Maintaining Lab Operations Icpoes and Icpms Support Topics April222020
Maintaining Lab Operations Icpoes and Icpms Support Topics April222020
Maintaining Lab Operations Icpoes and Icpms Support Topics April222020
extraordinary times
DE.43375
• Develop a new schedule/routine for working in the lab. This is a challenging time for everyone and routine helps
everyone acclimate to these impacts.
• Prioritize time in the lab - Can any tasks be shifted remote or online (training, remote monitoring, data analysis)? Is your
IT department aware of these and is bandwidth/VPN/remote access capable of handling this.
• Are service providers allowed on-site? Or is there remote work they can do? Discuss this before any scheduled visit.
Our service teams are currently offering free live video conferences to support labs around the world – more info at the
end of the presentation.
• Proactively replace lab consumables before you see performance issues. If ordering supplies, check if
shipping/receiving/logistics for your company has been affected.
• When you return to normal operations, have a detailed restart plan that outlines priorities and timelines. Agilent will
provide additional information on returning/restarting your lab in a few weeks.
ICP System Readiness
Paul Krampitz
Application Scientist
[email protected] 5800 ICP-OES
In This Section, We Will Discuss:
•Daily
• Inspect torch.
• Check nebulizer for blockage/pulsation.
• Rinse spray chamber after every use.
• Inspect peristaltic pump tubing.
• Empty waste vessel.
• Check water level in Argon Humidifier Accessory (if used).
• Wipe down exterior surfaces of your ICP.
• Inspect all other tubing and connections..
•Weekly
• Clean torch.
• Inspect cone (axial) or snout (radial).
Weekly Torch Maintenance
•Rinse torch with de-ionized water to remove salt deposits, and allow
to dry before use.
•To remove other deposits or stains:
• Soak the torch in aqua-regia (3:1 HCl/HNO3) overnight.
• Rinse well with water and allow to dry before use
•Slotted outer tube for use with Axial Plasma will show signs of de-
vitrification after first use
• DO NOT spend time cleaning
• Monitor for cracks
•Organic deposits:
• Remove deposits gently with spatula.
• Soak in H2SO4 & H2O2 (9:1).
Rinse with water, then methanol and dry.
• Rinse with CS2 to dissolve carbon.
• Injector tubes can be “flammed” with a propane torch or placed in a
muffle furnace.
•Torch lifetime is dependent on:
• Total dissolved solids level in samples.
• Plasma conditions.
• RF Power.
• Nebulizer flow.
• Plasma gas flow.
ICP Maintenance : Monthly/Yearly
•Monthly
• Clean spray chamber.
• Clean nebulizer.
• Inspect the state of induction coil.
• Verify that the water level in water recirculator is sufficient.
• Clean/check air filter on top of ICP.
•6 months
• Replace the water in the re-circulator/chiller and add Chloramine-T.
• Change argon filters (compressed gas cylinder).
•12 months
• Change argon filters (liquid dewar).
Spray Chamber Cleaning
•Glass Cyclonic
• Cleaning required when the sample aerosol begins to BEAD UP on the
spray chamber walls.
Soak in aqua-regia, rinse and replace.
Soak in Fluka 'RBS-25‘ or TritonX-100 (0.5%) overnight, rinse and
replace.
Glass Concentric :
• Soak in Aqua-Regia.
• Back Flush with Water Bottle or Vacuum.
Syringe
Nebulizer gas outlet
• Never sonicate as the inner capillary may shatter or crack leaving the
nebulizer useless.
Water Cooling System
•Turn the water cooler off and disconnect it from the main power supply.
•Unscrew and remove the lower filter nut.
• Pull out the micron mesh filter.
• Using a mild detergent, clean the filter then
rinse thoroughly with de-ioinized water.
•Re-assemble the water filter and tighten nut. Check for leaks when chiller
operational.
Air Filter
•Check monthly.
Poor precision:
• Determine if it is drift or noise related.
• Run the Cu/Mn Ratio Method to monitor the drift.
• Check the nebulizer for blockage.
• Check the torch and injector tube.
• Check the pump and pump tubing.
Drift Test Using Cu/Mn Ratio
•If deviation of the ratio is > 5%, clean nebulizer, spray chamber,
torch and replace pump tubes.
Troubleshooting: Noisy Signal
14.0
012.0
Mg
0
10.0
Ratio
0 8.0
Rati 06.0
o
0
4.0
02.0
00.0
0 0. 0. 1 1.
8 9 1.
1 1. 1.
Power 2 1.
3 4
(kW) 5
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Sample Introduction System Overview
Sample area
Nebuliser and spray chamber
What will be Torch Loader
covered in this
training . . . Torch
Peristaltic Pump
SVS +
Humidifier
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Sample Area
Make-up (sheath
gas) Connection
Future expansion
area (i.e. valve)
Nebuliser
Connection
Ball joint
connection and
clamp
Drain connection
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Nebuliser - Spray Chamber
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Torch Loader
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Torch Loader
Pre-optic/RF Box
alignment pins
Ignitor The torch loader aligns the torch
contact
with the pre-optics and RF box to
ensure the injector position is
Plasma Gas correct.
Aux Gas
Torch handle
switch
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Loading The Torch
Rubber ring
retains torch
until handle
closed
Insert torch
with arrow in
front
Fully open
handle Torch
remains in
place even
with handle
open
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Torch Outers
Axial with
radial
viewing slot
The torch outer and
intermediate tube are one
part.
Standard torch is fully
bonded and not removable.
Semi demountable torch is
Radial torch available.
With shorter
outer There is to types:
• Dual view with radial slot.
• Radial
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Torch injectors
Injector Setback* Use/Application
Dia.
2.4mm 0.5mm Dual View
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One Piece Torch
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Inert System (for HF)
Unique
clamp to
Ceramic hold ball
injector joint, spray
chamber
and torch
together
Plastic ball
Auxillary Gas joint coupling
Inert cyclonic spray Plasma Gas
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Assembling The Torch
Radial
Viewing slot When reassembling the torch it
is important to align so that:
a) The radial viewing slot on
the axial torch aligns with
the snout.
Torch alignment b) The plasma gas entry is
mark aligned with the base to
ensure correct tangential
flow.
Torch base
alignment mark
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Peristaltic Pump
Nut for pump pin
Peristaltic pump
interface board
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New Argon Humidifier Assembly (AHA)
To nebuliser
Uses semi permeable
membrane rather than
Use Grey bubbler.
4.0mm
connections Used with high salt samples to
Orange 3.2mm
connections
avoid blockages.
(for future use)
Partially fill bottle with DI
water.
Note: droplets of water may be
present inside the tubing, this
is normal and does not
indicate a problem
43 Confidentiality Label
ICP System Readiness
Paul Krampitz
Application Scientist
[email protected] 5800 ICP-OES
ICP-MS Top 5 tips to ensure ICP-MS performance
The main time robber in an ICP-MS lab is unplanned maintenance.
Tubing diameters
Drain tubing 1.52 mm ID
• Waste to be larger ID than sample ID
Agilent P/N G1833-65570
Chemical compatibility
• Ensure tubing is resistant to the solvent being used
Routine cleaning:
• Soak the end cap and spray chamber in 5% nitric acid or Citranox for
>30 mins
• Rinse, dry and refit
If you see precision problems or droplet formation on the walls of the spray
chamber (beading):
• Soak overnight in a 25% detergent solution
– Best to leave it soaking for 24 hours
– Use any laboratory detergent
e.g. Fluka RBS25, Triton X-100, Decon 90 etc.
ICP-MS 3 Cleaning the Torch
Visually check the torch, bonnet and shield when removing the
torch
• Replace if deformed or chipped
Do not sonicate!
For routine cleaning:
• Soak in >5% nitric acid for ~30 mins
For more stubborn stains:
• Soak in bleach (e.g. Chlorox ©) overnight
• Soak in aqua regia (1:3 HNO3:HCl)
For salt deposits:
• Rinse with water to remove deposits
• Soak the torch overnight in a beaker of 25% Fluka RBS-25
detergent
Rinse and allow to dry
Caution! Reinstall only when dry
Torch damage due to incomplete drying
ICP-MS Re-installing the Torch
3. Ensure the torch projection fits into the slot on the torch holder.
4. Can check the alignment of the RF coil when re-installing the torch.
If plasma fails to ignite, check all connections for possible air leaks
ICP-MS 4 What’s the Right Way to Clean Interface Cones?
Routine Cleaning:
Simple clean with pure water
• Dip a cotton swab (pn 9300-2574) in pure water and clean both
sides of the cone
• Rinse with pure water
• Ultrasonicate the cones in pure water for >5 mins (typ. 20 mins)
• Repeat as required (aim for water to stay clean)
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ICP-MS 4 What’s the Right Way to Clean Interface Cones?
The cones must not be stored in pure water for more than 30 minutes or they will
become damaged by corrosion.
.
ICP-MS Re-installing the Cleaned Cones
Li
Y
Tl
“Condition” cones prior to analysing samples with TDS > 0.5 %!
Condition new cones and cones after cleaning. Reduces drift due to
initial deposition of sample matrix on the clean cone surface
4. Samples.
Lens Maintenance
ICP-MS 4 Symptoms
Low sensitivity
1. Disassemble lens
2. Scrub all surfaces and orifices with Bar Keepers
Friend/polishing paper
3. Rinse with tap water – Very Important
4. Sonicate in pure water for 5 minutes
5. Repeat sonicating in pure water 2 more times
6. Dry using clean gas – nitrogen or argon
7. Reassemble
8. Reinstall and run Lens Shortage Test
7 port
For routine maintenance:
valve (incl.
online ISTD Fittings and ferrules
port) Check that they are not too tight and replace ferrules.
Tubing should be replace periodically.
Piston
pump
3-way
valve
ICP-MS Cell Gas Maintenance
• Use the “Maintenance Log” to record routine and non routine maintenance
activities
– Helps to prevent sample deposition inside the nebulizer after the run
3. Remove the sample capillary from the rinse, start the pump again and pump
any remaining rinse solution from the spray chamber
4. Release the pressure bars on the pump tubing and remove the bridges from
the securing slot
– Ensure the tubes are no longer stretched over the pump rollers
Daily:
− Argon and cell gas (He, H2, …) pressures
− Check peristaltic pump tubing for damage/deterioration
− Visual check of glassware
(connections OK, no filling of spray chamber or connector)
− Visual inspection of sample cone exterior (orifice shape & deposition)
Frequently, as needed - perform these operations:
− Empty the drain reservoirs
− Thorough visual inspection of interface cones
− Check nebulization
− Replace peristaltic pump tubing
− Clean/replace torch
− Check recirculation water level
Use the smart tools in the software Mass Hunter that can help you to overcome unplanned maintenance problems:
• Early Maintenance Feedback
• Maintenance Log
ICP-MS Other Support Resources for Agilent ICP-MS Users
Maintenance Video Disk (40 video clips for
maintenance)
Hardware maintenance
manual
Interactive troubleshooting
tool for high background
Interactive troubleshooting
tool for low sensitivity
Interactive troubleshooting
tool for plasma ignition
problem
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Additional online e-seminars and educational material
https://www.agilent.com/en/training-events/eseminars
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https://www.agilent.com/en/training-events/eseminars/lc-lc-ms-column-e-seminars
Register here https://www.agilent.com/en/training-events/eseminars/gc-gc-ms-webinars
https://www.agilent.com/en/training-events/eseminars/832
https://www.agilent.com/en/training-events/eseminars/etff-webinars
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In Summary
Given all that we are going through, Agilent remains a stable and continuing
resource to meet and exceed your analytical measurement needs
Any questions?
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Slides will be distributed to the email address you registered with.
Any doubts?
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