Agilent MSD EI CI Source Cleaning Installation Manual
Contents
1. 5971 and 5972 MSD Series it is not the preferred method of cleaning for the newer sources of the 5973 and 5975 MSD Series Instead apply the following approach 1 Make a slurry or paste of the alumina MICROGRIT supplied with the instrument by adding deionized water to a small amount of the MICROGRIT powder refer to Figure 4 The consistency should be a little thick 2 Use the supplied cotton tipped swabs to apply a small amount of the MICROGRIT water paste to the metal components Rubbing will remove enough material to produce a clean and shiny surface In cleaning the source bodies of the EI and CI sources it is important to also clean the fila ment holes Use a wooden toothpick to apply the MICROGRIT paste to the holes and also to remove or clear MICROGRIT from the filament holes as the last step in cleaning the source bodies The parts most prone to contamination are the source body repeller and drawout lens These should be cleaned with special attention 3 Rinse all parts in deionized water Remove as much MICROGRIT as possible at this stage Submerge all the rinsed parts in a beaker of deionized water and sonicate for about 5 min utes Steps 4 5 6 and 7 refer to Figure 5 5 Use metal tweezers to remove the parts care fully from the beaker of water and submerge them in a beaker of methanol pesticide or HPLC grade Sonicate for about 5 minutes 6 Use metal tweezers to remove the parts care full2. MSD El and CI Source Cleaning and e Installation e r ee a o Oe J Introduction During the course of operation eventually GC MSD sources require cleaning This can be indicated by a loss in analyte response that is not improved by GC inlet and column servicing or in source tuning by poor calibrant ion peak shapes or escalating repeller or electron multiplier voltages Consider Figure 1 which shows the difference in response for several pesticides before and after proper source cleaning Proper cleaning assembly and installation are essential to robust and reliable operation espe cially for the assembly of the CI ion source A vari ety of source cleaning methods exist in laboratories Technical Overview Charles Thomson Max Ruemler Mickey Freed Dave Peterson and Harry Prest around the world some advocating polishing com pounds soaps or harsh agents These most often work for a very limited application range and never are successful over the long term perfor mance of the source For example most polishing compounds and some soaps contain high molecu lar weight waxes which produce a raised back ground and lowered response Chemical agents can adversely affect the source surface chemistry and increase activity Based on many years of experience this overview describes a simple approach to cleaning and re installing the 5973 and 5975 ion electron i
3. e fA a i e amp 0 Sa J t vU lt a 3 nen aiiu b ee x Sonicate gt Sonicate gt Sonicate gt Sonicate 5 min 5 min 5 min 5 min Removes salts Removes polar agents Removes non polar agents Solvents must be very clean Especially the hexane Figure 5 lon Source cleaning sequence two squeaks are heard Remember that after the transfer line has been heated the ferrule will have to be tightened again It should be checked for tightness consistently as this is a major source of leaks when the transfer line is temperature cycled Another approach is to use the SilTite metal fer rules part number 5184 3569 for 0 2 to 0 25 mm id columns These ferrules must be carefully tight ened When properly installed they form a stable seal that does not require constant readjustment after temperature cycling An ion source should never be heated until it is established that there is a good vacuum This means checking that there are no leaks and that the water has been lowered Heating a source to operating temperatures in the presence of a leak or high water background can activate it essentially undoing the effort of the cleaning process A better procedure is to pump down the system with the source quad and GC zone temperatures cold i e set to 0O C wait 20 minutes and examine 1 Does the vacuum gauge indicate the manifold pressure is coming down Or is the foreline pressure dropping toward operating val
4. iles of the performance W Sample Log Table J 15 x Data Path C MSDCHEM 1 PFDTD Method Path C MSDCHEM 1 PFDTD T s i Method Data Comment ype i Keyword File KeywordString 1 Keyword Command BAKE 300200 8 Keyword Tune Sample 1 Checkout standard CHECKOUT Checkout Sample 1 Checkout standard CHECKOUT Checkout2 Read Barcode Cancel 1 Calls Bake Macro Bake Source Temp QuadTemp Hours This example sets source to 300 and quad to 200 for 8 hours 2 Runs AUTOTune 3 4 Checks Standards using the method CHECKOUT M Figure 9 Pumpdown sequence Checkout S www agilent com chem For More Information For more information on our products and services visit our Web site at www agilent com chem Agilent shall not be liable for errors contained herein or for incidental or consequential damages in connection with the furnishing performance or use of this material Information descriptions and specifications in this publication are subject to change without notice Agilent Technologies Inc 2006 Printed in the USA December 11 2006 5989 5974EN Eee Agilent Technologies
5. imums allowed 300 C for the ion source and 200 C for the quad in the Manual Tune Panel or from the Source Temperature Panel and saved Figure 8 An automated approach uses the macro Bake mac Here the user has pumped the system down checked that the system is leak free and loaded their method and this checkout sequence Typi cally this Checkout M method is used to confirm the performance of the instrument after a servic ing This macro operates in a sequence such as i Edit Parameters 5973N VENT_U Mi x File Execute Calibrate MoreParamns View scan 10 00 210 00 105 peaks lon Pol POS MassGain 245 Base 18 10 Abundance 33160 MassU ffs 10 100 Emission 34 6 AmuG ain 2152 EleEnergy 63 9 Amullts 124 Filament 1 idaig 0 029 i Acquisition amp Display Param E3 Masses Acquisition Mase 1 18 00 Mase 2 26 00 Mass 3 32 00 Samples 2 N 4 Averages 3 Step ize 0 10 Threshold 100 Window 30 DCPo Pus lt Repeller 28 11 lonFocus 89 2 HED ON From 10 00 Tol 210 00 Pilare 21 0 EMVolts f 1529 Profile Display Ent ffs 18 57 Scale SUTEERRE Autoset f Absolute PFTBA CLOSE C Relative Percent C Fised From 0 Taf 1000000 59 Tubospd 100 A Scale Factor 1 00 Cancel Help Emission 0 0 to 315 2 34 6 Th eal Scar 10 00 210 02 Samoles d Thresh 10 Prat Scan Ramp S mso Cancel Help Figure 7 Pumpdown bac
6. kground checking Input Bake parameters check tune fi Mp Y L Can not exceed TUNE file Source bake temperature 300 recommended setpoints 300 Quad bake temperature 200 recommended Bake temps 200 Bake Time in hours 6 Bake time Source final temperature 230 Quad final temperature Final Temps 150 Cancel Figure 8 This is for manual bakeout of the source and quad Add the file C MSD CHEM MSEXE Bake mac Call as macro bake mac go lt enter gt that shown in Figure 9 Line by line this checkout standard to see that the instrument is operating sequence within the required specifications of the user s analysis 1 Calls the bake mac and sets the baking temper atures of the ion source and quadrupole and the hours of bake time as BAKE SourceTemp Instructions for Downloading the Macros QuadrupoleTemp Hours Here the figure shows from the Agilent Web Site the source is baked at 300 C and the quadru pole at 200 C for 8 hours Go to http www chem agilent com cag servsup softdocs ssbMain html anch MS You must Regis ter and acquire a username and a password You also must have a valid MSD Productivity ChemSta tion registration number Then go to the MSD 2 Source and quadrupole return to the tempera tures of the loaded method tune file and then executes an AutoTune 3 Injects a method performance standard twice The user can then examine the tune report for air and water and the dataf
7. mpact ED inert and standard sources and the chemical ionization CI source Figure 1 mechanical cleaning Overlaid RTICs for Azinphos ethyl left and the Demeton isomers right before lower trace and after upper trace Agg Agilent Technologies Precautions Like all laboratory work involving flammable or potentially toxic solvents the appropriate precau tions should be taken All solvents glassware and foil must be clean and free of contamination and exchanged as necessary during the cleaning process Before starting a source cleaning consumables such as the filaments or spare parts such as repeller ceramics should be on hand Cleaning Procedure Source disassembly is described in the hardware manual and associated video refer to Agilent 5973 and 5975 Series MSD Hardware User Information DVD It is important that all ceramics the entrance and ion focus lenses insulator the source heater block all screws and the filaments are ai Disassembled and separated El source components Figure 2 Figure 3 El and CI Source metal components for cleaning always placed on a clean lintless material like sol vent rinsed or fired foil and are never exposed to any solvent refer to Figure 2 Separating the metal parts for cleaning makes this easier Figures 2 and 3 In the past the green paper was recommended for cleaning sources While this is still applicable to the Agilent
8. ues 2 Then if pressures look good enter the Manual Tune panel and examine the air and water values Figure 7 If nitrogen 28 m z has dropped to lt 25 000 counts absolute then the system is mainly airtight Water will drop more slowly and requires system baking 3 Load the analytical method The philosophy for operating in this manner is that if there is a leak the instrument zones are still cold so the user can troubleshoot immediately without waiting for the zones to cool The macro Bake mac is called as macro bake mac go lt enter gt from the command line The user is prompted for the baking temperatures and the duration of the bake refer to Figure 8 Bake mac should be loaded or located under the msdchem msexe directory This macro requires MSD ChemStation G1701DA rev DO8 or higher If the macro is not located under the directory users may obtain it from the Agilent Web site if they login as users and have a registration number for their software More detailed instructions are given below Figure 6 Installed and conditioned column in MSD Pull back column until 1 mm extends beyond the interface tip Analyzer Baking Automated Baking and Performance A useful macro allows baking of the source and Checkout quadrupole to lower water background and improve performance in tuning and acquisition This requires that the tune parameters allow higher source temperatures and these should be set to the max
9. y from the beaker of methanol and submerge them in a beaker of acetone pesticide or HPLC grade Sonicate for about 5 minutes T Use metal tweezers to remove the parts care fully from the beaker of acetone and submerge them in a beaker of hexane pesticide or HPLC grade Sonicate for about 5 minutes 8 Use metal tweezers to remove the parts care fully from the beaker of hexane and place them on clean foil or lint free tissue Carefully Figure 4 Microgrit and slurry reassemble the source as instructed in the manual Inspect the filaments and replace them if they look worn Be especially careful with the ceramics for the repeller to ensure that they are not cracked which usually happens if they have been overtightened 9 Immediately reinstall the source in the MSD Do not bother baking the source in an oven as the source should be very dry after the acetone rinse and free of organics after the hexane rinse which rapidly evaporates Only residues in your solvents will remain hence the require ment for very clean solvents Reinstallation Procedure If the GC column is being installed it should be properly conditioned outside the MSD first and then installed through the MSD transfer line After extending through the transfer line it should be trimmed and pulled back until just 1 mm extends past the tip of the transfer line interface Figure 6 Tighten the transfer line ferrule until i Methanol g Methan
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Agilent MSD EI CI Source Cleaning Installation Manual