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This week at the lab I tried to synthesize [Co(Me)(py)(DMG)2] this is a summary of the procedure:

Day 1:
 
  - Dissolved 2.7g of DMG in 100mL of EtOH with heat and stirring. 
  - Added 2.5g of CoCl₂·6H₂O, forming a dark green solution. 
  - Added 2mL of py and let it cool to room temperature. 
  - Passed air through the mixture for 30 minutes, turning the solution light brown (three phases were observed: a dark brown layer on top, a light brown suspension in the middle, and a small dark green phase at the bottom). 
  - Filtered under vacuum and washed with water, then ethanol, and finally ether, obtaining a brown powder. 

---

- **Day 2** 

  - Assembled a system with a Liebig condenser and a 2-neck round bottom flask, purging it with nitrogen for 5 minutes. 
  - Added 10mL of MeOH and deoxygenated it for another 5 minutes. 
  - Added 0.8g of the compound obtained on Day 1 (presumably [Co(Cl)(py)(DMG)₂]) and 2mL of methyl iodide, forming a dark-colored solution. 
  - Slowly added 0.4g of NaBH₄. Upon addition, an orange layer formed on top but disappeared once the NaBH₄ was consumed. 
  - Added a small quantity of water to precipitate the product. 
  - Filtered the solution, obtaining a brown-orange powder. This brown was different from the one obtained on Day 1 but still brown (maybe incomplete or partial reaction?) 

  - Repeated the procedure of day 2 step by step, starting with 0.8g of [Co(Cl)(py)(DMG)₂] provided by another lab mate (which appeared identical to the compound I obtained on day 1). This time, the expected orange powder, likely [Co(Me)(py)(DMG)₂], was obtained

I guess I did something wrong on day 1. The only different step on day 2 from the first try to the second try was that on the second the stirring was more intense (not a lot tho).

Any ideas? If cobalt had not been oxidized on day 1 it should've remained green instead of brown right?

I'd like to achieve something like that:

KI + KIO3 + HCl -> KI + I2 (+ HCl + KCl + H2O)

Focusing only at KI and KIO3
How can i count how many KI in the reaction need to be to "zeroed" KIO3? (and what amount of I2 be created)
From what amount the more grams of KI i add the more will be left untouched
Suppose we have an unlimited amount of HCl (focusing only on KI and KIO3, I2)

Hi There!

So I make calcium soap, i want to check the free alkali / free acid of the soap.
I have checked with method from AOCS using titration with ethanol as the solvent. But i got problem, because calcium soap can not dissolve in ethanol. therefore, i'm not sure whether my analysis is true or not. Is there any other method to check the free alkali/free acid for Calcium Soap?