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I will be treating carbon in 3 steps under reflux and I would really appreciate some suggestions, tips and advice on getting a proper and SAFE setup in the lab. I have at my disposal a fume hood and standard laboratory glassware.
Treatment 1: 20g carbon treated with 100mL 65% Nitric Acid under reflux for 24 hrs.
This is what I came up with, a 250mL round bottomed flask connected to a standard Liebig condenser held in the vertical position with cold water entering the bottom and hot from the top. Would a different condenser be more appropriate? I am not sure whether or not I should stopper of my condenser?
I might be able to get a round bottom flask heating mantle to use as the heat source if not then maybe an oil bath and a hot plate.
Treatment 2: 0.8 g of the Nitric Acid treated carbon (Treatment 1) to be further treated with 5mL Thionyl Chloride (SOCl2) and 5mL Benzene for 24hrs
The MSDS for Thionyl chloride says that upon contact with water or humid air, it releases HCl and SO2. This is a huge concern for me. What precautions should I take?
Should I vary my setup than the round bottom flask, heating mantle/hot plate and condenser setup? Also should I cap the stopper the top of the condenser?
Treatment 3: 0.8g of the carbon from Treatment 2 to be further treated with 2.60mL of Ethylene Diamine and 6mL of Chloroform under reflux for 48hrs.
Ethylene Diamine has a low flash point of 34 degC
Vary Setup ?
If want to scale up the treatments, specifically treatment 2 and 3, by using 20g of carbon rather than 0.8g and increasing the quantity of the other chemicals. What precautions should I take into consideration?
EDIT: After each treatment the carbon would be properly washed to remove any trace chemicals and dried to remove any moisture trapped.
Treatment 1: 20g carbon treated with 100mL 65% Nitric Acid under reflux for 24 hrs.
This is what I came up with, a 250mL round bottomed flask connected to a standard Liebig condenser held in the vertical position with cold water entering the bottom and hot from the top. Would a different condenser be more appropriate? I am not sure whether or not I should stopper of my condenser?
I might be able to get a round bottom flask heating mantle to use as the heat source if not then maybe an oil bath and a hot plate.
Treatment 2: 0.8 g of the Nitric Acid treated carbon (Treatment 1) to be further treated with 5mL Thionyl Chloride (SOCl2) and 5mL Benzene for 24hrs
The MSDS for Thionyl chloride says that upon contact with water or humid air, it releases HCl and SO2. This is a huge concern for me. What precautions should I take?
Should I vary my setup than the round bottom flask, heating mantle/hot plate and condenser setup? Also should I cap the stopper the top of the condenser?
Treatment 3: 0.8g of the carbon from Treatment 2 to be further treated with 2.60mL of Ethylene Diamine and 6mL of Chloroform under reflux for 48hrs.
Ethylene Diamine has a low flash point of 34 degC
Vary Setup ?
If want to scale up the treatments, specifically treatment 2 and 3, by using 20g of carbon rather than 0.8g and increasing the quantity of the other chemicals. What precautions should I take into consideration?
EDIT: After each treatment the carbon would be properly washed to remove any trace chemicals and dried to remove any moisture trapped.