Northern Michigan Operators Spring Seminar. Lab Issues

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1 Northern Michigan Operators Spring Seminar Lab Issues

2 Wastewater Laboratory Issues Changes to List of EPA Approved Procedures Methods Update Rule (MUR) Changes to MDEQ-OTCU Wastewater Lab Training Manual Speed Up Your Lab Without Compromising Data Integrity Luminescent Dissolved Oxygen Probe (LDO)

3 Monday, March 12, 2007 Federal Register Environmental Protection Agency 40 CFR Part 122, 136, et al. Guidelines Establishing Test Procedures for the Analysis of Pollutants Under the Clean Water Act; National Primary Drinking Water Regulations; and National Secondary Drinking Water Regulations; Analysis and Sampling Procedures; Final Rule Methods Update Rule

4 Methods Update Rule Sample Collection, Preservation, and Holding Time Requirements Changed general sample preservation temperature from 4 o C to 6 o C. For metals other than boron, hexavalent chromium, and mercury, the EPA will allow sample preservation with nitric acid 24 hours prior to analysis. (Acid preservation in the field for metals is not required)

5 Methods Update Rule Clarified that start of holding time for a grab sample starts at the time of sample collection. The holding time for a composite sample starts at the time the last sample component is collected. Analyze Immediately generally taken to be within 15 minutes. Preserve samples within 15 minutes of collection, unless otherwise instructed in method.

6 Methods Update Rule Withdrew approval for 105 methods from EPA s Methods for the Chemical Analysis of Water and Wastes

7 130.2 Hardness Titration, EDTA ph, Electrometric Non-Filterable Residue (TSS) Total Residue (Total Solids) Temperature Alkalinity 325.1,2,3 Chloride 330.1,2,3,4,5 Chlorine Residual 335.1,2,3 Cyanide 350.1,2,3 Ammonia N 351.3,4 Total Kjeldahl N 353.1,3 Nitrate-Nitrite N Nitrite N 360.1,2 Dissolved Oxygen Phosphorus, Single Reagent BOD COD Oil and Grease Withdrawn Some Old Standbys

8 EPA Lab Methods Were Made Greener Approved the replacement of the mercuric sulfate catalyst with copper sulfate for the determination of Total Kjeldahl Nitrogen Withdrew approval for all oil and grease methods that use Freon-113 as an extraction solvent

9 Changes to List of EPA Approved Procedures Methods Update Rule (MUR) 22 New Test Methods Approved for Wastewater and Drinking Water Anlaysis Approved About 200 Updated Methods ASTM Standard Methods Official Methods of Analysis of AOAC, Int.

10 Microbiological Test Methods March 26, 2007 USEPA Released Federal Register Notice, Guidelines, Establishing Test Procedures for the Analysis of Pollutant; Analytical Methods for Biological Pollutants; Final Rule. Modifies the EPA s Guidelines that establish approved bacterial testing procedures for analysis and sampling under the Clean Water Act.

11 EPA Approved E. coli Methods for Ambient Water Standard Methods 9221 B.1/9221 F multiple tube fermentation, presumptive followed by confirmed test using EC-MUG Medium 9222 B / 9222 G membrane filtration, total or fecal coliform followed by confirmation using EC-MUG or Nutrient Agar- MUG D membrane filtration, mtec agar, followed by Urea Substrate (2 step incubation)

12 EPA Approved E. coli Methods for Ambient Water USEPA membrane filtration, mtec agar, followed by Urea Substrate (2 step incubation) 1603 membrane filtration, modified mtec (2 step incubation) 1604 membrane filtration, MI agar or MI broth and TSA

13 EPA Approved E. coli Methods for Ambient Water Hach Chemical Co. mcoliblue-24 membrane filtration, incubation at 35 o C for 24 hrs IDEXX Laboratories, Inc. Colilert Colilert-18 mpn, multi-well, 24 hour incubation, MUG fluorescent mpn, multi-well, 18 hour incubation, MUG fluorescent

14 EPA Approved E. coli Methods for Wastewater and Biosolids USEPA membrane filtration, modified mtec (2 step incubation) Hach Chemical Co. mcoliblue-24 membrane filtration, incubation at 35 o C for 24 hrs IDEXX Laboratories, Inc. Colilert MPN, multi-well, 24 hour incubation, MUG fluorescent Colilert-18 MPN, multi-well, 18 hour incubation, MUG fluorescent

15 MDEQ OTCU Wastewater Laboratory Procedures Training Manual Lab Manual Changes 2008 Re-wrote many of the Discussions Reviewed Every Procedure Referenced Standard Methods, ASTM Deleted Nesslers for Ammonia COD Cyanide

16 MDEQ OTCU Wastewater Laboratory Procedures Training Manual Lab Manual Changes 2008 Added: Chloride Electrode Nitrate Electrode Total P 2 Reagent BOD Troubleshooting Glucose / Glutamic Acid Procedure 40 CFR Part 136, March 2007 Bacti Counting Procedure

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20 Speed Up Your Lab Without Sacrificing Data Integrity

21 Speed Up Your Lab Hach PhosVer 3 TNT (Test N Tube) Procedures

22 Speed Up Your Lab Membrane Filters Rather Than Gooch Crucibles for Suspended Solids

23 Speed Up Your Lab Bacti Media Ampules Heat Sink Bacti Incubator

24 Speed Up Your Lab A-1 Medium MPN for Fecal Coliform in 24 Hours

25 Speed Up Your Lab New Procedures for E-coli by MPN, Membrane Filtration Coliform Red E-Coli - Blue Hach m-coli Blue Idexx Quanti-Tray

26 Speed Up Your Lab Use Micro-Pipet for Prep of Standards, Spikes

27 Speed Up Your Lab Electrodes Ammonia Chlorine Residual Chloride Nitrate

28 Speed Up Your Lab Excel Spreadsheets Phosphorus Calibration Curve

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31 Speed Up Your Lab Excel Spreadsheets Quality Control Charts

32 Monthly Operational Reports Final Effluent Worksheet

33 EDMR Worksheet

34 Hach Luminescent Dissolved Oxygen Probe (LDO) No membranes! Infrequent calibrations Time and Date stamp, Operator and Sample ID No electrolyte to replace or anode to polish 1-year sensor life EPA recommended method* *Has Not Been Approved By EPA Region 5

35 YSI ProODO Handheld Optical Dissolved Oxygen Meter Based on usage, calibrations can be stable for up to one year and are stored in each sensor. Non-consumptive luminescent method eliminates stirring. Designed to fit in standard 300 ml BOD bottles. User-replaceable cables in lengths of 1 to 100-meters.

36 Orion 3-Star RDO Portable Meter RDO Optical Dissolved Oxygen Sensor Automatic temperature compensation and convenient press-on RDO caps. The RDO sensor has an internal clock that counts down the 365 day lifespan of a new RDO cap. The countdown begins when the RDO cap is installed on the RDO sensor, the sensor is connected to the meter and the first measurement is taken. The 365 day countdown cannot be reset or changed once the first measurement is taken.

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39 MWEA Regional Operators Meeting Lab Issues