10:30-11:45 VELAP Certification: Understanding Proficiency Testing Requirements and Common On-Site Assessment Issues* 1.25 (Cathy Westerman, DCLS)

Transcription

1 MORNING: 16 th ANNUAL GOOD LABORATORY PRACTICE CONFERENCE SCHEDULE August 3, 2010 Current Issues and Challenges 8:30-8:45 Welcome & Introduction (Wendy Harding, VA AWWA/VWEA LPC Chair) 8:45-9:30 Quality Systems and SOPs*.75/ ** (Marlene Moore, Advanced Systems, Inc.) 9:30-10:00 The Dynamic PT Program - Current and Future Changes* (Henry Beauchamp, Wibby Environmental) 10:00-10:30 BREAK The Proficiency Testing (PT) program is a very dynamic program in TNI. This presentation will discuss the current changes being discussed in the PT committee and the PT Board. Also on July 1, 2011, the new TNI NELAP accreditation standard will go into effect, replacing the 2003 NELAC standards. There are proficiency testing requirements that affect laboratories. The changes will also be discussed. The requirements of the PT accreditor will also change which is useful for the labs to know. 10:30-11:45 VELAP Certification: Understanding Proficiency Testing Requirements and Common On-Site Assessment Issues* 1.25 (Cathy Westerman, DCLS) AFTERNOON Session #1: 1:15-1:45 Cyanide Determination Using MICRODIST and the Importance of Mitigating Interferences (Angelina Moore, Hampton Roads Sanitation District)* Over the years various concerns have risen over the accuracy of determining total cyanide in wastewater. Among them, mitigating interferences and sample preparation are the most widely discussed. Even though addition of ascorbic acid to remove oxidizers is listed in the 40 CFR as an approved procedure in cyanide determination, the problems with using ascorbic acid have been reported. One paper stated that the addition of ascorbic acid can cause a positive and/or negative bias in determining cyanide, thus analysis of such samples should be done within the first twentyfour hours of collection. To explore the implications of ascorbic acid on cyanide determination, a study was conducted in In the study, ascorbic acid was added to high purity water and wastewater samples in which some of them were spiked with known concentration of cyanide. The concentrations of cyanide were determined in twenty-four hours of sample collection or preparation and after several days. The results of the study will be discussed. Also, a new technique, MICRODIST has been implemented in our lab to improve the efficiency of cyanide sample preparation through distillation. Benefits of using the MICRODIST system compared to Midi-Dist systems will be discussed. 1:45-2:15 Validation of a Solvent-Free Method for Membrane Recoverable Oil and Grease Analysis by Infrared Determination (ASTM D7575)*

2 2:15-2:45 BREAK (William Telliard, Consultant (EPA Retired)) Oil and grease is one of the five conventional pollutants covered by the 1974 Clean Water Act. The measurement of oil and grease in included in all of the National Pollution Discharge Elimination Systems (NPDES) permits, all pre-treatment permits, and all industrial Effluent Guidelines. It is important to note that it is the second most-enforced-against-parameter--second only to ph. As a result of the Montreal Protocol, which entered into force in 1989, EPA was required to move from a Freon extraction determination method to an n-hexane extraction mass-based determination method, creating four new issues: 1) a flammable liquid is required, 2) n-hexane is a known neurotoxin and carcinogen, 3) the analytical time is significantly increased, and 4) we are left with a large amount of n-hexane for disposal. Note that an estimated 1.1 million liters of n-hexane is used each year for EPA Method 1664A analyses. A new method "ASTM D7575"--A-Method for Solvent-Free Membrane Recoverable Oil and Grease by Infrared Determination will remedy the four issues listed above by removing the use of hexane or any other solvent from the analysis or cleanup. This new Green Chemistry method is currently under consideration for EPA's Method Update Rule. 2:45-3:15 Simplified Procedure for the Determination of Total Kjeldahl Nitrogen in Water and Wastewater* / ** (Cary B. Jackson, Ph.D., Hach Company) Total Kjeldahl Nitrogen (TKN) is defined as the sum of organic nitrogen and ammonia present in a wastewater sample. A preliminary digestion is used to oxidize carbon compounds to carbon dioxide, and convert organic forms of any nitrogen present (amino acids, proteins, peptides) to ammonia. The traditional digestion uses sulfuric acid in combination with mercury or copper catalysts and salts. Maco-digestion (500 ml) of at least two hours is followed by addition of sodium hydroxide, where the ammonia is distilled into boric acid or buffer solution. The ammonia distillate is then measured by back titration or nesslerization. In the simplified TKN method (stkn), inorganic and organic nitrogen (total nitrogen) are oxidized to nitrate by micro-digestion with peroxodisulfate. The micro-digestion (<2 ml) takes one hour and requires no distillation. The nitrate ion from the distillate is reacted with 2,6-Dimethylphenol in a solution of sulfuric acid and phosphoric acid to form nitrophenol where it is measured colorimetrically. A second sample is analyzed for nitrate-nitrite by reacting with 2,6- Dimethylphenol, measured colorimetrically, then subtracted from the results of the digested sample. stkn results are comparable to traditional macro digestion and analysis methods. 3:15-3:45 The Impact of Toxicity in Water and Wastewater* / ** (Tracy Weidman, SDIX) Toxicity, whether environmental or man-induced, has a tremendous impact not only on human health, but also on our water and wastewater treatment systems. This presentation will: define toxicity, describe contaminants of concern, discuss the importance of water security, and explain an overview of industry toxicity test methods. Session #2: 1:15-1:45 A Comparison of Recent EPA Alternate Test Procedures (ATPs): Non-Stirred vs. Stirred BOD Analysis by Optical Dissolved Oxygen Measurement* / ** (Kelly Sweazea, Thermo Scientific)

3 Optical dissolved oxygen (DO) probes are the biggest innovation in DO measurement since the 1950 s and 1960 s, when Clark-type polarographic and galvanic membrane electrodes were introduced for water and wastewater testing. Optical DO probes offer more than the portability, ease of calibration, and fast measurement associated with traditional membrane electrodes. Optical DO technology provides a probe that is easier to use, requires little or no maintenance, requires no sample flow or stirring, has improved accuracy at low DO levels, and shows minimal drift over time. Optical DO technology is written into DO methods by ASTM and USGS, and is currently being considered for incorporation into Standard Methods for the Examination of Water and Wastewater. Three new ATP Approval Letters were released by the EPA on November 3, 2009 for the measurement of DO, BOD, and CBOD by Optical Probe. The EPA will recommend inclusion in 40 CFR Part This presentation will focus on the methodology used in preparing the ATPs and statistical comparison of BOD results from the traditional Clark cell technology to the Optical DO technology, focusing on the effect of Non-Stirred to Stirred analysis. A total of over 3000 samples of 10 different matrices were analyzed by 10 individual laboratories. 1:45-2:15 Getting USEPA Regional 3 and State of Virginia Approval to use your Luminescent (LDO and RDO) DO Sensors* (Greg Starlin, Hach Company) 2:15-2:45 BREAK In 2006 the USEPA recommended the approval of ASTMD Method C (Measuring Dissolved Oxygen with a luminescent-based sensor) and Hach Method (Luminescence Measurement of Dissolved Oxygen in Water and Wastewater). Since that time, several Regions have exercised their authority under 40CFR part to allow use of luminescent DO methods. This presentation will cover the regulatory approval process and audit requirements in USEPA Region 3, State of Virginia, for probes using luminescent DO methods. Luminescent DO Methods, USEPA letters recommending interim approval, templates for approval request letters, QC data requirements, and Regulatory Contact information will be also be provided. [1] LDO is a registered trademark of Hach Company, Loveland, CO USA. RDO is a registered trademark of In-Situ Inc., Fort Collins, CO USA. 2:45-3:15 GC Troubleshooting* (Greg Hudson, Envirocompliance Laboratories) Gas Chromatography has become an indispensible tool in the environmental laboratory. Like many technological devices, the GC does a great job providing useful data when it operates at top performance; however, all technology comes with its own special needs. Although maintenance is often the best policy for preventing frustrating down-time, a basic understanding of the inner functions of a GC is critical in dealing with problems in day to day operation of the instrument. This session will provide a general overview of a typical Gas Chromatography system and offer some insight in approaching general troubleshooting techniques for these instruments. 3:15-3:45 Sampling Technique and How it Affects Sample Analysis* / ** (Lisa M. Galloway, City of Richmond, DPU ) The City of Richmond collects a variety of analytical samples: drinking water, wastewater, process control and industrial wastewater. The Water Treatment Plant and Wastewater Treatment Plant

4 Laboratories perform many different analyses to monitor the distribution system, treatment plant efficiency and industrial discharges. It is important to provide accurate and reliable results to the public and plant personnel. Sample collection is the beginning of the sample analysis process. Improper sampling can affect analytical results. This presentation will discuss sample collection procedures, documentation, sampling equipment, sample preservation and how these all affect sample analysis. Session #3 1:15-1:45 Overview of New EPA Method Determination of Residual Chlorine in Drinking Water Using an On-line Chlorine Analyzer* (Chris Griffin, Hach Company.) The new EPA Method (Sep 2009) may allow the use of on-line chlorine analyzers based on chemistry different from that of approved methods. This new method is performance based. In the method, Quality Control (QC) criteria are outlined to benchmark the performance of an on-line chlorine analyzer against the performance of approved grab sample chlorine methods. If the on-line analyzer meets the QC criteria in the method, the data are deemed equivalent to data obtained using the approved grab sample methods. Consequently, EPA Method can be used with any type of on-line chlorine analyzer - - even one where an approved method is not incorporated in the design. This presentation will review the scope and application of the Method, a review of typical on-line equipment choices, calibration requirements, routine procedures, and QC testing requirements. 1:45-2:15 All About IC: Using Ion Chromatography for Drinking Water Analysis* (Susan Miller, Fairfax Water) 2:15-2:45 BREAK An Ion Chromatograph (IC) is an integral part of a drinking water laboratory. This presentation will include discussion of all features of the IC with information for beginning IC analysts as well as information for more experienced IC users. There will be an explanation of two IC methods: EPA Method and The specific analytes to be discussed are: fluoride, chloride, nitrite, bromide, nitrate, sulfate, phosphate, and bromate. Quality control parameters for both methods will be outlined. One of the first steps to learning the IC is to learn how the instruments work. I will discuss the basic parts that make up an IC and how the sample flows through the instrument. Learning how to determine problems and troubleshoot them is also an important key to successful IC use. I will discuss what specific clues to look for when an analysis is not successful and how to remedy problems. These issues include problems with standard recoveries, blank contamination, low peak areas and matrix interference. The topic of manual integrations is another area of interest that will be covered. Many times manual integration can be avoided with proper detection parameters. In some cases, manual integration is necessary and I will discuss how to perform and document them appropriately. Purchasing IC equipment will be discussed as well by addressing issues such as how to pick a vendor and determining what your laboratory s needs are.

5 2:45-3:15 New EPA Methods: Determination of Disinfection by-products Bromate and Haloacetic Acids by Direct Injection of Drinking Waters With High Ionic Strength Matrices* (Richard Jack, Dionex Corporation) Bromate is regulated in drinking water at 10 ug/l. EPA Methods B, 317.0, and are approved by the US EPA for compliance monitoring. High concentrations of common anions produce poor bromate peak shapes and lower recoveries. This often requires the analyst to either dilute the sample which raises the minimum reporting limit (MRL) or pretreat the sample offline prior to analysis. Pretreatment of samples requires increased time and cost for each analysis. This paper describes a new EPA pending method (EPA 302.0) using two-dimensional (2D) ion chromatographic (IC). A second EPA pending method (EPA 557) was developed for Haloacetic Acid determination by direct injection using IC- MS/MS. Current EPA methods using GC-ECD require laborious sample preparation. HAA's are regulated as HAA(5) to 60 µgl. Both methods meet the regulatory limits set forth by the EPA Office 3:15-3:45 Continuous Imaging Fluid Particle Analyzer for the Detection, Identification and Enumeration of Taste & Odor Causing Algae and Cyanobacteris* (Harry Nelson, Fluid Imaging Technologies, Inc. Controlling nuisance taste and odor causing algae and cyanobacteria in surface water systems often require treatment methodologies (e.g., algaecides, Copper Sulfate applications, etc.) having significant and undesirable side effects. Effective algae monitoring programs can help the conscientious water quality professional minimize the number and volume of treatment applications by identifying bloom conditions early, but effective algae monitoring programs require daily and labor intensive data gathering, along with algae taxonomic expertise - resources that are unfortunately difficult for many municipalities to support. Fluid Imaging Technologies Inc. has developed an instrument for algal detection and analysis called a FlowCAM. The FlowCAM is a continuous imaging particle analyzer now being used for monitoring of microorganisms and particles in both marine and freshwater systems. A laser interacts with a high resolution digital camera to capture images and data of a passing particle or cell. The FlowCAM offers cell counts, size data, pattern recognition, volume calculation, organism classification, image management, and image library development. A key benefit of the technology is the collection of high resolution color digital images for further analysis and postprocessing. The FlowCAM s proprietary software uses a powerful image recognition algorithm providing the water quality professional with a means to automatically identify and quantify organisms of interest, such as algal species that can cause taste and odor occurrences, as well as cyanobacteria. An overview of the technology and software will be presented, along with specific case studies from applications by municipal water treatment organizations. *0.5 CPE Credits available for water operators (or designate time noted) **0.5 CPE Credits available for wastewater operators

6