innovations in icp sample introduction jerry dulude, glass expansion, inc. 4 barlows landing rd....
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Innovations in ICP Sample Introduction
Jerry Dulude, Glass Expansion, Inc.
4 Barlows Landing Rd.
Pocasset, MA
Glass Expansion
Summary of Discussion
Low Flow Nebulizers Helix O’ring-free Spray Chambers New Internal Standard Kit Niagara Rapid Rinse Accessory
Innovations in Sample Introduction
Glass Expansion
Applications of Low-Flow Nebulizers
Limited sample volumes Volatile samples Expensive waste disposal ICP-MS-LC interface
Low-Flow Nebulizers
Glass Expansion
Range of Low-Flow Nebulizers
MicroMist- Concentric glass nebulizer 0.05 to 0.6 ml/min
PolyCon- Concentric polyimide nebulizer 0.05 to 0.6ml/min
OpalMist- Concentric PFA nebulizer 0.01 to 0.6ml/min
Low-Flow Nebulizers
Glass Expansion
Transport Efficiency vs. Uptake
%EFFICIENCY
UPTAKE RATE (ML/MIN)
Indirect drain collection method
Low-Flow Nebulizers
Glass Expansion
Tertiary Flow Rate vs. Uptake
05
101520253035404550
0.03 0.11 0.27 0.5 0.61 1.4 2.1
uptake rate (ml/min)
ul/min
Tertiary Flow Rate (ul/min)
Low-Flow Nebulizers
Glass Expansion
Corroboration of Tertiary Flow Rates
Uptake rate
(ml/min)
Indirect Method
(mg/min)
Direct Method*
(mg/min)
0.03 15 14
0.11 23 21
Todoli, Hernandis, Canals, and Mermet, JAAS, 1999, 14, 1289-1295Using GE MicroMist nebulizer with U-tube absorption for measurement
Low-Flow Nebulizers
Glass Expansion
Primary Aerosol Size Distribution Comparison
20
60
100
D32 = 7.1
Nebulizer Gas Flow Rate = 1.0 L/Min Solution Uptake Rate = Natural Aspiration
MicroMist (0.03ml/min)
Diameter (m)10 20 30 40 50 600
D32 = 17.2
Conikal (2ml/min)
20
60
100
No
rmal
ized
Co
un
t
No
rmal
ized
Vo
lum
e
Diameter (m)10 20 30 40 500 60
Low-Flow Nebulizers
Glass Expansion
Tertiary Aerosol Size Distribution Comparison
No
rmal
ized
Co
un
t
Nebulizer Gas Flow Rate = 1.0 L/Min Solution Uptake Rate = Natural Aspiration
Conikal (2ml/min)
20
60
100D32 = 4.9
Diameter (m)
20
60
100D32 = 5.0
MicroMist (0.03ml/min)
10 20 40300 50
Baffled Cyclonic Spray Chamber
Low-Flow Nebulizers
Glass Expansion
New Micro-Flow OpalMist
All PFA construction Natural uptake rate of 0.010 ml/min Ultra-high purity applications Ideal for micro samples down to 20 ul volume
Low-Flow Nebulizers
Glass Expansion
Cyclonic Spray ChambersAdvances in Nebulizer Installation
1984 1993
1996
Helix O’ring free spray chamber
Glass Expansion
Helix O'ring-Free Spray Chamber
Helix O’ring free spray chamber
Reduced carryover
Faster washout Higher purity Can stand up to
ketones and other solvents
Glass Expansion
New Internal Standard KitBenefits of Internal Standardization
Compensate for physical interferences Viscosity Surface tension
Compensate for some chemical interferences High salts Mass related effects (ICP-MS)
Improve short term precision (simultaneous detectors)
Decrease long-term drift
Internal Standard Kit
Glass Expansion
New Modular Internal Standard Kit
Internal Standard Kit
Glass Expansion
IS Tee with Built-in Mixing Chamber
Internal Standard Kit
Glass Expansion
New Flared-End Pump Tubing
The final building block of a totally modular system
Internal Standard Kit
Glass Expansion
IS Schematic
Internal Standard Kit
Sample IS
Peri Pump
Glass Expansion
Niagara™ Rapid Rinse Accessory
Interfaces between ICP & Autosampler
Reduces required rinse time Programmable delay time Less than 8 inches high Includes adj. height stand
Rapid Rinse Accessory
Glass Expansion
How Niagara Works
Rapid Rinse Accessory
Analysis Rinse
Glass Expansion
Niagara Time Saving (30 sec rinse)
Standard System With Niagara
Probe to sample 5 5
Uptake delay 15 15
Stabilization 10 10
Read 15 15
Probe to rinse 5 5
Rinse 30 5
Total (seconds) 80 55
Rapid Rinse Accessory
= Rinse steps
Glass Expansion
Summary
MicroMist nebulizers Efficient sample consumption Minimum waste generation
Helix spray chambers Eliminate o’ring maintenance and contamination Reduce carryover
Internal standard kit Improved accuracy without the work Easy & inexpensive modular replacement
Niagara Rapid Rinse Accessory More samples per hour Faster sample turnaround time
Rapid Rinse Accessory