Slide 1: Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance
Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Alexander Ucci and Mark Sinnott Application Engineers May 30, 2019 1 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 2: Agenda
Agenda • Unboxing/“getting to know your column” • Install the column • Preventive measures • Corrective measures • Latest instrument developments Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 2 May 31, 2019 Keeping your GC Column Happy and Healthy:
Slide 3: Column Construction
Column Construction Polyimide coating Flexible polymeric coating; adds mechanical strength and temperature stability to fused silica Fused silica Amorphous glass-like tubing comprised of silicon dioxide; high temperature resistance, low reactivity. May contain rough edges creating active sites. Deac
Slide 4: The "Unboxing" of the GC Column
The “Unboxing” of the GC Column Important for identification and re-ordering Programmed temperature limit (<10 min) Isothermal temperature limits Unique to each column (identification) 4 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 5: What's Inside?
What’s Inside? Column tag contains useful information Column plug holds column ends together and protects against contamination. To put the column in storage, use this plug again or a piece of septa over the ends of the column. 5 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, C
Slide 6: Column Performance Summary
Column Performance Summary Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 6 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 7: Chromatographic Performance
Chromatographic Performance 320 °C Spec: 4.0 pA Meas: 2.1 pA 65 °C Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 7 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 8: Test Mixture Components
Test Mixture Components Compounds Purpose Hydrocarbons Efficiency Retention FAMEs, PAHs Retention Alcohols Activity Acids Acidic character Bases Basic character Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 8 May 31, 2019 Keeping your GC Column Happ
Slide 9: Column Installation Procedure
Column Installation Procedure • Install the column • Leak and installation check • Column conditioning • Setting linear velocity or flow rate • Bleed profile • Test mix Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 9 May 31, 2019 Keeping your GC Col
Slide 10: Contamination from French Fry Grease
Contamination from French Fry Grease Column: Agilent J&W DB-5ms, 30 m x 0.25 mm, 0.25 µm Carrier: H2, 60 cm/s, constant flow Injector: Split 1:20, 250 °C Detector: FID, 320 °C, N2 make up gas Oven: 40 °C for 0.75 min, 40-325 °C at 20 °C/min, 325 °C for 30 min Red: McFrench fry Blue: System blank Pro
Slide 11: "Touchless" Packaging
“Touchless” Packaging 11 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 12: Column Installation
Column Installation What type of ferrule should I use? Polyimide/ Flexible Polyimide Graphite graphite Metal Composition Re-use Max Temperature (°C) Use Limitation Polyimide (Vespel) Yes 280 Easy seal Shrink after heating causing leaks after thermal cycle; isothermal only Graphite Yes 450 FID, NPD,
Slide 13: Graphite/Polyimide Blend Capillary Ferrules
Graphite/Polyimide Blend Capillary Ferrules • Unfortunately, a leak occurred following normal temperature program runs • Studies show that the leaking continues with use of the ferrules - Not just after the first one or two runs Frequent retightening of the fitting is needed to maintain a leak-free
Slide 14: Better Connections: Self Tightening Column Nuts
Better Connections: Self Tightening Column Nuts Designed for use with short graphite/polyimide blend ferrules – both at the inlet and the MS interface – so that only one type of ferrule is needed for both ends of the column. For inlet or detector For mass spectrometer transfer line p/n 5190-5233 p/n
Slide 15: How Do Self Tightening Column Nuts Work?
How Do Self Tightening Column Nuts Work? • Ease-of-use – install in dark, small space in GC oven without wrenches • Wing design for finger-tight installation with graphite/polyimide blend ferrules • No tools, dramatically reduces force preventing over-tightening or damage • Robust stainless steel co
Slide 16: Benefit of Self Tightening Column Nuts
Benefit of Self Tightening Column Nuts Takes you from this… …to this Without retightening, the baseline remains flat after 400 runs with no indication of leaks when using the Self Tightening column nut. Ref. Technical note: 5991-3612EN 16 May 31, 2019 Keeping your GC Column Happy and Healthy: Instal
Slide 17: Column Installation
Column Installation Measuring the right distance White out Septa Keeping your GC Column Happy and Extra septa Healthy: Installation, Care, and Maintenance Agilent Restricted 17 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 18: Cutting the Column
Cutting the Column Gently scribe through the polyimide coating • Do not attempt to cut the glass Recommended tools • Diamond or carbide-tipped pencil, or sapphire cleaving tool • Ceramic wafer • Ocular Do not use • Scissors, file, and so on Keeping your GC Column Happy and Healthy: Installation, Car
Slide 19: Examples of Column Cuts
Examples of Column Cuts Bad Good Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 19 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 20: Column Installation
Column Installation How tight is tight? Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Over-tightened ferrule Agilent Restricted 20 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 21: Column Installation
Column Installation Leak check Do not use snoop • Electronic leak detector • IPA/water • Inject a nonretained peak Gas leak detector p/n G3388B Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 21 May 31, 2019 Keeping your GC Column Happy and Healthy: I
Slide 22: Leak and Installation Check
Leak and Installation Check Inject a nonretained compound Detector Compound FID Methane or butane ECD MeCl2 (headspace or diluted) NPD CH3CN-acetonitrile (headspace or diluted) TCD Air MS Air or butane The peak should be sharp and symmetrical Keeping your GC Column Happy and Healthy: Installation, C
Slide 23: Nonretained Peak Shapes
Nonretained Peak Shapes Good installation Improper installation or injector leak Check for: • Too low of a split ratio • Injector or septum leak • Liner problem (broken, leaking, misplaced) • Column position in injector and detector Keeping your GC Column Happy and Healthy: Installation, Care, and M
Slide 24: Calculating Linear Velocity
Calculating Linear Velocity Inject a nonretained compound and obtain the retention time: µ = Average linear L velocity (cm/s) µ= L = to = Column length (cm) Retention time (s) to He 20-40 cm/s H2 35-55 cm/s µ is dependent on column temperature, but Keeping your GC Column Happy and Healthy: Installat
Slide 25: Calculating Flow Rate
Calculating Flow Rate Inject a nonretained compound and obtain the retention time: 2 rL F = Flow rate (mL/min) F= r = Column radius (cm) L = Column length (cm) to to= Retention time (min) F is dependent on column temperature Measuring flow with a flow meter is often inaccurate Keeping your GC Column
Slide 26: Column Conditioning
Column Conditioning System must be leak free before conditioning column Heat the column to the lower of: • Isothermal maximum temperature or 20 to 30 °C above highest operation temperature. • Temperature programming is not necessary. Stop conditioning when the stable baseline is obtained: 1 to 2 hou
Slide 27: Generating a Bleed Profile
Generating a Bleed Profile Temperature program the column without an injection* 1.3e4 1.2e4 1.1e4 1.0e4 9000 8000 7000 6000 0 5 10 15 20 25 Time (min) *Agilent J&W DB-1 30 m x 0.32 mm id, 0.25 µm Temperature program // 40 °C, hold 1 min // 20 °C/min to 320 °C, hold 10 min 27 May 31, 2019 Keeping you
Slide 28: Own Test Mixture
Own Test Mixture • More specific to your application • Selective detectors • Concentrations specific to your application • Use same instrument conditions • Easiest to simply inject a calibration standard • Store for future measure of column performance Keeping your GC Column Happy and Healthy: Insta
Slide 29: ULTRA Scientific is Now Part of Agilent Technologies
ULTRA Scientific is Now Part of Agilent Technologies Agilent ULTRA Chemical Standards have: • Best in class online search, compare, and ordering capabilities • Rapid shipping: 99.9% of orders dispatched within 24 to 48 hours • Custom solutions • Sample preparation materials, columns, supplies, instr
Slide 30: Proper Care of your Column
Proper Care of your Column Page 30 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Agilent Restricted Restricted
Slide 31: Common Causes of Column Performance Degradation
Common Causes of Column Performance Degradation • Physical damage to the polyimide coating • Thermal damage • Oxidation (O2 damage) • Chemical damage by samples • Contamination Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 31 May 31, 2019 Keeping yo
Slide 32: Physical Damage to The Polyimide Coating
Physical Damage to The Polyimide Coating • The smaller the tubing diameter, the more flexible it is • Avoid scratches and abrasions • Immediate breakage does not always occur upon physical damage Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 32 May
Slide 33: Thermal Damage
Thermal Damage Degradation of the stationary phase is increased at higher temperatures • Rapid degradation of the stationary phase (breakage along the polymer backbone) caused by excessively high temperatures Isothermal limit = indefinite time Programmed limit = 5-10 minutes • Temporary "column fail
Slide 34: Oxidation (O2 Damage)
Oxidation (O2 Damage) Decreased retention Oxygen in the carrier gas rapidly degrades the stationary phase. The damage is Reduced response accelerated at higher temperatures. Damage along the polymer backbone is irreversible. (Premature filament failure/excessive source maintenance.) CH3 CH3 CH3 Si S
Slide 35: How to Prevent Column Damage by Oxygen
How to Prevent Column Damage by Oxygen • High-quality carrier gas (four 9s or greater) • Leak free injector and carrier lines – Change septa – Maintain gas regulator fittings Efficient, fast, easy • Appropriate impurity traps Keeping your GC Column Happy and Healthy: Installation, Care, and Maintena
Slide 36: Chemical Damage
Chemical Damage Bonded and cross-linked columns have excellent chemical resistance except for inorganic acids and bases. HCl NH3 KOH NaOH H2SO4 H3PO4 HF Chemical damage will be evident by excessive bleed, lack of inertness or loss of resolution/retention. Keeping your GC Column Happy and Healthy: In
Slide 37: Chemical Damage: What to do if it happens
Chemical Damage What to do if it happens • Remove 0.5 to 1 m from the front of the columns • Severe cases may require removal of up to 5 m Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 37 May 31, 2019 Keeping your GC Column Happy and Healthy: Instal
Slide 38: What is Normal Column Bleed?
What is Normal Column Bleed? Normal background signal generated by the elution of normal degradation products of the column stationary phase 1.3e4 Column bleed is influenced by: 1.2e4 • Phase type 1.1e4 • Temperature • Column dimensions 1.0e4 9000 Agilent J&W DB-624 30 m x 0.53 mm id, 3.0 µm 24 pA/2
Slide 39: Mass Spectrum of Phenylmethylpolysiloxane Column Bleed
Mass Spectrum of Phenylmethylpolysiloxane Column Bleed Normal background Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted Mass spectral library search is not always accurate 39 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care,
Slide 40: What is a Bleed Problem?
What is a Bleed Problem? An abnormal elevated baseline at high temperature It is not • A high baseline at low temperature • Wandering or drifting baseline at any temperature • Discrete peaks Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 40 May 31, 2
Slide 41: Column Contamination and Symptoms
Column Contamination and Symptoms • Fouling of GC and column • Poor peak shape by contaminants • Loss of separation (resolution) • Mimics nearly every • Changes in retention chromatographic problems • Reduced peak size • Baseline disturbances (semivolatiles only) Keeping your GC Column Happy and Hea
Slide 42: Typical Samples That Contain a Large Amount of Residues
Typical Samples That Contain a Large Amount of Residues Biological (blood, urine, tissue, plants) Soils Foods Wastewater Sludges All samples contain residues (even standards) Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 42 May 31, 2019 Keeping your
Slide 43: Other Sources of Contamination
Other Sources of Contamination •Septum and ferrule particles •Gas and trap impurities •Unknown sources (vials, syringes, and so on) Sample Vial Septum Bleed Profile: Contaminated wash solvent Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 43 May 31,
Slide 44: Types of Residues
Types of Residues Nonvolatile residues • Any portion of the sample that does not elute from the column or remains in the injector. Semivolatile residues • Any portion of the sample that elutes from the column after the current chromatographic run. Keeping your GC Column Happy and Healthy: Installati
Slide 45: Methods to Minimize Nonvolatile Residue Problems
Methods to Minimize Nonvolatile Residue Problems • Sample cleanup • Packed injection port liners • Guard columns Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 45 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintena
Slide 46: Agilent Bond Elut Sample Cleanup Products
Agilent Bond Elut Sample Cleanup Products Filtration cartridges and plates Solid Phase Extraction cartridges and plates Captiva EMR Lipid 46 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 47: Captiva EMR–Lipid Cleanup Improves Analytes S/N Ratio and Integration Accuracy
Captiva EMR–Lipid Cleanup Improves Analytes S/N Ratio and Integration Accuracy on GC/MS(/MS) of Pesticides in Olive Oil Pesticide Captan Permethrin Deltamethrin EMR-Lipid cleanup Zirconia sorbent cleanup + MRM (151.0 -> 79.1) Post-S 50ppb Fatty dSPE C1-3.D Counts x10 5 1.4 1.2 1 C18/PSA 0.8 0.6 clea
Slide 48: Guard Column or Retention Gap
Guard Column or Retention Gap Injector Detector The guard column is 3-5 m of deactivated fused silica tubing with the same Keeping your GC Column Happy and diameter as the analytical column. It is connected with a zero dead volume Healthy: Installation, Care, and Maintenance Agilent Restricted union
Slide 49: Nonvolatile Contamination: What to do if it happens
Nonvolatile Contamination What to do if it happens • Do not “bake out” the column • Front end maintenance – Clean or change the injector liner – Clean the injector – Cut off 0.5 - 1 m of the front of the column • Turn the column around • Solvent rinse the column (see appendix) • Cut the column in ha
Slide 50: Semivolatile Contamination: What to do if it happens
Semivolatile Contamination What to do if it happens • “Bake out” the column – Limit to 1-2 hours – Longer times may polymerize some contamination and reduce column life • Solvent rinse the column Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 50 May
Slide 51: Instrumentation: Leveraging Intelligence Innovations
Instrumentation: Leveraging Intelligence Innovations 51 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 52: Introducing the Agilent 8890 GC System
Introducing the Agilent 8890 GC System Flexible and expandable to meet your needs today and tomorrow Future-proof: Ready for anything — Powerful next generation electronic architecture — Expanded smart-connected functionality — Full suite of inlets, detectors, and accessories, CFT, Deans Switch, Bac
Slide 53: Agilent 8890 GC System
Agilent 8890 GC System Smart-connected GC Modern intuitive interface — 7-inch color touch screen — Configuration — Status — Methods — Sequence info — Troubleshooting, diagnostics, and help — Real-time chromatographic evaluation — Blank evaluation — Detector evaluation 53 May 31, 2019 Keeping your GC
Slide 54: Guided Troubleshooting/Step-by-Step Guides on the Agilent 8890 GC System
Some Examples of Guided Troubleshooting/Step-by-Step Guides on the Agilent 8890 GC System 54 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 55: GC Columns with Smart Key (for the Agilent 8890 GC only)
GC Columns with Smart Key (for the Agilent 8890 GC only) For immediate identification and use monitoring of your GC column • Available with the Agilent 8890 GC model only • Can track use of a GC column • Smart Key contains GC column information, including: – Part and serial numbers – Number of injec
Slide 56: Other Resources
Other Resources Resources Weblinks 1 Agilent 8890 GC brochure URL:https://www.agilent.com/cs/library/brochure s/brochure-gc-8890-5994-0476en-agilent.pdf 2 Smart Key product page (not for ordering URL: www.Agilent.com/chem/smartkey8890 Smart Keys) 3 Instruction sheet URL:https://www.agilent.com/cs/li
Slide 57: Agilent Intuvo 9000 GC System
Agilent Intuvo 9000 GC System 57 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 58: Common Frustrations with GC
Common Frustrations with GC • Measuring column length correctly • Cutting your column correctly • How tight is too tight? • Clipping columns to deal with active sites, then updating retention times 58 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent
Slide 59: Common Care and Maintenance Scheme for GC Columns / Intuvo
Common Care and Maintenance Scheme for GC Columns 1. Cut off 6 in to 1 ft of the inlet end of the column 2. Bake out the column for no more than 2 hours 3. Cut off more column (repeat as necessary) Intuvo… Change the Guard Chip Guard Column 59 May 31, 2019 Keeping your GC Column Happy and Healthy: I
Slide 60: Innovating the GC Flow Path
Innovating the GC Flow Path Conventional Intuvo flow path flow path Click-and-run Inlet Inlet direct connections Guard Chip Gold seal Flow Chip Nuts and ferrules To detector Classic capillary Intuvo planar column column To detector 60 May 31, 2019 Keeping your GC Column Happy and Healthy: Installati
Slide 61: Easier and Faster Maintenance with Intuvo
Easier and Faster Maintenance with Intuvo • No more ferrules • Direct face seal connections • Audible and tactile click lets you know connection is made • Less unplanned downtime • Fewer batch reruns, fewer samples lost 61 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, an
Slide 62: No More Measuring, Over-tightening, Trimming
No More Measuring Over-tightening Trimming 62 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 63: A New Portfolio of GC Consumables
A New Portfolio of GC Consumables UI inlet liners Guard Chip Smart Keys Intuvo Flow Chips No-trim column Tools and accessories 63 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 64: Tips to Assure a Good Column Installation
Tips to Assure a Good Column Installation Finger tighten until only one thread on each of the two nuts is showing. If more than one thread is showing, wiggle or reposition the column into place to further finger tighten the nuts to one thread. 64 May 31, 2019 Keeping your GC Column Happy and Healthy
Slide 65: Tips to Assure a Good Column Installation
Tips to Assure a Good Column Installation Check that the small integrated column nuts on the column are in form fitted place on the heater, in the instrument. Click and run. 65 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 66: Smart Key Technology
Smart Key Technology • Smart chip tells your Intuvo what you have • Sets temperature limits for you • Keep track of performance with read/writeable Smart Key 66 May 31, 2019 Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted
Slide 67: Agilent Intuvo 9000 Videos
Agilent Intuvo 9000 Videos The Agilent Intuvo 9000 GC System – Environmental Science Corporation (ESC) Discover higher GC productivity with the Agilent Intuvo 9000 GC system Playing time: 4:00 The Agilent Intuvo 9000 GC System Story Learn more about the Agilent Intuvo 9000 GC System Playing time: 2:
Slide 68: Always Remember
Always Remember • Start with a good installation • Maintain an oxygen-free system • Avoid physical, thermal, and chemical damage • Take steps to prevent contamination Keeping your GC Column Happy and Healthy: Installation, Care, and Maintenance Agilent Restricted 68 May 31, 2019 Keeping your GC Colu
Slide 69: Contact Agilent Chemistries and Supplies Technical Support
69 Contact Agilent Chemistries and Supplies Technical Support 1-800-227-9770 Option 3, Option 3: Option 1 for GC and GC/MS columns and supplies Option 2 for LC and LC/MS columns and supplies Option 3 for sample preparation, filtration, and QuEChERS Option 4 for spectroscopy supplies Option 5 for che