Help with Performic H2SO4 Hydrolysis please

[Mr_Reflux]

Swim wants to process 195g (approx. 180mls) iso-safrole using the modified performic. All steps seem standard except when it gets to the hydrolysis of the glycol. Using TFSE, TS11 and other sources  swim found that the only consistency was that 15% H2SO4 should be used. The actual amount of H2SO4, length of time, reflux or not, use methanol or not and the temperature ALL varied. Swim would have thought that this would have been standardized by now considering the peracid popularity.
So Swim is going to proceed with NO methanol, strong overhead stirring, no reflux, 15% H2SO4, 2 hours exact with preheated 15% H2SO4 and cooling with ice. But the question is how much H2SO4, if swim proceeds as above, to give the best yield.
And just another quickie. Before the glycol is hydrolyzed does it need washing. Swim separates the glycol after the 20 hour reaction but does not bother to extract with solvent. If so is it just a simple saturated sodium bicarb wash then straight into the 15%H2SO4?

Thanks

[RoundBottom]

this is from labtop's detailed writeup at the top of the newbie forum

Post 210298

(LaBTop: "Re: DETAILED METHODS for NON-CHEMISTS The Sequel !", Newbee Forum).

ISO: 125.0g (111.6mL)
Sodium Bicarb: 38.5g   
DCM: 510.3g (385.0mL)
      
Formic 88%: 194.8g (165.0mL)
H2O2 35%: 118.0g (106.1mL)

H2SO4 15%: 1370.0g 
(H2SO4 99%): 209.7g (114.0mL)
(H2O): 1160.3g (1160.3mL)

[LaBTop]

Many, many bees around here should learn one important simple labtechnique:
Thin Layer Chromatography (TLC, do a SEARCH on TLC here or at Rhodium.ws !).

TEST your isosafrole FIRST with TLC!
See if you get a more than 98% SINGLE spot, at a different place on the glass or paper plate, compared to sassafras and safrole!
You already checked the boiling points and any other here available data of your freshly made new compounds?
Because you could have ended up with still just Safrole again due to any mistake made, so use TLC with 3 different starting drops:
1. your original Sassafras oil,
2. your distilled/freezed-out Safrole
3. your supposed isosafrole!

If not done all of this first, rethink your labtechniques or/and your attitude, before you start doubting the methods proposed here!
Always doubt yourself first, you prolly make more common mistakes than the combined Hive resources.

TLC should be performed on all important steps in a first synthesis!
Combined with chemical data checks on all compounds.
This will also give any posts asking for help a MUCH heavier impact, and will convince the readers that you've done all you can to pinpoint the problem yourself FIRST!
You then will automatically receive much better answers.

Most, if not all problems brought to our attention here, are caused by sloppy labtechniques, hidden behind semi-scientific chemspeak from fresh members who have caught on to the words we use, but not yet to the skills needed.
The real cause is ofcourse :
More HASTE, less SPEED! LT/   : Take your time, don't do time.