Agilent Technologies, Inc. · NYSE:A
Agilent Technologies — Technical Presentation (November 2016)
49 slides from Agilent Technologies's technical presentation, November 2016
Slide 1: Guidelines for Trouble Shooting and Maintenance of ICP-OES Systems
Guidelines for Trouble Shooting and Maintenance of ICP-OES Systems Presented by Eric Vanclay, Spectroscopy Supplies Marketing Manager ICP-OES Maintenance & Trouble Shooting Nov. 2016
Slide 2: Agilent's Atomic Spectroscopy Portfolio
Agilent’s Atomic Spectroscopy Portfolio Flame AA MP-AES ICP-OES ICP-MS ICP-QQQ Agilent’s 5110 Agilent’s 8900 Agilent’s 55 and ICP-OES Agilent’s 7800 & Agilent’s 4210 ICP-QQQ with 200 Series includes the 7900 ICP-MS are MP-AES runs on MS/MS mode includes Fast world’s most robust, sensitive, air for t
Slide 3: Agilent 5110 SVDV ICP-OES Performance Highlights
Agilent 5110 SVDV ICP-OES Performance Highlights Dual View Minus the Wait! • Fastest sample Lowest throughput • Low gas consumption Cost of • Longer component life Ownership • Reduced maintenance costs • No compromise on Enhanced speed, precision or stability Analytical • System robustness and relia
Slide 4: Agilent 4210 MP-AES Performance Highlights
Agilent 4210 MP-AES Performance Highlights Lower Cost of •• Uses nitrogen for the emission source No hollow cathode lamps and no Ownership deuterium lamps • No flammable gases Safer • No manual cylinder handling • Lower detection limits compared to Higher FAAS • Larger linear dynamic range Performan
Slide 5: Agilent 8900 Triple Quadrupole ICP-MS
Agilent 8900 Triple Quadrupole ICP-MS LEAVE INTERFERENCES BEHIND WITH MS/MS Superior Performance Controlled reaction chemistry for consistent, reliable results Resolution of isobaric overlaps (beyond capability of high-resolution ICP-MS) Lowest detection limits, even for previously “difficult” eleme
Slide 6: Common ICP Problems Reported by Customers
Common ICP Problems Reported by Customers Sensitivity: • Sensitivity is worse than it used to be • I have a new application and I can’t get the sensitivity I need • I need lower detection limits for As & Se • How come I can’t get the instrument to meet published detection limits? Precision • Sensiti
Slide 7: Causes of Poor ICP-OES Sensitivity
Causes of Poor ICP-OES Sensitivity Sample Worn pump tubing introduction system Blocked nebulizer Blocked injector in torch Poor optimization – especially the neb. flow Optimization Method setting – using right wavelength? Wrong tubing type Interferences Standard High blank level (& sample) Standards
Slide 8: Causes of Poor ICP-OES Precision
Causes of Poor ICP-OES Precision Worn pump tubing Sample introduction Beading in spray chamber system Nebulizer condition and performance Air leaks in transfer tubing Torch alignment Optimization Poor optimization – especially the neb. flow Nebulizer choice for your samples Standard (& sample) Wash-
Slide 9: Causes of Poor Accuracy in ICP-OES
Causes of Poor Accuracy in ICP-OES Sample introduction Worn pump tubing system Blockage in nebulizer and/or torch Wrong wavelength choice - interferences Optimization Poor optimization – especially the neb. flow Choice of internal standard Insufficient stabilization time Standard preparation Standar
Slide 10: ICP-OES Sample Introduction System Tips
ICP-OES Sample Introduction System Tips Do: Check optimization each analysis Don’t: Assume system is still optimized Check/monitor the nebulizer uptake Assume nebulizer flow rate is the same Check/adjust the peri pump tubing Overtighten the pressure adj. screw Check the blank reading Use a simpl
Slide 11: Peri Pump Tubing Tips
Peri Pump Tubing Tips - Tubing diameters • Want tubing used for waste to be larger ID than sample ID - Chemical compatibility • Ensure tubing is resistant to the solvent being used - Replace frequently • Using “old” tubing can lead to problems with precision and stability • Typical lifetime is 1-2 w
Slide 12: Cleaning the Nebulizer
Cleaning the Nebulizer Never sonicate or attempt to clean with wire! For normal cleaning: • Reverse pump the nebulizer with the tip in solvent; OR • Apply suction from the wide end of the capillary using a vacuum aspirator; OR • Apply high pressure clean air via a tubing snugly fitted over the nebul
Slide 13: Performance Characteristics of Common Nebulizers
Performance Characteristics of Common Nebulizers Nebulizer Aerosol Achieved Dissolved HF Organics Self Ideal Sample Type Efficiency Precision Solids Resistance Compatibility Aspirates Type Tolerance OneNeb Excellent Excellent Good Excellent Excellent No Handles most (max. 150 um samples particles) S
Slide 14: Performance Challenges of a Concentric Nebulizer
Performance Challenges of a Concentric Nebulizer ICP-OES Maintenance & Trouble Shooting Nov. 2016 14
Slide 15: Universal OneNeb Nebulizer: A Quick Review
Universal OneNeb Nebulizer: A Quick Review Innovative design improves performance, reduces maintenance, enhances sample throughput, and reduces operating costs. • Direct replacement for a conventional concentric nebulizer • Virtually indestructible (even if dropped) • Resistant to HF & organic solve
Slide 16: And Now… Agilent's OneNeb Series 2 Nebulizer
And Now… Agilent’s OneNeb Series 2 Nebulizer • Improved version of the inert OneNeb universal Nebulizer - User replaceable capillary - ETFE body for improved robustness - Thicker wall sample capillary • Reduces kinking • Less chance of damage when connecting the peristaltic pump tubing - Suitable fo
Slide 17: Why Switch to the OneNeb?
Why Switch to the OneNeb? 1. Provides the ultimate flexibility • Handles different applications • Eliminates need to change nebulizers when changing applications 2. It’s inert – use it with any solution type (incl. HF & organics) 3. It’s virtually indestructible! 4. Easy to use – direct replacement
Slide 18: Performance Characteristics of ICP Spray Chambers
Performance Characteristics of ICP Spray Chambers Spray Aerosol Achieved Dissolved HF Organics Ideal Sample Chamber Efficiency Precision Solids Resistance Compatibility Type Type Tolerance Single pass Excellent Good Poor to Poor Good Environmental, food glass cyclonic Medium digests Double pass Good
Slide 19: Cleaning the ICP Spray Chamber
Cleaning the ICP Spray Chamber Can sonicate in a detergent solution (with care), rinse and dry Must clean the spray chamber when you see “beading” or droplet formation on the walls (or if precision degrades): • Soak overnight in a 25% detergent solution - Best to leave it soaking for 24 hours - Use
Slide 20: 700 Series ICP Torch Selection
700 Series ICP Torch Selection One piece quartz torch - Simple to use • Narrow bore injectors – organics - Recommended for most applications Semi-demountable torch - Injector is removable and changeable - Gives greater flexibility. • Alumina injector -fusions and HF digests • Quartz injectors for ot
Slide 21: 700 Series ICP Torch Cleaning
700 Series ICP Torch Cleaning Do NOT sonicate! Soak in conc. aqua regia (3:1 HCl: HNO3) overnight • Use a pipe cleaner dipped in aqua regia to remove persistent compounds from the injector tube Axial ICP • For salt deposits: - Rinse with water to remove deposits - Soak the torch overnight in a beake
Slide 22: 700 Series ICP Torch Alignment
700 Series ICP Torch Alignment • Torch alignment required after removing/replacing the torch • Ensures optics viewing highest emission signal from the plasma • Also useful as a quick performance check • Monitor the max. intensity • Positions for optimum Vertical & Horizontal position should not shif
Slide 23: 5100 Series ICP Torch Selection
5100 Series ICP Torch Selection Features moulded torch base designed for “plug and play” loading SVDV - Easy to install (3 steps) - Automatic torch alignment - no torch scanning required SVDV= Simultaneous Vertical Dual View - Automatic gas connection to eliminate confusion around gas line fitting -
Slide 24: 5100 Series ICP-OES Torch Cleaning
5100 Series ICP-OES Torch Cleaning 3 easy steps to cleaning the torch (see the torch cleaning guide (Agilent pub# G8000-90019) for more details): 1. Soak in 50% aqua regia for 1 hour 2. Thoroughly flush inside & outside using de-ionized water 3. Blow clean compressed air or nitrogen through the thre
Slide 25: 5100 Series ICP-OES Torch Cleaning
5100 Series ICP-OES Torch Cleaning Agilent’s torch cleaning stand (pn G8010-68021) provides a convenient, alternative way for users to clean their torches • Provides a stable platform to enable either the complete torch assembly or the bare injector/base assembly to be suspended in the acid cleaning
Slide 26: Improving Sensitivity – Integration Time
Improving Sensitivity – Integration Time • Solid-state detectors such as the VistaChip2 CCD detector • Improve S/N and detection limits by averaging noise over time • DL α 1/√t Mn 257 3s Detection Limits 0.05 0.04 0.03 mg/L 0.02 0.01 0.00 5s 10 s 30 s Integration Time ICP-OES Maintenance & Trouble S
Slide 27: Improving Sensitivity – Integration Time
Improving Sensitivity – Integration Time 460 440 440 420 5s Read Time 420 1sec Read time 400 400 380 380 360 360 340 340 320 320 300 300 280 280 440 420 30s Read Time Overlay multiple 400 50ppb readings of 380 Se at 196.026nm 360 340 320 300 DL α STDEV 280 ICP-OES Maintenance & Trouble Shooting Nov.
Slide 28: Improving Sensitivity – Sample Introduction
Improving Sensitivity – Sample Introduction • Single-pass spraychambers enhance sample transport efficiency • Improves S/N and detection limits • No degradation in short term precision when viewed axially 30 second axially viewed Detection Limits 4.5 Douple-pass Spraychamber 4.0 3.5 Single-pass Spra
Slide 29: Improving Sensitivity – MSIS Sample Introduction
Improving Sensitivity – MSIS Sample Introduction • Use the Multi-mode Sample Introduction System (MSIS) - A unique spray chamber for ICP-OES/MP-AES systems - Provides better sensitivity for determination of As, Se and Hg (& other hydride elements) - Simultaneous determination of routine elements and
Slide 30: Improving Sensitivity - MSIS Operating Principle
Improving Sensitivity - MSIS Operating Principle One system for analysis of even the most difficult elements. Prep and run your entire analysis on one system. Eliminates the need for multiple systems & batch testing of As, Hg, Se and others Improved productivity and cost/ labor savings ICP-OES Maint
Slide 31: Improving Sensitivity - MSIS Performance with 5100
Improving Sensitivity - MSIS Performance with 5100 Element IDL using Conv. IDL using Nebulization MSIS ug/L ug/L As 2.0 0.23 Se 2.4 0.1 Hg 1.0 0.037 Sb 2.4 0.075 Sn 1.1 0.29 Detection limits for non-hydride elements in simultaneous mode are equivalent to those achieved using conventional nebulizatio
Slide 32: ICP-OES System Tips – Wavelength Calibration
ICP-OES System Tips – Wavelength Calibration • “Wavelength Calibration” co-relates actual emission peak to the pixels on the detector chip • Periodic calibration required – typically once/month Needs wavelength - Monitor peak position w.r.t. peak marker to determine if calibration calibration requir
Slide 33: ICP-OES System Tips – Plasma Ignition Problems
ICP-OES System Tips – Plasma Ignition Problems In most cases, the plasma will ignite first time. If not, check the following (failure usually indicates presence of air): - First, try repeating the ignition step again - Have you changed argon cylinders recently? • Check the grade of argon • Try anoth
Slide 34: ICP-OES System Tips - Memory Effects
ICP-OES System Tips - Memory Effects • Typically observed when measuring high concentrations of selected analytes - Usually see high intensity for first replicate – subsequent replicates are more consistent - Common culprits: • Ag, Au, B, Hg, Mo, Si, Sn, W, Zn, Zr • The fix? - Check the rinse time u
Slide 35: ICP-OES – Potential Autosampler Issues
ICP-OES – Potential Autosampler Issues - More customers use autosamplers with ICP for automation - Issues to consider: • Confirm samples loaded in correct sample locations • Long transfer tube between sampler and ICP-OES - May need to program a longer sample uptake delay - May exacerbate problems wi
Slide 36: Recommended Procedures at End of the Day
Recommended Procedures at End of the Day 1. Aspirate acid rinse solution for a few minutes before shutting off the plasma - Helps to prevent sample deposition inside the nebulizer after the run 2. Extinguish the plasma and switch off the chiller 3. Remove the sample capillary from the rinse, start t
Slide 37: Agilent ICP-OES Performance Benefits
Agilent ICP-OES Performance Benefits Robust, stable analysis • Copes easily with difficult sample matrices such as organic solvents • Continuous wavelength coverage Long Term Stability ensures flexibility and gives you 250 ppb multi-element in 25% NaCl with confidence in your results: VDV configurat
Slide 38: Tips to Improve Standard Preparation
Tips to Improve Standard Preparation - How are they prepared? • Ensure purchased standards are still within “Use By” date • Use calibrated pipettes and class ‘A’ volumetric flasks for dilutions - Periodically, check accuracy & reproducibility of your pipettes • Use de-ionized water (Type I - conduct
Slide 39: Tips to Reduce Contamination
Tips to Reduce Contamination Contamination can come from anything that comes into contact with your sample during storage, digestion (dilution) and analysis • Check reagent purity - Always buy the best reagents - Always check the certificate of analysis for elevated levels - Caution if buying in lar
Slide 40: Tips to Improve Accuracy of Results
Tips to Improve Accuracy of Results - Sample preparation • Is the most appropriate digestion being used? • Are all of the analytes being quantitatively (and reproducibly) extracted and dissolved? - Many digestions are only partial extracts – efficiency will vary with the sample matrix - Some volatil
Slide 41: ICP-OES – Recommended Maintenance Schedule
ICP-OES – Recommended Maintenance Schedule Daily: • Check exhaust system operating (smoke test) • Inspect torch for injector blockage/other damage • Check nebulizer for blockage/pulsation • Inspect peristaltic pump tubing for stretching or flatness • After analysis is complete: - Aspirate rinse solu
Slide 42: ICP-OES – Recommended Maintenance Schedule
ICP-OES – Recommended Maintenance Schedule Monthly: • Clean spray chamber (or earlier if “beading” in spray chamber) • Clean nebulizer • Check the other sample introduction tubing and O-rings - Look for excessive wear, poor sealing or kinks and replace as necessary - Especially look at the transfer
Slide 43: Overview – Key Consumables for ICP-OES
Overview – Key Consumables for ICP-OES Sample introduction: - Peristaltic pump tubing - Torches - Transfer and drain tubing - Nebulizers - Spray chambers - Application kits (adapt your instrument to a new application) - ICP standard solutions - Ionization suppressant / buffer solutions Autosampling:
Slide 44: 700 Series ICP-OES Consumables Kits
700 Series ICP-OES Consumables Kits Part Number Description Content 7 x standard axial torches 1 x SeaSpray nebulizer 1 x Tubing and connectors kit 9910112800 Extended Value Pack – 2 x Spray chamber O-ring kits Axial ICP 1 x Double pass glass cyclonic spray chamber (incl. mounting bracket) 2 x Singl
Slide 45: 5100 Series ICP-OES Consumable Kits
5100 Series ICP-OES Consumable Kits Components in the Operating Supplies Kit 1 Easyfit demountable torch with 2 spare outer tubes 4 packs pump tubing (for sample + waste) Order one of the “ICP-OES Consumables Kits” 1 pack int. standard pump tubing & connectors • Each kit contains all the essential a
Slide 46: Links to Useful ICP-OES Resources
Links to Useful ICP-OES Resources • ICP-OES parts and supplies (On-line Store): http://www.chem.agilent.com/store/en_US/Cat-SubCat1ECS_30364/ICP-OES?navAction=push&navCount=0 • ICP-OES troubleshooting videos: http://www.agilent.com/en-us/products/icp-oes/icp-oes-supplies/nebulizers/icp-oes-nebulizer
Slide 47: Other Support Resources for Agilent ICP-OES Users
Other Support Resources for Agilent ICP-OES Users • Are you a member of Agilent’s PlasmaNet email forum? - This is a direct email link to other Agilent ICP-OES users worldwide • PlasmaNet allows you to: - Ask a question and get responses from other users doing the same application and/or Agilent Spe
Slide 48: Summary – To Achieve Quality Data
Summary – To Achieve Quality Data • Most “instrument” failures occur in the sample introduction area - Includes • Torch • Spray chamber • Nebulizer • Peristaltic pump tubing • Drain Assembly • Improper maintenance of this area can result in poor data quality • Frequently less experienced analysts ca
Slide 49: Questions
Questions http://www.agilent.com/chem/atomic ICP-OES Maintenance & Trouble Shooting Nov. 2016 49
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