._..~RCOLLECTION–_;.,;;.;;~—
BOX
NO. ~~-..:~~if–….-~—FO~
ER ~(JeJT~I?I. J uly 26 , 1973
0)4P371’E#~#stfl?~ Sr.~
Dr. !·lilllic.:m E. ! btt
Director
Division of Envirorlirental Control
Tec.~logy
Department of I:nergy
:·7a.shingta1 D.C. 20543
Dear or. ; iott:
-‘IUL ltriP – l -r-
4114 C1oarU …. “·,…, ·- … (31C)m-12111
IQISM_ …
Da ppa, Wt- CSIJt
01., ….
Enclosed is a copy of a paper pre ,:Jared by an AJ:X:. offi cial
in 1967, entitled “liistori cal r-.eviev1 of t he i·!al linckrodt
r.J.rport Cake . :• T’nis i s t he only v.rri ttcn info:t:.mation r
have been able to find on any Uranium nd.l l tailings left
in St • .WOuis.
}:1
If you should f ind any other infoi111ation on this subject,
I v.ould u?preciate yarr sen.d ing zre a <::q)Y . ..:.:..c.. .:..::» 1 • .P le~e feel 5:-ee to contact ne i f I nay :.>e of f’ l'(the~
ass 1s tance to yoo. r- n
N C!2
JPJ\:jj:
Sincerely, co < m ;i 0 - n -1(..~< -F.' ::0 J0<:1v . . • i-at .• 0 ~islative Assistant THIS WfATION'i:IIY rlt1Nl1:0 ON P'AI'CJII MADII. ¥UTH " t:CVCL&D l'lftlla ... .. HISTORICAL REVIEH · OF THE 1-'.ALLINCKRODT AIRPORT CAKE 1~ - .,. _' .. .. . In discussing the history of t~e airport cake raffinates, it is t necessary to define t hem and this has been attempted by the _ :_ simplified f~owsheet given in Figure 1. Mos t of the pitchblende ·; ·p r ocessed by K2lli::1ckrodt was obtained as a concentrate from the ' Belgian Congo in 1944 and was shipped to St. Louis from the Congo in 55-gall on metal drums. The pitchblende was digested in 56 per cent nitric acid (93-102°C) followed by sulfuric acid to precipitate the lead and radium \llhen the ore had a low sulfate content. The precipitate was removed by a string-di scharge rotary vacuum filter and was usually leached with sodium carbonate to remove · residual uranium. The sulfate cake was stored in a separate location. since the Belgians (African Metals ) maintained ownership of · the radium. These residues are•presently stored at the Lake Ontario Ordnance works at Niagara Falls, New York. Some pitchblende was al so processed at Fernald and a similar cake, still stored in silos at National Lead Company in Cincinnati, is known · as Fernald•s K-65 residue . Barium carbonate s lurry was then added to the supernate to remove the excess sulfate . The barium sulfate cake was removed by a continuous solid-bowl centrifuge, leached with sodium carbonate, and also stored in a separate area. · The supernate was made 1 ~ in nitric acid and the uranium extracted with diethvl Pt~~~- : 7ne uranium was stripped from the ether with dilute; nitric acid. ' In the first extraction colu::m a precipitate for.::~ed 'Which was, on ·· · occasion, ~emoved by a Sperry Fil terpres s . The Sperry Cake wa_s __ · · : found to be a good source of protactinL9m-231 and .~u~)processed ~ ' about 20 tons ( about eighty 55-gallon drums) and obtained approximately ~wo grams of protactinium-231. The supernate from the .Sperry Press and the aqueous uranium tails were de-etherized and tr~at ed with a hydrated lime slurry . The s upe~ a te frcm a continuous rotary vacuum leaf filter was di s charg~d to the river, and the limed fraction becawe the airport cake . The cake, up until 1960, was about 25 feec hig~ . and covered three acres. ··•· . . ..... ; ... ~ Organic I i ! HN03 Strip ! Urani uin Product Figure 1 Pitchblende Conce:ltrate v . ·. HN03 Digestion ~. H2so4 ll • Supernate ~ sa++ t Supernate I (J D iethy I Ether ' b . Aqueous --- ~ Ume ! Aqt·-•·->’)\
!11
!12
{13
/14 ·us
••
74)00{;
32,500
1, ;.oo
8,!00
350
117,050
Ta”ble I
Uranium Conten::
{Tons)
…..
;1.13
48
22
7
.-2 • 192
Dascriptio_!l
Pitchblende Raffincte1
Colorado Raffinate
Ba3 S04 Cake (unleached)
Barium Cake (leached) ·
Miscellaneous Residues
1 Estimated to contain
1,775,000 pounds Cobalt
• 2,085,000 pounds Nickel
1,098,000 pounds Ccpper
The i:”:~ten!: ~f tbe s~q~~-~~–fqr … Sale~~ was. tQ. allow private industry
to recover r.he valuable meta1.s: copper, nickel, and. co bait. -The
original request:”for bid offered the bidder several alternatives.
The purchaser could use the existing site for purposes of conca~
tra~ing and extracting a~y d~sired material or he could remove.
t~e residue from the site for processing or utilization elsewhere.
Th.e materials remaining after the purchaser8 s processing operanons
were over could be–disposed Ol: oythepurchase:::-at:l:n~\·]eldon
Spri-ngsdump s1._t_e_wnether ·or rioE pro.cessing .. was·-aone-ontfie-prE:-sc?nt
site o~ elsewhere. The Weldon. Spring·s–Quarcy~Dump-s1te wss a’ pit: ‘~
located in·St. Charles County on Ydssouri State Highway No. 94
. approximately five miles southwest of the \ve ldon Springs plant ~d ~ ~
approximately 30 rni~es frcrn the ai~port site. The site wa~ssible
by truck f~om Missouri State Route 94 and a spur track lead·
off the existing east way of the Atomic Energy Commission’s plant
track system providing railway access to the dump pi·t.
– 4 –
…..
1
In response to a ~equest in 1960, Mound made a cost estimate
based on a pro1uction rate of 1>000 grams of thorium-230 per year
·~ o\·~!7 a two to five-year period on the assumption the airport cake·
. i~ 3t. ~.ouis would be available. Pre.;urnably it may have been
I POE5ib!~ for Mound to obtain the thorium waste stream from the
1 private contractor hot~ever tha cost: estimate was based on start- :~ ,
‘j
‘ j
. ~
ir.g with unprc~~s~~d airport cake~ Inclu~ing manpower, shippi~g)
material, and arnortiza~ion of .c~piLal costs over a five-year
period, th~ estimated cosc of the thorium-230 was about $300 per
gram. At ~hat time, Mound was also instructed to make a survey
of all uranium mills in the country to determine if other potential
sources of thorium-230·existed ‘from which this amount of production
could be economically rnaint?ined. ?his survey is compiled in
MIJ1 .. l439, ~’Survey of Sources of Ionium, Thorium-230,~’ by P. E.
Figgins and H. W. Kirby •
Mound received word in September 1960 that the St~ Louis Area
Office was recommending that the bid be awarded to Contemporary
Metals; a company having a “portable processing plant.,. The AEC
talked with them about their probable process which was to be
‘:. car:ied oqt on site and it seemed that they were interested pri)
mar~ly in the cobalt and nickel. However, they also would have
!I’ a s~de st:ream. for co!’lc.entrating scandium and expected thorium to
. go 1.nto that stream.
. .
Later in 1960, word was received that it was quite unlikely that
tn~ private cont:rac~ would be awarded since the United States
~~ Geologic·al Survey forbid the clumping of the sludges, processed ·
:1 or not, into the quarries in question because of the high proba;
bjlity of contaminating’the Missouri River shortly above the
intak~s for the. St. Louis City and St. Louis County water supplies.
Due to the many· problems, the St. Louis Area Office was contacted
by_Oak.Ridge Operations and asked to hold up awarding any contract
:o~ airport sludge until the long range requirements for thorium-
230 could be fixed.

.i Ic is not clear exactly what transpired at this point (perhaps
;,·Conternporacy Hetals .bankrupted) since the material was subse-
. quently obtain~d by Co~~~~!l~_al !·~nin_g .. _and 1-A’d.ll~_I}.g _ of- Chicago
…. 5
· .. ..
£or $:26,000. Co~tine~~al borrowed $2~500~000 from Cc~~arcial
D,iscount of Chicago to buy ar.d p::oces-5-t:Ee-reiidu·e-s~–using the
riSidu:3 dS security. Concir.2ntal moved the macarial from the
l., i..,r… port t-.1:1 ~Q.th-=.r_si te in sp.”buroaQ.J1?z_glwoo..Q_. ‘!his mova required
ten dump trucks for five monch3 and co~t Continental $100,000.
they were unabl~ to maintai~ ~h~ loan paym~nts while they were
·. ~oving the materia:, so Caillffic~cia~ foreclosed tha loan • .. …
. fbe Commercial Discount Corp_Q_r_— Organic
HN03 Strip
J

1
~1
Aqt:ecus to
Mound
Adjus~ Addity
I
\~
10 Stage t-~idi-Mixcr
Org~ni~
H~03
<1 ..J>-,.
Strip
~1
Ac.u eous
t
Via
0
ste

~7
Organic
to
Recovery
10 Stage Midi-Mixer
..
..
Lime
Return to Airport·
– HN03
Scrub
— 0 rg~~~. ~ Scrub
.. )
Aqueous Product
~
Centrifuge
·-
. !’
. ‘
… -·-~ ….
A flowsheet for -t-he-·-Femo:v:al.-.of-.o.the.r … than the thorium and uranium
has not be.en developed and th_is. now see&7ls. a reas_onable thing to
do at this poinc:-‘!Ite-n-or-f’i””f·te·en-drums· ·o£ this r.~c:terial wera
processed to develop a flm~sheet for- the recovery of the thoriur.1,
uranium, copper, nickel, cobalt, selenium, and a ~are earth fraction,
it-migh:. be: possible to raduce t.~e ::adioactive contamin£”t.ion
of the final W8Ste raffinates such that they would be no problem
and could be disposed of alrno·s·t anywhere.
The 250 kilograms of thorium-230 contained in these raffinates
are more interesting than ionium per se; cost estimates are already
in existence for irradiation to protactinium-231 and subsequent
irradiation to uranium-232. Mound has twelve thorium-230 slugs
on hand that were irradiated in the }ITR at Idaho Falls in 1960.
It· ·is planned to process these capsules in order to develop a flowsheet
for the production of protactinium-231 •

·.
August: 15,. 1967
– 8 -.
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Post

1967-09-30 – Mallinckrodt – Fuel for the Atomic Age – Report on St Louis-Area Uranium Processing Operations

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. .
•mpletion Report On St. Louis· Arta Uranium Processing Operations, 1942 -1967
~ I
LEGAL NOTICE
This report was prepared as an account of Government
sponsored work. Neither the United States, nor the Commission,
nor any person acting on behalf of the Commission:
A. Makes any warranty or representation, expressed or
implied, with respect to the accuracy, completeness, or usefulness
of the information contained in this report, or that the use of any
information, apparatus, method, or process disclosed in this .report
may not infringe privately owned rights; or
B. Assumes any liabil ities \IIi th respect to the use of,
or for damages resulting from the use of any information, apparatus,
method, or process disclosed in this report.
As used in the above, 11person acting on behalf of the
Commission” includes any employee or contractor of the Commission,
or employee of such contractor, to the extent that such employee
or contractor of the Commission, or employee of such contractor
prepares, diss eminates, or provides access to, any information
pursuant to his employment or contract with the Commission, or his
employment with such contractor.
-II· * * *
This report was prepared by Fleishman-Hillard, Inc.,
St. Louis, Mo . , under Mallinckrodt Chemical Works -Uranium Division
Subcontract 25188-M of July 11, 1966, as modified. The report
was prepared in connection with Mallinckrodt Chemical Works’
performance under Contract No. W-14-108-Eng-8 (Principal Contract),
as modified, with the United States of America acting through the
United States Atomic Energy Commission.
,,,
FUEL FOR THE ATOMIC AGE
Completion Report On St. Louis-Area
Uranium Processing Operations, 1942 – 1967
September 30, 1967
I.e !
TABLE OF CONTENTS
Page
Section I, Fuel for the Atomic Age (General Summar~ . …. 1
Section II, Technological Developments
Part 1, Commercial Reduction and Casting of
Uranium Metal. • • • • • . • • • • • • • • • • • • • • • • • • • • • . • 8
Part 2, Development of the First Commercial
Process for Ether Extraction of
Uranyl Nitrate . . . . . . . . . . • . . . • • • . . • • . . . . . . . . 18
Part 3, Development of the Continuous
Ether-Extraction Process .•••..••••…. •• .• • 25
Part 4, Development of the Tributyl Phosphate-
Hexane Process for Uranium Purification . … 32
Part 5, Development of the Pot Process for
Converting Uranyl Nitrate to Orange
Oxide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . • . . . . . . . • 42
Part 6, Development of the Fluid-Bed
Denitration System .•• ..•• ••• •.•.•• . • •.• •••• 49
Part 7, Development of the First Factory
Process for Producing Brown Oxide …. .• … . 59
Part 8, First Factory Production of Green
Salt in St. Louts . ••…••. •• • … •. .. • ••.•• • 65
Part 9, Development of the Continuous-Process
Stirred-Bed Reactor for the Production
of Green Salt and Brown Oxide .. •• .• ••• ….• 72
PartJD, Advances in Continuous-Process
Production of UF4 – Development of
the Integrated Fluid-Bed System •••••.•••..• 81
Part ll, Development of the Dingot Process
for Producing Uranium Metal .••• .••• .• •• . .• • 96
I
Sect ion II (continued )
Part 12, Development of t he Electrolytic
Reduction Process .••..•.. • • • • • .• • • •..• … 109
Part 13, Miscellaneous Technical Developments •• ••• 114
Section III, Organization & Management
Part 1, Organization and Management •.••• • • ••.•••• • 118
Part 2, Material Accountability ..••..•• • • . • • • • • • . • 132
Part 3, Plant Security •••••••.••. • ••• . . . •.. • •.. • •• 136
Part 4, Heal th and Safety.. . . • . . . . . . . . . . . . . . . . . . . . 144
! · Section N , Producti on and Cost …… .. . . .. … … .. …. 157
!
Section V, Conclusions •..•••. • ••..•. • .. •••.•••..•.. •. . • 164
Bibliography . . . .. .. . . · …. . . . . . . . . .. . … . … .. . . , . . . . • . . 167
I .e
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– 1-
Section I
FUEL FOR THE ATOMIC AGE
An Introduction to the History
of Mallinckrodt Chemical Works • Uranium Production
and Development Activi ties
for the United States Government
11The story of the supply of uranium
is by itself a thrilling one, and
the production of enough pure metallic
uranium to do our task in time was a
technological and industri al miracle. 11
—- Arthur Holly Compton*
j * Arthur Holly Compton, Atomic Quest (New York : Oxford University
1 Press, 1956), p. 90.
-2-
On December 2, 1942, in the early days of vlorld War II,
the atomic age was born: the first self-sustaining, nuclear
chain reaction was achieved in what had been a squash court under
the West Stands of Stagg Field at the University of Chicago . On
that day, ” … man first liberated and controlled the power
within the atom. This event was known only to a few . To those
few it was a turning point in history, the birth of a new era.”*
The historic and dramatic accomplishment on that cold,
winter Wednesday in Chicago was the successful result of the
combined work, talents, and skill s of scientists, engineers,
technicians, and others working on related, super- secret projects
in various parts of the nation.
One of the most important parts of the hush- hush
scientific – industrial complex was the uranium project at the
Mallinckrodt Chemical Works plant in St . Louis, Missouri . Its ·
work was a vital link in the chain of activities which led to the
birth, and subsequent development and advancement of the atomic
age .
This document is a history of the Government’s uranium
operations in the St. Louis area. Officially, it i s €1. “completion
report” describing Mallinckrodt 1 s operat.ions from July l~ 1942,
through June 30, 1967, under Contract No~ W-14-108-ENG.-~ for
the United States of America. To provide perspective, the report
discusses significant event s and activities from Martin Heinrich
Klaproth1s discovery of uranium in 1789 to Ma llinckrodt’s initial
involvement in uranium-processing research in the spring of 1942.
It continues through the termination of the Company’s standby
contract with the AEC in June, 1967 .
Figure I is a chart summarizing the major contributions
of the Mallinckrodt organization to the Government ‘ s uranium
processing and development efforts in the St. Louis area during
the 25-year peri od from July, 1942, through June, 1967.
*Ibid . , p. 139 ·
-3-
TWENTY-FIVE YEARS OF URANIUM PROCESSING AND DEVELOPMENT
MAJOR CONTRIBUTIONS BY MALLINCKRODT CHEMICAL WORKS
* First Commercial Process for Ether Extraction of
Uranyl Nitrate
* First Factory Production of Orange Oxide from Uranyl
Nitrate
* First Factory Process for Producing Brown Oxide
* Early Production of Green Salt
* Early Commercial Reduction and Casting of Uranium
Metal
* First Stirred-Bed Reactor for Continuous-Process
Production of Green Salt and Brown Oxide
* First Commercial Continuous Ether-Extraction
Process
*
-1<· * * * First TBP-Kerosene and TBP-Hexane Processes for Uranium-Ore Refining Numerous· Advances in Uranium Metal Production, Including Slag Liner, Dingot-Extrusion, and Electrolytic Reduction First Successful, Commercial Fluid-Bed Denitration System First Integrated, Continuous-Process Fluid-Bed Uranium Production Adaption of Uranium Processing Equipment to Commercial Production of Purified Dense Theria Continuous Cost Reduction Through Advances in Manufacturing Practices and Scrap Recovery Consistent Fulfillment of AEC Production Objectives Figure I -4- . ~ Objectives Of The Report . e I The objectives which guided the preparation of this report were: (l) (2) (3) (4) (5) To provide a single document describing the major aspects of the technical and administrative history of the Government's uranium processing operations in the St. Louis area. To explain the rationale underlying the technical and administrative developments of the operations. To produce an evaluative instrument for comparing and appraising present and future operations of a similar nature. To provide a general guide for the establishment of similar operations in the future . To organize a one- source reference on the highlights of the first major processing contract to be phased out in line with the Government's evolving requirements. (6) To contribute to the literature in the fields of uranium-production technology, nuclear science, chemistry, and technical and administrative management. The report is \'lri tten in a semi- technical tone to make it meaningful and useful not only to persons with technical backgrounds, but also to those whose orientations are not primarily technical. Summary And Organization Of The Report This report consists of five major sections . This section, Section I, is an introduction and general summary of the entire document. Section II, which comprises the bulk of the report, is a history of the philosophy·behind the major technological developments of the St. Louis-area uranium operations. The emphasis of the material in Section II is on the rationale underlying the developments rather than on detailed descriptions of the developments themselves . The _ detailed descriptions can be found in a variety of other technical reports and documents . I I . -5- Because the uranium effort in the St. Louis area was primarily technical in nature, the history of the operation is, in large part, a technical history. It began in April, 1942, when Dr. Arthur Holly Compton, Dr. Norman Hilberry, and Dr . Frank H. Spedding approached Edward Mall+nckro d~, Jr., to seek his Qompany's assistance in preparing the extremely pure uranium compounds wnich were needed as fuel for an experimental atomic reactor at the University of Chicago. The reactor, if successful, would achieve a self-sustaining nuclear chain reaction. The whole project was of extreme importance to the national security. At the time, the United States had been engaged in World War II for nearly a year, and the nuclear reactor experiment had the potential for making a major contribution to the war effort. A successful nuclear fission reaction, on a proper scale, would release an incredibly enormous amount of energy, and could produce an explosion of immense proportions . The possibility that scientists of the Axis powers might develop a device to achieve such a frightening explosion made imperative a vast effort -- the Manhattan Project -- within the United States to develop such a device first . It was in this tense, wartime environment that Mallinckrodt was asked to produce the key uranium compounds which were needed before fur t her progress could be made. Dr . Compton and his associates at the University of Chicago already had approached several other major chemical producers to ask their assistance, but they all declined -- partly because of other wartime commitments, and partly because of the difficulty and risk involved in the uraniumpurification assignment. To produce the needed uranium fuel, impure uranium concentrates would have to be purified by extraction with ether . Never before had the extraction been achieved on anything but a laboratory scale, and even on that small scale, the explosive and erratic nature of the ether made the operation extremely hazardous, Dr. Compton turned to Mallinckrodt because he was familiar with the Company's outstanding reputation for safely producing highquality, high-purity products, and because he knew that the Company was expert in handling ether. Mallinckrodt accepted the challenging assignment, and within 50 days, the Company accomplished the "remarkabl e achievement" of producing highly purified uranium oxide on a tonnage scale. -6- At that time, the Company's uranium products included, uranium trioxide (U03, or orange oxide), and uranium dioxide (U02 , or brown oxide ) . Later in 1942, Mallinckrodt started production of uranium tetrafluoride (UF4, or green salt). When the first self-sustaining nuclear chain reaction was achieved on December 2, all of the uranium in the pile was in the form of uranium dioxide produced by Mal linckrodt or uranium metal prepared by others from intermediate materials produced by Mallinckrodt . A few months later, in July, 1943, Mallinckrodt started its first metal plant. During the 25 years that it was involved in uranium production, Mallinckrodt made numerous contributions to uraniumprocessing technology . This report discusses most of the Company ' s major contributions including the development of the first commercial process for ether extraction of uranyl nitrate; the first continuous ether-extraction process; the tributyl phosphate-hexane process for uranium purification; the pot process for converting uranyl nitrate to orange oxide; the fluid-bed denitration system for producing U03; the first factory process for producing brown oxide; improved methods for batch- type, factory production of green salt; the continuous-process, stirred-bed reactor for producing green sal t and brown oxide; advances in conti nuous- process production of green salt by means of the Mallinckrodt integrated fluid-bed system; improved methods for casting and reducing uranium metal; and the dingot and electrolytic reduction processes for producing uranium metal . Section III is a history of the administrative development of the St. Louis-area uranium operations beginning with the initial efforts in 1942 in Mallinckrodt 's building 25-2 research laboratory and continuing through the final act ivities at the AEC 's Weldon Spring facility in 1966. The subjects discussed in Section III include organization and management, Mallinckrodt ' s experience and qualifications, contractual arrangements, physical f acilities and plant services, material accountability, plant security, and health and safety . Section IV deals with production and costs. In addition to discussing cost accounting, the section provides an interpretive narrative concerning Mallinckrodt- AEC negotiations, and other pertinent subjects related to production and costs. Section V is a brief statement summarizing the conclusions of authorities concerning the significance of the work accomplished since 1942 by the Government's St. Louis-area uranium operations . .e .e -7- For almost a quarter of a century, Mallinckrodt successfully carried out its uranium-processing contracts with the Government, The Company, always surpassing its commitments under the requirements of the contracts, continually worked to lower costs, increase production and improve quality. In April, 1966, when the AEC announced its plans to terminate its St. Louis-area uranium production activities, Dr. Glenn T. Seaberg, Chairman of the Commission, praised Mallinckrodt for its excellent performance in the Government's atomic energy program. He called attention to the Company 's outstanding record of accomplishment for production operations and related process improvement and development programs. Dr. Seaberg said that Mallinckrodt 11can be justly proud of the important role it has played in the advancement of Re aceful uses of atomic energy and in our nation ' s defense efforts . 1 # '•. •,, o 0 fo •, • ,:.,• ,''••• .. : ..... • ' • ~ t .. • .... • . ... • ..... • ~ . .. .: ," , .·. ':', :. . ' , ¥ ••• • ' •• ·1 • •• ' • ~ :· ....: ',. ..; :~·:·:_(~:;. .: <;;.: ..: >~’- />_::::_ .> ..> . .: .. ,; . ·.· ‘·. ..
.. , .. ..
~-
…… Section II .. . ..
f:·j;::t~·: :· ·:·:· · … :::, ·>\_·. =···-·· .. .-‘Tec.ruiological Develo~~ents
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‘~.r!~.~-:;:~;:~~;_~~~–::·_ ::~ _-_;_~~~::_~_,:_~_::·_:~:~>~;-~-~-~-·::~-·_ ·_· : …. \~. …f .~._-_<_- -·._---)_::::-.......: _-;.:·:;·...: j:~-·-=: <<.· -~~::<:-:~ ...·. ·:. . ,.- -............. ~~::·.,:·:.:.~ ........ ·' .· ... ~~ · ... --~ - :-_.:,- ··.::\ rr:. .. .... .: : ·:. ,. ...: . . .·. -:·. :.' ,' :r ·:: '·?· '· .... . ... , • ·• .. :. ·-::-:-·.· .. ,'j: . . .... ' :: . :.:.·_ ·: . .:::: ·:· ~-·· ··: ... : : :-· . .. .·· . ... . ...·..· . . . .. · .· .' .. .... .. .. . .. , .-:,_: · • . . ; • ..;': ~,: •. :· .... - •. •• -.• • a.i ; . ; •. ;-::. :.; .: .. : : ·: .:.:. • .. •.• ,-. • ., tl •• •••• : • • : • • '··\ • • • •• •• · :. ~;. - ...: _ :: :. -::-::--·;::_ <·;' ::· (:~?:~·i.-;':. ':_,.·; .· .-: ·:·-.· ;,:·~-' ·... -->~-·. ._· .:·_. .1
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..· …
··-
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·.···.
~~~*~~~~~~~~~~~~~~~~~~~~~~~~~~~~J~~~~~~~~*;~2~·;·~~~ ~~t~~~~~:~J~ … ‘7i … , … 0 •••• • ••• ,. -·.
• 0 0 0 0 ,o, :.o: . t· .. .·. .. · ·.. . . .. . , ….
~~~~mif:r~i~·~~m:i~~~t-J.!~~;~·.:. :-:,:0··=-.· ::{·.- :;_;·:_·:.:;~~:i:/:::_~;;.-:~ ;-~,- ~: -….
. · .~:~ ·!·.:~.’-· -~-:~:·:.~.~-.. ~·/. ‘:·: -~ ;’ “.\
..,.,.-,;J~.~::·,:.y::, 93, 172, 186, 190, 192, 198, 199, 201, 211, 222 ,
223, 224, 225 .
Additional references may be found in some of the sources
indicated above.
#
– 25-
Section II
Part 3
DEVELOPMENT OF THE CONTINUOUS ETHER-EXTRACTION PROCESS
· In 1945-46, Mallinckrodt Chemical vlorks developed a
continuous ether-extraction process for purifying uranium, and
designed and constructed a large, tonnage-scale plant using the
process. With continuing improvements, the proces~ remained the
standard one at Mallinckrodt’s St . Louis operation until 1957
when tributyl-phosphate-hexane was introduced to replace ether.
Background
The original batch ether- extraction process, developed
on a crash basis, had several disadvantages. (The batch method
is discussed in detail in Section II, Part 2 . ) Chief among the
disadvantages were high operating costs and low percentages of
uranium recoveries . Further, removal of certain contaminants
from the uranium was insufficient, and the method required
relatively pure concentrates, which made extensive prior processing
of the starting materials necessary .
The New York Operations Office of the Manhattan District
initiated activity to explore the possibility of overcoming these
disadvantages. The office assigned to Yale University the task
of investigating the possiblities of a continuous ether- extraction
technique that would use feed solutions prepared directly from
pitchblende by nitric acid digestion .
The Yale work indicated that the approach might be
feasible, if a number of complicated inherent problems could be
solved.
Initial Development Work At Mallinckrodt
In the spring of 1945, as the Yale studies were being
completed, Mallinckrodt began research to develop a final, continuous,
counter- current ether-extraction process. Work was aimed at finding
a method-which would use feed solutions prepared directly from
pitchblende ores, or crude concentrates containing 30-80 per cent
black oxide.
I i .
– 26-
Mallinckrodt had to solve several complex problems,
some of which were revealed in the work at Yale. The major hurdles
were to:
– develop satisfactory methods to prepare
suitable feed solutions . ·
– cut down on impurity (especially molybdenum)
carry- through during extraction.
– ge.t more complete recovery of uranium.
‘rhe total job was two-fold: ( 1) development of workable
methods for preparing suitable feed solutions; and (2) research,
development, and design of the continuous extraction process and
equipment.
Preparation Of Suitable Feed Solutions
Mallinckrodt worked on developing two methods for
preparing feed solutions — one with pitchblende (containing
radium) as t he starting material, and one using radium-free
concentrates.
The method that Mallinckrodt developed for processing
pitchblende involved several steps . First, the original material
was ground, and then it was digested with nitric acid . The
resulting solution, however, contained -radium and sulfate , both
of which presented additional problems .
The radium posed a problem both because of its inherent
radioactivity hazards, and because of its high value . The sulfate
if not removed from the solution — would cause precipitation and
mechanical difficulties during extraction .
Mallinckrodt found techniques to overcome these problems .
The excess sulfate in the digestion batch was removed by precipitating
the sulfate with barium carbonate which also coprecipitated
the r.adium as sulfate . The precipitates were removed
by centrifuge techniques, leaving a feed solution with little
barium or sulfate.
Mallinckrodt’s preparation of feed solution using chemical
concentrates free of radium or sulfides and containing only
relatively small amounts of sulfate or calcium, involved simply the
digestion of the concentrates with nitric acid. The resulting
slurry, after adju~tment of free nitric acid and uranium content,
was used directly as the extraction feed .
-27-
One obstacle remained in the preparation of the extraction
feed . It was incomplete uranium dissolution. To dissolve the
uranium completely required an excess of nitric acid. During the
extraction process, the ether stripped the aqueous feed of acid
and this caused precipitation to occur . The prec ipitation, in turn,
caused sludging and emulsion which interfered with proper operation
of the extraction equipment. Mallinckrodt 1s solution to the
problem was to add a controlled concentration of nitric acid to the
ether to prevent the stripping.
Pilot Plant Development Of The Continuous Ether-Extraction Process
In addition to solving the problems associated with
developing feed-preparation processes, Mallinckrodt also had to
solve major problems in developing the extraction process itself.
In the spring of 1945, a pilot plant was built as an
annex to the batch ether-extraction plant then in use. The pilot
plant was used to carry out the extensive experimental work leading
to development of a practical, continuous, counter-current , dualcycle
ether-extraction process — one that could be translated into
a plant system.
In terms of the physical chemistry invo l ved, the continuous
process that Mallinckrodt developed was basically identical
to the batch process. An aqueous uranyl-nitrate feed solution is
dissolved in diethyl ether . Then the ether and water layers that
form are separated, and the purified uranyl nitrate is recovered
by further treatment of the e t her solution.
The continuous process developed by Mallinckrodt had two
cycles: (1) acid extraction, and (2) neutral extraction . The
process is illustrated in Figure II-3.1
Acid Extraction
The first stage of.the acid cycl e was the extraction
column, a tube packed with small cylindrical sections of ceramic
pipe to promote intimate mixing of the aqueous feed and the ether
phases. The ether was the continuous phase and was introduced into
the column at the bottom. It flowed counter-current to the aqueous
feed which moved by gravity from the top of the column . After
·passing through the extracting column, the uranium-enriched ether
phase overflowed from the top and was carried by pipe to the
bottom of a wash column.
The ether solution carried with it traces of impurities,
some of which were dissolved, and some of which were mechanically
entrained. (Part of the molybdenum, because it is soluble in ether,
was one of the impurities that was carried through.)
hffi noto
Solvbft ~lrott•
N.O. IIqvor
to Acid htJo<~on F.H Acfl"tlloont -28- WothWotor RoH'nott Coke Rhlolt to Acld$owor Produd Figure II-3 .1 THE FIRST COMMERCIAL CONTINUOUS ETHER-EXTRACTION SYSTEM was developed by Mallinckrodt as a dual-cycle process. -29- After it left the extraction column, the uranium-rich solvent stream was then passed through the wash column where small amounts of water were used to remove some of the impurities in the solution. · Re-extraction was the final step in the acid-extraction cycle. Large amounts of water were introduced into the top of the re-extraction column. The aqueous phase, f lowing by gravity from the top of the column, mixed with the uranium-rich solvent \'thich flowed counter- current to the water from the bottom of

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