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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>{{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>{{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>{{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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Due to its neutron-absorbing properties, [[boron-10]] found multiple uses at the [[Los Alamos Laboratory]],{{sfn|Manhattan District|1947c|p=VIII-19}} which raised a requirement for boron in both its natural form and enriched in the boron-10 isotope.{{sfn|Manhattan District|1947d|p=7.1}} This led to two lines of research at the Manhattan Project's [[SAM Laboratories]] at [[Columbia University]] in New York City: one aimed at developing a means of reducing boron compounds, and one at separating boron isotopes using an [[isotope fractionation]] process. Harshaw was awarded the contract to supply [[boron trifluoride]] ({{chem2|BF3}}), at least 97% pure. A total of {{convert|92,450|lb|kg|order=flip}} was supplied by 1 March 1946 for $72,770 ({{Inflation|US|72,770|1946|fmt=eq}}).{{sfn|Manhattan District|1947d|pp=7.2-7.7}}
Once the research into isotope separation had progressed sufficiently, the contract for the isotope separation was awarded to the [[Standard Oil Company of Indiana]], since fractionation was a common practice in the oil industry. While both boron trifluoride and [[dimethyl ether]] were gases at room temperature, their complex was a liquid. The [[American Cyanamid Company]] was awarded the contract for processing the boron trifluoride/dimeythl ether complex. The schedule called for the production of a kilogram of boron as soon as possible, five kilograms by 15 September 1944, and five kilograms per month thereafter. The plant in [[Stamford, Connecticut]], was ready on 7 July 1944.<ref>{{Cite web |last=Singer-Vine |first=Jeremy |last2=Emshwiller |first2=John R. |last3=Parmar |first3=Neil |last4=Scott |first4=Charity |title=American Cyanamid Co — Stamford, Conn. — Waste Lands America's forgotten nuclear legacy |url=https://www.wsj.com/graphics/waste-lands/site/25-american-cyanamid-co/ |access-date=2025-04-23 |website=The Wall Street Journal}}</ref> Production ceased on 30 June 1946, by which time Cyanamid had delivered {{convert|504|lb|order=flip}} of crystalline boron-10, {{convert|850|lb|order=flip}} of calcium fluoride-boron trifluoride complex enriched in the boron-10 isotope, and {{convert|242|lb|order=flip}} of calcium fluoride-boron trifluoride complex enriched in the boron-11 isotope.{{sfn|Manhattan District|1947d|pp=7.2-7.7}}
===Graphite===
[[Graphite]] was chosen as a [[neutron moderator]] in the Manhattan Project's nuclear reactors, as [[heavy water]], while a superior moderator, was not yet available in the necessary quantities and would take too much time to produce.{{sfn|Compton|1956|pp=98–100}} At first, it appeared that procurement of graphite would not be a problem, as hundreds of tons were produced in the United States every year. The problem was purity.{{sfn|Smyth|1945|pp=40–41}} The graphite obtained by the Columbia University in 1941 had been manufactured by the US Graphite Company in [[Saginaw, Michigan]]. While it was of high purity for a commercial product, it contained 2 parts per million of boron, a neutron poison.{{sfn|Smyth|1945|pp=69–70}}
Scientists at the National Bureau of Standards found that the boron in commercial graphite came from the foundry [[coke (fuel)|coke]] used in its production, which contained 15 times as much boron as petroleum-based coke. By substituting [[petroleum coke]] and altering some of the production steps, the [[National Carbon Company]] in New York<ref>{{Cite web |last=Singer-Vine |first=Jeremy |last2=Emshwiller |first2=John R. |last3=Parmar |first3=Neil |last4=Scott |first4=Charity |title=National Carbon Co. — New York, N.Y. — Waste Lands America's forgotten nuclear legacy |url=https://www.wsj.com/graphics/waste-lands/site/305-national-carbon-co/ |access-date=2025-04-23 |website=The Wall Street Journal}}</ref> and the Speer Carbon Company in [[St. Marys, Pennsylvania]], were able to make graphite that absorbed 20% fewer neutrons, which was sufficient to meet the Metallurgical Laboratory's stringent standards.{{sfn|Compton|1956|pp=97–98}}{{sfn|Jones|1985|pp=65–66}}{{sfn|Manhattan District|1947e|pp=12.7–12.9}}
===Polonium===
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