5975 inert MSD. Chris Sandy European GC-MS Product Specialist Agilent Technologies
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1 inert MSD Chris Sandy European GC-MS Product Specialist Agilent Technologies
2 Welcome to our e-seminar: Introduction of the new inert MSD for expanding your application capabilities Presenter: Chris Sandy
3 What Has Changed? What s the same? Reliability Quality Inertness But NOT Performance it s better! Slide 3
4 What s Different? Functional industrial design More efficient vacuum system Extended mass range AutoCI New sensitivity specifications Synchronous SIM/Scan EI with CI ion source 6850 GC control QuickSwap MSD interface Review of differentiators Slide 4
5 Quick Remove Top Cover Easy analyzer access Slide 5
6 Functional Front Window Wire connections Filament operation Column insertion CI Source identification Slide 6
7 Modified Mainframe Modified MSD mainframe for quick/easy turbo pump maintenance New turbo and mechanical vacuum pumps are more efficient for Helium and Hydrogen New 70 L/sec standard pump New 262 L/sec performance pump New 2.5 m 3 /hour mechanical pump (67% more capacity) Slide 7
8 Integrated Ion Gauge/Controller Greater vacuum precision Excellent for trouble shooting small leaks every system should have one! G3397A optional gauge/controller Local display Software display Slide 8
9 New Sensitivity Specifications EI Scan 5973 EI 1 pg OFN 60:1 100:1 182:1 s/n Slide 9
10 New Sensitivity Specifications CI Scan 5973 PCI 100 pg BZP NCI 1 pg/100 fg OFN 75:1 500:1 (1 pg) 125:1 300:1 (100 fg) 704:1 s/n (100 fg OFN under NCI) Slide 10
11 Extended Mass Range 1050 m/z for inert MSD Quadrupole modified New electronics 800 m/z for all 5973 MSDs (Software upgrade does not enable 1050 m/z) Slide 11
12 Extended Mass Range PBDE 209 Slide 12
13 Extended Mass Range PBDE inert MSD Theoretical Slide 13
14 AutoCI AutoCI Fully automated setup/tuning No external manual control CI made as easy as EI! The new CI interface The old 5973 manual CI interface Slide 14
15 Automated EI with CI Source March 2004: 5973 MSD Application note on EI with CI ion source EN Now: MSD Automated switching between EI and CI in a sequence Slide 15
16 Automated EI with CI Source Setup steps: 1. Install CI Source 2. Tune instrument in PCI create PCICH4.u 3. Auto create EI tune file create ei-cisource.u 4. Tune instrument in NCI NCICH4.u 5. Assign tune file with method and run in sequence Slide 16
17 6850 GC Control via 5973N MSD (G2570A) 5973 inert MSDs inert MSDs Slide 17
18 Agilent MSD Unique Features Inert Ion source Hyperbolic quad Quad temp CI system Analyzer modularity Slide 18
19 Synchronous SIM/Scan
20 Set Up Synchronous SIM/Scan SIM/Scan data analysis requires mixed mode data view. SIM/Scan data is saved in the same data file directory. Slide 20
21 Comparison of SIM/scan Implementations Implementation (1) coarse granularity Implementation (2) fine granularity at specific times Agilent Implementation fine granularity for whole acquisition time TIME Scan SIM Slide 21
22 Synchronous SIM/Scan AutoSIM AUTOSIM is a standard feature of G1701DA Software AUTOSIM provides rapid and automatic conversion of a Scan method to SIM/Scan AUTOSIM creates SIM method based on Calibration table The operator has fine control over SIM parameter settings The SIM ions/groups/times are saved automatically to the method Slide 22
23 Inject Standard Slide 23
24 AutoSIM Application note: EN Slide 24
25 Edit SIM Method AutoSIM automatically creates SIM groups and populates ions in each group Slide 25
26 Synchronous SIM/Scan Slide 26
27 Scan and SIM Chromatograms from SIM/Scan Analysis of 60 VOCs at 1 ppb Each Scan TIC: 1 ppb 60 VOCs.D\DATA.MS SIM TIC: 1 ppb 60 VOCs.D\DATASIM.MS Velocity XPT/6890N/ P&T/GC/MS system 20-m X 0.18 mm X 1.0 µm DB-VRX column Scan sampling rate = 2; Dwell =20 ms for SIM Slide 27
28 Synchronous SIM/Scan Analysis of VOC Target Gases at 1 ppb each Scan SIM VOC Gases (1 ppb each) 1. Dichlorodifluoromethane 2. Chloromethane 3. Vinyl chloride 4. Bromomethane 5. Ethyl chloride 6. Trichlorofluoromethane Slide 28
29 SIM/Scan and Scan-Only Sensitivity Comparison: 5-mL Purge of 1 ppb Ethyl Chloride (a Low Responding Gas) SIM (SIM/Scan) Scan (SIM/Scan) Scan (Scan only) RMS S/N Peak/Peak S/N SIM as part of SIM/Scan run gives 10X greater sensitivity Still get 8 scans across peak using same scan rate (n = 2) Slide 29
30 Why Our SIM/Scan is So Good Standard Electronics ~ 781 amu/sec 2 1 Fall off with increasing scan speed 100 Performance Electronics ~ 781 amu/sec 2 0 ~ 6250 amu/sec Nearly no fall off with increasing scan speed ~ 6250 amu/sec Moving from 2 3 to 2 2 doubles scans Phenanthrene Phenanthrene Slide 30
31 Scan SIM/scan Scan 45 to 555 => 510 amu 45 to 555 amu, Scan 2^2 SIM 4 ions, 40 ms 1563 amu/s 2^ amu/s a cycle 2.87 scan/sec 3.76 cycle/s Same width (SIM) 1 sec 2 sec 2^ amu/s 2.88 cycle/s 2^ amu/s 1.94 cycle/s For a 0.25 mm column, a typical peak width (at base) is 6 seconds. Switch from scan at 2^2 mode to SIM/scan@2^1, there will still be the same 15 cycles over the peak, but gets the 4-ion SIM group data for FREE. Slide 31
32 Synchronous SIM/Scan Key Features Performance Electronics really make the difference SIM Improvements 100 groups and 60 ions per group Minimum dwell time is reduced by half to 5 ms Even more data points per SIM peak Synchronous SIM/Scan available on 5973 MSDs with performance electronics (req. Smart Card 3+) Upgrades: G1088A and G1088B AND SW upgrade Slide 32
33 Synchronous SIM/Scan Application examples Allergens analysis: Proposed method, 26 Targets SIM/Scan mode - SIM table built with AUTOSIM - Quant with SIM target ion - Confirmation by DRS with Scan data Pesticides analysis with microfluidics technology for flexible GC and GC/MS analysis Slide 33
34 Allergens analysis in SIM/Scan After shave 1% v/v 1ul Split 20 : 1 SCAN SIM Slide 34
35 Allergens Overlaid SIM/Scan Slide 35
36 Allergens SIM/Scan analysis and deconvolution with DRS Quant based on SIM target ion Confirmation based on deconvoluted full mass spectrum With courtesy of Chris Sandy and J-F Garnier Slide 36
37 Synchronous SIM/Scan Great for target analysis and identifying unknowns SIM data for quantitation Scan data for confirmation of unknowns Our SIM/Scan delivers real performance based on superior electronics Slide 37
38 Overview of Microfluidic Technologies
39 Connections to Microfluidic Splitter To Detector 2 To Detector 1 Column Nut Metal Ferrule Channel Plate Deactivated, very low internal volume to prevent peak tailing or band broadening A single, special design metal ferrule More inert that graphite/vespel, does not leak at high oven temperatures Slide 39
40 Microfluidic Splitter hardware installation Deactivated microfluidic splitter operates to 350 C. Uses metal ferrules to eliminate leaks and retightening Makeup from Aux EPC Column in To Det 1 To MSD Slide 40
41 Microfluidic Splitter operating modes * (1) Single Column AUX EPC Blocked Column in MSD * Aux EPC Flow enables column change-over without venting MSD * Aux EPC Flow enables inlet / septum maintenance without ingress of air into column. Slide 41
42 Microfluidic Splitter operating modes (2) Splitter AUX EPC Column in Detector 1 MSD * Aux EPC Flow enables column change-over without venting MSD * Aux EPC Flow enables inlet / septum maintenance without ingress of air into column. Slide 42
43 Splitting to 2 Detectors Configuration for 2:1 Split to MSD Autosampler AUX EPC 3.8 psig mecd Effluent Splitter with Makeup m X 0.18 mm id Column 1.1 m X 0.18 mm id Inert MSD 6890N GC 15 m X 0.25 mm id X 0.25 um HP-5MS Slide 43
44 Microfluidic Splitter Chromatographically Transparent MSD ECD Slide 44
45 100 ppb VOAs, 100 ppm Gasoline in Water, Ambient Headspace Scan SIM ECD Slide 45
46 Microfluidic Splitter operating modes :(3) Dual Column Inlet AUX EPC Column 1 / Inlet 1 Column 2 / Inlet 2 MSD * Aux EPC Flow enables column change-over without venting MSD * Aux EPC Flow enables inlet / septum maintenance without ingress of air into column. Slide 46
47 Dual Column Configuration* Back : 30m x 0.25mm ID x 0.25um HP5-MS 25 mins Front : 12.4m x 0.25mm ID x 0.25um HP5-MS 6 mins *Requires performance turbo pump Slide 47
48 Microfluidic Splitter operating modes : (4) Dual Column Inlet + Olfactory Port + MSD AUX EPC Column 1 / Inlet 1 Column 2 / Inlet 2 MSD ODO II * Aux EPC Flow enables column change-over without venting MSD * Aux EPC Flow enables inlet / septum maintenance without ingress of air into column. Slide 48
49 Microfluidic Splitter operating modes * (5) Splitter mode with Backflush Splitter mode acquiring data AUX EPC 3.8 psig Column inlet psig Detector 1 MSD Backflush mode * Aux EPC Flow enables column change-over without venting MSD * Aux EPC Flow enables inlet / septum maintenance without ingress of air into column AUX EPC 25.0 psig Column inlet 1.0 psig Detector 1 MSD Slide 49
50 6890N/ inert Pesticide Analysis with 3-Way Splitter 1X method with 10:10:1 split FPD:MSD:ECD Auto-sampler Phosphorus FPD AUX EPC 3.8 psig uecd 3-way Effluent Splitter with Makeup 6890N GC Column 30 m X 0.25 mm id X 0.25 um HP-5MS Inert MSD Slide 50
51 1-injection-4-signal System, RTLocked, 30m x 0.25mm x 0.25um HP-5MS Samples: pesticide mix at 10, 1, and 0.1 ppm Injection: 10:1 split At the end of the column, eluent flow is split 3 ways: MSD:FPD:µECD = 10:10:1 Injection 10 ppm (10000 pg) 10:1 split 1000 pg ~480 pg ~48 pg ~480 pg SIM/Scan µecd FPD Slide 51
52 SIM/scan + 3-way splitter Ultimate Pesticide System Scan: ~ 480 pg SIM: ~ 480 pg µecd: ~ 48 pg FPD: ~ 480 pg 7 peaks Slide 52
53 QuickSwap MSD interface Available October 1st, 2005 Replacement for NoVent Column Remove column w/o venting Backflush mode Inlet maintenance reverse flow Removes heavies from column Maintain constant flow to MSD EPC inlet MS Transferline Microfluidic technology Requires performance turbo for flow rates > 2 cc/min Slide 53
54 Introduction to s and the new MSD Chemstation
55 What are s? s is short for Electronic Methods. Can now package existing GC/MSD methods Export them to other 5973 MSDs Export them to inert MSDs Slide 55
56 Benefits Fast setup of new inert MSD Method sharing between 5973 and MSDs Download apps from website and import entire method into MSD Slide 56
57 New inert s PBDE Flame Retardants SIM/Scan Pesticides in Water and Food VOCs via Headspace European method Residual Solvents via Headspace NIDA Drugs Slide 57
58 MSD Software Two GC/MS per GC and GC/MS control Retention time locking Custom reports s Four configurations Enhanced mode EnviroQuant DrugQuant Reformulated Gas Most popular GC/MS software in the world Slide 58
59 Instrument Control Enhancements Combined Top/Instrument Control Screen New icons for quick access to tune, EMF and print Configurable sequence table More right mouse click functions in editing sequences Printing selected sections of method and sequence Import of GC method parameters (excluding 5890 GC) Display of IP address(s) of GC and MSD instruments Slide 59
60 Data Analysis Enhancements Explorer-style navigation tool Interactive editing of Integration Parameters Switchable right mouse click functions Spreadsheet-like SIM Parameters Table Icons for custom tools, DA options, variable watch Toolbar on/off capabiity Selectable DA color themes Slide 60
61 Data Analysis Enhancements QEdit functionality is improved: Separate window for Baseline Display Generating reports directly from QEdit Custom configuring X-axis Slide 61
62 Explorer Navigation Explorer navigation Slide 62
63 Interactive Edit Integration Slide 63
64 Right Click Features Slide 64
65 SIM Parameter Table Slide 65
66 QEdit Baseline Display Reports Slide 66
67 Library Options NIST05 NEW Wiley 7 th ed Stan pesticide Pfleger/Maurer/Weber MS Drug Library, 3 rd ed NIST Chemical Structures Library Slide 67
68 Other Software Options Deconvolution Reporting Software - New Revison A.02 released Aug 1, 2005 Security Headspace software RTL Pesticide Database : FAMES, Flavors, Volatiles Organics, Organotin derivatives, PCB congeners, Forensic toxicology Slide 68
69 Expanding the portfolio of RTL / DRS Databases Updated RTL Pesticides Database, Nov 2005 Adding ~ 200 new compounds TIC Toxic Industrial Chemicals Database, Nov 2005 ~ 800 compounds (VOC, SVOC, Dioxins, PCBs and Pesticides) Slide 69
70 GC/MS Configurations 5973N inert inert XL EI with diffusion pump EI with standard turbo pump EI with performance turbo pump EI/PCI/NCI with performance turbo pump All systems available with choice of either 6850 or 6890 GCs Slide 70
71 Agilent Inert MSD Better reliability and quality Enhanced performance s AutoSIM and SIM/scan Higher mass range AutoCI Sensitivity Software improvements Slide 71
72 Wrap-up E-Seminar Questions Thank you for attending today s Agilent e-seminar. Our e-seminar schedule is expanding regularly. Please check our web site frequently at: If you would like to receive regular updates please update your account information under Stay Current with e-notes Slide 72
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