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Incoming links: Iron oxide
Steel is an iron-based alloy with controlled carbon content and impurities; its manufacture requires extracting iron from an ore and then adjusting the composition. In a modern plain-carbon classification, steel generally contains less than about carbon by mass, whereas pig iron is more carbon-rich. The historical practical contrast was with low-carbon wrought iron and readily cast but relatively brittle cast iron. Hardening by quenching is characteristic of suitable carbon-rich steels, but not every grade hardens in the same way.
Begin, for example, with an iron oxide ore. Preparation removes some earthy matter and, where appropriate, roasting expels moisture or converts a carbonate-bearing ore to oxide. A blast furnace receives the ore, coke and a flux such as limestone. The hot air blast sustains combustion of coke, generating heat and the carbon monoxide needed for much of the oxide reduction. Representative overall balances areCalcination of limestone provides calcium oxide. Combination with acidic gangue, represented by silica, gives a liquid slag:Actual slag is a multicomponent melt, rather than necessarily pure calcium silicate. The descending iron picks up carbon and other impurities and collects as molten pig iron. This first extraction product is not already finished steel.
Two important routes available in 1867 proceed from this stage. In the older indirect route, refining and puddling oxidize much of the carbon and remove slag-associated impurities to obtain wrought iron. Bars packed with charcoal are then heated for a prolonged period in the cementation process. Carbon enters the bars, giving blister steel; forging and welding can make shear steel, while melting suitable stock in covered crucibles produces more uniform crucible steel. The bar can acquire carbon through gas-mediated surface reactions and diffusion; the process should not be imagined as intact charcoal grains travelling through the iron.
In the Bessemer process, an air blast passes through molten pig iron in a converter. Oxidation of silicon, manganese and carbon supplies heat, while lowering the carbon content. Composition can be corrected by adding a controlled carbon- and manganese-bearing material such as spiegeleisen. Henry Bessemer's 1856 patent describes the central idea of maintaining the conversion by oxidizing constituents of the molten metal, without fuel for reheating during that stage.[ref]
Improvement in the manufacture of iron and steel by Henry Bessemer. US16082A, specification and final claim, 11 November 1856
The early acidic converter demanded suitable feed: it did not solve removal of phosphorus from every ore. Later basic converter practice must not be silently imported into a December 1867 account. Final casting, working and heat treatment determine the steel microstructure and properties as well as composition. The useful manufacturing chain is therefore ore → extracted carbon-rich iron → controlled composition → worked and appropriately heat-treated steel.
Establish that the stain contains blood; then state separately whether its human origin can be established. In 1867, a positive blood test could not reliably distinguish human blood from that of another mammal.
First record the position, extent, colour and underlying material of the stain. Keep a portion untouched, take a small scraping or cutting for examination, and test an unstained portion of the same material alongside it. The comparison is important: a coloured fabric, iron oxide or a vegetable colouring substance may resemble dried blood, and the material itself can interfere with a chemical test. Brown colour alone proves nothing.
For an examination practicable in 1867, use complementary observations:
- Moisten a small portion with an appropriate aqueous medium and examine it by microscopy. Recognisable red blood cells support the identification. Oval, nucleated red blood cells would point towards certain non-mammalian sources; human red blood cells are normally non-nucleated discs. Drying and extraction distort the cells, however, and their measured diameters overlap those of other mammals. An apparent match with human red blood cells therefore does not establish human origin.
- Apply the historical haemin crystal test to a separate portion: gently heat the material with acetic acid and a little sodium chloride on a covered microscope slide, then look for the characteristic brown crystalline product. A positive result supports the presence of a hemoglobin derivative. It does not identify the species.
- Where a suitable spectroscope is available, examine an extract for the characteristic absorption spectrum of hemoglobin and the changes produced by altering its chemical state. This adds a different kind of evidence, but the absorption spectrum is again shared by the blood of different species. Spectroscopy of blood was already developing before this examination; it should not be confused with later DNA profiling.[ref]Identification of blood by the National Institute of Justice. Unit II, §§3–6: historical development, microscopic examination, crystal tests and spectral methods
These observations should agree before the examiner expresses a positive conclusion. Failure to recover intact red blood cells does not exclude an old bloodstain; conversely, a colour reaction without suitable controls is weak evidence. A defensible period report would distinguish “blood identified, consistent with mammalian origin” from “human blood proved.” The second conclusion does not follow from the first.
For comparison, later precipitin tests use antibodies against human proteins to investigate species of origin. Modern DNA profiling can investigate the donor, subject to preservation and contamination limits. These are later developments, not procedures to attribute to an Oxford candidate in 1867.[ref]
Confirmatory blood tests by the National Institute of Justice. “Confirmatory Tests”: crystal formation versus human-origin testing with specific antisera
The main distinction is between metallic iron, iron(II) preparations, iron(III) preparations, and mixed iron oxides. The old prefixes “proto-” and “per-” ordinarily distinguish the lower and higher oxidation states here. “Peroxide of iron” means the historical iron(III) oxide preparation, not a modern peroxide containing an oxygen–oxygen bond.
The principal medicinal preparations can be grouped by the chemical form supplied:
- Iron(II) sulfate: Ferri sulphas, its granulated form, and its dried form supply iron(II). The ordinary and granulated salts are represented as ; the 1867 dried preparation is represented as . Drying principally changes the water of crystallization, rather than converting iron(II) into iron(III).
- Iron(II) carbonate: Ferri carbonas saccharata, the carbonate pill, and the compound iron mixture contain freshly formed iron(II) carbonate, . Exposure to air introduces higher iron oxides; sucrose helps preserve the lower oxidation state. Thus the saccharated material is a protected preparation rather than a pure, permanently stable salt.
- Iron(II) iodide: Ferri iodidum, its syrup, and its pill supply mainly . The historical solid includes water of crystallization and some iron oxide; the syrup again employs sucrose to retard deterioration.
- Iron(II) phosphate: Ferri phosphas and the corresponding syrup supply the lower iron phosphate, conventionally . The official precipitated material is partly oxidized, so describing the actual powder as chemically pure iron(II) phosphate would be too strong.
- Iron(III) chloride: the solution and tincture of “perchloride of iron” contain the higher chloride, , in an acidic liquid. This historical “perchloride” is unrelated to a perchlorate.
- Iron(III) nitrate: solution of “pernitrate of iron” contains the higher nitrate, , again in an acidic liquid. The solution of “persulphate” used to manufacture several other preparations supplies iron(III) sulfate, ; it is useful to distinguish this manufacturing reagent from the widely administered iron(II) sulfate.
- Iron(III) with organic acids: citrate of iron and ammonium, and tartarated iron, contain the higher iron in citrate or tartrate combinations. Citrate of iron and quinine is prepared from a higher iron compound, but should not be assumed to contain exclusively iron(III): the 1867 monograph reports blue reactions with both potassium ferrocyanide and potassium ferricyanide, consistent with an iron(II) component as well. The tartarated preparation also contains potassium; citrate of iron and quinine is made with Ammonia. They should be described as soluble pharmaceutical combinations, without pretending that every historical batch had a single simple molecular formula. The acetate tincture similarly contains the higher iron combined with acetic acid.
- Iron oxides: Ferri peroxidum hydratum (dried hydrated “peroxide”) and Ferri peroxidum humidum (the moist material) contain iron(III) as iron(III) oxide or hydrated iron(III) oxide. The magnetic oxide is a mixed iron(II)–iron(III) oxide preparation; expresses the ideal mixed oxide, rather than a claim that the historical hydrated powder was pure crystalline magnetite.
- Metallic iron: Ferrum redactum, used also in lozenges, contains finely divided iron in oxidation state zero together with magnetic oxide. The official preparation is therefore not all elemental iron. Iron wine made by contacting wire with wine obtains a dissolved tartrate-containing iron preparation from reaction with the wine's acids; the wire placed in the vessel should not be confused with the chemical form in the liquid ultimately dispensed.
These identifications follow the historical monographs, rather than the names of present commercial supplements.[ref]
British Pharmacopoeia by the General Medical Council (1867). “Ferri carbonas saccharata” through “Ferrum tartaratum”, pp. 130–141; the iron solutions, pp. 186–189; “Vinum ferri”, p. 367
A green iron(II) sulfate solution gives the characteristic blue reaction with potassium ferricyanide, whereas the higher iron solutions give blue with potassium ferrocyanide. Those diagnostic reactions explain why the official tests distinguish the two oxidation states; the historical colour test alone does not establish every detail of a complex preparation's composition.