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MN

Gas chromatographyGas chromatography

305

Page

Basic principles of GC

Introduction to GC 306 – 307

Capillary columns for GC

Brief selection guide for capillary columns 308 – 309OPTIMA

®

high performance capillary columns for GC 310 – 326PERMABOND

®

capillary columns for GC 330 – 331

Hints for use and maintenance of capillary columns

332

GC capillary columns for special applications 332 – 346

Summary

332,

capillary columns with thick films

333,

fast GC columns

334,

amine separations

335,

FAME separations

336,

GC analysis of petrochemical compounds

338,

environmental analyses

339,

triglyceride separation

340,

separation of silanes

341

, analysis of diethylene glycol

341

, enantiomer separation

342 – 346

Untreated capillaries, retention gaps and deactivated capillaries 347 – 347

Fused silica capillary columns – not chemically bonded 349

Derivatisation reagents

Summary, method development kits, selection guide for derivatisation of important functional groups in GC 350 – 351

Acylation, reagents and methods 352Methylation, reagents and methods 353 – 353Silylation, reagents and methods 355 – 358

Standards for GC

Environmental standards for GC 359 – 361Test mixtures for GC capillary columns 362 – 363

Accessories for GC

364 – 373

Accessories for capillary columns

364 – 365,

368,

Valco fittings for capillary GC

366 – 367

, accessories for packed GC columns

369

, products for gas flow meas-urement and in-line gas purification

369 – 371

, ferrules

372

, septa

373

user

Typewritten Text

Contact [email protected] or call 61 7 3205 5233

user

Typewritten Text

user

Typewritten Text

MN

Basic principles of GCBasic principles of GC

Introduction to GC

306

In this chapter we want to give a short and general introduc-tion for the beginner in gas chromatography. By no meansthis is meant as a complete treatise. For further informationplease refer to the references given below*.

The GC system

The chromatographic system is composed of the chromato-graph and a recorder for plotting chromatograms or a datastation for generation and evaluation of chromatograms. Thechromatograph consists of the sample injector, gas supplies,oven with temperature control for the chromatographic col-umn and the detector.It would take us too far to describe all injection techniques indetail. We just want to mention the different basic possibili-ties of direct and indirect sample injection. With

direct

injec-tion the sample is introduced into the column without contactwith other parts from glass or metal (on column injection).With

indirect

techniques the sample is injected into an evap-orator. The vapour then is transferred into the column eithercompletely or partially (split technique). With both techniquesthe injection can take place at low temperatures, at high tem-peratures or with temperature programming.The gas supply unit of a chromatograph has to provide allgases needed for a separation: the carrier gas and e.g. theburner gases for the flame ionisation detector (FID).The detector indicates a substance by generation of a moreor less intense electrical signal (response). Analogue(recorder) or digital (computer) processing of these signals

produces the chromatogram or a numerical report. Somedetectors are specific for certain classes of substances or forcertain atoms (P, N, etc.).

The separation process

The chromatographic separation is achieved by repeateddistribution of each sample component between two phases.One of these phases is stationary. The second, the mobilephase moves along this stationary phase.In Gas Chromatography (GC) the mobile phase is always agas (mostly N

2

, H

2

, He). The stationary phase in GSC (GasSolid Chromatography or adsorption chromatography) is aporous polymer solid, while in GLC (Gas Liquid Chromatog-raphy or partition chromatography) the stationary phase is amostly viscous gumlike liquid. Packed columns are com-pletely filled with a packing, liquid stationary phases beingcoated onto an inert support. Capillary columns do notrequire a support, because their inner wall is coated with thestationary phase (WCOT = Wall Coated Open Tubular).Transport of the components is achieved exclusively in thegas phase, separation is accomplished in the stationaryphase.The quality of a separation (resolution) depends on how longthe components to be separated stay in the stationary phaseand on how often they interact with this phase (selectivity).The type of interaction between component and phase(selectivity) is determined by the functional groups. Thepolarity of the phase is a function of stationary phase substit-uents.

The chromatogram

A chromatogram consists of a base line and a number ofpeaks.The area of a peak allows quantitative determinations.Starting point of a chromatogram is the time of injection of adissolved sample. The time interval between a peak and thepoint of injection is called retention time t

R

. A component canbe identified by its retention time (qualitative determination).The retention time is the sum of the residence time of a sol-ute in the mobile phase (t

0

) and in the stationary phase (t

R

' =net retention time);

t

0

is also known as dead time. It is the time required by acomponent to migrate through the chromatographic systemwithout any interaction with the stationary phase (also calledair or gas peak). The net retention time is the difference

sampleinjection

data system

gassupply

detector

recorder

capillarycolumn

chromatogram

Schematic presentation of a GC system

Schematic presentation of a chromatogram

Start

tR 1

tR 2

t0

w1/2

tR i= t0 + tR ’

i

tR i’

MN

Basic principles of GCBasic principles of GC

Introduction to GC

307

between total retention time and dead time t

0

. It indicateshow long a substance stays in the stationary phase.

The capacity factor (k’) is a measure for the position of asample peak in the chromatogram. The capacity factor isspecific for a given compound and constant under constantconditions.

The relative retention (

α

), also called separation factor orselectivity coefficient, is defined as

i.e. it is the ratio of two capacity factors, the reference sub-stance always being in the denominator. The relative reten-tion does not provide any information on the quality of a sep-aration, since for equal vaues of

α

two very broad peaks mayoverlap, (as shown in trace a), or may be completelyresolved (as in trace b), if they are correspondingly narrow.

For this reason the peak width at half height (w

1/2

) is takeninto account when considering the resolution R according to

The resolution R is a measure for the quality of a separation.The separation number SN is another value indicating thequality of a separation. It defines how many peaks can beresolved between two members of a homologous series ofe.g. n-paraffins.

If retention times are not too small, SN can be determined ina temperature programme.The number of theoretical plates (N

th

) characterises the qual-ity of a column (it should be determined for k’ > 5):

The height equivalent to a theoretical plate (h, HETP) is cal-culated by dividing the length L of the column by the numberof theoretical plates N

th

:

Such a plate is of course a theoretical hypothesis, represent-ing that portion of a column in which the partition equilibriumis established once. The smaller this value the better worksthe column.The relation between N, R and k' is

From this formula the number of plates N

th

required for agiven resolution R can be calculated.The Van Deemter equation shows how the plate height hdepends on the flow velocity u:

A = Eddy diffusion; A is a function of packing uniformity; forWCOT capillary columns A equals 0 (WCOT = WallCoated Open Tubular)

B = molecular axial diffusion; B is a function of the diffusioncoefficient of the component in the respective carrier gas

C = resistance to mass transferIn practice often higher velocities than u

opt.

are chosen, ifseparation efficiency is sufficient, since higher carrier veloci-ties mean shorter retention times.

* References:

D. Rood, ”A practical guide to care, maintainance and trou-bleshooting of capillary gas chromatographic systems“, 2ndedition, Hüthig Verlag, Heidelberg, 1995W. Blum, R. Aichholz ”Hochtemperatur-Gas-Chromatogra-phie“, Hüthig Verlag, Heidelberg, 1991G. Schomburg, “Gas Chromatography, A Practical Course“,Verlag Chemie, Weinheim, 1990K. Grob, “Classical Split and Splitless Injection Techniques inCapillary GC“, Hüthig Verlag, Heidelberg, 1986K. Grob, “Making and Manipulation of Capillary Columns forGas Chromatography“, Hüthig Verlag, Heidelberg, 1986P. Sandra, “Sample Introduction in Capillary Gas Chromatog-raphy, Volume 1“, Hüthig Verlag, Heidelberg, 1985E. Leibnitz, H. G. Struppe, “Handbuch der Gas-Chromatog-raphie“, Akademische Verlagsgesellschaft Geest u. PortigKG, Leipzig, Germany, 1984W. Jennings, “Gas Chromatography with Glass Capillary Col-umns“, Academic Press, New York 1978R. Kaiser, “Chromatographie in der Gasphase“, BI Hoch-schultaschenbücher, several volumes, Bibligraphisches Insti-tut, Mannheim, Germany, 1966

tR i

tR itR i

’ = t0–

tR it0–

ki’ = t0

α = k2’

k1’

retention time

a

b

R =tR 2

– tR1

(w1/2)2 + (w1/2)1

SN =tR 2

– tR1

(w1/2)2 + (w1/2)1

– 1

Nth = 5.54 ⋅ (tR i

w1/2) 2

h = HETP = L

Nth

R =1 α – 1 ki’

4 α ki’ + 1Nth⋅ ⋅ ⋅

u

HETP

Bu C . u

hmin

uopt.

HETP ABu---- C u⋅+ +=

MN

Capillary columns for GCCapillary columns for GC

Brief selection guide for capillary columns

308

For applications with MN GC capillary columns please ask for our catalogue ”GC Applications“

The large number of stationary phases and the variability ofcolumn parameters have caused a considerable diversifica-tion of our column programme. MN now offers more than 30different phases with a total of more than 650 Cat. Nos. Forthis reason especially the beginner may have some prob-lems to select the capillary column best suiting his particularseparation needs. This is why we will briefly explain the mostimportant criteria for column selection.A capillary column is characterised by the following parame-ters: e.g. Cat. No. 726325.25

A = lengthB = inner diameterC = type of chemical bonding, immobilisation D = polarity of the stationary phase E = film thicknessAll these parameters have to be optimised for each particularchromatographic task.

The separation efficiency (correctly speaking the number ofplates n) of a capillary column is directly proportional to thelength. However, the same relation is true for the retentiontime and thus for the total analysis time, making it desirableto use columns as short as possible. For routine separationsin general 25 m or shorter will be sufficient with the advan-tage of short analysis times. For difficult problems such asthe separation of complex mixtures with about 50 compo-nents or more 60 m columns may be necessary.Use of longer columns is not recommended. Doubling thecolumn length will only result in a 40% increase in resolution,since the resolution is proportional to the square root of thelength. However, the time needed for an isothermal analysiswill be doubled.

The inner diameter also influences the separation efficiencyof a capillary column: the lower the inner diameter the higheris the theoretically possible number of plates per meter. Thiswill increase the resolution of the column, which is oftenrequired for complex sample mixtures. Due to the low sam-ple capacity one normally has to work with split injection.Increasing the inner diameter while keeping the film thick-ness constant will increase the capacity. This is especiallyimportant for trace analyses and / or for the injection of largersample volumes. If you halve the diameter of the columnwhile keeping the film thickness constant, the capacity is alsoreduced by 50%. As a general rule one can say: a columnwith 0.32 mm ID and a film thickness of 0.25 µm has a maxi-mum capacity of 100 ng/component. Overloading the columnresults in a loss of resolution.

a) 0.1 to 0.2 mm inner diameter

OPTIMA

®

columns with this diameter are especially recom-mended for GC-MS with the advantage of high resolutionand short retention times with low carrier gas flows.

b) 0.25 mm inner diameter

Columns with this diameter are used for the analysis of com-plex mixtures. They are recommended as routine columnsfor high resolution, especially in research applications.

d) 0.32 mm inner diameter

A column with 0.32 mm ID is

the

column for routine analyseswith short retention times, yet increased capacity. With suita-ble film thickness it is the column of choice for trace analysesand on-column or splitless injection techniques. If you wantto use a mass selective detector (MSD), you are often limitedto smaller diameters, because many vacuum pumps cannothandle the high flow rates required for columns with largerdiameters.

e) 0.53 mm inner diameter

Compared to packed columns these capillaries show moreinert surfaces and higher reproducibility with at least equalseparation efficiency. They are not only

the

replacement forpacked columns, but

the

capillary for rapid separations withinert surface and highest capacity. The inner diameter0.53 mm is ideal for use with the thermal conductivity detector.

OPTIMA

®

:

the top quality of fused silica (FS) capillaries fromMACHEREY-NAGEL with chemically bonded (immobilised)stationary phases. A special treatment after immobilisation ofthe phase results in lower column bleeding. An immobilisedfilm of stationary phase tolerates injection of large samplevolumes in on-column or splitless sample injection tech-niques.

PERMABOND

®

:

FS capillary columns, also with immobilised(chemically bonded) stationary phase.

FS capillary columns

with non-immobilised phases.

Different substituents in the chemical structures of stationaryphases are responsible for the type of interaction (selectivity)between the phase and the solutes to be separated and thusdetermine the relative retention and the number of theoreti-cal plates required for a given resolution. The stationaryphase also limits the temperature range for chromatography.Nonpolar phases separate by efficiency (n) and retention (k')only, while polar phases offer additional interactions, whichmay influence or improve a separation. Selectivity has to beoptimised for the critical pair of components or the main com-ponent.You should always select the least polar column which solvesyour separation problem. About 70% of all separations canbe performed on non- to midpolar columns. These columnsgenerally feature high temperature stability. Nonpolar station-ary phases (e.g. 100% dimethylpolysiloxane phases) sepa-

A. Length

B. Inner diameter

A B C D E

25 m x 0.32 mm ID OPTIMA® 5, 1.0 µm film

C. Immobilisation

D. Stationary phase

MN


Brief selection guide for capillary columns

309

For applications with MN GC capillary columns visit our web site: www.mn-net.com

rate components mostly according to the height of the boilingpoint. Typical analytes are linear hydrocarbons (n-alkanes).When increasing the polarity of the phase, e.g. by introduc-tion of phenyl and / or cyanopropyl groups, separation isincreasingly influenced by differences in dipole moment andby charge transfer (e.g. for 5 – 50% diphenylpolysiloxanephases). Typical analytes are hydrocarbons, which containoxygen, sulphur, nitrogen, phosphorus or halogen atoms,unsaturated molecules which can be polarised and aromat-ics. For components featuring different hydrogen bondingcapacities and the ability to form strong hydrogen bonds, pol-yethylene glycol phases (Carbowax) are the best choice for aseparation. Typical analytes are alcohols and carboxylicacids.

Our programme of capillary columns comprises films from0.1 to 5.0 µm. The standard film thickness is 0.25 µm. If you work with thin films (0.1 – 0.2 µm), in general sub-stances are eluted faster, at lower temperatures and withbetter resolution than with a thick film (>0.2 µm). For high-boiling compounds, temperature labile or very closely elutingsample substances thin films are very well suited.Increasing the film thickness will increase the capacity andimprove inertness. Thick films are ideal for low-boiling com-pounds, often eliminating the need for cooling during chro-matography, since they increase elution temperatures, i.e.the components are retained more strongly. As a generalrule one can say: doubling the film thickness results in anincrease in elution temperature of about 15 – 20 °C underisothermal conditions. This is advantageous for aqueous sys-tems as well.Variation of the film thickness is often better than increasingthe column length as is shown in the following chromato-grams: The upper figure shows a separation with the special columnPERMABOND® P-100 with 0.5 µm film thickness and 100 mlength, while the lower figure shows the chromatogram on a10 m column with 5 µm film thickness. The second figure clearly demonstrates the high separationefficiency of a 10 m column with very thick film compared tothe 100 m column with thin film.According to the criteria cited above the following capillariesare suited for the larger part of all applications and can beconsidered as standard equipment for GC:1. Cat. No. 726314.25 25 m x 0.32 mm ID

OPTIMA® 5, 0.25 µm film2. Cat. No. 726318.25 25 m x 0.32 mm ID

OPTIMA® 1701, 0.25 µm film3. Cat. No. 723321.25 25 m x 0.32 mm ID

PERMABOND® CW 20 M, 0.25 µm film

4. Cat. No. 726440.30 30 m x 0.32 mm IDOPTIMA® δ-3, 0.25 µm filma suitable substitute for 1. and 2.

E. Film thickness

1 2

3

45

6 7

0 2 4 6 min

Analysis of hydrocarbons C1 – C5

Capillary column: PERMABOND® P-100, 0.5 µm film, 100 m x 0.25 mm ID, max. temperature 300/320 °C, Cat. No. 723890.100Chromatographic conditions:Injection volume: 100 µlCarrier gas: 200 kPa H2

(2.3 ml/min)Split: 200 ml/minTemperature: 31 °CDetector: FID, 250 °C, 28

Peaks:1. Methane2. Ethane3. Propane4. i-Butane5. Butane6. Methylbutane7. Pentane

2000

40

Separation of hydrocarbons C1 – C5

Capillary column: OPTIMA® 5, 5.0 µm film, 10 m x 0.32 mm ID, max. temperature 280 °C, Cat. No. 726940.10

Chromatographic conditions:Injection volume: 100 µlCarrier gas: 0.08 bar N2Split: 60 ml/minTemperature: 36 °CDetector: FID, 24

Peaks:1. Methane2. Ethane3. Propane4. i-Butane5. n-Butane6. Methylbutane7. n-Pentane

1 2

3

4 56 7

0 2 4 6 min

2000

30

MN


310


As a result of our efforts in research and development andthe continuous improvements in our manufacturing tech-niques we present OPTIMA® – a series of high performancecapillary columns for gas chromatography.OPTIMA® capillary columns provide

high thermal stabilityImproved temperature stability is the reason why OPTIMA®

capillary columns can be operated at about 40 °C highertemperatures compared to standard phases. High-boilingsolutes (with very low vapour pressures) "normally" havevery long retention times and rather broad peak shapes.OPTIMA® columns with their increased operation tempera-tures elute high-boiling compounds faster and with betterpeak shapes.

Maximum operating temperatures for OPTIMA® phases The first temperature is valid for isothermal operation, thesecond for short isotherms in a temperature programme.Temperature limits for 0.53 mm ID columns and for columnswith film thickness of 3 µm or greater are given with theordering information on the following pages.

reduced column bleedImproved manufacturing processes offer capillaries withlower bleed levels, which are especially recommended forGC-MS. Less column bleed yields increased sensitivity andaccuracy through a better signal to noise ratio for any kind ofdetector. Reduced column bleed improves detectability ofsolutes in qualitative and quantitative GC-MS analyses.

more inert columns due to optimised deactivationPolar compounds are frequently difficult to analyse, becausethey often give broad tailing peaks.Advances in deactivation technology for the OPTIMA® capil-laries result in an excellent chromatographic performanceyielding improved peak shapes of polar compounds com-bined with improved efficiency and sensitivity.In order to guarantee best industry standard capillaries withhighest reproducibility from capillary to capillary OPTIMA®

columns have to meet high specifications.For controlling quality MACHEREY-NAGEL determines thefollowing parameters:

efficiency by measuring the separation number (Trenn-zahl according to Kaiser) in a temperature programme.polarity by measuring retention indicesbleeding in a temperature programme with a test mixtureincluding high-boiling hydrocarbons inertness by measuring the peak height ratio for decyl-amine/C-12 (for non- to medium polar phases)

Phase max. operating temperatures

OPTIMA® 1 340/360 °COPTIMA® 5 340/360 °COPTIMA® δ-3 340/360 °COPTIMA® δ-6 340/360 °COPTIMA® 17 320/340 °COPTIMA® 1301 300/320 °COPTIMA® 1701 300/320 °COPTIMA® 624 280/300 °COPTIMA® 210 260/280 °COPTIMA® 225 260/280 °COPTIMA® 240 260/280 °COPTIMA® CN-100 240/260 °C

9

Capillary column: OPTIMA® 1, 0.35 µm film, 30 m x 0.32 mm ID, max. temp. 340/360 °C, Cat. No.726821.30

Carrier gas: 1.0 bar H2Temperature: 70 °C → 320 °C (10 min), 10 °C/min → 330 °C

(5 min)Detector: FID 300 °C, 105

Peaks:1. C-82. Dibutylamine3. C-104. Phenylethanol5. 2,6-Dichloroaniline6. 2,4-Dichlorophenol7. C-128. Decylamine9. Decanol

10. C-14

11. C-1612. C-1813. C-2014. C-2215. C-2416. C-2617. C-2818. C-3019. C-32

1

2

3

45

6

7

8

10 11 12 13 14 15161718 19

0 10 20 30 min

2112

70

OPTIMA® high performance capillary columns

For ordering information of OPTIMA® capillary columns please see pages 316 – 326.

MN


311



Comparison of separation properties for selected OPTIMA® phases

0 10 20 30 min

12

1

1

1

1

1

1

2

2

2

3 6

5

74 8 9 10

10

10

10

10

10

10

35

6 7 48 9

35

46 7

8 9

3

3

5

46 7

89

2

5

46 7 8 9

3 425

6 78 9

3 42

56 7

89

OPTIMA® 240

OPTIMA® 1701

OPTIMA® 210

OPTIMA® 5

OPTIMA® 1

0.5 µm film30 m x 0.32 mm IDmax. temp. 260/280 °CCat. No. 726096.30





incr

easi

ng

po

lari

ty

OPTIMA® 2250.5 µm film30 m x 0.32 mm IDmax. temp. 260/280 °CCat. No. 726084.30

OPTIMA® 170.5 µm film30 m x 0.32 mm IDmax. temp. 320/340 °CCat. No. 726744.30

Chromatographic conditions:Sample: MN-OPTIMA® test mixture (Cat. No. 722316)Injection: 1.0 µl, split 1:50Carrier gas: 80 kPa N2Temperature: 80 °C → Tmax (isothermal), 8 °C/minDetector: FID, 260 – 300 °C, 26

time [min]Peaks:

1. Undecane2. Dodecane3. Octanol4. Dimethylaniline5. Decylamine

6. Methyl decanoate7. Methyl undecanoate8. Henicosane9. Docosane

10. Tricosane

MN


312


OPTIMA® δ – the unique family of phases with autoselectivity

OPTIMA® δ-3 and OPTIMA® δ-6 are stationary phases,which exhibit not only a fixed polarity, like most polysiloxanephases, but additionally a polarity, which is influenced by thesample. The polymers consist of cross-linked methyl-phenyl-polysiloxane block polymers with defined composition, andextremely narrow molecular weight distribution, which areexclusively produced for MACHEREY-NAGEL. Especiallypolar analytes are able to induce a dipole moment in the sta-tionary phase, so that the molecules show stronger interac-tions with the phase. This enhanced interaction is maintainedat higher temperatures, where normally interactions betweenmolecule and phase become reduced due to the Brownianmovement. We call this phenomenon ”autoselectivity“,because the stationary phase adjusts itself to the polarity ofthe analytes. Thus OPTIMA® δ phases cover broad ranges ofpolarities. Compared with conventional phases, OPTIMA® δ-3 polarity ranges from approximately the nonpolar OPTIMA®

5 to the midpolar OPTIMA® 1701, while for OPTIMA® δ-6 thepolarity covers a range from about the midpolar OPTIMA® 17to the polar OPTIMA® 210. Due to this feature, the OPTIMA® δ columns show interestingpatterns of selectivity. For example, inversions in thesequence of peak elution may occur, which recommends thecolumns for reference use (e. g. in combination withOPTIMA® 5).In conventional midpolar phases the polarity is induced byphenyl, but especially by cyano and trifluoromethyl groups.The two latter often cause bleeding, which results in severeproblems with some detectors. In contrast, the OPTIMA® δphases show very high temperature limits (340/360 ˚C), aswell as the low bleed levels, which makes them ideal for theuse with mass selective (MSD) or phosphorus/nitrogendetectors (PND) in the field of environmental trace analysis.

Key features of the OPTIMA® δ are:Wide range of applications due to autoselectivity Outstanding thermal stability similar to non-polar phasesVery low bleed levelsExtremely inertMedium polar without CN groups

References:W. Röder, D. Lennartz, GIT 3/99, p. 226R. Looser, K. Ballschmiter, J. Chromatogr. 836 (1999), 271-284R. Baycan-Keller, M. Oehme, J. Chromatogr. 837 (1999),201 – 210

OV-1 SE-54 OV-17 OV-1701 OV-210 OV-240

OPTIMA® δ-3

OPTIMA® δ-6

conventional phase

OPTIMA® δpermanent dipole:constant interactions

permanent+ induced

dipole =autoselectivitydipoles of the analytes

permanent dipoles of the stationary phase

induced dipoles of OPTIMA® δ phases

range of polarities covered by OPTIMA® δ phases

MN


313


OPTIMA® δ – the unique family of GC phases with autoselectivity

Analysis of isomeric phenolsIsomeric phenols, such as chloro- and nitrophenols, are difficult to analyse with standard GC phases (e.g. OPTIMA® 5 or OPTIMA® 17) be-cause of coelutions. The autoselective OPTIMA® δ-3 is able to separate all 22 phenols due to stronger interactions occurring with more polar molecules, because polar analytes induce a dipole moment in the phase of the OPTIMA® δ-3. Capillary column: OPTIMA® δ-3, 0.25 µm film, 60 m x 0.25 mm ID, max. temperature 340/360 °C, Cat. No. 726420.60Chromatographic conditions:Injection: 1.0 µl, split 1:80Carrier gas: He, 1.3 barTemperature: 60 °C (3 min) → 320 °C, 6 °C/minDetector: MSD HP 5971Peaks:

1. Phenol2. 2-Chlorophenol3. 2-Methylphenol4. 4-Methylphenol5. 3-Methylphenol6. 2,4-Dimethylphenol7. 2-Nitrophenol8. 2,4-Dichlorophenol9. 2,6-Dichlorophenol

10. 4-Chloro-3-methylphenol11. 2,3,5-Trichlorophenol12. 2,4,6-Trichlorophenol13. 2,4,5-Trichlorophenol14. 2,3,4-Trichlorophenol15. 2,3,6-Trichlorophenol16. 2,3,5,6-Tetrachlorophenol17. 2,3,4,5-Tetrachlorophenol18. 2,3,4,6-Tetrachlorophenol19. 2,4-Dinitrophenol20. 3,4,5-Trichlorophenol21. 2-Methyl-4,6-dinitrophenol22. 2-Isopropyl-4,6-dinitrophenol 10 20 min

1

2 3

4

56

7

8

9

10

11

1213

14

15

16

17

18

19

20

21

22

2500

60

Separation of organochlorine pesticides (EPA 8081)Capillary column: OPTIMA® δ-6, 0.2 µm film, 50 m x 0.2 mm ID, max. temperature 340/360 ˚C, Cat. No. 726465.50Chromatographic conditions:Sample: EPA 8081 organochlorine pesticide calibration mix (Restek), 200 µg/ml each in toluene : hexane (1 : 1)Injection volume: 1 µl, Split 1: 30Carrier gas: 2.0 bar HeTemperature: 180 °C → 300 °C

(10 min), 4.0 °C/minDetector: MSD HP 5971Peaks:

1. α-BHC2. γ-BHC (lindane)3. β-BHC4. Heptachlor5. δ-BHC6. Aldrin7. Heptachlor epoxide8. γ-Chlordane9. α-Chlordane

10. Endosulfan I11. 4,4'-DDE12. Dieldrin13. Endrin14. 4,4'-DDD15. Endosulfan II16. 4,4'-DDT17. Endrin aldehyde18. Endosulfan sulphate19. Methoxychlor20. Endrin ketone

1 23

4

5

67

8 9

10

11 12

13

14

15

16

17

18

19

20

20 30 min

Abu

ndan

ce

1·105

2·105

3·105

4·10525

0430

MN


314



Max. temperature for isothermal operation 340 °C, max.temperature for short isotherms in a temperature pro-gramme 360 °CAutoselectivity resulting in a wide range of polarities fromapproximately the non-polar OPTIMA® 5 to the midpolarOPTIMA® 1701Analytes determine the polarity of the phaseMedium polar without CN groupsIdeal for MSD and PND detectorsUSP 49

Unique from MN, no similar phases

Ordering information Cat. No. for column length of10 m 12 m 15 m 20 m 25 m 30 m 50 m 60 m

0.1 mm ID (0.4 mm OD)0.10 µm film 726410.10 – – 726410.20 – – – –

0.2 mm ID (0.4 mm OD)0.20 µm film – – – – 726400.25 – 726400.50 –

0.25 mm ID (0.4 mm OD)0.25 µm film – – – – – 726420.30 – 726420.600.50 µm film – – – – – 726421.30 – –

0.32 mm ID (0.5 mm OD)0.25 µm film – – – – – 726440.30 – 726440.600.35 µm film – – – – – 726441.30 – 726441.601.00 µm film – – – – – 726442.30 – 726442.60

0.53 mm ID (0.8 mm OD)1.00 µm film – – – – – 726443.30 – –

Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends areclosed with septa, and thus protected from atmospheric oxygen. Additionally, we supply the corresponding test mixture with each column.In addition to this standard programme we will be happy to supply columns custom-made to your specifications.

Separation of organophosphorus pesticides (EPA 8140/8141) on OPTIMA® δ-3Capillary column: OPTIMA® δ-3, 0.2 µm film, 50 m x 0.2 mm ID, max. temperature 340/360 °C, Cat. No. 726400.50Chromatographic conditions: sample EPA 8140 OP pesticide calibration mix (Restek), 200 µg/ml each in hexane : acetone = 95 : 5Injection: 1 µl, split 1 : 30, carrier gas: 2.0 bar He, temperature: 150 °C → 300 °C (10 min), 2.5 °C/minDetector: MSD HP 5971Peaks:

1. Dichlorvos2. Mevinphos3. Demeton-s4. Ethoprop5. Naled6. Phorate7. Demeton-o8. Diazinon9. Disulfoton

10. Parathion-methyl11. Ronnel12. Fenthion13. Chlorpyrifos14. Trichloronate15. Merphos16. Stirofos17. Tokuthion18. Merphos oxidation product19. Fensulfothion20. Bolstar21. Azinphos-methyl 22. Coumaphos

1 2

3

4

5

6

7

8 9

10

11

12

13

14

15

1617

18

19

20

21

22

20 40 60 min

2504

90

MN


315



Max. temperature for isothermal operation 340 °C, max.temperature for short isotherms in a temperature pro-gramme 360 °CAutoselectivity resulting in a wide range of polarities fromapproximately the non-polar OPTIMA® 17 to the midpolarOPTIMA® 210Analytes determine the polarity of the phaseMedium polar without CN groupsIdeal for MSD and PND detectors

Unique from MN, no similar phases

Ordering information Cat. No. for column length of10 m 12 m 15 m 25 m 30 m 50 m 60 m

0.1 mm ID (0.4 mm OD)0.10 µm film 726490.10 – – – – – –

0.2 mm ID (0.4 mm OD)0.20 µm film – – – 726465.25 – 726465.50 –

0.25 mm ID (0.4 mm OD)0.25 µm film – – – – 726470.30 – 726470.60

0.32 mm ID (0.5 mm OD)0.25 µm film – – – – 726480.30 – 726480.600.35 µm film – – – – 726481.30 – 726481.60

0.53 mm ID (0.8 mm OD)1.00 µm film – – – – 726483.30 – –


20 40 60 min

Separation of organophosphorus pesticides (EPA 8140/8141) on OPTIMA® δ-6Capillary column: OPTIMA® δ-6, 0.2 µm film, 50 m x 0.2 mm ID, max. temperature 340/360 ˚C, Cat. No. 726465.50Chromatographic conditions:Sample: EPA 8140 OP pesticide calibration mix (Restek), 200 µg/ml each in hexane : acetone = 95 : 5Injection volume: 1 µl, split 1:30Carrier gas: 2.0 bar HeTemperature: 150 °C → 300 °C (10 min), 2.5 °C/minDetector: MSD HP 5971Peaks:

1. Dichlorvos2. Mevinphos3. Demeton-s4. Ethoprop5. Naled6. Phorate7. Demeton-o8. Diazinon9. Disulfoton

10. Parathion-methyl11. Ronnel12. Fenthion13. Chlorpyrifos14. Trichloronate15. Merphos16. Stirofos17. Tokuthion18. Merphos oxidation product19. Fensulfothion20. Bolstar21. Azinphos-methyl 22. Coumaphos

1

2

3

4

5

6

7

8

9

10

11

12

1314

15

16

17

18

19, 20

21

22

2504

20

MN


316



For columns with 0.2 – 0.32 mm ID and films < 3 µm themax. temperature for isothermal operation is 340 °C, the max. temperature for short isotherms in a tempera-ture programme is 360 °C for 0.53 mm ID columns with films < 3 µm the max. tem-peratures are 320 and 340 °C, resp.for thick film columns with films ≥ 3 µm the max. tempera-tures are 300 and 320 °C, resp.NonpolarSeparation of components according to boiling pointsThick film columns ≥ 3 µm film are especially recom-mended for solvent analysesSimilar phases: OV-1, DB-1, SE-30, HP-1, Ultra-1,SPB-1, CP-SIL 5 CB, Rtx-1, 007-1, BP1, MDN-1, AT-1,ZB 1, OV 101USP G 2

100% dimethylpolysiloxaneCH3

O Si

CH3 n

Ordering information Cat. No. for column length of

10 m 12 m 15 m 20 m 25 m 30 m 50 m 60 m

0.1 mm ID (0.4 mm OD)0.10 µm film 726024.10 – – 726024.20 – – – –0.40 µm film – – – 726025.20 – – – –

0.2 mm ID (0.4 mm OD)0.10 µm film – – – – 726832.25 – 726832.50 –0.20 µm film – 726834.12 – – 726834.25 – 726834.50 –0.35 µm film – 726837.12 – – 726837.25 – 726837.50 –0.50 µm film – – – – 726839.25 – 726839.50 –

0.25 mm ID (0.4 mm OD)0.10 µm film 726038.10 – 726038.15 – 726038.25 726038.30 726038.50 726038.600.25 µm film 726050.10 – 726050.15 – 726050.25 726050.30 726050.50 726050.600.50 µm film 726081.10 – 726081.15 – 726081.25 726081.30 726081.50 726081.601.00 µm film – – – – 726802.25 726802.30 726802.50 726802.60

0.32 mm ID (0.5 mm OD)0.10 µm film 726301.10 – 726301.15 – 726301.25 726301.30 726301.50 726301.600.25 µm film 726302.10 – 726302.15 – 726302.25 726302.30 726302.50 726302.600.35 µm film – – – – 726821.25 726821.30 726821.50 726821.600.50 µm film 726304.10 – 726304.15 – 726304.25 726304.30 726304.50 726304.601.00 µm film 726323.10 – 726323.15 – 726323.25 726323.30 726323.50 726323.603.00 µm film – – – – 726805.25 726805.30 726805.50 726805.605.00 µm film 726931.10 – 726931.15 – 726931.25 726931.30 – –

0.53 mm ID (0.8 mm OD)0.50 µm film 726519.10 – – – 726519.25 726519.30 – –1.00 µm film 726529.10 – 726529.15 – 726529.25 726529.30 – –2.00 µm film 726521.10 – 726521.15 – 726521.25 726521.30 – –5.00 µm film 726926.10 – 726926.15 – 726926.25 726926.30 726926.50 –

Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends areclosed with septa, and thus protected from atmospheric oxygen. Additionally, we supply the corresponding test mixture with each column.

In addition to this standard programme we will be happy to supply columns custom-made to your specifications.

MN


317



Max. temperature for isothermal operation 340 °C, max. temperature for short isotherms in a temperatureprogramme 360 °C Selectivity identical with OPTIMA® 1Phase with lowest bleedingIdeal for GC/MS and ECD applications and general anal-yses at trace level

Solvent analysisCapillary column: OPTIMA® 1, 1.0 µm film, 60 m x 0.32 mm ID, max. temperature 340/360 °C, Cat. No. 726323.60Chromatographic conditions:Sample: Solvent mixture, courtesy of J. Lutz, Alcan Rorschach, SwitzerlandInjection volume: 0.4 µl, split 1 : 60Carrier gas: H2, 120 KPaTemperature: 50 °C (9 min) → 90 °C, 4 °C/min → 280°C (2 min), 14 °C/minDetector: FID, 300 °C, 26

Peaks:1. Methanol2. Ethanol3. Acetone4. Isopropanol5. Methyl acetate6. n-Propanol7. Methyl ethyl ketone8. Ethyl acetate9. Isobutanol10. n-Butanol11. 1-Methoxy-2-propanol12. Isooctane13. Ethylglycol14. Isoheptane15. Methyl isobutyl ketone16. 1-Ethoxy-2-propanol17. Toluene18. Isobutyl acetate19. Butyl acetate20. 4-Hydroxy-4-methyl-2-pentanone21. 1-Methoxy-2-propyl acetate22. Xylene 23. Cyclohexanone24. Ethyl glycol acetate25. Butyl glycol26. Heptanol27. Ethyldiglycol28. Butyldiglycol29. Butyl glycol acetate30. Butyldiglycol acetate

10

20

30

40

50

60

70

80

10

1

3

2 4

5

6

7

8

910

1112

1314

15

1617

18

1920

21

23

24

25

26

27

30

2928

20 30min

mV

22

2013

90

CH3

O Si

CH3 n

100% dimethylpolysiloxane

Ordering information Cat. No. for column length of12 m 15 m 25 m 30 m 50 m 60 m

0.2 mm ID (0.4 mm OD)0.20 µm film – – 726201.25 – 726201.50 –0.35 µm film 726203.12 – – – – –

0.25 mm ID (0.4 mm OD)0.25 µm film – 726205.15 – 726205.30 – 726205.60

0.32 mm ID (0.5 mm OD)0.25 µm film – – – 726202.30 – –


MN


318



For columns with 0.2 – 0.32 mm ID and films < 3 µm themax. temperature for isothermal operation is 340 °C, the max. temperature for short isotherms in a tempera-ture programme is 360 °C for 0.53 mm ID columns with films < 3 µm the max. tem-peratures are 320 and 340 °C, resp.for thick film columns with films ≥ 3 µm the max. tempera-tures are 300 and 320 °C, resp.NonpolarStandard phase with large range of applicationSuitable for GC/MS (columns with small films)Similar phases: SE-54, SE-52, DB-5, HP-5, Ultra-2, SPB-5, CP-SIL 8, Rtx-5, 007-2, BP5, MDN-5, AT-5, ZB-5USP G 27

CH3

O Si

CH3 m

O Si

n

5% phenyl – 95% dimethylpolysiloxane

CH3

Ordering information Cat. No. for column length of

10 m 12 m 15 m 25 m 30 m 50 m 60 m

0.1 mm ID (0.4 mm OD)0.10 µm film 726846.10 – – – – – –

0.20 mm ID (0.4 mm OD)0.10 µm film – 726854.12 – 726854.25 – 726854.50 –0.20 µm film – – – 726857.25 – 726857.50 –0.35 µm film – 726860.12 – 726860.25 – 726860.50 –0.50 µm film – 726863.12 – 726863.25 – 726863.50 –

0.25 mm ID (0.4 mm OD)0.10 µm film – – – 726911.25 726911.30 726911.50 726911.600.25 µm film 726056.10 – 726056.15 726056.25 726056.30 726056.50 726056.600.35 µm film – – – 726623.25 726623.30 726623.50 726623.600.50 µm film – – – 726099.25 726099.30 726099.50 726099.601.00 µm film – – – 726807.25 726807.30 726807.50 726807.60

0.32 mm ID (0.5 mm OD)0.10 µm film 726313.10 – 726313.15 726313.25 726313.30 726313.50 726313.600.25 µm film 726314.10 – 726314.15 726314.25 726314.30 726314.50 726314.600.35 µm film – – – 726628.25 726628.30 726628.50 726628.600.50 µm film – – – 726316.25 726316.30 726316.50 726316.601.00 µm film 726325.10 – 726325.15 726325.25 726325.30 726325.50 726325.603.00 µm film – – – 726809.25 726809.30 726809.50 726809.605.00 µm film 726934.10 – 726934.15 726934.25 726934.30 – –

0.53 mm ID (0.8 mm OD)0.50 µm film 726523.10 – – 726523.25 726523.30 – –1.00 µm film 726541.10 – 726541.15 726541.25 726541.30 – –2.00 µm film 726525.10 – 726525.15 726525.25 726525.30 726525.50 726525.605.00 µm film 726916.10 – 726916.15 726916.25 726916.30 726916.50 –



MN


319



Max. temperature for isothermal operation 340 °C,max. temperature for short isotherms in atemperature programme 360 °C Selectivity identical with OPTIMA® 5New quality – even less bleedingIdeal for GC/MS and ECD applications andgeneral analyses at trace level

CH3

O Si

CH3 m

O Si

n

5% diphenyl – 95% dimethylpolysiloxane

Pyrolysis GC of chloroprene rubber Capillary column: OPTIMA® 5 MS, 1 µm film, 60 m x 0.32 mm ID, max. temperature: 340/360 °C, Cat. No. 726212.60 Method: 1 g solid are dissolved in 10 ml of hexane or methanol, 100 µl of this solution are pyrolysed in a crucible, headspaceChromatographic conditions:Temperature: 60 °C (5 min)

→ 320 °C, 8 °C/min

Detector: MSDchromatogram courtesy of Mrs. Engel, VW, Wolfsburg, Germany

10 20 30 40 50 60 70 min

2100

40

Analysis of PCB (W22 congener mix)Capillary column: OPTIMA® 5 MS, 0.2 µm film, 50 m x 0.20 mm ID, max. temperature: 340/360 °C, Cat. No. 726210.50Chromatographic conditions:Sample: PCB-W22 congener mix, 10 µl/mlInjection: 1 µlSplit: 80 ml/minCarrier gas: 0.5 bar HeTemperature: 220 °C → 300 °C (15 min), 1.5 °C/minDetector: ECD, 300 °C

Peaks:1. PCB 182. PCB 313. PCB 284. PCB 205. PCB 52

6. PCB 447. PCB 1018. PCB 1499. PCB 118

10. PCB 153

11. PCB 10512. PCB 13813. PCB 18014. PCB 17015. PCB 194

1

2

3 4

5

6 7 8

910

1112

13 1415

10 20 30 40 50

15

min

31

28

2111

80


0.2 mm ID (0.4 mm OD)0.20 µm film – 726210.12 – 726210.25 – 726210.50 –0.35 µm film – 726215.12 – 726215.25 – 726215.50 –

0.25 mm ID (0.4 mm OD)0.25 µm film – – 726220.15 – 726220.30 – 726220.600.50 µm film – – – – 726225.30 – 726225.601.00 µm film – – – – 726226.30 – –

0.32 mm ID (0.5 mm OD)0.25 µm film – – – – 726211.30 – –0.50 µm film – – – – 726213.301.00 µm film – – – 726212.25 – 726212.50 726212.60


NEW!

MN


320



Max. temperature for isothermal operation 320 °C, max.temperature for short isotherms in a temperature pro-gramme 340 °Cfor 0.53 mm ID columns the max. temperatures are 280and 300 °C, resp.Medium polarSuitable for higher temperaturesPreferred applications: steroids, pesticides, drug analy-sesSimilar phases: OV-17, DB-17, HP-50+, HP-17, SPB-50,SP-2250, Rtx-50, CP-SIL 24 CB, 007-17, ZB-50USP G3

phenylmethylpolysiloxane (50% phenyl)

CH3

O Si

n

Analysis of aromatic hydrocarbonsCapillary column: OPTIMA® 17, 0.5 film, 50 m x 0.32 mm ID, max. temperature 320/340 °C, Cat. No. 726744.50Chromatographic conditions:Injection volume: 0.2 µlCarrier gas: 50 kPa N2, split 1:150Temperature: 50 °C → 200 °C, 5 °C/minDetector: FID, 260 °C, 26

Peaks:1. Benzene2. Toluene3. Ethylbenzene4. m-Xylene5. o-Xylene6. Isopropylbenzene7. n-Propylbenzene8. p-Isopropyl-

benzene9. n-Butylbenzene

10. n-Hexylbenzene11. n-Octylbenzene

2105

40

1

23

4

5

67

8

9 1011

0 10 20 min


0.1 mm ID (0.4 mm OD)0.10 µm film 726848.10 – – – – – –

0.2 mm ID (0.4 mm OD)0.20 µm film – 726065.12 – 726065.25 – 726065.50 –0.50 µm film – 726066.12 – 726066.25 – 726066.50 –

0.25 mm ID (0.4 mm OD)0.15 µm film – – – 726742.25 726742.30 726742.50 726742.600.25 µm film 726022.10 – 726022.15 726022.25 726022.30 726022.50 726022.600.50 µm film 726067.10 – 726067.15 726067.25 726067.30 726067.50 726067.60

0.32 mm ID (0.5 mm OD)0.15 µm film – – – 726755.25 726755.30 726755.50 726755.600.25 µm film 726351.10 – 726351.15 726351.25 726351.30 726351.50 726351.600.35 µm film – – – 726757.25 726757.30 726757.50 726757.600.50 µm film – – – 726744.25 726744.30 726744.50 726744.60

0.53 mm ID (0.8 mm OD)1.00 µm film 726747.10 – 726747.15 726747.25 726747.30 – –


MN


321



Max. temperature for isothermal operation 300 °C,max. temperature for short isotherms in atemperature programme 320 °Cfor 0.53 mm ID columns the max. temperatures are280 and 300 °C, resp.

Medium polarSpecial selectivity due to high cyanopropyl contentReference column for structure identification, e.g. in com-bination with OPTIMA® 5Film thickness ≥ 1 µm for solvent analysesSimilar phases: OV-1701, DB-1701, CP-SIL 19 CB, HP-1701, Rtx-1701, SPB-1701, 007-1701, BP10, ZB-1701

14% cyanopropyl-phenyl – 86% dimethylpolysiloxane

CH3

O Si

CH3 m

O Si

n(CH2)3

CN

Analysis of Fusarium mycotoxinsF. Walker, B. Meier, Journal of AOAC Int. 81 (1998) 741 – 748Capillary column: OPTIMA® 1701, 0.35 µm film, 25 m x 0.32 mm ID, max. temperature 300/320 °C, Cat. No. 726 824.25 Injection: 1 µl, 250 °C, splitlessCarrier gas: N2, 30 cm/s, linearvelocity at 160 °CTemperature: 160 °C (3 min) → 240 °C, 6 °C/min → 270 °C,

30 °C/min (3 min)Detector: 63Ni-ECD, 320 °CPeaks: 1. 13.9 min Nivalenol (0.007 ppm)2. 15.1 min Deoxynivalenol (0.006 ppm)3. 17.3 min 15-O-Acetyl-4-deoxynivalenol (0.006 ppm)4. 17.6 min 3-Acetyldeoxynivalenol (0.005 ppm)

1

2

34

2106

60


0.2 mm ID (0.4 mm OD)0.20 µm film – 726841.12 – 726841.25 – 726841.50 –

0.25 mm ID (0.4 mm OD)0.25 µm film 726058.10 – 726058.15 726058.25 726058.30 726058.50 726058.600.50 µm film 726064.10 – 726064.15 726064.25 726064.30 726064.50 726064.601.00 µm film – – – – 726965.30 – –

0.32 mm ID (0.5 mm OD)0.10 µm film – – – 726317.25 726317.30 726317.50 726317.600.25 µm film 726318.10 – 726318.15 726318.25 726318.30 726318.50 726318.600.35 µm film 726824.10 – 726824.15 726824.25 726824.30 726824.50 726824.600.50 µm film – – – 726320.25 726320.30 726320.50 726320.601.00 µm film – – – 726929.25 726929.30 726929.50 726929.60

0.53 mm ID (0.8 mm OD)1.00 µm film 726545.10 – 726545.15 726545.25 726545.30 – –2.00 µm film 726735.10 – 726735.15 726735.25 726735.30 726735.50 –



MN


322



Max. temperature for isothermal operation 300 °C, max.temperature for short isotherms in a temperature pro-gramme 320 °CMedium polarIdeal for pesticide analysesSimilar phases: HP-1301, DB-1301, SPB-1301,Rtx-1301, CP-1301, 007-1301

6% cyanopropyl-phenyl – 94% dimethylpolysiloxane

CH3

O Si

CH3 m

O Si

n(CH2)3

CN


0.25 mm ID (0.4 mm OD)0.25 µm film – – – 726771.25 726771.30 726771.50 726771.60

0.32 mm ID (0.5 mm OD)0.25 µm film – – – 726777.25 726777.30 726777.50 726777.601.00 µm film – – – 726780.25 726780.30 726780.50 726780.60

0.53 mm ID (0.8 mm OD)1.00 µm film 726783.10 – – 726783.25 – – –



2106

20

2106

50

Analysis of a pesticide mixture Capillary column: OPTIMA® 1301, 0.25 µm film, 60 m x 0.25 mm ID, max. temperature 300/320 °C, Cat. No. 726 771.60 Injection: 3 µl, 80 °C (1 min) → 250°C (1 min), pulsed

splitlessCarrier gas: He, 54 ml/minTemperature: 80 °C (2 min) → 190 °C, 20 °C/min (12 min) →

240 °C, 2 °C/min (23 min) → 260°C, 10 °C/min (20 min)

Detector: ECDPeaks (0,1 ng/µl): 1. Propyzamide2. Vinclozolin3. Bromophos-ethyl4. 2,4-DDT5. Brompropylate

1

2

3

4

5

0 20 40 60min 0 20 40 60min

1

23

4

56

Analysis of a PCB mixtureCapillary column: OPTIMA® 1301, 0.25 µm film, 60 m x 0.25 mm ID, max. temperature 300/320 °C, Cat. No. 726 771.60Injection: 3 µl, 80 °C (1 min) → 250°C (1 min), pulsed

splitlessCarrier gas: He, 54 ml/minTemperature: 80 °C (2 min) → 190 °C, 20 °C/min (12 min) →

240 °C, 2 °C/min (23 min) → 260°C, 10 °C/min (20 min)

Detector: ECDPeaks (0,1 ng/µl): 1. PCB 282. PCB 523. PCB 1284. PCB 1535. PCB 1386. PCB 180

MN


323



Max. temperature for isothermal operation 280 °C, max.temperature for short isotherms in a temperature pro-gramme 300 °CMedium polarRecommended for environmental analysesSimilar phases: HP-624, HP-VOC, DB-624, DB-VRX,SPB-624, CP-624, RTX-624, RTX-Volatiles, 007-624,BP624, VOCOLUSP G 43

cyanopropyl-phenyl-dimethylpolysiloxane

Separation of volatile hydrocarbons by Headspace GCColumn: OPTIMA® 624, 1.8 µm film, 50 m x 0.32 mm ID, max. temperature: 280/300 °C, Cat. No. 726787.50, Injection: HS cryofocussion, splitless, 150 °CCarrier gas: N2, 2.11 ml/minTemperature: 36 °C (4 min), → 200 °C, 10 °C/min, (2 min)Detector: ECD, 260 °C

Peaks: 1. Dichloromethane (6,69 min)2. trans-1,2-Dichloroethene (7,27 min)3. cis-1,2-Dichloroethene (8,96 min)4. Trichloromethane (9,46 min)5. 1,1,1-Trichloroethane (9,85 min)6. Tetrachloromethane (10,17 min)7. Trichloroethene (11,44 min)8. 1,1,2-Trichloroethane (13,94 min)9. Tetrachloroethene (14,36 min)

Chromatogram courtesy of R. Mueller, G&P Torsten Plaar Umweltanalytik, Oldenburg, Germany

1

23

4 5

67

8

9

0 5 10 15 min

0

500

2103

30


0.2 mm ID (0.4 mm OD)1.10 µm film – – – 726784.25 – – –

0.25 mm ID (0.4 mm OD)1.40 µm film – – – 726785.25 726785.30 726785.50 726785.60

0.32 mm ID (0.5 mm OD)1.80 µm film – – – 726787.25 726787.30 726787.50 726787.60

0.53 mm ID (0.8 mm OD)3.00 µm film – – – 726789.25 726789.30 – –



MN


324



Max. temperature for isothermal operation 260 °C, max.temperature for short isotherms in a temperature pro-gramme 280 °CPolarRecommended for environmental analysesSimilar phases: OV-210, DB-210, Rtx-200, 007-210close equivalent to USP G 6

trifluoropropyl-methylpolysiloxane (50% trifluoropropyl)

CH

3

O Si

n

(CH

2

)

2

CF

3

Aromatic hydrocarbons (BTX)Capillary column: OPTIMA® 210, 0.5 µm film,

50 m x 0.25 mm ID, max. temperature 240/260 °C, Cat. No. 726874.50

Chromatographic conditions:Injection volume: 0.5 µlCarrier gas: 130 kPa N2 (1.1 ml/min)Split: 105 ml/minTemperature: 50 °CDetector: FID, 250 °C, 26

Peaks: 1. Benzene2. Toluene3. Ethylbenzene4. p-Xylene5. m-Xylene6. o-Xylene

2002

30

1 2

3

4

5

6

0 10 20min

Ordering information Cat. No.

for column length of10 m 15 m 25 m 30 m 50 m 60 m

0.25 mm ID

(0.4 mm OD)0.25 µm film

– 726871.15 726871.25 726871.30 726871.50 726871.60

0.50 µm film

726874.10 726874.15 726874.25 726874.30 726874.50 726874.600.32 mm ID


– 726877.15 726877.25 726877.30 726877.50 726877.60

0.50 µm film

– 726880.15 726880.25 726880.30 726880.50 726880.60



MN


325


OPTIMA

®

high performance capillary columns

Max. temperature for isothermal operation 260 °C, max.temperature for short isotherms in a temperature pro-gramme 280 °CPolarRecommended for fatty acid analysesSimilar phases: DB-225, HP-225, SP-2330, OV-225,Rtx-225, CP-SIL 43, 007-225, BP225close equivalent to USP G 7

CH

3

O Si

n

O Si

(CH

2

)

3

CN

CH

3

50% cyanopropyl-methyl – 50% phenylmethylpolysiloxane


for column length of15 m 25 m 30 m 50 m 60 m

0.25 mm ID


726118.15 726118.25 726118.30 726118.50 726118.600.32 mm ID


726352.15 726352.25 726352.30 726352.50 726352.60



Analysis of FAME in porcine fatColumn: OPTIMA® 225, 0.25 µm film, 25 m x 0.32 mm ID, max. temperature 260/280 °C, Cat. No. 726352.25 Injection volume: 1 µl, split 1:40Carrier gas: 60 kPa H2Temperature: 50 °C (2 min) → 125 °C, 30 °C/min → 160 °C, 5 °C/min → 180 °C, 20 °C/min → 200 °C, 3 °C/min → 220 °C, 20 °C/min (10 min)Detector: FID 260 °CPeaks:

1. C 4:0 2. C 5:0 3. C 6:0 4. C 8:0 5. C 10:06. C 11:07. C 12:08. C 13:09. C 13:1

10. C 14:011. C 14:112. C 15:013. C 15:114. C 16:015. C 16:116. C 17:017. C 17:1

18. C 18:019. C 18:120. C 18:221. C 18:322. C 19:023. C 20:024. C 20:125. C 20:226. C 20:427. C 20:328. C 20:529. C 22:030. C 22:131. C 22:232. C 22:633. C 24:034. C 24:1

Chromatograms courtesy of Dr. Bantleon, Mr. Leusche, Mr. Hagemann, VFG-Labor, Versmold, Germany

1

0

0

2

3 4

5

5

6

7 8 10 14 15 1819

20

9 11

10

10

20 min

13

12

15

mV

17

16

23

21

22

24

25

26 27

29

28

30

31 32

3334

0

0

5

8

2

5 7

10

11 12

15

14 18 2019

16

17

21

22

23

24

25

2627 32

10

10

20 min

15

mV

FAME standard FAME in porcine fat

2100

60

MN


326


OPTIMA

®


Max. temperature for isothermal operation 260 °C, max.temperature for short isotherms in a temperature pro-gramme 280 °CHighly polarRecommended for FAMEs, dioxins

No similar phases

33% cyanopropyl-methyl – 67% dimethylpolysiloxane

CH

3

O Si

CH

3 m

O Si

n

(CH

2

)

3

CN

CH

3


for column length of15 m 25 m 30 m 50 m 60 m

0.25 mm ID


726089.15 726089.25 726089.30 726089.50 726089.60

0.50 µm film

– 726090.25 726090.30 726090.50 726090.600.32 mm ID


– 726091.25 726091.30 726091.50 726091.60

0.35 µm film

– 726095.25 726095.30 726095.50 726095.60

0.50 µm film

– 726096.25 726096.30 726096.50 726096.60



Fatty acid methyl esters cis/trans C 18:1 (FAME)Capillary column: OPTIMA® 240, 0.25 film, 60 m x 0.25 mm ID, max. temperature 260/280 °C, Cat. No. 726089.60Chromatographic conditions:Sample: FAME mixture Injection volume: 1.0 µl, split 1 : 25Carrier gas: 150 kPa H2Temperature: 80 °C → 120 °C, 20 °C/min → 260 °C (10 min), 3 °C/minDetector: FID, 280 °CPeaks:

1. C 4:02. C 5:03. C 8:04. C 10:05. C 11:06. C 12:07. C 13:08. C 14:09. C 14:1

10. C 15:011. C 15:112. C 16:013. C 16:114. C 17:015. C 17:116. C 18:0

17. trans-C 18:118. cis-C 18:119. C 18:220. C 18:321. C 18:322. C 20:023. C 20:124. C 20:225. C 20:326. C 20:427. C 20:328. C 22:029. C 22:130. C 22:331. C 24:1

12

3

4 5

6

7

8

9

10

11

12

13

14

1516

1718

19

2021

2223

24

252627

2829

30

31

10 20 30 40 50min

3

mV

2016

20

MN


327


OPTIMA

®


max. temperature for isothermal operation 180 °C, max.temperature for short isotherms in a temperature pro-gramme 240 °Cmost polar phases of the MN column rangerecommended for dioxines, furanes, FAMEssimilar phases: SP-2340, CP-SIL 88

CN-100CN-100CN-100NEW!NEW!

O Si

n(CH2)3

CN

(CH2)3

CN

100% cyanopropyl-polysiloxane

Ordering information Cat. No. for a column length of60 m

0.25 mm ID (0.4 mm OD)0.25 µm film 726609.60



Analysis of furanesCapillary column: OPTIMA® CN-100, 0.25 µm film, 60 m x 0.25 mm ID, max. temperature 180/240 °C, Cat. No. 726609.60Chromatographic conditions:Injection: 1.0 µl, 275 °CCarrier gas: H2, 40 cm/s (3.2 cc/min)Temperature: 200 °C (1 min) → 240 °C (6 min), 3 °C/min → 275 °C (30 min), 15 °C/minDetector: ECD, 275 °CPeaks:

1. 1,3,6,8-TCDF2. 1,3,7,8-TCDF, 1,3,7,9-TCDF3. 1,3,4,7-TCDF4. 1,4,6,8-TCDF5. 1,2,4,7-TCDF, 1,3,6,7-TCDF6. 1,3,4,8-TCDF7. 1,2,4,8-TCDF, 1,3,4,6-TCDF8. 1,2,4,6-TCDF, 1,3,6,9-TCDF,

1,4,7,8-TCDF, 1,2,6,8-TCDF, 1,2,3,7-TCDF

9. 1,2,3,4-TCDF, 1,6,7,8-TCDF10. 1,2,3,8-TCDF, 1,4,6,7-TCDF,

2,4,6,8-TCDF, 1,2,3,6-TCDF11. 1,3,4,9-TCDF12. 1,2,7,8-TCDF13. 1,2,6,7-TCDF, 1,2,7,9-TCDF14. 1,2,4,9-TCDF, 2,3,6,8-TCDF15. 2,4,6,7-TCDF16. 1,2,3,9-TCDF, 2,3,4,7-TCDF17. 1,2,6,9-TCDF18. 2,3,7,8-TCDF19. 2,3,4,8-TCDF20. 2,3,4,6-TCDF21. 2,3,6,7-TCDF22. 3,4,6,7-TCDF23. 1,2,8,9-TCDF

1

2

3

4

5

6

7

8

9

10

11

12

13

14

15

16

17

18

19

20

21

22

23

12 14 16 18 20 min

{

2111

50

MN


328



max. temperature for isothermal operation 250 °C, max.temperature for short isotherms in a temperature pro-gramme 260 °Cpolarrecommended for solvent analysis and alcoholssuitable for aqueous solutionssimilar phases: DB-Wax, Supelcowax, HP-Wax, HP-INNOWAX, Rtx-Wax, CP-Wax 52 CB, Stabilwax, 007-CW, BP20, AT-Wax, ZB-WaxUSP G 16

WAXWAXWAXWAXWAXWAXWAXpolyethylene glycol 20000 dalton

H

H

O C

n

H OH

H

H

C

Ordering information Cat. No. for a column length of25 m 30 m 50 m 60 m

0.25 mm ID (0.4 mm OD)0.25 µm film 726600.25 726600.30 726600.50 726600.60

0.32 mm ID (0.5 mm OD)0.25 µm film 726321.25 726321.30 726321.50 726321.600.35 µm film 726296.25 726296.30 726296.50 726296.60



0 5 10 15 20 25

0

200000

400000

600000

800000 12 3 4

5

6 78 9

Grob testCapillary column: OPTIMA® WAX, 0.5 µm film, 50 m x 0.32 mm ID, max. temperature 250/260 °C, Cat. No. 726296.50Chromatographic conditions:Injection volume: 1 µlCarrier gas: 1.2 bar HeSplit: 1:20Temperature: 80 °C → 250 °C, 8 °C/minDetector: FID, 250 °CPeaks:1. Decane2. Undecane3. Octanol4. Methyl decanoate5. Dicyclohexylamine6. Methyl undecanoate7. Methyl dodecanoate8. 2,6-Dimethylaniline9. 2,6-Dimethylphenol

2111

70

NEW!NEW!

MN


329



max. temperature for isothermal operation 250 °C, max.temperature for short isotherms in a temperature pro-gramme 260 °Cpolarrecommended for FAMEs, free carboxylic acidssimilar phases: DB-FFAP, HP-FFAP, CP-SIL 58 CB, 007-FFAP, CP-FFAP CB, Nukolclose equivalent to USP G 35

FFAPFFAPFFAPFFAPpolyethylene glycol 2-nitroterephthalate

Ordering information Cat. No. for a column length of25 m 30 m 50 m 60 m

0.25 mm ID (0.4 mm OD)0.25 µm film 726116.25 726116.30 726116.50 726116.60

0.32 mm ID (0.5 mm OD)0.25 µm film 726341.25 726341.30 726341.50 726341.600.35 µm film 726344.25 726344.30 726344.50 –



0 10 20 30 40 50 60 70

0

6

12

18

1

23

4

5

67

8

9

1011

1213

14 15

FAME testCapillary column: OPTIMA® FFAP, 0.25 µm film, 60 m x 0.32 mm ID, max. temperature 250/260 °C, Cat. No. 726341.60Chromatographic conditions:Carrier gas: 1,2 bar He, splitTemperature: 55 °C → 250 °C, 6 °C/min Injector: 220 °C Detector: 220 °C Peaks:

1. C42. C63. C84. C105. C126. C147. C168. C189. C18:1 c/t

10. C18:211. C18:312. C2013. C2214. C22:115. C24

2111

40

NEW!NEW!

MN


330


Max. temperature for isothermal operation 300 °C, max.temperature for short isotherms in a temperature pro-gramme 320 °C

Max. temperature for isothermal operation 300 °C, max.temperature for short isotherms in a temperature pro-gramme 320 °C

PERMABOND® SE-30PERMABOND® SE-30 CH3

O Si

CH3 n

100% dimethylpolysiloxane

Ordering information Cat. No. for column length of10 m 25 m 50 m

0.25 mm ID (0.4 mm OD)0.25 µm film 723052.10 723052.25 723052.500.50 µm film 723087.10 723087.25 723087.50

0.32 mm ID (0.5 mm OD)0.25 µm film – 723306.25 723306.500.50 µm film 723308.10 723308.25 723308.50



PERMABOND® SE-52PERMABOND® SE-52CH3

O Si

CH3 m

O Si

n

5% phenyl – 95% dimethylpolysiloxane

CH3

Ordering information Cat. No. for column length of25 m 50 m

0.25 mm ID (0.4 mm OD)0.25 µm film 723054.25 723054.50

0.32 mm ID (0.5 mm OD)0.25 µm film 723310.25 723310.500.50 µm film 723312.25 723312.50



PERMABOND® capillary columns

MN


331


Max. temperature for isothermal operation 220 °C, max.temperature for short isotherms in a temperature pro-gramme 240 °CPolarRecommended for solvent analyses and alcoholsSuitable for aqueous solutionsSimilar phases: DB-Wax, Supelcowax, HP-Wax, HP-INNOWAX, Rtx-Wax, CP-Wax 52 CB, Stabilwax,007-CWUSP G 16

Max. temperature for isothermal operation 220 °C, max.temperature for short isotherms in a temperature pro-gramme 240 °CPolarRecommended for FAMEs, free carboxylic acidsSimilar phases: DB-FFAP, HP-FFAP, CP-SIL 58 CB, 007-FFAP, CP-FFAP CB, Nukol

PERMABOND® CW 20 MPERMABOND® CW 20 Mpolyethylene glycol H

H

O C

n

H OH

H

H

C

20000 dalton

Ordering information Cat. No. for column length of10 m 25 m 30 m 50 m 60 m

0.1 mm ID (0.4 mm OD)0.10 µm Film 723064.10 – – – –

0.25 mm ID (0.4 mm OD)0.25 µm film 723060.10 723060.25 723060.30 723060.50 723060.60

0.32 mm ID (0.5 mm OD)0.25 µm film 723321.10 723321.25 723321.30 723321.50 723321.600.35 µm film 723827.10 723827.25 – 723827.50 –0.50 µm film 723296.10 723296.25 723296.30 723296.50 723296.60

0.53 mm ID (0.8 mm OD)0.50 µm film 723515.10 723515.25 – – –1.00 µm film 723549.10 723549.25 723549.30 – –2.00 µm film 723517.10 723517.25 723517.30 723517.50 –


PERMABOND® FFAPPERMABOND® FFAPpolyethylene glycol 2-nitroterephthalic acid ester

Ordering information Cat. No. for column length of10 m 25 m 30 m 50 m 60 m

0.1 mm ID (0.4 mm OD)0.10 µm Film 723180.10 – – – –0.25 µm Film 723181.10 – – – –

0.25 mm ID (0.4 mm OD)0.10 µm film 723936.10 723936.25 – 723936.50 –0.25 µm film 723116.10 723116.25 723116.30 723116.50 723116.60

0.32 mm ID (0.5 mm OD)0.10 µm film 723356.10 723356.25 – 723356.50 –0.25 µm film 723341.10 723341.25 723341.30 723341.50 723341.600.35 µm film 723830.10 723830.25 – 723830.50 –0.50 µm film 723344.10 723344.25 723344.30 723344.50 723344.60

0.53 mm ID (0.8 mm OD)1.00 µm film 723555.10 723555.25 – 723555.50 –



PERMABOND® capillary columns

MN


332


OPTIMA® and PERMABOND® capillary columns

Important hints for use and maintenance of capillary columns

Oxygen-free carrier gas

Generally, use of oxygen-free carrier gas is recommendedfor all stationary phases, however, it is of vital importance forthe phases Carbowax 20M and FFAP, which are easily oxi-dised by traces of air. Remove the oxygen by passing thecarrier gas through an oxygen absorber cartridge (e.g.Oxisorb® cartridge, see page 370), which should beexchanged before it is completely exhausted.Lifetime of a column can also be increased, if you do notexceed the temperature limits indicated for each phase. Ifyou have any difficulties with your new MN column, pleasecontact us immediately, before the column is damaged oreven rendered worthless by improper handling.Flushing of capillary columns with immobilised phases

Immobilisation of a phase in a capillary column allowsremoval of contaminations by flushing with solvents. Forflushing we recommend the “inert” solvents usually appliedfor dissolving samples, such as e.g. methanol, methylenechloride, alkanes like pentane or aromatics like toluene.Aggressive substances, e.g. trifluoroacetic acid, chlorosi-lanes or alkalis etc. are not to be used. After flushing the col-umn should be dried with carrier gas at room temperatureand heated to the maximum allowed temperature (see certif-icate) with a slow temperature programme (about 2 °C/min).For our flushing unit for capillary columns with chemicallybonded phases, please see our range of capillary accessorieson page 365.Storage and conditioning

If capillary columns are not used for an extended period oftime, they should be stored closed and protected from light(FFAP, CW 20 M and Wax).

Prior to use capillary columns (especially with immobilisedphases) should be conditioned for several hours, ideally overnight, because basic substances, such as dicyclohexylaminefrom Grob test mixture, can be absorbed partially or evencompletely.

GC capillary columns for special applications · SummaryInstead of using standard columns, certain analytical separa-tion tasks can be performed more easily with chromato-graphic columns, which have been especially developed for

the respective problem. The following table summarises ourprogramme of GC speciality capillaries, the individual col-umn types are described in detail on the following pages.

Procedure for column conditioning(described here for an OPTIMA® 1 column with 0.25 µmfilm, 25 m length and 0.25 mm ID):

Install the column in the chromatograph observing thesafety precautionsHeat the column from ambient temperature to themaximum temperature allowed for isothermal opera-tion (first temperature in our descriptions, in this case340 °C) with about 2 °C/min using a carrier gas pres-sure of 0.5 barLeave the column at this temperature over night

As an alternative, you may use the following procedure:Apply a temperature programme with a heating rate of10 °C/min from 60 °C to the maxiumum temperatureallowed for temperature programmes (second tem-perature in our descriptions, in this case 360 °C) andrepeat it at least three times (better 5 times)

After these procedures the test chromatogram with theMN OPTIMA® test mixture (Cat. No. 722313) should bereproduced.Attention! When using ECD or MS detection or for columnswith a film thickness ≥ 1 µm the column should be sepa-rated from the detector during conditioning.

Separation problem / preferred application Recommended capil-lary column

Page

Volatile substances solvent analyses OPTIMA® 1 thick film columns (≥ 3 µm film) 316

for analytes in an aqueous matrix OPTIMA® 5 thick film columns (≥ 3 µm film) 318

OPTIMA® 624 323

Fast GC OPTIMA® δ-3, OPTIMA® δ-6OPTIMA® 1, OPTIMA® 5, OPTIMA® 17PERMABOND® CW 20 M, FFAPall 0.10 mm ID 334

Amines especially for polyfunctional amines OPTIMA® 5 Amine335

basic for amine separations FS-CW 20 M-AM

FAMEs Selecta® FAME plus 336

MN


GC capillary columns for special applications · Summary

333


Capillary columns with thick films

Chromatography of highly volatile substances requires athick film of stationary phase. The increased retention raiseselution temperatures far above room temperature, thusavoiding costly cooling of the chromatograph below ambienttemperature (see lower figure on page 309). Furthermore,problems caused by aqueous solutions on nonpolar station-ary phases are reduced or completely avoided. The increasein film thickness results in a very high capacity and inertness.This is especially useful for samples with widely differingconcentrations, or for the separation of volatile polar sub-stances as shown in the chromatogram on the right.Extremely active substrates present a special situation. Inmost cases such substances cause noticeable tailing, if theycome in contact with uncoated spots of the column wall.These interactions can be reduced by use of short columnswith thick films. This means a better coverage of the columnwall by the thicker film and a reduction of the column surfacedue to the reduced length.However, thick films also mean more phase in the column,and consequently higher bleeding. This results in lower max-imum operating temperatures for thick film columns.For ordering information see pages 316 and 318.

Petrochemical products (complex hydrocarbon mixtures) PERMABOND® P-100 338

Environmental analyses

volatile halogenated hydrocarbons PERMABOND® SE-54 HKW 339

PAH, PCB, pesticides, dioxins etc. OPTIMA® 1, OPTIMA® 1 MS 316

OPTIMA® 5, OPTIMA® 5 MS 318

OPTIMA® δ-3 314

OPTIMA® δ-6 315

Triglycerides OPTIMA® 1-TG340

OPTIMA® 17-TG

Silanes (monomeric, e.g. chlorosilanes) PERMABOND® Silane 341

Diethylene glycol, e.g. for the quality control of wine PERMABOND® CW 20 M-DEG 341

Enantiomer separation diamide type chiral polysiloxane PERMABOND® L-CHIRASIL-VAL 346

cyclodextrin phases FS-LIPODEX® A, FS-LIPODEX® BFS-LIPODEX® C, FS-LIPODEX® DFS-LIPODEX® E, FS-LIPODEX® G

342FS-HYDRODEX® β-PMFS-HYDRODEX® β-3 PFS-HYDRODEX® β-6-TBDM

SFC capillary columns with 0.05 mm ID, with or without integrated restriction

on request –

Separation problem / preferred application Recommended capil-lary column

Page

Alcohols in methylene chlorideCapillary column: PERMABOND® SE-54, 5,0 µm film, 25 m x 0,32 mm ID, max. temp. 280 °C, or corresponding column OPTIMA® 5, Cat. No. 726934.25Chromatographic conditions:Injection volume: 2 µlCarrier gas: 1 bar N2Split: 30 ml/minTemperature: 60 °CDetector: FID, 240 °C, 23

Peaks:1. Methanol2. Ethanol3. i-Propanol4. Methylene chloride5. Propanol

12

3

4

5

0 2 4 6 8 10 min

2014

60

MN


GC capillary columns for special applications · Fast GC

334


Fast GC columnsEfficiency in a laboratory is more and more determined bythe sample throughput. The higher the number of samplesper time unit run on an instrument, the higher is the produc-

tivity of the system. In industrial and commercial laboratorieshigh sample numbers are the rule. It is of high priority toobtain results as fast as possible. Since, for conventionalstandard analyses the analytical cycle (total measuring andcooling time) is 10 to 60 minutes, depending on the numberof components, productivity is limited by the high timerequirements. Thus it is necessary to shorten the analyticalcycle in order to reach a higher sample throughput.State-of-the-art instrumentation, and recent column develop-ment meet this demand with terms like high-speed GC, fastGC, very fast GC, ultra-fast GC. These stand for differentapproaches and techniques, which have been developedduring the past years to obtain faster GC separations, with-out loss of resolution. Apart from simultaneous decrease ofcolumn diameter and length, efforts center on temperature-programmed GC with extremely high heating rates, a sharpfocussing of the injected sample and high flow rates.Use of a column with smaller inner diameter combined withvery fast temperature programmes can reduce the analysistime by up to 80%, if the injection technique, and also thedetection and data acquisition speed are suited for thismethod. The amount of sample, which can be injected, is ofcourse limited by the inner diameter of the column and thethin film. It is important to find the optimum between fastchromatography and the resolution required. A reduction ofthe inner diameter is related to a higher column inlet pres-sure (head pressures of up to 10 bar), and a lower volumeflow of the mobile phase, as well as smaller peak widths andsample capacities. This requires the very fast injection ofvery small sample volumes against a high pressure. Highsensitivity detectors with small volume and extremely shortresponse time, as well as a very rapid data acquisition, andprocessing are required. If using e.g. a mass spectrometerfor the evaluation of data, scan rates of up to 6750 dalton/sare necessary to obtain sufficient data points for integration. Stationary phases for fast GC have to meet special demandsdue to the high heating rates applied. It is necessary to usespecially bonded phases in order to prevent column bleed-ing. The manufacturing process of the OPTIMA® columnsmeets exactly this requirement. OPTIMA® columns showvery low bleeding and provide long lifetimes, even when con-tinuously subjected to high heating rates.Reference:C. A. Cramers et al., J. Chromatogr. 856 (1999) 315 – 329C. A. Cramers et al., J. Chromatogr. 842 (1999) 3 – 13

Comparison of a separation on a 50 m standard capil-lary with separation on a 10 m fast GC column

A) Fast GC columnCapillary column: OPTIMA® 5, 0.1 µm film, 10 m x 0.1 mm ID, max. temperature 340/360 °C, Cat. No. 726846.10injection 1 µl, split 1 : 40, carrier gas 0.75 bar HeB) Standard GC columnCapillary column: OPTIMA® 5, 0.25 µm film, 50 x 0.25 mm ID, max. temperature 340/360 °C, Cat. No. 726056.50injection 1 µl, split 1 : 35, carrier gas 1.5 bar Heboth separations: temperature: 80 °C → 320 °C (10 min), 8 °C/min, detector: FID

While maintaining the temperature pro-gramme and halving the pressure a time saving of 30 % results with identi-cal separation efficiency

Peaks:1. Octanol2. Undecane3. Dimethylaniline4. Dodecane5. Decylamine6. Methyl decanoate 7. Methyl undeca-

noate8. Henicosane9. Docosane

10. Tricosane

1

2

3

4

5

6 78 910

0 10 20 min

1 2 3 45

6 7

8

910

0 10 20 min30

2112

60

Columns for fast GC Ordering information

Phase max. temperature ID [mm] film thickness [µm] Cat. No. (10 m) Cat. No. (20 m)OPTIMA® δ-3 340/360 °C 0,10 0,10 726410.10 726410.20OPTIMA® δ-6 340/360 °C 0,10 0,10 726490.10 –OPTIMA® 1 340/360 °C 0,10 0,10 726024.10 726024.20

0,10 0,40 – 726025.20OPTIMA® 5 340/360 °C 0,10 0,10 726846.10 –OPTIMA® 17 320/340 °C 0,10 0,20 726848.10 –PERMABOND® CW 20 M 220/240 °C 0,10 0,10 723064.10 –PERMABOND® FFAP 220/240 °C 0,10 0,10 723180.10 723180.20

0,10 0,25 723181.10 –For a detailed description of individual phases please see pages 312 – 331

MN


GC capillary columns for special applications – amine separations

335


OPTIMA® 5 Amine – the special column for theanalysis of aminesThe columns OPTIMA® 5 Amine have especially been devel-oped for the analysis of polyfunctional amines such as e.g.ethanolamines, amino-functionalised diols and similar com-pounds. This group of substances, which are important basicmaterials in industrial chemistry, shows strong tailing onstandard-deactivated columns. The OPTIMA® 5 Amine, how-ever, is deactivated with a special procedure, which enablesthe chromatography of these critical compounds. OPTIMA®

5 Amine columns also feature an improved linearity for thedetermination of active components at trace levels: thuseven for aliphatic and aromatic amines at concentrations of100 pg/peak they show practically no amine absorptions. All OPTIMA® 5 Amine columns are tested with the OPTIMA®

Amine test mixture (Cat. No. 722317), which among othersalso contains diethanolamine and propanol-pyridine. Thistest mixture is supplied with each column.

Similar phases: RTX Amine, PTA-5

FS-CW 20 M-AMPolyethylene glycol 20000 These are non-immobilised capillary columns based on poly-ethylene glycol, basic for amine separations.

Similar phases: Carbowax Amine, CP-Wax 51, CAM,Stabilwax DB

Separation of secondary and tertiary aminesCapillary column: OPTIMA® 5 Amine, 0.5 µm film, 30 m x 0.25 mm ID, max. temp. 300/320 °C, Cat. No. 726354.30Chromatographic conditions:Injection volume: 1 µlCarrier gas: 0.6 bar H2, split 1:100Temperature: 100 °C (3 min) → 280 °C, 10 °C/minDetector: FID, 280 °CPeaks:

1. Diethylamine2. Di-isopropylamine3. Triethylamine4. Di-n-propylamine5. Di-n-butylamine6. Tri-n-propylamine

7. Di-isobutylamine8. Tri-n-butylamine9. Di-isohexylamine

10. Dicyclohexylamine11. Dibenzylamine12. Tri-n-hexylamine

1

23

4

56

78

9

10

1112

10 20 min

2102

80

Ordering information Cat. No. for column length of10 m 25 m 30 m 50 m

OPTIMA® 5 Amine, OPTIMA® 5 with special deactivation, tested with critical amines, max. temp. 300/320 °C

0.1 mm ID (0.4 mm OD)0.40 µm film 726361.10 – –

0.2 mm ID (0.4 mm OD)0.35 µm film 726355.25 –

0.25 mm ID (0.4 mm OD)0.50 µm film – 726354.301.00 µm film – 726358.30

0.32 mm ID (0.5 mm OD)0.25 µm film – 726360.301.00 µm film – 726353.301.50 µm film – 726356.30

0.53 mm ID (0.8 mm OD)1.00 µm film – 726359.303.00 µm film – 726357.30

Capillary columns FS-CW 20 M-AM, basic for amine separations, max. temp. 220/240 °C

0.1 mm ID (0.4 mm OD)0.20 µm film 733111.10 – –

0.25 mm ID (0.4 mm OD)0.25 µm film – 733110.25 733110.50

0.32 mm ID (0.5 mm OD)0.25 µm film – 733299.25 733299.50

0.53 mm ID (0.8 mm OD)1.00 µm film 733551.10 733551.25 –

MN


GC capillary columns for special applications – FAME separations

336


Selecta® FAME plusOptimum cis/trans separation of FAMEsBetter separation numbers than FFAP or CW 20 MHigher polarity than carbowaxGood temperature stability (180 / 240 °C)Low column bleedEach column tested with FAMEs and supplied with FAME test certificate

With Selecta® FAME plus MACHEREY-NAGEL offers avery polar column with high cyanopropyl content. This column is very well suited for the analysis of fatty acidmethyl esters (FAMEs) and especially of their cis/trans iso-mers. Food legislation requires optimum separation forcis/trans C18-, C20 isomers, and this is easily achieved withSelecta® FAME plus columns. The high temperature stabilityallows separation of higher fatty acids (C23, C24) as well. Each column is individually tested with a 16-componentFAME mixture, which is then supplied with the column. Thusthe user can check the column performance at any time.Our recommendation for sample preparation: Methylation with TMSH is very well suited for sample prepa-ration of fatty acids. Lipids or triglycerides are converted tofatty acid methyl esters by a simple transesterification (seepage 353). Isomerisation of multiple unsaturated fatty acidshas not been observed.References:D. Lennartz, GIT Spezial Separation 2/2000, 82 – 83

25

1

2

3

4

56

7

8 910

11 /12

30 35

Separation of FAMEs from rape oilSince long free fatty acids have high boiling points, all samples have to be derivatised with TMSH (trimethylsulphonium hydrox-ide) prior to injection. For this purpose dissolve 100 mg sample in 5 ml tert.-butylmethylether. Take 100 µl of this sample, add 50 µl TMSH and inject directly. Due to the high reactivity of the reagent complete reaction is allready obtained at ambient temperature. Removal of excess reagent is not necessary, because in the in-jector block of the GC at 250 °C it is pyrolysed to form volatile methanol and dimethylsulphide .Column: SELECTA® FAME plus, 60 m x 0.25 mm ID

max. temperature 180/240 °C, Cat. No. 725530.60Carrier gas: 1.4 bar HeliumInjection: 1 µl, split: 1:30Temperature: 100 °C → 240 °C, 4 °C/min (10 min)Detector: FID, 250 °CSample: rape oilPeaks:1. C 16:02. C 16:13. C 18:04. C 18:1 cis isomers5. C 18:2 9cis,12trans6. C 18:2 9trans,12cis

7. C 18:2 cis isomers8. C 20:09. C 18:3 9cis,12cis,15trans10. C 18:3 9trans,12cis,15cis11. C 18:3 9cis,12cis,15cis12. C 20:1

2113

10

Ordering information Cat. No. for column length of60 m

Selecta® FAME plus for analysis of fatty acid methyl estersMN phase with the highest cyanopropyl contentmax. temperature for isothermal operation 180 °C, max. temperature for short isotherms in a temperature programme 240 °C0.25 mm ID (0.4 mm OD 725530.60

NEW!

MN


GC capillary columns for special applications – FAME separations

337


C6:0

30.0 min10.00.0 20.0

C8:0

C10:0

C10:1

C12:0

C14

:1

C14:0

C15

:0

C16:0

C16

:1C

17:0

C18:0 C18:1 cis

C18

:1 t

ran

s

C18

:2n

6 c

is

C18

:3n

3

FAMEs in butterColumn: Selecta® FAME plus, 60 m x 0.25 mm ID,

Cat. No. 725 530.60Carrier: He, 1.2 barInjection: 1.0 µl; split 1:40

Sample: in tert.-butyl methyl etherTemperature: 100 °C → 250 °C, 4 °C/minDetection: FID, 250 °CPeaks: see chromatogram

2505

60

32

1

30.0 min10.00.0 20.0

2 3 4

5

6

7

8

9 10 11

12

13 14 15

16 18

17 19 20

21

22

23/24

2526

27

28

29/30

3133 36

34

3537

Separation of 37 FAMEsColumn: Selecta® FAME plus, 60 m x 0.25 mm ID,

Cat. No. 725530.60Carrier: He, 1.2 barInjection: 1.0 µl; split 1:40

Sample: in tert.-butyl methyl etherTemperature: 100 °C → 250 °C, 4 °C/min Detection: FID, 250 °C

Peaks: FAMEs1. C4:0; 2. C6:0; 3. C8:0; 4. C10:0; 5. C11:0; 6. C12:0; 7. C13:0; 8. C14:0; 9. C14:1; 10. C15:0; 11. C15:1; 12. C16:0; 13. C16:1; 14. C17:0; 15. C17:1; 16. C18:0;

17. C18:1 trans; 18. C18:1 cis; 19. C18:2n6 trans; 20. C18:2n6 cis; 21. C20:0; 22. C18:3n6; 23. C20:1; 24. C18:3n3; 25. C21:0; 26. C20:2; 27. C22:0; 28. C20:3n6; 29. C22:1n9; 30. C20:3n3; 31. C20:4n6; 32. C23:0; 33. C22:2; 34. C24:0; 35. C20:5n3; 36. C24:1; 37. C22:6n3

2505

70

MN


GC capillary columns for special applications – petrochemical products

338


Capillary columns for the GC analysis of petrochemical products

The analysis of complex mixtures of hydrocarbons requires acolumn with high resolution (e.g. for the separation of m- andp-xylene) and sufficient capacity, combined with a nonpolarstationary phase with a film thickness, which is not too high.

Our 100 m capillary column PERMABOND® P-100, which iscoated with dimethylpolysiloxane (0.5 µm film thickness and0.25 mm ID), meets these requirements. The chromatogramof unleaded gasoline show the performance of the column.

Ordering information Cat. No. for column length of100 m

PERMABOND® P-100 for petrochemical analyses dimethylpolysiloxane max. temperature for isothermal operation 300 °C, max. temperature for short isotherms in a temperature programme 320 °C

0.25 mm ID (0.4 mm OD)0.50 µm film 723890.100

GC analysis of unleaded gasoline a) Capillary column: PERMABOND® P-100, 0.50 µm film, 100 m x 0.25 mm ID, max. temp. 300/320 °C, Cat. No. 723890.100Chromatographic conditions:Injection volume: 0.5 µlCarrier gas: 200 kPa H2 (2.3 ml/min)Split: 70 ml/minTemperature: 35 °C (15 min) → 200 °C (5 min), 2 °C/minDetector: FID 250 °C, 27

Peaks:1. n-Pentane2. n-Hexane3. Benzene4. n-Heptane5. Toluene6. n-Octane7. Ethylbenzene8. m-Xylene9. p-Xylene

10. o-Xylene11. n-Nonane12. Methyl-3-ethylbenzene13. 1,3,5-Trimethylbenzene14. 1,2,4-Trimethylbenzene15. 1,2,3-Trimethylbenzene16. Naphthalene17. 2-Methylnaphthalene18. 1-Methylnaphthalene19. Dimethylnaphthalene isomers

1 2 3

4

5

6

7

8

9 10

11

12

13

14

15

16

1718

19

20 40 60 80 min

2000

70

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GC capillary columns for special applications – environmental analyses

339


Our capillaries OPTIMA® 1 and OPTIMA® 5 have proventheir outstanding performance for the GC analysis of PAH,pesticides, PCB, dioxin screening and similar separationproblems. For confirming analytical results, especially forcomplex samples, phases OPTIMA® 17 or OPTIMA® 1701are used. For the analysis of halogenated hydrocarbons wehave optimised the parameters for our columns with the well-known polysiloxane phase SE-54 and offer the special col-umn PERMABOND® SE-54 HKW with 25 or 50 m length. Asan alternative and for confirming the analytical results forhalogenated hydrocarbons, we recommend the column

OPTIMA® 624, which shows advantages especially for thedetermination of 1,1,2-trichlorotrifluoroethane (F 113) be-sides dichloromethane. Both phases are also suited for de-termination of vinyl chloride and separation of cis/trans-1,2-dichloroethene. Thanks to the high capacity which resultsfrom the high film thickness, these columns show such anoutstanding resolution, that for most separations 25 m col-umns are sufficient. However, for head-space techniques orwhen extremely complex mixtures have to be analysed, 50 mcolumns may be required. For GC-MS coupling we recom-mend the phase OPTIMA® 624 with 0.2 or 0.25 mm ID.

2 4 6 8 10 12

0

800000

1600000

2400000

Abundance

min

1

2

3

4

56

7

89

10

11

1213

14 15

1617

1819

2021

2223

Volatile halogenated hydrocarbons and BTXCapillary column: PERMABOND® SE-54-HKW, 25 m x 0.32 mm ID,

max. temperature 300 °C, Cat. No. 723945.25Chromatographic conditions:Injection volume: 0.5 µlCarrier gas: 2.2 ml/min HeSplit: 48 ml/minTemperature: 40 °C (5 min) → 160 °C, 10 °C/minDetector: MSD 5971

Peaks: about 0.2 % in methanol1. Ethanol2. Trichlorofluoromethane (F 11)3. Pentane4. 1,1,2-Trichlorotrifluoroethane (F 113)5. Dichloromethane6. trans-1,2-Dichloroethene7. Hexane8. cis-1,2-Dichloroethene9. Trichloromethane

10. 1,1,1-Trichloroethane11. 1,2-Dichloroethane12. Tetrachloromethane + benzene13. Trichloroethene14. Bromodichloromethane15. Toluene16. Dibromochloromethane17. Tetrachloroethene18. Chlorobenzene19. Ethylbenzene20. m- + p-Xylene21. Tribromomethane22. o-Xylene23. Bromobenzene 20

0140


PERMABOND® SE-54-HKW for volatile halogenated hydrocarbons SE-54 optimised for volatile halogenated hydrocarbonsmax. temperature for isothermal operation 300 °C, max. temperature for short isotherms in a temperature programme 320 °C0.32 mm ID (0.5 mm OD) 1.80 µm film 723945.25 723945.50

4 6 8 10 12 14 16 18

0

200000

400000

600000

800000Abundance

min

1

2

3

4

56

7

89

10

11

12

1314

15

16

17

1819

20

21

2223

Peaks: 1. Vinyl chloride2. Trichlorofluoromethane (F 11)3. Pentane4. 1,1,2-Trichlorotrifluoroethane (F 113)5. Dichloromethane6. trans-1,2-Dichloroethene7. Hexane8. cis-1,2-Dichloroethene9. Trichloromethane

10. 1,1,1-Trichloroethane11. Tetrachloromethane12. 1,2-Dichloroethane + benzene13. Trichloroethene14. Bromodichloromethane15. Toluene16. Tetrachloroethene17. Dibromochloromethane18. Chlorobenzene19. Ethylbenzene20. m- + p-Xylene21. o-Xylene22. Tribromomethane23. Bromobenzene

Volatile halogenated hydrocarbons and BTX Capillary column: OPTIMA® 624, 50 m x 0.25 mm ID, max. temperature 260 °C, Cat. No. 726785.50Chromatographic conditions:Injection volume: 1 µlCarrrier gas: 0.9 ml/min He (constant flow)

Split: 50 ml/minTemperature: 40 °C (5 min) → 160 °C, 10 °C/minDetector: MSD 5971

2001

60

MN


GC capillary columns for special applications – triglyceride analyses

340


OPTIMA® capillary columns for triglyceride analyses

The analysis of triglycerides is on the threshold to high tem-perature gas chromatography and requires short capillarycolumns (max. 25 m and 0.32 mm ID) with low-bleeding sta-tionary phases.Our OPTIMA® programme – featuring low-bleeding, ther-mally stable stationary phases with optimum deactivation –offers two types of columns for this purpose:

OPTIMA® 1-TG (similar phases: SPB-1 TG, DB-1 HT, 400-1 HT, HT-5)OPTIMA® 17-TG

The OPTIMA® 1-TG, 25 m x 0.32 mm ID (Cat. No.726132.25) is the best choice in terms of low bleed level andoffers separation according to carbon number.If you need a separation according to degree of unsaturation,you should choose the OPTIMA 17-TG (Cat. No. 726131.25,25 m and 0.32 mm ID for optimum separation efficiency).The chromatogram shows a typical separation of triglycer-ides on OPTIMA® 1-TG.


OPTIMA® 1-TG 100% dimethylpolysiloxane, max. temperature 370 °C0.25 mm ID (0.4 mm OD) 726133.10 726133.250.32 mm ID (0.5 mm OD) 726132.10 726132.25

OPTIMA® 17-TG phenyl-methyl-polysiloxane (50% phenyl), max. temperature 370 °C0.32 mm ID (0.5 mm OD) 726131.10 726131.25

Triglycerides (from butter)Capillary column: OPTIMA® 1-TG, 25 m x 0.32 mm ID, max. temperature 370 °C, Cat. No. 726132.25Chromatographic conditions:Injection volume: 0.5 µlCarrrier gas: 80 kPa H2Temperature: 80 °C (1 min) → 250 °C, 20 °C/min

→ 370 °C (10 min), 5 °C/minDetector: FID, 380 °C, 26

Peaks:1. Cholesterol2. T-303. T-344. T-385. T-426. T-467. T-508. T-54

1 2

3

4

56

7

8

0 10 20 30 40 min

160 278 328 370 °C

2017

90

MN


GC capillary columns for special applications

341


Capillary column for silane analyses

Our capillary column PERMABOND® Silane has not beendeveloped for the separation of trimethylsilyl derivatives, butespecially for the analysis of monomeric silanes and chlo-rosilanes. It is also suited for the separation of dimericsiloxanes and silazanes, as shown in the followingchromatogram.

Capillary column for the determination of diethyl-ene glycol

This capillary column is especially tested with diethylene gly-col and recommended for the determination of diethyleneglycol, e.g. for the quality control of wine.

4 6 8 10

0

500000

1000000Abundance

min

1

2 3

4

5

6

7

ChloromethylsilanesCapillary column: PERMABOND® Silane, 50 m x 0.32 mm ID, max. temp. 240/260 ° C, Cat. No. 723409.50Chromatographic conditions:Injection volume: 0,5 µl gasCarrier gas: 1 ml/min He (constant flow)Split: 80 ml/minTemperature: 50 °C → 100 °C, 5 °C/minDetector: MSD 5971Peaks:1. Tetramethylsilane2. Dichloromethane3. Tetrachlorosilane4. Chlorotrimethylsilane5. Methyltrichlorosilane6. Dichlorodimethylsilane7. Hexamethyldisiloxane

2000

90

1

2

3

5 10 15min

Diethylene glycol standard in wineCapillary column: PERMABOND® CW 20 M-DEG, 25 m x 0.25 mm ID, max. temp. 220/240 ° C, Cat. No. 723063.25Chromatographic conditions:Injection volume: 0.5 µl Carrier gas: 1.2 bar N2Split: ~1 : 40Temperature: 80 °C → 200 °C, 10 °C/minDetector: FID 260 °C, 10 x 22

Peaks:DEG standard1. 1,4-Butanediol2. Diethylene glycol3. Glycerol

2015

00


PERMABOND® CW 20 M-DEG, diethylene glycol tested Polyethylene glycol 20000 max. temperature for isothermal operation 220 °C, max. temperature for short isotherms in a temperature programme 240 °C

0.25 mm ID (0.4 mm OD)0.25 µm film 723063.25

0.32 mm ID (0.5 mm OD)0.25 µm film 723327.25

PERMABOND® Silane for silane analysesmax. temperature for 0.32 mm ID 280 °C, for 0.53 mm ID max. temperature for isothermal operation 240 °C, max. temperature for short isotherms in a temperature programme 260 °C0.32 mm ID (0.5 mm OD) 723409.500.53 mm ID (0.8 mm OD) 723411.25

MN


GC capillary columns for special applications – enantiomer analyses

342


Capillary columns for enantiomer separation

Enantiodifferentiation is an important aspect in the activity ofbiological systems: enantiomers of chiral odour and flavourcomponents as well as pharmaceuticals can possess verydifferent properties. For this reason, separation and analysisof enantiomers gains increasing importance. Among the methods available for this purpose, today chro-matography provides the most impressive success.Especially capillary gas chromatography with chiral station-ary phases is the method of choice, because it features high

resolution and sensitivity combined with simple detectionand high precision. Reproducibility is excellent, the amountof substance required for the analysis is low.The most important chiral phases can be assigned to twotypes:

modified cyclodextrins (LIPODEX®, HYDRODEX®)chiral polysiloxanes of the diamide type (e.g. L-CHIRASIL-VAL)

Enantiomer separation based on chemically modified cyclodextrins

Cyclodextrins are cyclic oligosaccharides consisting of six(α-cyclodextrin), seven (β-cyclodextrin) or eight (γ-cyclodex-trin) glucose units bonded through α-1,4-linkages. By complete alkylation or by partial alkylation and (regiose-lective) acylation of these cyclodextrins one can synthesise anumber of different derivatives with varying enantioselectiv-ity, which have been intensively studied and which are wellsuited as chiral stationary phases for gas chromatographicenantiomer analyses.These stationary phases have considerably broadened theapplicability of gas chromatographic enantiomer separations:they allow the resolution of alcohols, diols, aldols, acetals,aminoalcohols, alkyl halides, amines, barbiturates, carbohy-drates, cyanhydrins, ketones, carboxylic acids, amino acids,hydroxycarboxylic acids, lactones, esters, olefins and evenalkanes.One important advantage of these phases is that manycompounds can be analysed without derivatisation.However, for certain substances enantioselectivity can befavourably influenced by formation of different derivatives.Cyclodextrin phases also show some disadvantages:• The basic separation mechanism, which is responsible for

the large number of successful separations, does not al-low a prediction, which phase could solve a given separa-tion problem.

• Even for compounds with small structural differences orwithin a homologous series the enantiodifferentiation canbe quite different.

For coating fused silica capillaries, cyclodextrins are eitherused as pure, undiluted phases (FS-LIPODEX®) or dissolvedin polysiloxane (FS-HYDRODEX®).

Enantiomer separation of amino acid methyl esters (TFA)

Capillary column: FS-LIPODEX♦ E, 25 m x 0.25 mm ID, max. temp. 200/220 °C, Cat. No. 723368.25Chromatographic conditions:Volume: 1 µlCarrier gas: 60 kPa H2

Split: about 1 : 100Temperature: 90 → 190 °C, 4 °C/minDetector: FID, 250 °C, AT 2

Peaks (D is eluted before L except for proline: L before D)1. Alanine, 2. Valine, 3. Leucine, 4. Proline, 5. Aspartic acid, 6. Phenylalanine

1

2

3 4

5

6

10 200 min

2025

92

For applications with chiral MN columns please ask for our catalogue ”Solutions for chiral chromatography“

MN



343


** LIPODEX® is patented under EP 0407 412 and US Re. 36.092

Test mixtures for chiral GC capillary columns

Summary of phases and ordering information Cat. No. for column length of 25 m 50 m

(all 0.25 mm ID / 0.4 mm OD)

LIPODEX® fused silica capillary columns with cyclodextrin phasesCapillary columns FS-LIPODEX® A**

hexakis-(2,3,6-tri-O-pentyl-)-α-cyclodextrin, max. temperature* 180 / 200 °Crecommended for carbohydrates, polyols, diols, hydroxycarboxylic acid esters, (epoxy-) alcohols, glycerol derivatives, spiroacetals, ketones, alkyl halides

723360.25 723360.50

Capillary columns FS-LIPODEX® B**

hexakis-(2,6-di-O-pentyl-3-O-acetyl)-α-cyclodextrin, max. temperature* 200 / 220 °Crecommended for lactones, diols (cyclic carbonates), aminols, aldols (O-TFA), glycerol derivatives (cyclic carbonates)

723362.25 723362.50

Capillary columns FS-LIPODEX® C**

heptakis-(2,3,6-tri-O-pentyl)-β-cyclodextrin, max. temperature* 200 / 220 °Crecommended for alcohols, cyanhydrins, olefins, hydroxycarboxylic acid esters, alkyl halides

723364.25 723364.50

Capillary columns FS-LIPODEX® D**

heptakis-(2,6-di-O-pentyl-3-O-acetyl)-β-cyclodextrin, max. temperature* 200 °C / 220 °Crecommended for amines (TFA), aminols (TFA), trans-cycloalkane-1,2-diols, trans-cycloalkane-1,3-diols (TFA), β-amino acid esters

723366.25 723366.50

Capillary columns FS-LIPODEX® E**

octakis-(2,6-di-O-pentyl-3-O-butyryl)-γ-cyclodextrin, max. temperature* 200 °C / 220 °Crecommended for α-amino acids, α- and β-hydroxycarboxylic acid esters, alcohols (TFA), di-ols (TFA), ketones, pheromones (cyclic acetals), amines, alkyl halides, lactones

723368.25 723368.50

Capillary columns FS-LIPODEX® G**

octakis-(2,3-di-O-pentyl-6-O-methyl)-γ-cyclodextrin, max. temperature* 220 / 240 °Crecommended for menthol isomers, ketones, alcohols, carboxylic acid esters, terpenes 723379.25 723379.50

HYDRODEX® fused silica capillary columns (cyclodextrin phases diluted with OV-1701)Capillary columns FS-HYDRODEX® β-PM

heptakis-(2,3,6-tri-O-methyl)-β-cyclodextrin diluted with OV-1701, max. temperature* 230 / 250 °Crecommended for hydroxycarboxylic acid esters, alcohols, diols, olefins, lactones, acetals 723370.25 723370.50Capillary columns FS-HYDRODEX® β-3P

heptakis-(2,6-di-O-methyl-3-O-pentyl)-β-cyclodextrin diluted with OV-1701, max. temperature* 230 / 250 °Crecommended for terpenes, dienes, allenes, terpene alcohols, 1,2-epoxyalkanes, carboxylic acids (esters), hydroxycarboxylic acid esters, pharmaceutics, pesticides

723358.25 723358.50

Capillary columns FS-HYDRODEX® β-6TBDM

heptakis-(2,3-di-O-methyl-6-O-t-butyldimethyl-silyl)-β-cyclodextrin diluted with OV-1701, max. temperature* 230 / 250 °Crecommended for γ-lactones, cyclopentanones, terpenes, esters, tartrates 723381.25 723381.50* The first temperature is valid for isothermal operation, the second for short isotherms in a temperature programme.

Test mixture for test compound (enantiomer mixture) pack of Cat. No.

LIPODEX® A, HYDRODEX® β-PM, β-3P, β-6-TBDM Phenylethanol 1 ml 722321LIPODEX® B Methylbutyrolactone 1 ml 722322LIPODEX® C, D Phenylethylamine (TFA) 1 ml 722323LIPODEX® E, G Phenylethanol (TFA) 1 ml 722319PERMABOND® L-CHIRASIL-VAL Amino acids (TFA)-(Iprop) 1 ml 722324

MN



344


The lipophilic phases of the LIPODEX® series, which wereintroduced by W. A. König (Hamburg) are listed in the tableabove together with some typical applications to facilitate se-lection of a suitable column. LIPODEX® E and G are theLIPODEX® phases with the broadest range of applications.LIPODEX® E is also a valuable supplement to PERM-ABOND® L-CHIRASIL-VAL for amino acid analyses. LIPODEX® G is especially well suited for the analysis ofmenthol isomers as is shown in the chromatogram below.

The high melting point of the methylated, hydrophilic cyclo-dextrin derivatives (HYDRODEX®) is disadvantageous foruse of the undiluted phases. V. Schurig (Tübingen) showedthat methylated cyclodextrin phases can be operated at tem-peratures below their melting point, if they are diluted withpolysiloxane (OV-1701). Numerous examples for separationswith heptakis-(2,3,6-tri-O-methyl)-β-cyclodextrin in glass orfused silica capillary columns have been described in the lit-erature.

References:W. A. König, High Resol. Chromatogr. 16 (1993) 312 – 323W. A. König, High Resol. Chromatogr. 16 (1993) 569 – 586W. A. König, Gas Chromatographic Enantiomer Separationwith Modified Cyclodextrins, Hüthig, Heidelberg, 1992W. A. König, The Practice of Enantiomer Separation by Cap-illary Gas Chromatography, Hüthig, Heidelberg, 1987V. Schurig, J. Chromatogr. A 906 (2001) 275 – 299

(+)-

Men

thol

(–)-

Neo

isom

enth

ol

(–)-

Men

thol

(+)-

Isom

enth

ol

(–)-

Isom

enth

ol

(+)-

Men

thof

uran

(–)-

Isop

uleg

ol

(+)-

Pip

erito

ne

(+)-

Pul

egon

e(–

)-M

enth

yl a

ceta

te

(+)-

tran

s-S

abin

ene

hydr

ate

(+)-

Men

thon

e(+

)-Is

omen

thon

e(–

)-M

enth

one

(–)-

Isom

enth

one

(+)-

Neo

men

thol

(–)-

Neo

men

thol

(+)-

Neo

isom

enth

ol

(–)-

Isop

uleg

ol

Separation of chiral constituents of peppermint oilW. A. König et al., High Resol. Chromatogr. 20 (1997) 55 – 61Capillary column: FS-LIPODEX® G, 25 m x 0.25 mm ID, max. temp. 220/240 °C, Cat. No. 723379.25

Chromatographic conditions:Carrier gas: HeTemperature: 75 °C, isothermalDetector: FID

Mentha arvensis(China)

Mentha piperita(Idaho)

Standard

0 10 20 40 60 80min30 50

2504

10

0 10 min

CH3

O

NH

NCH3

O

O

Enantiomer separation of hexobarbital (TFA)

Capillary column: HYDRODEX® β-3P, 25 m x 0.25 mm ID, max. temperature 250 °C, Cat. No. 723358.25

Chromatographic conditions:Injection volume: 0.1 µlCarrier gas: 60 kPa H2 (1.9 ml/min)Split: 130 ml/minTemperature: 210 °CDetector: FID, 250 °C, 25

2024

00


MN



345


Application of cyclodextrin phases Stationary phases based on modified cyclodextrins are notavailable with chemical bonding of the phase to the fused sil-ica surface. For this reason the phase can be partially dis-solved when injecting large amounts of solvents with split-less or on-column injection techniques (e. g. with cold trap).The result could be formation of droplets at the column inletwith corresponding loss of efficiency.Since cyclodextrin phases have a lower capacity (comparedto conventional or achiral stationary phases), you shouldavoid loss of efficiency due to overload conditions. To avoidthe above-mentioned effects and maintain a good column lifewe recommend the use of low-boiling solvents like dichlo-romethane or pentane and a split technique (ratio ≥ 1 : 50).

0 10 20min

Enantiomer separation of dichlorprop methyl esterCapillary column: HYDRODEX® β-3P, 25 m x 0.25 mm ID, max. temperature 250 °C, Cat. No. 723358.25Chromatographic conditions:Injection volume: 0.1 µl (~1% in methylene chloride)Carrier gas: 60 kPa H2 (1.9 ml/min)Split: 130 ml/minTemperature: 160 °CDetector: FID, 250 °C, 27

Cl

Cl

O CO2CH3CH

CH3

2025

42

Courtesy of Prof. W.A. König, Hamburg, Germany

Separation of isomeric antiinflammatory drugsCapillary column: HYDRODEX® β-6-TBDM, 25 m x 0.25 mm ID,max. temperature 250 °C, Cat. No. 723381.25

Chromatographic conditions:Carrier gas: HeTemperature: 135 °C → 200 °C, 1 °C/minDetector: FID

Peaks:1. Ibuprofen

2. Flurbiprofen

3. Fenoprofen

4. Naproxen

5. Ketoprofen

CO2CH3

CO2CH3

F

OCO2CH3

CH3O

CO2CH3

O

CO2CH3

1S R

2

3

4

5

0 5 10 15 20 30 40 50 min

2501

80Enantiomer separation of γ-lactones C8 – C12

Capillary column: LIPODEX® E, 25 m x 0.25 mm ID, max. temperature 200/220 °C, Cat. No. 723368.25Chromatographic conditions:Injection volume: 1 µl (~ 0.1% in methylene chloride)Carrier gas: 100 kPa H2 (2.7 ml/min)Split: 320 ml/minTemperature: 130 °C → 160 °C, 2 °C/minDetector: FID, 250 °C, 26

5 10 15 min0 2029

72

MN



346


PERMABOND® L-CHIRASIL-VAL

The diamide type chiral stationary phase L-CHIRASIL-VAL,which has been developed by E. Bayer and H. Frank forenantiomer separation of amino acids, is available fromMACHEREY-NAGEL with chemical bonding (immobilisation)of the phase in fused silica capillaries: PERMABOND® L-CHIRASIL-VAL Thus the user can enjoy all the well-known advantages of im-mobilised phases such as:

High stability and resulting longer column lifetimeNo dissolving of stationary phase when injecting largesample volumes

The ability to remove contaminants from e.g. physiologi-cal samples by flushing, again increasing column life.

When using L-CHIRASIL-VAL you should avoid the pres-ence of strong acids or bases. Special care has to be takento remove any excess of derivatising reagents because theycan react with the phase causing destruction of the column.Derivatisation does not only increase the volatility of theamino acids, but it also enhances resolution of the enantio-meric pairs as described by I. Abe et al. [HRC & CC 6 (1983)366] and seen from the following chromatograms.


PERMABOND® L-CHIRASIL-VAL capillary columns for enantiomer separations(N-2-methylpropionyl-L-valine-t-butylamide)-methylpolysiloxane, max. temperature 190 °C0.25 mm ID (0.4 mm OD) 723730.25 723730.500.32 mm ID (0.5 mm OD) 723732.25 723732.50

Enantiomer separation of amino acid derivativesCapillary column: PERMABOND® L-CHIRASIL-VAL, 25 m x 0.25 mm ID, max. temperature 190 °C, Cat. No. 723730.25

FID

Res

pons

e

D-A

la

L-A

la

D-V

alD

-Thr

L-V

al/

L-T

hr

Gly

D-a

llo-I

le D-I

leL-

allo

-Ile

L-Ile D

-Ser

D-L

euL-

Ser

L-Le

u

D-P

ro L-P

ro

D-C

ysL-

Cys

D-A

spL-

Asp

BH

T

D-M

etL-

Met

D-P

he/

D-G

lu

L-P

he/

L-G

lu

D-T

yrL-

Tyr

D-O

rnL-

Orn

D-L

ysL-

Lys

FID

Res

pons

e

D-A

laL-

Ala

D-V

alD

-Thr

L-V

alL-

Thr

Gly

D-a

llo-I

le

D-I

leL-

allo

-Ile

/L-

IleD

-Ser

D-L

euL-

Ser

/

L-Le

u

D-P

roL-

Pro D-C

ysL-

Cys

D-A

spL-

Asp

BH

T

D-M

etL-

Met

D-P

he

D-G

lu

L-P

he L-G

lu

D-T

yr L-T

yr

D-O

rn

L-O

rn

D-L

ys L-Ly

s

10 20 30min

10 20 30 min

Pentafluoropropionyl amino acid n-propyl esters Temperature programme:

Chromatograms courtesy of Priv. Doz. Dr. W. Brückner, Dipl. Lebensmittel-Chemiker M. Hausch, Inst. f. Food Technology, University Hohen-heim, Stuttgart, Germany, 1988

10 20 30 40 50 min

80°C 4min

5°C/min

128°C 4min4°C/min

5°C/min160°C

190°C 17min

Chromatographic conditions:Injection volume: 0.5 µlCarrier gas: 0.45 bar H2, split 1 : 30Detector: FID, 250 °C, AT 3

N-Pentafluoropropionyl amino acid 2-propyl esters Temperature programme:

10 20 30 40 50min

80°C 7min

4°C/min

120°C 3min

5°C/min

190°C 15min

2026

22


MN


Columns / restrictors for SFC are available on request!

347


Precolumns: untreated capillaries, retention gaps and deactivated capillaries

Untreated capillaries for capillary electrophoresisfor preparation of capillary columnsfor capillary LC applications

Deactivated capillary columns (precolumns)

Deactivated or untreated capillary columns can be used forthe preparation of capillary columns. As precolumns, deacti-

vated capillaries should be preferred to retention gaps,whenever a larger contamination capacity is required.

Ordering information Cat. No. for capillary length of 1 m

(pack of 3)10 m

(pack of 1)25 m

(pack of 1)

Capillaries for electrophoresis 0.025 mm ID (0.375 mm OD) 723793.1 723793.20.05 mm ID (0.375 mm OD) 723790.1 723790.20.075 mm ID (0.375 mm OD) 723791.1 723791.20.10 mm ID (0.375 mm OD) 723792.1 723792.2

Untreated capillaries 0.20 mm ID (0.4 mm OD) 723148.10 723148.250.25 mm ID (0.4 mm OD) 723101.10 723101.250.32 mm ID (0.5 mm OD) 723151.10 723151.250.53 mm ID (0.8 mm OD) 723501.10 723501.25

Untreated capillaries are supplied without cage. For empty cages please see page 364.

Ordering information Cat. No. for capillary length of 10 m 25 m

Methyl-Sil deactivated (max. temperature 320 °C) 0.25 mm ID (0.4 mm OD) 723106.10 723106.250.32 mm ID (0.5 mm OD) 723346.10 723346.250.53 mm ID (0.8 mm OD) 723558.10 723558.25

Phenyl-Sil deactivated (max. temperature 320 °C) 0.25 mm ID (0.4 mm OD) 723108.10 723108.250.32 mm ID (0.5 mm OD) 723348.10 723348.250.53 mm ID (0.8 mm OD) 723560.10 723560.25

CW deactivated (max. temperature 250 °C) 0.25 mm ID (0.4 mm OD) 723105.10 723105.250.32 mm ID (0.5 mm OD) 723349.10 723349.250.53 mm ID (0.8 mm OD) 723562.10 723562.25

Deactivated capillaries are supplied without cage. For empty cages please see page 364.

MN


Precolumns: untreated capillaries, retention gaps and deactivated capillaries

348


Retention gaps

The retention gap technique as developed by K. Grob (incombination with on-column injection) allows concentrationof a large sample volume in the capillary column.For this purpose a retention gap must be inert. In order toguarantee maximum migration velocity the retention gapmust not exhibit any noticeable retention.Choice of the retention gap depends on the solvent used: theflooded zone after injection should be between 20 – 30cm/µl.A Me-Sil retention gap is more inert than a Phe-Sil, while thePhe-Sil retention gap is less susceptible to contaminations.CW retention gaps can only be used up to 250 °C, while Me-Sil and Phe-Sil retention gaps are stable up to 320 °C. Retention gaps can also be used as transfer lines or precol-umns (contamination capacity about 5–10 µg).

Recommended application of retention gaps

Me-Sil retention gap: only for use with n-hexane and diethyl ether

Phe-Sil retention gap: for all solvents except metha-nol and water

CW retention gap: for all solvents and especially for methanol and water

Calculation example:

length of flooded zone: about 20 – 30 cm/µlretention gap: 10 m x 0.32 mm IDcapillary column: 25 m x 0.32 mm IDmax. injection volume: about 30 – 50 µl

Ordering information Cat. No. for capillary length of 10 m 25 m

Me-Sil retention gaps (max temperature 320 °C) 0.25 mm ID (0.4 mm OD) 723706.10 723706.250.32 mm ID (0.5 mm OD) 723707.10 723707.250.53 mm ID (0.8 mm OD) 723708.10 723708.25

Phe-Sil retention gaps (max temperature 320 °C) 0.25 mm ID (0.4 mm OD) 723709.10 723709.250.32 mm ID (0.5 mm OD) 723710.10 723710.250.53 mm ID (0.8 mm OD) 723711.10 723711.25

CW retent gaps (max. temperature 250 °C) 0.25 mm ID (0.4 mm OD) 723712.10 723712.250.32 mm ID (0.5 mm OD) 723713.10 723713.250.53 mm ID (0.8 mm OD) 723714.10 723714.25

Retention gaps are supplied without cage. For empty cages please see page 364.

MN


Fused silica capillary columns – not chemically bonded

349


Ordering information Cat. No. for column length of 10 m 25 m 50 m

Capillary columns FS-OV-1100% dimethylpolysiloxane (max. temperature 300 °C)0.32 mm ID (0.5 mm OD)

0.25 µm film 733302.10 733302.25 733302.501.00 µm film – 733323.25 733323.50

0.53 mm ID (0.8 mm OD)1.00 µm film – 733529.25 –

Capillary columns FS-SE-30100% dimethylpolysiloxane (max. temperature 300 °C)0.25 mm ID (0.4 mm OD)

0.25 µm film 733052.10 733052.25 733052.500.32 mm ID (0.5 mm OD)

0.25 µm film 733306.10 733306.25 733306.50

Capillary columns FS-SE-525% phenyl – 95% dimethylpolysiloxane (max. temperature 300 °C)0.25 mm ID (0.4 mm OD)

0.25 µm film – 733054.25 733054.50

Capillary columns FS-SE-545% diphenyl – 1% vinylmethyl – 94% dimethylpolysiloxane (max. temperature 300 °C)

0.25 mm ID (0.4 mm OD)0.25 µm film – 733056.25 733056.50

0.32 mm ID (0.5 mm OD)1.00 µm film – 733325.25 733325.50

Capillary columns FS-CW 20 MPolyethylene glycol 20 000 daltonmax. temperature for isothermal operation 200 °C, max. temperature for short isotherms in a temperature programme 220 °C

0.25 mm ID (0.4 mm OD)0.50 µm film – 733067.25 733067.50

0.32 mm ID (0.5 mm OD)0.25 µm film 733321.10 733321.25 733321.50

0.53 mm ID (0.8 mm OD)1.00 µm film – 733549.25 –

Capillary columns FS-FFAPPolyethylene glycol 2-nitroterephthalic acid estermax. temperature for isothermal operation 200 °C, max. temperature for short isotherms in a temperature programme 220 °C

0.25 mm ID (0.4 mm OD)0.25 µm film – 733116.25 733116.50

0.32 mm ID (0.5 mm OD)0.25 µm film 733341.10 733341.25 733341.50

As a courtesy to our customers who do not want to change their methods with non-bonded capillaries, we still offer this smallprogramme of fused silica capillaries with non-immobilised phases. Customised lengths (15, 30 or 60 m), film thicknesses ordiameters are available on special request. Excellent replacements for these not chemically bonded stationary phases are thecorresponding phases of our OPTIMA® or PERMABOND® series.

Products for GC with packed columns are available on request!

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Contact [email protected] or call 61 7 3205 5233

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