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Department of Environmental Quality

Quality Assurance for the Small Water Lab

SOUTHERN OREGON WATER AND WASTEWATER SHORT SCHOOL

8/16/2018

Scott Hoatson – Oregon DEQ [email protected]


Agenda – Not necessarily in this order

• Introduction• References• Appropriate Methods• Quality Assurance

• QA Expectations• Quality System• Documents and Records• Data Reporting

• Sampling and Storage

• QA / QC Requirements


Purpose of Monitoring

• The goal of the NPDES and SDWA programs is to preserve and protect water quality and human health.

• Facilities are required to self monitor and report to the State.

• Data must be scientifically valid and defensible and of known and acceptable precision and accuracy.


Where Do I Find Information ??

• Ecfr.gov

– 40 CFR Part 136.3 Identification of Test Procedures

– 40 CFR Part 136.7 Quality Assurance and Quality Control.

– 40 CFR Part 122.21 Application for a permit

• Handbook for the Analytical Quality Control In Water and Wastewater Laboratories (HB) – EPA-600/4-79-019, March 1979


More References

• NPDES Compliance Inspection Manual (CIM) - EPA 305-X-04-001, July 2004

• QA Guidance for Self-Monitoring Laboratories (NPDES and WPCF) DEQ09-LAB-0071-QAG 4/25/2013


QA References

• Field Sampling Reference Guide – DEQ86-LAB-0002-QAG 08/15/18

• DEQ– Quality Manual Template –


40 CFR 136.3

– https://www.ecfr.gov

Table I A – Approved Microbiology methods

Table I B – Approved Inorganic Methods

Table I C – Approved Organic Methods

Table I D - Approved Pesticide Methods

Table IE - Approved Radiologic Methods

READ THE FOOTNOTES!!!!!!


40 CFR 136.3 Part Dieux

• Table IF - Approved Methods for Pharmaceutical Pollutants

• Table IG - Approved Methods for Pesticide Active Ingredients

• Table IH - Approved Microbiological Methods for Ambient Water

• Table II - Required Containers, Preservation Techniques, and Holding Times


Compliance Testing

• Must use methods in 40 CFR 136.3• Standard Methods references

– New editions– You need to get:

• A new book or buy individual methods• Subscribe to Standard methods on-line


2017 Method Update Rule

• EPA re-evaluates methods approx. every 5 years. Goes for public comment before finalizing

• Signed - 8/7/2017 – Incorporated into 40 CFR part 136

• Updates Standard Methods – 22nd – 23rd

Editions• Fecal Coliforms by IDEXX Colilert 18• New MDL Procedure


APPROPRIATE METHODS


40 CFR part 136.3 Table 1 A


40 CFR part 136.3 Table 1 B


Very Outdated – Retire Them


21 Edition – 2005, 22 Edition 201223rd Edition - 2017


What about Hach Methods?


Nitrate Example

• Hach Method 10206 Approved– Hach TNT 835 (test kit) is NOT approved by

itself• The approved methods have associated

quality control requirements

• Test Kit “procedure” does not.


Hach Company TNTplusTM 830/831/832 Ammonia Method 10205

• “This method is equivalent to EPA 350.1, 351.1, and 351.2 for the purposes of regulatory reporting of Ammonia (as nitrogen) and Total Kjeldahl Nitrogen.”

• EPA said chemistry is equivalent (2007 EPA Memo)

• Hach method 10205 not in CFR. OK to cite 350.1 for Ammonia IF….


IF…

• You follow what is in 10205, not just what is in TNT 830/831.

• You should have a copy of EPA 350.1 (you can easily get from the internet. – Google or other another search engine


In Summary

• There is a Significant difference between the Hach Method and Test Kit instructions.

• Hach products are acceptable for use in many compliance tests provided The Method is followed.

• Also See QC requirements in 40 CFR 136.7


Quality Assurance

• QA refers to a total program for ensuring the reliability of data by utilizing administrative and technical procedures and policies regarding personnel, resources, and facilities. - CIM

• Quality Control (QC) are the activities related to ensuring a specific process meets requirements of project, program or data user.


Purpose of QA/QC

• ALL ABOUT TRACEABILITY:

– Ability to definitively demonstrate compliance

– Recreate the sampling and analytical activities

– Documentation should be able to stand on its own merit without explanation.

– Data of known and documented quality.

– Demonstration of laboratory competency


Quality Assurance Expectations (CIM)

• QA is required for all functions bearing on environmental measurements and includes activities such as:– project/study definition– sample collection and tracking– laboratory analysis– data validation analysis, reduction, and reporting – documentation– data storage systems.


40 CFR 136.7 Quality assurance and quality control

• The permittee/laboratory shall use suitable QA/QC procedures when conducting compliance analyses with any part 136 chemical method or an alternative method specified by the permitting authority.

• These QA/QC procedures are generally included in the analytical method or may be part of the methods compendium for approved Part 136 methods from a consensus organization.


40 CFR 136.7 continued

• The permittee/laboratory shall follow these QA/QC procedures, as described in the method or methods compendium. If the method lacks QA/QC procedures, the permittee/laboratory has the following options to comply with the QA/QC requirements:



• (a) Refer to and follow the QA/QC published in the “equivalent” EPA method for that parameter that has such QA/QC procedures;

• (b) Refer to the appropriate QA/QC section(s) of an approved part 136 method from a consensus organization compendium;



• (c)(1) Incorporate the following twelve quality control elements, where applicable, into the laboratory's documented standard operating procedure (SOP) for performing compliance analyses when using an approved part 136 method when the method lacks such QA/QC procedures. One or more of the twelve QC elements may not apply to a given method and may be omitted if a written rationale is provided indicating why the element(s) is/are inappropriate for a specific method


QA/QC in the CFR – 40 CFR 136.7

• Included in most methods

• Use QA/QC procedures in Compendium methods (e.g. Standard Methods, ASTM, etc)

• If not in above, incorporate 12 items


The Dirty Dozen (40 CFR 136.7)

1. Demonstration of Capability

2. Method Detection Limit

3. Method Blanks (MB)

4. Laboratory Control Sample (LCS)

5. Matrix Spike (MS) and MS Duplicate (MSD)

6. Internal Standards, surrogates, tracers


The Dirty Dozen (40 CFR 136.7) – cont.

7. Calibration and verification (Initial (ICV) and Continuing (CCV))

8. Control Charts (trend analysis)

9. Corrective action (root cause analysis)

10.QC Acceptance Criteria

11.Batch definitions (may drive QC frequency)

12.Frequency for conducting QC activities


Before You Start Running Samples


Method Validation

• Method Selection– Method appropriate to meet your needs– In our case methods found in 40 CFR 136.3

(NPDES) or 40 CFR 141 (SDWA)– www.ecfr.gov

• Develop Procedure (ATP)– 40 CFR 136.5

• Traceability of Measurements

• Show that it works (Validate)


Traceability Components

• Analyst• Date/time• Instrument• Standards• Reagents• Calibration• Analytical QC• Sample QC• Records Management


Method Validation

• Calibration– Titrations – Standardization of Titrant– Gravimetric – Balance Calibration– Microbiology

• Autoclave• Volumetric equipment• Water baths• Ovens• UV instruments

– Most other methods – Multipoint calibration


Method Validation

• Detection and Quantitation levels– MDL (method detection limit) – 40 CFR 136

Appendix B Revision 2– Reporting Limits (Quantitation Limits)

• Precision and Bias determination– Can also be used for Demonstration of capability

for the one analyst.• Demonstration of Capability

– Analyst specific


Reporting (QL) / Detection Limits (DL)

Detection Limit - What does it mean?• Within Calibration Range.

– QL – specified in permits – share with lab– LOQ – Limit of Quantitation– RL – Reporting Limit

• Estimated – Needs to be Qualified– LOD – Limit of Detection– MDL - Method Detection Limit


MDLs

40 CFR 136 Appendix B Revision 2

• New procedure in 2017 MUR. • Takes blank background levels

consideration


Data Qualifiers

• Data Qualifiers provide useful information to data users. Lab should not be hiding problems.

• Not always bad. e.g. Tight control limits may lead to more qualifiers

Pitfalls• Lab does not use qualifiers


Quality Assurance

• Quality Control Procedures– Calibration Verifications– Positive Controls (LCS, MS, SRM)– Negative Controls(Blanks, non-target bacteria,

etc.)

• Proficiency Testing

• Data Review


Quality Control (QC) Elements


Laboratory Quality Control (QC) Elements

• Positive Control – Show process performs correctly using a known test subject. – Lab Control Sample– Known coliforms

• Negative Controls – Shows that process doesn’t interfere with determination.– Blanks – Contamination– Non-coliform bacteria – False positives


Quality Control (QC) Elements

• BLANKS

• DUPLICATES

• STANDARD REFERENCE MATERIALS (good for validating method or DOC)

• BLANK SPIKES (Lab control samples)

• SPIKE SAMPLES

• SPLIT SAMPLES AND CERTIFICATION PROGRAMS (eg. DMRQA)


QC Elements - Negative Controls

• Blanks– Equipment Blanks– Instrument Blanks– Method Blanks (Includes sterile growth media)– Trip Blanks (Volatile Organics)

• Non-Target Bacteria– Media supports growth – Differentiate between types of bacteria.


QC Elements - Positive Controls

• Accuracy is determined by analyzing reference standards or spiked samples and is expressed as standard deviation form the theoretical value or average percent recovery.– Laboratory Control Samples– Matrix Spikes– SRM (Standard Reference Material)– Acceptance limits are in referenced method or

calculated from Control Charts.


QC Elements – Positive Controls

• Precision: Measure of the degree of agreement among replicate analyses of a sample.

• Determined by running duplicates and is expressed as standard deviation, range, or relative percent difference (RPD).– Lab Duplicates (batch), Split Samples

(Periodic), Duplicate Spikes (if duplicates not performed)


QA/QC Compliance inspection

• PRECISION, ACCURACY, CONTROL– Multiple replicates:

• blanks,• duplicates, • spikes, • and splits?

– Plotted precision and accuracy control charts?


Quality Manual

• Should support the laboratory data with an adequate documentation program that provides valid records of the control measures applied to all factors bearing on the final results of investigations.

• Because of the importance of laboratory analyses in determining practical courses of action that may be followed, quality assurance programs to insure the reliability of the water and wastewater data are essential.


Quality Manual (CIM)

• The 40 Code of Federal Regulations (CFR) Section 122.41(e) (conditions applicable to all permits), requires adequate laboratory and process controls, including appropriate QA procedures.

• Each permittee's laboratory must have a QA/QC program.


Quality Manual Cont (CIM)

• The laboratory must document the QA program in a written QA/QC manual and the lab should make it available to all personnel responsible for sample analyses.

• The manual must clearly identify the individuals involved in the QA program and document their responsibilities.


Quality Assurance Manual

• Simply Put: Documentation of the laboratories quality assurance program activities.

• It should be a living document and not just written and put on a shelf

• Review annually to make sure it reflects laboratory practices – only update if needed.


It doesn’t have to be huge

But you want it to have value


Quality Manual Templates

• DEQ Website: www.oregon.gov/deq/FilterDocs/QAManualTemplate.docx (borrowed by permission from VA)

• DEQ Lab: http://www.oregon.gov/deq/FilterDocs/DEQ91LAB0006QMP.pdf

• TNI – Compliant to 2009 TNI Standard available in MS Word http://www.nelac-institute.org/content/NELAP/howto.php

• Via Google: Search: “Environmental Laboratory Quality Manual Template”)


Quality Manual

• Describes the overall quality program• Documents the Laboratory’s quality policies

and procedures• Provides a tool for ensuring personnel are

both knowledgeable of and committed to these policies and procedures

• Demonstrates management commitment


Bottom Line

• Generate data of “Known and Documented Quality”


3 Fundamental Concepts

• Traceability• Process Improvement• Preventative Action


QM Table of Contents

• Introduction – Scope/Policy• Organization and Management

– Who can sign reports, QA documents• Position Descriptions / Roles• Document Control and Record Management• Subcontracting of Environmental Tests• Purchasing


QM Table of Contents – Part 2

• Control of Non-Conforming Work• Improvement• Corrective Action• Preventive Action• Control of Records• Audits• Management Reviews• Data Integrity• Personnel


QM Table of Contents Part 3

• Accommodations and Environmental Conditions (aka Facilities)

• Environmental Methods and Method validation

• Calibrations• Measurement Traceability• Sample Collection• Sample Handling• Quality Assurance• Reporting Results


Control of Documents

• Describes the overall review, approval and control process– Can be electronic– May refer to a separate SOP.– Only current versions in use and accessible to all

• Standard Operating Procedures (SOPs)– All procedures documented

• Quality Manual– Documentation of the quality system


Documented Procedures

• Sampling • Equipment calibration and maintenance• Analytical methods• QA/QC activities (40 CFR 136.7)• Data handling and reporting

• May be in electronic format (e.g. pdf)


Sampling Procedures

• Collection and analysis schedule for permitted parameters (and non-permitted)

• Collection Locations

• Sample Types (Grab, composite, sampler instructions) 40 CFR part 122.21

• Field Filtration – Dissolved metals


Sample Handling Procedures

• Proper preservation, containers, holding times, AND proper sample location,

• Security

• Chain-of-Custody• Proper storage

• Documentation


Facilities and Equipment Procedures

• Operating instructions for equipment such as balances, meters, incubators, and samplers.

• Adequate equipment (type and specifications)

• Maintenance schedules on major equipment • Cleaning (glassware, micro apparatus, etc)• Daily balance checks and annual service• Ovens • Daily water checks


Facilities and Equipment Procedures

• Pure Water? – Daily Conductivity Checks• Adequate equipment? • Equipment maintenance and calibration?

(Maintain log and schedule)• Clean area?• Adequate Standards and Reagents within

shelf-life? – Maintain Log• Documentation?


Laboratory Procedures

• EPA Approved procedures (40 CFR Part 136) Specified in Permit? – Written SOPs – Necessary unless following

method to the letter.– Calibration and maintenance– QA/QC Procedures used and adequate– Data Review/Approval

• Contract Laboratory Information• Documentation?


Proficiency Testing

• Blind Check Samples to assess routine performance.– Run like your regular samples– Do not run at same time as Check PT samples

• Major Facilities – Require DMRQA Studies

• Recommended for others.– Water Pollution


Proficiency Testing

• Corrective action required for failures– Why did it fail

– What did you do to correct the problem• Does it prevent recurrence?

– Was any other data affected?

– Must demonstrate you are on control


Data Handling

• Data sheets (or log books) must be dated, initialed by analyst, legible, and written in ink – Drawing a single line through the incorrect

recording should make any corrections, insertion of corrected result, initialed and dated, and contain a comment (NO CORRECTION FLUID OR TAPE)


Data Handling and Reporting

– ROUNDING to nearest EVEN number?• EXAMPLES: 4.45 = 4.4 and 4.35 = 4.4

– Significant Figures for each analysis (either 2 or 3)?

– Cross-checking calculations?– Correct formulas – Have spreadsheets been

verified and locked?– Proper Control Chart Use– 3 Years of Records


Data Handling

• Data sheets should include calibration measurements, incubator temperature records, and the time samples were placed in and removed from incubators, ovens, etc.

• Data sheets should include equations used for deriving final test results.

• Second Level Review – Another pair of eyes.• Qualify for QC failures, HT, preservation

etc*.


Control of Records

Record Management

• General Definition: The practice of maintaining records of an organization from the time they are created up to their eventual disposal.


What are Records?

• Raw Data files• Support equipment records• Standard Traceability log records• Calibration records• Other log books• Electronic files (instrument files)• Emails• Quality records: internal audits, management reviews,

corrective actions and preventative actions.• Etc.

• Technically “Records” include all of the above plus “Documents”


Record Management

• Records management and storage– Identification– Collection– Archives– Filing– Access– Disposal


Records ManagementTNI 2009 V1M2 4.13.3: Control of Records

• The laboratory shall retain all records for a minimum of five (5) years from generation of the last entry in the records. (Drinking Water – 10 years)

• Records that are stored only on electronic media shall be supported by the hardware and software necessary for their retrieval.

• The laboratory shall establish a record keeping system that allows the history of the sample and associated data to be readily understood through the documentation.

40 CFR 122.41 and 40 CFR 503 – 5 year retention


Records Management System

• This system shall produce unequivocal, accurate records that document all laboratory activities such as:– laboratory facilities, equipment– analytical methods and data – related laboratory activities, such as

• sample receipt, • sample preparation• data verification• inter-laboratory transfers of samples and/or

extracts.


Do you have all of the Records?


Fundamental Question

• Based on the documented information, can you say with confidence that the permitted facility is in compliance or not?


Subcontracting Work

• When do you use subcontract labs?

• How do you communicate your requirements to the subcontractor?

• Give them copy of permit!!

• Be sure they are clear on QLs and method requirements (don’t report SW 846 methods)


DO NOT USE the Yellow Pages Approach

• The Customer is ultimately responsible for the site / discharge / project.

• Not the Lab!!


Third Party Labs (Sub Contracting)

• Request report with QC (with qualifiers)

• Recommend using accredited labs– Receive Audits every two years– Analyze 2 PT samples per year– Meet a known standard of documentation

• If not accredited– Recommend visiting the lab yourself– Recommend asking for a “Raw Data Package” at

least once.


Communication Pitfalls

• Not giving requirements to the lab until after the project is over or not at all.– Lab may or may not have met your

requirements (wrong method, QL)– Have to backpedal to try and salvage data– OR resample and retest.


Ethics and Data Integrity

• What are your data integrity policies?

• Do you perform data integrity training?

• How would you handle a reported violation?

• Notification of clients/regulators if data is adversely impacted?


Self Evaluation Practices

• Audits/Assessments

• Corrective Actions

• Preventive Action

• Management Review


Audits/Assessments

• Internal - Self Monitoring• External - Outside Monitoring (DEQ,

ORELAP, etc)• Performance Audits – Check samples (PT

samples)


Findings

• Purpose – To get better and NOT to point blame

• What do you do with audit results?

• Document evaluation of cause and correction

• Can incorporate into Corrective Action process.


Corrective Actions

• Documented process

• How do you handle and document identified corrective actions– Paper– Spreadsheet– Data base


Corrective Action Process

• Identify Corrective Action

• Investigate for Cause

• Identify Corrective Action– Correction vs Corrective Action

• Implement Corrective Action

• Verify Effectiveness


Technical Corrective Actions

• QC failures– Reanalysis– Data Qualification

• Non-symptomatic random failures require no further action

• Review of failures over time may indicate need for Corrective actions


Reporting Results

• QC failures must be noted – Data user needs to know potential limitations of

the data• Qualifiers are preferred (Required for NELAP)• Narration is acceptable

• Subcontract labs must be identified

• Report Amendments– Identify as “revised” or “supplement” or “…”and

reason for change– Indicate what it is replacing or supplementing.


Need Help ?

• OELA – www.oelaonline.com– 2017 presentations available

• Linkedin.com – Discussion groups– “Water and Wastewater Laboratory

Professionals”– “Water and Wastewater Professionals”

• Call fellow plant operator

• DEQ – Permit Compliance Inspector


DEQ Website

DEQ Home Page: http://www.oregon.gov/DEQ

DEQ QA Guidance for Self Monitoring Laboratories (NPDES, WPCF)http://www.oregon.gov/deq/FilterDocs/QAguidanceSML.pdf


If Time Permits


Sampling and Sample Handling/Storage


– Sampling Technique can contribute up to 75% uncertainty to the final result.

– Incorrect Sampling can cause headaches for the lab. It can even cause sample analysis to be cancelled!

– Sampling is often overlooked in procedures, training, and defining roles and responsibilities.

• Document, Document, Document!– If done correctly, you can use sampling to add

statistical defensibility and to increase the value of your data!

• Sampling Procedures

Why is Sampling Important?


•From the Sample Collector’s Perspective•Writing and Understanding the Sampling Procedures

•Scheduling with Laboratory Needs in Mind!•Using the correct Supplies and Equipment•Having the right Preservatives•Preparing for the unknown (extra supplies, extra time, etc.)

•Using Established and Communicated Procedures

•Training and Technique

•Knowing your sample locations – should be in the permit

Sampling Procedures


• Effluent sampling should be representative of final discharge after all processing (e.g. after chlorination)

• Composites can be used for most tests EXCEPT (these need to be Grab) (40 CFR 122.21)

• Microbiological samples• pH, Temperature• DO, Cl2• Oil and Grease• Cr6+, Sulfite• Phenolics• VOCs

• Special handling if compositing (not automatic sampler) for VOC, phenolics, sulfide.

Grab Vs Composites


• Need to keep cold during compositing period

• Frequency usually flow based unless constant flow then it may be time based. (should be specified in permit)

• May be conducted manually or automatically

• The sample holding time starts at the end of the composite cycle.

24 Hour Composites


Loss of Analyte

• How we sample, preserve and store the sample can result in loss of analyte.– Volatile Organics

• Compositing• Acid Preservation (e.g. 2 CVE, Acrolein )

– Aromatic Compounds• Microbiological activity

– Semi-Volatile Organics• Breakdown from heat or sunlight

– Cr+6, NO2• Reduction or Oxidation


– Physicals• Solids, pH, Conductivity, Alkalinity, Turbidity, BOD• 1000 mL Poly (Temperature Preserved)

– Temperature Preservation is < 6o C unless “SAME DAY”» Same day still needs to show an attempt at cooling. The laboratory will

document whether it is “on ice”» Blue Ice is no longer recommended as an effective shipping coolant. » Bagging the Ice will keep any cooler leaks from causing problems

– More volume might be required if doing several of the above analyses.

• Physicals Concerns– Homogeneity

» What is an indicator of a non-homogenous sample?» Visual» Analytical (Method Duplicates, Field Duplicates)

– Shorter Holding Times

Sampling Supplies, Preservatives, and Volumes


– Nutrients• Total Phosphorous, Total Kjeldahl Nitrogen, Ammonia,

Nitrate/Nitrite– Typically Preserved with H2SO4 and Temperature < 6o C– Unpreserved = short holding time (48 hours)– 500 mL

• Orthophosphate, Anions (Sulfide, Chloride, Bromate, Nitrite)– Filtered in the field (0.45 µm filter)– Filtration Apparatus might be checked with a Field/Equipment

Blank



– Metals• Metals must be collected in 250 or 500 mL Poly bottles• Waters preserved with Nitric Acid (HNO3) to pH < 2 (no

thermal preservation is required!) (except Hg)– Total Recoverable Metals– Dissolved Metals

• Must be filtered in the field



• E. Coli, Total Coliform, Fecal, Enterococcus• Grab samples are collected in sterile polyethylene or borosilicate

glass bottles at discharge after disinfection. – Note: If at all possible, use the sample bottle directly to take the sample. Do not

use a scoop or other transfer device as they are susceptible to contamination. – Short holding-time (Results must be qualified if not met)– Thermal Preservation required (< 10oC)– Treated Water? Dechlorination by Sodium Thiosulfate (Na2S2O3)

• Note: Sodium sulfite (Na2SO3) that is used for dechlorination for the BOD5 method is toxic to gram-negative microbes such as coliform and therefore MUST NOT be used for dechlorination of coliform samples

• Approved Method???• Manufacturer’s CLAIM some equipment/methods are approved by EPA but

you still must check! – It might be approved only if you do an ATP study



Total Residual Chlorine

• Grab samples are to collected at discharge from chlorine contact chamber. Samples must be analyzed immediately.

• Approved Methods– Standard Methods (see CFR for year of issuance)– Iodometric Method I (SM 4500-Cl B) or II (SM 4500-CL C) – Amperometric Titration (SM 4500-CL D) – Amperometric Low level Titration (SM 4500-CL E) – DPD Ferrous Titration (SM4500-CL-F) – DPD Colorimetric (SM4500-CL-G) – **Historically, EPA and DEQ have approved DPD kits in

special cases.


– Semi-Volatiles• Amber Glass containers (light sensitive)

• Temperature Preserved (< 6o C)

• Volume is an important consideration– Does the lab need to run Matrix Quality Control on your

project? Would you like them to?– Usually one set of 3 Amber jars for a site per event



• Volatile Organic Compounds (VOCs)– These are collected in 40 mL vials (pre-preserved with HCl) in

sets of 3. – Transport Blanks are required! – Cannot be analyzed if there is ANY headspace in the container.



– Technique– Contamination – Preservative Quality and Expiration– Field Instrument Calibration– Cleaning between Sites

• Keeping your Sampling Gear Uncontaminated– GPS– Camera– Gloves– Safety Equipment

• Vehicle AND Chemical Safety

Other Sampling Considerations


Contamination

• As we drive detection levels down and seek out more analytes, the potential for influence from contamination increases.

• Examples– Mercury– Ethanol– DEET– PAHs


Contamination

• Possible sources– Sampling materials and equipment

• Bailers, autosamplers, etc. • Gloves

– Sample bottles• Certified clean (but not for ultra trace levels)• Some plastics have PAH contamination

– Reagents (Preservatives)• Buffers can affect other analytes

– Clothes, lotions, etc.


Quality Control

• Types of Quality Control– Laboratory

• This is performed with every analysis as part of the method.– Field

• This pertains to the specific project and can add defensibility to your data.

• Will your project benefit from additional QC?– Split Samples

• Independent Verification of Accuracy.• You could do the same analysis over and over again with

passing QC but still be inaccurate


• Field Duplicates– Must be collected within 5 minutes of each

other from the SAME sampling location –define in your QAM

– Common acceptance criteria is 20% RPD or a difference of < LOQ. This can vary by method and matrix. (i.e. Organic solid matrix may be as high as 50% RPD)

• LOQ (Limit of Quantitation) = MRL (Minimum Reporting Limit)

Types of Field Quality Control


Needed to ensure positive hits are real• Permit Compliance• Effluent Characterization

• Types– Equipment – Dissolved parameters, – Transfer - Identify possible contamination from field

environment– Transport (Trip) - Volatiles– Common Acceptance Criteria is <LOQ, < ½ LOQ, 1/10

action level (Depending on data use).

Field Quality Control - Blanks


• Split Samples are taken as one sample and then “split” to send one to the regular laboratory (or analyzed in your own) and one to a different laboratory. – Which parameters would you like to take split samples for?– Do you have procedures for splitting the sample to ensure

homogeneity?• Compare the two results

– Things to consider:• Both labs using same method?• Both labs have similar Reporting Limits?

Split Sampling


• What does “custody” mean?– A sample is considered “in custody” if:

• In someone’s physical possession or view OR• Locked up or kept in a secured location only available to authorized personnel• All changes in sample possession must be fully and completely documented, with the

date, time, and persons relinquishing and receiving the samples on the appropriate chain-on-custody record.

• Chain of Custody is “cradle to grave”– There must be a record of each person who was responsible for the

sample at every part of the sampling and analysis process.

Custody Procedures


Sample Receipt

• Preservation check• Holding time check• Compare to COC• Log-in – LIMs, Log book, etc• Unique sample number

• Sample Acceptance Policy?


Sample Handling and Storage

• Procedure for sub-sampling if done by lab• Storage

– Refrigeration– Temperature monitoring– How long

• Sample Shipping• Sample Disposal


Specific Methods

• BOD SM 5210• TSS SM 2540D• pH EPA 150.1 , SM 4500-H+ B• E. Coli Coliert, Colilert -18 (SM 9223B)• 40 CFR 136.7• SM 1020 – QA/QC - general• SM 2020 – QA/QC – 2000 Series• SM 4020 – QA/QC – Refers back to 1020• SM 9020 – QA/QC – 9000 Series


BOD - SM 5210B

• Storage and Pretreatment– Holding Time– Residual chlorine test– Initial pH

• Adjustment– Initial DO

• Supersaturation?– Temperature

• During composite collection• Storage


BOD – Equipment

• Reagents and Glassware• Incubator• DO Meter

– Membrane Probe– Luminescence Probe


BOD – Sample Seeding

• What is the Seed?– Added to samples that don’t have sufficient

biochemical activity to depletion criteria• Who needs to use Seed?

– Chlorinated– pH Adjusted– Non biological Wastewater– Any with insufficient microbial activity

• Seed Correction Factors


BOD - QC

• Unseeded Blank (dilution water) – Depletion < 0.2 mg/L

• Glucose Glutamic Acid (GGA)– Acts as LCS– Every 20 samples or weekly (minimum)– 198 +/- 30.5 mg/L (approx 15%)


More BOD - QC

• Minimum residual DO – 1.0 mg/L

• Minimum DO depletion– 2.0 mg/L

• Example:– Initial DO: 8.2 mg/L– Final DO: 7.1– Depletion <2.0 mg/L

• Use a different dilution that meets criteria


BOD – Other Things to Remember

• Sample bottles must be water-sealed before incubation

• Dilution water should be distilled or deionized

• At least 2 dilutions for each sample• Temperature monitor the incubator during

incubation period

• If criteria not met – Qualify, Qualify, Qualify


E. Coli SM 9223B

• Collection– Homogenize before “pouring off”

• Holding Time to set-up– < 8 hours from sample collection

• Bottles Lot Tested? Documented?– Fluorescence– Positive and Negative Controls

• Media Lot Tested? Documented?– Expiration, Traceability– Positive and Negative Controls


E. Coli SM 9223B

• Equipment– Incubator checks– Thermometer calibration

• Records– Times Documented (In and Out)

• Quantification– Test Sealer with dye


E. Coli SM 9223B

• Look for fluorescence with a 6-watt, 365-nm UV light within 5 inches of the sample in a dark environment.– UV bulbs fade over time– SM 9020 (3) Lab Equipment and Instrument.

• Clean with cloth/ethanol - monthly• UV light meter – test quarterly > 70% intensity• Test sterilization


E. Coli SM 9223B

• Comparators– These expire just like media

• Yellow colonies that do not fluoresce are positive for Total coliform.

• Duplicate Count? Duplicate Analyst?


Total Suspended Solids (TSS) – SM 2540D

• Sample Storage and Pretreatment– Storage Temperature < 6oC– Holding Time – 7 days

Samples MUST be shaken or stirred prior to pouring for analysis.


TSS - Equipment

• Glass fiber filters – Grades listed in method• Analytical Balance – weigh to 0.1 mg (4

place)• Desiccator that has good desiccant (use

color indicator dessicant)• Drying Oven – maintain 103o-105oC

– Record temp when placing into and removing from oven


TSS - QC

• Reagent Blank – each batch• Duplicate – per batch or 10% frequency• Laboratory Control Sample

– Old DMRQA or other PTs– Purchase– Diatomaceous earth

• SM 1020 – QA/QC - general• SM 2020 – QA/QC


TSS – General topics

• Pre-wash filters* or purchase pre-washed and weighed

• Dried and re-weighed to constant weight– If not, lab can establish drying time (and

document how it was determined)– Sample filters must be dried for at least an hour.

• Residue should be 1-200mg. – use more or less sample volume to achieve


pH – SM 4500 H+ B, EPA 150.1

• Sample Storage and Pretreatment– Samples collected in plastic or glass containers

– Analysis within 15 minutes of collection!


pH Equipment

• pH meter calibrated or verified each day• Probe stored in proper solution• Measurement to include temperature

correction?• pH meter accurate to at least 0.1 pH unit• Non-sealed electrodes refilled prior to use.


pH QC and General items

• Uncover filling hole before use• Calibrate per manufacture

– Using 4,7, and 10 buffers– Record the calibration slope

• Stir/swirl sample while taking reading• Replicates 10% frequency and readings with

0.2 pH units.• Record date and time of analysis

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