Data Management

Quality Assurance / Quality Control

The oversight of data QA/QC will be the responsibility of Mr. Peter Smith, who heads the instrument laboratory in the Department of Land Resource Science at the University of Guelph. He has twenty years of experience in quantifying both organic and inorganic analytes, in biological and mineral matrices. Specific to metals analyses, his laboratory contains graphite furnace atomic absorption spectrophotometer, with Zeeman background correction, as well as GF-AAS with deuterium lamp; ICP-AES; microwave digestion; X-ray diffraction. He has co-authored method development papers for Sn and Tl analyses in municipal sewage biosolids with Hale and Hargreaves (MSc with Hale, 2003). Consistent with the approach he used in MITE-RN, Smith will 'enrol' all MITHE-SN principal investigators in twice yearly round-robin QA/QC exercises coordinated by the National Laboratory for Environmental Testing (NLET, National Water Research Institute, CCIW, Burlington, ON). Sub-samples of waters and sediments are sent to all laboratories for analysis by their local procedures, and the results are then compared with the known values. Biological media for round-robin testing will be addressed by Smith, who will collect a large quantity of several matrices that are relevant to MITHE-SN projects, and have the metals of interest, in concentrations that are comparable to the assays being performed, determined. Each of these media will be homogenized, and then digested and analyzed for metals in Smith's laboratory, as well as one other MITHE-SN laboratory who achieves an 'excellent' rating, to establish the concentrations of metals of interest. Then, these materials will be included in the round-robin exercise for those laboratories that analyze such media. Following each round-robin exchange, Smith will then review the performance of each laboratory participating in MITHE-SN, working with any that do not receive a satisfactory rating to improve their metals analyses. The cost of MITHE-SN's participation in the NLET will be borne by Environment Canada as an in-kind contribution to the Network.

MITHE QA/QC 2005

There are essentially three ways we try to ensure the quality of data generated by MITHE researchers.

1. Each laboratory is required to submit a QA/QC report outlining: personnel, training requirements of analytical staff and graduate students, types of analytical instrumentation, analytes measured, concentration of analytes measured, and quality control protocols used in the laboratory, i.e., standard reference materials, blanks, cleaning procedures, digestion methods etc. Attached is a sample QA/QC report to follow. This report is due no later than May 31/05.
   
   
2. Researchers are required to participate in annual inter -laboratory performance studies. They are conducted by the National Laboratory for Environmental Testing, of Environment Canada at the National Water Research Institute. Participating laboratories receive blind samples and are required to analyze them for the elements they routinely measure. The cost is covered by Environment Canada.
   
   
3. Researchers are also required to write annual reports outlining changes in personnel, equipment or procedures that may affect their QA/QC protocols. If a lab receives a poor rating on the inter-lab study they must explain, why and what they did to correct the problem.

Quality Assurance / Quality Control

MITHE - RN Projects

Department of Land Resource Science Instrument Laboratory

University of Guelph

Revised Protocols – Feb. 2005

Personnel

Laboratory Supervisor - Peter S. Smith
MITHE Principal Investigators - Dr. Beverley Hale, University of Guelph.
Technician – Debbie Chan

Training Requirements
Peter Smith and Glen Wilson are the two senior laboratory technicians responsible for training personnel and ensuring proper analytical protocols are followed. New personnel including research assistants, technicians and graduate students are trained in sample preparation, method development, instrument operation, analysis and QA/QC using a hands-on approach through seminars and personalized instruction.

Instrument inspection and maintenance
Most of the equipment used in the Department of Land Resource Science is located in the Instrument Laboratory, isolated from potentially contaminating sample preparation areas. For each piece of equipment there is a logbook in which time and type of analysis are recorded. The senior laboratory technicians maintain all analytical equipment within the Instrument Laboratory. Manufacturers carry out periodic service to the instruments.

Quality control protocols:

Sample Description , Analytes and concentration range

Plant Tissues: Cd, Ni, As, Fe, Cu, S – low ppb to ppm
Soils and Sediments: Cd, Ni, As, Fe, Cu, S - low ppb to ppm

Sample Accountability and Identification .
Each sample brought into the laboratory is assigned a label that identifies the date the sample was collected, sample type, origin and the technician or graduate student responsible for handling the samples. This information is recorded in a laboratory manual.

Sample Storage and Preparation

• Plant samples are oven dried at 60 deg. C until constant weight. They are then finely ground in a Retsch ZM 100 plant grinder with a titanium rotor and sieve. Soils and sediments are refrigerated or frozen if preparation is not imminent
• Soils and sediments are air –dried and sieved with a <2mm polypropylene sieve. A 10.0 gram sub-sample is taken and oven dried at 105 deg. C for 24 hours for moisture content.
• Samples are digested using EPA SW 846 test methods 3050, 3050B, 3051, 3052 or modifications thereof depending on the analyte of interest, the matrix and the instrumentation used for analysis. All acids are of trace metal grade. All solutions are made up with 18Mohm/cm water.
• Solutions are stored in LDPE screw cap bottles.
• All glassware and bottles are acid washed and rinsed with 18.3 Mohm/cm water.
• All handling and preparation of samples is designed to minimize metal contamination.

Standards

Instrument standards:

• Multi- and single elementcalibration standards are made from single-element, certified ICP standards, traceable to NIST, purchased from SCP Science.

Certified reference materials include:

• Soils and sediments: NIST- SRM -2709 San Joaquin Soil, SRM 2711Montana Soil Moderately Elevated Concentrations, SRM –1944 New York /New Jersey Waterway Sediment

Plants:

• SRM 1573a Tomato Leaves, SRM 1570a Spinach Leaves, SRM 1547 Peach Leaves.

Instrumentation for metal analysis.

Atomic Absorption Spectroscopy:

• SpectrAA 880Z GFAAS: Low ppb to 100ppb, depending on analyte
• Varian SpectrAA-220 FAAS : Hi ppb to ppm, depending on analyte
• Atomic Emission Spectroscopy: Varian Vista Pro Axial ICP OES: 50 ppb to Hi ppm, depending on analyte.

QA/QC for Instrumentation and Analysis
When using flame AAS, the standard of highest value is used to optimize the instrument before analysis is begun. Quality control checks including one or more reference solutions are included in each set of analysis. References and standards are made from separate stock solutions yet contain the same matrix.

Standards are matrix matched to samples and prepared using 1000 m g L -1 NIST traceable certified elemental stock standard solutions. For each analysis, a 3-5 point calibration curve is constructed. NIST Standard Reference materials are used to check recoveries of each analyte.

The analysis is performed using the following format:

1. Blank- Reagent water with same concentration of acids as samples and standards.
2. QC standard 1- Calibration verification standard –SRM certified NIST traceable standard.
3. Control standard – spiked sample of 2-5 times known value.
4. Sample 1
5. Sample 2 etc.

Repeat 1,2, and 3 after twenty sample analyses.

If the QC standards or SRM reference solutions are not within 10% of the certified value then the analysis is repeated.

Data management
Any samples having suspect values are re-analyzed. The technician or graduate student who performed the analysis keeps a hard copy of the data. An electronic copy of the data is given to the principal investigator as well as other team members who require it.

General References:

• Benoit, G.(1994). Clean technique measurement of Pb, Ag, and Cd in freshwater: A redefinition of metal pollution. Environ. Sci.Technol, 28: 1987 -1991.
• Garfield , F. Klesta, E. and Hirsch, J. (2000) Quality Assurance Principles for Analytical Laboratories, 3 rd Edition . AOAC International.
• Hurley, J.P., et al. (1996). Trace metal assessment of Lake Michigan tributaries using low-level techniques. Environ. Sci. Technol., 30: 2093-2098.
• Moody, J. R. and Lindstrom , R. M.(1977). Selection and cleaning of plastic containers for storage of trace element samples, Anal. Chem., 49, 2264.
• Nolting, R.F. and de Jong J.T.M (1994). Sampling and analytical methods for the determination of trace metals in surface seawater. Intern. J. Environ. Anal. Chem ., 57: 189-196.
• Nriagu, J.O. et al. (1996). Dissolved trace metals in lakes Superior, Erie and Ontario. Environ. Sci. and Technol., 30: 178-187.
• Varian. (1986). SpectrAA-300 and SpectrAA-400: Operation Manual. Varian Australia Pty Ltd., Mulgrave, Victoria, Australia,.
• Varian.(1988). Analytical Methods for Graphite Tube Atomizers. Varian Australia Pty Ltd., Mulgrave, Victoria, Australia,.
• Varian.(1989). Flame Atomic Absorption Spectrometry: Analytical Methods. Varian Australia Pty Ltd., Mulgrave, Victoria, Australia,.
• USEPA SW- 846 On- Line Test Methods for Evaluating Solid Wastes Physical/ Chemical Methods, Series 3000.

Supervised by: