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GC Consumables Product Guide
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1. Solution Use high quality gas install gas traps Replace septa and insert a new inlet liner Cause Exceeded the maximum temperature of the capillary column phase Solution Lower the programmed maximum temperature Cause System has become active Solution Replace the inlet liner with a new deactivated liner cut 50 cm off the front of the column and re install Cause Splitless conditions have changed Solution Re check solvent and method temperatures Consider introducing an internal standard Cause Manual injection technique or operator has changed Solution Ensure technique is consistent Cause Dirty column if samples are dirty non volatile materials have deposited onto the column causing a change in polarity Solution Cut 50 cm off the front of the column and re install Cause Poor injection technique Solution Increase the manual plunger depression speed Cause The column has been inserted too far into the injector Solution Reposition the column according to the manufacturers recommendation Cause Too much sample injected onto column Solution Dilute the sample or increase the split ratio Cause Glass inlet liner has active surface Solution Replace with a fully deactivated inlet liner Cause Graphite ferrule contamination in the start of the column Solution Remove 5 cm off the front of the column and re install Cause Split gas
2. psi carryover ghost peaks and poor run to run reproducibility Se D is 2 250 10 798 e The inlet liner is a consumable and its life is influenced by the 2 250 34 7 399 quality of the sample and the frequency of use once the inlet 2 200 45 746 Dichloromethane as solvent liner is contaminated with septa particles it needs to be replaced Recommended replacement is every 100 200 injections e When peak shape deteriorates replace the inlet liner immediately and remove 30 cm from the front of the capillary column e When replacing the inlet liner it is the ideal time to replace the septa and the inlet liner sealing O ring GC Connections Ferrules are the smallest inexpensive and probably the most easily forgotten components that are used in every gas chromatograph Yet without ferrules the leak free sealing that is required at the detector and injector of a GC system would be impossible to achieve Always cut the column after passing through a graphite ferrule this eliminates the risk of graphite particles entering into the column and impacting your chromatography e Always re tighten Graphite Vespel ferrules by to V turn after the first 2 3 oven temperature cycles Graphite Vespel ferrules tend to creep during temperature cycling For GC MS connections always use SilTite metal ferrules to ensure a permanent leak free connection Cause Poor carrier gas quality
3. CI CI Un 221 75198 06 221 75199 06 Development Kit contains 1 each of C18 C8 Silica C8 5CX C2 1 of each phase 221 75198 05 221 75199 05 GC CONSUMABLES E e lt zm LL E a gt lt 92 SAMPLE INTRODUCTION SEPARATION O O 22 Un LLI CC D O CC SAMPLE INTRODUCTION Syringes Shimadzu Diamond syringes are the result of technological advancements in materials design and engineering Designed to meet the ever increasing levels of sensitivity required by today s analyses Shimadzu Diamond syringes give you a new level of accuracy and precision LONGER LIFE Shimadzu Diamond syringes have a longer life The improved solvent resistance and maximized operational temperature range along with the smoothest available internal glass surface ensure you receive the longest lifetime from your Shimadzu syringe SUPERIOR PERFORMANCE AND ROBUSTNESS Shimadzu Diamond syringes have superior performance and robustness with unsurpassed levels of operational strength and durability Potential for contamination is significantly reduced by the near zero syringe dead volume and minimized adhesive in the flow path REDUCED CARRYOVER Engineering enhancements have eliminated areas where fluid can become trapped and potentially cause carryover improving accuracy precision and analysis results Manual Autosampler or Instrument Syrin
4. SHIMADZU Excellence in Science GC Consumables Product Guide ZEIT U ER REI n GC Consumables Product Guide GC CONSUMABLES 4 SAMPLE INTRODUCTION SEPARATION NE TION Syringes P amp Connections P14 Contents GC Inlet Liners e11 MERS pes Septa HE TROUBLESHOOTING ef Accessories PIS GC CONSUMABLES GC Consumables are designed to complement your Shimadzu GC 2010 and GC 2014 System Shimadzu understands your chromatography analysis does not end with the selection of the GC column the combination of components selected for your instrument make an important contribution to successful chromatography Shimadzu GC Consumables are designed to provide you with the best separation possible SAMPLE INTRODUCTION Syringes SAMPLE INTRODUCTION Septa Shimadzu s syringes for both manual and Many chromatography problems are caused as a autosampler use incorporate Diamond Syringe result of the wrong septa material or Technology offering significantly improved levels inappropriate handling of the septa Shimadzu of durability clarity and accuracy Features of septa are selected to contribute low bleed and the Diamond Syringe Technology include optimum sealing for many injections e Longest working life in the industry e Improved solvent resistance e Greater operational temperature range e Reduced dead volume and carryover SAMPLE INTRODUCTION
5. 95 221 75189 LNRGC2010 20143 4MMIDPKT5 StraightThrough 5 0 3 4 95 221 75190 LNRGC2010 20143 4MMIDTAPFOC intowool PKT5 5 0 3 4 95 221 75191 LNRGC2010 2014SINGLETAPPKT5 5 0 3 4 95 221 75192 gt _ _ _ _ LNRGC2010 20140 75MMIDSPMEPKT5 5 0 0 75 95 221 75196 d GLASSINSERTSPLITLESS WBIWWOOLPKT5 5 0 3 4 95 221 75197 SAMPLE INTRODUCTION Septa High temperature silicone e Excellent durability resealing and solvent and tear resistant e Injection temperature up to 350 C lt gt 2 un Z O U CC 2010 CC 2014 Enduro Blue High thermal stable material in blue color 50 221 75180 2 O lt CC LLI CC LLI 1 ef gt lt WY SAMPLE INTRODUCTION Accessories Z 8 D Additional Accessories 2 Description EN C Capillary Ceramic Tube Cutter 3 pc 221 75181 5 Stainless Steel Nut 55 16 0125 5 670 11009 a SEPARATION O O SS un LLI RE CC D O CC SEPARATION Connections Ferrules are available in a variety of different materials shapes and sizes depending on their use the instrument and the size of the capillary column being used Probably the most important but difficult aspect of choosing a ferrule is the selection of the material type The table below will
6. GC Inlet Liners The GC inlet liner is where the sample is introduced and vaporized into the gaseous phase The geometry of each of Shimadzu s inlet liners is important and the correct choice of inlet liner can significantly improve the performance of the chromatography Inlet liner deactivation quartz wool quantity and position are essential to ensure reproducible and accurate sample introduction for each sample type SEPARATION GC Connections Ferrules and Unions Shimadzu provides an array of connection types for use in the GC each selected to ensure the best connection solution is achieved The correct 55 SEPARATION GC Capillary Columns selection of the connection type will eliminate dead volumes leaks during temperature cycling Shimadzu offers a range of stationary phases and problems with mismatched tubing sizes including non polar and polar functionalities SAMPLE PREPARATION MEPS MEPS is Micro Extraction by Packed Sorbent and is a development for sample preparation and handling MEPS is the miniaturization of conventional SPE packed bed devices from milliliter bed volumes to microliter volumes The MEPS approach to sample preparation is suitable for reversed phases normal phases mixed mode or ion exchange chemistries MEPS is available in a variety of common SPE phases MEPS BARREL INSERT AND NEEDLE The MEPS Barrel Insert and Needle BIN assembly Sp contains
7. If the injection port temperature is not specified in the method 250 C is usually the recommended temperature e Choose the appropriate inlet liner for your application review the inlet liner geometries in this Product Guide page 11 and suggested applications e f the inlet liner is not specified it is recommended to use a FocusLiner with quartz wool and bottom taper a The wool provides additional surface area for complete volatilization of the sample to minimize sample discrimination The two tapered sections Figure a It traps non volatile components and septum particles secure the quartz wool Quartz wool plug is in the plug effectively wiping the position to wipe needle tip needle tip during injection This results in improved reproducibility from reaching the column It wipes any sample from the syringe needle thereby Figure b Quartz wool plug can be moved in either direction preventing the needle increasing reproducibility and preventing sample residue build up at the septum e When choosing the inlet liner ensure the inlet liner volume wiping or sample is larger than the volume of vaporized sample If the vapor vaporization processes volume exceeds the liner s inner volume there will be an overflow of sample vapor from the liner resulting in Liquid Volume Inlet Temperature Inlet Pressure Gas Volume contamination of the inlet system which in turn leads to pU
8. help you choose the appropriate ferrule material for your application When choosing ferrules ensure you consider the following 1 The material that best suits your application 2 The connection type you want The following selection table will assist with your decision Features e Easy to use e Forms a stable seal e Soft material Porous to oxygen e Can be reused Forms a soft grip with capillary column e Low emissions e A composite of graphite and Vespel e Mechanically robust Hard material long lifetime e Forms a strong grip with capillary column e Cannot be reused with another capillary column Requires re tightening e Specifically developed to overcome the problems associated with the use of 10096 graphite and composite ferrules e Strong seal on capillary columns eak free The ferrule and nut expand and contract at the same rate eliminating any chance of leaks with temperature cycling e Nut does not need re tightening after initial temperature cycles Suitable Uses e Column to injector connection Non mass spectrometer detectors FID ECD TCD and NPD MS interfaces although even with a good seal will leak air compared to SilTite ferrules Ideal for MS interfaces due to leak free seal Not Suitable For Connecting columns to mass spectrometers as porous to oxygen High temperature applications Risks
9. names and logos used in this publication are trademarks and trade names of Shimadzu Corporation or its affiliates whether or not they are used with trademark symbol TM or amp Third party trademarks and trade names may be used in this publication to refer to either the entities or their products services Shimadzu disclaims any proprietary interest in trademarks and trade names other than its own For Research Use Only Not for use in diagnostic procedures The contents of this publication are provided to you as is without warranty of any kind and are subject to change without notice Shimadzu does not assume any responsibility or liability for any damage whether direct or indirect relating to the use of this publication C Shimadzu Corporation 2013 Printed in Japan 3655 05331 10AIT opino sejgeuunsuo 29
10. 0 12554 05 500 uL 50 25 0 5 0 2 Bevel 670 12510 20 500 uL 51 22 0 028 0 37 LC 670 12554 06 1 mL V Luer Lock 221 54778 01 Plunger Pk 1 221 54778 11 5mL Luer Lock 221 54778 02 Plunger Pk 1 221 54778 12 10 mL Luer Lock 221 54778 03 Plunger Pk 1 221 54778 13 25 mL Luer Lock 221 54778 04 Plunger Pk 1 221 54778 14 50 mL Luer Lock 221 54778 05 Plunger Pk 1 221 54778 15 100 mL Luer Lock 221 54778 06 Plunger Pk 1 221 54778 16 Luer Lock Needles 50 23 0 63 0 32 Bevel 221 54778 51 50 19 1 07 0 65 Bevel 221 54778 52 50 14 2 1 1 6 Bevel 221 54778 54 Syringe Valves 5 mL to 100 mL Luer Lock 221 54778 49 1mL to 100 mL Luer Lock 221 54778 50 SAMPLE INTRODUCTION GC Inlet Liners The GC inlet functions as the interface between the syringe and the GC capillary column where the sample is introduced vaporized mixed with carrier gas and transferred to the column Shimadzu instruments offer several types of inlets split splitless programmable temperature vaporization PTV and on column The inlet liner prevents the sample contacting the metal walls of the injector block Inlet liner geometry and packing materials enable the inlet liner to achieve greater heated surface area this additional surface area can often improve sample vaporization Conversely choosing the wrong inlet liner geometry can significantly decrease the reproducibility and quality of analysis Trace Level Analys
11. 21 74830 01 Plunger 1 221 74830 10 Syringes for AOC 5000 10 uL 50 26 0 47 0 11 Cone 221 75175 10 uL 50 23 0 63 0 11 Cone 221 75175 01 10 uL 80 26 0 47 0 11 Cone 221 75176 10 uL 80 23 0 63 0 11 Cone 221 75176 01 10 uL V 50 26 0 47 0 11 Cone 221 75175 02 10 uL 50 23 0 63 0 11 Cone 221 75175 03 25 uL 50 23 0 63 0 24 Cone 221 75177 1mL 50 26 0 47 0 15 Side Hole Dome 221 75178 1 mL V 50 23 0 63 0 15 Side Hole Dome 221 75178 01 2 5 mL V 50 26 0 47 0 15 Side Hole Dome 221 75179 2 5 mL 50 23 0 63 0 15 Side Hole Dome 221 75179 01 MEPS Syringes for AOC 5000 100 uL 221 75202 01 Plunger 1 221 75202 03 250 uL 221 75202 02 Plunger Pk 1 221 75202 04 Manual Syringes 5 uL 50 26 0 47 0 11 Bevel 221 75170 10 uL 50 26 0 47 0 11 Bevel 670 12552 01 10 uL 50 26 0 47 0 11 Bevel 221 75170 01 Plunger Pk 2 221 75170 02 10 uL 51 22 0 028 0 17 LC 670 12554 01 25 uL 50 25 0 5 0 2 Bevel 670 12510 31 25 uL 50 25 0 5 0 2 Bevel 221 75171 Plunger Pk 1 221 75171 01 25 uL 51 22 0 028 0 37 LC 670 12554 02 50 uL 50 25 0 5 0 2 Bevel 670 12510 36 50 uL 50 25 0 5 0 2 Bevel 221 75172 Plunger Pk 1 221 75172 03 50 uL 51 22 0 028 0 37 LC 670 12554 03 100 uL 50 25 0 5 0 2 Bevel 670 12510 18 100 uL 50 25 0 5 0 2 Bevel 221 75172 01 Plunger Pk 1 221 75172 04 100 uL 51 22 0 028 0 37 LC 670 12554 04 250 uL 50 25 0 5 0 2 Bevel 670 12510 19 250 UL 50 29 0 5 0 2 Bevel 221 75172 02 Plunger Pk 1 221 75172 05 250 uL 51 22 0 028 0 37 LC 67
12. Can leave residue inside your column If not re tightened after installation and Over tightening of the seal can e Can extrude into the injector or temperature cycles of the GC air may introduce leaks into the system detector if it is over tightened enter the column or detector Follow the recommended installation decreasing sensitivity of the analysis and instructions to avoid this problem possibly degrading the column as well as components of the system Operating Upper limit of 450 C Upper limit of 325 C No temperature limit in GC use Temperature 14 GC CONSUMABLES gt lt oc ee 255 3 LLI Ce Graphite GFF 505 050 10 221 75182 uj Graphite Vespel GVF16 005 10 670 15003 04 gt gt _ 6 __ 3 gt CS e lt L GVF16 008 10 670 15003 07 GVF16 004 10 670 15003 03 Metal SilTite 0 25 mm ID Column 10 221 72563 04 SilTite 0 32 mm ID Column 10 221 72563 05 5 SilTite 0 53 mm ID Column 10 221 72563 08 gt SilTite 1 32 ID Column 10 221 75200 04 E SilTite Kit 10 32 0 25 mm ID Column 1 221 75200 z SilTite Kit 10 32 0 32 mm ID Column 1 221 75200 01 Q SilTite Kit 10 32 0 53 mm ID Column 1 221 75200 02 SilTite Kit 1 32 ID Column 1 221 75200 03 SilTite Nut 10 32 0 8 mm ID Column 5 221 75186 z 9 l
13. Dirty Samples only if quartz wool is present Gaseous Samples also purge amp trap headspace Straight EE Straight inlet liners facilitate higher split flows Narrow bore straight inlet liners facilitate fast GC work Small injection volumes of less than 0 5 uL are best used with a narrow bore Narrow bore straight inlet liners improve focussing of gaseous samples purge trap amp headspace Inlet Liner Deactivation Every batch of inlet liners are tested for inertness using the EPA 8081B method This standard method ensures that each batch of inlet liners has less than 3 Endrin breakdown from a 1 ppm injection 11 GC CONSUMABLES SAMPLE PREPARATION E U E o Lu E lt Un SEPARATION TROUBLESHOOTING 12 GC 2010 LINERGC20103 4MMIDGNWWOOLPKT5 5 0 3 4 95 221 75193 O LNRGC20103 4MMIDGNPKT5 5 0 3 4 95 221 75194 a GC 2014 LNRGC20143 4MMIDGNPKT5 5 0 3 4 95 221 41444 05 LLL LNRGC20142 6MMIDPKT5 5 0 2 6 95 221 41544 05 n LNRGC20142 6MMIDTAPPKT5 5 0 2 6 95 221 41599 05 LINERGC20143 4MMIDWWOOLGNPKT5 5 0 3 4 95 221 75195 GC 2010 GC 2014 LNRGC2010 20143 4MMIDTAPFOC ontowool PKT5 5 0 3 4 95 221 75187 LNRGC2010 20143 4MMIDFOC ontowool PKT5 5 0 3 4 95 221 75188 LNRGC2010 20143 4MMIDFOC intowool PKT5 5 0 3 4
14. al diameter um 0 film thickness um similar chromatography e Columns should be conditioned to the maximum continuous temperature unless specified When conditioning columns with a film thickness 1 um at the maximum operation temperature it is recommended to do the initial conditioning without a connection to the detector to minimize contamination from the siloxane bleed Formula calculate Phase Ratio Column Length e Always try to select the shortest column length that will provide the required resolution for the application If the 3 7min ll 15 meters maximum column length available is being used and resolution of the sample mixture is still inadequate then try R 2 91 changing the stationary phase or internal diameter 7 5 30 meters e Resolution is proportional to the square root of the column efficiency therefore doubling the column length will only R 4 15 15 3min increase the resolving power of the column by do T4 meters approximately 4096 0 20 min Effect of Length Injection The function of the GC sample inlet is to introduce a representative portion of the sample as a narrow band onto the chromatographic column failure to achieve this objective will significantly reduce the separation capability of the GC column Because most samples are liquids an essential feature of the common GC inlet type is that the sample and solvent are vapo
15. choice for general liquid dispensing Side Hole Dome Samples are filled and dispensed through the side hole eliminating septum plugging of the needle Ideal for large volume gas injection The solid domed tip minimizes septum damage Valves OPEN 3 CLOSE The push button valve attaches directly to any luer lock 1 mL 100 mL Shimadzu syringe 1 E OPEN 4 CLOSE The push button valve attaches to any luer lock 5 mL 100 mL Shimadzu syringe GC CONSUMABLES SAMPLE PREPARATION E U E oc Lu E lt 54 SEPARATION TROUBLESHOOTING 10 Syringe PTFE Tipped Needle Length Needle Needle OD Needle ID Voltaic Plunger Ter Gauge Gaia Needle Tip P N Spare Parts P N Syringes for AOC 20i 5 uL 42 23 0 63 0 11 Cone 22175173 10 uL V 42 23 0 63 0 11 Cone 221 74469 Plunger C2 221 75173 01 10 uL 42 23 0 63 0 11 Cone 221 34618 10 uL 42 23 26 0 63 0 47 0 11 Dome 221 37282 02 10 uL 42 23 0 63 0 11 221 75174 Plunger 2 221 75174 02 Needle Pk 2 221 75174 01 50 uL 42 23 0 63 0 24 Cone 221 45243 250 uL 42 23 0 63 0 24 221 45244 Plunger 2 221 45244 01 MEPS Syringe for AOC 20i 100 uL 2
16. e preparation and analysis in a single platform AOC MEPS System lut bn 0707 Conditioning Sampling Dry MEPS BIN Elution Injection to GC When automated by AOC MEPS system the injection volume is much larger compared to the commonly used GC injection volumes of 1 2 uL With AOC MEPS the typical injections are 50 to 200 IIL of elution solvent into the analytical instrument A large volume injection volume technique should be employed that removes the solvent volume from inside the injector unit while condensing the target compounds PTV Inlet Liner for AOC MEPS System AOC 20i GC 2010 PTV configuration 3 5 2 5 95 221 4830 09 AOC 201 MEPS Syringe for AOC 20i 100 uL 221 74830 01 Plunger 1 221 4830 10 C18 5 221 74830 03 Silica 5 221 74830 04 C8 SCX 5 221 74830 05 C2 5 221 74830 06 C8 5 221 74830 07 PDVB 5 221 74830 02 SDVB 5 221 74830 11 HDVB 5 221 74830 12 Development Kit contains 1 each of C18 C8 Silica C8 SCX C2 1 of each phase 221 74830 08 AOC 5000 MEPS Syringes for AOC 5000 BEE 221 75202 01 Plunger 1 221 75202 02 Plunger 1 221 7520203 221 5202 04 C18 221 75198 01 221 75199 01 Silica 221 75198 02 221 75199 02 C8 SCX 221 7 5198 05 221 7 5199 03 C2 221 75198 04 221 75 199 04 C8
17. es A bottom taper focuses sample onto the head of the column and minimizes sample contact with metal parts of the inlet The addition of quartz wool to your inlet liner promotes TC Active Compounds 00 mixing of analytes aids the vaporization of liquid samples and works as a trap to collect non volatile residue in the sample i e protects capillary column from dirty samples inerTM Ensures quartz wool remains in the correct position in the General Purpose FocusLiner 9 MN D liner Excellent reproducibility results from the wiping of the Split Concentrated Samples l ae sample from the syringe needle and the prevention of droplet formation Minimizes high molecular weight discrimination Bottom taper focuses sample onto the head of the column Trace Level Analyses Taper FocusLiner and minimizes contact with metal parts of the inlet Excellent Splitless Dirty Samples reproducibility results from the wiping of the sample from Wide Boiling Point Range the syringe needle and the prevention of droplet formation Minimizes high molecular weight discrimination Direct Taper Direct inlet liners facilitate maximum transfer of sample by Trace Level Analyses Direct connecting directly to the GC column and inhibiting sample Active Compounds eee degradation due to hot metal components inside inlet Split Splitless General Purpose Concentrated Samples
18. fferences in dipole moments or charge distributions e To separate compounds that differ more in their hydrogen bonding capacities for example aldehydes and alcohols polyethylene glycol type phases are best suited such as CBP 20 Column Diameter e The smaller the diameter the greater the efficiency and better resolution Fast columns 0 1 mm ID are used for faster analysis because the same resolution can be achieved in a shorter time Film Thickness e For samples with a variation in solute concentration a thicker film column is recommended This will reduce the 47min possibility of broad overloaded peaks coeluting with other R Resolution 3 14 0 25 um compounds of interest If the separation of two solutes is R 3 60 sufficient and co elution is still unlikely even with large 7 Amin differences in concentration then a thinner film can be used 0 50 um R 4 96 The greater the film thickness the greater the retention of moet 1 solutes therefore the higher the elution temperature As Hull T _ 1 0 um rule doubling the film thickness results in an increase in 20 min elution temperature of approximately 15 20 C under Eet of Elm Thickness isothermal conditions Using a temperature program the increase in elution temperature is slightly less e Maintain phase ratio among different ID columns to yield id B 44 where phase ratio id column intern
19. flow is too low Solution Increase split flow or use the solvent effect to focus peaks Cause The column is contaminated Solution Cut 50 cm off the front of the column and re install Cause Mass spectrometer sampling rate is too low Solution Increase sampling rate or reduce the number of ions detected in SIM mode Cause Co elution of peaks Solution Change the temperature program or polarity of the column Cause Leaking septum Solution Tighten septum cap or replace septa Cause Dirty column if samples are dirty non volatile materials have deposited onto the column causing a change in polarity Solution Cut 50 cm off the front of the column and re install Cause Syringe is blocked or leaking around plunger Solution Inspect syringe and change if damaged Cause Column is blocked Solution Cut 5 cm off the front and back ends of the column and re install Cause Syringe has become contaminated from previous run Solution Ensure syringe has been thoroughly washed with solvent between injections Cause Septum bleed Solution Will appear as discrete peaks in a thermal gradient and disappear in an isothermal run Replace septum Cause A backflush event has occurred Solution Inject twice the amount of pure solvent repeat if necessary 19 SAMPLE PREPARATION GC CONSUMABLES SAMPLE INTRODUCTION Z C lt CC LLI WY TROUBLESHOOTING SHIMADZU Shimadzu Corporation www shimadzu com an Company names product service
20. ges If a syringe is being used by hand a manual syringe should be selected If a syringe is installed in an AOC autosampler then choose the appropriate syringe and volume to suit your instrument and application Shimadzu autosampler syringes are specifically designed to meet instrument dimensional specifications have an accuracy of better than x 1 and are designed for precise worry free overnight sampling Needle Tip Styles Cone GC Autosampler The cone shaped needle tip is specially developed to withstand multi injection demands and improve septum lifetime when used with the AOC autosampler The cone design effectively parts the septum during piercing instead of cutting it as would a bevel needle Bevel Manual GC _ The standard general purpose needle tip style supplied with many Shimadzu syringes is a 20 bevel tip It is the preferred option for manual injection where piercing the septum in exactly the same place is difficult The bevel tip is designed for optimum septum penetration and prevention of septum coring Dome M This style needle is recommended for use with predrilled septa The tip is rounded and polished to help septum penetration LC HPLC _ These needles are used for LC and HPLC valve injection and have a 90 square tip with rounded and polished edges This eliminates damage to the valve s rotor seal and stator face This needle tip style is a good
21. rized prior to reaching the column These GC inlets are known as Vaporizing injectors Below are several tips on the injector but you should also consider the function of the injection process and how it influences the chromatography If the injection is not performed correctly you will end up with poor accuracy and poor precision If you have an autosampler fitted you should follow the recommendations in your user manual to determine whether the autosampler is performing to specification The Syringe e Syringe life is influenced by the quality of the sample and the frequency of use a blunt needle will potentially deposit septa material into the inlet liner and severely impact your chromatography e For the best syringe life ensure your syringe is rinsed five to ten times with clean solvent after use Syringe washing also helps to eliminate carryover but remember to discard the initial washes e For optimal reproducibility and accuracy the smallest volume injected from any syringe should be no less than 10 of its total capacity for example the smallest recommended injection volume from a 10 uL syringe would be 1 pL SAMPLE INTRODUCTION SAMPLE PREPARATION GC CONSUMABLES SEPARATION 0 zm Wal LL oc 18 The Injector FocusLiner Conventional Liners e If you are doing trace analysis work or working with high injection port temperatures replace the septum regularly e
22. t oc LLI Un TROUBLESHOOTING 15 16 TROUBLESHOOTING The purpose of this information is to help you troubleshoot the performance of your chromatography your system manual is an excellent guide to help you troubleshoot the performance of the system The separation of structurally diverse analytes is often complicated by chance coelutions with other analytes or with matrix related compounds Often the column is blamed but while such coelutions make analysis difficult they do not necessarily indicate a faulty column poor chromatography or method design No single column or method will resolve all compounds that can be chromatographed so selecting a column that matches the needs of the application is an important first step Rather than attempting to modify a method to resolve coeluting peaks selecting a column with subtly different selectivity can achieve this aim without significant changes to established methods elution orders or run times The following are good starting points to not only develop the ideal method for your chromatography but also a guide on where you can troubleshoot to improve your desired separation Phase Selection e Select the least polar phase that will perform the separation you require Non polar stationary phases separate analytes predominantly by order of boiling point Increase the amount of phenyl and or cyanopropyl content in the phase and the separation is then influenced more by di
23. the stationary phase and is built into the TO BARREL syringe needle NEEDLE MEPS PACKED BED PTFE SEALING RING SAMPLE SIZE AND SENSITIVITY Sample volumes may be as little as 10 uL by taking multiple aliquots of 100 uL or 250 uL samples of 1 mL or larger be concentrated AUTOMATION Extract samples and make injections on line using a single device reducing sample processing times and the need for operator intervention SORBENT LIFE BIN life is dependent on the specific matrix being analyzed For example C18 analysis of whole plasma samples is conservatively 25 100 samples before the BIN needs to be changed BIN life of cleaner samples is significantly longer Chromatogram of 22 pesticides standard solution 40 ng mL 94 LLI lt E N 24 O L SAMPLE PREPARATION SEPARATION SAMPLE INTRODUCTION TROUBLESHOOTING CARRYOVER The small quantity of phase in the MEPS BIN is easily and effectively washed between samples to reduce the possibility of carryover This washing process is not practical with off line SPE devices With automation of MEPS washing occurs while the previous sample is running FLEXIBLE AND EASY TO USE The dimensions of the sorbent bed ensure performance remains identical to conventional SPE devices when used for extraction of similar samples The AOC MEPS system was developed to incorporate MEPS into a process automation workflow combining sampl
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