Agilent Technologies, Inc. · NYSE:A
Agilent Technologies — Technical Presentation (January 2020)
38 slides from Agilent Technologies's technical presentation, Jan 20, 2020
Slide 1: Mass Spectrometer Optimization
Mass Spectrometer Optimization Angela Smith Henry, Ph.D. Applications Chemist CSD Supplies Division 1 January 20, 2020 Mass Spectrometer Optimization Agilent Restricted
Slide 2: Agilent Inert Flow Solution
Agilent Inert Flow Solution Agilent UltiMetal Plus – TCD, FPD, NPD/FID jets Agilent UltiMetal Plus inlet weldment, shell and transfer lines Agilent Ultra Inert inlet liner Agilent UltiMetal Plus ferrules Agilent UltiMetal Plus capillary flow technology devices, Ultimate union Agilent J&W Ultra Inert
Slide 3: Is MS Method Development Different to Other GC Detectors
Is MS Method Development Different to Other GC Detectors How do I know if my flow conditions, gain, and scan speed are right? 3 January 20, 2020 Mass Spectrometer Optimization Agilent Restricted
Slide 4: Is MS Method Development Different to other GC Detectors?
Is MS Method Development Different to other GC Detectors? What do we need to think about? MS amenable parameters Column dimensions Length x 0.25 mm x <1 μm Column flow 1 to 2 mL/min** (**MS dependent) Solvent delay Dependent on solvent, column, GC parameters Source and quadrupole temperatures Analys
Slide 5: InertPlus vs. High Efficiency Source Mass Spectrometers
InertPlus vs. High Efficiency Source Mass Spectrometers InertPlus, extractor source High efficiency source (HES) • Inert source body • Inert source body • Familiar source body design to 5975 • Redesigned ion optics for greater ion transfer efficiency • Extractor lens voltage bias can increase ion tr
Slide 6: Data Quality: What Are the Best Flow Conditions to Use for MSD?
Data Quality: What Are the Best Flow Conditions to Use for MSD? Use constant flow methods 5977 Extractor, InertPlus, or older sources • Suggested flow rate range: 1 to 2 mL/min • Optimal flow: 1 to 1.2 mL/min 5977B High Efficiency (HES) source • Suggested flow rate range 1 to 1.5 mL/min • Optimal fl
Slide 7: Data Quality: What Is the Proper Column Installation into MSD?
Data Quality: What Is the Proper Column Installation into MSD? Agilent 5977 extractor or InertPlus, or 5975 MSD 5977B HES Installation length: 1 to 2 mm beyond end of Installation length: 5 mm beyond end of transfer line transfer line 5977 HES 5 mm beyond transfer line 1-2 mm beyond transfer line 59
Slide 8: Data Quality: Choosing the Right Type of Tune
Data Quality: Choosing the Right Type of Tune InertPlus, extractor source High Efficiency Source (HES) • Atune • Atune – Default, typical tune – Default, typical tune • Etune • HES_Atune – Applies voltage to extractor lens – Applies voltage to all optics – May get better sensitivity and S/N ratio –
Slide 9: Data Quality: How Do I Know if My Scan Speed Is Right?
Data Quality: How Do I Know if My Scan Speed Is Right? Best acquisition frequency • ~ 2.5 to 5 Hz Optimal number of points across peak • 8 to 12+ points across a peak Set scan speed at N=1 or N=2 • Frequency in 2.5 to 5 Hz range • Generally most samples will have 8 to 12+ points across a peak What a
Slide 10: Data Quality: How Do I Know if My Gain Is Right?
Data Quality: How Do I Know if My Gain Is Right? • Good practice: Start at gain 1 Process for testing gain levels: Do I need to increase my gain? • Best practice: Choose lowest gain factor for detection of most and least intense • Test gain factor in highest and lowest ions over target concentration
Slide 11: Data Quality: Source and Quadrupole Temperatures
Data Quality: Source and Quadrupole Temperatures Are they really that important? Source Quadrupole “Default” – 230 °C Default – 150 °C = Recommended Recommended: 250 to 280 °C More forgiving than source temperature Turn up the heat when: Turn up the heat when: • Running PAHs – up to 300 or 320 °C •
Slide 12: If My System Is Leak-free, What Should My Air Ion Abundances Be?
If My System Is Leak-free, What Should My Air Ion Abundances Be? • These are just estimates – H2O: ~2,000 counts (less is ok) – N2: ~10,000 counts (less is ok)* – O2: ~3,000 counts (less is ok) *Make sure to purge your Gas Clean filter High vacuum gauge pressure (for SQ): ~1 x10-5 torr† † dependent
Slide 13: Good Habit: Run a Manual Scan to Review Background Peaks
Good Habit: Run a Manual Scan to Review Background Peaks Understand what the normal scan range background looks like • Look at your normal scan range and an extended scan range • 35 to 500 and 10 to 700 • Use your normal threshold • Perform the scan after initial set-up and after major changes (new
Slide 14: Good Habit for Filament Care: Have an Extra Pair Ready
Good Habit for Filament Care: Have an Extra Pair (or Two) Ready • Have (at least) two extra filaments ready Filament may fail soon – More than one GC/MS system? Keep >2 on hand, depending on the number of systems. • Check filaments when you clean the source – Look for discoloration behind the filame
Slide 15: Good GC Habits and Flow Path = Happy MS
Good GC Habits and Flow Path = Happy MS 15 January 20, 2020 Mass Spectrometer Optimization Agilent Restricted
Slide 16: Good Habit: Have System Baselines
Good Habit: Have System “Baselines” Known standard: Agilent Semivolatiles checkout standard 5190-0473 What kind of system baselines? • System blank – Should only see a rise in baseline with temperature (column bleed) • Solvent blank – May contain contaminant peaks (for example, phthalates, siloxanes
Slide 17: Let's Talk About Gas Quality and Filters
Decreased retention Let’s Talk About Gas Quality and Filters Reduced response • Oxygen in carrier gas is detrimental to GC/MS – Reduced response – Elevated background – Irreversible column damage – Impaired electron multiplier function – Premature filament, liner lifetime • Use UHP carrier gases – 9
Slide 18: I Have Gas Filters and High-Quality Gas, but I Still Have a High Background
I Have Gas Filters and High-Quality Gas, but I Still Have a High Background Use manual tune (before any experiments) to check for leaks/background • Ions 18, 28, 32 m/z 21 January 20, 2020 Mass Spectrometer Optimization Agilent Restricted
Slide 19: I Have Gas Filters and High-Quality Gas, but I Still Have a High Background
I Have Gas Filters and High-Quality Gas, but I Still Have a High Background Use manual tune (before any experiments) to check for leaks/background. • Ions 18, 28, 32 m/z 60,000 counts for N2 is definitely high What to check: 1. Verify gas fittings are leak-free Water/methanol mixture (external to GC
Slide 20: I Have Gas Filters and High-Quality Gas, but I Still Have a High Background
I Have Gas Filters and High-Quality Gas, but I Still Have a High Background Use manual tune (before any experiments!) to check for leaks/background. • Ions 18, 28, 32 m/z 60,000 counts for N2 is definitely high What to check: 1. Gas line fittings (done) 2. Check the vent valve, MSD transfer line nut
Slide 21: Use Leak Detector or Electronics Duster to Find Your Leaks
Use Leak Detector or Electronics Duster to Find Your Leaks Why use a leak detector? Typical Electronic Duster Components and Ions • High sensitivity 1,1- m/z • Recommended for leak detection in gas plumbing difluoroethane 51,65 and fittings 1,1,1- m/z 69 trifluoroethane 1,1,1,2- m/z tetrafluoroethan
Slide 22: Using Electronics Duster to Find System Leaks: Manual Tune
Using Electronics Duster to Find System Leaks: Manual Tune Navigate to MSD Manual Tune in the Data Acquisition • Instrument > Edit Tune Parameters Or • View > Tune Vacuum Control – Parameters > Manual Tune MassHunter data acquisition 25 January 20, 2020 Mass Spectrometer Optimization Agilent Restric
Slide 23: Using Electronics Duster to Find System Leaks: Manual Tune
Using Electronics Duster to Find System Leaks: Manual Tune • Use Profile tab to watch the main ions (69 and 83 m/z for my electronics duster) • Spray short bursts at vent valve, transfer line, and side door 26 January 20, 2020 Mass Spectrometer Optimization Agilent Restricted
Slide 24: Check the Transfer Line Nut for Leaks
Check the Transfer Line Nut for Leaks • Using a graphite/vespel ferrule – Install with the flat end of ferrule facing the MSD • Nut “loosens” with heat cycles • If you find a leak: – Tighten in small increments and then check again until no leak – Try to not overtighten the nut • If you have to appl
Slide 25: Self Tightening Column Nuts: No Leaks, No Downtime, No Frustration
Self Tightening Column Nuts: No Leaks, No Downtime, No Frustration • Spring-driven piston continuously presses against ferrule • Automatically retightens when ferrule shrinks • Wing design for finger tightening • Easier and faster to install • Collar holds column in place • No tools needed For mass
Slide 26: Easier Installation into the Mass Spectrometer with the New Self Tightening Column Nut and Collar
Easier Installation into the Mass Spectrometer with the New Self Tightening Column Nut and Collar 29 January 20, 2020 Mass Spectrometer Optimization Agilent Restricted
Slide 27: Good Habit: Check Other Connection Points in the GC
Good Habit: Check Other Connection Points in the GC • Check the inlet – Installed with a quarter turn with a wrench • Inlet nut may need slight tightening after heating cycles – Or, preswage flexi-metal ferrules – Or, use Self Tightening column nut for inlet • Use graphite/vespel ferrules with self-
Slide 28: Remember to Do Pre-emptive Maintenance, so This Doesn't Happen to You
Remember to Do Pre-emptive Maintenance, so This Doesn’t Happen to You Known, good run Recent run methampehetamine oxycodone MDA MDEA MDMA Trazadone 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 min 31 January 20, 2020 Mass Spectrometer Optimization Agilent Restricted
Slide 29: Thank you for your attention
START FINISH Step 1 Step 2 Step 3 Step 4 Step 5 What does a Develop steps working Half split the Make repairs, Put the system to prevent re- GC/MS look problem as necessary back together occurrence like? Thank you for your attention 32 January 20, 2020 Mass Spectrometer Optimization Agilent Restrict
Slide 30: 40% off GC and LC Columns, Sample Preparation Products, and Supplies
40% off GC and LC Columns, Sample Preparation Products, and Chromatography, Dissolution, and Spectroscopy Supplies. Please reference promotion code 1592 when ordering. ORDER TODAY – this promotion only lasts thru January 28th, 2020! **Valid in US, Canada, and Mexico ONLY. Valid on orders up to list
Slide 31: January 20, 2020 Mass Spectrometer Optimization
34 January 20, 2020 Mass Spectrometer Optimization Agilent Restricted
Slide 32: Switching Methods from High Flow Rates or Different Column Dimensions
Switching Methods from High Flow Rates or Different Column Dimensions Method translator 35 January 20, 2020 Mass Spectrometer Optimization Agilent Restricted
Slide 33: Too Many Peaks Case Study: What Are These Repeating Peaks?
Too Many Peaks Case Study: What Are These Repeating Peaks? Is it column bleed? Are these peaks from my solvent? 36 January 20, 2020 Mass Spectrometer Optimization Agilent Restricted
Slide 34: Septum Maintenance: TIC of an Inlet Septum
Septum Maintenance: TIC of an Inlet Septum Common ions for Septa contamination in wash vials or inlet liners can be diagnosed by looking for siloxane polymers in your total ion siloxane chromatogram. Each peak in the chromatogram corresponds to a cyclized (ring structure) siloxane molecule. These mo
Slide 35: One Last High Background Discussion: Troubleshooting Column Bleed
One Last High Background Discussion: Troubleshooting Column Bleed Have you installed or conditioned the column? Column bleed Are you exceeding the column’s upper temperature limit? Is your column’s film size too thick? Could leaks be present in your flow path, or Original chromatogram are your carri
Slide 36: What Steps Should I Follow When Troubleshooting?
What Steps Should I Follow When Troubleshooting? 40 January 20, 2020 Mass Spectrometer Optimization Agilent Restricted
Slide 37: Follow a Logical Troubleshooting Procedure
Follow a Logical Troubleshooting Procedure START FINISH Step 1 Step 2 Step 3 Step 4 Step 5 What does a Develop steps working Half-split the Make repairs, Put the system to prevent re- GC/MS look problem as necessary back together occurrence like? 41 January 20, 2020 Mass Spectrometer Optimization Ag
Slide 38: Troubleshooting Starting Points
Troubleshooting Starting Points • Do method parameters match what you see in/on the system Check parameters • Are sample/wash vials dirty or have particulates? • Watch syringe moving/make an injection, or remove syringe and manually pull up solution. Autosampler • Try a manual injection to rule out
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