Product Glycerin Peak
Splitting
Troubleshooting
Agilent GC 8890
Product Glycerin Peak Splitting
Troubleshooting
• Problem Statement: Found multiple noises and splitted
product glycerin peak after analysis.
• Initial Rectification: As we run Crude glycerin samples on
same column therefore it is suggested to replace new GC
column as old one get contaminated by impurities in crude
glycerin which is not removing even after recommended
washing/cleaning methods.
Product Glycerin Peak Splitting
Troubleshooting
• Column Replacement: On 14-March-2025 new column was
installed by HA Shah representative “Ajel Azeem” and
troubleshooting training was also conducted.
• Batch Analysis Carried Out: To check the performance of
column run of Batch No.1309 was carried out but the
subjected issue was not resolved, as splitted Glycerin peak
was obtaining as before.
Product Glycerin Peak Splitting
Troubleshooting
• Sample was run as per method, but it was suggested by Ajel
to vary the injection volume to check the behavior of Glycerin
peak. For this concern 1µL (as per method),2µL, 3µL and 5µL
injection volume runs were carried out.
Product Glycerin Peak Splitting
Troubleshooting
• 1µL run (Method injection volume)
Product Glycerin Peak Splitting
Troubleshooting
• 2µL run
Product Glycerin Peak Splitting
• 3µL run Troubleshooting
Product Glycerin Peak Splitting
• 5µL run Troubleshooting
Product Glycerin Peak Splitting
Troubleshooting
• It is observed that peak splitting increases with increase in
injection volume.
• It is requested by Ajel to provide him chromatograms of
Standard and Methanol before he conclude anything. So,
analysis performed as requested.
Product Glycerin Peak Splitting
Troubleshooting
• 3 runs of System Suitability (Standard), 2 runs of Methanol,
and 1 run of Blank (Air) were carried out for this.
Product Glycerin Peak Splitting
Troubleshooting
•1
st
run of System Suitability
Product Glycerin Peak Splitting
Troubleshooting
•2
nd
run of System Suitability
Product Glycerin Peak Splitting
Troubleshooting
•3
rd
run of System Suitability
Product Glycerin Peak Splitting
• Peak View of Troubleshooting
System Suitability
DEG EG
Internal Std. Glycerin
Product Glycerin Peak Splitting
•1
st
run of MethanolTroubleshooting
Product Glycerin Peak Splitting
•2
nd Troubleshooting
run of Methanol
Product Glycerin Peak Splitting
• Blank run Troubleshooting
Product Glycerin Peak Splitting
• Batch No.1407 Troubleshooting
Run-01
Product Glycerin Peak Splitting
• Batch No.1407 Troubleshooting
Run-02
Product Glycerin Peak Splitting
Troubleshooting
• QC Lab Analysis Summary for Troubleshooting
Method recommends use of Primary Standards which is USP Standards, we use secondary
standards (Merck) brand, although results achieved were meeting success criteria with given
relative retention times and resolution requirements as mentioned in method.
No peak splitting and noises were found in system suitability run.
2 different batches were run for this troubleshooting and both of their runs were splitting and
noises were found as well.
Same solvent (Methanol) used for the preparation of samples and Standards (System Suitability).
Same syringe used for Standards and Samples but after rinsing with methanol and respective
solution after every run.
All 3 System Suitability Runs were meeting success criteria.
