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    Update On The Standard Methods 23rd Edition MELA

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    This document provides an overview and summary of updates to Standard Methods for the Examination of Water and Wastewater for the 23rd Edition. It discusses revisions made to quality assurance methods, as well as methods for examining physical/aggregate properties, metals, inorganic nonmetallics, organic constituents, radioactivity, toxicity, microbiology, and biology. For Part 4000 (inorganic nonmetallics), it outlines modifications to existing methods for chloride, chlorine, nitrate, silica, sulfite, and TKN, as well as plans for new methods involving cyanide, nitrate by reductase colorimetry, total nitrogen by HTCO and chemiluminescence, and total nitrogen by persulf

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    Update On The Standard Methods 23rd Edition MELA

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    micro biology
    152 views39 pages
    This document provides an overview and summary of updates to Standard Methods for the Examination of Water and Wastewater for the 23rd Edition. It discusses revisions made to quality assurance methods, as well as methods for examining physical/aggregate properties, metals, inorganic nonmetallics, organic constituents, radioactivity, toxicity, microbiology, and biology. For Part 4000 (inorganic nonmetallics), it outlines modifications to existing methods for chloride, chlorine, nitrate, silica, sulfite, and TKN, as well as plans for new methods involving cyanide, nitrate by reductase colorimetry, total nitrogen by HTCO and chemiluminescence, and total nitrogen by persulf

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    Update on the Standard Methods 23rd Edition MELA

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    This document provides an overview and summary of updates to Standard Methods for the Examination of Water and Wastewater for the 23rd Edition. It discusses revisions made to quality assurance methods, as well as methods for examining physical/aggregate properties, metals, inorganic nonmetallics, organic constituents, radioactivity, toxicity, microbiology, and biology. For Part 4000 (inorganic nonmetallics), it outlines modifications to existing methods for chloride, chlorine, nitrate, silica, sulfite, and TKN, as well as plans for new methods involving cyanide, nitrate by reductase colorimetry, total nitrogen by HTCO and chemiluminescence, and total nitrogen by persulf

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    152 views39 pages

    Update On The Standard Methods 23rd Edition MELA

    Uploaded by

    micro biology
    This document provides an overview and summary of updates to Standard Methods for the Examination of Water and Wastewater for the 23rd Edition. It discusses revisions made to quality assurance methods, as well as methods for examining physical/aggregate properties, metals, inorganic nonmetallics, organic constituents, radioactivity, toxicity, microbiology, and biology. For Part 4000 (inorganic nonmetallics), it outlines modifications to existing methods for chloride, chlorine, nitrate, silica, sulfite, and TKN, as well as plans for new methods involving cyanide, nitrate by reductase colorimetry, total nitrogen by HTCO and chemiluminescence, and total nitrogen by persulf

    Copyright:

    © All Rights Reserved
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    of 39

    Update on Standard Methods for the Examination

    of Water and Wastewater, 23rd Edition


    and what’s new for Part 4000

    William Lipps
    Analytical & Measuring Instrument Division
    October 2017
    Thank You
    [email protected]
    23rd Edition
    Standard Methods is a joint effort of these
    societies
    American Public Health American Water Works Water Environment Federation
    Association (APHA) Association (AWWA) (WEF)

    Editor Editor Editor

    PC PC PC

    JTG JTG JTG


    Parts or Chapters of Standard Methods
    Part 1000 Quality Assurance

    Part 2000 Physical and Aggregate Properties

    Part 3000 Metals

    Part 4000 Inorganic Nonmetallic Constituents

    Part 5000 Aggregate Organic Constituents

    Part 6000 Individual Organic Compounds

    Part 7000 Radioactivity

    Part 8000 Toxicity

    Part 9000 Microbiological Examination

    Part 10000 Biological Examination


    Part 1000 – Quality Assurance

    Revised 1020 QA/QC for more consistency with:


    • 2020
    • 3020
    • 4020
    • 5020
    • 6020

    Revisions to 1040 – Method Development and Evaluation


    Part 2000 – Physical and Aggregate
    Properties
    New Method 2510C Total Intensity Odor – numerically rate perceived odor

    Clarification to Method 2330 – Calcium Carbonate Saturation

    Clarifications and minor additions to:

    • 2540 – Solids
    • Quality control
    • Sources of Error
    • Interferences
    Part 3000 – Metals

    Revised 3020 QA/QC


    Part 4000 – Inorganic Nonmetallic Constituents

    Revised 4020 QA/QC

    Revised 4500-CN-
    • Sampling, preservation, pretreatment
    • Interferences

    Revised 4500-NO3-
    • Reagent preparation, calibration, interferences

    New Method 4500-O Dissolved Oxygen (optical probe)


    • 46 PT samples, 2 matrices, 3 manufacturer’s probes
    • 85 side by side with membrane probe
    Part 5000 – Aggregate Organic Constituents

    Revised 5020 QA/QC

    Update 5210 BOD


    • Plastic bottles
    • Optical probe
    • pH adjust 6.5 – 7.5
    • 2 or more blanks < 0.2 mg/L

    Update 5310 TOC


    • Remove 5310C
    • Update QC criteria – moved to Introduction

    Update 5910 UV- Absorbing Organic Constituents


    • Buffer preparation and Sample preparation updated
    Part 6000 – Individual Organic Compounds

    Revised 6020 QA/QC

    New Method 6810 – Pharmaceuticals and Personal Care Products


    • 13 target compounds
    • LCMSMS
    • Single lab study – reagent water, drinking water, wastewater
    • Collaborative study – 5 laboratories
    Part 7000 – Radioactivity

    Revised 7010 Introduction


    • Reflect current regulations
    • Reference sources for standards
    • Discuss radioactive equilibria
    Revised 7020 QC slightly
    Revised 7040 Facilities

    New method in online version – 7110D


    • Liquid Scintillation Method for Gross Alpha-Beta
    • Works in high TDS matrices
    • SDWA Expedited Method
    Part 8000 – Toxicity

    Revised:
    • 8010 introduction growth equation
    • 8020 – adds residual chlorine check
    Hi!
    • Revisions and updates to all sections
    Part 9000 – Microbiological Examination

    Updated:
    • 9020 QA/QC,
    • 9030 Apparatus,
    • 9040 Washing and Sterilization,
    • 9050 Culture and Media
    • 9060 Sample collection
    New information on:
    • 9215 Heterotrophic Plate Count
    • 9221 Multiple Tube Fermentation
    • 9222 Membrane Filtration
    • 9223 Enzyme Substrate Coliform
    • 9230 Fecal Enterococcus/Streptococcus
    • 9250 Actinomycetes
    • 9610 Fungi
    Part 10000 –Biological Examination

    10900 Aquatic Organisms –

    Color Algae drawings replaced with


    Color Algae photographs
    23rd Edition
    Standard Methods is a joint effort of these
    societies
    American Public Health American Water Works Water Environment Federation
    Association (APHA) Association (AWWA) (WEF)

    Editor Editor Editor

    PC PC PC

    JTG JTG JTG


    The Standard Methods Organization
    American Public Health American Water Works Water Environment Federation
    Association (APHA) Association (AWWA) (WEF)

    Dr. Ellen Braun- Dr. Andrew D. Dr. Terry E.


    Howland Eaton Baxter

    8000 3000 1000

    9000 4000 2000

    10000 5000 7000

    6000

    Nathan Edman, E-mail: [email protected]) is Standard Methods Manager and


    acts as secretary to the JEB.
    Part 4000 – Inorganic Nonmetallic
    Constituents, what’s new?
    Inevitable editorial changes

    Modify existing methods

    Develop and validate new methods


    Modify existing Methods

    • Technical change requires validation


    study

    • Limited data in some

    • Equivalency?
    Chloride methods

    • Titration methods and IC can disagree

    • Interferences in titration
    Lab 4500-CL C 4500-CL D 4110B
    • Compare methods 1 3
    2 40 20
    • Collaborative study
    3 40 61
    4 13
    5 11
    6 17
    Chlorine – low level amperometric

    • Used in on-line analyzers

    • 10 ppb ML listed in method

    • Need collaborative study to validate new ML


    Nitrate – UV method

    • May be applicable to wastewater

    • JTG to draft modified method

    • Needs collaborative study for wastewater


    Silica – Manual molybdenum blue

    • Being used as test kits (in Drinking water)

    • Different complex reagents

    • Collaborative study (equivalency)

    • Allow alternative complex reagents in text


    Sulfite – iodometric titration

    • Lot’s of questions regarding Normality and the calculation

    • JTG to clarify method

    • Perform collaborative study


    Sulfide – manual methylene blue

    • Very old test with minimal data

    • JTG to test new (single) reagent recipe

    • If successful, re-write and collaborative study


    Sulfate – manual turbidimetric

    • Adds BaCl2 with a “scoop”

    • Acid drainage samples (high metals) interfere

    • Test interference removal

    • Test 10% BaCL2 solution with suspending agent

    • Re-write method, collaborative study


    Total Kjeldahl Nitrogen – with block digestion

    • Already a TKN method

    • No block digestion

    • Change Nicotinic Acid to Glycine

    • Need to prepare draft

    • Need single lab study


    New Methods

    • Literature search
    • Draft method
    • Single lab data
    • Ruggedness testing
    • Collaborative study
    Cyanide methods – gas diffusion

    • EPA, ISO, and ASTM method exist

    • Free, available, and total cyanide


    planned

    • New interference studies planned


    (compare to WAD and CATC)

    • More holding time

    • Limited collaborative study (?)


    Nitrate method – reductase by manual
    colorimetry
    • ATP, and ASTM method exist for discrete analyzers

    • Draft Written

    • New collaborative study done

    • Will ballot soon


    Total Nitrogen – HTCO with chemiluminescence
    detection
    • ASTM method

    • Draft Standard Methods Written (kind of)

    • Collaborative study done

    • Will ballot soon


    Total Nitrogen – Persulfate with nitrate by
    reductase
    • Oxidation procedure already

    • Waiting for nitrate method

    • Need to show equivalency with TN

    • Collaborative study planning


    What is method validation anyway?
    Described in SM 1040 B

    • Single Operator Tests

    • Analysis of real matrices

    • Ruggedness Testing

    • Collaborative Study
    Single operator tests

    • MDL

    • Calibration Model

    • Replicates at each concentration

    • Matrix spikes, with replicates, at each concentration

    • Comparison with existing method (equivalency test)


    Method Ruggedness

    Factor Nominal Variation

    Mixing Time 10 minutes 12 minutes

    Sample Size 5 grams 10 grams

    Acid Concentration 1M 1.1 M

    Heat to 100 ºC 95 ºC

    Hold heat for 5 minutes 10 minutes

    Stirring yes no

    pH adjust 6.0 6.5


    Collaborative Study – variables tested

    • Laboratory – at least three

    • Apparatus – model and manufacturer differences

    • Concentration dependency – three or more concentrations

    • Matrix effects – matrices of concern (at least three)

    Example = 5 labs, 4 concentrations in triplicate


    Thank You
    [email protected]

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