LABORATORY ISSUES

1
LABORATORY ISSUES

• DATA INTERPRETATION
• AND
• QUALITY ASSURANCE/QUALITY CONTROL

2
SUMMARY

• Laboratory Lingo
• Analysis Methods
• Quality Assurance/ Quality Control
• Reviewing and Evaluating Reports
• Resource List

3
LABORATORY LINGO

• Abbreviations
• Refer to handout
• Definitions
• Refer to handout
• Common words and terms from reports

4
DEFINITIONS

• Accuracy
• The nearness to the true value.
• Atomic Absorption Spectroscopy
• An analysis method used to determine metals. A
  digested sample of wastewater is exposed to a
  heat source that vaporizes the metal atoms
  causing them to absorb light energy. Each metal
  has a unique light frequency. The light loss is
  proportional to the number of metal atoms
• Digestion
• A wastewater sample preparation step using acid
  and heat that converts the samples metals into a
  uniform dissolved state.

5
DEFINITIONS (Continued)

• Blank
• Matrix that has negligible or unmeasurable
  amounts of the substance of interest.
• Instrument Blank
• Solvent or reagent blanks that measure
  interference or contamination from an analytical
  instrument.
• Solvent Blank
• Solvent used to dilute or extract the sample are
  analyzed to correct for impurities in the
  solvent.
• Reagent Blank
• Reagent used to prepare the samples are analyzed
  to correct reagent for impurities.

6
DEFINITIONS (Continued)

• Matrix Spike Blank
• Solvent or reagent blanks spike with analytes of
  interest.
• Trip Blank
• Test sample of analyte free media taken from the
  laboratory to the sampling site and returned to
  the laboratory unopened.
• Field Blank
• Ultra pure water that is carried to the sampling
  site and exposed to air to account for any
  airborne contamination.
• Equipment Blank
• Ultra pure water is rinsed through sampling
  equipment prior to sampling to account for any
  contamination.

7
DEFINITIONS (Continued)

• Duplicate
• Two samples taken at the same time from one
  location.
• Replicate Analysis
• Identical analysis are carried out on the same
  sample
• multiple times to measure analytical precision.
• Precision
• The degree of agreement among replicate analyses
  of a
• sample.
• Matrix
• The composition of the tested media. Typically
  water, solid,
• or gas.

8
DEFINITIONS (Continued)

• Gas Chromatography/Mass Spectrophotometry
• A prepared sample of wastewater is introduced
  into a column of special tubing which is
  precisely heated. The organic compounds are
  vaporized and carried to another column of tubing
  using an inert gas. A detector measures the
  electrical activity or mass spectra specific to
  each compound. The mass spectrophotometers
  computer contains a library of known mass
  spectra. The unknown compound is identified by
  comparing to known mass spectra.

9
DEFINITIONS (Continued)

• Pollutant
• Conventional Pollutant
• BOD, TSS, Fecal coliform, Oil and Grease, and pH
• Non-conventional Pollutant
• Any pollutant that is neither a toxic pollutant
  nor a conventional pollutant (Phosphorus)
• Toxic Pollutant
• Any pollutant listed as toxic under section 307
  (a)(1) of the Clean Water Act or in the case of
  sludge use disposal practices, any pollutant
  identified in regulations implementing sections
  405 (d) of the Clean Water Act.

10
ANALYSIS METHODS

• Water (NPDES)
• Sludge (NPDES)
• Hazardous Waste (RCRA)

11
ANALYSIS METHODS FOR WATER (NPDES)

• Guidelines for Establishing Test Procedures for
  the Analysis of Pollutants. 40 CFR Part 136.
• EPA Methods for Chemical Analysis of Water and
  Wastewater, EPA 600/4-79-020
• Standard Methods for the Examination of Water and
  Wastewater, 18th Edition
• American Society for Testing and Materials
• United States Geological Survey

12
ANALYSIS METHODS FOR WATER (NPDES)

• Physical Properties
• Total Suspended Solids
• EPA 160.2
• SM. 2540 D
• Temperature
• EPA 170.1
• SM. 2550 B

13
ANALYSIS METHODS FOR WATER (NPDES)

• Metals
• Atomic Absorption Direct Aspiration
• EPA 600/4-79-020
• SM. 3111 B or C
• Atomic Absorption Furnace
• EPA 600/4-79-020
• SM. 3113 B
• Inductively Coupled Plasma
• EPA 200.7
• SM. 3120 B

14
ANALYSIS METHODS FOR WATER (NPDES)

• Metals
• Atomic Absorption Cold Vapor
• EPA 245.1 and 245.2
• SM. 3112 B
• Colorimetric
• EPA 600/4-79-020
• SM. 3500

15
ANALYSIS METHODS FOR WATER (NPDES)

• Inorganic Nonmetallics
• Cyanide
• EPA 335.1, 335.2 and 335.3
• SM. 4500-CN C, 4500-CN D, 4500-CN E, and 4500-CN
  G
• pH
• EPA 150.1
• SM. 4500-H B

16
ANALYSIS METHODS FOR WATER (NPDES)

• Organic Aggregates
• Biochemical Oxygen Demand
• EPA 405.1
• SM. 5210 B
• Chemical Oxygen Demand
• EPA 410.1, 410.2, 410.3, and 410.4
• SM. 5220 C
• Oil and Grease
• EPA 413.1, 1664 (Hexane Extractable Material)
• SM. 5520 B
• Phenol
• EPA 420.1, and 420.2

17
ANALYSIS METHODS FOR WATER (NPDES)

• Individual Organic Compounds
• Volatile Organic Compounds
• EPA 624
• Base/Neutral and Acid Compounds
• EPA 625
• Various other compounds
• EPA 601, 602, 603, 604, 606, 609, 610, and 612
• Pesticides
• EPA 608, 625

18
ANALYSIS METHODS FOR SLUDGES (NPDES)

• Test Methods for Evaluating Solid Waste,
  Physical/Chemical Methods,
• EPA Publication SW-846
• Standard Methods for the Examination of Water and
  Wastewater, 18th Edition.

19
ANALYSIS METHODS FOR HAZARDOUS WASTE (RCRA)

• Toxic Characteristic Leachate Procedure (TCLP)
• TCLP Metals SW 1311/6010A
• TCLP Mercury SW 7470
• TCLP Volatile Organics SW1311/8260

20
QUALITY ASSURANCE/QUALITY CONTROL

• Quality Assurance
• A set of operating principals that, if followed
  during sample analysis, will produce data of
  known and defensible quality.
• Quality Control
• The internal day to day activities that control
  and assess the quality of the measurements.

21
QUALITY CONTROL

• Calibrations
• Duplicates
• Spikes
• Surrogate (similar analyte)
• Standard (same analyte)
• Standards
• Blanks
• Trip, Lab, Matrix, Solvent, Reagent, Instrument

22
QUALITY ASSURANCE

• Control Charts
• Audits
• System
• Performance
• Data

23
REVIEWING AND EVALUATING LAB REPORTS

• Checklist
• Were the samples received by the lab in good
  condition and within holding times?
• Were custody seals used? Was the seal intact upon
  arrival?
• Were samples preserved to the proper pH level?
• Was the sample temperature acceptable upon
  arrival?
• Was the name of the sampler listed on the report?
• Were the correct dates listed on the report?
• Were the correct times listed on the report?
• Were the correct methods used?
• Were any analysis problems recorded and reported?
• Was a QA/QC report submitted?
• Were blanks, standards and spikes within control
  limits?

24
RESOURCE LIST

• Local Pretreatment Contact
• Laboratory Customer Service Representative or Lab
  Manager
• Internet
• www.epa.gov
• Information Sources Link
• Test Methods Index
• www.epa.gov/OST (Office of Science and
  Technology)
• Catalog of Publications
• www.epa.gov/cincl (National Environmental
  Publications Information)
• waterpubs_at_epamail.epa.gov (Office of Water
  Resource Center)
• 202-260-7786
• www.ntis.gov (National Technical Information
  Service (NITS))
• www.wef.org
• Technical discussions