Innovations in ICP Sample Introduction Jerry Dulude, Glass Expansion, Inc. 4 Barlows Landing Rd. Pocasset, MA

Innovations in Sample Introduction 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 UPTAKE RATE (ML/MIN) Indirect drain collection method Low-Flow Nebulizers Glass Expansion

Tertiary Flow Rate vs. Uptake (ul/min) Low-Flow Nebulizers Glass Expansion

Corroboration of Tertiary Flow Rates Uptake rate (ml/min) Indirect Method (mg/min) Direct Method* 0.03 15 14 0.11 23 21 Todoli, Hernandis, Canals, and Mermet, JAAS, 1999, 14, 1289-1295 Using GE MicroMist nebulizer with U-tube absorption for measurement Low-Flow Nebulizers Glass Expansion

Primary Aerosol Size Distribution Comparison Nebulizer Gas Flow Rate = 1.0 L/Min Solution Uptake Rate = Natural Aspiration D32 = 17.2 Conikal (2ml/min) 20 60 100 Normalized Count MicroMist (0.03ml/min) Normalized Volume 20 60 100 D32 = 7.1 Diameter (mm) 10 20 30 40 50 60 Diameter (mm) 10 20 30 40 50 60 Low-Flow Nebulizers Glass Expansion

Tertiary Aerosol Size Distribution Comparison Nebulizer Gas Flow Rate = 1.0 L/Min Solution Uptake Rate = Natural Aspiration Baffled Cyclonic Spray Chamber Conikal (2ml/min) 20 60 100 D32 = 4.9 Diameter (mm) 20 60 100 D32 = 5.0 MicroMist (0.03ml/min) 10 40 30 50 Normalized Count 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 Chambers Advances in Nebulizer Installation 1993 1984 1996 Helix O’ring free spray chamber Glass Expansion

Helix O'ring-Free Spray Chamber Reduced carryover Faster washout Higher purity Can stand up to ketones and other solvents Helix O’ring free spray chamber Glass Expansion

New Internal Standard Kit Benefits 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 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 Peri Pump Sample IS Internal Standard Kit 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 Analysis Rinse Rapid Rinse Accessory Glass Expansion

Niagara Time Saving (30 sec rinse) Standard System With Niagara Probe to sample 5 Uptake delay 15 Stabilization 10 Read Probe to rinse Rinse 30 Total (seconds) 80 55 = Rinse steps Rapid Rinse Accessory Glass Expansion

Summary MicroMist nebulizers Helix spray chambers 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 Glass Expansion