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Troubleshooting Problems With Peak Shape

This document discusses troubleshooting problems with peak shape in chromatography. It describes several issues that can cause peak tailing, split peaks, or peak fronting such as column contamination, blocked frits, sample overload, or solvent incompatibility. It provides possible causes and recommendations for prevention or solutions such as using purer stationary phases, changing mobile phase conditions, cleaning or replacing the column, optimizing temperature, or modifying the sample.

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Mubarak Patel
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104 views

Troubleshooting Problems With Peak Shape

This document discusses troubleshooting problems with peak shape in chromatography. It describes several issues that can cause peak tailing, split peaks, or peak fronting such as column contamination, blocked frits, sample overload, or solvent incompatibility. It provides possible causes and recommendations for prevention or solutions such as using purer stationary phases, changing mobile phase conditions, cleaning or replacing the column, optimizing temperature, or modifying the sample.

Uploaded by

Mubarak Patel
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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8/13/22, 9:34 AM Troubleshooting Problems with Peak Shape

Troubleshooting Problems with Peak Shape


pharmaceuticalsky.com/2022/08/troubleshooting-problems-with-peak-shape.html

Peak Tailing

Possible
Cause Prevention/Solution

Interaction
with active silanols Use
ultra-high purity silica-based stationary
phase

Add
basic mobile phase additive (eg. TEA)

–
not needed with ultra-high purity phases

Chelation
with metal ions in stationary Use
ultra-high purity silica-based stationary
phase phase

Add
basic mobile phase additive (eg. TEA)

–
not needed with ultra-high purity phases

Wrong
mobile phase pH Decrease
mobile phase pH to suppress

silanol
ionization

Increase
buffer concentration.

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8/13/22, 9:34 AM Troubleshooting Problems with Peak Shape

Blocked
frit Reverse
flush the column

Use
in-line filter

Column
void Reverse
flush the column

Replace
the column

Unswept
dead volume Minimize the number of connections

Use
shorter connection tubing

Check
all fittings are tight

Split Peaks

Possible
Cause Prevention/Solution

Contamination
on guard or Remove
guard cartridge and carry out analysis –
analytical column inlet replace guard if necessary

The reverse flush analytical column

For
strongly retained contaminants, try the
regeneration procedure

Replace
column

Blocked
frit Reverse
flush the column

Use
in-line filter

Sample
solvent incompatible with Inject
sample in the mobile phase
the mobile phase

Simultaneous
elution of the Use
sample clean-up prior to injection
second component
Change
selectivity by changing mobile phase or
column phase

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8/13/22, 9:34 AM Troubleshooting Problems with Peak Shape

Column
overloaded Use
higher capacity stationary phase

Increase
column diameter

Decrease
sample amount

Peak Fronting

Possible
Cause Prevention/Solution

Formation
of channels in column Replace
the column

Operate
within recommended pH limits of
the column

Column
overloaded Inject a smaller volume or more dilute
sample solution

Use
higher capacity stationary phase

Sample
solvent incompatible with the Inject
sample in the mobile phase
mobile phase

Low
temperature Increase
column temperature

PEOPLE ALSO READ: What is Ghost Peaks?


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