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Componente
Informacion TecnicaThe Wrench
Vol. 6 Issue 1
Winter 2009
Problems with Peak Shape
Poor peak shape can cause a loss of resolution between adjoining peaks, it can lead to poor injection to injection reproducibility, or it may cause an injection to fail method acceptance criteria. Poor peak shape includes issues such as tailing, fronting, split peaks, and shouldered peaks.
The causes of poor peak shape are varied. They include everything from poorly developed methods, to contaminated columns or in other parts of the system, to extra system volume or poor system connections.
The following chart covers some of these common problems and possible remedies.
|
Problem |
Indication |
Cause |
Solution |
|
Peak Tailing
|
Initial Peaks fronting |
Too strong a sample solvent |
Samples should be dissolved in mobile phase or solvent weaker than mobile phase |
|
|
|
|
|
|
|
All peaks fronting |
Column overload |
Reduce injection volume |
|
|
|
|
Reduce sample concentrations |
|
|
|
|
Use a column with a larger i.d. |
|
|
|
|
|
|
Split Peaks
|
|
Void or channel in column |
Replace column |
|
|
|
Dirty column frit |
Replace frit |
|
|
|
|
|
|
|
|
Dirty Column |
Back flush or replace |
|
|
|
|
|
|
|
|
Sample solvent not suitable for use with mobile phase |
Ensure that sample and mobile phase solvents are compatible – make any necessary adjustments |
|
|
|
|
|
|
Peak Shoulders
|
Shoulder on 1 or 2 peaks |
Mobile phase is at a pH near the pKa of the analyte |
Adjust pH of mobile phase to be at least 2 pH units away from the pKa of the sample analytes
Adjust mobile phase to separate the 2 peaks |
|
|
|
|
|
|
|
|
|
|
|
|
Shoulder on all peaks |
Dirty Inlet frit |
Replace |
|
|
|
|
|
|
|
|
Dirty Guard Column |
Replace |
|
|
|
|
|
|
|
|
Dirty Column |
Back flush or replace |
Top of page
Historical Wrench Articles
| Title | Issue | |
| Plunger Seals | Vol. 2 Issue 1 | Plunger Seal .pdf |
| HPLC Preventative Maintenance |
Vol. 2 Issue 2 |
Prevt. Maint .pdf |
| System Backpressure |
Vol 2 Issue 3 |
System Backpressure .pdf |
| Choosing a Lamp Vendor |
Vol 3 Issue 1 |
Lamp choices .pdf |
| Instrument Qualification and Aftermarket Parts |
Vol.3 Issue 2 |
IQ and aftermatket .pdf |
| Material Solvent Compatibility |
Vol.4 Issue 1 |
Solvent Compatibility .pdf |
| Mobile Phase Buffers |
Vol.4 Issue 2 |
Mobile Phase Buffers .pdf |
| Sample and Mobile Phase Filtering |
Vol.5 Issue 1 |
Filtering.pdf |
Top of Page
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