What I would really like to do is start amassing equipment needed for some routine quantitative analyses. I've done many titrations in my life and volumetric analysis is what I know best, but I'd like if possible to develop methods that are more specific and more apt to automation. Titration with coulometric generation of reagents seems like it might be a feasible amateur project.

I've done volumetric analysis at home. For fun. Burets are fairly easy to get online ($20 will get you a serviceable 50 mL model) but availability of pure reagents for use as "primary standards" (for standardization of volumetric reagent solutions) is nonexistent to the private citizen. I taught myself to prepare and recrystallize a number of inorganic compounds in order to do my work.

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For alkalimetric titrations I used solutions of NaOH made from hardware-store lye, and standardized with the following:

Oxalic acid dihydrate (recrystallized commercial Daly's oxalic acid)

Sulphamic acid (recrystallized TileLab sulfamic acid)

Potassium tetroxalate dihydrate (prepared from oxalic acid and potassium carbonate and recrystallized) (this compound is less satisfactory as a standard)

Acidimetric titrations are a bit more work to prepare for. HCl solutions made from hardware-store muriatic acid are easily prepared, but standardization is more difficult. I had best luck with:

Sodium tetraborate decahydrate (prepared by recrystallization of commercial borax at 55 °C, and stored in a container with a high humidity to suppress efflorescence)

Sodium carbonate (prepared by baking out sodium sesquicarbonate prep'd by crystallizing a hot NaHCO3 solution)

What I really would have liked were some alternatives for acidimetric standards. "Tris" base, tris(hydroxymethyl)aminomethane, is a good one but not easily made at home! Another I found out about was 4-aminopyridine, also inaccessible. I tried and failed to synthesize potassium bicarbonate by passing CO2 gas into a K2CO3 solution.

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