Gas chromatography. 298

Transcription

1 Gas chromatography 98

2 Basics The GC system Transport of the components occurs exclusively in the mobile phase, while separation only takes place in the stationary phase. The quality of a separation (resolution) depends on the residence time of the components within the stationary phase and on the rate of interactions. The type of interaction between component and phase (selectivity) is determined by the functional groups of the stationary phase. The polarity of the phase is a function of its 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 t R w ½ t R Configuration of a gas chromatograph Gas supply: carrier gas and - if necessary - detector gases e.g., for FID detector Sample injector: During direct injection, the sample is applied to the column without touching any other parts made from glass or metal (on-column injection). During indirect injection, the sample is brought into an evaporator and is then transferred onto the column either completely, or partially (split technique). Both techniques allow working at low temperatures, high temperatures and the use of temperature programming. Capillary column: the heart of the GC system 4 -controlled oven 5 Detector: indicates a substance by generating an electrical signal (response). Some detectors are specific for certain classes of substances or for certain elements (e.g., P, N). 6 Data station for configuration of a gas chromatograph The separation process Chromatographic separation is achieved through continuous distribution of each sample component between the mobile and the stationary phase: In GC, the mobile phase is always a gas, mostly either He, N or H. The stationary phase is often a viscous, gum-like liquid adhered to the inner wall of a capillary column (WCT = Wall Coated pen Tubular). 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 Ri 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 Ri : net retention time = difference between total retention time and dead time t 0. It indicates how long a substance stays in the stationary phase. ther terms characterizing a separation: k : retention factor: a measure for the position of a sample peak in the chromatogram. The retention factor is specific for a given compound and constant under constant conditions. k i = t Ri t 0 α: relative retention, also called separation factor or selectivity coefficient, is the ratio of two capacity factors. The reference substance is always in the denominator. α = t 0 k k 00

3 Basics The relative retention does not provide any information on the quality of a separation. For equal values of α two very broad peaks may overlap (as shown in a), or may be completely resolved (as in b), if they are accordingly narrow. a b t [min] R: resolution: a measure for the quality of a separation, taking (w / ) into account according to: R =.8 t R - t R (w / ) + (w / ) N: number of theoretical plates: characterizes the quality of a column (should be determined for k > 5). 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 Nth. The smaller this value the more efficient the column. (t Ri ) N = 5.54 (w / ) h = HETP = The Golay equation shows how the plate height h depends on the flow velocity u: B: molecular axial diffusion; B is a function of the diffusion coefficient of the component in the respective carrier gas HETP h min u optimal C: resistance to mass transfer B u B HETP = +C u u C u In practice often higher velocities than u opt. are chosen, if separation efficiency is sufficient. Higher carrier velocities mean shorter retention times. L N u Parameters characterizing a capillary column PTIMA 5.0 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 MACHEREY-NAGEL offers ranges from 0. to 5.0 μm. The standard film thickness is 0.5 μm. Thin films (0. 0. μm) are very well suited for high-boiling, temperature-sensitive or almost contemporaneously eluting substances. Increasing the film thickness will increase the capacity, the retention for low-boiling substances and the inertness of the column. This is especially helpful for samples with a broad range of concentrations, or the separation of volatile polar substances. A better coverage of the column wall by a thicker film and a reduced column surface due to a shorter column have a positive impact on the separation of very active substrates, that may cause noticeable tailing when they come in contact with non-coated spots of the column wall. Thick films, however, always mean more stationary phase in the column, hence increased column bleeding. Therefore, maximum operating temperatures for thick-film columns are reduced. In addition, thick-film columns may have a lesser separating capacity. C. Column length The separating efficiency (better the number of plates N) of a column is directly proportional to its length. Most routine separations are carried out on 5 or 0 m columns, while more complex samples may require 50 or 60 m. 0 m columns are common for Fast GC (see page 40). 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 at low carrier gas flow 0.5 mm ID: for analysis of complex mixtures 0. mm ID: for routine analysis with short retention times, but increased capacity 0.5 mm ID: for rapid separations with inert surface and highest capacity 0

4 USP listing USP listing of MN GC phases Code Specifications MN GC phases Page USP G / G dimethylpolysiloxane oil PTIMA 0 PTIMA MS PTIMA MS Accent PTIMA -TG 48 PERMABND SE-0 6 PERMABND P-00 5 USP G 50 % phenyl - 50 % methylpolysiloxane PTIMA 7 7 PTIMA 7 MS 8 PTIMA 7-TG 48 USP G6 trifluoropropylmethylpolysiloxane PTIMA 0 9 USP G7 50 % -cyanopropyl - 50 % phenylmethylpolysiloxane PTIMA 5 0 USP G6 polyethylene glycol (average molecular weight ~ 5 000); high molecular weight compound of polyethylene glycol and diepoxide PTIMA WAX PTIMA WAXplus PERMABND CW 0 M 7 PERMABND CW 0 M-DEG 54 FS-CW 0 M-AM 5 USP G9 5 % phenyl 5 % cyanopropyl 50 % methylsiloxane PTIMA 5 0 USP G5 high molecular weight compound of polyethylene glycol and diepoxide, which is esterified with terephthalic acid PTIMA FFAP 4 PTIMA FFAPplus 5 PERMABND FFAP 8 USP G7 5 % phenyl 95 % methylpolysiloxane PTIMA 5 4 PTIMA 5 Amine 50 PTIMA 5 HT 49 PTIMA 5 MS 5 PTIMA 5 MS Accent 6 PERMABND SE-5 6 USP G8 5 % phenyl 75 % methylpolysiloxane PTIMA 5 MS 6 USP G 0 % phenylmethyl 80 % dimethylpolysiloxane PTIMA 5 MS 6 USP G5 high molecular weight compound of polyethylene glycol and diepoxide, which is esterified with nitroterephthalic acid PTIMA FFAP 4 PTIMA FFAPplus 5 PERMABND FFAP 8 USP G6 % vinyl 5 % phenylmethylpolysiloxane PTIMA 5 4 PTIMA 5 Amine 50 PTIMA 5 HT 49 PTIMA 5 MS 5 PTIMA 5 MS Accent 6 PERMABND SE-54 HKW 5 USP G8 dimethylpolysiloxane oil PTIMA 0 PTIMA MS PTIMA MS Accent PTIMA -TG 48 PERMABND SE-0 6 PERMABND P-00 5 USP G4 5 % phenyl 65 % dimethylpolysiloxane PTIMA 5 MS 6 USP G4 6 % cyanopropylphenyl 94 % dimethylpolysiloxane PTIMA 0 PTIMA 0 MS PTIMA 64 PTIMA 64 LB USP G46 4 % cyanopropylphenyl 86 % methylpolysiloxane PTIMA 70 4 PTIMA 70 MS 5 USP G49 proprietary derivatized phenyl groups on a polysiloxane backbone PTIMA δ- 9 0

5 MACHEREY-NAGEL GmbH & Co. KG Neumann-Neander-Str Düren Germany DE / International: CH: FR: Tel.: Fax: info@mn-net.com Tel.: Fax: sales-ch@mn-net.com Tel.: Fax: sales-fr@mn-net.com No. Name Ret.Time Area Rel.Area Height min mv*min % mv ctanol 7,5 0, 7,0 5, Undecane 8,4 0,78 8,9 7, Dim e -aniline 9,50 0,60 8,7 5,5 4 Dodecane 9,96 0,9 9,6 7,4 5 De cylamine 0,8 0,49 7,99 6,0 6 C0-ester,6 0,6 7,7 5,4 7 C-ester,95 0,9 7,70 5,5 8 He ne icos ane 4, 0,4,85 8, 9 Docos ane 5,6 0,45 4,50 8,4 0 Tricosane 6,55 0,464 4,9 8,4 MACHEREY-NAGEL GmbH & Co. KG Neumann-Neander-Str Düren Germany DE / International: CH: FR: Tel.: Fax: info@mn-net.com i US: 0, 5,0 0,0 5,0 0,0 5,0 0,0 5,0 40,0 Tel.: Fax: sales-us@mn-net.com Tel.: Fax: sales-ch@mn-net.com Tel.: Fax: sales-fr@mn-net.com US: Tel.: Fax: sales-us@mn-net.com min Additional information for GC columns Scope of delivery Each column is individually tested and supplied with test certificate and test chromatogram, but without fittings or ferrules. Columns have fused ends or are sealed with septa, to protect them from atmospheric oxygen. Further more an instruction leaflet is enclosed. Manufactured by MACHEREY-NAGEL PTIMA LIPDEX HYDRDEX Made in Germany Gebrauchsanleitung GC User Manual Manuel d utilisation Fused silica capillary column ctanol Undecane Dime-anil ne Decylamine C0-ester Dode cane C-ester Heneicosane Docosane Tricosane GC cages The standard size of a GC cage is 7 inches. n request, all columns can be supplied on a 5 inch ( cm) cage e.g., for the Agilent GC To order, please add an E at the end of the REF number (e.g., E) 7 inches standard size e.g., REF inches special cage e.g., REF E Integrated guard column To prolong column life, even at highly contaminated or matrix-containing samples, MN offers the option to add an integrated guard column. All capillary columns are available with a 0 m guard column with respective deactivation. To order, please add V at the end of the REF number (e.g., V). Guard column combinations with other lengths, IDs or different deactivation are available on request. Without integrated guard column e.g., REF With integrated guard column e.g., REF V 0

6 MACHEREY-NAGEL derivatization reagents Purpose of derivatization 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 inserted by derivatization (e.g., trifl uoroacetates) for specifi c detection (ECD) with the advantage of high sensitivity Infl uence of elution orders and fragmentation patterns in MS by a specifi c derivatization We provide reagents for - Silylation - Alkylation (methylation) - Acylaction For x 0 ml, x 50 ml and 6 x 50 ml also as screw neck vial Product range from page 57 onwards 04

7 Separation properties of PTIMA phases PTIMA FFAP PTIMA FFAPplus steigende Polarität PTIMA WAX PTIMA WAXplus PTIMA PTIMA PTIMA 0 increasing polarity PTIMA 7 PTIMA 7 MS PTIMA 70 PTIMA 70 MS PTIMA 5 MS PTIMA 0 PTIMA 0 MS PTIMA 64 PTIMA 64 LB PTIMA 5 PTIMA 5 MS PTIMA 5 MS Accent PTIMA 5 HT PTIMA PTIMA MS PTIMA MS Accent Peaks:. Undecane. Dodecane. ctanol 4. Dimethylaniline 5. Decylamine 6. Methyl decanoate 7. Methyl undecanoate 8. Henicosane 9. Docosane 0. Tricosane All columns: 0.5 μm film, 0 m x 0.5 mm ID Sample: MN PTIMA test mixture (REF 76) Injection:.0 μl, split 5 ml/min Carrier gas: 0.80 bar He : 80 C T max (isothermal), 8 C/min (0 min T max ) Detector: FID C 05

8 Summary of MN phases for GC verview of PTIMA MN phases Phase Composition Page Relative polarity temperature Maximum PTIMA 0 PTIMA MS 00 % dimethylpolysiloxane 40 / 60 C PTIMA MS Accent PTIMA 5 5 % phenyl 95 % methylpolysiloxane 4 40 / 60 C PTIMA 5 MS 5 % diphenyl 95 % dimethylpolysiloxane 5 40 / 60 C PTIMA 5 MS Accent silarylene phase with selectivity similar to 5 % diphenyl 95 % dimethylpolysiloxane 6 40 / 60 C PTIMA XLB silarylene phase like above, optimized silarylene content for low bleeding 7 40 / 60 C PTIMA δ- phase with autoselectivity / 60 C PTIMA δ-6 phase with autoselectivity / 60 C PTIMA 0 6 % cyanopropylphenyl 94 % dimethylpolysiloxane 00 / 0 C PTIMA 0 MS silarylene phase with low bleeding: polarity similar to 6 % cyanopropylphenyl 94 % dimethylpolysiloxane 00 / 0 C PTIMA 64 6 % cyanopropylphenyl 94 % dimethylpolysiloxane PTIMA 64 LB like above, phase with low bleeding 80 / 00 C PTIMA 70 4 % cyanopropylphenyl 86 % dimethylpolysiloxane 4 80 / 00 C PTIMA 70 MS silarylene phase with low bleeding: polarity similar to 4 % cyanopropylphenyl 86 % dimethylpolysiloxane 5 80 / 00 C = nonpolar, = polar First temperature (long term temperature) for isothermal operation, second value for the max. temperature (short term temperature) in a temperature program. Please note th For details refer to the description of individual phases. 4 Phases which provide a similar selectivity based on chemical and physical properties See description on page 8 GC columns for special separations can be found from page 9 onwards. 06

9 Summary of MN phases for GC Structure USP Similar phases Si n G / G / G8 PERMABND SE-0, V-, DB-, SE-0, HP-, SPB -, CP-Sil 5 CB, Rtx -, 007-, BP, MDN-, AT -, ZB-, V-0 5 % diphenyl 95 % dimethylpolysiloxane Si m Si n G7 / G6 PERMABND SE-5, SE-54, SE-5, HP-5, SPB -5, CP-Sil 8, Rtx -5, 007-5, BP5, MDN-5, AT -5, ZB-5 Si m Si n G7 / G6 DB-5, DB-5MS, HP-5MS, Ultra-, Equity -5, CP-Sil 8CB low bleed/ms, Rxi -5MS, Rtx -5SIL-MS, Rtx -5MS, 007-5MS, BPX 5, MDN-5S, AT -5MS, VF-5MS Si Si Si G7 / G6 n o Si Si Si DB-XLB, Rxi -XLB, Rtx -XLB, MDN-, VF-XMS n o see description page 8 G49 no similar phases see description page 8 no similar phases Si Si G4 HP-0, DB-0, SPB -0, Rtx -0, CP-0, NC (CH ) m n NC (CH ) Si Si Si Si G4 VF-0ms, Rxi -0Sil MS, TG-0MS NC (CH ) m m n Si Si G4 HP-64, HP-VC, DB-64, DB-VRX, SPB -64, CP-64, Rtx -64, Rtx -Volatiles, , BP64, VCL NC (CH ) m n Si Si G46 V-70, DB-70, CP-Sil 9 CB, HP-70, Rtx -70, SPB -70, , BP0, ZB-70 NC (CH ) m n NC NC (CH ) Si (CH ) m Si Si m Si n G46 VF-70ms, TG-70MS, V-70, DB-70, HP-70, Rtx -70, SPB -70, CP Sil 9 CB, , BP0, ZB-70 at for columns with 0.5 mm ID and for columns with thicker films temperature limits are generally lower. 07

10 Summary of MN phases for GC Phase Composition Page Relative polarity temperature Maximum PTIMA 5 MS silarylene phase with selectivity similar to 5 % diphenyl 65 % dimethylpolysiloxane 6 60 / 70 C PTIMA 7 phenylmethylpolysiloxane, 50 % phenyl 7 0 / 40 C PTIMA 7 MS silarylene phase with selectivity similar to 50 % phenyl 50 % methylpolysiloxane 8 40 / 60 C PTIMA 0 trifluoropropylmethylpolysiloxane (50 % trifluoropropyl) 9 60 / 80 C PTIMA 5 50 % cyanopropylmethyl 50 % phenylmethylpolysiloxane 0 60 / 80 C PTIMA 40 % cyanopropylmethyl 67 % dimethylpolysiloxan 60 / 80 C PTIMA WAX polyethylene glycol Da 40 / 50 C PTIMA WAXplus polyethylene glycol with optimized cross-linking 60 / 70 C PTIMA FFAP polyethylene glycol -nitroterephthalate 4 50 / 60 C PTIMA FFAPplus polyethylene glycol -nitroterephthalate with optimized cross-linking 5 50 / 60 C = nonpolar, = polar First temperature (long term temperature) for isothermal operation, second value for the max. temperature (short term temperature) in a temperature program. Please note t For details refer to the description of individual phases. Phases which provide a similar selectivity based on chemical and physical properties GC columns for special separations can be found from page 9 onwards. 08

11 Summary of MN phases for GC Structure USP Similar phases Si Si Si Si G8 / G / G4 DB-5 MS, HP-5, SPB -5, Rxi -5SIL MS, Rtx-5, 007-5, BPX -5, MDN-5, AT -5 MS, ZB-5, V-, VF-5 MS m n o Si G V-7, DB-7, HP-50+, HP-7, SPB -50, SP-50, Rxi -7, Rtx -50, CP-Sil 4 CB, 007-7, ZB-50 m Si Si Si G V-7, AT -50, BPX -50, DB-7, DB-7ms, HP-50+, HP-7, SPB -50, SPB -7, SP-50, Rtx -50, CP-Sil 4 CB, 007-7, VF-7ms, ZB-50 m n Si G6 V-0, DB-0, Rtx -00, F C (CH ) n NC Si (CH ) m m = n Si n G7 / G9 DB-5, HP-5, V-5, Rtx -5, CP-Sil 4, 007-5, BP5 NC Si (CH ) m Si n no similar phases H H C H H C H n H G6 PERMABND CW 0 M, DB-Wax, Supelcowax, HP-Wax, HP-INNWAX, Rtx-Wax, CP-Wax 5 CB, Stabilwax, 007-CW, BP0, AT-Wax, ZB-Wax DB-Wax, Supelcowax, HP-Wax, HP-INNWAX, Rtx-Wax, CP-Wax 5 CB, Stabilwax, 007-CW, BP0, AT-Wax, ZB-Wax C N C (CH CH ) m n G5 / G5 PERMABND FFAP, DB-FFAP, HP-FFAP, CP-Wax 58 FFAP CB, 007-FFAP, CP-FFAP CB, Nukol, AT-000, SPB-000, BP, V-5 DB-FFAP, HP-FFAP, CP-SIL 58 CB, 007-FFAP, CP-FFAP CB, Nukol hat for columns with 0.5 mm ID and for columns with thicker films temperature limits are generally lower. 09

12 PTIMA nonpolar capillary columns PTIMA 00 % dimethylpolysiloxane USP G / G / G8 Nonpolar phase Structure see page 07 Separation of components according to boiling points Thick film columns μm film are especially recommended for solvent analysis. Columns with mm ID and films < μm: T max 40 C (long-term temperature), T max 60 C (short-term max. temperature in a temperature program) 0.5 mm ID, films < μm: T max 0 and 40 C, resp. Thick film columns with films μm: max. temperatures 00 and 0 C, resp. Similar phases PERMABND SE-0 (see page 6), V-, DB-, SE-0, HP-, SPB -, CP-Sil 5 CB, Rtx -, 007-, BP, MDN-, AT -, ZB-, V-0 PTIMA 0. mm ID (0.4 mm D) 0 m m 5 m 0 m 5 m 0 m 50 m 60 m 0.0 μm film μm film mm ID (0.4 mm D) 0.0 μm film μm film μm film μm film mm ID (0.4 mm D) 0.0 μm film μm film μm film μm film mm ID (0.5 mm D) 0.0 μm film μm film μm film μm film μm film μm film μm film mm ID (0.8 mm D) 0.50 μm film μm film μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. 0

13 PTIMA nonpolar capillary columns Solvent analysis MN Appl. No. 090 Column: PTIMA, 60 m x 0. mm ID,.0 μm fi lm Sample: solvent mixture, courtesy of J. Lutz, Alcan Rorschach, Switzerland Injection: 0.4 μl, split :60 Carrier gas: H, 0 kpa : 50 C (9 min) 90 C, 4 C/min 80 C ( min), 4 C/min Detector: FID 00 C Peaks:. Methanol. Ethanol. Acetone 4. -Propanol 5. Methyl acetate 6. n-propanol 7. Methyl ethyl ketone 8. Ethyl acetate 9. Isobutanol 0. n-butanol. -Methoxy--propanol. Isooctane. Ethyl glycol 4. Isoheptane 5. 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 5. Butyl glycol 6. Heptanol 7. Ethyl diglycol 8. Butyl diglycol 9. Butyl glycol acetate 0. Butyl diglycol acetate min

14 PTIMA nonpolar capillary columns PTIMA MS 00 % dimethylpolysiloxane USP G / G / G8 Selectivity identical to PTIMA, Phase with low bleeding Structure see page 07 GC/MS and ECD, general analysis at trace level T max 40 C (long-term temperature), T max 60 C (short-term max. temperature in a temperature program) Similar phases Ultra-, DB-MS, HP-MS, Rxi -MS, Rtx -MS, Equity -, AT -MS, VF-MS, CP-Sil 5 CB MS PTIMA MS 0. mm ID (0.4 mm D) m 5 m 5 m 0 m 50 m 60 m 0.0 μm film μm film mm ID (0.4 mm D) 0.5 μm film mm ID (0.5 mm D) 0.5 μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. PTIMA MS Accent 00 % dimethylpolysiloxane USP G / G / G8 Selectivity identical to PTIMA, nonpolar phase Lowest column bleed Solvent rinsing for removal of impurities applicable Increased sensitivity due to an unmatched low background level Structure see page 07 Ideal for ion trap and quadrupole MS detectors Perfect inertness for basic compounds All-round phase for environmental analysis, trace analysis, EPA methods, pesticides, PCB, food and drug analysis T max 40 C (long-term temperature), T max 60 C (short-term max. temperature in a temperature program) Similar phases Ultra-, DB-MS, HP-MS, Rxi -MS, Rtx -MS, Equity -, AT -MS, VF-MS, CP-Sil 5 CB MS

15 PTIMA nonpolar capillary columns Column: Sample: Injection: Carrier gas: : PTIMA MS Accent, 0 m x 0. mm ID, 0.50 μm fi lm 0. μg/ml in hexane, 840 / 84 P pesticides calibration mix A and 84 P pesticides calibration mix B; IS triphenyl phosphate and tributyl phosphate 50 C, splitless (hold min) He, ml/min, constant pressure EPA 840 / 84 / 84 A rganophosphorus pesticides MN Appl. No C 80 C, 0 C/min ( min) 00 C, 8 C/min ( min) Detector: FPD (Flame Photometric Detector), 80 C Peaks:. Dichlorvos. Hexamethylphosphoramide. Mevinphos 4. Trichlorfon 5. TEPP 6. Thionazin 7. Demeton- 8. Ethoprop 9. Tributyl phosphate (IS) 0. Dicrotophos. Monocrotophos. Naled. Sulfotepp 4. Phorate 5. Dimethoate 6. Demeton-S 7. Dioxathion 8. Terbufos 9. Fonophos 0. Phosphamidon isomer. Diazinon. Disulfoton. Phosphamidon 4. Dichlorofenthion 5. Parathion-methyl 6. Chlorpyrifos-methyl 7. Ronnel 8. Fenitrothion 9. Malathion 0. Fenthion. Aspon. Parathion-ethyl. Chlorpyrifos 4. Trichloronate 5. Chlorfenvinphos 6. Merphos 7. Crotoxyphos 8. Stirofos 9. Tokuthion 40. Merphos oxidation product 4. Fensulfothion 4. Famphur 4. Ethion 44. Bolstar 45. Carbophenothion 46. Triphenyl phosphate (IS) 47. Phosmet 48. EPN 49. Azinphos-methyl 50. Leptophos 5. Tri-o-cresyl phosphate 5. Azinphos-ethyl 5. Coumaphos min PTIMA MS Accent 0. mm ID (0.4 mm D) 5 m 5 m 0 m 50 m 60 m 0.0 μm film mm ID (0.4 mm D) 0.5 μm film μm film mm ID (0.5 mm D) 0.5 μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0.

16 PTIMA weakly polar capillary columns PTIMA 5 5 % phenyl 95 % methylpolysiloxane USP G7 / G6 Nonpolar phase Structure see page 07 Standard phase with large range of application Columns with mm ID and films < μm: T max 40 C (long-term temperature), T max 60 C (short-term max. temperature in a temperature program) 0.5 mm ID, films < μm: T max 0 and 40 C, resp. Thick film columns with films μm: max. temperatures 00 and 0 C, resp. Similar phases PERMABND SE-5 (see page 6), SE-54, SE-5, HP-5, SPB -5, CP-Sil 8, Rtx -5, 007-5, BP5, MDN-5, AT -5, ZB-5 PTIMA 5 0. mm ID (0.4 mm D) 0.0 μm film mm ID (0.4 mm D) 0 m 5 m 5 m 0 m 50 m 60 m 0.0 μm film μm film μm film μm film mm ID (0.4 mm D) 0.0 μm film μm film μm film μm film μm film mm ID (0.5 mm D) 0.0 μm film μm film μm film μm film μm film μm film μm film mm ID (0.8 mm D) 0.50 μm film μm film μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. Further applications can be found online in our application database at /apps 4

17 PTIMA weakly polar capillary columns PTIMA 5 MS 5 % diphenyl 95 % dimethylpolysiloxane USP G7 / G6 Selectivity identical to PTIMA 5 Phase with low bleeding Structure see page 07 GC/MS and ECD, applications and general analysis at trace level Perfect inertness for basic compounds T max 40 C (long-term temperature), T max 60 C (short-term max. temperature in a temperature program) Similar phases DB-5, DB-5MS, HP-5MS, Ultra-, Equity -5, CP-Sil 8CB low bleed/ms, Rxi -5MS, Rtx -5SIL-MS, Rtx -5MS, 007-5MS, BPX 5, MDN-5S, AT -5MS, VF-5MS Analysis of various phenols MN Appl. No. 00 Column: Sample: PTIMA 5 MS, 0 m x 0.5 mm ID, 0.5 μm fi lm 5 ppm of each compound except N-i-propylaniline (9.4 ppm) 4 Methode: SPME : Detector: 40 C ( min) 40 C, 6 C/min 0 C, 0 C/min MSD 8 Peaks:. Toluene-D 8. Phenol. -Methylphenol (o-cresol) Nitrobenzene-D 5 5. N-i-Propylaniline 6.,4-Dichlorophenol 7. 4-Chlorophenol 8. 4-Bromo--chlorophenol 9. -Bromophenol Chloro--methylphenol.,4-Dibromophenol. -Hydroxybiphenyl 4. -Cyclohexylphenol 4. Hexafl uorobisphenol A 6 Courtesy of Riedel-de-Haën, Seelze, Germany min PTIMA 5 MS 0. mm ID (0.4 mm D) m 5 m 5 m 0 m 50 m 60 m 0.0 μm film μm film mm ID (0.4 mm D) 0.5 μm film μm film μm film mm ID (0.5 mm D) 0.5 μm film μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. 5

18 PTIMA weakly polar capillary columns PTIMA 5 MS Accent silarylene phase USP G7 / G6 Chemically bonded, cross-linked silarylene phase with polarity similar to a 5 % diphenyl - 95 % dimethylpolysiloxane phase Lowest column bleed, nonpolar phase, solvent rinsing for removal of impurities applicable Structure see page 07 Ideal for ion trap and quadrupole MS detectors Perfect inertness for basic compounds All-round phase for environmental analysis, trace analysis, EPA methods, pesticides, PCB, food and drug analysis T max 40 C (long-term temperature), T max 60 C (short-term max. temperature in a temperature program) Film thickness > 0.5 μm: T max 0 and 40 C, resp. Similar phases DB-5, DB-5MS, HP-5MS, Ultra-, Equity -5, CP-Sil 8CB low bleed/ms, Rxi -5MS, Rtx -5SIL-MS, Rtx -5MS, 007-5MS, BPX 5, MDN-5S, AT -5MS, VF-5MS Increased sensitivity due to an unmatched low background level The bleed comparison test of PTIMA 5 MS Accent with a conventional 5 MS phase shows the outstanding performance of the silarylene phase. Background noise at 40 C The unmatched low background level of the PTIMA 5 MS Accent, which is approximately three times lower compared to a 5 MS brand column, provides significantly increased sensitivity and allows its application in trace analysis particularly of high-boiling compounds Standard 5 MS phase 90. PTIMA 5 MS Accent FID signal in mv s s PTIMA 5 MS Accent 0. mm ID (0.4 mm D) m 5 m 5 m 0 m 50 m 60 m 0.0 μm film μm film mm ID (0.4 mm D) 0.5 μm film μm film μm film mm ID (0.5 mm D) 0.5 μm film μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. 6

19 PTIMA weakly polar capillary columns PTIMA XLB silarylene phase Chemically bonded, cross-linked silarylene phase, optimized silarylene content for lowest column bleed, nonpolar phase, perfect inertness for basic compounds, solvent rinsing for removal of impurities applicable Structure see page 07 Ideal for ion trap and quadrupole MS detectors, ultra low bleed phase, highly selective for environmental and trace analysis, pesticides, recommended phase for PCB separations T max 40 C (long-term temperature), T max 60 C (short-term max. temperature in a temperature program) Similar phases DB-XLB, Rxi -XLB, Rtx -XLB, MDN-, VF-XMS Column: Injection: Carrier gas: : PTIMA XLB, 0 m x 0.5 mm ID, 0.5 μm fi lm Rapid separation of PCB and PAH MN Appl. No. 90 μl, Standard ng/μl, 50 C, pulsed, splitless, pulse.8 bar in min 60 ml/min He 40 C ( min) 40 C ( min), 0 C/min 40 C (5 min), 0 C/min Detektion: MS source 0 C, interface 80 C, quadrupole 50 C Peaks:. Naphthalene. -Methylnaphthalene. Acenaphthylene 4. Acenaphthene 5. Fluorene 6. Phenanthrene 7. Anthracene 8. PCB- 9. PCB-8 0. PCB-5. Fluoranthene. PCB-0. Pyrene 4. PCB Methylfl uoranthene 6. PCB-8 7. PCB-5 8. PCB-8 9. PCB-6 0. PCB-80. Benz[a]anthracene. Chrysene. PCB PCB Benzo[b]fl uoranthene 6. Benzo[k]fl uoranthene 7. Benzo[a]pyrene 8. Dibenz[ah]anthracene 9. Indeno[,,-cd]pyrene 0. Benzo[ghi]perylene Courtesy of Centre d Analyses de Recherche, Lab. d Hydrologie, Illkirch, France : PCB- 8/9 0 9: PCB-8 8 % separation in less than 0 min! benzo[b]fl uoranthene / benzo[k]fl uoranthene 75 % separation in 7 min! min PTIMA XLB 0.5 mm ID (0.4 mm D) 0 m 60 m 0.5 μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. 7

20 5 PTIMA δ phases with autoselectivity Range of polarities covered by PTIMA δ phases 7 PTIMA δ- 70 PTIMA δ-6 All stationary GC phases can be classified by their polarities. While the selectivity of common GC phases is generally determined by permanent dipole-dipole interactions, PTIMA δ- and PTIMA δ-6 show an additional feature. Large, polarizable groups in the polymer chain of the stationary phase enable the analyte to induce a further dipole moment that increases 0 40 with the polarity of said analyte. We call this phenomenon Autoselectivity, because the column adjusts itself to the polarity of the analyte. The implemented polymers consist of cross-linked polysiloxanes with a defined composition and an extremely narrow distribution of molecular weight. PTIMA δ phases cover broad ranges of polarities. Compared with conventional phases, PTIMA δ- polarity ranges from approximately the nonpolar PTIMA 5 to the midpolar PTIMA 70, while for PTIMA δ-6 the polarity covers a range from about the midpolar PTIMA 7 to the polar PTIMA 0. PTIMA δ phases show 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 analyze with standard GC phases (e.g., PTIMA 5 or PTIMA 7) because of co-elutions. The autoselective PTIMA 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 PTIMA δ- (see chromatogram page 9). Separation characteristics of PTIMA δ phases PTIMA 7 PTIMA 70 of PTIMA δ phases Wide range of application due to autoselectivity utstanding thermal stability similar to nonpolar phases Low bleed levels Medium polar without CN groups PTIMA δ PTIMA δ PTIMA 0 Conditions and peaks (see page 05) about PTIMA δ phases can be found on page 9 and page 0. 8

21 PTIMA δ phases with autoselectivity PTIMA δ- polysiloxane phase with autoselectivity USP G49 Medium polar without CN groups Autoselectivity resulting in a polarity range from approximately the nonpolar PTIMA 5 to the midpolar PTIMA 70 (see page 8) Analytes determine the polarity of the phase Similar phases Exclusive from MN Ideal for MSD and PND detectors mm ID: T max 40 C (long-term temperature), T max 60 C (short-term max. temperature in a temperature program) 0.5 mm ID: T max 0 and 40 C, resp. Analysis of isomeric phenols MN Appl. No Column: Injection:.0 μl, split :80 Carrier gas: : PTIMA δ-, 60 m x 0.5 mm ID, 0.5 μm fi lm He,. bar Detector: MSD HP 597 Peaks:. Phenol. -Chlorophenol. -Methylphenol 4. 4-Methylphenol 5. -Methylphenol 6.,4-Dimethylphenol 7. -Nitrophenol 8.,4-Dichlorophenol 9.,6-Dichlorophenol 0. 4-Chloro--methylphenol.,,5-Trichlorophenol.,4,6-Trichlorophenol 60 C ( min) 0 C, 6 C/min.,4,5-Trichlorophenol 4.,,4-Trichlorophenol 5.,,6-Trichlorophenol 6.,,5,6-Tetrachlorophenol 7.,,4,5-Tetrachlorophenol 8.,,4,6-Tetrachlorophenol 9.,4-Dinitrophenol 0.,4,5-Trichlorophenol. -Methyl-4,6-dinitrophenol. -Isopropyl-4,6-dinitrophenol min PTIMA δ- 0. mm ID (0.4 mm D) 0 m 0 m 5 m 0 m 50 m 60 m 0.0 μm film mm ID (0.4 mm D) 0.0 μm film mm ID (0.4 mm D) 0.5 μm film μm film mm ID (0.5 mm D) 0.5 μm film μm film μm film mm ID (0.8 mm D).00 μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. 9

22 PTIMA δ phases with autoselectivity PTIMA δ-6 polysiloxane phase with autoselectivity Medium polar without CN groups Autoselectivity resulting in a polarity range from approximately the midpolar PTIMA 7 to the polar PTIMA 0 (see page 8) Analytes determine the polarity of the phase Similar phases Exclusive from MN Ideal for MSD and PND detectors mm ID: T max 40 C (long-term temperature), T max 60 C (short-term max. temperature in a temperature program) 0.5 mm ID: T max 0 and 40 C, resp. Column: Sample: Injection: μl, split :0 Carrier gas: : PTIMA δ-6, 50 m x 0. mm ID, 0. μm fi lm EPA 840 P pesticide calibration mix (Restek), 00 μg/ml each in hexane acetone (95:5).0 bar He Detector: MSD HP 597 Peaks:. Dichlorvos. Mevinphos. Demeton-S 4. Ethoprop 5. Naled 6. Phorate 7. Demeton- 8. Diazinon 9. Disulfoton 0. Ronnel. Parathion-methyl. Chlorpyrifos 50 C 00 C (0 min),.5 C/min. Trichloronate 4. Fenthion 5. Merphos 6. Stirofos 7. Tokuthion 8. Merphos oxidation product 9. Fensulfothion 0. Bolstar. Azinphos-methyl. Coumaphos Separation of organophosphorus pesticides (EPA 840 / 84) MN Appl. No min PTIMA δ-6 0. mm ID (0.4 mm D) 0.0 μm film mm ID (0.4 mm D) 0 m 5 m 0 m 50 m 60 m 0.0 μm film mm ID (0.4 mm D) 0.5 μm film mm ID (0.5 mm D) 0.5 μm film μm film μm film mm ID (0.8 mm D).00 μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. 0

23 PTIMA medium polar capillary columns PTIMA 0 6 % cyanopropyl-phenyl 94 % dimethylpolysiloxane USP G4 Midpolar phase Structure see page 07 Pesticide analysis For corresponding columns with higher film thickness see PTIMA 64 T max 00 C (long-term temperature), T max 0 C (short-term max. temperature in a temperature program) Similar phases HP-0, DB-0, SPB -0, Rtx -0, CP-0, Analysis of a pesticide mixture Analysis of a PCB mixture MN Appl. No. 060 MN Appl. No Column: PTIMA 0, 60 m x 0.5 mm ID, 0.5 μm fi lm Column: PTIMA 0, 60 m x 0.5 mm ID, 0.5 μm fi lm Injection: μl (0. ng/μl), 80 C ( min) 50 C ( min) Injection: μl (0. ng/μl), 80 C ( min) 50 C ( min) pulsed splitless pulsed splitless Carrier gas: He, 54 ml/min Carrier gas: He, 54 ml/min : 80 C ( min) 90 C, 0 C/min ( min) 40 C, C/min ( min) 60 C, 0 C/min (0 min) : 80 C ( min) 90 C, 0 C/min ( min) 40 C, C/min ( min) 60 C, 0 C/min (0 min) Detector: ECD Detector: ECD Peaks :. Propyzamide. Vinclozolin 5 Peaks :. PCB-8. PCB-5. Bromophos-ethyl 4.,4-DDT 4. PCB-8 4. PCB-5 5. Brompropylate 5. PCB-8 6. PCB min min PTIMA mm ID (0.4 mm D) 5 m 0 m 50 m 60 m 0.5 μm film mm ID (0.5 mm D) 0.5 μm film μm film mm ID (0.8 mm D).00 μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. Further applications can be found online in our application database at /apps

24 PTIMA medium polar capillary columns PTIMA 0 MS 6 % cyanopropyl-phenyl 94 % dimethylpolysiloxane USP G4 Chemically bonded, cross-linked silarylene phase with selectivity similar to 6 % cyanopropyl-phenyl 94 % dimethylpolysiloxane, symmetric substituted cyanopropylsilanes and integrated phenyl rings (silarylene) Midpolar phase with very low bleed Perfect deactivation Structure see page 07 Similar phases VF-0ms, Rxi -0Sil MS, TG-0MS Specially suitable for sophisticated environmental analysis (e.g., EPA methods for PAHs, PCBs and pesticides) 00 % ion trap and quadrupol MS compatibility T max 00 C (long-term temperature), T max 0 C (short-term max. temperature in a temperature program) PTIMA 0 MS 0.5 mm ID (0.4 mm D) 0 m 60 m 0.5 μm film mm ID (0.5 mm D) 0.5 μm film μm film mm ID (0.8 mm D).00 μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0.

25 PTIMA medium polar capillary columns PTIMA 64 6 % cyanopropyl-phenyl 94 % dimethylpolysiloxane USP G4 Midpolar phase Structure see page 07 Environmental analysis For corresponding columns with lower film thickness see PTIMA 0 T max 80 C (long-term temperature), T max 00 C (short-term max. temperature in a temperature program) Similar phases HP-64, HP-VC, DB-64, DB-VRX, SPB -64, CP-64, Rtx -64, Rtx -Volatiles, , BP64, VCL PTIMA 64 LB 6 % cyanopropyl-phenyl 94 % dimethylpolysiloxane Midpolar phase with low bleeding Structure see page 07 Halogenated hydrocarbons, volatiles, aromatic compounds, solvents etc. Column: Injection: Carrier gas: Solvents and semi-volatiles MN Appl. No. 50 PTIMA 64 LB, 0 m x 0. mm ID,.8 μm fi lm; retention gap Phe-Sil 0.5 m x 0.5 mm μl (0 ppm per substance in acetone), cold on-column. bar He : 45 C ( min) 50 C (6 C/min) 00 C (8 C/min), 0 min 00 C Detector: FID 80 C Peaks:. Acetone. Ethyl acetate. Tetrahydrofuran 4. Cyclohexane 5. -Methyl--butanol 6. -Butanol 7. Pyridine 8. Toluene 9. Dimethylformamide 0. Dimethylsulfoxide. Decane. -ctanol. Acetophenone 4. Butyrophenone 5. Heptanophenone 6. 5-Methoxyindole 7. Dibenzylamine 8. Methyl eicosanoate 9. Methyl cis--docosenoate 0. Methyl docosanoate min PTIMA mm ID (0.4 mm D).0 μm film mm ID (0.4 mm D) 5 m 0 m 50 m 60 m.40 μm film mm ID (0.5 mm D).80 μm film mm ID (0.8 mm D).00 μm film PTIMA 64 LB 0. mm ID (0.5 mm D).80 μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0.

26 PTIMA medium polar capillary columns PTIMA 70 4 % cyanopropyl-phenyl 86 % dimethylpolysiloxane USP G46 Midpolar phase, special selectivity due to high cyanopropyl content Structure see page 07 Reference column for structure identification, e.g., in combination with PTIMA 5 Film thickness μm for solvent analysis T max 80 C (long-term temperature), T max 00 C (short-term max. temperature in a temperature program) 0.5 mm ID: T max 80 and 00 C, resp. Similar phases V-70, DB-70, CP-Sil 9 CB, HP-70, Rtx -70, SPB -70, , BP0, ZB-70 Analysis of aromatic hydrocarbons MN Appl. No Column: PTIMA 70, 5 m x 0. mm ID, 0.5 μm fi lm Injection: μl, split :40 Carrier gas: 0.6 bar N : 60 C 0 C, 4 C/min Detector: FID 60 C 6 7 Peaks:. Benzene. Toluene. Ethylbenzene 4. p-xylene 5. o-xylene 6. Phenol 7. -Methylphenol 8.,6-Dimethylphenol 9. 4-Methylphenol 0.,4-Dimethylphenol.,4,6-Trimethylphenol min PTIMA mm ID (0.4 mm D) 0 m 5 m 5 m 0 m 50 m 60 m 0.0 μm film mm ID (0.4 mm D) 0.5 μm film μm film μm film mm ID (0.5 mm D) 0.5 μm film μm film μm film μm film mm ID (0.8 mm D).00 μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. Further applications can be found online in our application database at /apps 4

27 PTIMA medium polar capillary columns PTIMA 70 MS silarylene phase USP G46 Chemically bonded, cross-linked silarylene phase with selectivity similar to 4 % cyanopropyl-phenyl 86 % dimethylpolysiloxane, symmetric substituted cyanopropylsilanes and integrated phenyl rings (silarylene) Midpolar phase with very low bleed Perfect deactivation Structure see page 07 Similar phases Environmental analysis (e.g., PAHs, PCBs, pesticides) Reference column for structure identification, e.g., in combination with PTIMA 5 MS 00 % ion trap and quadrupole MS compatibility T max 80 C (long-term temperature), T max 00 C (short-term max. temperature in a temperature program) VF-70ms, TG-70MS, V-70, DB-70, HP-70, Rtx -70, SPB -70, CP Sil 9 CB, , BP0, ZB-70 Separation of triazine pesticides (EPA 69) MN Appl. No Column: PTIMA 70 MS, 0 m x 0.5 mm ID, 0.5 μm fi lm Injection: μl, 50 C, split : Carrier gas: 4 cm/s He : 60 C ( min) 80 C, 5 C/min 0 C, C/min Detector: MSD Peaks:. Prometon. Atraton. Propazine Atrazine 5. Simazine 6. Terbuthylazine 7. Secbumeton 8. Prometryn 9. Ametryn 0. Simetryn. Terbutryn min PTIMA 70 MS 0.5 mm ID (0.4 mm D) 0 m 60 m 0.5 μm film μm film μm film mm ID (0.5 mm D) 0.5 μm film μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. 5

28 PTIMA medium polar capillary columns PTIMA 5 MS silarylene phase USP G4 / close equivalent to USP G8 / G Chemically bonded cross-linked silarylene phase with selectivity similar to 5 % phenyl 65 % methyl polysiloxane, midpolar phase, polymer without CN groups Very low column bleeding Structure see page 09 Ideal for ion trap detectors ptimum column for confirmation of analytical results in combination with a MS or 5 MS All-round phase for environmental analysis, ultra trace analysis, EPA methods, pesticides, PCB, food and drug analysis T max 60 C (long-term temperature), T max 70 C (short-term max. temperature in a temperature program) Similar phases DB-5 MS, HP-5, SPB -5, Rxi -5SIL MS, Rtx-5, 007-5, BPX -5, MDN-5, AT -5 MS, ZB-5, V-, VF-5 MS Column: Injection: μl, split :0 PTIMA 5 MS, 0 m x 0.5 mm ID, 0.5 μm fi lm Carrier gas: 0.6 bar H : 00 C ( min) 00 C (0 min), 6 C/min Detector: MSD PAH in accordance with EPA 60 MN Appl. No. 90 Peaks. Naphthalene. Acenaphthylene. Acenaphthene 4. Fluorene 5. Phenanthrene 6. Anthracene 7. Fluoranthene 8. Pyrene 9. Benz[a]anthracene 0. Chrysene. Benzo[b]fl uoranthene. Benzo[k]fl uoranthene. Benzo[a]pyrene 4. Indeno[,,-cd]pyrene 5. Dibenz[ah]anthracene 6. Benzo[ghi]perylene min PTIMA 5 MS 0.5 mm ID (0.4 mm D) 0 m 60 m 0.5 μm film mm ID (0.5 mm D) 0.5 μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. Further applications can be found online in our application database at /apps 6

29 PTIMA medium polar capillary columns PTIMA 7 phenylmethylpolysiloxane (50 % phenyl) USP G Midpolar phase Structure see page 09 Steroids, pesticide, drug analysis T max 0 C (long-term temperature), T max 40 C (short-term max. temperature in a temperature program) 0.5 mm ID: T max 00 and 0 C resp. Similar phases V-7, DB-7, HP-50+, HP-7, SPB -50, SP-50, Rxi -7, Rtx -50, CP-Sil 4 CB, 007-7, ZB-50 Analysis of pesticides MN Appl. No Column: PTIMA 7, 5 m x 0. mm ID, 0.0 μm fi lm Sample: pesticides, standard of the cantonal laboratory Schaffhausen (Switzerland), 0. mg/ml or 0.0 mg/ml each Injection:.0 μl, s without split Carrier gas: He, 5 cm/s : 00 C ( min), 8 C/min 50 C, 0 C/min 0 C Detector: MSD HP Peaks:. Dichlorphos. Naled. Vinclozolin 4. Chlorthalonil 5. Chlorpyrifos 6. Dichlofl uanid 7. Procymidon 8. Captan 9. Folpet 0. Carbophenothion. Iprodion. Captafol. Coumaphos min PTIMA 7 0. mm ID (0.4 mm D) 0.0 μm film mm ID (0.4 mm D) 0 m m 5 m 5 m 0 m 50 m 60 m 0.0 μm film μm film mm ID (0.4 mm D) 0.5 μm film μm film μm film mm ID (0.5 mm D) 0.5 μm film μm film μm film μm film mm ID (0.8 mm D).00 μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. 7

30 PTIMA polar capillary columns PTIMA 7 MS silarylene phase USP G Medium polar silarylene phase with selectivity analogue to 50 % phenyl 50 % methylpolysiloxane, no CN groups in the polymer Structure see page 09 Ideal for ion trap detectors ptimum reference column in combination with a MS or 5 MS All-round phase for environmental analysis, ultra-trace analysis, EPA methods, pesticide, PCBs, food and drug analysis T max 40 C (long-term temperature), T max 60 C (short-term max. temperature in a temperature program) Similar phases V-7, AT -50, BPX -50, DB-7, DB-7ms, HP-50+, HP-7, SPB -50, SPB -7, SP-50, Rtx -50, CP-Sil 4 CB, 007-7, VF-7ms, ZB-50 Column: Sample: phenol mix 604 PTIMA 7 MS, 0 m x 0.5 mm ID, 0.5 μm fi lm Injection:.0 μl, 0 C, split :0 Carrier gas: 0.8 bar He : 00 C, 0 C/min 50 C Detector: FID 80 C Peaks:. Phenol. -Chlorophenol.,4-Dimethylphenol 4. -Nitrophenol 5.,4-Dichlorophenol 6. 4-Chloro--methylphenol 7.,4,6-Trichlorophenol 8. 4-Nitrophenol 9.,4-Dinitrophenol 0. -Methyl-4,6-dinitrophenol. Pentachlorophenol Analysis of phenols MN Appl. No min PTIMA 7 MS 0.5 mm ID (0.4 mm D) 0 m 60 m 0.5 μm film mm ID (0.5 mm D) 0.5 μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. Further applications can be found online in our application database at /apps 8

31 PTIMA polar capillary columns PTIMA 0 trifluoropropyl-methylpolysiloxane (50 % trifluoropropyl) close equivalent to USP G6 Midpolar phase Structure see page 09 Similar phases V-0, DB-0, Rtx -00, Environmental analysis, especially for o-, m- and p-substituted aromatic hydrocarbons T max 60 C (long-term temperature), T max 80 C (short-term max. temperature in a temperature program) Aromatic hydrocarbons (BTX) MN Appl. No. 000 Column: PTIMA 0, 50 m x 0.5 mm ID, 0.5 μm fi lm Injection: 0.5 μl, split 05 ml/min Carrier gas: 0 kpa N (. ml/min) : 50 C Detector: FID 50 C Peaks:. Benzene. Toluene. Ethylbenzene 4. p-xylene 5. m-xylene 6. o-xylene min PTIMA mm ID (0.4 mm D) 5 m 5 m 0 m 50 m 60 m 0.5 μm film μm film mm ID (0.5 mm D) 0.5 μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. 9

32 PTIMA polar capillary columns PTIMA 5 50 % cyanopropyl-methyl 50 % phenylmethylpolysiloxane close equivalent to USP G7 / G9 Midpolar phase Structure see page 09 Similar phases V-0, DB-0, Rtx -00, Fatty acid analysis T max 60 C (long-term temperature), T max 80 C (short-term max. temperature in a temperature program) Column: Injection: μl, split :40 PTIMA 5, 5 m x 0. mm ID, 0.5 μm fi lm Analysis of FAME in porcine fat MN Appl. No Carrier gas: 60 kpa H : 50 C ( min) 5 C, 0 C/min 60 C, 5 C/min 80 C, 0 C/min 00 C, C/min 0 C, 0 C/min (0 min) Detector: FID 60 C Peaks:. C4:0. C5:0. C6:0 4. C8:0 5. C0:0 6. C:0 7. C:0 8. C:0 9. C: 0. C4:0. C4:. C5:0. C5: 4. C6:0 5. C6: 6. C7:0 7. C7: 8. C8:0 9. C8: 0. C8:. C8:. C9:0. C0:0 4. C0: 5. C0: 6. C0:4 7. C0: 8. C0:5 9. C:0 0. C:. C:. C:6. C4:0 4. C4: FAME Standard FAME in porcine fat min min Courtesy of Dr. Bantleon, Mr. Leusche, Mr. Hagemann, VFG-Labor, Versmold, Germany PTIMA 5 0. mm ID (0.4 mm D) 0.0 μm film mm ID (0.4 mm D) 0 m 5 m 5 m 0 m 50 m 60 m 0.5 μm film mm ID (0.5 mm D) 0.5 μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. 0

33 PTIMA polar capillary columns PTIMA 40 % cyanopropyl-methyl 67 % dimethylpolysiloxane Midpolar phase Structure see page 09 FAMEs, dioxins T max 60 C (long-term temperature), T max 80 C (short-term max. temperature in a temperature program) Column: Sample: PTIMA 40, 60 m x 0.5 mm ID, 0.5 μm fi lm FAME mixture Injection:.0 μl, split :5 Carrier gas: 50 kpa H : 80 C 0 C, 0 C/min 60 C (0 min), C/min Detector: FID 80 C Fatty acid methyl esters cis/trans C8: (FAME) MN Appl. No. 060 Peaks:. C4:0. C5:0. C8:0 4. C0:0 5. C:0 6. C:0 7. C:0 8. C4:0 9. C4: 0. C5:0. C5:. C6:0. C6: 4. C7:0 5. C7: 6. C8:0 7. trans-c8: 8. cis-c8: 9. C8: 0. C8:. C8:. C0:0. C0: 4. C0: 5. C0: 6. C0:4 7. C0: 8. C:0 9. C: 0. C:. C4: min PTIMA mm ID (0.4 mm D) 5 m 0 m 50 m 60 m 0.5 μm film μm film mm ID (0.5 mm D) 0.5 μm film μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. Further applications can be found online in our application database at /apps

34 PTIMA polar capillary columns PTIMA WAX polyethylene glycol Da USP G6 Polar phase Structure see page 09 Solvent analysis and alcohols, suitable for aqueous solutions T max 40 C (long-term temperature), T max 50 C (short-term max. temperature in a temperature program) 0.5 mm ID: T max 0 and 40 C resp. Similar phases PERMABND CW 0 M (see page 7), DB-Wax, Supelcowax, HP-Wax, HP-INNWAX, Rtx-Wax, CP-Wax 5 CB, Stabilwax, 007-CW, BP0, AT-Wax, ZB-Wax Modified Grob test MN Appl. No. 70 Column: PTIMA WAX, 50 m x 0. mm ID, 0.5 μm fi lm Injection: μl, split :0 Carrier gas:, bar He : 80 C 50 C, 8 C/min Detector: FID 50 C Peaks: 5. Decane. Undecane. ctanol 4. Methyl decanoate 5. Dicyclohexylamine 6. Methyl undecanoate 7. Methyl dodecanoate 8.,6-Dimethylaniline 9.,6-Dimethylphenol min PTIMA WAX 0.5 mm ID (0.4 mm D) 5 m 0 m 50 m 60 m 0.5 μm film mm ID (0.5 mm D) 0.5 μm film μm film mm ID (0.8 mm D).00 μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. Further applications can be found online in our application database at /apps

35 PTIMA polar capillary columns PTIMA WAXplus cross-linked polyethylene glycol USP G6 Polar phase with improved cross-linking for lower column bleed and better temperature stability Structure see page 09 Broad range of application, e.g., for solvents and alcohols, suitable for aqueous solutions T max 60 C (long-term temperature), T max 70 C (short-term max. temperature in a temperature program) Similar phases DB-Wax, Supelcowax, HP-Wax, HP-INNWAX, Rtx-Wax, CP-Wax 5 CB, Stabilwax, 007-CW, BP0, AT-Wax, ZB-Wax Alcohols MN Appl. No. 460 Column: PTIMA WAXplus, 0 m x 0.5 mm ID, 0.5 μm fi lm Injection: 0. μl, split :80 Carrier gas:. bar He : 40 C 60 C, C/min (5 min) Detector: FID 60 C Peaks:. Methanol. -Propanol. Ethanol 4. -Propanol 5. -Methyl--propanol 6. -Butanol 7. 4-Methyl--pentanol 8. -Pentanol 9. -Methyl--pentanol 0. -Hexanol. Cyclohexanol. -Heptanol 4 8 min PTIMA WAXplus 0.5 mm ID (0.4 mm D) 0 m 60 m 0.5 μm film μm film mm ID (0.5 mm D) 0.5 μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0.

36 PTIMA polar capillary columns PTIMA FFAP polyethylene glycol -nitroterephthalate USP G5 / close equivalent to USP G5 Polar phase (FFAP = Free Fatty Acid Phase) Structure see page 09 Fatty acid methyl esters (FAMEs), free carboxylic acids mm ID: T max 50 C (long-term temperature), T max 60 C (short-term max. temperature in a temperature program) 0.5 mm ID: T max 0 and 40 C, resp. Similar phases PERMABND FFAP (see page 8), DB-FFAP, HP-FFAP, CP-Wax 58 FFAP CB, 007-FFAP, CP-FFAP CB, Nukol, AT-000, SPB-000, BP, V-5 FAME test MN Appl. No. 40 Column: PTIMA FFAP, 60 m x 0. mm ID, 0.5 μm fi lm Injection:.0 μl, 0 C, split :40 Carrier gas:. bar He : 55 C 50 C, 6 C/min Detector: FID 0 C Peaks:. C4. C6. C8 4. C0 5. C 6. C4 7. C6 8. C8 9. C8: cis/trans 0. C8:. C8:. C0. C 4. C: 5. C min PTIMA FFAP 0. mm ID (0.4 mm D) 0.0 μm film mm ID (0.4 mm D) 0 m 5 m 0 m 50 m 60 m 0.5 μm film mm ID (0.5 mm D) 0.5 μm film μm film mm ID (0.8 mm D) 0.50 μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. 4

37 PTIMA polar capillary columns PTIMA FFAPplus polyethylene glycol -nitroterephthalate USP G5 / close equivalent to G5 Polar phase Structure see page 09 FAMEs, free carboxylic acids T max 50 C (long-term temperature), T max 60 C (short-term max. temperature in a temperature program) Similar phases DB-FFAP, HP-FFAP, CP-SIL 58 CB, 007-FFAP, CP-FFAP CB, Nukol FAMEs from biodiesel MN Appl. No Column: PTIMA FFAPplus, 0 m x 0.5 mm ID, 0.5 μm fi lm Injection: μl, 60 C, split :5 9 Carrier gas: 40 cm/s He : 70 C ( min) 40 C, 0 C/min (0 min) Detector: MS-EI, ion source 00 C, interface temperature 50 C Peaks: Methyl esters of:. Caproic acid (C6:0) Caprylic acid (C8:0). Capric acid (C0:0) 4. Lauric acid (C:0) 7 5. Myristic acid (C4:0) 6. Palmitic acid (C6:0) 7. Palmitoleic acid (C6:) 8. Stearic acid (C8:0) 9. leic acid (C8: cis) 0. Linoleic acid (C8: cis) 0 4. Nonadecanoic acid (C9:0). Linolenic acid (C8:) 5. Arachidic acid (C0:0) 4. Behenic acid (C:0) 5. Erucic acid (C: cis) 6. Lignoceric acid (C4:0) Nervonic acid (C4: cis) min PTIMA FFAPplus 0.5 mm ID (0.4 mm D) 0 m 60 m 0.5 μm film μm film mm ID (0.5 mm D) 0.5 μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. Further applications can be found online in our application database at /apps 5

38 PERMABND capillary columns PERMABND SE-0 00 % dimethylpolysiloxane USP G / G / G8 Nonpolar phase T max 00 C (long-term temperature), T max 0 C (short-term max. temperature in a temperature program) Similar phases PTIMA (see page 0) PERMABND SE mm ID (0.4 mm D) 5 m 50 m 0.5 μm film mm ID (0.5 mm D) 0.5 μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. PERMABND SE-5 5 % phenyl 95 % dimethylpolysiloxane USP G7 Nonpolar phase T max 00 C (long-term temperature), T max 0 C (short-term max. temperature in a temperature program) Similar phases PTIMA 5 (see page 4) PERMABND SE mm ID (0.4 mm D) 5 m 0.5 μm film mm ID (0.5 mm D) 0.5 μm film μm film 7.5 In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. 6

39 PERMABND capillary columns PERMABND CW 0 M polyethylene glycol Dalton USP G6 Polar phase Similar phases See PTIMA WAX (see page ) Solvent analysis and alcohols, suitable for aqueous solutions mm ID: T max 0 C (long-term temperature), T max 40 C (short-term max. temperature in a temperature program) 0.5 mm ID: T max 00 and 0 C, resp. PERMABND CW 0 M 0. mm ID (0.4 mm D) 0.0 μm film mm ID (0.4 mm D) 0 m 5 m 0 m 50 m 60 m 0.5 μm film mm ID (0.5 mm D) 0.5 μm film μm film μm film mm ID (0.8 mm D) 0.50 μm film μm film μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. Further applications can be found online in our application database at /apps 7

40 PERMABND capillary columns PERMABND FFAP polyethylene glycol -nitroterephthalate USP G5 / close equivalent to G5 Polar phase Similar phases See PTIMA FFAP (see page 4) FAMEs, free carboxylic acids mm ID: T max 0 C (long-term temperature), T max 40 C (short-term max. temperature in a temperature program) 0.5 mm ID: T max 00 and 0 C, resp. PERMABND FFAP 0. mm ID (0.4 mm D) 0 m 0 m 5 m 0 m 50 m 60 m 0.0 μm film μm film mm ID (0.4 mm D) 0.0 μm film μm film mm ID (0.5 mm D) 0.0 μm film μm film μm film μm film mm ID (0.8 mm D).00 μm film In addition to this standard program we will be happy to supply columns custom-made to your specifications. Information about scope of delivery, special cages and integrated guard columns see additional information for GC columns on page 0. Further applications can be found online in our application database at /apps 8

41 Special GC columns overview Capillary columns for special GC separations Certain analytical separations can be accomplished more easily with chromatographic columns, that have been especially developed for that task, compared with standard columns. The following table summarizes our program of GC speciality capillaries, the individual columns will be described in detail on the following pages. verview Separation/special application Recommended capillary column Page Fast GC column with 0.0 mm ID Enantiomer separation cyclodextrin phases Biodiesel PTIMA, PTIMA 5, PTIMA δ-, PTIMA δ-6 PTIMA 7, PTIMA 5, PTIMA FFAP PERMABND CW 0 M, PERMABND FFAP FS-LIPDEX A, FS-LIPDEX B, FS-LIPDEX C FS-LIPDEX D, FS-LIPDEX E, FS-LIPDEX G FS-HYDRDEX β-pm, FS-HYDRDEX β- P, FS-HYDRDEX β-6tbdm, FS-HYDRDEX β-6tbde, FS-HYDRDEX β-6tbde, FS-HYDRDEX β-tbdac, FS-HYDRDEX γ-dimm Methanol analysis PTIMA BioDiesel M 46 FAME analysis PTIMA BioDiesel F 46 Glycerol and triglycerides PTIMA BioDiesel G 46 Triglycerides High temperature GC Amines PTIMA -TG 48 PTIMA 7-TG 48 PTIMA 5 HT 49 Polyfunctional amines PTIMA 5 Amine 50 Amine separations FS-CW 0 M-AM 5 Petrochemical products (complex hydrocarbon mixtures) Environmental analysis of volatile halogenated hydrocarbons Silanes (monomeric, e.g., chlorosilanes) Diethylene glycol, e.g., for the quality control of wine PERMABND P-00 5 PERMABND SE-54 HKW 5 PERMABND Silane 54 PERMABND CW 0 M-DEG

42 Capillary columns for Fast GC 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 programs can reduce the analysis time by up to 80 % High sensitivity detectors with small volume and very short response time, as well as very rapid data acquisition and processing Small inner diameters result in high column inlet pressures and a lower volume flow of the mobile phase: very fast injection of very small samples against a high pressure Amount of sample, which can be injected, is limited by the inner diameter and the thin film High heating rates place special demands on stationary phases. PTIMA columns meet exactly this requirement: very low bleeding, long lifetimes, even for continuous high heating rates Comparison of a separation on a 50 m standard capillary with separation on a 0 m fast GC column MN Appl. No. 60 Peaks:. ctanol. Undecane. Dimethylaniline 4. Dodecane 5. Decylamine A) Fast GC column Column: PTIMA 5, 0 m x 0. mm ID, 0. μm fi lm Injection μl, split :40, Carrier gas 0.75 bar He B) standard GC column Column: PTIMA 5, 50 m x 0.5 mm ID, 0.5 μm fi lm Injection μl, split :5, Carrier gas.5 bar He 6. Methyl decanoate 7. Methyl undecanoate 8. Henicosane 9. Docosane 0. Tricosane Both separations: min min : 80 C 0 C (0 min), 8 C/min Detector: FID While maintaining the temperature program and halving the pressure a time saving of 0 % results with identical separation effi ciency. 40

43 Capillary columns for Fast GC Columns for Fast GC Phase Maximum temperature ID [mm] Film thickness [μm] REF (0 m) REF (0 m) PTIMA 40 / 60 C PTIMA 5 40 / 60 C PTIMA δ- 40 / 60 C PTIMA δ-6 40 / 60 C PTIMA 7 0 / 40 C PTIMA 5 60 / 80 C PTIMA FFAP 50 / 60 C PERMABND CW 0 M 0 / 40 C PERMABND FFAP 0 / 40 C PTIMA 5 Amine 00 / 0 C FS-CW 0 M-AM 0 / 40 C FS-LIPDEX E 00 / 0 C FS-HYDRDEX β-6tbdm 0 / 50 C In addition to this standard program, all MN GC phases can be custom-made as fast GC columns Further applications can be found online in our application database at /apps 4

44 Capillary columns for enantiomer separation LIPDEX cyclodextrin phases for enantiomer separation Base material: cyclic oligosaccharides consisting of six (α-cyclodextrin), seven (β-cyclodextrin) or eight (γ-cyclodextrin) glucose units bonded through,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 analysis Important advantage: many compounds can be analyzed without derivatization (however, for certain substances enantioselectivity can be favorably 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 following table shows typical applications. Note: Water as solvent is strictly forbidden for all cyclodextrin phases Dry the sample with our CHRMAFIX Dry (Na S 4 ) cartridges (see page 6) Use suitable nonpolar solvent Phase Cyclodextrin derivate T max [ C] LIPDEX A LIPDEX B LIPDEX C LIPDEX D LIPDEX E LIPDEX G hexakis-(,,6-tri--pentyl)-α-cd 00 / 0 carbohydrates, polyols, diols, hydroxycarboxylic acid esters, (epoxy-) alcohols, glycerol derivatives, spiroacetals, ketones, alkyl halides hexakis-(,6-di--pentyl---acetyl)-α-cd 00 / 0 lactones, diols (cyclic carbonates), aminols, aldols (-TFA), glycerol derivatives (cyclic carbonates) heptakis-(,,6-tri--pentyl)-β-cd 00 / 0 Alcohols, cyanhydrins, olefins, hydroxycarboxylic acid esters, alkyl halides heptakis-(,6-di--pentyl---acetyl)-β-cd 00 / 0 aminols (TFA), β-amino acid esters, trans-cycloalkane-,-diols, trans-cycloalkane-,- diols, trans-cycloalkane-,-diols (TFA) octakis-(,6-di--pentyl---butyryl)-γ-cd 00 / 0 α-amino acids, α- and β-hydroxycarboxylic acid esters, alcohols (TFA), diols (TFA), ketones, pheromones (cyclic acetals), amines, alkyl halides, lactones octakis-(,-di--pentyl-6--methyl)-γ-cd 0 / 40 menthol isomers, ketones, alcohols, carboxylic acid esters, terpenes 0 m 0.0 mm ID FS-LIPDEX A FS-LIPDEX B FS-LIPDEX C FS-LIPDEX D FS-LIPDEX E FS-LIPDEX G All columns with 0.4 mm D 5 m 0.5 mm ID 50 m 0.5 mm ID

45 Capillary columns for enantiomer separation Column: Enantiomer separation of amino acid methyl esters (TFA) MN Appl. No. 059 FS-LIPDEX E, 5 m x 0.5 mm ID Injection: μl, split ~ : 00 Carrier gas: 60 kpa H : C, 4 C/min Detector: FID 50 C Separation of chiral constituents of peppermint oil MN Appl. No W. A. König et al., High Resol. Chromatogr. 0 (997) 55 6 Column: Carrier gas: 50 kpa H : 75 C, isothermal Detector: FS-LIPDEX G, 5 m x 0.5 mm ID FID Peaks: (D is eluted before L except for proline: L before D). Alanine. Valine. Leucine 4. Proline 5. Aspartic acid 6. Phenylalanine Peaks:. (+)-trans-sabinene hydrate. (+)-Menthone. (+)-Isomenthone 4. ( )-Menthone 5. ( )-Isomenthone 6. (+)-Menthofuran 7. ( )-Isopulegol 8. ( )-Menthyl acetate 9. (+)-Pulegone 4 0. (+)-Neomenthol. ( )-Neomenthol. (+)-Neoisomenthol. (+)-Menthol 4. ( )-Neoisomenthol 5. (+)-Piperitone 6. ( )-Menthol 7. (+)-Isomenthol 8. ( )-Isomenthol min Mentha arvensis (China) Cyclodextrin derivates 8 R 6 R R R 6 R R R R 6 R n R R R 6 R R 5 Mentha piperita (Idaho) Standard min R 6 R R R 6 Further applications can be found online in our application database at /apps 4

46 Capillary columns for enantiomer separation HYDRDEX cyclodextrin phases for enantiomer separation Cyclodextrin derivatives (see page 4) with high melting point: for GC enantiomer separation diluted with polysiloxanes Enantiomer separation of dichlorprop methyl ester MN Appl. No. 054 Column: FS-HYDRDEX β-p, 5 m x 0.5 mm ID Injection: 0. μl (~ % in CH Cl ), split 0 ml/min Carrier gas: 60 kpa H (.9 ml/min) : 60 C Detector: FID 50 C Separation of isomeric antiinflammatory drugs MN Appl. No. 050 Courtesy of Prof. W.A. König, Hamburg, Germany Column: FS-HYDRDEX β-6tbdm, 5 m x 0.5 mm ID Carrier gas: He : 5 C 00 C, C/min Detector: FID Peaks:. Ibuprofen H C CH 4. Naproxen CH Cl Cl CH C. Flurbiprofen. Fenoprofen F CH 5. Ketoprofen H H C CH min S R min Phase HYDRDEX β-pm HYDRDEX β-p HYDRDEX β-6tbdm HYDRDEX β-6tbde HYDRDEX β-tbdac HYDRDEX γ-tbdac HYDRDEX γ-dimm Cyclodextrin derivative (diluted with optimized polysiloxane) T max [ C] heptakis-(,,6-tri--methyl)-β-cd 0 / 50 hydroxycarboxylic acid esters, alcohols, diols, olefins, lactones, acetals heptakis-(,6-di--methyl---pentyl)-β-cd 0 / 50 terpenes, dienes, allenes, terpene alcohols,,-epoxyalkanes, carboxylic acids (esters), hydroxycarboxylic acid esters, pharmaceuticals, pesticides heptakis-(,-di--methyl-6--t-butyldimethyl-silyl)-β-cd 0 / 50 γ-lactones, cyclopentanones, terpenes, esters, tartrates heptakis-(,-di--ethyl-6--t-butyldimethyl-silyl)-β-cd 0 / 50 essential oils heptakis-(,-di--acetyl-6--t-butyldimethyl-silyl)-β-cd 0 / 40 alcohols, esters, ketones, aldehydes, δ-lactones octakis-(,-di--acetyl-6--t-butyldimethyl-silyl)-γ-cd 0 / 40 cyclic ketones, aromatic ketones, oxiranes, aromatic esters, aromatic amides octakis-(,-di--methoxymethyl-6--t-butyldimethylsilyl)-γ-cd 0 / 40 ketones, terpenes, cyclic ethers, alcohols, amines 44

47 Capillary columns for enantiomer separation Column: Injection: Separation of (R/S) citronellol + citronellal MN Appl. No. 440 FS-HYDRDEX β-tbdac, 50 m x 0.5 mm ID μl, :000 in CH Cl, split 5 ml/min Separation of essential oils MN Appl. No. 980 / 990 / 000 Column: FS-HYDRDEX γ-tbdac, 50 m x 0.5 mm ID Injektor: 0 C Carrier gas:.5 bar H : 00 C Detector: FID 0 C Carrier gas:. bar H : 5 C Detector: FID 0 C Peaks:. (R)/(S)-Citronellal. (S)/(R)-Citronellal. (S)-Citronellol 4. (R)-Citronellol Peaks:. Fenchone (.5 mg/ml). Menthone (0.5 mg/ml). Menthol ( mg/ml) H min min HYDRDEX FS-HYDRDEX β-pm FS-HYDRDEX β-p FS-HYDRDEX β-6tbdm FS-HYDRDEX β-6tbde FS-HYDRDEX β-tbdac FS-HYDRDEX γ-tbdac FS-HYDRDEX γ-dimm All columns with 0.4 mm D 0 m 0.0 mm ID 5 m 0.5 mm ID 50 m 0.5 mm ID Further applications can be found online in our application database at /apps 45

48 Capillary columns for biodiesel analysis PTIMA BioDiesel for the analysis of biodiesel (DIN EN 44 / ASTM D 675) PTIMA BioDiesel M for analysis of methanol in accordance with DIN EN 40 The methanol content in biodiesel as specified in DIN EN 40 must not exceed 0. %. The column PTIMA Bio- Diesel M allows the GC headspace analysis of the methanol content in biodiesel in the concentration range from 0.0 to 0.5 % with -propanol as internal standard. T max 40 C (long-term temperature), T max 60 C (short-term max. temperature in a temperature program) Similar phases Select Biodiesel for Methanol, Trace TR-BioDiesel (M) PTIMA BioDiesel F for analysis of FAMEs in accordance with DIN EN 40:0 The analysis of biodiesel requires separation of typical FAMEs between myristic acid (C 4 ) and nervonic acid (C 4 :) methyl esters. This analysis is possible on PTIMA BioDiesel F in only min. Additionally, linolenic acid methyl ester can be determined due to the good resolution. The extended standard DIN EN 40:0 also covers smaller FAMEs starting from C 6 (see application 450 on opposite page). Change of the internal standard from C 7 to C 9 also allows the analysis of animal fats. T max 40 C (long-term temperature), T max 50 C (short-term max. temperature in a temperature program) Similar phases Select Biodiesel for FAME, Trace TR-BioDiesel (F) PTIMA BioDiesel G for analysis of glycerol and glycerides in accordance with DIN EN 405 The capillary column PTIMA BioDiesel G allows determination of free glycerol and residues of mono-, di- and triglycerides in FAMEs intended as additives for mineral oils. The procedure can be applied for FAMEs from rapeseed oil, sunflower oil and soy bean oil. Glycerol as well as monoand diglycerides are derivatized to more volatile substances by addition of MSTFA in the presence of pyridine (see page 6). T max 80 C (long-term temperature), T max 400 C (short-term max. temperature in a temperature program) Similar phases Select Biodiesel for Glycerides, Trace TR-BioDiesel (G), MET-Biodiesel 46

49 Capillary columns for biodiesel analysis Column: Sample: PTIMA BioDiesel F, 0 m x 0.5 mm ID 50 μg/ml each in dichloromethane Injection: 0 μl, 50 C, split :0 Carrier gas: :. bar He Detector: FID 60 C Peaks:. C6:0. C8:0. C0:0 4. C:0 5. C4:0 6. C6:0 7. C6: 8. C8:0 80 C 50 C (8.5 min), 0 C/min 9. C8: 0. C8: Analysis of FAMEs from biodiesel in accordance with DIN EN 40:0. C9:0, int. st.. C8:. C0:0 4. C:0 5. C: 6. C4:0 MN Appl. No min Analysis of glycerol and glycerides from biodiesel MN Appl. No. 640 Column: PTIMA BioDiesel G, 0 m x 0.5 mm ID Sample: A) standard in n-heptane B) biodiesel Injection: μl, 50 C, CIS (5 C 50 C, C/s) Carrier gas: 0.8 bar H, split :.6 : 50 C (.5 min) 80 C, 5 C/min 4 80 C, 7 C/min 70 C (0 min), 0 C/min Detector: FID 80 C 5 6 Peaks:. Glycerol (TMS). Butanetriol (TMS), IS. Monoolein = glycerol monooleate (TMS) + monoacylglycerides 4. Tricaprin (glycerol tricaprate), IS 5. Diolein = glycerol dioleate (TMS) + diacylglycerides 6. Triolein = glycerol trioleate + triacylglycerides A B min PTIMA BioDiesel PTIMA BioDiesel M 0 m 0 m 0. mm ID (0.5 mm D) PTIMA BioDiesel F 0.5 mm ID (0.4 mm D) PTIMA BioDiesel G 0.5 mm ID (0.4 mm D)

50 Capillary columns for triglyceride analysis PTIMA -TG 7-TG for triglyceride analysis USP G / G / G8 (-TG) USP G (7-TG) Short capillary columns (max. 5 m and 0. mm ID) with low-bleeding stationary phases thermally stable with optimized deactivation Similar phases der PTIMA -TG: SPB- TG, DB- HT, 400- HT, HT-5 PTIMA -TG 00 % dimethylpolysiloxane offers separation according to carbon number PTIMA 7-TG phenyl-methyl-polysiloxane (50 % phenyl) for separation according to degree of unsaturation T max 70 C (both phases) Column: Injection: PTIMA -TG, 5 m x 0. mm ID 0.5 μl Triglycerides (from butter) MN Appl. No Carrier gas: 80 kpa H : 80 C ( min) 50 C, 0 C/min 70 C (0 min), 5 C/min Detector: FID 80 C 7 Peaks:. Cholesterol. T-0. T-4 4. T-8 5. T-4 6. T T T C min PTIMA -TG PTIMA 7-TG PTIMA -TG 0 m 5 m 0.5 mm ID (0.4 mm D) mm ID (0.5 mm D) PTIMA 7-TG 0. mm ID (0.5 mm D)

51 Capillary columns for high temperature GC PTIMA 5 HT for high temperature GC USP G7 / G6 Chemically bonded, cross-linked silarylene phase with polarity similar to a 5 % diphenyl - 95 % dimethylpolysiloxane phase Nonpolar phase, low bleeding Similar phases DB-5HT, VF-5HT, HT-5, XTI-5HT, ZB-5HT Ideal for MS detectors, can be rinsed with solvents For simulated distillation, hydrocarbon, fuel and oil analysis, high-boiling analytes T max 80 C (long-term temperature), T max 400 C (short-term max. temperature in a temperature program) Column: Sample: PTIMA 5 HT, 5 m x 0. mm ID, 0.5 μm fi lm Separation of motor oil / mineral oil (type A + B), rapid determination in accordance with DIN H-5 / IS DIS MN Appl. No. 400 mineral oil type A + B (hydrocarbon index kit acc. to EN IS 977-) in hexane Injection: μl, splitless, 00 C Carrier gas: : 0.6 bar He Detector: FID 80 C 40 C (5 min) 90 C, 50 C/min Peaks:. Decane (C0). Tetracontane (C40) min PTIMA 5 HT 0.5 mm ID (0.4 mm D) 5 m 0 m 0.0 μm film μm film mm ID (0.5 mm D) 0.0 μm film μm film Further applications can be found online in our application database at /apps 49

52 Capillary columns for amine separation PTIMA 5 Amine special column for analysis of amines USP G7 / G6 Nonpolar phase Improved linearity for analysis of active components at trace levels: no amine absorptions even for aliphatic and aromatic amines at concentrations of 00 pg/peak Tested with the PTIMA Amine test mixture (REF 77), which contains, amongst others, diethanolamine and propanol-pyridine (this test mixture is supplied with each column) Similar phases Rtx -5 Amine, PTA-5 Especially deactivated for the analysis of polyfunctional amines such as ethanolamines, amino-functionalized diols and similar compounds, which are important base materials in industrial chemistry, and show strong tailing on standard-deactivated columns T max 00 C (long-term temperature), T max 0 C (short-term max. temperature in a temperature program) Column: PTIMA 5 Amine, 0 m x 0.5 mm ID,.0 μm fi lm Separation of secondary and tertiary amines MN Appl. No Injection: μl, split :00 Carrier gas: 0.6 bar H : 00 C ( min) 80 C, 0 C/min Detector: FID 80 C 5 Peaks:. Diethylamine. Di-isopropylamine. Triethylamine 4. Di-n-propylamine 5. Di-n-butylamine 6. Tri-n-propylamine 7. Di-isobutylamine 8. Tri-n-butylamine 9. Di-isohexylamine 0. Dicyclohexylamine. Dibenzylamine. Tri-n-hexylamine min PTIMA 5 Amine 0. mm ID (0.4 mm D) 0.40 μm film mm ID (0.4 mm D) 0 m 5 m 0 m 0.5 μm film mm ID (0.4 mm D) 0.50 μm film μm film mm ID (0.5 mm D) 0.5 μm film μm film μm film mm ID (0.8 mm D).00 μm film μm film

53 Capillary columns for amine separation FS-CW 0 M-AM polyethylene glycol 0 000, non-immobilized USP G6 Polyethylene glycol, basic for amine separations T max 0 C (long-term temperature), T max 40 C (short-term max. temperature in a temperature program) Similar phases Carbowax Amine, CP-Wax 5, CAM, Stabilwax DB FS-CW 0 M-AM 0. mm ID (0.4 mm D) 0.5 μm film mm ID (0.4 mm D) 0 m 5 m 50 m 0.5 μm film mm ID (0.5 mm D) 0.5 μm film μm film mm ID (0.8 mm D).00 μm film Further applications can be found online in our application database at /apps MACHEREY-NAGEL CHRMAFIL syringe filters Ideal for the filtration of GC, HPLC and UHPLC sample solutions Diverse membrane types and fi lter sizes for a variety of applications ptimal fl ow geometry because of star-shaped distribution device Lowest content of extractable substances Luer lock inlet, Luer outlet Prefi ltration of solvents protects sensitive instrument parts and chromatography columns from solid contamination and increases their lifetime. Find CHRMAFIL products from page 8 onwards. 5

54 Capillary columns for hydrocarbons PERMABND P-00 for analysis of petrochemical products USP G / G / G8 Extra long column with nonpolar dimethylpolysiloxane phase High resolution and sufficient capacity for analysis of complex mixtures of hydrocarbons T max 00 C (long-term temperature), T max 0 C (short-term max. temperature in a temperature program) PERMABND P mm ID (0.4 mm D) 00 m 0.50 μm film PERMABND SE-54-HKW for volatile halogenated hydrocarbons USP G6 SE-54 optimized for volatile halogenated hydrocarbons For the analysis of halogenated hydrocarbons, we recommend our optimized column PERMABND SE-54-HKW at 5 or 50 m length with our approved polysiloxane phase SE-54. As an alternative, or to verify analytical results, the PTIMA 64 has proven itself as advantageous, especially for the determination of,,-trichlorotrifluoroethane (F ) along with dichloromethane. T max 00 C (long-term temperature), T max 0 C (short-term max. temperature in a temperature program) Both phases are also suited for the determination of vinyl chloride as well as for the separation of cis/trans isomers of,-dichloroethene. The high film thickness secures a high capacity and an outstanding resolution. For GC/MS coupling, we recommend PTIMA 64 LB or PTIMA 64 with 0. or 0.5 mm ID Volatile halogenated hydrocarbons MN Appl. No. 480 Column: PERMABND SE-54-HKW, 50 m x 0. mm ID Injection: μl, split ~ :0 Carrier gas: 0.9 bar He : 5 C (5 min) 60 C (5 min), 0 C/min Detector: ECD 00 C Peaks:. Dichloromethane (795 ng/ml). Trichloromethane (75 ng/ml).,,-trichloroethane (67 ng/ml) 4.,-Dichloroethane (00 ng/ml) 5. Tetrachloromethane (5.9 ng/ml) 6. Trichloroethene (4.6 ng/ml) 7. Bromodichloromethane (0 ng/ml) 8. Dibromochloromethane ( ng/ml) 9. Tetrachloroethene (8 ng/ml) 0. Tribromomethane (8.9 ng/ml) min 5

55 Capillary columns for hydrocarbons Column: Injection: Carrier gas: : PTIMA 64, 50 m x 0.5 mm ID,.40 μm fi lm μl, split 50 ml/min Detector: MSD 597 Peaks:. Vinyl chloride. Trichlorofl uoromethane (F ). Pentane 4.,,-Trichlorotrifl uoroethane (F ) 5. Dichloromethane 6. trans-,-dichloroethene 7. Hexane 8. cis-,-dichloroethene 9. Trichloromethane 0.,,-Trichloroethane. Tetrachloromethane 0.9 ml/min He (constant fl ow) 40 C (5 min) 60 C, 0 C/min Volatile halogenated hydrocarbons and BTX.,-Dichloroethane + benzene. Trichloroethene 4. Bromodichloromethane 5. Toluene 6. Tetrachloroethene 7. Dibromochloromethane 8. Chlorobenzene 9. Ethylbenzene 0. m- + p-xylene. o-xylene. Tribromomethane. Bromobenzene MN Appl. No min PERMABND SE-54-HKW 0. mm ID (0.5 mm D) 5 m 50 m.80 μm film Further applications can be found online in our application database at /apps 5

56 Capillary columns for silane DEG PERMABND Silane for silane analysis 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 0. mm ID: T max 60 C (long-term temperature), T max 80 C (short-term max. temperature in a temperature program) 0.5 mm ID: T max 40 and 60 C, resp. PERMABND Silane 5 m 50 m 0. mm ID (0.5 mm D) mm ID (0.8 mm D) 74.5 Chloromethylsilanes MN Appl. No Column: PERMABND Silane, 50 m x 0. mm ID Injection: 0.5 μl gas, split 80 ml/min Carrier gas: ml/min He (constant fl ow) : 50 C 00 C, 5 C/min Detector: MSD 597 Peaks:. Tetramethylsilane. Dichloromethane 5. Tetrachlorosilane 6 4. Chlorotrimethylsilane 5. Methyltrichlorosilane 6. Dichlorodimethylsilane 4 7. Hexamethyldisiloxane Column: Diethylene glycol standard in wine MN Appl. No PERMABND CW 0 M-DEG, 5 m x 0.5 mm ID Injection: 0.5 μl, split ~:40 Carrier gas:. bar N : 80 C 00 C, 0 C/min Detector: FID 60 C Peaks: DEG standard.,4-butanediol. Diethylene glycol. Glycerol min min PERMABND CW 0 M-DEG for determination of diethylene glycol USP G6 Polyethylene glycol (diethylene glycol tested) Determination of diethylene glycol (DEG), e.g., for the quality control of wine T max 0 C (long-term temperature), T max 40 C (short-term max. temperature in a temperature program) PERMABND CW 0 M-DEG 0.5 mm ID (0.4 mm D) 5 m 0.5 μm film mm ID (0.5 mm D) 0.5 μm film 77.5 Further applications can be found online in our application database at /apps 54

57 Fused silica capillaries Untreated capillaries Capillary electrophoresis Preparation of capillary columns Capillary LC applications Untreated capillaries Capillaries for electrophoresis m Pack of 0 m Pack of 0.05 mm ID (0.4 mm D) mm ID (0.4 mm D) mm ID (0.4 mm D) mm ID (0.4 mm D) Untreated capillaries 5 m Pack of 0.0 mm ID (0.4 mm D) mm ID (0.4 mm D) mm ID (0.5 mm D) mm ID (0.8 mm D) Untreated capillaries are supplied without cage. Deactivated capillary columns precolumns / guard columns As precolumns / guard columns, whenever a larger contamination capacity is required Preparation of capillary columns Deactivated capillary columns 0 m 5 m Methyl-Sil deactivated (T max 0 C) 0.5 mm ID (0.4 mm D) mm ID (0.5 mm D) mm ID (0.8 mm D) Phenyl-Sil deactivated (T max 0 C) 0.5 mm ID (0.4 mm D) mm ID (0.5 mm D) mm ID (0.8 mm D) CW deactivated (T max 50 C) 0.5 mm ID (0.4 mm D) mm ID (0.5 mm D) mm ID (0.8 mm D) Untreated capillaries are supplied without cage. For a considerably longer lifetime, even for contaminated or matrix-containing samples, MN offers the option of integrated precolumns. All capillary columns are available with a 0 m guard column with matched deactivation. For ordering, please add V at the end of the REF number. Guard column combinations with other lengths, IDs or different deactivation are available on request. 55

58 Fused silica capillaries Retention gaps The retention gap technique in combination with on-column injection allows to concentrate 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 T max 50 C (CW retention gaps), T max 0 C (Me-Sil and Phe-Sil retention gaps) Note: Calculation example: length of flooded zone ~ 0 0 cm/μl, retention gap 0 m x 0. mm ID, capillary column: 5 m x 0. mm ID, max. injection volume ~ 0 50 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 Retention gaps can also be used as transfer lines or precolumns (contamination capacity about 5 0 μg). Retention gaps 0 m 5 m Me-Sil retention gaps (T max 0 C) 0.5 mm ID (0.4 mm D) mm ID (0.5 mm D) mm ID (0.8 mm D) Phe-Sil retention gaps (T max 0 C) 0.5 mm ID (0.4 mm D) mm ID (0.5 mm D) mm ID (0.8 mm D) CW retention gaps (T max 50 C) 0.5 mm ID (0.4 mm D) mm ID (0.5 mm D) mm ID (0.8 mm D) Retention gaps are supplied without cage. For a considerably longer lifetime, even for contaminated or matrix-containing samples, MN offers the option of integrated precolumns. All capillary columns are available with a 0 m guard column with matched deactivation. For ordering, please add V at the end of the REF number. Guard column combinations with other lengths, IDs or different deactivation are available on request. 56

59 Reagents / methods for derivatization Derivatization reagents Derivatization reagents: To improve volatility, increase thermal stability or to achieve a lower limit of detection in gas chromatography Prerequisite: quantitative, rapid and reproducible formation of only one derivative Halogen atoms inserted by derivatization, e.g., trifluoroacetates, allow the specific detection in an ECD with the advantage of high sensitivity. Specific derivatizations may influence elution orders and fragmentation patterns in a MS We provide reagents for - acylation - alkylation (methylation) - silylation For x 0 ml, x 50 ml and 6 x 50 ml also available with screw closure Derivatization method development kits* Designation Contents of the kit REF Which type of derivatization is suited best for your sample (alkylation, acylation or silylation)? Acylation kit x ml each of TMSH, MSTFA, MBTFA 7095 Which is the proper reagent for acylation? x ml each of MBTFA, TFAA, MBHFBA Alkylation kit Which is the proper reagent for methylation? x ml each of TMSH, DMF-DMA 7095 Silylation kit Which is the proper reagent for silylation? x ml each of MSTFA, BSTFA, TSIM, MSHFBA 7095 * These products contain harmful substances which must be specially labeled as hazardous. For detailed information please see SDS. Selection guide for derivatization of important functional groups in GC Function Method Derivative Recommended reagents alcohols, phenols R H sterically hindered amines primary, secondary hydrochlorides amides amino acids Carboxylic acids (fatty acids) salts carbohydrates steroids silylation acylation alkylation silylation silylation acylation silylation silylation acylation silylation alkylation (a) + acylation (b) silylation alkylation silylation silylation acylation silylation acylation R TMS R C R R R R TMS R NR TMS R NR C R R NR TMS BSA, MSTFA, MSHFBA, TSIM, SILYL-0, SILYL-, SILYL-9 TFAA, HFBA, MBTFA, MBHFBA TMSH TSIM, BSTFA, SILYL-99 BSA, MSTFA, MSHFBA, SILYL-99 TFAA, HFBA, MBTFA, MBHFBA MSTFA not stable R C NH C R TFAA, MBTFA, HFBA, MBHFBA R CH(NH TMS) C TMS R CH(NH C-R) C R R C TMS susceptible to hydrolysis R C R R C TMS susceptible to hydrolysis BSA, BSTFA, MSTFA, MSHFBA a) MeH/TMCS, TMSH b) TFAA, HFBA, MBTFA, MBHFBA BSA, MSTFA, MSHFBA, TMCS, TSIM, SILYL-0, SI- LYL-, Silyl-9 DMF-DMA, MeH/TMCS ( M), TMSH TMCS MSTFA, TSIM, HMDS, SILYL-9 TFAA, MBTFA BSA, TSIM TFAA, MBTFA, HFBA, MBHFBA These products contain harmful substances which must be specially labeled as hazardous. For detailed information please see SDS. Due to their purpose, derivatization reagents are very reactive substances. For this reason, they should be stored cool and protected from moisture. For easy access with a syringe, our derivatization reagents are supplied in vials with crimp caps (exception DMCS and TMCS with screw closure). Vials with pierced sealing disks have limited stability and should be used soon. The derivatization procedures can be found on page

60 CF CF Reagents / methods for derivatization General reaction mechanisms Silylation Alkylation (Methylation) example TMSH Analyte X H+ H C Si Y Analyte X Si + HY Analyte + X H + TMSH H - Analyte X + S + H X = e.g.,, S, C, etc. Y = rest of silylation reagents X = e.g.,, S, C, etc. Acylation Analyte X H + Y R Analyte X R + HY X = e.g.,, S, NH, etc. Y = rest of acylation reagents MACHEREY-NAGEL derivatization reagents for GC Content of brochure Product range for acylation, alkylation and silylation reagents Protocols for derivatization Diverse tips and hints rdner now your derivatization brochure KATEN0044 Chromatography MACHEREY-NAGEL Derivatization reagents for GC i() CF CF N C C CF C N N CF Si() Si() C N N C N CF Si() Si() C CF C N Si() Si() CH C Si(CH Enhance your GC analysis N C Si() N Si() CF C N Si() N C Si(CH n Ultrapure n Highly reactive n Cost-effective 58

61 Reagents / methods 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 5 C Cl M 0.5 g/mol, Bp C (760 mm Hg), Density d0 /4 =.60 Anhydrides By-products of acylation with anhydrides: corresponding acids excess reagent and the acid formed are to be removed Trifluoroacetic acid anhydride TFAA: CF C C CF M 0.04 g/mol, Bp C (760 mm Hg), Density d0 /4 =.490 Heptafluorobutyric acid anhydride HFBA: C F 7 C C C F 7 M g/mol, Bp C (760 mm Hg), Density d0 /4 =.665 Bisacylamides By-products: corresponding neutral acylamides: high volatility Easily removed; due to the neutral conditions and their favorable chromatographic characteristics, the removal of surplus bisacylamides and their by-products is often not necessary. Therefore, the sample preparation is much easier. N-methyl-bis(trifluoroacetamide) MBTFA: CF C N( ) C CF M.08 g/mol, Kp 4 C (760 mm Hg), Density d0 /4 =.55 N-methyl-bis(heptafluorobutyramide) MBHFBA: C F 7 C N( ) C CF7 M 4. g/mol, Kp C (760 mm Hg), Density d0 /4 =.67 59

62 Reagents / methods for acylation Methods for acylation Acylation with fluorinated acid anhydrides (TFAA, HFBA) Applicable for alcohols, phenols, carboxylic acids, amines, amino acids and steroids, stable derivatives for FID or ECD detection Procedure see page 67 or online at /apps TFAA: MN Appl. Nr. 04 HFBA: MN Appl. Nr. 04 Acylation with fluorinated acid amides (MBTFA, MBHFBA) Recommended for alcohols, primary and secondary amines as well as for thiols under mild, neutral conditions MBTFA also forms very volatile derivatives with carbohydrates [7]. Procedure see page 67 or online at /apps MBTFA: MN Appl. Nr. 05 MBHFBA: MN Appl. Nr. 05 Acylation reagents* Substance Packing unit 0 x ml 0 x ml x 0 ml 5 x 0 ml HFBA MBTFA MBHFBA PFBC TFAA * These products contain harmful substances which must be specially labeled as hazardous. For detailed information please see SDS. n request for x 0 ml, x 50 ml and 6 x 50 ml also available with screw closure. 60

63 Reagents / methods for alkylation / methylation Alkylation / methylation reagents DMF-DMA N,N-dimethylformamide dimethylacetal H C H C N Methylation reagents M 9.7 g/mol, Kp C (760 mm Hg), Density d0 /4 = TMSH (0. mol/l in methanol) Trimethylsulfonium hydroxide H C H C S + H Methylation reagents M g/mol Methods for alkylation / methylation Methylation with TMSH Suited for free acids, chlorophenoxycarboxylic acids, their salts and derivatives as well as for phenols and chlorophenols [8] The great advantage is the simplification of the sample preparation. Lipids or triglycerides can be converted to the corresponding fatty acid methyl esters (FAMEs) by simple transesterification. This reaction is very elegant and convenient, because it is only necessary to add the reagent (0. mol/l in methanol) to the sample solution. Removal of surplus reagent is not required, since at 50 C inside the injector of the gas chromatograph, TMSH will pyrolyze solely to volatile methanol and dimethylsulfide. Due to high reactivity, a complete conversion is usually obtained at ambient temperature. Heating (e.g., 0 min at 00 C) in a closed sample vial may be necessary, however. Procedure see page 67 or online at /apps MN Appl. Nr. 060 Methylation with DMF-DMA Applicable for fatty acids, primary amines and (partially) amino acids, under formation of N-dimethyl-aminomethylene amino acid methyl esters [9] Since DMF-DMA is a poor solvent, it is essential to use a mixture of DMF-DMA with pyridine, THF, acetone (barbiturates) or another solvent. Procedure see page 67 or online at /apps MN Appl. Nr. 070 Methylation with methanol TMCS ( M) Suited for the esterification of free carboxylic acids and the transesterification of glycerides. Formation of HCl catalyzes the reaction. TMCS, resp. silyl ethers remove the water and thus drive the reaction to completion. The mixture should be freshly prepared. Procedure see page 67 or online at /apps MN Appl. Nr. 080 For GC separation of FAMEs from natural butter fat after derivatization with TMSH see Appl at /apps Alkylation reagents* Packing unit Substance 0 x ml 0 x ml x 0 ml 5 x 0 ml DMF-DMA TMSH * These products contain harmful substances which must be specially labeled as hazardous. For detailed information please see SDS. n request for x 0 ml, x 50 ml and 6 x 50 ml also available with screw closure. 6

64 Reagents / methods for silylation Silylation reagents The most common form of silylation in GC is the replacing of active hydrogen atoms with a trimethylsilyl group (TMS derivative). Less frequently, trialkylsilyl groups or dimethylsilyl groups with longer alkyl chains are also in use. The alkylsilyl group increases volatility and enhances thermal stability of the sample. Silylation can be catalyzed 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 amide (e.g., BSA, MSTFA) > TMS amine = TSIM > Enol--TMS ether > S-TMS ether > -TMS ether > TMS--TMS Stability of the TMS derivatives: -TMS ether > S-TMS ether > Enol--TMS ether > TMS amine > TMS amide BSA N,-bis-trimethylsilyl-acetamide H C C Si( ) N Si( ) M 0.4 g/mol, Bp 7 7 C (5 mm Hg), Density d0 /4 = 0.8 Strong silylation reagent 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. Dissolved in DMF, BSA is the prime derivatization reagent for phenols. Alcohols, amines, carboxylic acids, phenols, steroids, biogenic amines and alkaloids are derivatized to stable TMS derivatives BSTFA N,-bis-trimethylsilyl-trifluoroacetamide F C C Si( ) N Si( ) M 57.4 g/mol, Bp 40 C ( mm Hg), Density d0 /4 = 0.96 Powerful trimethylsilyl donor with approx. the same donor strength as the nonfluorinated analog BSA Advantage of BSTFA over BSA: greater volatility of its reaction products, particularly useful for GC analysis of low boiling TMS amino acids BSTFA is nonpolar (less polar than MSTFA) and can be mixed with acetonitrile for improved solubility. For the silylation of fatty acid amides, hindered hydroxyl groups and other difficult to silylize compounds, e.g., secondary alcohols and amines, we recommend BSTFA + % trimethylchlorosilane (TMCS), available under the designation SILYL-99 (see page 66). Silylation with BSA, BSTFA or SILYL-99 (BSTFA + % TMCS) Procedure see page 67 or online at /apps BSA MN Appl. Nr. 09 BSTFA MN Appl. Nr. 09 SILYL-99 MN Appl. Nr. 09 Silylation with BSA in combination with other silylation reagents Procedure see page 67 or online at /apps MN Appl. Nr. 00 6

65 Reagents / methods for silylation Silylation reagents* Packing unit Substance 0 x ml x 0 ml 5 x 0 ml x 50 ml x 00 ml BSA BSTFA SILYL-99 (BSTFA TMCS (99:)) * These products contain harmful substances which must be specially labeled as hazardous. For detailed information please see SDS. n request for x 0 ml, x 50 ml and 6 x 50 ml also available with screw closure. MSTFA N-methyl-N-trimethylsilyl-trifluoroacetamide F C C N Si( ) M 99. g/mol, Bp 70 C (75 mm Hg), Density d0 /4 =. The most volatile trimethylsilyl amide available, very strong TMS donor which does not cause noticeable FID fouling even during long-time measuring series 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. The addition of protic solvents in submolar quantities, e.g., TFA for extremely polar compounds (hydrochlorides) or pyridine for carbohydrates), can improve the already good dissolving power of MSTFA. Advantages: complete conversion with high reaction rates, even without a catalyst ( % TMCS or TSIM); the by-product of the reaction (N-methyltrifluoroacetamide) shows a high volatility and a short retention time MSHFBA N-methyl-N-trimethylsilyl-heptafluorobutyramide F 7 C C N Si( ) M 99. g/mol, Bp 48 C (760 mm Hg) Similar to MSTFA in reactivity and chromatography Either applied 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 Carboxylic acids, alcohols, phenols, primary and secondary amines and amino acids Especially useful for flame ionization detection due to the large ratio of fluorine to silicon of 7:, since degradation of the surplus MSHFBA does not produce Si but volatile, non-corrosive silicon compounds MBDSTFA N-methyl-N-tert-butyldimethylsilyl-trifluoroacetamide F C C N Si( ) M 4. g/mol, Bp 70 C (760 mm Hg), Density d0 /4 =. C 4 H 9 Silylation reagent that donates a tert-butyldimethylsilyl group (TBDMS) for derivatizing active hydrogen atoms in hydroxyl, carboxyl and thiol groups as well as primary and secondary amines Fast reactions (typically 5 0 min) with high yields (> 96 %), by-products are neutral volatiles TBDMS ethers are 0 4 times more stable than the corresponding TMS ethers Due to the large protecting group, chromatographic retention times are longer. This may have a beneficial impact on some separations. The high concentration of M ions is an interesting topic for GC/MS. 6

66 Reagents / methods for silylation Silylation with MSTFA, MSHFBA or MBDSTFA Procedure see page 67 or online at /apps MSTFA MN Appl. Nr. MSHFBA MN Appl. Nr. MBDSTFA MN Appl. Nr. Silylation reagents* Packing unit Substance 0 x ml 0 x ml x 0 ml 5 x 0 ml x 00 ml 6 x 50 ml 6 x 00 ml x 00 ml MSTFA MSHFBA MBDSTFA * These products contain harmful substances which must be specially labeled as hazardous. For detailed information please see SDS. n request for x 0 ml, x 50 ml and 6 x 50 ml also available with screw closure. Ultrapure derivatization reagents for acylation, alkylation and silylation. 64

67 Reagents / methods for silylation DMCS Dimethyldichlorosilane H C Si Cl Cl M 9.06 g/mol, Bp 70 C (760 mm Hg), Density d0 /4 =.07 HMDS Hexamethyldisilazane H C H C Si H C N H Si M 6.4 g/mol, Bp 6 C (760 mm Hg), Density d0 /4 = TMCS Trimethylchlorosilane H C Si Cl M 08.7 g/mol, Bp 57 C (760 mm Hg), Density d0 /4 = TSIM N-trimethylsilyl-imidazole H C Si N N M 40. g/mol, Bp C (760 mm Hg), Density d0 /4 = 0.96 Used to form dimethylsilyl (DMS) derivatives Weak TMS donor; used as a sole reagent, it is slow and not very effective. Aprotic solvents like acetonitrile, pyridine, dimethylformamide, carbon disulfide and dimethylacetamide recommend themselves for use with HMDS. ften used as a catalyst with other trimethylsilyl reagents Strongest hydroxyl silylator It is remarkable that TSIM reacts quickly and smooth with hydroxyl (even tert. H) and carboxyl groups, but not with amines. Hence it is especially suited for multiple derivatizations, when compounds with various functional groups are to be derivatized in different ways (e.g., --TMS, -N-HFB derivatives of catecholamines). DMS derivatives are much more susceptible to hydrolysis than TMS derivatives, it is therefore vital to have strictly anhydrous conditions during the conversion. With catalytic quantities, e.g., % of, or as a mixture with TMCS (:, v/v; SILYL- and SILYL-0) it is perfectly suited for a quick and quantitative trimethylsilylation of organic compounds. As a sole reagent, it can be used to prepare TMS derivatives of organic acids. Alcohols, phenols, organic acids, steroids, hormones, glycols, nucleotides, narcotics Reagent of choice for carbohydrates and most steroids (even strongly hindered steroids) Silylation with TSIM or SILYL-9 (TSIM pyridine :9) Procedure see page 67 or online at / apps TSIM: MN Appl. Nr. SILYL-9: MN Appl. Nr. 65

68 Reagents / methods for silylation Silylation reagents* Packing unit Substance 0 x ml x 0 ml 5 x 0 ml 6 x 50 ml DMCS HMDS TMCS TSIM * These products contain harmful substances which must be specially labeled as hazardous. For detailed information please see SDS. n request for x 0 ml, x 50 ml and 6 x 50 ml also available with screw closure. Reagent mixtures for silylation* Packing unit Mixture Composition 0 x ml x 0 ml 5 x 0 ml x 50 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:) * These products contain harmful substances which must be specially labeled as hazardous. For detailed information please see SDS. n request for x 0 ml, x 50 ml and 6 x 50 ml also available with screw closure. Due to their purpose, derivatization reagents are very reactive substances. For this reason, they should be stored cool and protected from moisture. For easy access with a syringe, our derivatization reagents are supplied in vials with crimp caps (exception DMCS and TMCS with screw closure). Vials with pierced sealing disks have limited stability and should be used soon. Silylation with SILYL- or SILYL-0 s: sugars, glycols, sterically unhindered alcohols, carboxylic acids, acids in urine, hydroxy fatty acids, nucleotides, steroids, vitamin D, xanthone derivatives Procedure see page 67 or online at /apps SILYL- MN Appl. Nr. SILYL-0 MN Appl. Nr. -trimethylsilylation with MSTFA followed by N-trifluoroacetylation with MBTF Procedure see page 67 or online at /apps MSTFA / MBTFA MN Appl. Nr

69 Derivatization procedures Acylation with fluorinated acid anhydrides TFAA MN Appl. No. 04 HFBA MN Appl. No. 04 Dissolve 0. to mg sample in 0. ml solvent, add 0. ml of the anhydride and heat to C for h. If the sample needs 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. therwise, use a volatile solvent and evaporate solvent, excess reagent and free acid in a stream of nitrogen. Dissolve residue in 50 μl hexane, chloroform etc. and inject aliquot portions. with fluorinated acid amides MBTFA MN Appl. No. 05 MBHFBA MN Appl. No. 05 Add 0.5 ml MBTFA or MBHFBA to about mg sample. If there is no reaction at ambient temperature, heat the reaction mixture to 0 C. Compounds 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 is chromatographed directly. Alkylation (Methylation) with TMSH MN Appl. No. 060 Dissolve 00 mg sample (e.g., butter) in 5 ml of a solvent (e.g., tert.-butyl methyl ether). Add 50 μl reagent to 00 μl of this solution. The mixture is injected directly. The temperature of the injector must be at least 50 C. with DMF-DMA MN Appl. No. 070 Add ml of a mixture of DMF-DMA and pyridine (:) to 50 mg fatty acids. The sample can be injected as soon as a clear solution has formed. It is recommended, however, to heat the solution to C for 0 5 min. with methanol TMCS MN Appl. No. 080 Add ml methanol TMCS to about 50 mg carboxylic acid or glyceride and heat. Then evaporate in a stream of nitrogen and dissolve again for injection in, e.g., n-heptane. Silylation with BSA, BSTFA oder SILYL-99 (BSTFA + % TMCS) BSA MN Appl. No. 09 BSTFA MN Appl. No. 09 SILYL-99 MN Appl. No. 09 Add 0.5 ml of the silylation reagent to 0 mg sample; if necessary, add some solvent (normally pyridine or DMF [dimethylformamide]). Heat to C for 0 min to increase the reaction rate. drops of TMCS (trimethylchlorosilane) or TSIM will also speed up the reaction. with BSA in combination with other silylation reagents MN Appl. No. 00 BSA alone silylates all sterically unhindered hydroxyl groups of the steroid skeleton; addition of TMCS will enable reaction of moderately hindered H groups (reaction time 6 h at 60 C). After addition of TSIM even strongly hindered hydroxyl groups will react (reaction time 6 4 h at 60 C). with MSTFA, MSHFBA or MBDSTFA MSTFA MN Appl. No. MSHFBA MN Appl. No. MBDSTFA MN Appl. No. Dissolve 0 5 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 h and can be analyzed directly. If TFA is used as a solvent, proceed as follows [0]: dissolve mg sample in 00 µl TFA. Dropwise add 0.9 ml of the silylating reagent. After cooling the sample can be chromatographed directly. with TSIM or SILYL-9 (TSIM pyridine :9) TSIM MN Appl. No. SILYL-9 MN Appl. No. Dissolve 0 5 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 analyzed directly. Recommended solvent pyridine. When using SILYL-9, the presence of water does not interfere. with SILYL- or SILYL-0 SILYL- MN Appl. No. SILYL-0 MN Appl. No. Carefully add SILYL- or SILYL-0 to 0 mg of the sample. Precipitated ammonium chloride does not interfere. If the sample should not dissolve within 5 min, heat to 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 derivatization of -ketosteroids we recommend to use DMF (dimethylformamide) -trimethylsilylation with MSTFA followed by N-trifluoroacetylation with MBTFA MN Appl. No. 40 Completely silylate mg of the sample with 0. ml MSTFA, e.g., as described on page 6. After addition of 0. ml MBTFA the N-trimethylsilyl group is replaced by the N-trifluoroacetyl group. The mixture can be analyzed directly. 67

70 Test mixtures for GC capillary columns Test mixtures Test mixtures for GC capillary columns to control the performance of fused silica capillary columns and the GC system Test mixtures* Designation Pack of REF Activity test mixture (FA-TMS test according to Donike) in MSTFA/n-hexane ( + 4) Grob test mixture (modified) in n-hexane MN PTIMA test mixture in pentane MN PTIMA amine test mixture in ethanol FAME test mixture in hexane mg/ml each of TMS capric acid (C0), TMS myristic acid (C4), TMS stearic acid (C8), TMS behenic acid (C), hexadecane (C6), eicosane (C0), tetracosane (C4), octacosane (C8) (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.) 0. % each of undecane, dodecane, octanol, dimethylaniline, decylamine, methyl decanoate, methyl undecanoate, henicosane, docosane, tricosane (chromatograms see page 05) 0. % diisobutylamine, % diethanolamine, 0. %,6-dimethylaniline, 0. % o-propanol-pyridine, 0. % dicyclohexylamine, 0. % dibenzylamine 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 4) * These products contain harmful substances which must be specially labeled as hazardous. For detailed information please see SDS. ml 707 ml 70 ml 76 ml 77 ml 70 Grob test mixture (modified) (REF 70) MN Appl. No. 50 Column: PTIMA 5, 50 m x 0.5 mm ID,.0 μm fi lm Injection: μl, split :40, 80 C Carrier gas:.5 bar H : 80 C 80 C (0 min), 8 C/min Detector: FID 80 C Peaks:. n-decane. -ctanol. n-undecane 4.,6-Dimethylphenol 5.,6-Dimethylaniline 6. Methyl decanoate 7. Methyl undecanoate 8. Dicyclohexylamine 9. Methyl dodecanoate min 68

71 Test mixtures for GC capillary columns Column: Activity test mixture (REF 707) MN Appl. No. 40 PTIMA 5, 5 m x 0. mm ID,.0 μm fi lm Injection: μl, split :40, 00 C Carrier gas: 0.6 bar H : 50 C 00 C (8 min), 0 C/min Detector: FID 00 C Column: PTIMA Amine test mixture (REF 77) Injection: μl, split :40 MN Appl. No PTIMA 5 Amine, 0 m x 0. mm ID,.5 μm fi lm Carrier gas: 0.6 bar H : 00 C 80 C, 0 C/min Detector: FID 80 C Peaks:. TMS capric acid (C 0 ). Hexadecane (C 6 ). TMS myristic acid (C 4 ) 4. Eicosane (C 0 ) 5. TMS stearic acid (C 8 ) 6. Tetracosane (C 4 ) 7. TMS behenic aicd (C ) 8. ctacosane (C 8 ) Peaks:. Diisobutylamine. Diethanolamine.,6-Dimethylaniline 4. o-propanol-pyridine 5. Dicyclohexylamine 6. Dibenzylamine min 0 min 69

72 Ferrules for capillary columns Ferrules Graphite ferrules provide the highest temperature stability (up to 450 C). They are reusable, if handled with care. We also offer /6 graphite ferrules specially designed for Carlo Erba / Fisons or for Agilent gas chromatographs. Vespel ferrules with 40 % graphite. -stable up to 400 C and reusable. Ferrules Bore (= column D) Graphite Vespel T max 450 C /6 ferrules 0.4 mm mm /6 ferrules for Carlo Erba (Fisons) instruments 0.8 mm /6 ferrules for Hewlett-Packard (Agilent) instruments 0.4 mm mm mm /8 ferrules no bore 7084 /4 ferrules no bore mm mm % Graphite 400 C 70

73 Septa for capillary column Injection Port Septa blister pack for cleanliness and easily handling BT septa for highest demands in GC and GC-MS pierced, soft CenterGuide AG septa with higher durability than BT pierced, hard CenterGuide Marathon Septa with extreme durability for > 400 injections pierced CenterGuide Injection port septa Septum grade BT septa AG septa Marathon septa D T max 9 mm 400 C mm 400 C mm 400 C Shimadzu 00 C Pack of Standard Septa in classical plastic container Standard septa (ST) beige silicone, 60 shore A, 4 mm High temperature septa (HT) red non-bleeding silicone, 60 shore A, mm (0 C max.) Silicone septa soft, transparent Silicone / PTFE septa white silicone, one side coated with grey PTFE, mm Classical septa Septum grade Standard septa (ST) High temperature septa (HT) Silicone septa Silicone septa / PTFE D 9 mm mm mm mm mm mm 706 Pack of