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pressure drop to zero upon mixing large percentage of ACN
Discussions about HPLC, CE, TLC, SFC, and other "liquid phase" separation techniques.
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pressure drop to zero upon mixing large percentage of ACN with buffer in different HPLC apparatuses. and i don't know the problem.
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- tom jupille
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What buffer and what concentration? Many buffers have limited solubility in ACN and may precipitate.
-- Tom Jupille
LC Resources / Separation Science Associates
tjupille@lcresources.com
+ 1 (925) 297-5374
LC Resources / Separation Science Associates
tjupille@lcresources.com
+ 1 (925) 297-5374
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For example with phosphate buffer. Than it may already have blocked your column and, depending what HPLC system, the pistons and valves of your pump head are affected.
Gerhard Kratz, Kratz_Gerhard@web.de
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but if it precipitate , i think the pressure will rise, but the pressure drops and didn't rise.
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Did you check your pump head for leakage?
Gerhard Kratz, Kratz_Gerhard@web.de
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Are you doing online mixing, or pumping premixed mobile phases ?
Do you degas either mobile phase component ?, if so, how ?
Is the pressure drop rapid and sudden, or gradual, does the pressue fluctuate while it is dropping.
The more you tell us, the more we can help you.
Peter
Do you degas either mobile phase component ?, if so, how ?
Is the pressure drop rapid and sudden, or gradual, does the pressue fluctuate while it is dropping.
The more you tell us, the more we can help you.
Peter
Peter Apps
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Hello
As pressure problems can be result of different things please paste chromatogram with pressure profile (it is really important to see profile as it helps with diagnostics).
Also please put information below:
-pump type: quat/isocratic/binary
-degasser info
-gradient timetable
-pump parameters (compression, stroke etc)
Without those information you can't expect quick and clear answer.
Regards
Tomasz Kubowicz
As pressure problems can be result of different things please paste chromatogram with pressure profile (it is really important to see profile as it helps with diagnostics).
Also please put information below:
-pump type: quat/isocratic/binary
-degasser info
-gradient timetable
-pump parameters (compression, stroke etc)
Without those information you can't expect quick and clear answer.
Regards
Tomasz Kubowicz
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- tom jupille
- Site Admin
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- Joined: Wed Aug 11, 2004 4:55 pm
Unless some of the precipitate prevents a check valve from sealing.but if it precipitate , i think the pressure will rise, but the pressure drops and didn't rise.
At this point, unless you give us some more information, anything we can say is pure guesswork.
-- Tom Jupille
LC Resources / Separation Science Associates
tjupille@lcresources.com
+ 1 (925) 297-5374
LC Resources / Separation Science Associates
tjupille@lcresources.com
+ 1 (925) 297-5374
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- Posts: 4
- Joined: Sat Aug 22, 2015 6:56 am
i am doing online mixing... and i degas all mobile phase component... and the pressure drop rapidly and suddenly and doesn't fluctuate while dropping...Are you doing online mixing, or pumping premixed mobile phases ?
Do you degas either mobile phase component ?, if so, how ?
Is the pressure drop rapid and sudden, or gradual, does the pressue fluctuate while it is dropping.
The more you tell us, the more we can help you.
Peter
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- Posts: 4
- Joined: Sat Aug 22, 2015 6:56 am
the HPLC is waters. the pump type is Quaternary, and it's isocratic system.the stroke volume is 100 μl , the reservoirs to sparge is 0 ml/min for the four channels. pump mode is isocratic accelerate to 10 ml/min in 2 min. the degas mode is on. the pressure drops suddenly to zero...Hello
As pressure problems can be result of different things please paste chromatogram with pressure profile (it is really important to see profile as it helps with diagnostics).
Also please put information below:
-pump type: quat/isocratic/binary
-degasser info
-gradient timetable
-pump parameters (compression, stroke etc)
Without those information you can't expect quick and clear answer.
Regards
Tomasz Kubowicz
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- tom jupille
- Site Admin
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- Posts: 4978
- Joined: Wed Aug 11, 2004 4:55 pm
This is like playing "20 questions"
You still haven't told us what buffer and what concentration.
A useful experiment is to mix your buffer with acetonitrile in various ratios (1:1, 4:1, 9:1 ACN:buffer) in test tubes and hold them up to the light to check for "sparklies" indicative of precipitation.

You still haven't told us what buffer and what concentration.
A useful experiment is to mix your buffer with acetonitrile in various ratios (1:1, 4:1, 9:1 ACN:buffer) in test tubes and hold them up to the light to check for "sparklies" indicative of precipitation.
-- Tom Jupille
LC Resources / Separation Science Associates
tjupille@lcresources.com
+ 1 (925) 297-5374
LC Resources / Separation Science Associates
tjupille@lcresources.com
+ 1 (925) 297-5374
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- Joined: Tue Aug 17, 2004 7:59 pm
Could also be that you're using ruby/sapphire check valves and that one (or both) are floating when they see the ACN conc. jump. Ceramic check valves are better for systems using lots of ACN.
Thanks,
DR

DR

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