Innovations in ICP Sample Introduction

1
Innovations in ICP Sample Introduction

• Jerry Dulude, Glass Expansion, Inc.
• 4 Barlows Landing Rd.
• Pocasset, MA

2
Summary of Discussion

• Low Flow Nebulizers
• Helix Oring-free Spray Chambers
• New Internal Standard Kit
• Niagara Rapid Rinse Accessory

Innovations in Sample Introduction
3
Applications of Low-Flow Nebulizers

• Limited sample volumes
• Volatile samples
• Expensive waste disposal
• ICP-MS-LC interface

Low-Flow Nebulizers
4
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
5
Transport Efficiency vs. Uptake
EFFICIENCY
UPTAKE RATE (ML/MIN)
Indirect drain collection method
Low-Flow Nebulizers
6
Tertiary Flow Rate vs. Uptake
Tertiary Flow Rate (ul/min)
Low-Flow Nebulizers
7
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, 1289-1295
• Using GE MicroMist nebulizer with U-tube
  absorption for measurement

Low-Flow Nebulizers
8
Primary Aerosol Size Distribution Comparison
Nebulizer Gas Flow Rate 1.0 L/Min Solution
Uptake Rate Natural Aspiration
Normalized Count
MicroMist (0.03ml/min)
Normalized Volume
Low-Flow Nebulizers
9
Tertiary Aerosol Size Distribution Comparison
Nebulizer Gas Flow Rate 1.0 L/Min Solution
Uptake Rate Natural Aspiration
Baffled Cyclonic Spray Chamber
Normalized Count
Low-Flow Nebulizers
10
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
11
Cyclonic Spray ChambersAdvances in Nebulizer
Installation
1993
1984
1996
Helix Oring free spray chamber
12
Helix O'ring-Free Spray Chamber

• Reduced carryover
• Faster washout
• Higher purity
• Can stand up to ketones and other solvents

Helix Oring free spray chamber
13
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
14
New Modular Internal Standard Kit
Internal Standard Kit
15
IS Tee with Built-in Mixing Chamber
Internal Standard Kit
16
New Flared-End Pump Tubing
The final building block of a totally modular
system
Internal Standard Kit
17
IS Schematic
Peri Pump
Sample
IS
Internal Standard Kit
18
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
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How Niagara Works
Rinse
Analysis
Rapid Rinse Accessory
20
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
Rinse steps
Rapid Rinse Accessory
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Summary

• MicroMist nebulizers
• Efficient sample consumption
• Minimum waste generation
• Helix spray chambers
• Eliminate oring 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