Gas chromatography. Gas chromatography. Basic principles of GC. Capillary columns for GC. Derivatisation reagents.

Transcription

1 Gas chromatography Gas chromatography Basic principles of GC Page Introduction to GC Brief selection guide for capillary columns OPTIMA high performance capillary columns for GC 0 6 PERMABOND capillary columns for GC 0 Hints for use and maintenance of capillary columns GC capillary columns for special applications 46 Summary, capillary columns with thick films, fast GC columns 4, amine separations, FAME separations 6, GC analysis of petrochemical compounds 8, environmental analyses 9, triglyceride separation 40, separation of silanes 4, analysis of diethylene glycol 4, enantiomer separation 4 46 Untreated capillaries, retention gaps and deactivated capillaries Fused silica capillary columns not chemically bonded 49 Derivatisation reagents Summary, method development kits, selection guide for derivatisation of important functional groups in GC 0 Acylation, reagents and methods Methylation, reagents and methods Silylation, reagents and methods 8 Standards for GC Environmental standards for GC 9 6 Test mixtures for GC capillary columns 6 6 Accessories for GC 64 7 Accessories for capillary columns 64 6, 68, Valco fittings for capillary GC 66 67, accessories for packed GC columns 69, products for gas flow measurement and in-line gas purification 69 7, ferrules 7, septa 7 0

2 Basic principles of GC Basic principles of GC Introduction to GC Schematic presentation of a GC system gas supply chromatogram sample injection recorder capillary column detector data system In this chapter we want to give a short and general introduction for the beginner in gas chromatography. By no means this is meant as a complete treatise. For further information please refer to the references given below*. The GC system The chromatographic system is composed of the chromatograph and a recorder for plotting chromatograms or a data station for generation and evaluation of chromatograms. The chromatograph consists of the sample injector, gas supplies, oven with temperature control for the chromatographic column and the detector. It would take us too far to describe all injection techniques in detail. We just want to mention the different basic possibilities of direct and indirect sample injection. With direct injection the sample is introduced into the column without contact with other parts from glass or metal (on column injection). With indirect techniques the sample is injected into an evaporator. The vapour then is transferred into the column either completely or partially (split technique). With both techniques the injection can take place at low temperatures, at high temperatures or with temperature programming. The gas supply unit of a chromatograph has to provide all gases needed for a separation: the carrier gas and e.g. the burner gases for the flame ionisation detector (FID). The detector indicates a substance by generation of a more or less intense electrical signal (response). Analogue (recorder) or digital (computer) processing of these signals produces the chromatogram or a numerical report. Some detectors are specific for certain classes of substances or for certain atoms (P, N, etc.). The separation process The chromatographic separation is achieved by repeated distribution of each sample component between two phases. One of these phases is stationary. The second, the mobile phase moves along this stationary phase. In Gas Chromatography (GC) the mobile phase is always a gas (mostly N, H, He). The stationary phase in GSC (Gas Solid Chromatography or adsorption chromatography) is a porous polymer solid, while in GLC (Gas Liquid Chromatography or partition chromatography) the stationary phase is a mostly viscous gumlike liquid. Packed columns are completely filled with a packing, liquid stationary phases being coated onto an inert support. Capillary columns do not require a support, because their inner wall is coated with the stationary phase (WCOT = Wall Coated Open Tubular). Transport of the components is achieved exclusively in the gas phase, separation is accomplished in the stationary phase. The quality of a separation (resolution) depends on how long the components to be separated stay in the stationary phase and on how often they interact with this phase (selectivity). The type of interaction between component and phase (selectivity) is determined by the functional groups. The polarity of the phase is a function of stationary phase substituents. The chromatogram Schematic presentation of a chromatogram Start t 0 t R w / A chromatogram consists of a base line and a number of peaks. The area of a peak allows quantitative determinations. Starting point of a chromatogram is the time of injection of a dissolved sample. The time interval between a peak and the point of injection is called retention time t R. A component can be identified by its retention time (qualitative determination). The retention time is the sum of the residence time of a solute in the mobile phase (t 0 ) and in the stationary phase (t R ' = net retention time); t R i = t 0 + t R i t 0 is also known as dead time. It is the time required by a component to migrate through the chromatographic system without any interaction with the stationary phase (also called air or gas peak). The net retention time t R i is the difference t R 06

3 Basic principles of GC Basic principles of GC Introduction to GC between total retention time t R i and dead time t 0. It indicates how long a substance stays in the stationary phase. = t 0 t R i t R i The capacity factor (k ) is a measure for the position of a sample peak in the chromatogram. The capacity factor is specific for a given compound and constant under constant conditions. t R i t 0 k i = t 0 The relative retention (α), also called separation factor or selectivity coefficient, is defined as α = k k i.e. it is the ratio of two capacity factors, the reference substance always being in the denominator. The relative retention does not provide any information on the quality of a separation, since for equal vaues of α two very broad peaks may overlap, (as shown in trace a), or may be completely resolved (as in trace b), if they are correspondingly narrow. Such a plate is of course a theoretical hypothesis, representing that portion of a column in which the partition equilibrium is established once. The smaller this value the better works the column. The relation between N, R and k' is R = α k i N 4 α k i + th From this formula the number of plates N th required for a given resolution R can be calculated. The Van Deemter equation shows how the plate height h depends on the flow velocity u: HETP h min B u HETP = A + B ū -- + C u C. u u opt. u a b retention time For this reason the peak width at half height (w / ) is taken into account when considering the resolution R according to t R t R R = (w / ) + (w / ) The resolution R is a measure for the quality of a separation. The separation number SN is another value indicating the quality of a separation. It defines how many peaks can be resolved between two members of a homologous series of e.g. n-paraffins. t R t R SN = (w / ) + (w / ) If retention times are not too small, SN can be determined in a temperature programme. The number of theoretical plates (N th ) characterises the quality of a column (it should be determined for k > ): t R N th =.4 ( i ) w / The height equivalent to a theoretical plate (h, HETP) is calculated by dividing the length L of the column by the number of theoretical plates N th : h = HETP = L N th A = Eddy diffusion; A is a function of packing uniformity; for WCOT capillary columns A equals 0 (WCOT = Wall Coated Open Tubular) B = molecular axial diffusion; B is a function of the diffusion coefficient of the component in the respective carrier gas C = resistance to mass transfer In practice often higher velocities than u opt. are chosen, if separation efficiency is sufficient, since higher carrier velocities mean shorter retention times. * References: D. Rood, A practical guide to care, maintainance and troubleshooting of capillary gas chromatographic systems, nd edition, Hüthig Verlag, Heidelberg, 99 W. Blum, R. Aichholz Hochtemperatur-Gas-Chromatographie, Hüthig Verlag, Heidelberg, 99 G. Schomburg, Gas Chromatography, A Practical Course, Verlag Chemie, Weinheim, 990 K. Grob, Classical Split and Splitless Injection Techniques in Capillary GC, Hüthig Verlag, Heidelberg, 986 K. Grob, Making and Manipulation of Capillary Columns for Gas Chromatography, Hüthig Verlag, Heidelberg, 986 P. Sandra, Sample Introduction in Capillary Gas Chromatography, Volume, Hüthig Verlag, Heidelberg, 98 E. Leibnitz, H. G. Struppe, Handbuch der Gas-Chromatographie, Akademische Verlagsgesellschaft Geest u. Portig KG, Leipzig, Germany, 984 W. Jennings, Gas Chromatography with Glass Capillary Columns, Academic Press, New York 978 R. Kaiser, Chromatographie in der Gasphase, BI Hochschultaschenbücher, several volumes, Bibligraphisches Institut, Mannheim, Germany,

4 Brief selection guide for capillary columns The large number of stationary phases and the variability of column parameters have caused a considerable diversification of our column programme. now offers more than 0 different phases with a total of more than 60 Cat. Nos. For this reason especially the beginner may have some problems to select the capillary column best suiting his particular separation needs. This is why we will briefly explain the most important criteria for column selection. A capillary column is characterised by the following parameters: e.g. Cat. No. 76. m x 0. mm ID OPTIMA,.0 µm film A B C D E A = length B = inner diameter C = type of chemical bonding, immobilisation D = polarity of the stationary phase E = film thickness All these parameters have to be optimised for each particular chromatographic task. A. Length The separation efficiency (correctly speaking the number of plates n) of a capillary column is directly proportional to the length. However, the same relation is true for the retention time and thus for the total analysis time, making it desirable to use columns as short as possible. For routine separations in general m or shorter will be sufficient with the advantage of short analysis times. For difficult problems such as the separation of complex mixtures with about 0 components or more 60 m columns may be necessary. Use of longer columns is not recommended. Doubling the column length will only result in a 40% increase in resolution, since the resolution is proportional to the square root of the length. However, the time needed for an isothermal analysis will be doubled. B. Inner diameter The inner diameter also influences the separation efficiency of a capillary column: the lower the inner diameter the higher is the theoretically possible number of plates per meter. This will increase the resolution of the column, which is often required for complex sample mixtures. Due to the low sample capacity one normally has to work with split injection. Increasing the inner diameter while keeping the film thickness constant will increase the capacity. This is especially important for trace analyses and / or for the injection of larger sample volumes. If you halve the diameter of the column while keeping the film thickness constant, the capacity is also reduced by 0%. As a general rule one can say: a column with 0. mm ID and a film thickness of 0. µm has a maximum capacity of 00 ng/component. Overloading the column results in a loss of resolution. a) 0. to 0. mm inner diameter OPTIMA columns with this diameter are especially recommended for GC-MS with the advantage of high resolution and short retention times with low carrier gas flows. b) 0. mm inner diameter Columns with this diameter are used for the analysis of complex mixtures. They are recommended as routine columns for high resolution, especially in research applications. d) 0. mm inner diameter A column with 0. mm ID is the column for routine analyses with short retention times, yet increased capacity. With suitable film thickness it is the column of choice for trace analyses and on-column or splitless injection techniques. If you want to use a mass selective detector (MSD), you are often limited to smaller diameters, because many vacuum pumps cannot handle the high flow rates required for columns with larger diameters. e) 0. mm inner diameter Compared to packed columns these capillaries show more inert surfaces and higher reproducibility with at least equal separation efficiency. They are not only the replacement for packed columns, but the capillary for rapid separations with inert surface and highest capacity. The inner diameter 0. mm is ideal for use with the thermal conductivity detector. C. Immobilisation OPTIMA : the top quality of fused silica (FS) capillaries from MACHEREY-NAGEL with chemically bonded (immobilised) stationary phases. A special treatment after immobilisation of the phase results in lower column bleeding. An immobilised film of stationary phase tolerates injection of large sample volumes in on-column or splitless sample injection techniques. PERMABOND : FS capillary columns, also with immobilised (chemically bonded) stationary phase. FS capillary columns with non-immobilised phases. D. Stationary phase Different substituents in the chemical structures of stationary phases are responsible for the type of interaction (selectivity) between the phase and the solutes to be separated and thus determine the relative retention and the number of theoretical plates required for a given resolution. The stationary phase also limits the temperature range for chromatography. Nonpolar phases separate by efficiency (n) and retention (k') only, while polar phases offer additional interactions, which may influence or improve a separation. Selectivity has to be optimised for the critical pair of components or the main component. You should always select the least polar column which solves your separation problem. About 70% of all separations can be performed on non- to midpolar columns. These columns generally feature high temperature stability. Nonpolar stationary phases (e.g. 00% dimethylpolysiloxane phases) sepa- For applications with GC capillary columns please ask for our catalogue GC Applications 08

5 Brief selection guide for capillary columns rate components mostly according to the height of the boiling point. Typical analytes are linear hydrocarbons (n-alkanes). When increasing the polarity of the phase, e.g. by introduction of phenyl and / or cyanopropyl groups, separation is increasingly influenced by differences in dipole moment and by charge transfer (e.g. for 0% diphenylpolysiloxane phases). Typical analytes are hydrocarbons, which contain oxygen, sulphur, nitrogen, phosphorus or halogen atoms, unsaturated molecules which can be polarised and aromatics. For components featuring different hydrogen bonding capacities and the ability to form strong hydrogen bonds, polyethylene glycol phases (Carbowax) are the best choice for a separation. Typical analytes are alcohols and carboxylic acids. E. Film thickness Our programme of capillary columns comprises films from 0. to.0 µm. The standard film thickness is 0. µm. If you work with thin films (0. 0. µm), in general substances are eluted faster, at lower temperatures and with better resolution than with a thick film (>0. µm). For highboiling compounds, temperature labile or very closely eluting sample substances thin films are very well suited. Increasing the film thickness will increase the capacity and improve inertness. Thick films are ideal for low-boiling compounds, often eliminating the need for cooling during chromatography, since they increase elution temperatures, i.e. the components are retained more strongly. As a general rule one can say: doubling the film thickness results in an increase in elution temperature of about 0 C under isothermal conditions. This is advantageous for aqueous systems as well. Variation of the film thickness is often better than increasing the column length as is shown in the following chromatograms: The upper figure shows a separation with the special column PERMABOND P-00 with 0. µm film thickness and 00 m length, while the lower figure shows the chromatogram on a 0 m column with µm film thickness. The second figure clearly demonstrates the high separation efficiency of a 0 m column with very thick film compared to the 00 m column with thin film. According to the criteria cited above the following capillaries are suited for the larger part of all applications and can be considered as standard equipment for GC:. Cat. No m x 0. mm ID OPTIMA, 0. µm film. Cat. No m x 0. mm ID OPTIMA 70, 0. µm film. Cat. No. 7. m x 0. mm ID PERMABOND CW 0 M, 0. µm film 4. Cat. No m x 0. mm ID OPTIMA δ-, 0. µm film a suitable substitute for. and. Analysis of hydrocarbons C C Capillary column: PERMABOND P-00, 0. µm film, 00 m x 0. mm ID, max. temperature 00/0 C, Cat. No Injection volume: 00 µl Carrier gas: 00 kpa H (. ml/min) Split: 00 ml/min Temperature: C Detector: FID, 0 C, 8. Methane. Ethane. Propane 4. i-butane. Butane 6. Methylbutane 7. Pentane min Separation of hydrocarbons C C Capillary column: OPTIMA,.0 µm film, 0 m x 0. mm ID, max. temperature 80 C, Cat. No Injection volume: 00 µl Carrier gas: 0.08 bar N Split: 60 ml/min Temperature: 6 C Detector: FID, 4. Methane. Ethane. Propane 4. i-butane. n-butane 6. Methylbutane 7. n-pentane min For applications with GC capillary columns visit our web site: 09

6 OPTIMA high performance capillary columns As a result of our efforts in research and development and the continuous improvements in our manufacturing techniques we present OPTIMA a series of high performance capillary columns for gas chromatography. OPTIMA capillary columns provide high thermal stability Improved temperature stability is the reason why OPTIMA capillary columns can be operated at about 40 C higher temperatures compared to standard phases. High-boiling solutes (with very low vapour pressures) "normally" have very long retention times and rather broad peak shapes. OPTIMA columns with their increased operation temperatures elute high-boiling compounds faster and with better peak shapes. Maximum operating temperatures for OPTIMA phases The first temperature is valid for isothermal operation, the second for short isotherms in a temperature programme. Temperature limits for 0. mm ID columns and for columns with film thickness of µm or greater are given with the ordering information on the following pages. Phase max. operating temperatures OPTIMA 40/60 C OPTIMA 40/60 C OPTIMA δ- 40/60 C OPTIMA δ-6 40/60 C OPTIMA 7 0/40 C OPTIMA 0 00/0 C OPTIMA 70 00/0 C OPTIMA 64 80/00 C OPTIMA 0 60/80 C OPTIMA 60/80 C OPTIMA 40 60/80 C OPTIMA CN-00 40/60 C reduced column bleed Improved manufacturing processes offer capillaries with lower bleed levels, which are especially recommended for GC-MS. Less column bleed yields increased sensitivity and accuracy through a better signal to noise ratio for any kind of detector. Reduced column bleed improves detectability of solutes in qualitative and quantitative GC-MS analyses. more inert columns due to optimised deactivation Polar compounds are frequently difficult to analyse, because they often give broad tailing peaks. Advances in deactivation technology for the OPTIMA capillaries result in an excellent chromatographic performance yielding improved peak shapes of polar compounds combined with improved efficiency and sensitivity. In order to guarantee best industry standard capillaries with highest reproducibility from capillary to capillary OPTIMA columns have to meet high specifications. For controlling quality MACHEREY-NAGEL determines the following parameters: efficiency by measuring the separation number (Trennzahl according to Kaiser) in a temperature programme. polarity by measuring retention indices bleeding in a temperature programme with a test mixture including high-boiling hydrocarbons inertness by measuring the peak height ratio for decylamine/c- (for non- to medium polar phases) Capillary column: OPTIMA, 0. µm film, 0 m x 0. mm ID, max. temp. 40/60 C, Cat. No Carrier gas:.0 bar H Temperature: 70 C 0 C (0 min), 0 C/min 0 C ( min) Detector: FID 00 C, 0. C-8. Dibutylamine. C-0 4. Phenylethanol.,6-Dichloroaniline 6.,4-Dichlorophenol 7. C- 8. Decylamine 9. Decanol 0. C-4. C-6. C-8. C-0 4. C-. C-4 6. C-6 7. C-8 8. C-0 9. C min 70 For ordering information of OPTIMA capillary columns please see pages 6 6. For applications with GC capillary columns please ask for our catalogue GC Applications 0

7 OPTIMA high performance capillary columns Comparison of separation properties for selected OPTIMA phases OPTIMA µm film 0 m x 0. mm ID max. temp. 60/80 C Cat. No OPTIMA 0. µm film 0 m x 0. mm ID max. temp. 60/80 C Cat. No OPTIMA 0 0. µm film 0 m x 0. mm ID max. temp. 60/80 C Cat. No OPTIMA µm film 0 m x 0. mm ID max. temp. 0/40 C Cat. No OPTIMA 7 0. µm film 0 m x 0. mm ID max. temp. 0/40 C Cat. No OPTIMA 0. µm film 0 m x 0. mm ID max. temp. 40/60 C Cat. No increasing polarity OPTIMA 0. µm film 0 m x 0. mm ID max. temp. 40/60 C Cat. No time [min] 0 0 min Sample: -OPTIMA test mixture (Cat. No. 76) Injection:.0 µl, split :0 Carrier gas: 80 kpa N Temperature: 80 C T max (isothermal), 8 C/min Detector: FID, C, 6. Undecane. Dodecane. Octanol 4. Dimethylaniline. Decylamine 6. Methyl decanoate 7. Methyl undecanoate 8. Henicosane 9. Docosane 0. Tricosane For applications with GC capillary columns visit our web site:

8 OPTIMA δ the unique family of phases with autoselectivity permanent dipole: constant interactions dipoles of the analytes OV- conventional phase OPTIMA δ- SE-4 OV-7 OV-70 OV-0 OV-40 OPTIMA δ-6 OPTIMA δ permanent dipoles of the stationary phase induced dipoles of OPTIMA δ phases permanent + induced dipole = autoselectivity range of polarities covered by OPTIMA δ phases OPTIMA δ- and OPTIMA δ-6 are stationary phases, which exhibit not only a fixed polarity, like most polysiloxane phases, but additionally a polarity, which is influenced by the sample. The polymers consist of cross-linked methyl-phenylpolysiloxane block polymers with defined composition, and extremely narrow molecular weight distribution, which are exclusively produced for MACHEREY-NAGEL. Especially polar analytes are able to induce a dipole moment in the stationary phase, so that the molecules show stronger interactions with the phase. This enhanced interaction is maintained at higher temperatures, where normally interactions between molecule and phase become reduced due to the Brownian movement. We call this phenomenon autoselectivity, because the stationary phase adjusts itself to the polarity of the analytes. Thus OPTIMA δ phases cover broad ranges of polarities. Compared with conventional phases, OPTIMA δ- polarity ranges from approximately the nonpolar OPTIMA to the midpolar OPTIMA 70, while for OPTIMA δ-6 the polarity covers a range from about the midpolar OPTIMA 7 to the polar OPTIMA 0. Due to this feature, the OPTIMA δ columns show interesting patterns of selectivity. For example, inversions in the sequence of peak elution may occur, which recommends the columns for reference use (e. g. in combination with OPTIMA ). In conventional midpolar phases the polarity is induced by phenyl, but especially by cyano and trifluoromethyl groups. The two latter often cause bleeding, which results in severe problems with some detectors. In contrast, the OPTIMA δ phases show very high temperature limits (40/60 C), as well as the low bleed levels, which makes them ideal for the use with mass selective (MSD) or phosphorus/nitrogen detectors (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 phases Very low bleed levels Extremely inert Medium polar without CN groups References: W. Röder, D. Lennartz, GIT /99, p. 6 R. Looser, K. Ballschmiter, J. Chromatogr. 86 (999), 7-84 R. Baycan-Keller, M. Oehme, J. Chromatogr. 87 (999), 0 0 For applications with GC capillary columns please ask for our catalogue GC Applications

9 OPTIMA δ the unique family of GC phases with autoselectivity Analysis of isomeric phenols Isomeric phenols, such as chloro- and nitrophenols, are difficult to analyse with standard GC phases (e.g. OPTIMA or OPTIMA 7) because of coelutions. The autoselective OPTIMA δ- is able to separate all phenols due to stronger interactions occurring with more polar molecules, because polar analytes induce a dipole moment in the phase of the OPTIMA δ-. Capillary column: OPTIMA δ-, 0. µm film, 60 m x 0. mm ID, max. temperature 40/60 C, Cat. No Injection:.0 µl, split :80 Carrier gas: He,. bar 8 Temperature: 60 C ( min) 0 C, 6 C/min 6 Detector: MSD HP Phenol 4. -Chlorophenol. -Methylphenol Methylphenol. -Methylphenol 6.,4-Dimethylphenol 7. -Nitrophenol 8.,4-Dichlorophenol 9.,6-Dichlorophenol 0. 4-Chloro--methylphenol ,,-Trichlorophenol 6 0.,4,6-Trichlorophenol.,4,-Trichlorophenol 4.,,4-Trichlorophenol.,,6-Trichlorophenol 6.,,,6-Tetrachlorophenol 9 7.,,4,-Tetrachlorophenol 8.,,4,6-Tetrachlorophenol 9.,4-Dinitrophenol 0.,4,-Trichlorophenol. -Methyl-4,6-dinitrophenol. -Isopropyl-4,6-dinitrophenol 0 0 min Separation of organochlorine pesticides (EPA 808) Capillary column: OPTIMA δ-6, 0. µm film, 0 m x 0. mm ID, max. temperature 40/60 C, Cat. No Sample: EPA 808 organochlorine pesticide calibration mix (Restek), 00 µg/ml each in toluene : hexane ( : ) Injection volume: µl, Split : 0 Carrier gas:.0 bar He 0 Temperature: 80 C 00 C (0 min), 4.0 C/min 4 0 Detector: MSD HP α-bhc 0. γ-bhc (lindane) 4. β-bhc Heptachlor. δ-bhc 6. Aldrin 7. Heptachlor epoxide 8. γ-chlordane 9. α-chlordane Endosulfan I. 4,4'-DDE. Dieldrin. Endrin ,4'-DDD. Endosulfan II 6. 4,4'-DDT 7. Endrin aldehyde 8. Endosulfan sulphate 9. Methoxychlor 0. Endrin ketone 0 0 min Abundance For applications with GC capillary columns visit our web site:

10 OPTIMA high performance capillary columns Unique from, no similar phases Max. temperature for isothermal operation 40 C, max. temperature for short isotherms in a temperature programme 60 C Autoselectivity resulting in a wide range of polarities from approximately the non-polar OPTIMA to the midpolar OPTIMA 70 Analytes determine the polarity of the phase Medium polar without CN groups Ideal for MSD and PND detectors USP 49 Separation of organophosphorus pesticides (EPA 840/84) on OPTIMA δ- Capillary column: OPTIMA δ-, 0. µm film, 0 m x 0. mm ID, max. temperature 40/60 C, Cat. No sample EPA 840 OP pesticide calibration mix (Restek), 00 µg/ml each in hexane : acetone = 9 : Injection: µl, split : 0, carrier gas:.0 bar He, temperature: 0 C 00 C (0 min),. C/min Detector: MSD HP 97. Dichlorvos. Mevinphos. Demeton-s 4. Ethoprop. Naled 6. Phorate 7. Demeton-o 8. Diazinon 9. Disulfoton 0. Parathion-methyl. Ronnel. Fenthion. Chlorpyrifos 4. Trichloronate. Merphos 6. Stirofos 7. Tokuthion 8. Merphos oxidation product 9. Fensulfothion 0. Bolstar. Azinphos-methyl. Coumaphos 4 0 m m m 0 m m 0 m 0 m 60 m 0. mm ID (0.4 mm OD) 0.0 µm film mm ID (0.4 mm OD) 0.0 µm film mm ID (0.4 mm OD) 0. µm film µm film mm ID (0. mm OD) 0. µm film µm film µm film mm ID (0.8 mm OD).00 µm film Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are closed 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. For applications with GC capillary columns please ask for our catalogue GC Applications min

11 OPTIMA high performance capillary columns Unique from, no similar phases Max. temperature for isothermal operation 40 C, max. temperature for short isotherms in a temperature programme 60 C Autoselectivity resulting in a wide range of polarities from approximately the non-polar OPTIMA 7 to the midpolar OPTIMA 0 Analytes determine the polarity of the phase Medium polar without CN groups Ideal for MSD and PND detectors Separation of organophosphorus pesticides (EPA 840/84) on OPTIMA δ-6 Capillary column: OPTIMA δ-6, 0. µm film, 0 m x 0. mm ID, max. temperature 40/60 C, Cat. No Sample: EPA 840 OP pesticide calibration mix (Restek), 00 µg/ml each in hexane : acetone = 9 : Injection volume: µl, split :0 Carrier gas:.0 bar He 8 4 Temperature: 6 9 Detector: MSD HP 97 9, Dichlorvos 0 C 00 C (0 min),. C/min. Mevinphos. Demeton-s 4. Ethoprop. Naled 6. Phorate 7. Demeton-o 8. Diazinon 7 9. Disulfoton 0 0. Parathion-methyl. Ronnel. Fenthion. Chlorpyrifos 4. Trichloronate. Merphos 8 6. Stirofos 7. Tokuthion 8. Merphos oxidation product 9. Fensulfothion 0. Bolstar. Azinphos-methyl. Coumaphos min m m m m 0 m 0 m 60 m 0. mm ID (0.4 mm OD) 0.0 µm film mm ID (0.4 mm OD) 0.0 µm film mm ID (0.4 mm OD) 0. µm film mm ID (0. mm OD) 0. µm film µm film mm ID (0.8 mm OD).00 µm film Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are closed 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. For applications with GC capillary columns visit our web site:

12 OPTIMA high performance capillary columns 00% dimethylpolysiloxane O CH Si CH n For columns with mm ID and films < µm the max. temperature for isothermal operation is 40 C, the max. temperature for short isotherms in a temperature programme is 60 C for 0. mm ID columns with films < µm the max. temperatures are 0 and 40 C, resp. for thick film columns with films µm the max. temperatures are 00 and 0 C, resp. Nonpolar Separation of components according to boiling points Thick film columns µm film are especially recommended for solvent analyses Similar phases: OV-, DB-, SE-0, HP-, Ultra-, SPB-, CP-SIL CB, Rtx-, 007-, BP, MDN-, AT-, ZB, OV 0 USP G 0 m m m 0 m m 0 m 0 m 60 m 0. mm ID (0.4 mm OD) 0.0 µm film µm film mm ID (0.4 mm OD) 0.0 µm film µm film µm film µm film mm ID (0.4 mm OD) 0.0 µm film µm film µm film µm film mm ID (0. mm OD) 0.0 µm film µm film µm film µm film µm film µm film µm film mm ID (0.8 mm OD) 0.0 µm film µm film µm film µm film Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are closed 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. For applications with GC capillary columns please ask for our catalogue GC Applications 6

13 OPTIMA high performance capillary columns Solvent analysis Capillary column: OPTIMA,.0 µm film, 60 m x 0. mm ID, max. temperature 40/60 C, Cat. No Sample: Solvent mixture, courtesy of J. Lutz, Alcan Rorschach, Switzerland Injection volume: 0.4 µl, split : 60 Carrier gas: H, 0 KPa Temperature: 0 C (9 min) 90 C, 4 C/min 80 C ( min), 4 C/min Detector: FID, 00 C, 6 mv min 0. Methanol. Ethanol. Acetone 4. Isopropanol. Methyl acetate 6. n-propanol 7. Methyl ethyl ketone 8. Ethyl acetate 9. Isobutanol 0. n-butanol. -Methoxy--propanol. Isooctane. Ethylglycol 4. Isoheptane. Methyl isobutyl ketone 6. -Ethoxy--propanol 7. Toluene 8. Isobutyl acetate 9. Butyl acetate 0. 4-Hydroxy-4-methyl--pentanone. -Methoxy--propyl acetate. Xylene. Cyclohexanone 4. Ethyl glycol acetate. Butyl glycol 6. Heptanol 7. Ethyldiglycol 8. Butyldiglycol 9. Butyl glycol acetate 0. Butyldiglycol acetate 090 CH Max. temperature for isothermal operation 40 C, max. temperature for short isotherms in a temperature programme 60 C Selectivity identical with OPTIMA Phase with lowest bleeding Ideal for GC/MS and ECD applications and general analyses at trace level 00% dimethylpolysiloxane O Si CH n m m m 0 m 0 m 60 m 0. mm ID (0.4 mm OD) 0.0 µm film µm film mm ID (0.4 mm OD) 0. µm film mm ID (0. mm OD) 0. µm film Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are closed 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. For applications with GC capillary columns visit our web site: 7

14 OPTIMA high performance capillary columns % phenyl 9% dimethylpolysiloxane CH O Si n CH O Si CH m For columns with mm ID and films < µm the max. temperature for isothermal operation is 40 C, the max. temperature for short isotherms in a temperature programme is 60 C for 0. mm ID columns with films < µm the max. temperatures are 0 and 40 C, resp. for thick film columns with films µm the max. temperatures are 00 and 0 C, resp. Nonpolar Standard phase with large range of application Suitable for GC/MS (columns with small films) Similar phases: SE-4, SE-, DB-, HP-, Ultra-, SPB-, CP-SIL 8, Rtx-, 007-, BP, MDN-, AT-, ZB- USP G 7 0 m m m m 0 m 0 m 60 m 0. mm ID (0.4 mm OD) 0.0 µm film mm ID (0.4 mm OD) 0.0 µm film µm film µm film µm film mm ID (0.4 mm OD) 0.0 µm film µm film µm film µm film µm film mm ID (0. mm OD) 0.0 µm film µm film µm film µm film µm film µm film µm film mm ID (0.8 mm OD) 0.0 µm film µm film µm film µm film Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are closed 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. For applications with GC capillary columns please ask for our catalogue GC Applications 8

15 OPTIMA high performance capillary columns % diphenyl 9% dimethylpolysiloxane O Si n O CH Si CH Pyrolysis GC of chloroprene rubber Capillary column: OPTIMA MS, µm film, 60 m x 0. mm ID, max. temperature: 40/60 C, Cat. No Method: g solid are dissolved in 0 ml of hexane or methanol, 00 µl of this solution are pyrolysed in a crucible, headspace Temperature: 60 C ( min) 0 C, 8 C/min Detector: MSD chromatogram courtesy of Mrs. Engel, VW, Wolfsburg, Germany m 0040 Max. temperature for isothermal operation 40 C, max. temperature for short isotherms in a temperature programme 60 C Selectivity identical with OPTIMA NEW! New quality even less bleeding Ideal for GC/MS and ECD applications and general analyses at trace level Analysis of PCB (W congener mix) Capillary column: OPTIMA MS, 0. µm film, 0 m x 0.0 mm ID, max. temperature: 40/60 C, Cat. No Sample: PCB-W congener mix, 0 µl/ml Injection: µl Split: 80 ml/min Carrier gas: 0. bar He Temperature: 0 C 00 C ( min),. C/min Detector: ECD, 00 C 8. PCB 8. PCB. PCB 8 4. PCB 0. PCB PCB PCB 0 8. PCB PCB 8 0. PCB PCB 0. PCB 8. PCB PCB 70. PCB min min 0 m m m m 0 m 0 m 60 m 0. mm ID (0.4 mm OD) 0.0 µm film µm film mm ID (0.4 mm OD) 0. µm film µm film µm film mm ID (0. mm OD) 0. µm film µm film µm film Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are closed 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. For applications with GC capillary columns visit our web site: 9

16 OPTIMA high performance capillary columns phenylmethylpolysiloxane (0% phenyl) O CH Si Max. temperature for isothermal operation 0 C, max. temperature for short isotherms in a temperature programme 40 C for 0. mm ID columns the max. temperatures are 80 and 00 C, resp. Medium polar Suitable for higher temperatures Preferred applications: steroids, pesticides, drug analyses Similar phases: OV-7, DB-7, HP-0+, HP-7, SPB-0, SP-0, Rtx-0, CP-SIL 4 CB, 007-7, ZB-0 USP G n Analysis of aromatic hydrocarbons Capillary column: OPTIMA 7, 0. film, 0 m x 0. mm ID, max. temperature 0/40 C, Cat. No Injection volume: 0. µl Carrier gas: 0 kpa N, split :0 Temperature: 0 C 00 C, C/min Detector: FID, 60 C, 6. Benzene. Toluene 8. Ethylbenzene 4. m-xylene. o-xylene 6. Isopropylbenzene 7. n-propylbenzene p-isopropylbenzene n-butylbenzene 0. n-hexylbenzene. n-octylbenzene min 0 m m m m 0 m 0 m 60 m 0. mm ID (0.4 mm OD) 0.0 µm film mm ID (0.4 mm OD) 0.0 µm film µm film mm ID (0.4 mm OD) 0. µm film µm film µm film mm ID (0. mm OD) 0. µm film µm film µm film µm film mm ID (0.8 mm OD).00 µm film Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are closed 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. For applications with GC capillary columns please ask for our catalogue GC Applications 0

17 OPTIMA high performance capillary columns 4% cyanopropyl-phenyl 86% dimethylpolysiloxane CH O Si O Si Analysis of Fusarium mycotoxins F. Walker, B. Meier, Journal of AOAC Int. 8 (998) Capillary column: OPTIMA 70, 0. µm film, m x 0. mm ID, max. temperature 00/0 C, Cat. No Injection: µl, 0 C, splitless Carrier gas: N, 0 cm/s, linearvelocity at 60 C Temperature: 60 C ( min) 40 C, 6 C/min 70 C, 0 C/min ( min) Detector: 6 Ni-ECD, 0 C..9 min Nivalenol (0.007 ppm).. min Deoxynivalenol (0.006 ppm). 7. min -O-Acetyl-4-deoxynivalenol (0.006 ppm) min -Acetyldeoxynivalenol (0.00 ppm) (CH ) CN n CH m 0660 Max. temperature for isothermal operation 00 C, max. temperature for short isotherms in a temperature programme 0 C for 0. mm ID columns the max. temperatures are 80 and 00 C, resp. Medium polar Special selectivity due to high cyanopropyl content Reference column for structure identification, e.g. in combination with OPTIMA Film thickness µm for solvent analyses Similar phases: OV-70, DB-70, CP-SIL 9 CB, HP- 70, Rtx-70, SPB-70, , BP0, ZB m m m m 0 m 0 m 60 m 0. mm ID (0.4 mm OD) 0.0 µm film mm ID (0.4 mm OD) 0. µm film µm film µm film mm ID (0. mm OD) 0.0 µm film µm film µm film µm film µm film mm ID (0.8 mm OD).00 µm film µm film Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are closed 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. For applications with GC capillary columns visit our web site:

18 OPTIMA high performance capillary columns 6% cyanopropyl-phenyl 94% dimethylpolysiloxane CH O Si O Si Max. temperature for isothermal operation 00 C, max. temperature for short isotherms in a temperature programme 0 C Medium polar Ideal for pesticide analyses Similar phases: HP-0, DB-0, SPB-0, Rtx-0, CP-0, (CH ) CN n CH m 0 m m m m 0 m 0 m 60 m 0. mm ID (0.4 mm OD) 0. µm film mm ID (0. mm OD) 0. µm film µm film mm ID (0.8 mm OD).00 µm film Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are closed 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. Analysis of a pesticide mixture Capillary column: OPTIMA 0, 0. µm film, 60 m x 0. mm ID, max. temperature 00/0 C, Cat. No Injection: µl, 80 C ( min) 0 C ( min), pulsed splitless Carrier gas: He, 4 ml/min Temperature: 80 C ( min) 90 C, 0 C/min ( min) 40 C, C/min ( min) 60 C, 0 C/min (0 min) Detector: ECD Peaks (0, ng/µl):. Propyzamide. Vinclozolin. Bromophos-ethyl 4 4.,4-DDT. Brompropylate Analysis of a PCB mixture Capillary column: OPTIMA 0, 0. µm film, 60 m x 0. mm ID, max. temperature 00/0 C, Cat. No Injection: µl, 80 C ( min) 0 C ( min), pulsed splitless Carrier gas: He, 4 ml/min Temperature: 80 C ( min) 90 C, 0 C/min ( min) 40 C, C/min ( min) 60 C, 0 C/min (0 min) Detector: ECD Peaks (0, ng/µl):. PCB 8. PCB. PCB 8 4. PCB. PCB PCB min min For applications with GC capillary columns please ask for our catalogue GC Applications

19 OPTIMA high performance capillary columns cyanopropyl-phenyl-dimethylpolysiloxane Max. temperature for isothermal operation 80 C, max. temperature for short isotherms in a temperature programme 00 C Medium polar Recommended for environmental analyses Similar phases: HP-64, HP-VOC, DB-64, DB-VRX, SPB-64, CP-64, RTX-64, RTX-Volatiles, , BP64, VOCOL USP G 4 Separation of volatile hydrocarbons by Headspace GC Column: OPTIMA 64,.8 µm film, 0 m x 0. mm ID, max. temperature: 80/00 C, Cat. No , Injection: HS cryofocussion, splitless, 0 C Carrier gas: N,. ml/min Temperature: 6 C (4 min), 00 C, 0 C/min, ( min) Detector: ECD, 60 C. Dichloromethane (6,69 min). trans-,-dichloroethene (7,7 min). cis-,-dichloroethene (8,96 min) 4. Trichloromethane (9,46 min).,,-trichloroethane (9,8 min) 6. Tetrachloromethane (0,7 min) 7. Trichloroethene (,44 min) 8.,,-Trichloroethane (,94 min) 9. Tetrachloroethene (4,6 min) min Chromatogram courtesy of R. Mueller, G&P Torsten Plaar Umweltanalytik, Oldenburg, Germany 0 m m m m 0 m 0 m 60 m 0. mm ID (0.4 mm OD).0 µm film mm ID (0.4 mm OD).40 µm film mm ID (0. mm OD).80 µm film mm ID (0.8 mm OD).00 µm film Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are closed 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. For applications with GC capillary columns visit our web site:

20 OPTIMA high performance capillary columns trifluoropropyl-methylpolysiloxane (0% trifluoropropyl) CH O Si (CH ) CF n Aromatic hydrocarbons (BTX) Capillary column: OPTIMA 0, 0. µm film, 0 m x 0. mm ID, max. temperature 40/60 C, Cat. No Injection volume: 0. µl Carrier gas: 0 kpa N (. ml/min) Split: 0 ml/min Temperature: 0 C Detector: FID, 0 C, 6. Benzene. Toluene. Ethylbenzene 4. p-xylene. m-xylene 6. o-xylene 000 Max. temperature for isothermal operation 60 C, max. temperature for short isotherms in a temperature programme 80 C Polar Recommended for environmental analyses Similar phases: OV-0, DB-0, Rtx-00, close equivalent to USP G min 0 0 m m m 0 m 0 m 60 m 0. mm ID (0.4 mm OD) 0. µm film µm film mm ID (0. mm OD) 0. µm film µm film Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are closed 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. For applications with GC capillary columns please ask for our catalogue GC Applications 4

21 OPTIMA high performance capillary columns 0% cyanopropyl-methyl 0% phenylmethylpolysiloxane CH CH Max. temperature for isothermal operation 60 C, max. temperature for short isotherms in a temperature programme 80 C Polar Recommended for fatty acid analyses Similar phases: DB-, HP-, SP-0, OV-, Rtx-, CP-SIL 4, 007-, BP close equivalent to USP G 7 O Si (CH ) CN O Si n Analysis of FAME in porcine fat Column: OPTIMA, 0. µm film, m x 0. mm ID, max. temperature 60/80 C, Cat. No. 76. Injection volume: µl, split :40 Carrier gas: 60 kpa H Temperature: 0 C ( min) C, 0 C/min 60 C, C/min 80 C, 0 C/min 00 C, C/min 0 C, 0 C/min (0 min) Detector: FID 60 C. C 4:0 8. C 8:0. C :0 9. C 8:. C 6:0 0. C 8: 4. C 8:0. C 8:. C 0:0. C 9:0 6. C :0. C 0:0 7. C :0 4. C 0: 8. C :0. C 0: 9. C : 6. C 0:4 0. C 4:0 7. C 0:. C 4: 8. C 0:. C :0 9. C :0. C : 0. C : 4. C 6:0. C :. C 6:. C :6 6. C 7:0. C 4:0 7. C 7: 4. C 4: mv FAME standard 0 4 mv FAME in porcine fat Chromatograms courtesy of Dr. Bantleon, Mr. Leusche, Mr. Hagemann, VFG-Labor, Versmold, Germany min min m m 0 m 0 m 60 m 0. mm ID (0.4 mm OD) 0. µm film mm ID (0. mm OD) 0. µm film Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are closed 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. For applications with GC capillary columns visit our web site:

22 OPTIMA high performance capillary columns % cyanopropyl-methyl 67% dimethylpolysiloxane CH CH No similar phases O Si O Si Max. temperature for isothermal operation 60 C, max. temperature for short isotherms in a temperature programme 80 C Highly polar Recommended for FAMEs, dioxins (CH ) CN n CH m Fatty acid methyl esters cis/trans C 8: (FAME) Capillary column: OPTIMA 40, 0. film, 60 m x 0. mm ID, max. temperature 60/80 C, Cat. No Sample: FAME mixture Injection volume:.0 µl, split : Carrier gas: 0 kpa H Temperature: 80 C 0 C, 0 C/min 60 C (0 min), C/min Detector: FID, 80 C 4. C 4:0 7. trans-c 8: mv. C :0 8. cis-c 8: C 8:0 9. C 8: 0 4. C 0:0 0. C 8: 8. C :0. C 8: 6. C :0. C 0:0 7. C :0. C 0: C 4:0 4. C 0: 9. C 4:. C 0: 0. C :0 6. C 0:4 6. C : 7. C 0:. C 6:0 8. C :0. C 6: 9. C : 4 4. C 7:0 0. C :. C 7:. C 4: 6. C 8: min 0 m m 0 m 0 m 60 m 0. mm ID (0.4 mm OD) 0. µm film µm film mm ID (0. mm OD) 0. µm film µm film µm film Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are closed 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. For applications with GC capillary columns please ask for our catalogue GC Applications 6