Chromatography Forum

Please any one suggest a method suitable for Acetic acid GC-FID with HSS injection.

For API Residual solvents.

Hi try out the follwing method which we uses for quantifying acetic acid in our API

STANDARD PREPARATION:

Weigh around 100mg of formic acid in 100mlvolmetric flask and make up to mark by using diluent. Transfer 5ml in to the head space vial and crimp it with cap.

SAMPLE PREPARATION:

Weigh around 100mg of sample and transfer in to head space vial. Add 5ml of diluent and crimp it with cap. Prepare the sample in duplicate.

DILUENT:
1% p-toluenesulphonic acid in ethanol

HEAD SPACE PERAMETERS:
Oven: 60’C
Loop: 120 ‘C
Transfer line: 120 ‘C
Vial equilibration: 15.00 min
Pressurization: 0.10 min
Loop fill: 0.50 min
Loop equilibration: 0.50 min
Injection: 1.00 min
GC cycle time: 15.00 min
Shake: High

OVEN:
Initial temp. : 40 ‘C
Hold time : 4.20min
Equilibration time: 3.00min
Ramp: 40 ‘C/min
Final temp. : 200 ‘C
Hold time: 2.00min

Try this out and reply if u found any problem

Two problems that I anticipate are that there is no column, and no calibration.

Peter

We need to sticky a thread titled "WOW L@@K - THE ANSWER TO ALL YOUR ACETIC ACID QUESTIONS - HOT!!" and then when you click it gives you information about LC and IC