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- Posts: 221
- Joined: Thu Mar 03, 2011 8:05 pm
- Location: New Hampshire, USA
Sorry, but I've been offline for awhile. Have you had any success?
Don
LGC Standards
Discussions about sample preparation: extraction, cleanup, derivatization, etc.
xie wrote:
Hi jdjaw,
I'm interested in your method of Diazomethane generation as I'm trying to get Method 515.4 going. Currently we use 515.1. Can you tell me specifically how much Diazald you put in the inner tube? Is that a solution or just the powder? The only other chemicals needed are MeOH, NaOH, MTBE? How many samples can you esterify with the amount produced? Do you have a part number for the apparatus? Much appreciated.
Looking forward to your response...
jdjaw wrote:xie wrote:
Hi jdjaw,
I'm interested in your method of Diazomethane generation as I'm trying to get Method 515.4 going. Currently we use 515.1. Can you tell me specifically how much Diazald you put in the inner tube? Is that a solution or just the powder? The only other chemicals needed are MeOH, NaOH, MTBE? How many samples can you esterify with the amount produced? Do you have a part number for the apparatus? Much appreciated.
Looking forward to your response...
The diazald we do not measure out. We just make sure there is excess in the inside part of the apparatus. My understanding is that after the generation you want there to still be powder in the inside bulb. 2 mL of MeOH goes into the inside portion of the appartus with the diazald. 5 mL of MTBE goes into the outside tube. After everything is sealed 12-14 drops of 6N NaOH is added through the septa at the top slowly, about 1 drop every 5 seconds. We let the reaction go for 30 minutes. The part number is 281155 from wheaton.
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