Course Information
Course Title: Compliant Analysis of Water, Wastes and Related Solid Environmental Samples Using Inductively Coupled Plasma Atomic Emission and Mass Spectrometry
Categories: 1 - Atomic Spectrometry
2 - Atomic Spectroscopy
3 - Mass Spectrometry
4 - Quality/Regulatory/Compliance
5 - Environmental Analysis
6 - Regulatory Compliance
7 - Sample Preparation
8 - Spectroscopy
9 - Inductively Coupled Plasma
Instructor(s): Isaac (Joe) Brenner Course Number: 3
Affiliation: Brenner Scientific
Course Date: 03/07/2009 - Saturday Course Length: 1 Day Course
Start Time: 08:30 AM End Time: 05:00 PM
Fee: $425 ($625 after 2/9/09) Textbook Fee:

Course Description
This one-day short course will address the application of ICP-AES and ICP-MS for compliant analysis of water, wastewater and related solid wastes using USEPA 200.5, 200.7, 200.8, SW 846 6010C, and 6020A These procedures will be evaluated using QA/QC criteria and figures of merit such as IDLs, MDLs, LLCV, LLICV, CCV, ICV, LDRs, recovery from spiked matrix solutions and CRMs. This course will provide an insight to practical water and waste sample analysis highlighting sampling strategies, sample preparation, instrumentation, spectroscopic and nonspectroscopic interference effects and validation. The course will commence with a brief overview of sample collection and chain of custody procedures, sample preservation, holding times, and containers. Sample preparation schemes provided by USEPA (filtration, open vessel and microwave digestion) will be described and their efficiencies compared using recovery, contamination, sample throughput, and cost. Instrumentation will be reviewed - axial vs. radial CCD and CID ICP-AES and Collision vs. Reaction cells ICP-MS. Instrument setup and optimization routines will be described. Emphasis will be placed on nonspectroscopic interference effects associated with sample introduction, the plasma, plasma-MS interface, and spectroscopic interferences, such as spectral overlap in AES and polyatomic ions in MS. Methods for their correction and compensation will be presented. ISO 17025 accreditation and analytical uncertainty will be addressed and the question of EPA procedures meeting requirements of ISO 17025 evaluated .

Target Audience
Laboratory managers, quality control and assurance specialists and managers, environmental chemists, scientists and engineers, geochemists, biologists, toxicologists, legal and. administrative officers in national institutions and industries of all categories. University academics involved in instructing environmental chemistry. For those participants planning to undertake compliant analysis of water and wastes using regulated procedures, the course will provide essential guidelines for establishing standard operating procedures and managing the QA/QC manual. For those already active in complaint analysis of waters and wastes using ICP-AES and MS and are embarking on an accreditation process such as ISO 17025, this course saves time and human and technical resources. For management and end users the course will provide important insights to QA/QC requirements and uncertainty. Indeed the message is the confidence in the methods and the operators. A basic knowledge of ICP-AES and MS and sample preparation is an advantage but not essential. The instructor will step through all the analytical requirements of the various compliant procedures and address individual requirements.

Course Outline
Course outline
MORNING
1. INTRODUCTION
1.1. Why compliant analysis
1.2. Importance of accreditation and ISO 17025 
1.3. Built-in QA/QC routines - Highlights of Compliant analysis – ISO 17025
1.4. Cost effective validation
2. SAMPLING STRATEGIES
2.1. Containers
2.2. Holding times
2.3. Types of samples  - hazardous and nonhazardous
3. DECISION MAKING – WHICH COMPLIANT PROCEDURE
3.1. Criteria
3.1.1. Recognized by regulation authorities
3.1.2. Flexibility – performance based
3.1.3. Integrated sample preparation procedures
3.1.4. Integrated QA/QC routines that meet  accreditation requirements 
4. STATUS OF ICP-AES INSTRUMENTATION
4.1. ICP-AES – CIDs and CCDs 4.2. ICP-MS - importance of the interface. Collision and reaction cells
4.3. Sample introduction system – contamination free and rapid washout
5. SAMPLE PREPARATION
5.1. SW846
5.1.1. Open vessel and microwave assisted
5.1.2.  3005A, 3015A, 3050A and B, 3051A, 3052  
5.2. Comparison of sample preparation routines
6. APPROVED ICP METHODS 
7. ICP-AES
7.1.1. EPA 200.7, 200.5 
7.1.2. Axial vs radial ICPs – the 200.5 paradox
7.1.3. SW 846 6010C
7.1.4. PLASMA OPTIMIZATION – MgII 280/MgI 285 nm
8. ICP-MS
8.1. 200.8
8.2. 6020A
10.1. Instrumental Figures of Merit and optimization
10.1.1. Sensitivity and Instrumental background
10.1.2. Short and long term term RSDS
10.1.3. % CeO/Ce, Ce++
10.1.4. Polyatomic interferences  - Collision and reaction cells
11. BLANKS 
11.1.1. Field blank
11.1.2. Equipment blank – sampler, bottles
11.1.3. Calibration blank
11.1.4.  Method Blank (Reagent blanks). 
11.1.5. Rinse blank
12. CALIBRATION PROTOCOLS 
12.1.1. Calibration blank
12.1.2. Multielement calibration standards 
13. INTERFERENCE EFFECTS - Non Spectral interferences 
13.1. Fundamental aspects
13.2. Physical interferences – sample introduction
13.3. Memory effects
13.4. Ca and Na induced matrix effects
13.5. Use of internal standards
13.6. Robust ICPs, effect of power
13.7. Spectroscopic interferences  - polyatomic ions
14. ANALYTICAL FIGURES OF MERIT AND QA/QC CRITERIA 
14.1. QC acceptance requirement
14.2. Instrumental Detection limits (IDLs)- comparison of requirements, 
14.3. Method detection limits (MDLs,) CRQLs. 
14.4. Linear Dynamic Range (LDR)
14.5. Quantitative limit (RLs)
14.6. Initial calibration/verification (Primary and secondary (ICV and CCV)
14.7. LLCV, LLICV, LLQD
14.8. Instrument performance check (IPC)
4.9. Control standards- synthetic standards
14.10. Interference check with spikes
14.11. Recovery 
14.12. Long term variations – compensation using internal standards
14.13. Dilution tests
14.14. CRM and quality control sample (QCS)
14.15. Sequence of analysis
14.16. SPECIFIC REQUIRMENTS FOR ICP-MS 
15. QA/QC 15.1. QA/QC system
15.2. EPA built-in criteria
15.3. ISO 17025 requirements – practical uncertainty
16. CONCLUSIONS
16.1. Participant discussion and problem solving
16.2. Do EPA procedures meet the requirements of ISO 17025 for formal accreditation

Course Instructor's Biography
Dr. Isaac (Joe) Brenner is an independent consultant for QA/QC, accreditation and method validation at the Dan Region of Cities Authority for Effluents and the Environment in Israel. He is a certified independent ISO 17025 auditor for analysis of waters and wastes. He currently serves as a senior scientist and visiting professor in the departments of Environmental Chemistry in Toledo and Barcelona, Spain, in the Institute of Analytical Chemistry in the Graz Technical University. Austria, and in the Department of Earth Sciences and Earth Dynamics Research Center, National Cheng Kung University, Tainan, Taiwan . Dr Brenner was the application laboratory manager in Jobin Yvon, Longjumeau, France, a senior analytical adviser for ICP and ICP-MS at the Varian Research Center, Palo Alto and for ICP-MS and AES at Thermo Fisher Scientific in Winsford, UK and Madrid, Spain. Dr. Joe Brenner has delivered more than 600 presentations, short courses, round table discussions at universities, international symposiums, research institutes, and instrument manufacturer forums; he has 100 peer-reviewed scientific publications.