Sunday, November 22, 2020
  1. Synthesis of Sodium Thioantimonate and Antimony(V) Sulfide
    1. This same basic method (with some modifications) can be used to produce sodium thioarsenate 

Saturday, November 21, 2020
  1. Synthesis of Potassium Platinocyanide Trihydrate K2Pt(CN)4•3H2O
    1. From atomistry: "Gmelin, who discovered the ferricyanides, observed that by heating to redness a mixture of platinum sponge and potassium ferrocyanide, a compound results in which platinum replaces iron. Analysis of the product crystallized from water showed it to have the formula K2Pt(CN)4•3H2O..."
    2. From theodora: "Spongy platinum is produced when ammonium platinochloride is ignited; platinum black on the reduction of acid solutions of platinum salts; and colloidal platinum by passing an electric arc between two platinum wires under the surface of pure water (G. Bredig, Zeit. phys. Chem., 1901, 37, pp. 1, 323). Platinum is practically unoxidizable; it combines directly with phosphorus, arsenic, antimony, silicon, boron, and fluorine, and with almost all other metals. It is practically unattacked by all acids, dissolving only in aqua regia or in mixtures which generate chlorine. When fused with alkaline hydroxides in the presence of air it forms platinates. It is readily attacked by fused nitrates, and by potassium cyanide and ferrocyanide. All the platinum compounds when heated strongly decompose, and leave a residue of the metal. Of platinum salts, in the true sense of the word, none exist; there is no carbonate, nitrate, sulphate, &c; halide salts, however, are known, but are obtained in an indirect manner."
    3. Melting point of potassium ferrocyanide = 300oC; "boils" (decomposes) at 400oC.
    4. Atomic weight of platinum = 195.084 grams per mole
    5. Molar mass of potassium ferrocyanide trihydrate = 422.39 grams per mole
    6. Mass of platinum = 0.53 grams of platinum black
    7. Moles of platinum = 0.00271677841340 moles
    8. 0.00271677841340 moles of potassium ferrocyanide trihydrate = 1.15 grams
Wednesday, November 18, 2020
  1. Synthesis of Sodium Sulfide Na2S
    1. Preparation of Ferrous Sulfide by combination of 7 parts iron powder and 4 parts sulfur
      1. Iron powder = 85.05 grams or 1.522965 moles of iron
      2. Flowers of sulfur = 48.6 grams or 1.51567129 moles of sulfur
      3. Total mass of ferrous sulfide produced = 128.17 grams
    2. FeS + H2SO4 → FeSO4 + H2S
      1. ​​​​​​​Ferrous sulfide = 87.910 grams per mole so 128.17 grams is1.457968 moles
    3. ​​​​​​​H2S + 2NaOH → Na2S + H2O
      1. ​​​​​​​Some sulfide is lost as elemental sulfur and hydrogen sulfide must be present in excess to ensure full conversion of the hydroxide to alkali sulfide.
      2. Use 1 mole of NaOH.
Monday, November 16, 2020
  1. Synthesis of Ammonium Iodate (Recommended by Alexander K.)
    1. Ba(IO3)2 + (NH4)2SO4 → BaSO4 + 2NH4IO3
      1. Barium Iodate solubility in water = 0.035 grams per 100 mLs of water at 20oC (142.97 times more soluble than BaSO4)
        1. ​​​​​​​Barium Iodate Monohydrate Molar Mass = 505.15 g/mol
        2. 7.83 grams of barium iodate is 0.0155 moles
      2. Ammonium Sulfate solubility in water = 75.4 grams per 100 mLs of water at 20oC
        1. ​​​​​​​Ammonium Sulfate Molar Mass = 132.14 g/mol
        2. 0.0155 moles ammonium sulfate is 2.0482 grams 
      3. Barium Sulfate solubility in water = 0.0002448 grams per 100 mLs of water at 20oC
Sunday, November 15, 2020
  1. Synthesis of Thallium(I) Triiodide 
    1. Taken from the Handbook for Preparative Inorganic Chemistry Volume 1 page 876-877
    2. Incredible stroke of luck!!! A tremendously useful source on thallium compounds has apparently existed all this time! A Comprehensive Treatise on Inorganic and Theoretical Chemistry, Volume 5. Thus far I have only found this source in this one place.
    3. Rubidium tetraiodothallate(III) dihydrate can be prepared from thallic iodide and rubidium iodide in the correct stoichiometric proportions.
    4. Reagents Needed:
      1. 0.51 grams thallium(I) iodide, 0.001540 moles
        1. Molar mass 331.27 g/mol
      2. Molar mass of RbI 212.3723 g/mol
        1. 0.001540 moles of RbI = 0.327 grams
        2. Solubility of RbI in MeOH = 11.1 grams / 100 grams of MeOH at 18o​​​​​​​C
      3. ​​​​​​​Molar mass of diiodine 253.8089 g/mol
        1. ​​​​​​​​​​​​​​0.001540 moles of I2 = 0.391 grams

  1. Synthesis of "Blue Lanthanum Acetate"
    1. When a cold aqueous solution of lanthanum acetate is made ammoniacal, a colloidal basic acetate is precipitated; if a little solid iodine be added to the precipitate a blue adsorption compound is produced, similar in appearance to the familiar "starch-iodide" precipitate. The blue substance may conveniently be prepared by adding a solution of iodine in potassium iodide to a cold solution of lanthanum acetate (or nitrate acidified with acetic acid), adding ammonia cautiously until very little iodine is left unchanged, and then warming the mixture very gently.
    2. The following is taken from "A Colorimetric Microanalytical Method For Acetate And Fluoroacetate" by John O. Hutchens and Beatrice M. Kass, Received for publication June 24, 1948

Saturday, October 31, 2020
  1. Recovered amounts of thallium(I) halides
    1. TlCl = 1.47 grams, 0.006129597 moles
      1. Molar Mass = 239.82 grams per mole
    2. TlBr = 2.61 grams, 0.0091807661 moles
      1. ​​​​​​​Molar Mass = 284.29 grams per mole
      2. Use 0.59 grams TlBr in order to turn all TlCl into Tl3[TlCl3Br3]. Dissolve in 13.83 mL and react with 0.497 grams Br2 to obtain 0.15M TlBr3 
    3. TlI = 0.51 grams, 0.00153952968877 moles
      1. ​​​​​​​​​​​​​​Molar Mass = 331.27 grams per mole
      2. React with 0.3907 grams I2 to make TI3
Monday, October 26, 2020
  1. Synthesize of Thallium(I) Azide
    1. Molar mass of thallium(I) azide = 246.4035 grams per mole
    2. Molar mass of sodium azide = 65.0099 grams per mole
    3. 100 grams of water will dissolve x grams of thallium(I) azide
      1. At 0oC it dissolves 0.171 grams
      2. At 10oC it dissolves 0.236 grams
      3. At 20oC it dissolves 0.364 grams
      4. "It is sparingly soluble in cold, more readily soluble in hot water, from which it separates on cooling in tetragonal needles isomorphous with the potassium and rubidium salts." Atomistry article on Thallous Azide
    4. ​​​​​​​"Thallous azide slowly turns brown in sunlight. It melts at 334° in an atmosphere of carbon dioxide, and is reduced to thallium when heated in hydrogen. When suddenly heated or subjected to shock, it explodes.​​​​​​​" Atomistry article on Thallous Azide
    5. "Although it is not nearly as sensitive to shock or friction as lead azide, it can easily be detonated by a flame or spark. It can be stored safely dry in a closed non-metallic container." Wikipedia article on thallium(I) azide
  2. ​​​​​​​Synthesize Thallium(I) Chloride
    1. ​​​​​​​Cesium hexachlorothallate, HoPIC page 873
    2. TlBr2Cl
  3. Synthesize Thallium(I) Bromide
    1. ​​​​​​​Thallium(I) Hexabromothallium(III), HoPIC page 875
    2. TlBrCl2 
  4. Synthesize Thallium(I) Iodide
    1. ​​​​​​​Thallium(I) Triiodide HoPIC page 876
    2. Cesium Tetraiodothallate Tl3+ + CsCl + NaI → Cs[TlI4] Orange red hexagons or rectangles
Saturday, October 24, 2020
  1. Synthesis of Bismuth Thiocyanate
    1. THIOCYANIC ACID. [CAS: 463-56-9]. Aqueous solution of hydrogen thiocyanate, HSCN, formula weight 59.08, yellow solid below mp 5 ◦ C, unstable gas at room temperature. The acid is moderately stable only when dilute and cold. The salts of this acid are known as thiocyanates. Thiocyanic acid is formed by reaction of barium thiocyanate solution and dilute sulfuric acid, and filtering off barium sulfate, or by the action of hydrogen sulfide on silver thiocyanate, filtering off silver sulfide. Sodium, potassium, barium, or calcium thiocyanate may be made by reaction of sulfur and the corresponding cyanide by heating to fusion. Ammonium thiocyanate (plus ammonium sulfide) may be made by reaction of ammonia and carbon disulfide, a reaction which probably accounts for the presence of ammonium thiocyanate in the products of the destructive distillation of coal. This reaction corresponds to the formation of ammonium cyanate from ammonia and carbon dioxide. Silver, lead, copper(I), and thallium(I) thiocyanates are insoluble and mercury(II), bismuth, and tin(II) thiocyanates slightly soluble. All of these are soluble in excess of soluble (e.g., ammonium) thiocyanate, forming complexes. Iron(III) thiocyanate gives a blood-red solution, used in detecting either Fe(III) or thiocyanate in solution, and is extracted from water by amyl alcohol. It is not formed in the presence of fluoride, phosphate and other strongly complexing ions. When thiocyanic acid is treated with certain oxidizing agents, e.g., nitric acid, sulfuric acid and hydrocyanic acid are formed, but the action of lead tetraacetate on the acid, or of bromine in ether on lead(II) thiocyanate, gives thiocyanogen (“Rhodan”) NCSSCN, a yellow, volatile oil, mp about −3 ◦ C, which polymerizes irreversibly at room temperature to insoluble, brick-red parathiocyanogen (NCS) x . Thiocyanogen reacts with organic compounds like a free halogen. It liberates iodine from iodides. In water it is rapidly hydrolyzed to sulfuric and hydrocyanic acids. When thiocyanic acid is treated with reducing agents, e.g., aluminum and dilute hydrochloric acid, hydrogen sulfide plus carbon plus ammonium chloride are formed. Source: Van Nostrands Encyclopedia of Chemistry, 2005, pages 1613-1614
      1. Reactions of thiocyanic acid
    2. For every 1 mL of dilute 1.57M H2SO4 0.455 grams of barium thiocyanate dihydrate is needed
      1. Dissolve 15 grams of barium thiocyanate dihydrate in 20 mLs of water and chill the solution
        1. Molar mass of barium thiocyanate dihydrate = 289.5 grams per mole
      2. Combine 32.97 mL of 1.57M H2SO4 with 75 mLs of chilled water
        1. ​​​​​​​M1V1=M2V2
          1. ​​​​​​​(1.57M)(33mL)=M2(75mL)
          2. M2 = 0.69 M
        2. ​​​​​​​Final thiocyanic acid concentration = 1.38M (assuming no rinsing so it will be lower than this IRL)
      3. Combine solutions and filter out barium sulfate. Final molarity of thiocyanic acid (not accounting for rinsing) is 1.38M. Solution must be kept cold!
      4. Combine with bismuth subcarbonate
        1. ​​​​​​​Molar mass of bismuth subcarbonate = 509.9685 grams per mole
        2. Stoichiometric amount of bismuth subcarbonate = 26.42 grams
        3. Use 10 grams of (BiO)2CO3 so that the thiocyanic acid is in excess
Tuesday, October 20, 2020
  1. Synthesis of Thallium(I) Chlorate and Uranyl Chlorate
    1. Molar Mass of Barium Chlorate Monohydrate = 322.24 grams per mole
    2. 1.02 grams of thallium converted into thallium sulfate 
      1. 204.3833 grams per mole so 0.0049906230 moles
      2. Tl2SO4 + Ba(ClO3)2 → BaSO2(s) + 2TlClO3
      3. 0.0049906230 moles Barium Chlorate Monohydrate = 1.61 g
    3. 2 grams of uranyl sulfate trihydrate 
      1. 420.138 grams per mole so 0.004760 mols 
      2. UO2SO4 + Ba(ClO3)2 → BaSO2(s) + UO2(ClO3)2
      3. 0.004760 mols Barium Chlorate Monohydrate = 1.53 g
      4. The solid is unstable and readily decomposes
Sunday, October 18, 2020
  1. Synthesis of Bismuth Thiocyanate
    1. 1.57 M H2SO4 = 0.00157 moles per mL
    2. Barium thiocyanate dohydrate = 289.53 grams per mole
      1. For every 1 mL of dilute H2SO4 0.455 grams of barium thiocyanate dihydrate is needed
Tuesday, October 13, 2020
  1. Synthesis of Potassium Cobalticyanide
    1. Cobaltous Cyanide Co(CN)2 → Potassium Cobaltocyanide K4[Co(CN)6] → Heat Solution in Air → Potassium Cobalticyanide K3[Co(CN)6]
      1. Mass of cyanide bottle (full) + lid + label:
        1. 53.62, 53.65, 53.61, 53.64, 53.61, Average = 53.626
      2. Mass of cyanide bottle (empty) + lid + label:
        1. 49.69, 49.70, 49.68, 49.70, 49.70, Average = 49.694
      3. Total mass of potassium cyanide = 3.932, 0.06038 moles
        1. Molar mass of potassium cyanide = 65.12 grams / mole
      4. ​​​​​​​For every 1 mole of cobalt 6 moles of cyanide are needed so 0.06038/6= 0.010063472 moles of Co2+​​​​​​​
        1. 0.010063472 moles of CoCl2•6H2O (237.93g/mol) = 2.394 grams
    2. Nickel Cobalticyanide Ni3[Co(CN)6]2
      1. Nickel Chloride Hexahydrate Molar Mass = 237.69 g/mol
      2. For every mole of Co2+ 3 moles of Ni2+ are needed so 0.010063472 x 3 = 0.030190416 moles = 7.18 grams of NiCl2•6H2O needed
Friday, October 9, 2020
  1. Antimony(III) Sulfide By Union Of The Elements
    1. Atomic mass of antimony = 121.76 grams per mole 
    2. Atomic mass of sulfur = 32.065 grams per mole
      1. 20.59 grams of antimony = 0.169103153745 moles
      2. 3 molar equivalents of sulfur = 0.5073094612352168 moles
      3. Mass of sulfur needed = 16.27 grams of recrystallized sulfur
  2. Antimony(III) Sulfide By Reaction of Potassium Antimonyl Tartrate and Ammonium Thiocyanate
    1. Molar Mass of Ammonium Thiocyanate = 76.12 grams per mole
    2. Molar Mass of Potassium Antimonyl Tartrate Hydrate = 475.02 grams per mole
    3. Reaction: C8H10K2O15Sb2 + 3NH4SCN → Sb2S3 + ?
      1. 15 grams of ammonium thiocyanate = 0.197057 moles
      2. Number of moles potassium antimonyl tartrate needed = 0.197057/3 = 0.06568567 moles
      3. Number of grams potassium antimonyl tartrate needed = 31.20 grams
Saturday, October 3, 2020
  1. Synthesis of Potassium Antimony Tartrate (for Antimony Trisulfide Synthesis)
    1. Equation: 2KC4H5O6 + Sb2O3 → C8H10K2O15Sb2
    2. 41.99 grams of potassium bitartrate
      1. Molar mass = 188.177 grams per mole
      2. Total amount = 0.223141 moles 
    3. Antimony(III) oxide
      1. Molar mass = 291.518 grams per mole
      2. Amount needed = 0.1115704 moles
      3. Mass Needed = 32.52480 grams
  2. Synthesis of Crystalline Antimony Trisulfide
    1. " the prolonged heating at a high temperature of potassium antimonyl tartrate with a solution of ammonium thioeyanate."

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