recycle chromatography
Download
Skip this Video
Download Presentation
RECYCLE CHROMATOGRAPHY

Loading in 2 Seconds...

play fullscreen
1 / 45

RECYCLE CHROMATOGRAPHY - PowerPoint PPT Presentation


  • 228 Views
  • Uploaded on

RECYCLE CHROMATOGRAPHY. Jiri SEVCIK Prague, the Czech Republic. ABOUT. CHARACTERISTICS SEPARATION EFFICIENCY RESOLUTION RECYCLE CHROMATOGRAPHY HW. multi d imensional chromatography SYSTEMS. serial parallel. K D1 <> K D2 <> K Dd. SCHEMATICS of recycle chromatography.

loader
I am the owner, or an agent authorized to act on behalf of the owner, of the copyrighted work described.
capcha
Download Presentation

PowerPoint Slideshow about ' RECYCLE CHROMATOGRAPHY' - arlene


An Image/Link below is provided (as is) to download presentation

Download Policy: Content on the Website is provided to you AS IS for your information and personal use and may not be sold / licensed / shared on other websites without getting consent from its author.While downloading, if for some reason you are not able to download a presentation, the publisher may have deleted the file from their server.


- - - - - - - - - - - - - - - - - - - - - - - - - - E N D - - - - - - - - - - - - - - - - - - - - - - - - - -
Presentation Transcript
recycle chromatography

RECYCLECHROMATOGRAPHY

Jiri SEVCIK

Prague, the Czech Republic

RECYCLE GC

about
ABOUT
  • CHARACTERISTICS
  • SEPARATION EFFICIENCY
  • RESOLUTION
  • RECYCLE CHROMATOGRAPHY HW

RECYCLE GC

multi d imensional chromatography systems
multidimensional chromatographySYSTEMS

serial

parallel

KD1 <> KD2 <> KDd

RECYCLE GC

schematics of recycle chromatography
SCHEMATICSof recycle chromatography

INJECT R1

tM

w0

INTERFACE

tMex

wew

COLUMN

tRa/ , tRb/

wa , wb

R2 DETECT

tMdet

wdet

LOOP COUNTER

i

RECYCLE GC

recycle chromatography parameters
RECYCLE CHROMATOGRAPHYPARAMETERS
  • retention time
  • elution profile width
  • separation efficiency
  • resolution

RECYCLE GC

retention time in recycle chromatography
RETENTION TIMEin recycle chromatography

INJECT R1

tM

INTERFACE

tMex

COLUMN

tRa/ , tRb/

R2 DETECT

tMdet

LOOP COUNTER

i

RECYCLE GC

recycle chromatography retention time
RECYCLE CHROMATOGRAPHYRETENTION TIME
  • from an injector to a detector
  • within a loop
  • after i loops

RECYCLE GC

recycle chromatography retention time1
RECYCLE CHROMATOGRAPHYRETENTION TIME
  • retention time between consecutive cycles is constant
  • total retention time is additive

RECYCLE GC

elution profile width of recycle chromatography
ELUTION PROFILE WIDTHof recycle chromatography

INJECT R1

w0

INTERFACE

wew

COLUMN

wa , wb

R2 DETECT

wdet

LOOP COUNTER

i

RECYCLE GC

recycle chromatography elution profile width
RECYCLE CHROMATOGRAPHYELUTION PROFILE WIDTH
  • from an injector to a detector
  • within a loop
  • after i loops

RECYCLE GC

recycle chromatography elution profile width1
RECYCLE CHROMATOGRAPHYELUTION PROFILE WIDTH
  • elution profile width between consecutive cycles is constant
  • total peak width is additive in form of their variances

RECYCLE GC

recycle chromatography separation efficiency
RECYCLE CHROMATOGRAPHYSEPARATION EFFICIENCY
  • number of effective plates
  • after a loop

RECYCLE GC

recycle chromatography separation efficiency1
RECYCLE CHROMATOGRAPHYSEPARATION EFFICIENCY
  • number of effective plates after i loops

RECYCLE GC

recycle chromatography extra column effects
RECYCLE CHROMATOGRAPHYEXTRA COLUMN EFFECTS
  • number of effective plates after i loops

RECYCLE GC

recycle chromatography extra column effects2
RECYCLE CHROMATOGRAPHYEXTRA COLUMN EFFECTS
  • ratio ni / n1
  • aninlet part of a column is unefficient

THUS

  • efficienty increases faster in recycle system than in nonrecycle system
  • it is not correct to express separation efficiency in terms of the theoretical plate number

RECYCLE GC

separation in recycle chromatography
SEPARATION IN RECYCLE CHROMATOGRAPHY
  • retention interval of unseparated mixture
  • in one-dimensional system
  • in recycle system

tD

tb ta

RECYCLE GC

separation in recycle chromatography1
SEPARATION IN RECYCLE CHROMATOGRAPHY
  • retention interval of unseparated mixture

increases over the column lenght untill 1st peak leaves the column while the last one just enters the column

  • then peak will merge again

THUS

  • maximum number of cycles

tD

tb ta

RECYCLE GC

resolution in recycle chromatography
RESOLUTIONIN RECYCLE CHROMATOGRAPHY
  • retention order can not change because of the same st.phase (a remains constant)

RECYCLE GC

required separation efficiency in recycle chromatography
REQUIRED SEPARATION EFFICIENCYIN RECYCLE CHROMATOGRAPHY
  • for required resolution
  • a , k and n can be optimized
  • if Rab = 1 an optimum number of cycles results

RECYCLE GC

the optimal number of cycles in recycle chromatography
THE OPTIMAL NUMBER OF CYCLESIN RECYCLE CHROMATOGRAPHY
  • for isomers a=1.01 , k=5and n=20,000

Rab1 = 0,29 and

the optimal number of cycles iopt= 3.3

RECYCLE GC

recycle chromatography maximal number of cycles
RECYCLE CHROMATOGRAPHYMAXIMAL NUMBER of CYCLES

merged at start

maximal separation

merged once again

RECYCLE GC

recycle capillary gc principle
recycle capillary GCPRINCIPLE
  • recycling analysed mixture through single capillary column
  • by means of peristaltic pump as mobile phase source
  • and controling actually achieved separation by means of end column splitter

RECYCLE GC

recycle capillary gc construction
recycle capillary GCCONSTRUCTION
  • peristaltic pump providing optimal column flow for columns from 5 to 50 meters
  • fixed end column splitter

RECYCLE GC

instrumentation interface in recycle chromatography
INSTRUMENTATION - interface IN RECYCLE CHROMATOGRAPHY

peristaltic pump

R1 40 mm (injector)

R2 40 mm (detector MS)

flow

column

RECYCLE GC

recycle capillary gc application
recycle capillary GCAPPLICATION
  • suited for componds up to C10
  • for limited number of compounds with similar physicochemical and chiral properties
  • first time separation of 3 stereoisomers of 3,4-dimethylhexane

on β–cyclodextrine

with 2,000,000 plates

RECYCLE GC

nonselective separation
nonselective separation
  • Carbowax 20M
  • 300 m, 250 µm
  • n = 500,000
  • n-dodecene isomers

RECYCLE GC

selectivity of separation
selectivity of separation
  • separation of isomers also with a functional group in middle of carbon chain
  • n-dodecenes

RECYCLE GC

about1
ABOUT
  • CHARACTERISTICS
  • SEPARATION EFFICIENCY
  • RESOLUTION
  • RECYCLE CHROMATOGRAPHY HW

RECYCLE GC

new gc methods development
sample preparation

efficiency

selectivity

hyphenation

sensitivity

detection

software

ITP - GC

recycle GC

stationary phases

comprehensive

thermal modulation

spectral detectors

deconvolution

NEW GC METHODS development

toward reduced ultimate uncertainty

RECYCLE GC

ad