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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RECYCLECHROMATOGRAPHY

Jiri SEVCIK

Prague, the Czech Republic

RECYCLE GC


ABOUT

  • CHARACTERISTICS

  • SEPARATION EFFICIENCY

  • RESOLUTION

  • RECYCLE CHROMATOGRAPHY HW

RECYCLE GC


multidimensional chromatographySYSTEMS

serial

parallel

KD1 <> KD2 <> KDd

RECYCLE GC


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 chromatographyCOMPONENTS AND VARIATIONS

RECYCLE GC


RECYCLE CHROMATOGRAPHYPARAMETERS

  • retention time

  • elution profile width

  • separation efficiency

  • resolution

RECYCLE GC


RETENTION TIMEin recycle chromatography

INJECT R1

tM

INTERFACE

tMex

COLUMN

tRa/ , tRb/

R2 DETECT

tMdet

LOOP COUNTER

i

RECYCLE GC


RECYCLE CHROMATOGRAPHYRETENTION TIME

  • from an injector to a detector

  • within a loop

  • after i loops

RECYCLE GC


RECYCLE CHROMATOGRAPHYRETENTION TIME

  • retention time between consecutive cycles is constant

  • total retention time is additive

RECYCLE GC


RECYCLE CHROMATOGRAPHYRETENTION TIME PROOF of ADDITIVITY

RECYCLE GC


RECYCLE CHROMATOGRAPHYRETENTION TIME PROOF of ADDITIVITY

RECYCLE GC


RETENTION TIMEIN RECYCLE CHROMATOGRAPHY

RECYCLE GC


ELUTION PROFILE WIDTHof recycle chromatography

INJECT R1

w0

INTERFACE

wew

COLUMN

wa , wb

R2 DETECT

wdet

LOOP COUNTER

i

RECYCLE GC


RECYCLE CHROMATOGRAPHYELUTION PROFILE WIDTH

  • from an injector to a detector

  • within a loop

  • after i loops

RECYCLE GC


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 CHROMATOGRAPHYPEAK WIDTH PROOF of ADDITIVITY

RECYCLE GC


RECYCLE CHROMATOGRAPHYPEAK WIDTH PROOF of ADDITIVITY

RECYCLE GC


PEAK WIDTHIN RECYCLE CHROMATOGRAPHY

RECYCLE GC


RECYCLE CHROMATOGRAPHYSEPARATION EFFICIENCY

  • number of effective plates

  • after a loop

RECYCLE GC


RECYCLE CHROMATOGRAPHYSEPARATION EFFICIENCY

  • number of effective plates after i loops

RECYCLE GC


RECYCLE SEPARATION EFFICIENCYPROOF of ADDITIVITY

RECYCLE GC


RECYCLE CHROMATOGRAPHYEXTRA COLUMN EFFECTS

  • number of effective plates after i loops

RECYCLE GC


RECYCLE CHROMATOGRAPHYEXTRA COLUMN EFFECTS

  • ratio ni / n1

RECYCLE GC


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 CHROMATOGRAPHYEXTRA COLUMN EFFECTS

RECYCLE GC


SEPARATION IN RECYCLE CHROMATOGRAPHY

  • retention interval of unseparated mixture

  • in one-dimensional system

  • in recycle system

tD

tb ta

RECYCLE GC


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 EFFICIENCYPROOF of ADDITIVITY

RECYCLE GC


MAXIMUM NUMBER OF CYCLESIN RECYCLE CHROMATOGRAPHY

tD

tb ta

RECYCLE GC


RESOLUTIONIN RECYCLE CHROMATOGRAPHY

  • retention order can not change because of the same st.phase (a remains constant)

RECYCLE GC


MAXIMUM AVAILABLE RESOLUTIONIN RECYCLE CHROMATOGRAPHY

RECYCLE GC


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 EFFICIENCYNUMBER of CYCLES

RECYCLE GC


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 CHROMATOGRAPHYMAXIMAL NUMBER of CYCLES

merged at start

maximal separation

merged once again

RECYCLE GC


MS-SIM separation of GC non separated isomers

RECYCLE GC


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 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

peristaltic pump

R1 40 mm (injector)

R2 40 mm (detector MS)

flow

column

RECYCLE GC


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

  • Carbowax 20M

  • 300 m, 250 µm

  • n = 500,000

  • n-dodecene isomers

RECYCLE GC


selectivity of separation

  • separation of isomers also with a functional group in middle of carbon chain

  • n-dodecenes

RECYCLE GC


MS-SIM separation of GC non separated isomers

RECYCLE GC


ABOUT

  • CHARACTERISTICS

  • SEPARATION EFFICIENCY

  • RESOLUTION

  • RECYCLE CHROMATOGRAPHY HW

RECYCLE GC


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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