Capillary columns for GC

Transcription

1 GC Contents Basic principles of GC Summary of MN standard phases for GC 00 0 OPTIMA high performance capillary columns 0 0 PERMABOND capillary columns Capillary columns for special applications 4 Summary Fast GC 4 Amine separation 6 Enantiomer separation 0 4 Untreated capillaries, retention gaps and deactivated capillaries 6 Fused silica capillary columns, not chemically bonded 6 Reagents for GC Derivatisation reagents Method development kits, concise selection guide 7 Acylation reagents 8 Methylation reagents 9 Silylation reagents 40 4 Test mixtures for GC Test mixtures for capillary columns 44 4 Environmental test mixtures for GC Accessories for GC Ferrules for GC 48 Valco fused silica adaptors and other connectors for capillary columns 49 Glass injection liners, septa Systems for point-of-use gas purification Tools and general accessories for GC 4 MN 97

2 Basic principles of capillary GC The GC system 6 compose the chromatograph:. gas supplies: carrier gas and e. g. burner gases for a flame ionisation detector (FID). sample injector: with direct injection the sample is introduced into the column without contact with other parts from glass or metal (on-column injection); with indirect injection the sample is introduced into an evaporator, and the vapour is then transferred into the column either completely or partially (split technique); both techniques allow low temperatures, high temperatures or temperature programming. capillary column: the heart of the GC system 4. detector: indicates a substance by generation of an electrical signal (response). Some detectors are specific for certain classes of substances or for certain elements (P, N, etc.).. oven with temperature control 6 and/or 7 serve for evaluation of the separation 6. recorder for analogue plotting of chromatograms 7. data station for digital evaluation of chromatograms 4 7 The separation process Chromatographic separation is achieved by repeated distribution of each sample component between two phases: In GC, the mobile phase is always a gas (mostly N, H, He). The stationary phase is a mostly viscous gumlike liquid coated to the inner wall of a capillary column (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. 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 A chromatogram consists of a base line and a number of peaks. The area of a peak allows quantitative determinations: A t 0 t R w / A: starting point of a chromatogram = time of injection of a dissolved solute A component can be identified by its retention time (qualitative determination): t Ri = t 0 + t Riʼ t 0 : dead time = residence time of a solute in the mobile phase (time required by a component to migrate through the chromatographic system without any interaction with the stationary phase) t Ri : retention time = time interval between peak i and the point of injection t Riʼ: net retention time = difference between total retention time and dead time t 0. It indicates how long a substance stays in the stationary phase. Other terms characterising a separation: kʼ: capacity factor: 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. kʼi = t Ri t 0 t 0 t R 98 MN

3 Basic principles of capillary GC α: relative retention, also called separation factor or selectivity coefficient, is the ratio of two capacity factors, the reference substance always being in the denominator. α = kʼ kʼ The relative retention does not provide any information on the quality of a separation, since for equal values 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. a b t [min] R: resolution: a measure for the quality of a separation, taking the peak width at half height (w / ) into account according to t R t R R = (w / ) + (w / ) N th : number of theoretical plates: characterises the quality of a column (should be determined for kʼ > ). 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. The smaller this value the better works the column. N th =.4 ( t Ri w / ) h = HETP = L N th The Van Deemter equation shows how the plate height h depends on the flow velocity u: HETP h min B u u opt. HETP = A + B ū -- + C u C u A Eddy diffusion; for WCOT capillary columns A = 0 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. u Parameters characterising a capillary column OPTIMA,.0 μm film 0 m x 0. mm ID A B C D A. Stationary phase Different chemical structures of stationary phases are responsible for the type of interaction (selectivity) between the phase and the analytes. The stationary phase also limits the temperature range for chromatography. For a detailed summary of MN phases for GC please see the following chapter. B. Film thickness reaches from 0. to.0 µm. The standard film thickness is 0. µm. Thin films (0. 0. µm) are very well suited for high-boiling compounds, temperature labile or very closely eluting substances. Increasing film thickness will increase the capacity, the retention time for low boiling compounds and improve inertness. This is especially useful for samples with widely differing concentrations, or for the separation of volatile polar substances. Better coverage of the column wall by a thicker film and a reduction of the column surface due to a reduced length are favourable for extremely active substrates, which in many cases cause noticeable tailing, if they come in contact with uncoated spots of the column wall. Thick films also mean more phase in the column, and consequently higher bleeding. This results in lower maximum operating temperatures for thick film columns. In addition, thick film columns may have a lower efficiency. C. Column length column length is directly proportional to the separation efficiency (number of plates N). Routine separations are most frequently performed on or 0 m columns, while complex mixtures may require 0 or 60 m columns. 0 m columns with 0. mm ID are used for fast GC (see page 4) D. Inner diameter (ID) the lower the ID, the higher is the theoretically possible number of plates per meter; mm ID: for high resolution and short retention times with low carrier gas flows 0. mm ID: for analyses of complex mixtures 0. mm ID: for routine analyses with short retention times, but increased capacity 0. mm ID: for rapid separations with inert surface and highest capacity MN 99

4 Summary of MN phases for GC MN offers more than 40 different phases for gas chromatography from very nonpolar to polar columns. Nonpolar stationary phases (e. g. 00 % dimethylpolysiloxane phases) separate by volatility (i. e. boiling point) only. Typical analytes are linear hydrocarbons (n-alkanes). Polar phases offer additional interactions, which may improve a separation. When increasing the polarity, e. g. by introducing 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 (WAX) are the best choice for a separation. Typical analytes are alcohols and carboxylic acids. 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 task. About 70 % of all separations can be performed on non- to midpolar columns. These columns generally feature high temperature stability. For columns for special separations please see page. Comparison of separation properties of selected OPTIMA phases OPTIMA 40 max. temp. 60/80 C Cat. No OPTIMA max. temp. 60/80 C Cat. No OPTIMA 0 max. temp. 60/80 C Cat. No OPTIMA 70 max. temp. 0/40 C Cat. No OPTIMA 7 max. temp. 0/40 C Cat. No OPTIMA max. temp. 40/60 C Cat. No OPTIMA max. temp. 40/60 C Cat. No increasing polarity min 0 All columns: 0. µm film, 0 m x 0. mm ID Sample: MN-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 00 MN

5 Summary of MN phases for GC Phase Composition max. Temperature USP Similar phases Page OPTIMA 00 % dimethylpolysiloxane 40/60 C OPTIMA MS 00 % dimethylpolysiloxane 40/60 C OPTIMA MS Accent OPTIMA OPTIMA MS OPTIMA MS Accent OPTIMA XLB 00 % dimethylpolysiloxane 40/60 C % phenyl 9 % dimethylpolysiloxane % diphenyl - 9 % dimethylpolysiloxane silarylene phase with selectivity similar to % diphenyl 9 % dimethylpolysiloxane silarylene phase as above, higher aromatic content 40/60 C 40/60 C 40/60 C G G G8 G G G8 G G G8 G7 G6 G7 G6 G7 G6 PERMABOND SE-0 (page ), OV-, DB-, SE-0, HP-, SPB-, CP-Sil CB, Rtx -, 007-, BP, MDN-, AT -, ZB-, OV-0 Ultra-, DB-MS, HP-MS, Rtx -MS, Equity -, AT -MS, VF-MS, CP-Sil CB MS PERMABOND SE- (page ), SE-4, SE-, DB-, HP-, SPB-, CP-Sil 8, Rtx -, 007-, BP, MDN-, AT -, ZB- DB-MS, HP-MS, Ultra-, Equity -, CP-Sil 8CB low bleed/ms, Rtx -SIL-MS, Rtx -MS, 007-MS, BPX, MDN-S, AT -MS, VF-MS /60 C DB-XLB, Rtx -XLB, MDN-, VF-XMS OPTIMA δ- phase with autoselectivity 40/60 C G49 no similar phases 0 OPTIMA δ-6 phase with autoselectivity 40/60 C no similar phases 04 OPTIMA 7 OPTIMA 0 OPTIMA 64 phenylmethylpolysiloxane, 0 % phenyl 6 % cyanopropylphenyl 94 % dimethylpolysiloxane 6 % cyanopropylphenyl 94 % dimethylpolysiloxane OPTIMA 64 LB as above, low bleed phase 80/00 C G4 OPTIMA 70 OPTIMA 0 OPTIMA OPTIMA 40 OPTIMA WAX OPTIMA FFAP 4 % cyanopropylphenyl 86 % dimethylpolysiloxane trifluoropropylmethylpolysiloxane (0 % trifluoropropyl) 0 % cyanopropylmethyl 0 % phenylmethylpolysiloxane % cyanopropylmethyl 67 % dimethylpolysiloxane polyethylene glycol daltons polyethylene glycol -nitroterephthalate 0/40 C G OV-7, DB-7, HP-0+, HP-7, SPB-0, SP- 0, Rtx -0, CP-Sil 4 CB, 007-7, ZB-0 00/0 C G4 HP-0, DB-0, SPB-0, Rtx -0, CP-0, /00 C G4 HP-64, HP-VOC, DB-64, DB-VRX, SPB-64, CP-64, Rtx -64, Rtx -Volatiles, , BP64, VOCOL OV-70, DB-70, CP-Sil 9 CB, HP-70, 00/0 C G46 Rtx -70, SPB-70, , BP0, ZB /80 C G6 OV-0, DB-0, Rtx -00, /80 C G7 G9 DB-, HP-, OV-, Rtx -, CP-Sil 4, 007-, BP 7 60/80 C no similar phases 8 0/60 C G6 0/60 C PERMABOND CW 0 M (page ), DB- Wax, Supelcowax, HP-Wax, HP-INNOWax, Rtx -Wax, CP-Wax CB, Stabilwax, 007-CW, BP0, AT -Wax, ZB-Wax PERMABOND FFAP (page ), DB-FFAP, HP- FFAP, CP-SIL 8 CB, 007-FFAP, CP-FFAP CB, Nukol first temperature for isothermal operation, second value for short isotherms in a temperature programme Please note, that for columns with 0. mm ID and for columns with thicker films temperature limits are generally lower. For details refer to the description of individual phases. phases which provide a similar selectivity based on chemical and physical properties G G 9 0 see description on page 0 MN 0

6 OPTIMA δ unique phases with autoselectivity permanent dipole: constant interactions dipoles of the analytes conventional phase permanent dipoles of the stationary phase induced dipoles of OPTIMA δ phases OPTIMA δ- OPTIMA δ-6 OV- SE-4 OV-7 OV-70 OV-0 OV-40 OPTIMA δ permanent + induced dipole: autoselectivity range of polarities covered by OPTIMA δ phases Key features of the OPTIMA δ are: wide range of applications due to autoselectivity outstanding thermal stability similar to nonpolar phases low bleed levels extremely inert medium polar without CN groups All stationary phases in GC offer a selectivity, called polarisability, that is influenced by the sample, but OPTIMA δ- and OPTIMA δ-6 offer this valuable feature to a greater extent than any other phase. The polymers consist of cross-linked polysiloxane 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 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. 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-. 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 Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are melted or closed with septa, and thus protected from atmospheric oxygen. Additionally, we supply the corresponding test mixture with each column. On request, all columns can be supplied on a inch ( cm) cage for the Agilent GC 680. For ordering, please add an E at the end of the catalogue number (e. g E) 0 MN

7 OPTIMA δ unique phases with autoselectivity OPTIMA δ- medium polar without CN groups analytes determine the polarity of the phase unique from MN, no similar phase ideal for MSD and PND detectors USP G49 polysiloxane phase with autoselectivity 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 Analysis of isomeric phenols 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 9 Detector: MSD HP 97. Phenol. -Chlorophenol. -Methylphenol 4. 4-Methylphenol. -Methylphenol 6.,4-Dimethylphenol 7. -Nitrophenol 8.,4-Dichlorophenol 9.,6-Dichlorophenol 0. 4-Chloro--methylphenol.,,-Trichlorophenol.,4,6-Trichlorophenol.,4,-Trichlorophenol 4.,,4-Trichlorophenol.,,6-Trichlorophenol 6.,,,6-Tetrachlorophenol 7.,,4,-Tetrachlorophenol 8.,,4,6-Tetrachlorophenol 9.,4-Dinitrophenol 0.,4,-Trichlorophenol. -Methyl-4,6-dinitrophenol. -Isopropyl-4,6-dinitrophenol min MN Appl. No Length 0 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 In addition to this standard programme we will be happy to supply columns custom-made to your specifications. MN 0

8 OPTIMA δ unique phases with autoselectivity OPTIMA δ-6 medium polar without CN groups analytes determine the polarity of the phase unique from MN, no similar phase ideal for MSD and PND detectors polysiloxane phase with autoselectivity 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 Separation of organophosphorus pesticides (EPA 840/84) 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 0 Temperature: Detector: MSD HP 97. Dichlorvos. Mevinphos. Demeton-s 4. Ethoprop. Naled 6. Phorate 7. Demeton-o 8. Diazinon 9. Disulfoton 0. Ronnel. Parathion-methyl. Chlorpyrifos. Trichloronate 4. Fenthion. Merphos 6. Stirofos 7. Tokuthion 8. Merphos oxidation product 9. Fensulfothion 0. Bolstar. Azinphos-methyl. Coumaphos MN Appl. No C 00 C (0 min),. C/min 0. mm ID (0.4 mm OD) 0.0 µm film Length 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. µm film mm ID (0. mm OD) 0. µm film µm film µm film mm ID (0.8 mm OD).00 µm film In addition to this standard programme we will be happy to supply columns custom-made to your specifications MN

9 OPTIMA high performance capillary columns OPTIMA 00 % dimethylpolysiloxane nonpolar phase O Si n similar phases: PERMABOND SE-0 (page ), OV-, DB-, SE-0, HP-, SPB-, CP-Sil CB, Rtx-, 007-, BP, MDN-, AT-, ZB-, OV-0 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. separation of components according to boiling points thick film columns µm film are especially recommended for solvent analysis USP G / G / G8 Length 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 In addition to this standard programme we will be happy to supply columns custom-made to your specifications. Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are melted or closed with septa, and thus protected from atmospheric oxygen. Additionally, we supply the corresponding test mixture with each column. On request, all columns can be supplied on a inch ( cm) cage for the Agilent GC 680. For ordering, please add an E at the end of the catalogue number (e. g E) MN 0

10 OPTIMA high performance capillary columns Solvent analysis 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. Methanol. Ethanol. Acetone 4. -Propanol. Methyl acetate 6. n-propanol 7. Methyl ethyl ketone 8. Ethyl acetate 9. Isobutanol 0. n-butanol. -Methoxy--propanol. Isooctane. Ethyl glycol 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 OPTIMA MS selectivity identical to OPTIMA O Si n min 0 similar phases: Ultra-, DB-MS, HP-MS, Rtx- MS, Equity-, AT-MS, VF-MS, CP-Sil CB MS MN Appl. No % dimethylpolysiloxane max. temperature for isothermal operation 40 C, max. temperature for short isotherms in a temperature programme 60 C phase with low bleeding ideal for GC/MS and ECD applications and general analyses at trace level USP G / G / G8 Length 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 In addition to this standard programme we will be happy to supply columns custom-made to your specifications MN

11 OPTIMA high performance capillary columns OPTIMA MS Accent selectivity identical to OPTIMA O Si n NEW! increased sensitivity due to an unmatched low background level USP G / G / G8 00 % dimethylpolysiloxane max. temperature for isothermal operation 40 C, max. temperature for short isotherms in a temperature programme 60 C lowest column bleed, nonpolar phase, ideal for ion trap and quadrupol MS detectors perfect inertness for basic compounds solvent rinsing for removal of impurities applicable application areas: all-round phase for environmental analyses, trace analyses, EPA methods, pesticides, PCB, food and drug analyses similar phases: Ultra-, DB- MS, HP- MS, Rtx- MS, Equity-, AT- MS, VF- MS, CP-Sil CB MS EPA 840 / 84 / 84 A Organophosphorus pesticides Column: OPTIMA MS Accent, 0.0 µm film, 0 m x 0. mm ID, Cat. No Sample: 0. µg/ml in hexane, 840/84 OP pesticides calibration mix A and 84 OP pesticides calibration mix B; IS triphenyl phosphate and tributyl phosphate Injection: splitless (hold min) Inj. temperature: 0 C Carrier gas: He, ml/min, constant pressure Temperature: 00 C 80 C, 0 C/min ( min) 00 C, 8 C/min ( min) Detector: FPD (Flame Photometric Detector), 80 C. Dichlorvos,. Hexamethylphosphoramide,. Mevinphos, 4. Trichlorfon,. TEPP, 6. Thionazin, 7. Demeton-0, 8. Ethoprop 9. Tributyl phosphate (IS), 0. Dicrotophos,. Monocrotophos,. Naled,. Sulfotepp, 4. Phorate,. Dimethoate, 6. Demeton-S, 7. Dioxathion, 8. Terbufos, 9. Fonophos, 0. Phosphamidon isomer,. Diazinon,. Disulfoton,. Phosphamidon, 4. Dichlorofenthion,. Parathion-methyl, 6. Chlorpyrifos methyl, 7. Ronnel, 8. Fenitrothion, 9. Malathion, 0. Fenthion,. Aspon,. Parathion-ethyl,. Chlorpyrifos, 4. Trichloronate,. Chlorfenvinphos, 6. Merphos, 7. Crotoxyphos, 8. Stirofos, 9. Tokuthion, 40. Merphos oxidation product, 4. Fensulfothion, 4. Famphur, 4. Ethion, 44. Bolstar, 4. Carbophenothion, 46. Triphenyl phosphate (IS), 47. Phosmet, 48. EPN, 49. Azinphos-methyl, 0. Leptophos,. Tri-o-cresyl phosphate,. Azinphos-ethyl,. Coumaphos MN Appl. No min Length 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 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 melted or closed with septa, and thus protected from atmospheric oxygen. Additionally, we supply the corresponding test mixture with each column. MN 07

12 OPTIMA high performance capillary columns OPTIMA nonpolar phase O Si m O Si similar phases: PERMABOND SE- (page ), SE-4, SE-, DB-, HP-, SPB-, CP-Sil 8, Rtx-, 007-, BP, MDN-, AT-, ZB- n % phenyl 9 % methylpolysiloxane 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. standard phase with large range of application USP G7 / G6 Length 0 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 In addition to this standard programme we will be happy to supply columns custom-made to your specifications. Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are melted or closed with septa, and thus protected from atmospheric oxygen. Additionally, we supply the corresponding test mixture with each column. On request, all columns can be supplied on a inch ( cm) cage for the Agilent GC 680. For ordering, please add an E at the end of the catalogue number (e. g E) 08 MN

13 OPTIMA high performance capillary columns OPTIMA MS selectivity identical to OPTIMA O Si O Si m n similar phases see OPTIMA MS Accent page 0 % diphenyl 9 % dimethylpolysiloxane max. temperature for isothermal operation 40 C, max. temperature for short isotherms in a temperature programme 60 C phase with low bleeding ideal for GC/MS and ECD applications and general analyses at trace level perfect inertness for basic compounds USP G7 / G6 Analysis of various phenols Column: OPTIMA MS, 0 m x 0. mm ID, 0. µm film, Cat. No , max. temperature 40/60 C Sample: ppm of each compound except N-i-propylaniline (9.4 ppm) Method: SPME Temperature: 40 C ( min) 40 C, 6 C/min 0 C, 0 C/min Detector: MSD. Toluene-D 8. Phenol. -Methylphenol (o-cresol) 4. Nitrobenzene-D. N-i-Propylaniline 6.,4-Dichlorophenol 7. 4-Chlorophenol 8. 4-Bromo--chlorophenol 9. -Bromophenol 0. 4-Chloro--methylphenol.,4-Dibromophenol. -Hydroxybiphenyl. -Cyclohexylphenol 4. Hexafluorobisphenol A Courtesy of Riedel-de-Haën, Seelze, Germany MN Appl. No min Length 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 In addition to this standard programme we will be happy to supply columns custom-made to your specifications. MN 09

14 OPTIMA high performance capillary columns OPTIMA -MS Accent chemically bonded, cross-linked silarylene phase with polarity similar to a % diphenyl - 9 % dimethylpolysiloxane phase O Si O Si Si increased sensitivity due to an unmatched low background level The bleed comparison test of the OPTIMA -MS Accent with a conventional -MS phase shows the outstanding performance of the silarylene phase. Background noise at 40 C FID signal in mv O Si standard MS phase s n max. temperature for isothermal operation 40 C, max. temperature for short isotherms in a temperature programme 60 C, for columns with films > 0. µm max. temperatures are 0 and 40 C, respectively lowest column bleed, nonpolar phase, ideal for ion trap and quadrupol MS detectors solvent rinsing for removal of impurities applicable application areas: all-round phase for environmental analyses, trace analyses, EPA methods, pesticides, PCB, food and drug analyses similar phases: DB- MS, HP- MS, Ultra-, Equity-, CP-Sil 8 CB low bleed/ms, Rtx-SIL-MS, Rtx- MS, 007- MS, BPX, MDN-S, AT- MS, VF- MS USP G7 / G6 NEW! silarylene phase The unmatched low background level of the OPTIMA MS Accent, which is approximately three times lower compared to a MS brand column, provides significantly increased sensitivity and allows the application in trace analyses particularly of high-boiling compounds OPTIMA MS Accent s Length 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 melted or closed with septa, and thus protected from atmospheric oxygen. Additionally, we supply the corresponding test mixture with each column. 0 MN

15 OPTIMA high performance capillary columns OPTIMA XLB chemically bonded, cross-linked silarylene phase, optimised silarylene content for lowest column bleed O Si O Si Si similar phases: DB-XLB, Rtx-XLB, MDN-, VF-XMS O Si n NEW! Rapid separation of PCB and PAH Column: OPTIMA XLB, 0. µm film, 0 m x 0. mm ID, Cat. No Injection volume: µl, standard 0.00 ng/µl Injection: 0 C, pulsed, splitless, pulse.8 bar in min Purge flow: 60 ml/min He Temperature: 40 C ( min) 40 C ( min), 0 C/min 40 C ( min), 0 C/min Detection: MS source 0 C, interface 80 C, quadrupol 0 C : PCB- 9: PCB-8 8/9 0 8 % separation in less than 0 min! silarylene phase max. temperature for isothermal operation 40 C, max. temperature for short isotherms in a temperature programme 60 C, lowest column bleed, nonpolar phase, ideal for ion trap and quadrupol MS detectors perfect inertness for basic compounds solvent rinsing for removal of impurities applicable application areas: ultra low bleed phase, highly selective for environmental and trace analyses, pesticides recommended phase for PCB separations 4 6 benzo[b]fluoranthene / benzo[b]fluoranthene 7 % separation in 7 min! min Courtesy of Centre d Analyses de Recherche, Lab. d Hydrologie, F-6400 Illkirch, France MN Appl. No. 90. Naphthalene. -Methylnaphthalene. Acenaphthylene 4. Acenaphthene. Fluorene 6. Phenanthrene 7. Anthracene 8. PCB- 9. PCB-8 0. PCB-. Fluoranthene. PCB-0. Pyrene 4. PCB-77. -Methylfluoranthene 6. PCB-8 7. PCB- 8. PCB-8 9. PCB-6 0. PCB-80. Benz[a]anthracene. Chrysene. PCB PCB-94. Benzo[b]fluoranthene 6. Benzo[k]fluoranthene 7. Benzo[a]pyrene 8. Dibenz[ah]anthracene 9. Indeno[,,-cd)pyrene 0. Benzo[ghi]perylene Length 0 m 60 m 0. mm ID (0.4 mm OD) 0. µm film On request, all columns can be supplied on a inch ( cm) cage for the Agilent GC 680. For ordering, please add an E at the end of the catalogue number (e. g E). MN

16 OPTIMA high performance capillary columns OPTIMA 7 medium polar phase O Si m similar phases: OV-7, DB-7, HP-0+, HP-7, SPB-0, SP-0, Rtx-0, CP-Sil 4 CB, 007-7, ZB-0 phenylmethylpolysiloxane (0 % phenyl) 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 00 and 0 C, resp. suitable for higher temperatures preferred applications: steroids, pesticides, drug analyses USP G Column: Samples: OPTIMA 7, 0.0 µm film, m x 0.0 mm ID, max. temperature 0/40 C, Cat. No pesticides, standard of the cantonal laboratory Schaffhausen (Switzerland), 0. mg/ml or 0.0 mg/ml each Injection volume:.0 µl Carrier gas: He, cm/s, sec without split Temperature: 00 C ( min), 8 C/min 0 C, 0 C/min 0 C Detector: MSD HP 97 Analysis of pesticides min. Dichlorphos. Naled. Vinclozolin 4. Chlorthalonil. Chlorpyrifos 6. Dichlofluanid 7. Procymidon 8. Captan 9. Folpet 0. Carbophenothion. Iprodion. Captafol. Coumaphos MN Appl. No Length 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 In addition to this standard programme we will be happy to supply columns custom-made to your specifications. On request, all columns can be supplied on a inch ( cm) cage for the Agilent GC 680. For ordering, please add an E at the end of the catalogue number (e. g E) MN

17 OPTIMA high performance capillary columns OPTIMA 70 medium polar phase O Si (CH ) m O CN similar phases: OV-70, DB-70, CP-Sil 9 CB, HP-70, Rtx-70, SPB-70, , BP0, ZB-70 Si Analysis of aromatic hydrocarbons Column: OPTIMA 70, 0. µm film, m x 0. mm ID, Cat. No. 768., max. temperature 00/0 C Injection volume: µl Carrier gas: 0.6 bar N Split: :40 Temperature: 60 C 0 C, 4 C/min Detector: FID 60 C. Benzene. Toluene. Ethylbenzene 4. p-xylene. o-xylene 6. Phenol 7. -Methylphenol 8.,6-Dimethylphenol 9. 4-Methylphenol 0.,4-Dimethylphenol.,4,6-Trimethylphenol MN Appl. No % cyanopropyl-phenyl 86 % dimethylpolysiloxane n 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. special selectivity due to high cyanopropyl content reference column for structure identification, e. g. in combination with OPTIMA film thickness µm for solvent analyses USP G min Length 0 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. µm film µm film µm film µm film mm ID (0.8 mm OD).00 µm film µm film In addition to this standard programme we will be happy to supply columns custom-made to your specifications. MN

18 OPTIMA high performance capillary columns OPTIMA 0 6 % cyanopropyl-phenyl 94 % dimethylpolysiloxane medium polar phase O Si O (CH ) m Si n max. temperature for isothermal operation 00 C, max. temperature for short isotherms in a temperature programme 0 C ideal for pesticide analyses for corresponding columns with higher film thickness see OPTIMA 64 USP G4 CN similar phases: HP-0, DB-0, SPB-0, Rtx-0, CP-0, Analysis of a pesticide mixture Column: OPTIMA 0, 0. µm film, 60 m x 0. mm ID, max. temperature 00/0 C, Cat. No Injection: µl (0. ng/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 :. Propyzamide. Vinclozolin. Bromophos-ethyl 4.,4-DDT 4. Brompropylate 0 0 min MN Appl. No. 060 Analysis of a PCB mixture Column: OPTIMA 0, 0. µm film, 60 m x 0. mm ID, max. temperature 00/0 C, Cat. No Injection: µl (0. ng/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 :. PCB-8. PCB-. PCB-8 4. PCB-. PCB-8 6. PCB min MN Appl. No. 060 Length 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 In addition to this standard programme we will be happy to supply columns custom-made to your specifications. Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are melted or closed with septa, and thus protected from atmospheric oxygen. Additionally, we supply the corresponding test mixture with each column. 4 MN

19 OPTIMA high performance capillary columns OPTIMA 64 medium polar phase O Si (CH ) m O Si CN similar phases: HP-64, HP-VOC, DB-64, DB-VRX, SPB-64, CP-64, Rtx-64, Rtx-Volatiles, , BP64, VOCOL 6 % cyanopropyl-phenyl 94 % dimethylpolysiloxane n max. temperature for isothermal operation 80 C, max. temperature for short isotherms in a temperature programme 00 C recommended for environmental analyses for corresponding columns with lower film thickness see OPTIMA 0 USP G4 OPTIMA 64 LB 6 % cyanopropyl-phenyl 94 % dimethylpolysiloxane excellent Low Bleed columns for halogenated hydrocarbons, volatiles, aromatic compounds, solvents etc. Solvents and semi-volatiles Column: OPTIMA 64 LB,.8 µm film, 0 m x 0. mm ID, Cat. No ; retention gap Phe-Sil 0. m x 0. mm, 00 C (8 C/min), 0 min 00 C Cat. No Carrier gas:. bar He Temperature: 4 C ( min) 0 C (6 C/min) 4 7 Injection: µl (0 ppm per substance in acetone), 8 cold on-column Detection: FID 80 C 6. Acetone. Decane 7. Ethyl acetate. Octanol- 8. Tetrahydrofuran. Acetophenone 9 4. Cyclohexane 4. Butyrophenone Methyl--butanol-. Heptanophenone 6. Butanol- 6. Methoxy--indole 9 7. Pyridine 7. Dibenzylamine 0 8. Toluene 8. Methyl eicosanoate 9. Dimethylformamide 9. Methyl cis--docosenoate 0. Dimethylsulfoxide 0. Methyl docosanoate OPTIMA 64 OPTIMA 64 LB MN Appl. No min Length 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 mm ID (0. mm OD).80 µm film In addition to this standard programme we will be happy to supply columns custom-made to your specifications. On request, all columns can be supplied on a inch ( cm) cage for the Agilent GC 680. For ordering, please add an E at the end of the catalogue number (e. g E) MN

20 OPTIMA high performance capillary columns OPTIMA 0 trifluoropropyl-methylpolysiloxane (0 % trifluoropropyl) polar phase O Si (CH ) CF n similar phases: OV-0, DB-0, Rtx-00, max. temperature for isothermal operation 60 C, max. temperature for short isotherms in a temperature programme 80 C recommended for environmental analyses, especially for o-, m- and p-substituted aromatic hydrocarbons close equivalent to USP G6 Aromatic hydrocarbons (BTX) 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 MN Appl. No min Length 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 In addition to this standard programme we will be happy to supply columns custom-made to your specifications. Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are melted or closed with septa, and thus protected from atmospheric oxygen. Additionally, we supply the corresponding test mixture with each column. 6 MN

21 OPTIMA high performance capillary columns OPTIMA 0 % cyanopropyl-methyl 0 % phenylmethylpolysiloxane polar phase O Si O Si max. temperature for isothermal operation 60 C, max. temperature for short isotherms in a temperature programme 80 C recommended for fatty acid analyses close equivalent to USP G7 / G9 (CH ) n CN similar phases: DB-, HP-, OV-, Rtx-, CP-Sil 4, 007-, BP 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 FAME standard FAME in porcine fat C4:0 8. C8: C:0 9. C8: 9. C6:0 4. C8:0. C0:0 6. C:0 7. C:0 8. C:0 9. C: 0. C4:0. C4: 0. C8:. C8:. C9:0. C0:0 4. C0:. C0: 6. C0:4 7. C0: 8. C0: 8. C:0. C: 9. C:0 0. C: C6:0. C:. C6:. C:6 6. C7:0. C4: C7: 4. C4: Courtesy of Dr. Bantleon, Mr. Leusche, Mr. Hagemann, VFG-Labor, Versmold, Germany MN Appl. No min min 0.0 mm ID (0.4 mm OD) 0.0 µm film Length 0 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 In addition to this standard programme we will be happy to supply columns custom-made to your specifications. On request, all columns can be supplied on a inch ( cm) cage for the Agilent GC 680. For ordering, please add an E at the end of the catalogue number (e. g E) MN 7

22 OPTIMA high performance capillary columns OPTIMA 40 polar phase O Si O Si % cyanopropyl-methyl 67 % dimethylpolysiloxane max. temperature for isothermal operation 60 C, max. temperature for short isotherms in a temperature programme 80 C recommended for FAMEs, dioxins (CH ) m n CN no similar phases Fatty acid methyl esters cis/trans C 8: (FAME) 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. C4:0 7. trans-c8:. C:0 8. cis-c8: 4. C8:0 9. C8: C0:0 0. C8: 0. C:0. C8: 6. C:0. C0:0 7. C:0. C0: 8 8. C4:0 4. C0: C4:. C0: 9 0. C:0 6. C0:4. C: 7. C0: 6. C6:0 8. C:0 0. C6: 9. C: 4. C7:0 0. C: 4. C7:. C4: 6. C8:0 MN Appl. No min Length 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 In addition to this standard programme we will be happy to supply columns custom-made to your specifications. 0 Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are melted or closed with septa, and thus protected from atmospheric oxygen. Additionally, we supply the corresponding test mixture with each column. 8 MN

23 OPTIMA high performance capillary columns OPTIMA WAX polar phase H O H C H H C H n OH similar phases: PERMABOND CW 0 M (page ), DB-Wax, Supelcowax, HP-Wax, HP-INNOWAX, Rtx-Wax, CP-Wax CB, Stabilwax, 007-CW, BP0, AT-Wax, ZB-Wax polyethylene glycol dalton for columns with mm ID the max. temperature for isothermal operation is 0 C, the max. temperature for short isotherms in a temperature programme is 60 C for 0. mm ID columns the max. temperatures are 0 and 40 C, resp. recommended for solvent analysis and alcohols suitable for aqueous solutions USP G6 Modified Grob test Column: OPTIMA WAX, 0. µm film, 0 m x 0. mm ID, max. temperature 0/60 C, Cat. No Injection volume: µl Carrier gas:. bar He Split: :0 4 6 Temperature: 80 C 0 C, 8 C/min Detector: FID 0 C. Decane. Undecane. Octanol 4. Methyl decanoate. Dicyclohexylamine 6. Methyl undecanoate 7. Methyl dodecanoate 8.,6-Dimethylaniline 9.,6-Dimethylphenol MN Appl. No min Length 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 µm film In addition to this standard programme we will be happy to supply columns custom-made to your specifications. On request, all columns can be supplied on a inch ( cm) cage for the Agilent GC 680. For ordering, please add an E at the end of the catalogue number (e. g E) MN 9

24 OPTIMA high performance capillary columns OPTIMA FFAP polar phase similar phases: PERMABOND FFAP (page ), DB-FFAP, HP-FFAP, CP-Sil 8 CB, 007-FFAP, CP-FFAP CB, Nukol close equivalent to USP G / G polyethylene glycol -nitroterephthalate for columns with mm ID the max. temperature for isothermal operation is 0 C, the max. temperature for short isotherms in a temperature programme is 60 C for 0. mm ID columns the max. temperatures are 0 and 40 C, resp. recommended for FAME, free carboxylic acids FAME test Column: OPTIMA FFAP, 0. µm film, 60 m x 0. mm ID, max. temperature 0/60 C, Cat. No Carrier gas:. bar He, split Temperature: C 0 C, 6 C/min Injection:.0 µl, 0 C Detector: FID 0 C 4. C4. C6. C C0. C C4 7. C6 8. C C8: cis/trans 0. C8: 4. C8:. C0. C 4. C:. C4 0.0 mm ID (0.4 mm OD) 0.0 µm film MN Appl. No min Length 0 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) 0.0 µm film µm film In addition to this standard programme we will be happy to supply columns custom-made to your specifications. Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are melted or closed with septa, and thus protected from atmospheric oxygen. Additionally, we supply the corresponding test mixture with each column. 0 MN

25 PERMABOND capillary columns PERMABOND SE-0 nonpolar phase 00 % dimethylpolysiloxane max. temperature for isothermal operation 00 C, max. temperature for short isotherms in a temperature programme 0 C O Si n Length m 0 m 0. mm ID (0.4 mm OD) 0. µm film mm ID (0. mm OD) 0. µm film µm film In addition to this standard programme we will be happy to supply columns custom-made to your specifications. PERMABOND SE- nonpolar phase O Si m O Si Length n % phenyl 9 % dimethylpolysiloxane m 0. mm ID (0.4 mm OD) 0. µm film mm ID (0. mm OD) 0. µm film µm film 7. max. temperature for isothermal operation 00 C, max. temperature for short isotherms in a temperature programme 0 C In addition to this standard programme we will be happy to supply columns custom-made to your specifications. Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Column ends are melted or closed with septa, and thus protected from atmospheric oxygen. Additionally, we supply the corresponding test mixture with each column. MN

26 PERMABOND capillary columns PERMABOND CW 0 M polar phase H H H O C C OH H H n similar phases see OPTIMA WAX page 9 polyethylene glycol dalton mm ID: max. temperature for isothermal operation 0 C, max. temperature for short isotherms in a temperature programme 40 C 0. mm ID: max temperatures 00 and 0 C, resp. recommended for solvent analyses and alcohols suitable for aqueous solutions USP G6 Length 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. µm film mm ID (0. mm OD) 0. µm film µm film µm film mm ID (0.8 mm OD) 0.0 µm film µm film µm film In addition to this standard programme we will be happy to supply columns custom-made to your specifications. PERMABOND FFAP polar phase similar phases see OPTIMA FFAP page 0 polyethylene glycol -nitroterephthalate mm ID: max. temperature for isothermal operation 0 C, max. temperature for short isotherms in a temperature programme 40 C; 0. mm ID: max temperatures 00 and 0 C, resp. recommended for FAME, free carboxylic acids Length 0 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 mm ID (0. mm OD) 0.0 µm film µm film µm film µm film mm ID (0.8 mm OD).00 µm film In addition to this standard programme we will be happy to supply columns custom-made to your specifications. MN

27 Capillary columns for special separations Capillary columns for special GC separations Certain analytical separations can be performed more easily with chromatographic columns, which have been especially developed for the respective task. The following table summarises our programme of GC speciality capillaries, the individual column types are described in detail on the following pages. Separation / special application Recommended capillary column Page Fast GC OPTIMA δ-, OPTIMA δ-6 OPTIMA, OPTIMA, OPTIMA 7, OPTIMA, OPTIMA FFAP PERMABOND CW 0 M, FFAP all 0.0 mm ID 4 Amines polyfunctional amines OPTIMA Amine amine separations FS-CW 0 M-AM 6 Petrochemical products (complex hydrocarbon mixtures) PERMABOND P-00 6 Environmental analyses volatile halogenated hydrocarbons PERMABOND SE-4 HKW 7 Triglycerides OPTIMA -TG OPTIMA 7-TG Silanes (monomeric, e. g. chlorosilanes) PERMABOND Silane 9 Diethylene glycol, e. g. for the quality control of wine PERMABOND CW 0 M-DEG 9 Enantiomer separation cyclodextrin phases FS-LIPODEX A FS-LIPODEX B FS-LIPODEX C FS-LIPODEX D FS-LIPODEX E FS-LIPODEX G FS-HYDRODEX β-pm FS-HYDRODEX β- P FS-HYDRODEX β-6tbdm FS-HYDRODEX β-tbdac FS-HYDRODEX γ-tbdac diamide type chiral polysiloxane PERMABOND L-CHIRASIL-VAL MN

28 Capillary columns for special separations Columns for fast GC characteristics of fast GC: decreased column diameters, high heating rates and decreased column lengths for faster GC separations with high resolution efficiency small inner diameters combined with very fast temperature programmes can reduce the analysis time by up to 80 % high heating rates place special demands on stationary phases: OPTIMA columns meet exactly this requirement, as they show very low bleeding and provide long lifetimes, even when continuously subjected to high heating rates small inner diameters result in high column inlet pressures and a lower volume flow of the mobile phase, which as a consequence require very fast injection of very small samples against a high pressure the amount of sample, which can be injected, is limited by the inner diameter and the thin film high sensitivity detectors with small volume and extremely short response time, as well as a very rapid data acquisition and processing are required Comparison of a separation on a 0 m standard capillary with separation on a 0 m fast GC column A) Fast GC column B) standard GC column Column: OPTIMA, 0. µm film, 0 m x 0. mm ID, Column: OPTIMA, 0. µm film, 0 m x 0. mm ID, max. temperature 40/60 C, Cat. No max. temperature 40/60 C, Cat. No injection µl, split : 40, carrier gas 0.7 bar He injection µl, split :, carrier gas. bar He both separations: temperature: 4 80 C 0 C (0 min), 8 C/min, detector: FID 6 7 While maintaining the temperature programme and halving the 8 pressure a time saving of 0 % results with identical separation efficiency.. Octanol 8. Undecane Dimethylaniline 4. Dodecane. Decylamine 6. Methyl decanoate 7. Methyl undecanoate 8. Henicosane 9. Docosane 0. Tricosane MN Appl. No min min Phase max. temperature ID [mm] film thickness [µm] Cat. No. (0 m) Cat. No. (0 m) 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 60/80 C OPTIMA FFAP 0/60 C PERMABOND CW 0 M 0/40 C PERMABOND FFAP 0/40 C OPTIMA Amine 00/0 C FS-CW 0 M-AM 0/40 C FS-LIPODEX E 00/0 C FS-HYDRODEX β-6tbdm 0/0 C In addition to this standard programme, all MN GC phases can be custom-made as fast GC columns. 4 MN

29 Capillary columns for special separations OPTIMA Amine especially deactivated for the analysis of polyfunctional amines such as ethanolamines, amino-functionalised diols and similar compounds, which are important base materials in industrial chemistry, and shows strong tailing on standard-deactivated columns similar phases: Rtx- Amine, PTA- USP G7 / G6 special column for analysis of amines max. temperature for isothermal operation 00 C, max. temperature for short isotherms in a temperature programme 0 C improved linearity for analyses of active components at trace levels: no amine absorptions even for aliphatic and aromatic amines at concentrations of 00 pg/peak tested with the OPTIMA Amine test mixture (Cat. No. 77), which among others also contains diethanolamine and propanol-pyridine (this test mixture is supplied with each column) Separation of secondary and tertiary amines Column: OPTIMA Amine, 0. µm film, 0 m x 0. mm ID, max. temperature 00/0 C, Cat. No Injection volume: µl Carrier gas: 0.6 bar H, split :00 Temperature: 00 C ( min) 80 C, 0 C/min Detector: FID 80 C. Diethylamine. Di-isopropylamine. Triethylamine 4. Di-n-propylamine. Di-n-butylamine 6. Tri-n-propylamine 7. Di-isobutylamine 8. Tri-n-butylamine 9. Di-isohexylamine 0. Dicyclohexylamine. Dibenzylamine. Tri-n-hexylamine 0. mm ID (0.4 mm OD) 0.40 µm film MN Appl. No. 080 Length 0 m m 0 m 0. mm ID (0.4 mm OD) 0. µm film mm ID (0.4 mm OD) 0.0 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 µm film min MN

30 Capillary columns for special separations FS-CW 0 M-AM polyethylene glycol 0 000, non-immobilised polyethylene glycol, basic for amine separations similar phases: Carbowax Amine, CP-Wax, CAM, Stabilwax DB USP G6 max. temperature for isothermal operation 0 C, max. temperature for short isotherms in a temperature programme 40 C Length 0 m m 0 m 0. 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 7. PERMABOND P-00 extra long column with nonpolar dimethylpolysiloxane phase high resolution and sufficient capacity for analysis of complex mixtures of hydrocarbons USP G / G / G8 0. mm ID (0.4 mm OD) Length for analyses of petrochemical products max. temperature for isothermal operation 00 C, max. temperature for short isotherms in a temperature programme 0 C 00 m 0.0 µm film MN

31 Capillary columns for special separations PERMABOND SE-4-HKW for volatile halogenated hydrocarbons SE-4 optimised for volatile halogenated hydrocarbons USP G6 max. temperature for isothermal operation 00 C, max. temperature for short isotherms in a temperature programme 0 C For the analysis of halogenated hydrocarbons we recommend our optimised columns PERMABOND SE- 4 HKW with or 0 m length with the well-known polysiloxane phase SE-4. As an alternative and for confirming analytical results, columns OPTIMA 64 show advantages especially for the determination of,,-trichlorotrifluoroethane (F ) besides dichloromethane. Both phases are also suited for determination of vinyl chloride and separation of cis/trans-,-dichloroethene. The high film thickness results in high capacity and outstanding resolution. For GC-MS coupling we recommend the phase OPTIMA 64 LB or OPTIMA 64 with 0. or 0. mm ID. Volatile halogenated hydrocarbons Column: PERMABOND SE-4-HKW, 0 m x 0. mm ID, max. temperature 00 C, Cat. No Injection volume: µl Carrier gas: 0.9 bar He Split: about :0 Temperature: C ( min) 60 C ( min), 0 C/min Detector: ECD 00 C Dichloromethane (79 ng/ml) 8. Chloroform (7 ng/ml).,,-trichloroethane (67 ng/ml) 4.,-Dichloroethane (00 ng/ml). Carbon tetrachloride (.9 ng/ml) 6. Trichloroethylene (4.6 ng/ml 7. Bromodichloromethane (0 ng/ml) 8. Dibromochloromethane ( ng/ml) 9. Tetrachloroethylene (8 ng/ml) 0. Bromoform (8.9 ng/ml) 6 0 MN Appl. No min Volatile halogenated hydrocarbons and BTX Column: OPTIMA 64, 0 m x 0. mm ID, max. temperature 60 C, Cat. No Injection volume: µl Carrier gas: 0.9 ml/min He (constant flow), split 0 ml/min Temperature: 40 C ( min) 60 C, 0 C/min Detector: MSD 97. Vinyl chloride. Trichlorofluoromethane (F ). Pentane 4.,,-Trichlorotrifluoroethane (F ). Dichloromethane 6. trans-,-dichloroethene 7. Hexane 8. cis-,-dichloroethene 9. Trichloromethane 0.,,-Trichloroethane. Tetrachloromethane.,-Dichloroethane + benzene. Trichloroethene 4. Bromodichloromethane. Toluene 6. Tetrachloroethene 7. Dibromochloromethane 8. Chlorobenzene 9. Ethylbenzene 0. m- + p-xylene. o-xylene. Tribromomethane. Bromobenzene MN Appl. No min Length m 0 m 0. mm ID (0. mm OD).80 µm film MN 7

32 Capillary columns for special separations OPTIMA -TG OPTIMA 7-TG OPTIMA -TG 00 % dimethylpolysiloxane offers separation according to carbon number similar phases: SPB- TG, DB- HT, 400- HT, HT- USP G / G / G8 for triglyceride analyses max. temperature for both phases: 70 C short capillary columns (max. m and 0. mm ID) with low-bleeding stationary phases thermally stable with optimum deactivation OPTIMA 7-TG phenyl-methyl-polysiloxane (0 % phenyl) for separation according to degree of unsaturation USP G Column: OPTIMA -TG, m x 0. mm ID, max. temperature 70 C, Cat. No. 76. Injection volume: 0. µl Carrier gas: 80 kpa H Temperature: Detector: FID 80 C, 6. Cholesterol. T-0. T-4 4. T-8. T-4 6. T T-0 8. T-4 80 C ( min) 0 C, 0 C/min 70 C (0 min), C/min Triglycerides (from butter) C MN Appl. No min Length 0 m m OPTIMA -TG 0. mm ID (0.4 mm OD) mm ID (0. mm OD) OPTIMA 7-TG 0. mm ID (0. mm OD) MN

33 Capillary columns for special separations PERMABOND Silane developed especially for the analysis of monomeric silanes and chlorosilanes (not for the separation of trimethylsilyl derivatives) also suited for the separation of dimeric siloxanes and silazanes for silane analyses for columns with 0. mm ID the max. temperature for isothermal operation is 60 C, the max. temperature for short isotherms in a temperature programme is 80 C; for 0. mm ID columns the max. temperatures are 40 and 60 C, resp. Length m 0 m 0. mm ID (0. mm OD) mm ID (0.8 mm OD) 74. Chloromethylsilanes Column: PERMABOND Silane, 0 m x 0. mm ID, max. temp. 60/80 C, Cat. No Injection volume: 0, µl gas Carrier gas: ml/min He (constant flow) Split: 80 ml/min Temperature: 0 C 00 C, C/min Detector: MSD 97. Tetramethylsilane. Dichloromethane. Tetrachlorosilane 4. Chlorotrimethylsilane. Methyltrichlorosilane 6. Dichlorodimethylsilane 7. Hexamethyldisiloxane min 7 MN Appl. No PERMABOND CW 0 M-DEG polyethylene glycol (diethylene glycol tested) USP G6 Diethylene glycol standard in wine Column: PERMABOND CW 0 M-DEG, m x 0. mm ID, max. temp. 0/40 C, Cat. No Injection volume: 0. µl Carrier gas:. bar N Split: ~ : 40 Temperature: 80 C 00 C, 0 C/min Detector: FID 60 C, 0 x DEG standard.,4-butanediol. Diethylene glycol. Glycerol MN Appl. No min for determination of diethylene glycol max. temperature for isothermal operation 0 C, max. temperature for short isotherms in a temperature programme 40 C recommended application: determination of diethylene glycol, e. g. for the quality control of wine Length m 0. mm ID (0.4 mm OD) 0. µm film mm ID (0. mm OD) 0. µm film 77. MN 9

34 Capillary columns for enantiomer separation LIPODEX cyclodextrin phases for enantiomer separation base material: cyclic oligosaccharides consisting of six (α-cyclodextrin), seven (β-cyclodextrin) or eight (γcyclodextrin) glucose units bonded through α-,4-linkages regioselective alkylation and/or acylation of the hydroxyl groups leads to lipophilic phases with varying enantioselectivity, which are well suited for GC enantiomer analyses important advantage: many compounds can be analysed without derivatisation (however, for certain substances enantioselectivity can be favourably influenced by formation of derivatives) A large number of separations have been achieved, however, it is not possible to make a general prediction, which phase could solve a given separation task. Even for compounds with small structural differences or within homologous series the enantiodifferentiation can be quite different. The descriptions below list some of the typical separations possible with individual phases. LIPODEX is patented under EP and US Re LIPODEX A recommended for carbohydrates, polyols, diols, hydroxycarboxylic acid esters, (epoxy-) alcohols, glycerol derivatives, spiroacetals, ketones, alkyl halides LIPODEX B recommended for lactones, diols (cyclic carbonates), aminols, aldols (O-TFA), glycerol derivatives (cyclic carbonates) LIPODEX C recommended for alcohols, cyanhydrins, olefins, hydroxycarboxylic acid esters, alkyl halides LIPODEX D recommended for amines (TFA), aminols (TFA), transcycloalkane-,-diols, trans-cycloalkane-,-diols (TFA), β-amino acid esters hexakis-(,,6-tri-o-pentyl)-α-cyclodextrin max. temperature for isothermal operation 00 C, max. temperature for short isotherms in a temperature programme 0 C hexakis-(,6-di-o-pentyl--o-acetyl)-α-cyclodextrin max. temperature for isothermal operation 00 C, max. temperature for short isotherms in a temperature programme 0 C heptakis-(,,6-tri-o-pentyl)-β-cyclodextrin max. temperature for isothermal operation 00 C, max. temperature for short isotherms in a temperature programme 0 C heptakis-(,6-di-o-pentyl--o-acetyl)-β-cyclodextrin max. temperature for isothermal operation 00 C, max. temperature for short isotherms in a temperature programme 0 C LIPODEX E recommended for α-amino acids, α- and β-hydroxycarboxylic acid esters, alcohols (TFA), diols (TFA), ketones, pheromones (cyclic acetals), amines, alkyl halides, lactones octakis-(,6-di-o-pentyl--o-butyryl)-γ-cyclodextrin max. temperature for isothermal operation 00 C, max. temperature for short isotherms in a temperature programme 0 C LIPODEX G recommended for menthol isomers, ketones, alcohols, carboxylic acid esters, terpenes octakis-(,-di-o-pentyl-6-o-methyl)-γ-cyclodextrin max. temperature for isothermal operation 0 C, max. temperature for short isotherms in a temperature programme 40 C 0 MN

35 Capillary columns for enantiomer separation Enantiomer separation of amino acid methyl esters (TFA) Column: FS-LIPODEX E, m x 0. mm ID, max. temp. 00/0 C, Cat. No Volume: µl Carrier gas: 60 kpa H Split: about :00 Temperature: C, 4 C/min Detector: FID, 0 C, AT (D is eluted before L except for proline: L before D). Alanine. Valine. Leucine 4. Proline. Aspartic acid 6. Phenylalanine min 4 6 MN Appl. No. 09 Separation of chiral constituents of peppermint oil W. A. König et al., High Resol. Chromatogr. 0 (997) 6 Column: FS-LIPODEX G, m x 0. mm ID, max. temp. 0/40 C, Cat. No Carrier gas: He Temperature: 7 C, isothermal Detector: FID. (+)-trans-sabinene hydrate. (+)-Menthone. (+)-Isomenthone 4. ( )-Menthone. ( )-Isomenthone 6. (+)-Menthofuran 7. ( )-Isopulegol 8. ( )-Menthyl acetate 9. (+)-Pulegone (+)-Neomenthol. ( )-Neomenthol. (+)-Neoisomenthol. (+)-Menthol 4. ( )-Neoisomenthol. (+)-Piperitone 6. ( )-Menthol 7. (+)-Isomenthol 8. ( )-Isomenthol MN Appl. No Mentha arvensis (China) Mentha piperita (Idaho) 8 Standard min Length 0 m m 0 m all columns 0.4 mm OD 0.0 mm ID 0. mm ID 0. mm ID FS-LIPODEX A FS-LIPODEX B FS-LIPODEX C FS-LIPODEX D FS-LIPODEX E FS-LIPODEX G MN

36 Capillary columns for enantiomer separation HYDRODEX cyclodextrin phases for enantiomer separation cyclodextrin derivatives with high melting point: for GC enantiomer separation diluted with polysiloxanes HYDRODEX β-pm heptakis-(,,6-tri-o-methyl)-β-cyclodextrin (CD) phase diluted with optimised polysiloxane recommended for hydroxycarboxylic acid esters, alcohols, diols, olefins, lactones, acetals max. temperature for isothermal operation 0 C, max. temperature for short isotherms in a temperature programme 0 C HYDRODEX β-p phase diluted with optimised polysiloxane recommended for terpenes, dienes, allenes, terpene alcohols,,-epoxyalkanes, carboxylic acids (esters), hydroxycarboxylic acid esters, pharmaceutics, pesticides HYDRODEX β-6tbdm phase diluted with optimised polysiloxane recommended for γ-lactones, cyclopentanones, terpenes, esters, tartrates Enantiomer separation of dichlorprop methyl ester Column: HYDRODEX β-p, m x 0. mm ID, max. temperature 0 C, Cat. No. 78. Injection volume: 0. µl (~% in CH Cl ) Carrier gas: 60 kpa H (.9 ml/min) Split: 0 ml/min Temperature: 60 C Detector: FID, 0 C, 7 Cl Cl O CH CO heptakis-(,6-di-o-methyl--o-pentyl)-β-cd max. temperature for isothermal operation 0 C, max. temperature for short isotherms in a temperature programme 0 C heptakis-(,-di-o-methyl-6-o-t-butyldimethyl-silyl)-β-cd max. temperature for isothermal operation 0 C, max. temperature for short isotherms in a temperature programme 0 C Separation of isomeric antiinflammatory drugs Courtesy of Prof. W.A. König, Hamburg, Germany Column: HYDRODEX β-6tbdm, m x 0. mm ID, max. temperature 0 C, Cat. No. 78. Carrier gas: He Temperature: C 00 C, C/min Detector: FID. Ibuprofen O 4. Naproxen. Flurbiprofen. Fenoprofen H C O F CH OH COOH O. Ketoprofen O O OH S R H C 4 O OH COOH 0 0 min min MN Appl. No. 04 MN Appl. No MN

37 Capillary columns for enantiomer separation HYDRODEX β-tbdac heptakis-(,-di-o-acetyl-6-o-t-butyldimethyl-silyl)-β-cd phase diluted with optimised polysiloxane recommended for alcohols, esters, ketones, aldehydes, δ-lactones etc. max. temperature for isothermal operation 0 C, max. temperature for short isotherms in a temperature programme 40 C HYDRODEX γ-tbdac phase diluted with optimised polysiloxane recommended for cyclic ketones, aromatic ketones, oxiranes, aromatic esters, aromatic amides etc. octakis-(,-di-o-acetyl-6-o-t-butyldimethyl-silyl)-γ-cd NEW! max. temperature for isothermal operation 0 C, max. temperature for short isotherms in a temperature programme 40 C Separation of (R/S) citronellol + citronellal Capillary column: FS-HYDRODEX β-tbdac, 0 m x 0. mm ID, max. temp. 0/40 C, Cat. No Carrier gas:. bar H, split ml/min Temperature: 00 C Injection: µl, :000 in CH Cl Detector: FID, 0 C. (R)/(S)-Citronellal. (S)/(R)-Citronellal. (S)-Citronellol 4. (R)-Citronellol OH O min 4 MN Appl. No. 440 Separation of essential oils Capillary column: FS-HYDRODEX γ-tbdac, 0 m x 0. mm ID, max. temp. 0/40 C, Cat. No Carrier gas:. bar H Temperature: C Injector: 0 C Detector: FID, 0 C. Fenchone (. mg/ml). Menthone (0. mg/ml). Menthol ( mg/ml) min MN Appl. No. 980 / 990 / 000 Length 0 m m 0 m all columns 0.4 mm OD 0.0 mm ID 0. mm ID 0. mm ID FS-HYDRODEX β-pm FS-HYDRODEX β-p FS-HYDRODEX β-6tbdm FS-HYDRODEX β-tbdac FS-HYDRODEX γ-tbdac MN

38 Capillary columns for enantiomer separation PERMABOND L-CHIRASIL-VAL (N--methylpropionyl-L-valine-t-butylamide)- methylpolysiloxane immobilised diamide type chiral stationary phase max. temperature 90 C Enantiomer separation of N-pentafluoropropionyl amino acid n-propyl esters Column: PERMABOND L-CHIRASIL-VAL, m x 0. mm ID, max. temperature 90 C, Cat. No Injection volume: 0. µl Carrier gas: 0.4 bar H, split : 0 Temperature: 80 C (4 min) 8 C (4 min), C/min 60 C, 4 C/min 90 C (7 min), C/min Detector: FID 0 C, AT Peaks (N-pentafluoropropionyl n-propyl esters):. D-Alanine. L-Serine + D-leucine. L-Alanine. L-Leucine. D-Threonine 4. D-Proline 4. D-Valine. L-Proline. L-Threonine 6. BHT 6. L-Valine 7. D-Cysteine 7. Glycine 8. L-Cysteine 8. D-allo-Isoleucine 9. D-Aspartic acid 9. D-Isoleucine + L-allo-isoleucine 0. L-Aspartic acid 0. L-Isoleucine. D-Methionine. D-Serine. L-Methionine D-Phenylalanine 4. L-Phenylalanine. D-Glutamic acid 6. L-Glutamic acid 7. D-Tyrosine 8. L-Tyrosine 9. D-Ornithine 0. L-Ornithine. D-Lysine. L-Lysine min Courtesy of Priv. Doz. Dr. W. Brückner, Dipl. Lebensmittel-Chemiker M. Hausch, Inst. f. Lebensmitteltechnologie, Universität Hohenheim, Stuttgart, Germany MN Appl. No Length m 0 m 0. mm ID (0.4 mm OD) mm ID (0. mm OD) Test mixtures for chiral GC capillary columns Test mixture for test compound (enantiomer mixture) pack of Cat. No. LIPODEX A, HYDRODEX β-pm, β-p, β-6tbdm, phenylethanol ml 7 β-tbdac, γ-tbdac LIPODEX B methylbutyrolactone ml 7 LIPODEX C, D phenylethylamine (TFA) ml 7 LIPODEX E, G phenylethanol (TFA) ml 79 PERMABOND L-CHIRASIL-VAL amino acids (TFA)-(Iprop) ml MN

39 Fused silica capillaries Untreated capillaries recommended applications: for capillary electrophoresis for preparation of capillary columns for capillary LC applications Length m (pack of ) 0 m (pack of ) Capillaries for electrophoresis 0.0 mm ID (0.4 mm OD) mm ID (0.4 mm OD) mm ID (0. mm OD) m (pack of ) 0.0 mm ID (0.4 mm OD) Untreated capillaries 0.0 mm ID (0.4 mm OD) mm ID (0.4 mm OD) mm ID (0. mm OD) mm ID (0.8 mm OD) Untreated capillaries are supplied without cage. For empty cages please see page 4. Deactivated capillary columns (precolumns) recommended applications: for preparation of capillary columns as precolumns, whenever a larger contamination capacity is required. Length 0 m m Methyl-Sil deactivated (max. temperature 0 C) 0. mm ID (0.4 mm OD) mm ID (0. mm OD) mm ID (0.8 mm OD) Phenyl-Sil deactivated (max. temperature 0 C) 0. mm ID (0.4 mm OD) mm ID (0. mm OD) mm ID (0.8 mm OD) CW deactivated (max. temperature 0 C) 0. mm ID (0.4 mm OD) mm ID (0. mm OD) mm ID (0.8 mm OD) Deactivated capillaries are supplied without cage. For empty cages please see page 4. MN

40 Fused silica capillaries Retention gaps The retention gap technique in combination with on-column injection allows concentration of a large sample volume in the capillary column. choice of the retention gap depends on the solvent used: the flooded zone after injection should be between 0 0 cm/µl Me-Sil retention gap: only for use with n-hexane and diethyl ether Phe-Sil retention gap: for all solvents except methanol and water CW retention gap: for all solvents and especially for methanol and water calculation example: length of flooded zone ~ 0 0 cm/µl, retention gap 0 m x 0. mm ID, capillary column: m x 0. mm ID, max. injection volume ~ 0 0 μl A retention gap must be inert without any noticeable retention Me-Sil retention gaps are more inert than Phe-Sil, while Phe-Sil is less susceptible to contamination max. temperatures: for CW retention gaps 0 C, for Me-Sil and Phe-Sil retention gaps 0 C Retention gaps can also be used as transfer lines or precolumns (contamination capacity about 0 µg). Length 0 m m Me-Sil retention gaps (max temperature 0 C) 0. mm ID (0.4 mm OD) mm ID (0. mm OD) mm ID (0.8 mm OD) Phe-Sil retention gaps (max temperature 0 C) 0. mm ID (0.4 mm OD) mm ID (0. mm OD) mm ID (0.8 mm OD) CW retention gaps (max. temperature 0 C) 0. mm ID (0.4 mm OD) mm ID (0. mm OD) mm ID (0.8 mm OD) Retention gaps are supplied without cage. For empty cages please see page 4. Fused silica capillary columns not chemically bonded Length m 0 m Capillary columns FS-OV- 00% dimethylpolysiloxane (max. temperature 00 C) 0. mm ID (0. mm OD) 0. µm film µm film Capillary columns FS-SE-4 % diphenyl % vinylmethyl 94% dimethylpolysiloxane (max. temperature 00 C) 0. mm ID (0.4 mm OD) 0. µm film MN

41 Reagents and procedures for derivatisation Derivatisation reagents for improved volatility, better thermal stability or a lower limit of detection in gas chromatography prerequisite: quantitative, rapid and reproducible formation of only one derivative halogen atoms introduced by derivatisation (e. g. trifluoroacetates) allow specific detection (ECD) with the advantage of high sensitivity elution orders and fragmentation patterns in MS can be influenced by a specific derivatisation reagents for silylation, acylation, and alkylation (methylation) available Derivatisation method development kits Designation Contents of the kit Cat. No. Derivatisation method development kit which type of derivatisation is best suited for your sample (alkylation, acylation or silylation)? x ml each of TMSH, MSTFA, MBTFA 709 Acylation kit which is the proper reagent for acylation? x ml each of MBTFA, TFAA, MBHFBA 7090 Alkylation kit which is the proper reagent for methylation? x ml each of TMSH, DMF-DMA 709 Silylation kit which is the proper reagent for silylation? x ml each of MSTFA, BSTFA, TSIM, MSHFBA 709 Selection guide for derivatisation of important functional groups in GC Function method derivative recommended reagents Alcohols, silylation RʼO TMS BSA, MSTFA, MSHFBA, TSIM, SILYL-0, SILYL-, SILYL-9 Phenols acylation RʼO CO R TFAA, HFBA, MBTFA, MBHFBA RʼOH alkylation RʼO R TMSH sterically hindered silylation RʼO TMS TSIM, BSTFA, SILYL-99 Amines silylation Rʼ NRʼʼ TMS BSA, MSTFA, MSHFBA, SILYL-99 primary, secondary acylation Rʼ NRʼʼ CO R TFAA, HFBA, MBTFA, MBHFBA hydrochlorides silylation Rʼ NRʼʼ TMS MSTFA Amides silylation not stable acylation Rʼ CO NH CO R TFAA, MBTFA, HFBA, MBHFBA Amino acids silylation Rʼ CH(NH TMS) CO O TMS BSA, BSTFA, MSTFA, MSHFBA alkylation (a) + acylation (b) Rʼ CH(NH - CO-R) CO O R a) MeOH/TMCS, TMSH b) TFAA, HFBA, MBTFA, MBHFBA Carboxylic acids (fatty acids) silylation Rʼ CO O TMS susceptible to hydrolysis BSA, MSTFA, MSHFBA, TMCS, TSIM, SILYL- 0, SILYL-, Silyl 9 alkylation Rʼ CO O R DMF-DMA, MeOH/TMCS ( M), TMSH salts silylation Rʼ CO O TMS TMCS susceptible to hydrolysis Carbohydrates silylation MSTFA, TSIM, HMDS, SILYL-9 acylation TFAA, MBTFA Steroids silylation BSA, TSIM acylation TFAA, MBTFA, HFBA, MBHFBA Reagents for GC MN 7

42 Reagents and procedures for acylation Acylation reagents Acyl halides by-product of acylation with acyl halides: corresponding hydrohalic acids excess of reagent and acid have to be removed or trapped by a suitable base (e. g. pyridine) Pentafluorobenzoyl chloride PFBC: C 6 F CO Cl m.w. 0., Bp 8 9 C (760 mm Hg), density d0 /4 =.60 Anhydrides by-products of acylation with anhydrides: corresponding acids excess reagent and the acid formed have to be removed Trifluoroacetic acid anhydride m.w. 0.04, Bp C (760 mm Hg), TFAA: CF CO O CO CF density d0 /4 =.490 Heptafluorobutyric acid anhydride m.w , Bp C (760 mm Hg), HFBA: C F 7 CO O CO C F 7 density d0 /4 =.66 Reagents for GC Bisacylamides by-products: corresponding neutral acylamides, which can be easily removed due to their high volatility; because of neutral conditions and favourable chromatographic properties often removal of the bisacylamide is not necessary. Thus sample preparation is much more convenient. N-methyl-bis(trifluoroacetamide) m.w..08, Bp 4 C (760 mm Hg), MBTFA: CF CO N( ) CO CF density d0 /4 =. N-methyl-bis(heptafluorobutyramide) m.w. 4., Bp 6 66 C (760 mm Hg), MBHFBA: C F 7 CO N( ) CO C F 7 density d0 /4 =.67 Methods for acylation Acylation with fluorinated acid anhydrides: Acylation with TFAA or HFBA can be used for alcohols, phenols, carboxylic acids, amines, amino acids and steroids forming volatile, stable derivatives suited for FID as well as for ECD detection. Procedure: Dissolve 0. to mg of the sample in 0. ml solvent, add 0. ml of the respective anhydride and heat to C for hours. If the sample need not be concentrated prior to the analysis and if there is no danger of catalytically induced side reactions, pyridine is used as solvent. The reaction solution can be injected directly into the gas chromatograph. Otherwise use a volatile solvent and evaporate solvent, excess reagent and acid in a stream of nitrogen. Dissolve the residue in 0 µl hexane, chloroform etc. and inject aliquot portions. MN Appl. No. 040 Acylation with fluorinated acid amides: This method is recommended for alcohols, primary and secondary amines as well as for thiols under mild, neutral conditions. MBTFA also forms very volatile derivatives with carbohydrates [J. Sullivan and L. Schewe, J. Chromatogr. Sci. (977) 96 97]. Procedure: Add 0. ml MBTFA or MBHFBA to about mg sample. If there is no reaction at ambient temperature, heat the reaction mixture to 0 C. Compounds which are difficult to dissolve, can be trifluoroacetylated in suitable solvent mixtures. It is recommended to use a ratio of solvent to MBTFA or MBHFBA of 4 :. The reaction mixture can be chromatographed directly. MN Appl. No. 00 Packing unit Code 0 x ml 0 x ml x 0 ml x 0 ml HFBA MBTFA MBHFBA PFBC TFAA Due to their purpose, derivatisation reagents are very reactive substances. For this reason they should be stored cool and protected from moisture. Our derivatisation reagents are supplied in vials with crimp caps for easy access with a syringe. Vials with pierced sealing disks have limited stability and should be used soon. 8 MN

43 Reagents and procedures for methylation Alkylation reagents Except for some special cases (e. g. enantiomer separation of amino acids with PERMABOND L-CHIRASIL-VAL) in GC generally methylation is the only type of alkylation used. Methylation reagents N,N-dimethylformamide dimethylacetal DMF-DMA m.w. 9.7 Bp C (760 mm Hg), density d0 /4 = Trimethylsulphonium hydroxide TMSH (0. M in methanol) m.w H C H C S + OH H C N H C O O Methods for methylation Methylation with TMSH Methylation with TMSH [W. Butte, J. Chromatogr. 6 (98) 4] is recommended for free acids, chlorophenoxycarboxylic acids, their salts and derivatives as well as for phenols and chlorophenols. One great advantage is simplification of the sample preparation. Lipids or triglycerides can be converted to the corresponding fatty acid methyl esters (FAMEs) by a simple transesterification. Isomerisations of multiple unsaturated fatty acids have not been observed. This reaction is very elegant and convenient, because it is just necessary to add the reagent (0. M in methanol) to the sample solution. Removal of excess reagent is not required, since in the injector of the gas chromatograph at 0 C pyrolysis to volatile methanol and dimethylsulfide will occur. Due to the high reactivity, complete derivatisation is often obtained at ambient temperature. However, heating (e. g. 0 min at 00 C) in a closed sample vial may be necessary. Procedure: Dissolve 00 mg sample (e. g. butter) in ml of a suitable solvent (e. g. tert.-butyl methyl ether). Add 0 µl reagent to 00 µl of this solution. The mixture is injected directly. The temperature of the injector must be at least 0 C. MN Appl. No. 060 Methylation with DMF-DMA Methylation with DMF-DMA can be applied for fatty acids, primary amines and (partially) amino acids forming N-dimethyl-aminomethylene amino acid methyl esters [Thenot et al., Anal. Letters (97) 7, 9 9]. DMF- DMA is a poor solvent, for this reason it is necessary to use a mixture of DMF-DMA with pyridine, THF, acetone (barbiturates) or another solvent. Procedure: Add ml of a mixture of DMF-DMA and pyridine (:) to 0 mg fatty acids. As soon as a clear solution has formed, the sample can be injected. However, it is recommended to heat the solution to C for 0 minutes. MN Appl. No. 070 Methylation with methanol/tmcs A molar solution of TMCS in methanol is suited for the esterification of free carboxylic acids and transesterification of glycerides. Formation of HCl catalyses the reaction. TMCS and silyl ether remove water and thus drive the reaction to completion. The mixture should be prepared fresh. Procedure: Add ml methanol/tmcs to about 0 mg carboxylic acid or glyceride and heat. Then evaporate in a stream of nitrogen and dissolve again for injection in e. g. n-heptane. MN Appl. No. 080 Reagents for GC For GC separation of FAMEs from natural butter fat after derivatisation with TMSH see Appl at Packing unit Code 0 x ml 0 x ml x 0 ml x 0 ml DMF-DMA TMSH MN 9

44 Reagents and procedures for silylation Silylation reagents Usually the term silylation in GC stands for replacement of active hydrogen atoms by a trimethylsilyl group (TMS derivative). Sometimes, however, trialkylsilyl groups or dimethylalkylsilyl groups with longer alkyl chains are used for derivatisation. The trialkylsilyl group increases volatility and enhances thermal stability of the sample. Silylation can be catalysed either acidic by addition of TMCS or basic by addition of pyridine or TSIM (e. g. for sterically hindered functionalities like tert. alcohols). Reactivity of silylation reagents (acc. to M. Donike): TMS amides (e. g. BSA, MSTFA) > TMS amine = TSIM > Enol-O-TMS ether > S-TMS ether > O-TMS ether > TMS-O-TMS Stability of the TMS derivatives: O-TMS ether > S-TMS ether > Enol-O-TMS ether > TMS amine > TMS amide Reagents for GC BSA BSTFA SILYL-99 O Si( ) R C N,O-bis-trimethylsilyl-acetamide m.w. 0.4, Bp 7 7 C ( mm Hg), density d0 /4 = 0.8 BSA: R = N Si( ) strong silylation reagent, which forms very stable TMS derivatives of a wide variety of compounds, e. g. alcohols, amines, carboxylic acids, phenols, steroids, biogenic amines and alkaloids not recommended for use with carbohydrates or very low molecular weight compounds good solvent for polar compounds, but frequently used in combination with a solvent (pyridine, DMF etc.) or with other silylation reagents. When used with DMF, BSA is the reagent of choice for derivatising phenols. N,O-bis-trimethylsilyl-trifluoroacetamide BSTFA: R = CF m.w. 7.4, Bp 40 C ( mm Hg), density d0 /4 = 0.96 powerful trimethylsilyl donor with approximately the same donor strength as the nonfluorinated analog BSA advantage of BSTFA over BSA: greater volatility of its reaction products (particularly useful for GC of some lower boiling TMS amino acids. BSTFA is nonpolar (less polar than MSTFA), and can be mixed with acetonitrile for improved solubility. For silylating fatty acid amides, hindered hydroxyls and other compounds, which are difficult to silylate (like secondary alcohols and amines), we recommend BSTFA + % trimethylchlorosilane (TMCS), available under the designation SILYL-99. Silylation with BSA, BSTFA or SILYL-99 (BSTFA + % TMCS) Silylation with BSA in combination with other silylation reagents Procedure: add 0. ml of the silylation reagent to 0 mg sample; if necessary, add some solvent (normally pyridine or DMF [dimethylformamide] are used). Heat to C for 0 min to increase the reaction rate. drops of TMCS (trimethylchlorosilane) or TSIM will also speed up the reaction. MN Appl. No. 090 Procedure: BSA alone silylates all sterically unhindered hydroxyl groups of the steroid skeleton; addition of TMCS will enable reaction of moderately hindered OH groups (reaction time 6 hours at 60 C). After addition of TSIM even strongly hindered hydroxyl groups will react (reaction time 6 4 hours at 60 C). MN Appl. No. 00 Packing unit 0 x ml x 0 ml x 0 ml x 0 ml x 00 ml BSA BSTFA SILYL-99 (BSTFA TMCS (99:) Due to their purpose, derivatisation reagents are very reactive substances. For this reason they should be stored cool and protected from moisture. Our derivatisation reagents are supplied in vials with crimp caps for easy access with a syringe. Vials with pierced sealing disks have limited stability and should be used soon MN

45 Reagents and procedures for silylation MSTFA MSHFBA MBDSTFA N-methyl-N-trimethylsilyl-trifluoroacetamide m.w. 99., Bp 70 C (7 mm Hg), density d0 /4 =. the most volatile trimethylsilyl amide available R CO N MSTFA: Rʼ = CF, Rʼʼ = Si ( ) R very strong TMS donor which does not cause any noticeable FID fouling even after long-time measuring series The already good solution characteristics can be improved by addition of submolar quantities of protic solvents (e. g. TFA for extremely polar compounds such as hydrochlorides) or pyridine (e. g. for carbohydrates). recommended application: carboxylic acids, hydroxy and ketocarboxylic acids, amino acids, amines, alcohols, polyalcohols, sugars, mercaptans and similar compounds with active hydrogen atoms. Even amine hydrochlorides can be silylated directly. advantages: complete reaction with high reaction rates, even without a catalyst ( % TMCS or TSIM) the by-product of the reaction (N-methyltrifluoroacetamide) features high volatility and short retention time N-methyl-N-trimethylsilyl-heptafluorobutyramide MSHFBA: Rʼ = C F 7, Rʼʼ = m.w. 99., Bp 48 C (760 mm Hg) similar to MSTFA in reactivity and chromatography recommended application: carboxylic acids, alcohols, phenols, primary and secondary amines and amino acids used either alone or in combination with a catalyst (TMCS, TSIM) or another silylation reagent with or without solvent the by-product N-methylheptafluorobutyric amide has a lower retention time than the silylating reagent especially useful for flame ionisation detection due to the large ratio of fluorine to silicon of 7 :, since degradation of the excess of MSHFBA does not produce SiO but volatile, non-corrosive silicon compounds N-methyl-N-tert-butyldimethylsilyl-trifluoroacetamide MBDSTFA: Rʼ = CF, Rʼʼ = C 4 H 9 m.w. 4., Bp C (760 mm Hg), density d0 /4 =. silylation reagent which donates a tert-butyldimethylsilyl group (TBDMS) for derivatising active hydrogen atoms in hydroxyl, carboxyl and thiol groups as well as primary and secondary amines fast reactions (typically 0 min) with high yields (> 96%) by-products are neutral and volatile TBDMS ethers are 0 4 times more stable than the corresponding TMS ethers chromatographic retention times are longer due to the large protecting group, which may improve some separations; because of the high molecular ion concentration at M + -7 useful for GC-MS applications Reagents for GC Silylation with MSTFA, MSHFBA or MBDSTFA Procedure: Dissolve 0 mg sample in 0.8 ml solvent, then add 0. ml of the silylation reagent. The reaction mixture can be heated to C for up to hour and can be analysed directly. If TFA is used as a solvent, proceed as follows [M. Donike, J. Chromatogr. 8 (97) 7]: dissolve mg sample in 00 µl TFA. Dropwise add 0.9 ml of the silylating reagent. After cooling the sample can be chromatographed directly. MN Appl. No. 0 Packing unit 0 x ml 0 x ml x 0 ml x 0 ml x 00 ml 6 x 0 ml 6 x 00 ml x 00 ml MSHFBA MSTFA MBDSTFA MN 4

46 Reagents and procedures for silylation DMCS HMDS TMCS TSIM Dimethyldichlorosilane m.w. 9.06, Bp 70 C (760 mm Hg), density d0 /4 =.07 DMCS: ( ) SiCl used to form dimethylsilyl (DMS) derivatives DMS derivatives are much more susceptible to hydrolysis than TMS derivatives, therefore strictly anhydrous conditions during reaction are very important. Hexamethyldisilazane HMDS: ( ) Si NH Si( ) m.w. 6.4, Bp 6 C (760 mm Hg), density d0 /4 = weak TMS donor; used alone reaction is slow and not very effective after addition of catalytic quantities of TMCS (e. g. %) or as a mixture with TMCS (:, v/v; SILYL- and SILYL-0) a fast and quantitative reagent for trimethylsilylation of organic compounds Aprotic solvents like acetonitrile, pyridine, dimethylformamide, carbon disulphide and dimethylacetamide are recommended for use with HMDS. Reagents for GC Trimethylchlorosilane TMCS: ( ) SiCl m.w. 08.7, Bp 7 C (760 mm Hg), density d0 /4 = often used as a catalyst with other trimethylsilyl reagents Without additives it can be used for preparing TMS derivatives of organic acids. N-Trimethylsilyl-imidazole m.w. 40., Bp C (760 mm Hg), density d0 /4 = 0.96 TSIM: Si N N strongest hydroxyl silylator; reagent of choice for carbohydrates and most steroids (even highly hindered steroids) The reagent is unique in that it reacts quickly and smooth with hydroxyl (even tert. OH) and carboxyl groups, but not with amines. This characteristic makes TSIM particularly useful in multi-derivatisation schemes for compounds with different functional groups, which are to be derivatised differently (e. g. -O- TMS / -N-HFB derivatives of catecholamines). recommended application: alcohols, phenols, organic acids, steroids, hormones, glycols, nucleotides, narcotics Silylation with TSIM or SILYL-9 (TSIM pyridine :9) Procedure: Dissolve 0 mg sample in 0.8 ml solvent, then add 0. ml of the silylation reagent. The reaction mixture can be heated to C for up to hour and can be analysed directly. recommended solvent pyridine When using SILYL-9, the presence of water does not interfere. MN Appl. No. 0 Packing unit of 0 x ml x 0 ml x 0 ml 6 x 0 ml DMCS * HMDS * TMCS * * TSIM * in vials with screw caps 4 MN

47 Reagents and procedures for silylation Reagent mixtures for silylation Code 0 x ml x 0 ml x 0 ml x 0 ml x 00 ml SILYL-7 BSA - HMDS - TSIM (:7:) SILYL-9 TSIM - pyridine (:9) SILYL- HMDS - TMCS (:) SILYL-0 HMDS - TMCS - pyridine (::0) SILYL-99 BSTFA - TMCS (99 : ) Due to their purpose, derivatisation reagents are very reactive substances. For this reason they should be stored cool and protected from moisture. Our derivatisation reagents are supplied in vials with crimp caps for easy access with a syringe. Vials with pierced sealing disks have limited stability and should be used soon. Silylation with SILYL- or SILYL-0 Procedure: Carefully add SILYL- or SILYL-0 to 0 mg of the sample. A precipitate of ammonium chloride does not interfere. If the sample should not dissolve within minutes, heat to 7 8 C. If no mutarotation is to be expected, you may dissolve the sugar in warm pyridine first and then add the silylation reagent. In some cases it may be advantageous to use a different solvent instead of pyridine. For derivatisation of -ketosteroids we recommend to use DMF (dimethylformamide). MN Appl. No. 0 suitable for sugars, glycols, sterically unhindered alcohols, carboxylic acids, acids in urine, hydroxy fatty acids, nucleotides, steroids, vitamin D, xanthone derivatives O-Trimethylsilylation with MSTFA followed by N-trifluoroacetylation with MBTFA Procedure: Completely silylate mg of the sample with 0. ml MSTFA e. g. as described on page 4. After addition of 0. ml MBTFA the N-trimethylsilyl group is replaced by the N-trifluoroacetyl group. The mixture can be analysed directly. MN Appl. No. 40 Reagents for GC MN 4

48 Test mixtures for GC capillary columns Test mixtures for GC Test mixtures for GC capillary columns are used for controlling the performance of fused silica capillary columns and the GC system Test mixtures for chiral GC columns see page 4 Designation Pack of Composition Cat. No. Polarity mixture POL (qualitative) in n-pentane ml -butanol, benzene, methyl butyrate, toluene, cyclopentanone, -octene, dibutyl ether 706 Reagents for GC Activity test mixture (FA-TMS test according to Donike) in MSTFA/nhexane ( + 4) Grob test mixture (modified) in n-hexane MN OPTIMA test mixture in pentane MN OPTIMA amine test mixture in ethanol FAME test mixture in hexane ml mg/ml each of TMS capric acid (C 0 ), TMS myristic acid (C 4 ), TMS stearic acid (C 8 ), TMS behenic acid (C ), hexadecane (C 6 ), eicosane (C 0 ), tetracosane (C 4 ), octacosane (C 8 ) ml (in mg/ml) n-decane (~.8), n-undecane (~.9), n-octanol (~.6),,6-dimethylphenol (~.),,6-dimethylaniline (~.), methyl decanoate (~ 4.), dicyclohexylamine (~.), methyl undecanoate (~ 4.), methyl dodecanoate (~ 4.) ml 0. % each of undecane, dodecane, octanol, dimethylaniline, decylamine, methyl decanoate, methyl undecanoate, henicosane, docosane, tricosane (chromatograms see page 00) ml 0. % diisobutylamine, % diethanolamine, 0. %,6-dimethylaniline, 0. % o-propanol-pyridine, 0. % dicyclohexylamine, 0. % dibenzylamine ml 0. % each of FAMEs C4, C6, C8, C0, C, C4, C6, C8, C8: cis, C8: trans, C8:, C8:, C0, C, C:, C4 (chromatogram see page 0) MN

49 Test mixtures for GC capillary columns Separation of the OPTIMA Amine test mixture (Cat. No. 77) Column: OPTIMA Amine,.0 µm film, 0 m x 0. mm ID, max. temp. 00/0 C, Cat. No Injection volume: µl Carrier gas: 0.6 bar H Split: :0 Temperature: 00 C 90 C, 0 C/min Detector: FID, 80 C, 6. Diisobutylamine. Diethanolamine.,6-Dimethylaniline 4. o-propanol-pyridine. Dicyclohexylamine 6. Dibenzylamine Polarity mixture POL (qualitative) (Cat. No. 706) Column: OPTIMA Wax, 0. µm film, m x 0. mm ID, max. temp. 0/60 C, Cat. No Injection: µl, split : 0, 0 C Carrier gas: 0.7 bar N Temperature: 80 C isothermal Detector: FID, 0 C, 0, 7. n-pentane. n-octene-() 6. Dibutyl ether 4. Benzene. Methyl butyrate 6. Toluene 7. n-butanol 8. Cyclopentanone min MN Appl. No. 000 Activity test mixture (Cat. No. 707) Column: OPTIMA,.0 µm film, m x 0. mm ID, max. temp. 40/60 C, Cat. No Injection: µl, split : 40, 00 C Carrier gas: 0.6 bar H Temperature: 0 C 00 C (8 min), 0 C/min Detector: FID, 00 C, 0,. TMS capric acid (C 0 ). Hexadecane (C 6 ). TMS myristic acid (C 4 ) 4. Eicosane (C 0 ). TMS stearic acid (C 8 ) 6. Tetracosane (C 4 ) 7. TMS behenic acid (C ) 8. Octacosane (C 8 ) min 8 8 MN Appl. No. 0 Grob test mixture (modified) (Cat. No. 70) Column: OPTIMA,.0 µm film, 0 m x 0. mm ID, max. temp. 40/60 C, Cat. No Injection: µl, split : 40, 80 C Carrier gas:. bar H Temperature: 80 C 80 C (0 min), 8 C/min Detector: FID, 80 C, 0, 6. n-decane. -Octanol. n-undecane 4.,6-Dimethylphenol.,6-Dimethylaniline 6. Methyl decanoate 7. Methyl undecanoate 8. Dicyclohexylamine 9. Methyl dodecanoate Reagents for GC min MN Appl. No min MN Appl. No. 0 MN 4

50 Test mixtures for environmental analyses Reagents for GC Designation Pack of Composition Cat. No. Haloform test mixture in n-pentane (qualitative) Haloform test mixture in methanol for headspace analyses (qualitative) Haloform test kit (qualitative) Pesticide test mixture in n-hexane (qualitative) PAH test mixture acc. to EPA in toluene PAH test mixture acc. to German drinking water specifications in toluene BTX test mixture in methanol ml 9 halogenated hydrocarbons acc. to German drinking water specifications (in ng/ml): dichloromethane (79), chloroform (7),,,-trichloroethane (67), carbon tetrachloride (80), trichloroethylene (7), bromodichloromethane (00), dibromochloromethane (), tetrachloroethylene (8), bromoform (4) ml 9 halogenated hydrocarbons in increased concentration for calibration acc. to German Industrial Standard DIN 8407, part (in µg/ml): dichloromethane (8.4), chloroform (4.9),,,-trichloroethane (.4), carbon tetrachloride (.9), trichloroethylene (4.6), bromodichloromethane (0), dibromochloromethane (4.), tetrachloroethylene (6.), bromoform (8.9) x ml ml each of 9 single undiluted halogenated hydrocarbons and ml each of test mixtures Cat. Nos. 7 and 77 ml 0 µg/ml each of α-bhc, HCB, β-bhc, γ-bhc, δ-bhc, heptachlor, aldrin, dieldrin, endrin, p,pʼ-ddt, mirex ml 0 µg/ml each of naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, indeno[,,-cd]pyrene, dibenz[a,h]anthracene, benzo[ghi]perylene ml 0 µg/ml each of fluoranthene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, indeno[,,-cd]pyrene, benzo[ghi]perylene ml 0 ng/µl each of benzene, ethylbenzene, toluene, m-, o-, p-xylene 77 PAH test mixture acc. to EPA for GC (Cat. No. 74) Column: soptima, 0. µm film, 0 m x 0. mm ID, max. temperature 40/60 C, Cat. No Sample: PAH test mixture according to EPA (0 µg/ml each in toluene) Injection volume:.0 µl Carrier gas: H, 70 KPa Split: : Temperature: 00 C, 7 C/min 00 C Detector: FID, 00 C, Naphthalene 8. Acenaphthylene. Acenaphthene 4. Fluorene. Phenanthrene 6. Anthracene 9 7. Fluoranthene 0 8. Pyrene 9. Benz[a]anthracene 0. Chrysene. Benzo[b]fluoranthene. Benzo[k]fluoranthene. Benzo[a]pyrene 4. Indeno[,,-cd]pyrene. Dibenz[ah]anthracene 6. Benzo[ghi]perylene 4 6 MN Appl. No min 46 MN

51 Test mixtures for environmental analyses PAH test mixture acc. to German drinking water specifications (Cat. No. 7) Column: OPTIMA, 0. µm film, m x 0. mm ID, max. temp. 40/60 C, Cat. No Injection volume: µl Carrier gas: 0.6 bar H, split : 0 Temperature: 80 C 80 C 00 C, 4 C/min Detector: FID 00 C, 4. Fluoranthene. Benzo[b]fluoranthene. Benzo[k]fluoranthene 4. Benzo[a]pyrene. Indeno[,,-cd]pyrene 6. Benzo[ghi]perylene Haloform test mixture (Cat. No. 7) Column: FS-SE-4, 0. µm film, 0 m x 0. mm ID, max. temperature 00 C, Cat. No Injection volume: µl Carrier gas: bar N Split: about : 0 Temperature: 4 C (0 min) 0 C, 8 C/min Detector: ECD 60 C, 8. Dichloromethane. Chloroform.,,-Trichloroethane 4. Carbon tetrachloride. Trichloroethylene 6. Bromodichloromethane 7. Dibromochloromethane 8. Tetrachloroethylene 9. Bromoform min MN Appl. No Pesticide test mixture (Cat. No. 7) Column: OPTIMA, 0. µm film, m x 0. mm ID, max. temp. 40/60 C, Cat. No Injection volume: 0. µl (test mixture diluted to µg/ml per component) in n-hexane Carrier gas: 00 kpa H Split: 0 ml/min Temperature: Detector: ECD 00 C, 0. α-bhc. HCB. β-bhc 4. γ-bhc. δ-bhc 6. Heptachlor 7. Aldrin 8. Dieldrin 9. Endrin 0. p,p -DDT. Mirex 00 C 70 C, 8 C/min min MN Appl. No. 90 BTX test mixture (Cat. No. 77) Column: HYDRODEX β-pm, 0 m x 0. mm ID, max. temperature 0 C, Cat. No Injection volume: µl (0 ng/µl each in methanol) Carrier gas: 0 kpa H (.4 ml/min) Split: 40 ml/min Temperature: 60 C 00 C, C/min Detector: FID 0 C, 4 M = Methanol M. Benzene. Toluene. p-xylene 4. m-xylene. Ethylbenzene 6. o-xylene 4 6 Reagents for GC min MN Appl. No min MN Appl. No. 0 MN 47

52 Accessories for capillary columns Ferrules for GC Graphite ferrules provide the highest temperature stability (up to 40 C). They are reusable when handled with care. We also offer /6" graphite ferrules specially designed for Carlo Erba / Fisons or for Agilent gas chromatographs. Vespel ferrules come in three types: pure Vespel, Vespel with % graphite and Vespel with 40 % graphite. All versions are stable up to 400 C and reusable. Teflon ferrules can only be used up to 0 C. They are not reusable and not recommended for temperature programming. However, they show the best chemical inertness of all ferrules. (packing unit 0 ferrules) Accessories for GC Bore (= column OD) Graphite Vespel Teflon plain + % graphite + 40 % graphite max. temp. 40 C 400 C 400 C 400 C 0 C /6" ferrules no bore mm mm mm mm mm 7080 /6" /6" ferrules for Carlo Erba / Fisons instruments 0.4 mm mm mm /6" ferrules for Hewlett-Packard / Agilent instruments 0.4 mm mm mm 708 /8" ferrules no bore mm mm mm /6" /8" /4" ferrules no bore mm mm /6" /8" mm /4" mm ferrules no bore mm 7069 If you are in doubt about the correct size / Cat. No. please send us an old, used ferrule for the right selection MN

53 Accessories for capillary columns Connectors for capillary GC columns Graphseal connecting system for capillaries based on the Graphseal ferrule: a stainless steel ferrule filled with graphite the ideal sealing material for capillaries The capillary is mounted on a /6" exit (detector, injector etc.) with the appropriate ferrule, a Graphseal nut (with slit) and an adaptor (see table below). Glass connectors for fused silica capillary columns from 0. to 0. mm ID manufactured from deactivated glass with slightly tapered inner diameter; used to join two fused silica capillaries of equal or different diameters. Advantages compared to stainless steel fittings are easy connection without tools, optical control during connection, negligible heat capacity and no dead volume. PTFE shrinking tube can also be used for connecting capillaries. The minimum inner diameter expanded is.7 mm, the maximum ID shrunk is 0.40 mm. Shrinking occurs above 0 C. Connections with PTFE shrinking tube are applicable up to 00 C only. They should never be used above 0 C. Description Pack of Cat. No. Specification Graphseal connecting system for capillary columns Graphseal adaptor set 7080 Graphseal nut, slotted nuts 708 Graphseal ferrule, 0.4 mm bore 0 ferrules 7087 Graphseal ferrule, 0. mm bore 0 ferrules 7088 Graphseal ferrule, 0.8 mm bore 0 ferrules 7089 Universal capillary glass connectors linear connectors linear 0 connectors Y splitter connector PTFE shrinking tube, thinwalled /6" exit, injector or detector Graphseal insert, 0.8 mm bore Graphseal reducing unit 4 Graphseal ferrule slotted nut 6 capillary + + Graphseal adaptor 7080 m 7080 for connecting capillaries, min. ID expanded.7 mm, max. ID shrunk 0.40 mm Accessories for GC MN 49

54 Accessories for capillary columns Valco fused silica adaptors and fittings for capillary GC one-piece FS adaptors: recommended for use in fittings where the polyimide ferrule need not be removed two-part removable FSR adaptors: recommended for use in Valco valves; consists of a liner which slides over the fused silica tubing, and a ferrule, both made of high temperature polyimide alloys the liner with an enlarged diameter at one end fits within the nut, thus ensuring that the liner and the tube within are removed as the nut is unscrewed from the valve (see figure below) The /6" FSR adaptor comes with a special counterbored /6" nut (ZCN) to receive the liner. The /" adaptor works with standard Valco /" nuts. liner standard ferrule Accessories for GC Union with FS adaptors capillary fitting capillary nut one-piece polyimide adaptors Union with FSR adaptors capillary fitting capillary nut ferrule Valve with FSR adaptors valve body capillary slot 0. mm orifice liner nut FSR: liner ferrule rotor To order Valco fittings for use with fused silica adaptors (FS or FSR recommended), add suffix J to the fitting code and specify the appropriate number of adaptors separately. The stainless steel ferrules normally provided with the fittings are omitted since they are replaced by the FS (or FSR) adaptors. Again, for /6 FSR adaptors use the counterbored nut ZCN supplied with the adaptor. Examples: ) Connection of capillaries with 0. mm ID and 0.4 mm OD: either use a / union ZU.TJ and FS adaptors FS.4 or a / union ZU.TJ and removable FSR adaptors FSR.4 ) Connection of capillaries with 0. mm ID and 0.8 mm OD: we recommend either a /6 union ZUTJ and FS adaptors FS-.8 or a /6 union ZUTJ and removable FSR adaptors FSR.8 If capillaries and have different outer diameters, the corresponding different FS adaptors have to be used. For use of fused silica adaptors with Valco valves please order the number of adaptors (FSR required) when you order the valve, or when you want to use an existing valve with open tubular columns. Please note that for /6 FSR adaptors you have to use the special counterbored nut ZCN which is supplied with the adaptors FSR. and FSR.8. Examples: ) For connecting a capillary with 0. mm ID (0. mm OD) to a valve with / fittings we recommend the removable FSR adaptor FSR.. ) For connecting a capillary with 0. mm ID (0.8 mm OD) to a valve with /6 fittings we recommend the removable FSR adaptor FSR MN

55 Accessories for capillary columns Valco code Description Pack of Cat. No. One-piece fused silica adaptors for capillary OD FS.- /" < 0. mm 7440 FS.4- /" mm 744 FS.- /" mm 7444 FS.4- /6" < 0.4 mm FS.- /6" mm FS.8- /6" mm Removable fused silica adaptors (incl. nuts) FSR.- /" < 0. mm FSR.4- /" mm 7440 FSR.- /" mm 744 FSR.- /6" < 0. mm 74 FSR.8- /6" mm 744 Replacement liners FSL.- /" < 0. mm 744 FSL.4- /" mm 744 FSL.- /" mm 7444 FSL.- /6" < 0. mm 744 FSL.8- /6" mm 7446 Special nut for fused silica adaptors ZCN /6" counterbored 7447 For standard Vespel ferrules as well as standard nuts please see the Valco programme, which is available on request. Unions, Tees and crosses for fused silica adaptors (without ferrules, but incl. standard nuts) ZU.TJ /" /" for butt connection 7448 ZUTJ /6" /6" for butt connection 74 ZT.J /" Tee 744 ZTCJ /6" Tee, capillary bore 746 ZX.J /" cross 744 ZXCJ /6" cross, capillary bore 747 Tools for Valco fused silica adaptors OEW open end wrench (/6" x /4") 744 for use with /" fittings PV pin vise and drill index (0.4 to.0 mm) 7444 application see text below Accessories for GC Should a tube break in a straight-through union, remove the nuts and the tube opposite the broken one. Clear the fitting by passing a drill or wire of appropriate diameter into the unbroken side and through the centre of the fitting. A pin vise and drill index are used for removing ferrules from Tee and cross fittings, and for enlarging the interior diameter of FS adaptors (Valco code PV). For other fittings and valves for GC please ask for our VICI / Valco programme. MN