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The following month, the Manhattan District's headquarters moved to Oak Ridge, but the Materials Section and its successors remained in New York until 1954.{{sfn|Jones|1985|p=308}}{{sfn|Harris|1962|p=30}} Nichols, who succeeded Marshall as district engineer on 13 August 1943,{{sfn|Nichols|1987|p=101}} felt that this was a better ___location for it, as it was close to the ports of entry and warehouses for the ores and the headquarters of several of the firms supplying feed materials. He reorganised the section as the Madison Square Area; engineer areas are normally named after their ___location, and the office was located near [[Madison Square]].{{sfn|Jones|1985|p=308}}
As area engineer, Ruhoff was responsible for nearly four hundred personnel by 1944, of whom three-quarters were in New York. There were two field offices that were responsible for procurement: Murray Hill in New York and Colorado in [[Grand Junction, Colorado]], and five responsible for feed materials processing: Iowa (in [[Ames, Iowa]]), [[St. Louis]],<ref name=":0" /> [[Wilmington, Delaware|Wilmington]],<ref name=":1" /> [[Beverly, Massachusetts|Beverly]]<ref name=":2" /> and [[Tonawanda, New York|Tonawanda]].{{sfn|Jones|1985|p=308}} Ruhoff was succeeded in October 1944 by Lieutenant Colonel W. E. Kelley, who in turn was succeeded by Lieutenant Colonel G. W. Beeler in April 1946.{{sfn|Manhattan District|1947a|pp=1.15–1.16}}
The original goal of the feed materials program in 1942 was to acquire approximately {{convert|1,700|ST|t|order=flip}} of black oxide. By the time of the dissolution of the Manhattan District at the end of 1946, it had acquired about {{convert|10,000|ST|order=flip}}. The total cost of the feed materials program up to 1 January 1947 was approximately USD$90,268,490 ({{Inflation|US|90,268,490|1947|fmt=eq}}), of which $27,592,360 ({{Inflation|US|27,592,360|1947|fmt=eq}}) was for procurement of raw materials, $58,622,360 ({{Inflation|US|58,622,360|1947|fmt=eq}}) for refining and processing operations, and $3,357,690 ({{Inflation|US|3,357,690|1947|fmt=eq}}) for research, development, and quality control.{{sfn|Manhattan District|1947a|pp=S1–S4}}
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After the Belgian Congo, the next most important source of uranium ore was Canada. Canadian ore came from the [[Eldorado Mine (Northwest Territories)|Eldorado Mine]] in the [[Great Bear Lake]] area, not far south of the [[Arctic Circle]].{{sfn|Jones|1985|pp=310–311}}{{sfn|Hewlett|Anderson|1962|pp=85–86}} In May 1930, [[Gilbert LaBine]] went prospecting in the area. LaBine was the managing director of Eldorado Gold Mines, a firm he co-founded in January 1926 with his brother Charlie, but which no longer had any gold mines.{{sfn|Bothwell|1984|pp=17–19}}
On 16 May, LaBine found pitchblende near the shores of Echo Bay at a mine site that became [[Port Radium]].{{sfn|Bothwell|1984|pp=23–25}}<ref>{{cite magazine |title=Science: Radium |magazine=[[Time (magazine)|Time]] |url=https://time.com/archive/6757353/science-radium/ |access-date=25 February 2025 }}</ref> Eldorado also established a processing plant at Port Hope, Ontario, the only facility of its kind in North America. To run it, LaBine hired Marcel Pochon,<ref>{{Cite book |last=Sanger |first=Penny |url=https://porthopehistory.com/nuclearindustry/blindfaith.html |title=Blind faith - The nuclear industry in one small town |date=1981 |publisher=McGraw-Hill Ryerson |isbn=978-0-07-092423-9 |___location=Toronto, New York}}</ref> a French chemist who had learned how to refine radium under [[Pierre Curie]], who was working at the recently closed [[South Terras mine]] in Cornwall.{{sfn|Bothwell|1984|pp=55–57}}<ref>{{cite web |title=How Canada supplied uranium for the Manhattan Project |publisher=CBC Documentaries |url=https://www.cbc.ca/documentaries/how-canada-supplied-uranium-for-the-manhattan-project-1.7402051 |access-date=25 February 2025 |archive-date=11 February 2025 |archive-url=https://web.archive.org/web/20250211161617/https://www.cbc.ca/documentaries/how-canada-supplied-uranium-for-the-manhattan-project-1.7402051 |url-status=live }}</ref><ref>{{cite magazine |title=Science: Radium |magazine=[[Time (magazine)|Time]] |url=https://content.time.com/time/subscriber/article/0,33009,758086-2,00.html |access-date=25 February 2025 |url-access=subscription |archive-date=10 October 2023 |archive-url=https://web.archive.org/web/20231010121538/https://content.time.com/time/subscriber/article/0,33009,758086-2,00.html |url-status=live }}</ref> Ore was mined at Port Radium and shipped via [[Great Bear River|Great Bear]], [[Mackenzie River|Mackenzie]] and [[Slave River]]s to [[Waterways, Alberta]], and thence by rail to Port Hope.{{sfn|Bothwell|1984|pp=11–15}}<ref name="Macleans">{{cite magazine |title=Port Radium's Eldorado - The Mine that Shook the World |first=Ronald A. |last=Keith |magazine=Maclean's Magazine |date=15 November 1945 |via=Republic of Mining |url=https://republicofmining.com/2016/09/14/port-radiums-eldorado-the-mine-that-shook-the-world-by-ronald-a-keith-macleans-magazine-november-15-1945/ |access-date=26 February 2025}}</ref> Two [[towboat]]s were acquired: the ''Radium King'' and ''Radium Queen'', and they pulled ore [[scow]]s named ''Radium One'' to ''Radium Twelve''.{{sfn|Bothwell|1984|pp=66–67}}<ref>{{cite news |title=Discouraging Difficulties Overcome by Eldorado Pioneers |newspaper=[[Edmonton Bulletin]] |date=11 December 1945 |page=16 |via=newspapers.com |url=https://www.newspapers.com/article/the-edmonton-bulletin/113391751/ |access-date=26 February 2025}}</ref> Great Bear Lake is only navigable between early July and early October, being icebound the rest of the year,{{sfn|Bothwell|1984|pp=11, 41}} but mining activity continued year-round.{{sfn|Manhattan District|1947a|p=3.1}}
Competition from Union Minière was fierce and served to drive the price of radium down from CAD$70 per milligram in 1930 ({{Inflation|CA|70|1930|fmt=eq}}) to CAD$21 per milligram in 1937 ({{Inflation|CA|21|1937|fmt=eq}}). Boris Pregel negotiated a cartel deal with Union Minière under which each company gained exclusive access to its home market and split the rest of the world 60:40 in Union Minière's favor. The outbreak of war in September 1939 blocked access to hard-won European markets, especially Germany, a major customer for ceramic-grade uranium. Union Minière lost its refinery at [[Olen, Belgium|Olen]] when Belgium was overrun, forcing it to use Eldorado's mill at Port Hope.{{sfn|Bothwell|1984|pp=71–75}} With sufficient stocks on hand for five years of operations, Eldorado closed the mine in June 1940.{{sfn|Manhattan District|1947a|p=3.1}}{{sfn|Bothwell|1984|pp=102–107}}
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The next step in the refining process was the conversion of black oxide into orange oxide ({{chem2|UO3}}) and then into brown oxide ({{chem2|UO2}}).{{sfn|Manhattan District|1947a|pp=8.1–8.4}} On 17 April 1942,{{sfn|Fleishman-Hillard|1967|p=18}} [[Arthur Compton]], the head of the Manhattan Project's Metallurgical Project,{{sfn|Compton|1956|pp=82–83}} along with [[Frank Spedding]] and [[Norman Hilberry]],{{sfn|Ruhoff|Fain|1962|p=4}} met with Edward Mallinckrodt Sr., the chairman of the board of Mallinckrodt,<ref>{{cite journal |title=Edward Mallinckrodt, Jr. 1878–1967 |journal=[[Radiology (journal)|Radiology]] |date=1 March 1967 |volume=88 |issue=3 |page=594 |doi=10.1148/88.3.594 }}</ref> and inquired whether his company could produce the extremely pure uranium compounds that the Manhattan Project required. It was known that [[uranyl nitrate]] ({{chem2| UO2(NO3)2}}), was soluble in [[diethyl ether|ether]] ({{chem2|(CH3CH2)2O}}), and this could be used to remove impurities.{{sfn|Ruhoff|Fain|1962|p=4}} This process had never been attempted on a commercial scale, but it had been demonstrated in the laboratory by [[Eugène-Melchior Péligot]] a century before. What had also been amply demonstrated in the laboratory was that ether was erratic, explosive and dangerous to work with.{{sfn|Fleishman-Hillard|1967|pp=18–19}}{{sfn|Compton|1956|p=93}}
Mallinckrodt agreed to undertake the work for $15,000 ({{Inflation|US|15,000|1942|fmt=eq}}).{{sfn|Ruhoff|Fain|1962|p=4}}{{sfn|Fleishman-Hillard|1967|p=20}} A [[pilot plant]] was set up in the alley between Mallinckrodt buildings 25 and K in downtown St. Louis.<ref name=":0">{{Cite web |last=Singer-Vine |first=Jeremy |last2=Emshwiller |first2=John R. |last3=Parmar |first3=Neil |last4=Scott |first4=Charity |title=St. Louis Downtown Site — St. Louis, Mo. — Waste Lands America's forgotten nuclear legacy |url=https://www.wsj.com/graphics/waste-lands/site/438-st-louis-downtown-site/ |access-date=2025-04-23 |website=The Wall Street Journal}}</ref> The pilot plant produced its first uranyl nitrate on 16 May, and samples were sent to the [[University of Chicago]], [[Princeton University]] and the [[National Bureau of Standards]] for testing.{{sfn|Ruhoff|Fain|1962|pp=7–8}}{{sfn|Fleishman-Hillard|1967|p=20}}
The production process involved adding black oxide to {{convert|1,000|USgal|L|adj=on|order=flip}} stainless steel tanks of hot concentrated nitric acid to produce a solution of uranyl nitrate. This was filtered through a stainless steel filter press and then concentrated in {{convert|300|USgal|L|adj=on|order=flip}} pots heated by steam coils to {{convert|248|F|C|order=flip}}, the [[boiling point]] of uranyl nitrate. The molten uranyl nitrate was cooled to {{convert|176|F|C|order=flip}} and then pumped into ether that had been chilled to {{convert|0|C}} in an ice water [[heat exchanger]]. The purified material was washed with distilled water and then boiled to remove the ether, producing orange oxide.{{sfn|Fleishman-Hillard|1967|p=20}}{{sfn|Ruhoff|Fain|1962|pp=7–8}} This was then reduced to brown oxide by heating in a hydrogen atmosphere.{{sfn|Manhattan District|1947a|pp=8.1–8.4}} The production plant was established in two empty buildings: the dissolving and filtering was conducted in Building 51 and the ether extraction and aqueous re-extraction in Building 52. The plant operated around the clock,{{sfn|Fleishman-Hillard|1967|p=20}}{{sfn|Ruhoff|Fain|1962|pp=7–8}} and by July it was producing a ton of brown oxide each day, six days a week, at a unit price of {{convert|1.56|$/lb|2|order=flip}} (equivalent to ${{Inflation|US|{{convert|1.56|/lb|order=flip|disp=number}}|1942}}/kg in {{Inflation/year|US}}).{{sfn|Manhattan District|1947a|pp=8.1–8.4}}
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As various improvements were incorporated into the process, the plant's capacity rose from its designed capacity of {{convert|52|ST|t|order=flip}} per month to {{convert|165|ST|t|order=flip}} per month. At the same time, the cost of brown oxide fell from {{convert|1.11|to|0.70|$/lb|2|order=flip}} (equivalent to ${{Inflation|US|{{convert|1.11|/lb|order=flip|disp=number}}|1942}}/kg to ${{Inflation|US|{{convert|0.70|/lb|order=flip|disp=number}}|1942}}/kg in {{Inflation/year|US}}), so Mallinckrodt refunded $332,000 ({{Inflation|US|332,000|1942|fmt=eq}}) to the government.{{sfn|Manhattan District|1947a|pp=8.1–8.4}} The Mallinckrodt plant closed in May 1946, by which time it had produced {{convert|4,190|ST|t|order=flip}} of brown and orange oxide at a cost of $4,745,250 ({{Inflation|US|4,745,250|1942|fmt=eq}}). In May 1945, Mallinckrodt decided to build a new brown oxide plant. Construction commenced on 15 June 1945, and was completed on 15 June 1946. Between then and 1 January 1947, it produced {{convert|507|ST|t|order=flip}} of brown and orange oxide at a unit cost of {{convert|0.82|$/lb|2|order=flip}} (equivalent to ${{Inflation|US|{{convert|0.82|/lb|order=flip|disp=number}}|1942}}/kg in {{Inflation/year|US}}).{{sfn|Manhattan District|1947a|pp=8.1–8.4}}
Other brown oxide plants were operated by Linde in Tonawanda,<ref>{{Cite web |last=Singer-Vine |first=Jeremy |last2=Emshwiller |first2=John R. |last3=Parmar |first3=Neil |last4=Scott |first4=Charity |title=Linde Air Products, Ceramics Plant — Tonawanda, N.Y. — Waste Lands America's forgotten nuclear legacy |url=https://www.wsj.com/graphics/waste-lands/site/246-linde-air-products-ceramics-plant/ |access-date=2025-04-23 |website=The Wall Street Journal}}</ref> and DuPont in [[Deepwater, New Jersey]],<ref name=":1">{{Cite web |last=Singer-Vine |first=Jeremy |last2=Emshwiller |first2=John R. |last3=Parmar |first3=Neil |last4=Scott |first4=Charity |title=DuPont Deepwater Works — Deepwater, N.J. — Waste Lands America's forgotten nuclear legacy |url=https://www.wsj.com/graphics/waste-lands/site/141-dupont-deepwater-works/ |access-date=2025-04-23 |website=The Wall Street Journal}}</ref> using the process devised by Mallinckrodt, but only Mallinckrodt also shipped orange oxide.{{sfn|Manhattan District|1947a|pp=8.1–8.4}} Production commenced at Deepwater in June 1943, and by 1 January 1947 it had produced {{convert|1,970|ST|t|order=flip}} of brown oxide.{{sfn|Manhattan District|1947a|pp=8.4–8.7}} Much of the Deepwater feed was recovered scrap material. This was converted into a [[uranyl peroxide]] ({{chem2|UO4}}) that could be fed into the brown oxide process as if it were black oxide.{{sfn|Reed|2014|p=471}} Production commenced at Tonawanda in August 1943 and it produced {{convert|300|ST|t|order=flip}} of brown oxide before being closed in early 1944. Mallinckrodt was already producing {{convert|110|ST|t|order=flip}} of brown oxide per month or the Manhattan Project's requirement for {{convert|160|ST|t|order=flip}} and Union Carbide wanted to use the facilities for nickel compounds production for the [[K-25]] project.{{sfn|Manhattan District|1947a|pp=8.4–8.7}}
=== Green salt and uranium hexafluoride ===
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Before the war, the only uranium metal available commercially was produced by the [[Westinghouse Electric and Manufacturing Company]], using a photochemical process. Brown oxide was reacted with [[potassium fluoride]] in large vats on the roof of Westinghouse's plant in [[Bloomfield, New Jersey]].{{sfn|Hewlett|Anderson|1962|pp=65–66}} This produced ingots the size of a [[Quarter (United States coin)|quarter]] that were sold for around $20 per gram. [[Edward Creutz]], the head of the Metallurgical Laboratory's group responsible for fabricating the uranium, wanted a metal sphere the size of an orange for his experiments. With Westinghouse's process, this would have cost $200,000 ({{Inflation|US|200,000|1942|fmt=eq}}) and taken a year to produce.{{sfn|Compton|1956|pp=90–91}}
The hydride or "hydramet" process was developed by Peter P. Alexander, at Metal Hydrides, which used [[calcium hydride]] ({{chem2|CaH2}}) as the [[reducing agent]].{{sfn|Alexander|1943|p=3}}{{sfn|Wilhelm|1960|p=59}}<ref>{{Cite journal |last=Adams |first=David L. |date=March 1996 |title=Metal Hydrides and the Dawn of the Atomic Age |url=https://pubs.acs.org/doi/abs/10.1021/ed073p205 |journal=Journal of Chemical Education |language=en |volume=73 |issue=3 |pages=205 |doi=10.1021/ed073p205 |issn=0021-9584}}</ref> By this means the Metal Hydrides plant in Beverly, Massachusetts,<ref name=":2">{{Cite web |last=Singer-Vine |first=Jeremy |last2=Emshwiller |first2=John R. |last3=Parmar |first3=Neil |last4=Scott |first4=Charity |title=Ventron Corporation — Beverly, Mass. — Waste Lands America's forgotten nuclear legacy |url=https://www.wsj.com/graphics/waste-lands/site/67-ventron-corporation/ |access-date=2025-04-23 |website=The Wall Street Journal}}</ref> managed to produce a few pounds of uranium metal. Unfortunately, the calcium hydride used contained unacceptable amounts of [[boron]], a neutron poison, making the metal unsuitable for use in a reactor. Some months would pass before Clement J. Rodden from the National Bureau of Standards and Union Carbide found a means to produce sufficiently pure calcium hydride.{{sfn|Hewlett|Anderson|1962|pp=65–66}}{{sfn|Manhattan District|1947e|pp=12.9–12.10}} Meal Hydrides managed to produce {{convert|41|ST|t|order=flip}} of metal by the time operations were suspended on 31 August 1943. It then started reprocessing scrap uranium metal, and produced {{convert|1,090|ST|t|order=flip}} at a cost of $0.33 per pound.{{sfn|Manhattan District|1947a|pp=10.7–10.7}}
At the [[Ames Project]] at [[Iowa State College]], Frank Spedding and [[Harley Wilhelm]] began looking for ways to create the uranium metal. At the time, it was produced in the form of a powder, and was highly [[pyrophoric]]. It could be pressed and [[sintered]] and stored in cans, but to be useful, it needed to be melted and cast. Casting presented difficulty because uranium corroded [[crucible]]s of beryllium, magnesia and graphite. To produce uranium metal, they tried reducing uranium oxide with hydrogen, but this did not work. While most of the neighboring elements on the [[periodic table]] can be reduced to form pure metal and [[slag]], uranium did not behave this way.{{sfn|Payne|1992|pp=66–67}} (At the time it was mistakenly believed that uranium belonged under [[chromium]], [[molybdenum]] and [[tungsten]] in the periodic table.{{sfn|Wilhelm|1960|p=60}}) In June 1942 they tried reducing the uranium with carbon in a hydrogen atmosphere, with only moderate success. They then tried aluminium, magnesium and calcium, all of which were unsuccessful. The following month the Ames team found that molten uranium could be cast in a graphite container.{{sfn|Payne|1992|pp=66–67}} Although graphite was known to react with uranium, this could be managed because the carbide formed only where the two touched.{{sfn|Corbett|2001|pp=15–16}}
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