Chemistry Reference
A collection of syntheses.

Anhydrous Magnesium Sulfate from Epsom Salts

  • Epsom salts => Magnesium Sulfate Heptahydrate
  • Dry in a thin layer; stirring often
  • heat to 150C (300F) for 1 hours => monohydrate
  • heat to 200C (390F) for 30 min => anhydrous
  • heat to 250C (480F) for 30 min => just to be sure
  • yield: 49% weight basis; nearly quantitative on a molar basis
  • 120.366 g/mol (anhydrous)
  • 246.47 g/mol (heptahydrate) (Hippie3 2003)

Nitric Acid

Sulfuric Acid + Potassium Nitrate <-> Potassium Bisulfate + Nitric Acid

  • 500mL flask
  • 100mL water
  • 202g KNO3
  • 116mL 93% Sulfuric Acid
  • collect all distillate (~163mL; ~50% nitric acid)
  • stop after reaction flask begins to foam excessively
  • immediately clean all glassware
  • redistill nitric acid
    • everything over 118 C is azeotropic 68% (Doug’s Lab 2015)

Copper Catalysts for Primary Alcohol Dehydrogenation

Cu/Al2O3 + Urea

approximately 23% wt. Cu with 41 sq.m/g Cu surface area

  • 20.6g (0.110 mol) of Cu(NO3)2 is added to 2L 1.2M Urea solution in a 3L flask
  • 20g of 200 mesh gamma-alumina is added
  • the solution is heated to 90-95C with constant stirring for 7+ hours or until pH=7.5
  • the solution is filtered; washed with dH2O; calcined at 400C for 24 hrs
  • the resulting catalyst is reduced with flowing hydrogen at 250C for 5 hrs
    • alternatively, catalyst can be activated in situ with primary alcohol

Sivaraj and Kantarao (1988)

Cu/SiO2 + Ammonia

approximately 17% wt Cu with 41 sq.m/g Cu surface area

  • 11.3g Cu(NO3)2*3H2O is dissolved in 150ml dH2O
  • 18ml of 28% Ammonia soln. is added over 30 min with stirring
  • 12g of fumed SiO2 is added
  • stir for 4hrs at 35C
  • heat soln to 90C for 2 hrs or until pH reaches 6-7
  • filter and wash with dH2O
  • dry overnight at 120C
  • calcine at 450C for 4 hrs (Dong et al. 2016)

Cu/SiO2 + Urea

19% wt Cu; 18 sq.m/g Cu surface area

  • 11.3g Cu(NO3)2*3H2O is dissolved in 150ml dH2O with 28.2g urea
  • 12.0g fumed SiO2 is added under stirring
  • heat to 90C until pH reaches 6-7
  • filter soln; wash with dH2O
  • dry overnight at 120C
  • calcine at 450C for 4 hrs (Dong et al. 2016)

Carbon Dioxide Generator

\(MgSO_{4}\cdot7H_{2}O + 2NaHCO_{3} \to 2NaSO_{4} + Mg(OH)_{2} + 8H_{2}O + 2CO_{2}\)

For every liter of \(CO_{2}\) (45mmol; 1.98g) required, mix 5.54g epsom salts (magnesium sulfate heptahydrate) with 1.89g sodium bicarbonate.

Chloroform Synthesis

Assuming calcium hypochlorite is roughly twice the enthalpy of formation of the sodium variety (twice the number of hypochlorite groups), the total enthalpy change for this synthesis is 670 kJ/mol chloroform.

For every mole of chloroform produced (120g; 81 ml), approximately 2kg (110 mol) of ice will melt. I believe the hth pool chlorine product uses pre-hydrated hypochlorite, so the heat of solution isn’t an issue. If anhydrous hypochlorite is used, an additional 940 kJ/mol will be evolved.

Procedure

For each mole (81ml) of chloroform produced:

  • 2kg of ice is added to a suitable glass or plastic container
  • 215g of pure calcium hypochlorite is added as 370g of 58% hypochlorite pool chlorinator
  • A few hundred mLs of water may be needed to dissolve the hypochlorite
  • 1 mol of butanone (90ml), acetone (74ml), 95% ethanol (61ml), or isopropanol (76ml) is added over the course of a few minutes with stirring

Standard enthalpy of formation

  • butanone = -273.3 kJ/mol
  • chloroform = -134.3 kJ/mol
  • sodium hypochlorite = -347.1 kJ/mol
  • calcium hypochlorite < -150 cal/g (-90 kJ/mol)
  • propionic acid = -510.8 kJ/mol

Heat of solution

  • calcium hypochlorite = 150 kcal/mol (627 kJ/mol)

Enthalpy change of fusion

  • water = 6.01 kJ/mol

Heat capacity

  • water = 75.4 J/(mol K)

Copper Barium Chromite

  • 12.6g ammonium dichromate (100 mmol)+ 33 ml H2O
  • 25g copper II sulfate pentahydrate (100 mmol) + 60ml H2O
  • 42ml 10% ammonia
  • 2g barium carbonate (10mmol) + nitric acid

Ammonia

  • 200ml water
  • 90g urea
  • 120g sodium hydroxide
  • bubble through 100ml water
  • heat for 3 hours

36.8g 51g ammonia produced

Trimethyl Borate

Make Wildfire | NurdRage

  • 200g borax
  • 650ml methanol
  • slowly add 100g sulfuric acid with reflux condenser in place
  • fractionally distill methanol-TMB azeotrope at 54C over ~10 hours

Methyl Borate | Sciencemadness (u/Magpie)

  • 50g boric acid (calcined to boric oxide)
  • 183ml methanol

Sources

Log

References

Dong, Xiaohuan, Xiangang Ma, Hengyong Xu, and Qingjie Ge. 2016. “Comparative Study of Silica-Supported Copper Catalysts Prepared by Different Methods: Formation and Transition of Copper Phyllosilicate.” Catalysis Science & Technology 6 (12): 4151–8. https://doi.org/10.1039/C5CY01965F.

Doug’s Lab. 2015. “Nitric Acid Day!” https://www.youtube.com/watch?v=mG4OaPTWPOA.

Hippie3. 2003. “Making Your Own Dessicant from Epsom Salts.” Mycotopia. https://mycotopia.net/archives/discus/messages/5/31575.html?1061997827.

Sivaraj, Ch., and P. Kantarao. 1988. “Characterization of Copper/Alumina Catalysts Prepared by DepositionPrecipitation Using Urea Hydrolysis: I. Nitrous Oxide Decomposition and Reaction of Ethanol.” Applied Catalysis 45 (1): 103–14. https://doi.org/10.1016/S0166-9834(00)82396-9.