Sample preparation Methods Analysis Biodiesel Analysis guide www.trajanscimed.com
Biodiesel is taking its place as one of the new cleaner and greener solutions required to meet the world s growing energy needs. New feedstocks, production techniques and applications are continuing to drive the production capabilities of biodiesel to meet consumer demand. This is increasing the analysis required by biodiesel producers. This guide has been created as a resource for biodiesel analysis. Inside you will find method information, products and solutions designed to ensure you can effectively and reliably complete fuels testing according to either ASTM International or European National (EN) methods. The latest information about our products and applications can always be found at our website: www.trajanscimed.com Sample preparation Methods Analysis 2
Introduction to biodiesel analysis The rising price of oil is driving fuel prices to new highs, causing substantial global economic impacts. This economic situation combined with the desire for cleaner and greener energy solutions has created the demand for new fuels. Companies and consumers are looking for alternative ways of deriving fuel from available sources. One alternative fuel achieving both environmental and economic requirements is biodiesel. Biodiesel is diesel derived from vegetable oils, animal fats and waste food by-products, usually cooking oil. Major investment is currently being made into the development of algae and other specifically bred plant crops that will increase yield and enable biodiesel to become a major component of our energy infrastructure. Product process The most widely accepted form of biodiesel production is trans-esterification, where typically oil is mixed with a solvent, usually methanol, and catalyzed by sodium methoxide, which causes the oil to be split into biodiesel and glycerine by-products. The biodiesel will then be processed for use in vehicles and the waste products split-off and sold separately. Glycerols, the major waste components, need to be minimized to trace levels within the fuel to prevent engine malfunction. Both the ASTM International and European National (EN) standards for biodiesel fuel certification require the fuel to be tested for total glyercol content before it can be released for sale. The European biodiesel standard mandates the completion of additional tests such as methanol and FAMEs. Biodiesel guide contents Trajan consumables - GC selection 6-7 Sample preparation 8 Capillary columns - BPX-BIOD GC 9 Method library: 1-17 - ASTM 6584 / EN1415 free glycerine, mono-glycerides, di glycerides, tri-glyerides - EN1413 Determination of ester and linolenic acid methyl ester contents - EN1411 Determination of methanol content Biodiesel analysis - Optimized chromatography supplies 18-28 Information resources 29-3 Biodiesel analysis guide 3
Syringes Inlet liners Ferrules 4
Septa The combination of components selected for your instrument make an important contribution to successful separations. Choose Trajan to improve your chromatography. GC columns Biodiesel analysis guide 5
Trajan consumables GC selection Syringes SGE syringes for autosamplers incorporate a vibrant color scheme, distinguished by volume, enabling easy identification of syringes installed in instruments. Choose from a comprehensive range of SGE syringe options including plunger protection, removable or fixed s, a range of gauge and length options as well as tip style alternatives. Color Syringe volumes Yellow 1 nl (1 µl) 1 ml 1 ml (1 L) Lime 5 nl (5 µl) 5 µl 5 ml Dark orange 1 µl 1 ml Green 25 µl 25 ml Purple 5 µl 5 ml Aqua 1 µl 1 ml Gray 25 µl 2.5 ml 2 ml (2 L) Light orange 5 nl (.5 µl) 5 µl 5 ml (.5 L) Septa The role of septa for GC analysis is key as many chromatographic problems are caused by use of inappropriate septa material or inappropriate handling of the septa. Desired septa attributes: Reliably seal against the carrier gas pressure in the inlet. Capable of being pierced and resealed time after time. Must not contaminate or bleed material into the chromatographic system. Material Max operating temperature Key features GP grade 2 C Low temperature applications EC grade 35 C, 3 C for 17 mm Low bleed MN grade 35 C, 3 C for 17 mm Premium septa for autosamplers HT grade 4 C, 33 C for 17 mm Outstanding mechanical properties for the highest temperature applications 6
Inlet liners The inlet liner is where the sample is introduced and vaporized into the gaseous phase. The design of the liner is crucial, as is liner deactivation, to ensure reproducible and accurate chromatography. To optimize your results for different sample types, SGE Inlet liners are color coded by geometry for ease of selection. Color Injection technique Sample types Liner geometry Dark Green Splitless Trace level analyses. Active compounds. Taper / Gooseneck Blue Split General purpose. Concentrated samples. Dirty samples. Aqua Splitless Trace level analyses. Dirty samples. Wide boiling point range. Orange Direct Trace level analyses. Active compounds. FocusLiner Tapered FocusLiner ConnecTite Purple Split Splitless General purpose. Concentrated samples. Dirty samples (only if quartz wool is present). Gaseous samples (also Purge and Trap, Headspace). Straight Yellow Gray Splitless LVI PTV LVI Trace level analyses. Low boiling point compounds. Active compounds. Trace level analyses. Large volume injections. Double Taper PTV/LVI Connectors and ferrules GC connections are designed to minimize time spent on installation, and are suitable for a wide range of applications. Poorly defined or selected connections can lead to an increase in dead volume, leaks and mismatched tubing s after temperature cycling. Material Uses Advantages Limitations 1% FID, NPD, high temperature Graphite 85% Vespel / 15% Graphite MS and oxygen-sensitive detectors Easy-to-use stable seal Higher temperature limit Can be easily removed Can be re-used Long lifetime High temperature limit MS compatible Siltite Metal MS and oxygen-sensitive detectors Long lifetime High temperature limit MS compatible Not for MS or oxygen-sensitive detectors Soft, easily deformed or destroyed Possible system contamination Cannot be re-used Must be re-tightened after initial temperature cycles Cannot be re-used Biodiesel analysis guide 7
Sample preparation Biodiesel requires quantitative measurement of the composition of the sample. Consequently liquid handling accuracy and precision are critical to the success of the final application. evol, the world s first digitally controlled analytical syringe and 21 R&D1 award winner, provides the accuracy and precision required in biodiesel analytical laboratories. evol XR makes everyone an expert Speed up and simplify laboratory workflow Improve accuracy and reproducibility Standardize results independent of operator skill evol is the coupling of two precision devices: a digitally controlled electronic drive and an XCHANGE enabled analytical syringe. XCHANGE syringes are easily and quickly changed allowing them to be dedicated to individual liquids or methods to prevent possible cross-contamination of reagents. evol is ergonomic, comfortable and easy to use. evol is easily calibrated and calibration factors saved for each syringe, enabling laboratories to comply with stringent global laboratory standards. evol is suitable for use with volatile samples. evol is programmable to store a laboratory workflow (up to 98 steps). evol is suitable for direct injection onto a chromatography column with a consistent flow rate. evol s stainless steel enables direct injection through septa. Now available! evol XR 1 ml syringe Password protection options enabling standardization of work processes. Slow aspirate and dispense for titrations and reaction rate control. 1 ml syringe provides more flexibility to improve workflows. evol Electronic Syringe starter kit contains: Description Part number evol XR kit contains: 2912-3 evol syringes 5 μl, 1 μl and 1 ml - Stand - Universal charger - Comprehensive instruction manual - Disc with manual in multiple languages evol only 29125 8
BPX-BIOD GC SGE GC columns Each ASTM and EN biodiesel method has been evaluated to demonstrate the suitability of BPX-BIOD GC columns to achieve optimal separation. Each BPX-BIOD GC column is tested at the maximum operating temperature for the column, and specific tests are undertaken to ensure the column meets inertness specifications and separation performance. This means you can be confident of a reliable separation, column after column. Please refer to the table below and method library on the following pages (6-14) to find the best high temperature column for your biodiesel analysis. Method Description Column ID Length (m) Film thickness (μm) Part number ASTM D6584* BPX BIOD6584.32 1.1 54118SG53 ASTM D6584* BPX BIOD6584.32 15.1 541181SG53 EN1413* BPX BIOD2.32 3.25 544331 EN1415* BPX BIOD5.32 1.1 541181SG53 EN1411* BPX BIOD1.32 3 3 54731 EN1411** BPX - BIOD Wax.32 3.25 544332 EN1411** BPX - BIOD Wax.32 3 1 544441 *Recommended column in method. **Alternative column recommended in method. Includes guard column. Biodiesel analysis guide 9
Method library ASTM D6584 / EN 1415 free and total glycerine Column part number Phase Column 54118SG53 BIOD-BPX6584 or BPX-BIOD5 1 m x.32 mm ID x.1 μm with 2 m x.53 mm ID guard column Initial temperature 5 C, 1 min Rate 1 15 C/min to 18 C Rate 2 7 C/min to 23 C Rate 3 7 C/min Final temperature 38 C, 1 min Detector FID at 4 C Carrier gas He Carrier gas flow 3 ml/min Low level ASTMD6584 / EN1415 standard 35 35 3 3 25 2 15 1 5 Glycerol 3.852 Butanetriol (IS) 4.555 9.195 Monopalmitin 13.393 Monolein 14.865 Tricaprin (IS) 18.77 Diolein 2.13 Triolein 22.167 25 2 15 1 5 3 4 5 6 7 8 9 1 11 12 13 14 15 16 17 18 19 2 21 22 23 24 Minutes High level ASTMD6584 / EN1415 standard 35 35 3 25 2 15 1 5 Glycerol 3.857 Butanetriol (IS) 4.555 9.193 13.125 Monopalmitin 13.445 Monolein 14.953 Tricaprin (IS) 18.77 Diolein 2.145 Triolein 22.188 3 25 2 15 1 5 3 4 5 6 7 8 9 1 11 12 13 14 15 16 17 18 19 2 21 22 23 24 Minutes 1
Minutes Good yellow grease biodiesel and bad yellow grease biodiesel compared with ASTMD6584 / EN1415 standard 5 5 5 5 45 4 35 3 25 2 45 4 35 3 25 2 Glycerol Butanetriol (IS) Monopalmitin Monolein Tricaprin (IS) Diolein Triolein 45 4 35 3 25 2 45 4 35 3 25 2 Good Yellow yellow Grease grease Bad Yellow yellow Grease grease Standard 15 15 15 15 1 1 1 1 5 5 5 5 3 4 5 6 7 8 9 1 11 12 13 14 15 16 17 18 19 2 21 22 23 24 Minutes Soy derived biodiesel sample compared to ASTMD6584 / EN1415 standard 5 5 45 45 4 35 3 25 2 15 1 Glycerol Butanetriol (IS) Monopalmitin Monolein Tricaprin (IS) Diolein Triolein 4 35 3 25 2 15 1 Soy derived biodiesel Standard 5 5 3 4 5 6 7 8 9 1 11 12 13 14 15 16 17 18 19 2 21 22 23 24 Minutes Biodiesel analysis guide 11
Method library EN1413 determination of ester and linolenic acid methyl ester contents Column part number 544331 Phase BPX-BIOD2 Column 3 m x.32 mm ID x.25 μm Initial temperature 21 C, 9 min Rate 2 C/min Final temperature Carrier gas Carrier gas flow Injection volume 24 C, 6 min He 1.5 ml / min 1 μl RT # Components Wt% 2.58 8 C14: (Myristic) 4 2.74 9 C14:1 (Myristoleic) 2 2.96 1 C15: (Pentadecanoic) 2 3.17 11 C15:1 (cis-1-pentadecenoic) 2 3.48 12 C16: (Palmitic) 6 3.68 13 C16:1 (Palmitoleic) 2 4.17 14 C17: (Heptadecanoic) 2 4.44 15 C17:1 (cis-1-heptadecenoic) 2 5.12 16 C18: (Stearic) 4 5.41 17 C18:1n9c (Oleic) 4 5.41 18 C18:1n9t (Elaidic) 2 6.2 19 C18:2n6c (Linoleic) 2 6.2 2 C18:2n6t (Linolelaidic) 2 6.49 21 C18:3n6 (γ-linolenic) 2 7.2 22 C18:3n3 (α-linolenic) 2 8.16 23 C2: (Arachidic) 4 8.64 24 C2:1n9 (cis-11-eicosenoic) 2 9.6 25 C2:2 (cis-11, 14-Eicosadienoic) 2 1.3 26 C2:3n6 (cis-8,11, 14-Eicosatrienoic) 2 1.3 3 C21: (Henicosanoic) 2 1.35 27 C2:3n3 (cis-11,14, 17-Eicosatrienoic) 2 1.51 28 C2:4n6 (Arachidonic) 2 11.21 29 C2:5n3 (cis-5,8,11,14 17-Eicosapentaenoic) 2 11.31 31 C22: (Behenic) 4 11.63 32 C22:1n9 (Erucic) 2 12.38 33 C22:2 (cis-13, 16-Docosadienoic) 2 12.78 35 C23: (Tricosanoic) 2 14.56 36 C24: (Lignoceric) 4 15.8 34 C22:6n3 (cis-4,7,1,13,16, 19-Docosahexaenoic) 2 15.8 37 C24:1n9 (Nervonic) 2 12 45 8 45 4 4 35 35 3 17,18 3 25 25 2 15 9 1 11 13 14 15 16 19,2 23 26,3 31 36 2 15 1 21 22 24 25 27 28 29 32 33 35 34,37 1 5 5 3 4 5 6 7 8 9 1 11 12 13 14 15 16 Minutes 12
FAME profile of IQAEP B214 yellow grease C17: C18:1 24 C18:2 24 22 C18: 22 2 2 18 18 16 C16: 16 14 14 12 12 1 1 8 C14: 8 6 6 4 C18:3 4 2 C2: C2:1 C22: C24: 2 1 2 3 4 5 6 7 8 9 1 11 12 13 14 15 16 Minutes FAME profile of good yellow grease C17: C18:1 24 24 22 22 2 2 18 C18:2 18 16 16 14 C18: 14 C16: 12 12 1 1 8 8 6 6 C18:3 4 C14: 4 2 C2: C2:1 C22: C24: 2 1 2 3 4 5 6 7 8 9 1 11 12 13 14 15 16 Minutes Biodiesel analysis guide 13
Method library EN1413 continued FAME profile of bad yellow grease C17: C18:1 24 24 22 22 2 2 18 C18:2 18 16 16 14 14 C16: 12 C18: 12 1 1 8 8 6 6 4 C14: 4 C18:3 2 C2: C2:1 C22: C24: 2 1 2 3 4 5 6 7 8 9 1 11 12 13 14 15 16 Minutes FAME profile of canola C18:1 24 C17: 24 22 22 2 C18:2 2 18 18 16 16 14 14 12 C16: 12 1 1 8 C18:3 8 6 6 4 C18: 4 2 C14: C2:1 C2: C22: C24: 2 1 2 3 4 5 6 7 8 9 1 11 12 13 14 15 16 Minutes 14
FAME profile of sunflower C17: C18:1 24 24 22 22 2 2 18 C18:2 18 16 16 14 14 C16: 12 C18: 12 1 1 8 8 6 6 4 C14: 4 C18:3 2 C2: C2:1 C22: C24: 2 1 2 3 4 5 6 7 8 9 1 11 12 13 14 15 16 Minutes FAME profile of soy / tallow C17: C18:1 24 24 22 22 2 2 18 C18:2 18 16 16 14 14 C16: 12 C18: 12 1 1 8 8 6 6 4 C14: 4 C18:3 2 C2: C2:1 C22: C24: 2 1 2 3 4 5 6 7 8 9 1 11 12 13 14 15 16 Minutes Biodiesel analysis guide 15
Method library EN1411 methanol content in biodiesel Column part number 54731 Phase BPX-BIOD1 Column 3 m x.32 mm ID x 3. µm Initial temperature 21 C, 6 min Rate 2 C/min Final temperature 24 C, 6 min Detector 25 C Carrier gas He Carrier gas flow 1.5 ml/min Injection volume 1 μl Methanol content using EN1411 recommended column - 2. ml/min flow - 5 C - 2 μl injection 15 15 14 14 13 13 12 Methanol 2.3 min 12 11 11 1 1 9 9 8 8..5 1. 1.5 2. 2.5 3. 3.5 4. 4.5 5. 5.5 6. 6.5 7. 7.5 8. Minutes 15 15 14 14 13 Methanol 2.3 min 13 12 12 11 11 1 1 9 9 8 8 7 7 6 6 5 5 4 4 3 3 2 2-Propanol 3.7 min 2 1 1 Calibration solution A - 25 μl of.5% standard on BP1 column with 5 μl of IPA / 5 g of sample 7 7 6 6 5 5 4 2-Propanol 3.7 min 4 3 3 2 2 1 1..5 1. 1.5 2. 2.5 3. 3.5 4. 4.5 5. 5.5 6. 6.5 7. 7.5 8. Minutes 16
Calibration solution B - 25 μl of.1% standard on BP1 column with 5 μl of IPA / 5 g of sample 15 15 14 14 13 13 12 Methanol 2.3 min 12 11 11 1 1 9 9 8 8 7 7 6 6 5 5 4 2-Propanol 3.7 min 4 3 3 2 2 1 1..5 1. 1.5 2. 2.5 3. 3.5 4. 4.5 5. 5.5 6. 6.5 7. 7.5 8. Minutes Calibration Solution C - 25 μl of.1% standard on BP1 column with 5 μl of IPA / 5 g of sample 15 15 14 14 13 13 12 12 11 11 1 1 9 9 8 8 7 7 6 6 5 2-Propanol 3.7 min 5 4 4 3 Methanol 2.3 min 3 2 2 1 1..5 1. 1.5 2. 2.5 3. 3.5 4. 4.5 5. 5.5 6. 6.5 7. 7.5 8. Minutes Biodiesel analysis guide 17
Biodiesel analysis Optimized chromatography supplies SGE syringes 1-5 μl NanoVolume Specifications Accuracy and reproducibility Borosilicate glass barrel outer diameter (OD) Scale length International standards traceability ± 2 % (dispensed volume) 6.5 mm and 8 mm.5 µl (6.5 mm OD barrel) = 27.5 mm,.5 µl (8 mm OD barrel) = 63.7 mm, 1 µl = 54.1 mm, 63.7 mm, 5 µl = 48.7 mm Syringe volume Needle length (mm) Needle gauge Needle OD (mm) 8. mm outer diameter (OD) barrel Needle ID (mm) Needle tip 1 µl 5 23.63.155 Cone 1 µl 5 23.63.155 Bevel 1 µl 7 23.63.155 Cone 1 µl 7 23.63.155 Bevel 1 µl 115 23.63.155 Cone 1 µl 7 26.47.155 Cone 5 µl 5 23.63.365 Cone 5 µl 5 23.63.365 Bevel 5 µl 7 23.63.365 Cone 5 µl 7 23.63.365 Bevel 5 µl 115 23.63.365 Cone 5 µl 7 23.63.365 Nozzle Description 1. μl NanoVolume syringe with 5 cm.63 mm OD cone tipped 1. μl NanoVolume syringe with 5 cm.63 mm OD bevel tipped 1. μl NanoVolume syringe with 7 cm.63 mm OD cone tipped 1. μl NanoVolume syringe with 7 cm.63 mm OD bevel tipped 1. μl NanoVolume syringe with 11.5 cm.63 mm OD bevel tipped 1. μl NanoVolume syringe with 7 cm.47 mm OD cone tipped 5. μl NanoVolume syringe with 5 cm.63 mm OD cone tipped 5. μl NanoVolume syringe with 5 cm.63 mm OD bevel tipped 5. μl NanoVolume syringe with 7 cm.63 mm OD cone tipped 5. μl NanoVolume syringe with 7 cm.63 mm OD bevel tipped 5. μl NanoVolume syringe with 11.5 cm.63 mm OD cone tipped 5. μl NanoVolume syringe with 7 cm.63 mm OD nozzle tipped Replacement and plunger Syringe 3455 5 3456 51 3457 55 346 56 3459 51 3461 57 3555 8 3556 81 3557 82 3558 83 3559 84 356 85 Syringes fitted with repeating adaptor The SGE repeating adaptor (RAX) is attached to a syringe to ensure reproducibility of sample volumes. Syringe volume Needle length (mm) Needle gauge Needle OD (mm) 8. mm outer diameter (OD) barrel Needle ID (mm) Needle tip 1 µl 5 23.63.155 Cone 1 µl 7 23.63.155 Cone Description 1. μl NanoVolume syringe with 5 cm.63 mm OD cone tipped and repeating adaptor 1. μl NanoVolume syringe with 7 cm.63 mm OD cone tipped and repeating adaptor Replacement and plunger Syringe 3455 55 3457 553 18
Manual and on-column syringes 1-5 μl PTFE tipped plunger Specifications Accuracy and reproducibility Borosilicate glass barrel outer diameter (OD) Scale length International standards traceability ± 1 % (dispensed volume) 1 µl = 6.5 mm, 25 5 µl = 8 mm 1 µl = 54.1 mm, 25 5 µl = 6 mm Syringe volume Fixed PTFE tipped plunger Needle length (mm) Needle gauge Needle OD (mm) Needle ID (mm) Needle tip 1 µl P 5 26.47.11 Bevel 1 µl P 7 26.47.11 Bevel 25 µl P 5 25.5.2 Bevel 5 µl P 5 25.5.2 Bevel 1 µl P 5 25.5.2 Bevel 25 µl P 5 25.5.2 Bevel 5 µl P 5 25.5.2 Bevel Removable 1 µl P 5 26.47.11 Bevel 25 µl P 5 25.5.2 Bevel 5 µl P 5 25.5.2 Bevel 1 µl P 5 25.5.2 Bevel 25 µl P 5 25.5.2 Bevel 5 µl P 5 25.5.2 Bevel Guided plunger 1 µl P 5 26.47.11 Bevel On-column 1 µl P 75.17.11 Oncolumn Description 1 μl fixed syringe with GT plunger and 5 cm.47 mm OD bevel tipped 1 μl fixed syringe with GT plunger and 7 cm.47 mm OD bevel tipped 25 μl fixed syringe with GT plunger and 5 cm.5 mm OD bevel tipped 5 μl fixed syringe with GT Plunger & 5 cm.5 mm OD bevel tipped 1 μl fixed syringe with GT plunger and 5 cm.5 mm OD bevel tipped 25 μl fixed syringe with GT plunger and 5 cm.5 mm OD bevel tipped 5 μl fixed syringe with GT plunger and 5 cm.5 mm OD bevel tipped 1 μl removable syringe with GT plunger and 5 cm.47 mm OD bevel tipped 25 μl removable syringe with GT plunger and 5 cm.5 mm OD bevel tipped 5 μl removable syringe with GT plunger and 5 cm.5 mm OD bevel tipped 1 μl removable syringe with GT plunger and 5 cm.5 mm OD bevel tipped 25 μl removable syringe with GT plunger and 5 cm.5 mm OD bevel tipped 5 μl removable syringe with GT plunger and 5 cm.5 mm OD bevel tipped 1 μl removable guided plunger syringe with GT plunger and 5 cm.47 mm OD bevel tipped Replacement Replacement plunger 6 PK syringe Syringe 3181 222 22 3181 228 31815 32 3182 42 31825 52 3183 62 31835 72 3711 31811 2252 225 3811 31815 325 3811 3182 425 3811 31825 525 3811 3183 625 3811 31835 725 3711 3185 2455 1R-GT-OCCE 37675 31811 25 Biodiesel analysis guide 19
Agilent Technologies GC supplies SGE autosampler syringes All s are 42 mm long with a cone tip. Agilent 7673, 7683, 7693A and 685 ALS Volume Needle gauge (OD mm) Fixed tapered 5 µl 23-26s (.63/.47) 1 µl 23-26s (.63/.47) 1 µl 23-26s (.63/.47) gas tight Fixed straight Description 5 μl fixed Agilent syringe with 4.2 cm.63/.47 mm OD cone tipped dual gauge 1 μl fixed Agilent syringe with 4.2 cm.63/.47 mm OD cone tipped dual gauge 1 μl fixed Agilent syringe with GT plunger and 4.2 cm.63/.47 mm OD cone tipped dual gauge Syringe Spare Spare plunger 1821 1 2821 1 2826 1 3188 2 5 µl 23 (.63) 5 μl fixed Agilent syringe with 4.2 cm.63 mm OD cone tipped 181 1 1 µl 23 (.63) 1 μl fixed Agilent syringe with 4.2 cm.63 mm OD cone tipped 281 1 Removable tapered 5 µl 23-26s (.63/.47) 5R-AG-.63/.47C 1825 1 3673 2 1 µl 23-26s (.63/.47) 1R-AG-.63/.47C 2825 1 3773 2 Removable striaght 1 µl 23 (.63) 1BR-AG-.63C 61 1 34715 1** ** Denotes plunger and kit. Septa Instrument Diameter Septa type Agilent Technologies 789, 689, 589, 588, 489 and 685 Part no. 11 HT 25 41898 11 EC 25 4192 SGE Inlet liners Description and geometry sketch OD (mm) ID (mm) Length (mm) For Agilent 589, 685, 689, 789 and HP489 Split/splitless FocusLiner Split, straight-through liner 6.3 4 78.5 6.3 4 78.5 Part no. 1 9221 5 922 25 92219 1 9271 5 927 25 92222 The SGE Inlet liner range is color coded by geometry to simplify selection. FocusLiner Straight 2
Ferrules Instrument Column ID Ferrule ID Part no. 15% graphite / 85% Vespel ferrules.1-.25 mm.4 mm 1 7319.32 mm.5 mm 1 73111.53 mm.8 mm 1 73113 For injectors and detectors at for 1/8" OD packed columns 1/8" 1 72669 atmospheric pressure e.g. FID for 1/4" OD packed columns 1/4" 1 72667.1-.25 mm.4 mm 1 72663.32 mm.5 mm 1 72654.53 mm.8 mm 1 72655 SilTite metal ferrules.1-.25 mm.4 mm 1 *732 For GC-MS interface connection (starter kit).32 mm.5 mm 1 *7321.53 mm.8 mm 1 *7322.1-.25 mm.4 mm 1 #7327 For split/splitless injectors.32 mm.5 mm 1 #73271 (starter kit).45-.53 mm.8 mm 1 #73272 1/32".81 mm 1 #73273 Replacement SilTite metal ferrules For all connections.1-.25 mm.4 mm 1 7322.32 mm.5 mm 1 73221.53 mm.8 mm 1 73222 1/32".81 mm 1 73219 Replacement SilTite nuts For GC-MS interface connection 5 73224 For split/splitless injector 5 73226 Replacement SilTite base seals For split/splitless injector 2 734 1 7341 * Includes 1 ferrules, 2 SilTite nuts. # Includes 1 ferrules, 2 SilTite nuts and 2 SilTite inlet base seals. Biodiesel analysis guide 21
PerkinElmer GC supplies SGE autosampler syringes All s are 7 mm long with a cone tip style. PerkinElmer AutoSystem Volume Fixed Needle gauge (OD mm) 5 µl 26 (.47) 5 µl 23 (.63) 5 µl gas tight 5 µl gas tight 26 (.47) 23 (.63) 5 µl 23 (.63) Description 5 μl fixed PerkinElmer syringe with 7 cm.47 mm OD cone tipped 5 μl fixed PerkinElmer syringe with 7 cm.63 mm OD cone tipped.5 μl NanoVolume Agilent Syringe with 4.2 cm.47 mm OD cone tipped 5 μl fixed PerkinElmer syringe with GT plunger and 7 cm.63 mm OD cone tipped 5 μl fixed PerkinElmer syringe with 7 cm.63 mm OD cone tipped Syringe Spare plunger 1953 1 1954 1 1955 1 3187 2 1957 1 3187 2 467 1 Septa Instrument Diameter Septa type PerkinElmer Sigma, 9, 99, 8 series, AutoSystem and Clarus Part no. 11 HT 25 41898 11 HT 25 4192 SGE Inlet liners Description and geometry sketch OD (mm) ID (mm) Length (mm) For PerkinElmer AutoSystem and Clarus 5, 6 Split/splitless FocusLiner Split, straight-through liner 6.2 4 92 6.2 4 92 Part no. 1 92921 5 9292 25 929225 1 9211 5 921 25 92125 The SGE Inlet liner range is color coded by geometry to simplify selection. FocusLiner Straight 22
Ferrules Instrument Column ID Size of nut Ferrule ID Part no. 15% graphite / 85% Vespel ferrules.1-.25 mm 1/16".4 mm 1 72663.1-.25 mm 1/8".4 mm 1 72673.32 mm 1/16".5 mm 1 72654 For injectors and detectors at.32 mm 1/8".5 mm 1 72672 atmospheric pressure e.g. FID.45-.53 mm 1/16".8 mm 1 72655.45-.53 mm 1/8".8 mm 1 72671 1/8 OD packed columns 1/8" 1/8" 1 72669 1/4 OD packed columns 1/4" 1/4" 1 72667 SilTite metal ferrules.1-.25 mm.4 mm 1* 732 For GC-MS interface connection (starter kit).32 mm.5 mm 1* 7321.53 mm.8 mm 1* 7322 Replacement SilTite ferrules.1-.25 mm.4 mm 1 7322 For GC-MS interface.32 mm.5 mm 1 73221 connection.53 mm.8 mm 1 73222 1/32".81 mm 1 73219 Replacement SilTite nuts For GC-MS interface connection 5 73224 For split/splitless injector 5 73226 *Includes 1 ferrules, 2 SilTite nuts. Biodiesel analysis guide 23
Shimadzu GC supplies SGE autosampler syringes All s are 42 mm long with a cone tip style. Shimadzu AOC6 Volume Needle gauge (OD mm) Description Syringe Spare Spare plunger Fixed 5 µl 26 (.47) 5F-5.7-.63C 1865 1 1 µl 26 (.47) 1F-5.7-.63C 2865 1 1 µl gas tight 26 (.47) 1F-GT-5.7-.63C 2866 1 3281 1 25 µl gas tight 26 (.47) 25F-GT-5.7-.63C 3866 1 32815 1 1 µl gas tight 26 (.47) 1F-GT-5.7-.63C 5866 1 32825 1 Removable 1µL 23 (.63) 1BR-5.7-.63C 68 1 3478* 1 3478* 1 * Replacement and plunger is supplied as a set. Septa Instrument Shimadzu 9A, 14, 15A, 16, 17A, GC-21, GC-214 and GC-23 Septa type Part no. HT 5 41895 EC 5 4195 SGE Inlet liners Description and geometry sketch OD (mm) ID (mm) Length (mm) Part no. For GC-23 (SPL-23 injector), GC-21 (SPL-21 injector), GC-214 (SPL-214 injector) and GC-17A (SPL-17 injector) 1 92591 5 3.4 95 5 9259 Split/splitless FocusLiner * 25 925925 1 92621 5 3.4 95 Split/splitless FocusLiner * 5 9262 1 92641 6.3 4 95 Split, straight-through liner * 5 9264 * When using a standard 42 mm for autosamplers, the sample will be injected on top of the wool for this liner. The SGE Inlet liner range is color coded by geometry to simplify selection. FocusLiner Straight 24
O-rings and sealing rings Description Usage Part no. Graphite sealing ring Can be used at temperatures up to 45 C. For 14, 15A and 16 (SPL-14 injector) 1 7261 Graphite sealing ring Can be used at temperatures up to 45 C. For 17A (SPL-17 injector) 1 7267 Viton o-ring Can be used at temperatures up to 3 C. For GC-21 and GC-214 (SPL-21 injector and SPL-214 injector) 1 726533 Ferrules Column ID Description Part no. GC14A, GC17A, GC-21, GC-214 and GC-23 detectors/injectors (not for MS interfaces or QP21 injector).1-.25 mm ID columns SilTite metal - initial installation 1* 7335.1-.25 mm ID columns SilTite ferrules 1 73227.32 mm ID columns SilTite metal - initial installation 1* 73351.32 mm ID columns SilTite ferrules 1 73228.45-.53 mm ID columns SilTite metal - initial installation 1* 73352.53 mm ID columns SilTite ferrules 1 73229 n/a SilTite metal nuts - slotted 5 73232 QP5/55 standard MS interface QP5-I.1-.25 mm ID columns 15% Graphite/ 85% Vespel ferrules 1 726563 QP5-I.32 mm ID columns 15% Graphite/ 85% Vespel ferrules 1 726564 QP5-II and QP55.1-.25 mm ID columns 15% Graphite/ 85% Vespel ferrules 1 726561 QP5-II and QP55.32 mm ID columns 15% Graphite/ 85% Vespel ferrules 1 726562.1-.25 mm ID columns SilTite metal - initial installation 1* 7324.1-.25 mm ID columns SilTite ferrules 1 73227.32 mm ID columns SilTite metal - initial installation 1* 7325.32 mm ID columns SilTite ferrules 1 73228.53 mm ID columns SilTite metal - initial installation 1* 7326.53 mm ID columns SilTite ferrules 1 73229 QP5/55 wide bore MS interface, QP21 injector and QP21 standard MS interface.1-.25 mm ID columns 15% Graphite/ 85% Vespel ferrules 1 72663.32 mm ID columns 15% Graphite/ 85% Vespel ferrules 1 72654.45-.53 mm ID columns 15% Graphite/ 85% Vespel ferrules 1 72655.1-.25 mm ID columns SilTite metal - initial installation 1* 732.1-.25 mm ID columns SilTite ferrules 1 7322.32 mm ID columns SilTite metal - initial installation 1* 7321.32 mm ID columns SilTite ferrules 1 73221.45-.53 mm ID columns SilTite metal - initial installation 1* 7322.45-.53 mm ID columns SilTite ferrules 1 73222 n/a SilTite metal nuts 5 73224 * Includes 1 ferrules, 2 SilTite nuts. Replacement parts Material Part no. Replacement SilTite nuts For GC-21 and GC-23 GC-MS system 5 73224 For GC-21 and GC-23 GC-MS system with QP5 series MS 5 73224 For GC-21/GC-23/GC-214 GC injectors and atmospheric detectors 5 73224 QP5 jet separator MS interface 5 73224 QP5 direct MS interface 5 73233 For all injectors jet separator (starter kit), except GC-21/GC-23/GC-214 5 73232 Biodiesel analysis guide 25
Thermo Scientific GC supplies SGE autosampler syringes All s have a cone tip style. Thermo Scientific TriPlus RSH Volume Removable Needle gauge (OD mm) 5 µl 23 (.47) 57 5 µl 26 (.47) 57 1 µl 23 (.47) 57 1 µl 26 (.47) 57 Fixed 1 µl 23 (.63) 57 1 µl gas tight 23 (.63) 57 1 µl 23 (.63) 85 1 µl gas tight 23 (.63) 85 1 µl 26 (.47) 57 1 µl gas tight 26 (.47) 57 1 µl 26 (.47) 85 1 µl gas tight 26 (.47) 85 Needle length (mm) Description 5 μl removable CTC RTC and Thermo RSH syringe with 5.7 cm.63 mm OD cone tipped 5 μl removable CTC RTC and Thermo RSH syringe with 5.7 cm.47 mm OD cone tipped 1 μl removable CTC RTC and Thermo RSH syringe with 5.7 cm.63 mm OD cone tipped 1 μl removable CTC RTC and Thermo RSH syringe with 5.7 cm.47 mm OD cone tipped 1 μl fixed CTC RTC and Thermo RSH syringe with 5.7 cm.63 mm OD cone tipped 1 μl fixed CTC RTC and Thermo RSH syringe with GT plunger and 5.7 cm.63 mm OD cone tipped 1 μl fixed CTC RTC and Thermo RSH syringe with 8.5 cm.63 mm OD cone tipped 1 μl fixed CTC RTC and Thermo RSH syringe with GT plunger and 8.5 cm.63 mm OD cone tipped 1 μl fixed CTC RTC and Thermo RSH syringe with 5.7 cm.47 mm OD cone tipped 1 μl fixed CTC RTC and Thermo RSH syringe with GT plunger and 5.7 cm.47 mm OD cone tipped 1 μl fixed CTC RTC and Thermo RSH syringe with 8.5 cm.47 mm OD cone tipped 1 μl fixed CTC RTC and Thermo RSH syringe with GT plunger and 8.5 cm.47 mm OD cone tipped Syringe 1871 1 1875 1 2871 1 2875 1 2861 1 2862 1 2863 1 2864 1 2865 1 2866 1 2867 1 2868 1 Septa Instrument Diameter Septa type Thermo Scientific TRACE 13 Series GC Part no. 11 HT 25 41898 11 EC 25 4192 26
SGE Inlet liners Description and geometry sketch OD (mm) ID (mm) Length (mm) For Thermo Scientific TRACE 13 Series GC Split/splitless FocusLiner Split, straight-through liner 6.3 4 78.5 6.3 4 78.5 Part no. 1 9221 5 922 25 92219 1 9271 5 927 25 92222 The SGE Inlet liner range is color coded by geometry to simplify selection. O-rings and sealing rings FocusLiner Straight Description Usage Part no. For Thermo Scientific TRACE 13 Series GC Viton o-ring Temperatures up to 3 C. Suitable for liners with OD of 6.3 mm 1 726532 Graphite sealing ring Temperatures up to 45 C. Suitable for all inlet liners above except 924 and 9241 1 7265 Graphite sealing ring Temperatures up to 45 C. Suitable for use with liners 924 and 9241 1 7266 SilTite FingerTite ferrules Description Column ID Ferrule ID Part no. For Thermo Scientific TRACE 13 Series GC SilTite FingerTite INJ / FID starter kit.1-.25 mm.4 mm * 7361 SilTite FingerTite capillary / FID starter kit.1-.25 mm.4 mm * 73611 SilTite FingerTite INJ / MS starter kit.1-.25 mm.4 mm * 73612 Replacement parts SilTite FingerTite ferrule.4 mm.1-.25 mm.4 mm 1 7363 SilTite FingerTite ferrule.5 mm.32 mm.5 mm 1 73631 SilTite FingerTite ferrule.7 mm.53 mm.7 mm 1 73632 SilTite FingerTite ferrule blanking 2 73633 SilTite FingerTite female nut 5 73636 SilTite FingerTite INJ base seal.1-.25 mm 2 7364 SilTite FingerTite MS adaptor 1 73612 SilTite FingerTite injector.1-.25 mm 1 73614 * Each starter kit includes all the parts necessary to convert one GC system (one injector and one detector) to the SilTite FingerTite system. In addition there are five SilTite FingerTite nuts, ten SilTite FingerTite ferrules, and a ferrule install tool which allows you to seat the ferrule in the correct position on the capillary column. Biodiesel analysis guide 27
Thermo Scientific GC supplies Ferrules Instrument Column ID Ferrule ID Part no. 15% graphite / 85% Vespel ferrules.1-.25 mm.4 mm 1 7319.32 mm.5 mm 1 73111 For TRACE 13 injectors and detectors at atmospheric.53 mm.8 mm 1 73113 pressure e.g. FID for 1/8" OD packed columns 1/8" 1 72669 for 1/4" OD packed columns 1/4" 1 72667.1-.25 mm.4 mm 1 72663 For TRACE 13 GC-MS interface.32 mm.5 mm 1 72654 connection.53 mm.8 mm 1 72655 1% graphite ferrules.1-.32 mm.5 mm 1 72635 For TRACE 13 injectors and detectors at atmospheric.45-.53 mm.8 mm 1 72636 pressure e.g. FID (not for GC-MS) for 1/8" OD packed columns 1/8" 1 7262 for 1/4" OD packed columns 1/4" 1 7261 SilTite metal ferrules.1-.25 mm.4 mm 1* 7345 GC-MS interface connection (starter kit).32 mm.5 mm 1* 73451.53 mm.8 mm 1* 73452.1-.25 mm.4 mm 1 7327 For TRACE 13 split/splitless injectors.32 mm.5 mm 1 73271 (starter kit).45-.53 mm.8 mm 1 73272 1/32".81 mm 1 73273 Replacement SilTite nuts SilTite metal nuts 5 73224 Replacement SilTite metal ferrules.1-.25 mm.4 mm 1 7333 For All GC-MS interface.32 mm.5 mm 1 73331 connections.53 mm.8 mm 1 73332 1/32".81 mm 1 73333.1-.25 mm.4 mm 1 7322 For TRACE 13 connections.32 mm.5 mm 1 73221.53 mm.8 mm 1 73222 1/32".81 mm 1 73219 Replacement SilTite nuts SilTite metal nuts 5 7323 For TRACE 13 GC-MS interface connection 5 73224 For TRACE 13 split/splitless injector 5 73226 Replacement SilTite base seals For TRACE 13 split/splitless injector 2 734 1 7341 * Includes ten ferrules, two SilTite nuts. # To be used in combination with brass nut ( 13485). 28
Information resources For official methodolgy ASTM International ASTM International, formerly known as the American Society for Testing and Materials (ASTM), is a globally recognized leader in the development and delivery of international voluntary consensus standards. www.astm.org/standards/d6584.htm DIN Deutsches Institut fur Normung A range of international standards and reference for EN methods. www.din.de Industry resources National Biodiesel Board Body responsibly for the development of the US biodiesel industry. www.biodiesel.org Journals BioDiesel Magazine Biodiesel industry journal for news on commercial and technical developments. www.biodieselmagazine.com BioFuels International Industry journal for biofuels that features biodiesel related news. www.biofuels-news.com Biodiesel analysis guide 29
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Biodiesel Analysis guide This guide has been created as a resource for biodiesel analysis. Inside you will find method information, products and solutions designed to ensure you can effectively and reliably complete fuels testing according to either ASTM Internationally or European National (EN) methods. The latest information about our products and applications can be found at our website: www.trajanscimed.com. Visit us at www.trajanscimed.com or contact your regional Trajan representative for assistance and further information. BR-392-G_RevF Trajan Scientific Australia Pty Ltd 11/217 Trajan Scientific and Medical Science that benefits people Trajan is actively engaged in developing and delivering solutions that have a positive impact on human wellbeing. Our vision revolves around collaborative partnerships that improve workflows, delivering better results. www.trajanscimed.com