Recycle chromatography
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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.

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RECYCLE CHROMATOGRAPHY

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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 components and variations

recycle chromatographyCOMPONENTS AND VARIATIONS

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


Recycle chromatography retention time proof of additivity

RECYCLE CHROMATOGRAPHYRETENTION TIME PROOF of ADDITIVITY

RECYCLE GC


Recycle chromatography retention time proof of additivity1

RECYCLE CHROMATOGRAPHYRETENTION TIME PROOF of ADDITIVITY

RECYCLE GC


Retention time in recycle chromatography1

RETENTION TIMEIN RECYCLE CHROMATOGRAPHY

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 peak width proof of additivity

RECYCLE CHROMATOGRAPHYPEAK WIDTH PROOF of ADDITIVITY

RECYCLE GC


Recycle chromatography peak width proof of additivity1

RECYCLE CHROMATOGRAPHYPEAK WIDTH PROOF of ADDITIVITY

RECYCLE GC


Peak width in recycle chromatography

PEAK WIDTHIN RECYCLE CHROMATOGRAPHY

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 separation efficiency proof of additivity

RECYCLE SEPARATION EFFICIENCYPROOF of ADDITIVITY

RECYCLE GC


Recycle chromatography extra column effects

RECYCLE CHROMATOGRAPHYEXTRA COLUMN EFFECTS

  • number of effective plates after i loops

RECYCLE GC


Recycle chromatography extra column effects1

RECYCLE CHROMATOGRAPHYEXTRA COLUMN EFFECTS

  • ratio ni / n1

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


Recycle chromatography extra column effects3

RECYCLE CHROMATOGRAPHYEXTRA COLUMN EFFECTS

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


Recycle separation efficiency proof of additivity1

RECYCLE SEPARATION EFFICIENCYPROOF of ADDITIVITY

RECYCLE GC


Maximum number of cycles in recycle chromatography

MAXIMUM NUMBER OF CYCLESIN RECYCLE CHROMATOGRAPHY

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)

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Maximum available resolution in recycle chromatography

MAXIMUM AVAILABLE RESOLUTIONIN RECYCLE CHROMATOGRAPHY

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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


Recycle separation efficiency number of cycles

RECYCLE SEPARATION EFFICIENCYNUMBER of CYCLES

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


Ms sim separation of gc non separated isomers

MS-SIM separation of GC non separated isomers

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

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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

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Ms sim separation of gc non separated isomers1

MS-SIM separation of GC non separated isomers

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


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