Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
Author: Subject: Strange white powder while making Phthalic Acid
Housane
Hazard to Others
***




Posts: 127
Registered: 3-9-2018
Location: Worcester, England
Member Is Offline

Mood: Let’s make

[*] posted on 30-3-2021 at 10:53
Strange white powder while making Phthalic Acid


I've just tried to replicate Nile reds Phthalic acid video at 1/2 scale and when pouring in the NaOH I got 2 layers instantly and then after reflux I get an orange layer and some powdery white solid, any idea what may have happened?



Green QD's so far

Feel free to correct grammar or incorect knknowledge. We are all learning.
View user's profile View All Posts By User
Syn the Sizer
National Hazard
****




Posts: 591
Registered: 12-11-2019
Location: Canada
Member Is Offline


[*] posted on 30-3-2021 at 11:25


My guess is there was some impurities in the solution. Possibly still polymer which is probably the orange colour. The powder could also be cause by that as well.
Do you know what alcohol was estered with the phthalic acid as the plasticizer?
To be honest, it is fairly cheap to buy phthalic anhydride pure. Are you just doing this for fun or are you having a hard time sourcing it?
View user's profile View All Posts By User
DraconicAcid
International Hazard
*****




Posts: 4278
Registered: 1-2-2013
Location: The tiniest college campus ever....
Member Is Offline

Mood: Semi-victorious.

[*] posted on 30-3-2021 at 11:49


Would the orange layer be the alcohol that you're hydrolyzing off the phthalate ester?



Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
View user's profile View All Posts By User
Housane
Hazard to Others
***




Posts: 127
Registered: 3-9-2018
Location: Worcester, England
Member Is Offline

Mood: Let’s make

[*] posted on 30-3-2021 at 13:00


Alcohol was isopropanol and I didn't have a soxhlet so it was just refluxed In a flask to extract it



Green QD's so far

Feel free to correct grammar or incorect knknowledge. We are all learning.
View user's profile View All Posts By User
Housane
Hazard to Others
***




Posts: 127
Registered: 3-9-2018
Location: Worcester, England
Member Is Offline

Mood: Let’s make

[*] posted on 30-3-2021 at 13:02


Is it worth repeating without the 2nd reflux as I got the 2 layers as described in the video?



Green QD's so far

Feel free to correct grammar or incorect knknowledge. We are all learning.
View user's profile View All Posts By User
DraconicAcid
International Hazard
*****




Posts: 4278
Registered: 1-2-2013
Location: The tiniest college campus ever....
Member Is Offline

Mood: Semi-victorious.

[*] posted on 30-3-2021 at 13:12


If the gloves you're starting with contain di(ethylhexyl)phthalate, then you would have ethylhexanol as a byproduct, which would be upper orange layer.



Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
View user's profile View All Posts By User
Syn the Sizer
National Hazard
****




Posts: 591
Registered: 12-11-2019
Location: Canada
Member Is Offline


[*] posted on 30-3-2021 at 15:42


That would make sense. I have never synthesized the acid from gloves, I just buy it.
View user's profile View All Posts By User
Housane
Hazard to Others
***




Posts: 127
Registered: 3-9-2018
Location: Worcester, England
Member Is Offline

Mood: Let’s make

[*] posted on 30-3-2021 at 16:56


Ok, thanks for the help I’m going to try without 2nd reflux again.

Do you think the white is waste as well or product, it has a minty kinda air freshener smell




Green QD's so far

Feel free to correct grammar or incorect knknowledge. We are all learning.
View user's profile View All Posts By User

  Go To Top