PCRP Appendices FINAL 29062010 - WA Health/media/Files/Corporate... · 2016. 6. 28. · CAS No Parameter Units LOR 3-Jun-05 3-Jun-05 10-Jun-05 10-Jun-05 9-Jun-05 20-Jun-05 DBP NO

Appendices

i

Contents

Contents ........................................................................................................................ i

Appendix 1: ...................................................................................................................1

Preliminary Sampling Event Results ..................................................................................................1

Appendix 2 ..................................................................................................................12

List of chemicals not analysed and in the original PCRP list...............................................................12

Appendix 3- Sampling and Analysis Plan/Work Instruction and Reporting..........................14

Sampling and Analysis Plan ............................................................................................................14 Work Instruction and Reporting .....................................................................................................31

Appendix 4 ..................................................................................................................95

Chemical Methods - See separate Appendix 4 documents. ..............................................................95

Appendix 5 ..................................................................................................................96

Health Recommendations..............................................................................................................96

Appendix 6 ................................................................................................................114

Environmental Guideline Recommendations.................................................................................114

Appendix 7 ................................................................................................................123

Publications ................................................................................................................................123

Appendices

1

Appendix 1:

Preliminary Sampling Event Results

Organic Chemicals

Woodman

Point WWTP Beenyup WWTP

Woodman Point

WWTP Beenyup WWTP KWRP KWRP

CAS No Parameter Units LOR 3-Jun-05 3-Jun-05 10-Jun-05 10-Jun-05 9-Jun-05 20-Jun-05

VOCs

71-43-2 Benzene ug/L 2

Appendices

2

542-75-6 1,3-Dichloropropene ug/L 2

Appendices

3

631-64-1 Dibromoacetic acid (DBA)

71133-14-7 Dichlorobromoacetic acid (DCBA) ug/L 0.1

Appendices

4

Chelating agents

60-00-4 EDTA ug/L 0.5 210 210 210 210 0.7 0.7

139-13-9 NTA ug/L 0.6 7.7 2 12 1.4

Appendices

5

2276-90-6 iotalamic acid ng/L 100

Appendices

6

Other

947-92-2 n-nitroso-dicyclohexylamine ng/L 1

Pesticides

Woodman

Point WWTP

Beenyup

WWTP

Woodman

Point WWTP

Beenyup

WWTP KWRP KWRP

CAS No Parameter Units LOR 3-Jun-05 3-Jun-05 10-Jun-05 10-Jun-05 9-Jun-05 20-Jun-05

309-00-2 Aldrin ug/L 0.01

Revision Number: 0 - DRAFT - Page Number: 8

10605-21-7 Carbendazim ug/L 0.2


51-03-6 Piperonyl butoxide ug/L 0.1


1/03/7440 Niobium ug/L 0.1


Appendix 2

List of chemicals not analysed and in the original PCRP list

CAS Parameter Reason for exclusion

Pesticides

6923-22-4 Monocrotophos No method available

17804-35-2 Benomyl No method available

4726-14-1 Nitralin Obsolete as pesticide

21725-46-2 Cyanazine No method available

1982-47-4 Chloroxuron Obsolete as pesticide

122-39-4 Diphenylamine No method available

75-99-0 Dalapon No method available

1689-84-5 Bromoxynil No method available

43222-48-6 Difenzoquat methyl sulfate No method available

85-00-7 Diquat No method available

1910-42-5 Paraquat No method available

23135-22-0 Oxymal No method available

28249-77-6 Thiobencarb No method available

1071-83-6 Glyphosate No method available

3337-71-1 Asulam No method available

2593-15-9 Etridiazole No method available

25954-13-6 Fosamine ammonium salt No method available

25954-13-6 Fosamine ammonium salt No method available

77-47-4 Hexachlorocyclopentadiene No method available

67747-09-5 Prochloraz No method available

6190-65-4 Atrazine-desethyl No method available

35367-38-5 Diflubenzuron No method available

1861-32-1 Dacthal No method available

887-54-7 DCPA mono-acid degradate Analysis only if Dacthal above LOR

2136-79-0 DCPA di-acid degradate Analysis only if Dacthal above LOR

55512-33-9 Pyridate No method available

1646-87-3 Aldicarb sulfoxide Analysis only if Aldicarb above LOR

1646-88-4 Aldicarb sulfone Analysis only if Aldicarb above LOR

33089-61-1 Amitraz No method available

105827-78-9 Imidacloprid No method available

86479-06-3 Hexaflumuron No method available

64628-44-0 Triflumuron No method available

95737-68-1 Pyriproxifen No method available

101-21-3 Chlorpropham No method available

137-42-8 Metam sodium No method available

319-85-7 beta-BHC

VOCs

526-73-8 1,2,3-trimethylbenzene

593-60-2 Bromoethene

67-72-1 Hexachloroethane

DBPS

506-68-3 Cyanogen bromide

75519-19-6 Tribromoacetonitrile (TBAN)

17157-48-1 Bromoacetaldehyde

107-20-0 Chloroacetaldehyde

79-02-7 Dichloroacetaldehyde


Pharmaceuticals and PCP

3380-34-5 Triclosan (bactericide)

101-20-2 Trichlocarban (trichlocarban)

134-62-3 N.N-diethyl-m-toluamide (DEET)

Brominated Flame Retardants

79-94-7 Tetrabromobisphenol-A (TBBPA)

NO CAS Polybrominated Biphenyl (PBB)

NO CAS Polybrominated Diphenyl Ether (PBDE)

25637-99-4 HexabromocycLORodecane (HBCD) textilex

Phenols

90-43-7 2 phenylphenol (biphenyl-2-ol)

88-75-5 2-nitrophenol

100-02-7 4-nitrophenol (p-nitrophenol)

51-28-5 2,4-dinitrophenol

131-89-5 4,6- Dinitro-o-cyclohexyl phenol

Alkyl phenols (APs)

104-40-5 4 n-nonylphenol

1806-26-4 4 n-octylphenol

14938-35-3 4 n-Pentylphenol

98-54-4 4 tert-butylphenol

Alkyl phenol polyethoxylates (APEOs)

104-35-8 4-Nonylphenol monoethoxylate (NP1EO)

20427-84-3 4-Nonylphenol diethoxylate (NP2EO)

2315-67-5 Octylphenol monoethoxylate (OP1EO)

2315-61-9 Octylphenol diethoxylate (OP2EO)

80-05-7 Bisphenol A (4,4'-Dihydroxy-2,2-diphenylpropane)

119-61-9 Benzophenone

Organotins

56-35-9 Tributyl tin oxide (TBTO)

78736-54-9 monobutyl tin (MBT)

1002-53-5 dibutyl tin (DBT)

688-73-3 tributyl tin (TBT)

1461-25-2 tetrabutyltin

1124-19-2 monophenyl tin (MPT)

1135-99-5 diphenyl tin (DPT)

5424-25-9 triphenyl tin

5424-25-9 tetraphenyl tin

870-08-6 Dioctyltin oxide

Other

79-06-1 Acrylamide

92-87-5 Benzidine

91-94-1 3,3'-dichlorobenzidine

121-14-2 2,4-dinitrotoluene

606-20-2 2,6-dinitrotoluene

122-66-7 1,2-diphenylhydrazine

110-75-8 2-chloroethyl vinyl ether

108-60-1 Bis (2-chloroisopropyl) ether

111-44-4 Bis(2-chloroethyl) ether

78-59-1 Isophorone

98-95-3 Nitrobenzene


Appendix 3- Sampling and Analysis Plan/Work

Instruction and Reporting

Sampling and Analysis Plan

Premier’s Collaborative Research Project (PCRP)

– Characterising treated wastewater for drinking

purposes following reverse osmosis treatment

Prepared for PCRP project partners

Department of Health

Department of Water

Department of Environment and Conservation

Water Corporation

CSIRO Land and Water

Curtin University

Chemistry Centre WA

National Measurement Institute

University of Western Australia

July 2007


PURPOSE OF THE DOCUMENT

This document records the PCRP’s sampling and analysis technical planning process as a

Sampling and Analysis Plan (SAP). The SAP provides a high level overview of sampling and

analysis, for endorsement by the PCRP Steering Committee. The Work Instruction and

Reporting (WIR) document sits under the SAP, providing more detailed and updated

information.

The SAP provides, in one place, a clear and complete plan and its quality objectives, and

identifies the key personnel and their roles.

It is also a form of metadata, in that it provides qualifying information about how data was

intended to be collected.

A SAP outlines the following elements: See section(s):

• what the project’s goals/objectives/questions or issues are; 1.1

• who will use the data collected; 1.1

• what information will be obtained from the data collected; 0

• what decision(s) will be made from the information obtained; 1.1

• how the project will be administered and funded 1.2

• how, when, and where project data will be acquired or generated; 0, 0, 0

• what type, quantity, and quality of data are specified; 0, 0, 0

• what possible problems may arise and what actions can be taken to mitigate

their impact on the project; 0

• how, where and by whom the data will be managed; 0

• how, when and by whom the data will be analysed, assessed, and reported; 0

• how, when and by whom the success of the project will be evaluated. 0

ACKNOWLEDGMENTS

The major elements of this SAP are derived from “Guidance for Quality Assurance Project

Plans (EPA QAG-5)”, provided by the United States Environmental Protection Authority

(USEPA).

This document attempts to follow the NWQMS Volume 7 Australian Guidelines for Water

Quality Monitoring and Reporting (2000).

PCRP Sampling and Analysis Plan

Page Number: 17 Version Number: 2

REVISION STATUS

Ver Date Authors Description of Version

1 June 2006 Melissa Bromly, Palenque Blair,

Clemencia Rodriguez, Tom Rose

Starting draft.

2 July 2007 Melissa Bromly, Sharon McNeil Major revision following Sampling Events 1&2. SAP has been

revised to form a high level document, for Steering Committee

endorsement. The Work Instruction and Reporting (WIR)

document will sit under the SAP with more detailed and

updated information.

DISTRIBUTION LIST

Ver Date Sent out to Purpose

1 June 2006 PCRP HRA group For comment

2 25 July 2007 PCRP Technical Group For comment



Table Of Contents

PURPOSE OF THE DOCUMENT 2

ACKNOWLEDGMENTS 2

REVISION STATUS 3

DISTRIBUTION LIST 3

TABLE OF CONTENTS 4

1. PROJECT MANAGEMENT ..................................................................................................... 19

1.1 Purpose and Background ............................................................................................................... 19

1.2 Project Organisation ...................................................................................................................... 19

2. PROJECT PLAN ..................................................................................................................... 20

2.1 Analytes of Interest........................................................................................................................ 20

2.2 Data Collection Sites ...................................................................................................................... 21

2.3 Additional Related Work................................................................................................................ 22

2.4 Sampling Regime............................................................................................................................ 22

2.5 Equipment and infrastructure........................................................................................................ 22

2.6 Training .......................................................................................................................................... 22

2.7 Occupational Safety and Health Issues .......................................................................................... 23

3. DATA COLLECTION............................................................................................................... 23

3.1 Sample Collection........................................................................................................................... 23

3.2 Results ............................................................................................................................................ 24

3.3 Quality Assurance Program............................................................................................................ 24

3.4 Contingencies................................................................................................................................. 25

4. MEASUREMENT AND ANALYSIS SPECIFICATIONS ............................................................... 26

4.1 Sample Analyses............................................................................................................................. 26

5. DATA MANAGEMENT .......................................................................................................... 28

5.1 Data organisation and layout......................................................................................................... 28

5.2 Data storage system....................................................................................................................... 28

5.3 Data management protocols ......................................................................................................... 28

6. APPENDIX A - REFERENCES.................................................................................................. 29

7. APPENDIX B– PCRP PROJECT PLAN...................................................................................... 30



PROJECT MANAGEMENT

1.1 Purpose and Background

This document describes a sampling and analysis plan to meet the PCRP objectives:

• Analyse the final treated wastewaters from 3 Water Corporation’s large Metropolitan

wastewater treatment plants (WWTPs) to characterise their microbial and chemical

constituents and understand any seasonal and catchment differences in trace

contaminants of concern in relation to human and environmental health;

• Analyse the permeate characteristics to assess the performance of the existing

micro-filtration/reverse osmosis (MF/RO) treatment process at the Kwinana Water

Reclamation Plant (KWRP) to consistently produce water of the required standard

from treated wastewater from the Woodman Point WWTP; and

• Analyse the permeate characteristics to assess the effectiveness of MF/RO treatment

to remove target contaminants present in treated wastewater from the

Corporation’s other Metropolitan WWTPs (Beenyup and potentially Subiaco);

The parameters to be monitored and analysed over three years are:

1. A comprehensive suite of known and potential trace chemical contaminants in

Perth’s (secondary) treated wastewaters, including endocrine disrupting substances,

disinfection by-products, other chemicals of concern (COCs) e.g. in pharmaceuticals

and personal care products; and micro-organisms and nutrients/salts;

2. Operating processes to evaluate the reliability and operational performance of the

MF/RO treatment plant at Kwinana to consistently treat wastewater to a high

quality; and

3. Microbial and chemical constituents (as in 1 above) in the permeate of MF/RO

treatment of Beenyup and potentially Subiaco secondary effluents.

The three year PCRP Project commenced in October 2005, and is due for completion in

November 2008. See PCRP Project Plan (Appendix B) for details.

1.2 Project Organisation

The partners undertaking this project are Department of Health, Department of Water,

Department of Environment and Conservation, Water Corporation, Chemistry Centre, Curtin

University, National Measurement Institute, CSIRO Water for a Healthy Country and

University of Western Australia.

Project schedule

The project schedule at July 2007 is shown below. Further changes to the schedule will be

recorded in the Work Instruction and Reporting (WIR) document.

Deliverable Date

1. Finalise target list of COCs and other analytes Completed



2. Set up analytical chemistry methods 80%

3. Confirm project methodology re sampling frequency,

statistics and chemistry 50%

4. Design, construct and commission test MF/RO plant By Sept 2007

5. Sample waste and product water streams Dec 2006 - Oct 2008

6. Undertake specialised analytical chemistry procedures Dec 2006 - Oct 2008

7.

Compare waste streams-characterise seasonal &

catchment differences from the three treatment plants

and KWRP

Dec 2006 - Oct 2008

7. Initiate Communication Plan appropriate to risks and

initial results TBA

8. Report findings Jan 2007 - Nov 2008

9. Final Report Nov 2008

10. Publish results May 2007 - Nov 2008

+

11. Communicate results at conferences and to community Feb 2007 - Nov 2008 +

Detailed Research Objectives and Performance Specifications are provided in the PCRP

Project Plan (Appendix B).

Costs and Funding

This project is being funded by a Premier’s Collaborative Research Program Grant and by the

participating organisations.

Water Corporation’s involvement is outline in Water Corporation Contract CN-06-12744

‘Premier’s Collaborative Research Program – Characterising Treated Wastewater for Drinking

Purposes following Reverse Osmosis Treatment’.

Document and Records Management

The SAP will be provided to the PCRP Steering Committee for endorsement. The endorsed

copy will be held on file by the Water Corporation Project Manager.

Operational schedules for each project component are provided in the Project Plan

(Appendix B). These are developed by each of the project streams.

PROJECT PLAN

See PCRP Project Plan for details (Appendix B).

1.3 Analytes of Interest



The PCRP Steering Committee endorsed the starting list of target analytes and analytical

methods. As this is updated during the project, changes will be endorsed the Steering

Committee at quarterly meetings, and recorded in the WIR (WIR Appendix B).

The parameters to be tested fall into 4 groups:

• basic water and wastewater characteristics

• regulated chemical contaminants, and

• unregulated chemical contaminants, and

• microbiological contaminants.

1.4 Data Collection Sites

Parties have agreed to the following sampling sites commencing with Event 3: • KWRP post-MF influent

• KWRP post-RO final effluent

• Raw bulk water (before treatment) at the Wanneroo Water Treatment Plant

• Pilot Plant post-MF effluent at Beenyup WWTP

• Pilot Plant post-RO final effluent at Beenyup WWTP

and potentially:

• Pilot Plant post-MF effluent at Subiaco WWTP

• Pilot Plant post-RO final effluent at Subiaco WWTP

Sites for sampling in each Sampling Event will be determined by the Technical Working

Group, and recorded in the WIR. From Event 3 onwards, a field blank1 will be taken at each

sampling location on each sampling day. Trip blanks2 will also be taken, but not analysed

unless inconsistencies are detected in the field blanks.

1 Field Blanks: Blanks filled at each location on the day of sampling.

2 Trip Blanks: Blanks that travel with the samples during sampling, but are not opened.



The following additional testing will also be carried out as part of the PCRP: • Health Risk Assessment Control: Raw bulk water sampled before conventional drinking water

treatment will be analysed. One sample per season will be collected as baseline reference for the

calculation of the relative health risk. Treated drinking water testing would be considered later only if

considered necessary by the PCRP Steering Committee.

• Tracer tests: Dosing pre-MF/RO, with sampling post-MF and post-RO (i.e. challenge testing).

1.5 Additional Related Work

Environmental Risk Assessment Control: As a baseline to conduct environmental risk assessment, Gnangara

groundwater quality has been analysed for the same set of analytes in existing production & monitoring bores.

To date two sampling events have occurred, one in winter 2006, the other in summer 2007. Eight bores were

sampled: 2 Leederville confined aquifer bores, 2 Superficial PVC monitoring bores, 4 superficial stainless steel

production bores, spread across the pristine area that currently or is proposed to provide drinking water from

Gnangara Mound. This includes areas upstream from or potentially in the impact area of proposed MAR trials

and schemes. This is being conducted separately from the PCRP.

Also separate from the PCRP, the Department of Water and Water Corporation, with others, are partners in a

project ‘Development of an Ecotoxicity Toolbox to Evaluate Water Quality for Recycling, Stage 1 – Beenyup

WWTP’. This will subject wastewater from three stages of the treatment to ecotoxicity and chemical testing.

Tests will be applied for cytotoxicity (Microtox or potentially IPAM), genotoxicity/carcinogenicity (Ames or SOS

umu) and endocrine toxicity (A-screen and E-screen).

1.6 Sampling Regime

Quantitative hierarchical sampling was planned to be carried out for one week per season,

over two years. It was planned that these events would be quarterly, attempting to capture

seasonal variation in effluent characteristics.

It is noted that sampling should occur over not more than 1 week. Beyond this is inefficient

for analyses at Curtin.

Samples will be taken by grab and composite samples. Grab samples will be taken for

volatile compounds, and also to compare grab and composite sampling results. From Event

3 onwards, most analytes will be composite sampled.

1.7 Equipment and infrastructure

The WWTP and RO pilot plant equipment and infrastructure is owned and operated by the

Water Corporation. Laboratories will use their own equipment and infrastructure.

1.8 Training



Water Corporation and CSIRO Standard Operating Procedures (SOPs) will apply. A Water

Corporation Job Safety Assessment has been completed (WIR Appendix D).

1.9 Occupational Safety and Health Issues

Personnel collecting samples at WWTPs and personnel analysing samples at Curtin, CSIRO and CCWA, SGS and

other outsource laboratories will follow the OHS regulations established for each institution.

DATA COLLECTION

1.10 Sample Collection

1. Determine sample dates

Sample dates will be predetermined by the Technical Working Group. Scheduled sampling

events are:

1. November/December 2006

2. May/June 2006

3. September 2007

4. December 2007

5. March 2007

6. June 2007

Specific dates during the sampling events will be recorded in: • Sampling Plan (WIR Appendix C); and

• Technical Working Group minutes

2. CSIRO requests bottles

CSIRO will request bottles required for each day. Bottles will be delivered pre-labelled with

the following information: • delivery laboratory;

• sample date;

• analysis to be undertaken; and

• any preservatives required or contained within.

CSIRO will be responsible for the sample name on the bottle.

For Day 1 of each sampling event, bottles will be delivered to CSIRO by the laboratories (one

week prior to the sampling event), with any preservative required. For subsequent sampling

days CSIRO will collect bottles when dropping off samples from the previous day. In the

event that the laboratory does not have bottles ready, the laboratory is responsible for

delivering the bottles to CSIRO.

CSIRO to use: • Sampling Record Sheet (WIR Appendix E)

3. CSIRO collects samples



CSIRO is responsible for sample collection. If delivery of samples is not possible on the day

of collection, samples will be stored chilled overnight at CSIRO, and delivered the following

day. The Sampling Record Sheet will also act as a Chain of Custody Sheet. CSIRO to use: • Sampling Record Sheet (WIR Appendix E)

• Review of Sampling (WIR Appendix F)

4. On-line measurements

Online measurements are to be taken by CSIRO as detailed in the WIR. Use: • Sampling Record Sheet (WIR Appendix E)

5. Distribute samples

Samples will be distributed to the laboratories by CSIRO, as labelled on bottles. Laboratories

will sign Sampling Record Sheet as a Chain of Custody Sheet. Use: • Sampling Record Sheet (WIR Appendix E)

6. Analysis

Laboratories to conduct analysis with appropriate QA/QC and reporting of uncertainty,

detailed in the WIR. QA/QC requirements are discussed in WIR. Use: • Results Template (WIR Appendix G), or laboratory alternative (for NMI)

7. Reporting

Review sampling, detailing any problems, breakages etc that occurred during the Sampling Event. Use:

• Review of Sampling (WIR Appendix F)

1.11 Results

Each project group will forward data to the Department of Health (c/o Clemencia Rodriguez)

for addition to the master database, with copies of data to be provided to Department of

Water and Water Corporation. The Water Corporation Technical Representative will store

hard copies of results on a Project File.

CCWA and Curtin will provide results in the template developed by the Project Partners (WIR

Appendix G). NMI and other outsource laboratories will report results using its own

reporting format.

1.12 Quality Assurance Program

A Quality Assurance (QA) program will be implemented to manage overall data quality. The program will

incorporate both sampling and analytical procedures and will seek to:

• Identify contamination by the inclusion of trip, field and laboratory blanks;

• Estimate sample homogeneity and sampling reproducibility by the inclusion of field replicates;

• Estimate analytical accuracy and analyte recovery using appropriate methods (e.g. external

calibration, internal standard addition, laboratory performance check samples, analysis of spiked

samples);

• Validate analytical methods using accepted quality control procedures and interlaboratory testing; and

• Provide basic measures of data quality including Limits of Detection and Quantitation, and method

precision.



As NATA accredited laboratories, the Chemistry Centre and NMI will follow their respective QA programs

already in place for the analyses they undertake for the project. Curtin will develop an in-house QA program for

all analytical methods developed during the project.

See:

• Quality Assurance Program (WIR Appendix H)

1.13 Contingencies

In the event of unforeseen circumstances on sampling (e.g. autosampler failure), the Water

Corporation Technical Representative will decide on whether to proceed with sampling and

analysis, or whether the sampling (day or event) is cancelled. Water Corporation will inform

laboratories as described in the WIR.

An alternative sampling (day or event) will occur as agreed between the Project Partners.



MEASUREMENT AND ANALYSIS SPECIFICATIONS

Note: Laboratories are required to provide summary of methods for the final report.

1.14 Sample Analyses

The analyses to be completed by each laboratory is detailed in the WIR. In summary:

Laboratory Analyte Method

VOCs

Purge and trap GC-MS, plus other

GC-MS methods for specific

compounds

Trihalomethanes Purge and trap GC-MS

Haloacetic acids LLE and derivatization GC-MS, IC or

purge and trap GC-MS

Haloacetonitriles LLE-GC-MS

Haloaldehydes LLE-GC-MS

Haloketones LLE-GC-MS

NitrosoDBP SPE-GC-MS

PAHs SBSE-GC-MS

Brominated flame

retardants SBSE-GC-MS

Phenols Derivatization and SBSE-GC-MS

Alkyl phenols Derivatization and SBSE-GC-MS

Alkyl phenol

polyethoxylates

SPE-LC-MS/MS or Derivatization

and SBSE-GC-MS

Hormones SPE-LC-MS/MS

Chelating Agents LLE and derivatization GC-MS

Organotins LLE and derivatization GC-MS

Pharmaceuticals SPE-LC-MS/MS (4 methods) or

SBSE-GC-MS

Curtin University

Other To be confirmed

Dioxins HRGC-HRMS

PCBs HRGC-HRMS

Selected hormones and

antibiotics for

comparison with Curtin

results

TBA NMI

Cyanide and Chromium

VI TBA

Pesticides TBA CCWA

Metals TBA

SGS Standard wastewater

parameters Various



Anions ICP-MS

Acronyms: Ion chromatography (IC), Gas Chromatography Mass Spectrometry (GC-MS),

Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS), Liquid Liquid Extraction

(LLE), Stirbar Sorptive Extraction (SBSE), Solid Phase Extraction (SPE), Solid Phase

Microextraction (SPME), High Resolution Gas Chromatography (HRGC), High Resolution Mass

Spectrometry (HRMS), Ion Coupled Plasma Mass Spectrometry (ICP-MS); To Be Advised

(TBA).



DATA MANAGEMENT

1.15 Data organisation and layout

An Excel spreadsheet for capture of the relevant information is provided in the WIR

(Appendix G). This will be managed by the Department of Health (c/o Clemencia Rodriguez).

1.16 Data storage system

Electronic and hard copies of all raw instrumental, quantification and sample data will be

made. Hard copies will be kept in two separate locations; one copy with the originator of

the data, and one copy with the Department of Health (c/o Clemencia) for incorporation into

the results spreadsheet. Spreadsheet backups are performed weekly by the Department of

Health (c/o Clemencia), and a copy provided to the Water Corporation.

1.17 Data management protocols

Results from Curtin and Chemistry Centre will be delivered to the Department of Heath (c/o

Clemencia Rodriguez) for manual consolidation in the master spreadsheet and electronic

distribution to the Project Partners.

Consolidation of results will be randomly audited by Water Corporation personnel as

described in the WIR.



APPENDIX A - REFERENCES

APHA (1998): Standard Methods for the Examination of Water and Wastewater. 20th

Edition, American Public Health Association, Water Environment Federation, American

Water Works Association, Washington USA.

Australian and New Zealand Environment and Conservation Council (ANZECC) and the

Agriculture and Resource Management Council of Australia and New Zealand (ARMCANZ),

Australian Guidelines for Water Quality Monitoring and Reporting (2000) - Chapters 1-7

Paper No. 7, Canberra ACT.

U.S. ENVIRONMENTAL PROTECTION AGENCY. 2002. EPA Guidance for Quality Assurance

Project Plans.

Washington, D.C., (EPA QA/G-5)

PCRP Work Instruction and Reporting


APPENDIX B– PCRP PROJECT PLAN

To open Appendix, double click the page below



Work Instruction and Reporting

Premiers Collaborative Research Project

(PCRP) – Characterising treated wastewater

for drinking purposes following reverse

osmosis treatment

Prepared for PCRP project partners

Department of Health

Department of Water

Department of Environment and Conservation

Water Corporation of Western Australia

CSIRO Land and Water

Curtin University of Technology

Chemistry Centre WA

National Measurement Institute

October 2007



PURPOSE OF THE DOCUMENT

The Work Instruction and Reporting (WIR) document acts as a work instruction for the sampling and

reporting undertaken in the Premier’s Collaborative Research Project (PCRP) – Characterising Treated

Wastewater for Drinking Following Reverse Osmosis Treatment. A Sampling and Analysis Plan (SAP) is

the overarching document that has been endorsed by the PCRP Steering Committee, outlining the

responsibilities of the organisations involved during sampling and reporting. The WIR is placed under

the SAP and outlines working instructions for:

• sample collection;

• sample analyses; and

• data reporting.

This document will be updated throughout the lifetime of the PCRP. Water Corporation will act as the

document custodian for the WIR.

The partners undertaking this project are:

• Department of Health (DoH)

• Department of Water (DoW)

• Department of Environment and Conservation (DEC)

• Water Corporation of Western Australia

• Chemistry Centre of Western Australia (CCWA)

• Curtin University of Technology (Curtin)

• National Measurement Institute (NMI)

• CSIRO Water for a Healthy Country (CSIRO)

• University of Western Australia (UWA)

REVISION STATUS

Ver Date Authors Sent out to Description of Version

1 July 2007 Sharon McNeil, Melissa Bromly Starting draft.

DISTRIBUTION LIST

Ver Date Sent out to Purpose

1 June 2006 PCRP HRA group For comment

2 25 July 2007 PCRP Technical Group For comment

3 Sept 2007 PCRP Technical Group For comment



TABLE OF CONTENTS

PURPOSE OF THE DOCUMENT 2

REVISION STATUS 2

DISTRIBUTION LIST 2

TABLE OF CONTENTS 3

1. PROJECT PLAN ......................................................................................................................35

1.1 Analytes of Interest ......................................................................................................................... 35

1.2 Data Collection Sites........................................................................................................................ 35

1.3 Sampling Regime ............................................................................................................................. 36

1.4 Occupational Safety and Health Issues ........................................................................................... 36

2. SAMPLING AND DATA COLLECTION.....................................................................................36

2.1 Determine Sample Dates................................................................................................................. 36

2.2 Sample Bottles................................................................................................................................. 39

2.3 Sample Collection............................................................................................................................ 39

2.4 On-line Measurements.................................................................................................................... 41

2.5 Field Measurements........................................................................................................................ 41

2.6 Sample Distribution......................................................................................................................... 41

2.7 Reporting......................................................................................................................................... 42

2.8 Contingencies .................................................................................................................................. 42

3. MEASUREMENT AND ANALYSIS SPECIFICATIONS................................................................43

3.1 Sample Analysis ............................................................................................................................... 43

3.2 Analytical Quality Assurance ........................................................................................................... 43 3.2.1 Method Validation...............................................................................................................................44

4. Documentation ....................................................................................................................44

4.1 Master Database ............................................................................................................................. 44

4.2 Sampling Form................................................................................................................................. 44

4.3 Review of Sampling Event ............................................................................................................... 44 4.3.1 Curtin Results Reporting Template......................................................................................................44

5. DATA MANAGEMENT...........................................................................................................45

5.1 Data organisation and layout .......................................................................................................... 45

5.2 Data storage system........................................................................................................................ 45

5.3 Data management protocols........................................................................................................... 45

6. DATA ANALYSIS AND REPORTING ........................................................................................45

6.1 Removing Analytes from List of Analytes........................................................................................ 45

7. PROJECT ASSESSMENT .........................................................................................................45

APPENDIX A – LIST OF ANALYTES..............................................................................................47

CCWA 47



Curtin University ...................................................................................................................................... 51

CURTIN PREPARES QA/QC for NMI.......................................................................................................... 56

NMI 57

SGS 58

APRENSA.................................................................................................................................................. 59

OTHER...................................................................................................................................................... 59

APPENDIX B – CHANGES TO LIST OF ANALYTES........................................................................59

APPENDIX C – CONTACT DETAILS FOR WWTP..........................................................................60

APPENDIX D – JSA .....................................................................................................................61

APPENDIX E – SAMPLING FORMS .............................................................................................63

APPENDIX F – SAMPLE EVENT SUMMARY ................................................................................77

Sample Event Plan 1 ................................................................................................................................ 77

Sample Event Review 1............................................................................................................................ 78





APPENDIX G – RESULTS TEMPLATE FOR CURTIN AND CCWA ..................................................91

APPENDIX J – Proficiency Testing Undertaken .........................................................................94



2 PROJECT PLAN

2.1 Analytes of Interest

The analytes to be tested have been divided into 4 groups:

• basic water and wastewater characteristics;

• regulated chemical contaminants;

• unregulated chemical contaminants; and

• microbiological contaminants.

The analytes are listed in Appendix A, according to the laboratory that is responsible for analysis. Also

contained in Appendix A is the analysis method and limit of reporting (LOR).

As more information becomes available on each analyte, the List of Analytes will be reviewed.

Changes to the List of Analytes will be documented in Appendix B, including the reasons for the

changes.

2.2 Data Collection Sites

Parties agreed to the following sampling sites:

• Influent to KWRP from Woodman Point WWTP (Panel 1)

• KWRP post-MF influent (Panel 6)

• KWRP post-RO final effluent (Panel 7)

• KWRP post-RO final effluent pre-dam (Panel 8)

• Raw bulk water (before treatment) at the Wanneroo Water Treatment Plant

• Pilot Plant pre-MF effluent at Beenyup WWTP (SP 1)

• Pilot Plant post-MF effluent at Beenyup WWTP (SP 5)

• Pilot Plant post-RO final effluent at Beenyup WWTP (SP 6)

• and potentially:

• Pilot Plant post-MF effluent at Subiaco WWTP

• Pilot Plant post-RO final effluent at Subiaco WWTP

Raw Feedwater

(Secondary Effluent)

Basket Strainer

Backwash to drain

Microfiltration

Backwash to drain

Reverse Osmosis Stage 1

Reject to drain

Reverse Osmosis Stage 2

Stage 1 Permeate

Sample Point

Stage 2 Permeate

Sample Point

Combined Permeate

RO Feed tank

Basic Process Flow Diagram - Beenyup Pilot Plant

Chemical Dosing

(Chlorine, Ammonia, Acid)

Sample

Point 1

Sample

Point 5

Sample

Point 6

Sample

Point 7

The following additional testing will also be carried out as part of the PCRP:

• Health Risk Assessment Control: Raw bulk water sampled before conventional drinking water

treatment will be analysed. One sample per season will be collected as baseline reference for

the calculation of the relative health risk. Treated drinking water testing would be

considered later only if considered necessary by the PCRP Steering Committee.

• Tracer tests: Dosing pre-MF/RO, with sampling post-MF and post-RO (i.e. challenge testing)



2.3 Sampling Regime

Quantitative hierarchical sampling was planned to be carried out for one week, quarterly, over two

years. It was planned that these events would be quarterly, to capture seasonal variation in effluent.

The sampling dates are:

1. 29 Nov-06 to 6 Dec-06

2. 24 May-07 to 19 Jun-07

3. 21 Sept-07 to 30 Sept-07

4. 14 Jan-08 to 18 Jan-08

5. 10 Mar-08 to 16 Mar-083

6. 09 Jun-08 to 15 Jun-084

2.4 Occupational Safety and Health Issues

Personnel collecting samples at WWTPs will be required to complete inductions at each site. Contact

Details for each plant are contained in Appendix C. A Job Safety Analysis requires completion prior to

the first sample event for each sample location. This is attached in Appendix D.

Personnel analysing samples at Curtin, CSIRO, NMI and CCWA will follow the Occupational Safety and

Health regulations established for each institution.

3 SAMPLING AND DATA COLLECTION

3.1 Determine Sample Dates

Sample events will be predetermined by the Technical Working Group. These are listed for each event

in Table 1. Changes to the Sampling Event can not occur 10 days prior to the Sampling Event. The

Water Corporation’s technical representative will distribute the sample forms (Appendix E) to CSIRO,

10 days prior to the sampling event.

The Water Corporation technical representative will coordinate the sampling with each sample site.

Also the Water Corporation technical representative will be responsible for setting the controls on the

autosampler.

3 Tentative Dates

4 Tentative Dates



Table 1: Sampling Events for PCRP Project

KWRP Wanneroo Raw Subiaco WWTP Beenyup WWTP Sampling

Event Panel 1 Panel 6 Panel 7 Panel 8 Pinjar line Wanneroo line Effluent Pilot Plant Post MF RO

Permeate Effluent (SP 1)

Pilot Plant Post MF (SP

6) RO Permeate (SP 7)

Wed

29-11-06

Wed

29-11-06

Wed

29-11-06

Sun

03-12-06

Sun

03-12-06

Sun

03-12-06

1. Dec-06

Tues

06-12-06

Tues

06-12-06

Tues

06-12-06

Thur

24-05-07

Thur

24-05-07

Thur

24-05-07

Wed

30-05-07

Wed

30-05-07

Wed

30-05-07

Mon

04-06-07

Mon

04-06-07

Mon

04-06-07

Thur

07-06-07

Thur

07-06-07

Thur

07-06-07

Tues

12-06-07

Tues

12-06-07

2. May-07

Tues

19-06-07

Fri

21/09/07

Fri

21/09/075

Fri

21/09/07

Mon

24/09/07

Mon

24/09/07

Tues

25/09/07

Tues

25/09/07

Wed 26/09/07 Wed 26/09/07 1 Wed 26/09/07

Thur

27/09/07

Thur

27/09/07

3. Sept-07

Fri

28/09/07

Fri

28/09/07

Mon

14/01/086

Mon

14/01/087

Tues

15/01/08

Tues

15/01/08

Wed

16/01/08

Wed

16/01/08

Wed

16/01/08

Wed

16/01/08

Thurs

17/01/08

Thurs

17/01/08

4. Jan-08

Fri

18/01/08

Fri

18/01/08

Mon 31/03/08 Mon 31/03/08

Tues 01/04/08 Tues 01/04/08 Tues 01/04/08

Thurs 03/04/08 Thurs 03/04/08 Thurs 03/04/08

Fri 04/04/08 Fri 04/04/08

5. Mar-08

Sun 06/04/08 Sun 06/04/08

Thurs 05/06/08 Thurs 05/06/08 Thurs 05/06/08

Fri 06/06/08 Fri 06/06/08 Fri 06/06/08

Sun 08/06/08 Sun 08/06/08

Mon 09/06/08 Mon 09/06/08

6. June-08

Tues 10/06/08 Tues 10/06/08

5 DBPs only

6 Includes full replicate of Panel 1

7 Includes full replicate of Panel 7



Sampling

Event Beenyup WWTP

Primary Effluent Post Secondary

treatment Pre-Cl Inlet Post-Cl Pre-MF Post MF Post RO RO Reject

MF Reject

Mon

06-10-08

Mon

06-10-08

Mon

06-10-08

Mon

06-10-08

Mon

06-10-08

Mon

06-10-08

Mon

06-10-08

Mon

06-10-08

wed

08-10-08

wed

08-10-08

wed

08-10-08

wed

08-10-08

wed

08-10-08

wed

08-10-08

wed

08-10-08

wed

08-10-08

7. Oct-08

Nitroso

Sampling

Thur

09-10-08

Thur

09-10-08

Thur

09-10-08

Thur

09-10-08

Thur

09-10-08

Thur

09-10-08

Note: From Event 3 onwards, a field blank8 will be taken at each sampling location on each sampling day. Trip blanks

9 will also be taken, but not analysed unless inconsistencies are detected in the field blanks.

8 Field Blanks: Blanks filled at each location on the day of sampling.

9 Trip Blanks: Blanks that travel with the samples during sampling, but are not opened.



3.2 Sample Bottles

Sample Bottle Labelling

CSIRO will request the bottles required from the laboratories. The laboratories supplying the bottles

will be labelled with the following information:

• sample analyses required;

• laboratory the sample will be submitted to; and

• preservatives and/or dechlorinating agents the bottles contains.

CSIRO will label the bottles with the following information:

• sample name; and

• sample date.

Sample Bottle Preparation

Sampling containers should be cleaned using a method appropriate for the analyses being carried out.

Sample preservatives and/or dechlorinating agent are added to some containers in order to preserve

specific analytes against degradation before analysis.

Below summarises the responsibilities for preparing bottles:

• Water Corporation will provide 20L and 10 L bottles to Curtin for annealing;

• CCWA will provide bottles for their samples to Curtin for annealing;

• CCWA will provide bottles to CSIRO for the radiological samples;

• Bottles required for SGS samples will be provided by CSIRO;

• Other than those bottles mentioned above, all other laboratories will be responsible for their

own samples bottles including the addition of preservatives and/or dechlorinating agents.

Curtin will prepare sampling bottles in accordance with CWQRC Sampling Standard Operating

Procedure (SOP) 01 (WQSP01-1a).

Sample Bottle Delivery

For Day 1 of each sampling event, bottles will be delivered to CSIRO by the laboratories, with the

preservatives required (at least 7 days prior to the event).

For subsequent sampling days, CSIRO will collect bottles when delivering samples from the previous

day. In the event that the laboratory does not have bottles ready, the laboratory is responsible for

delivering the bottles to CSIRO.

3.3 Sample Collection

CSIRO will be responsible for sample collection and distribution of the samples to the laboratories.

Sampling forms will detail information on the samples to be collected, sample bottles to use,

preservatives and/or dechlorinating agents required and any other sampling requirements.

Grab and composite samples will be collected. Grab samples are required for VOC (Volatile Organic

Carbon) and Gross α and β radiation samples as well as providing a comparison to composite samples.

Grab samples are taken either directly from a sapling tap or through the manual cycles from an

autosampler. The sampling taps are initially flushed and the water then passed through a flow cell for

field measurements. It is not possible to conduct field measurements from the autosampler due to

the sample being dispensed in 200mL-500mL cycles.

Grab samples are collected by tilting the sample bottles underneath the sampling tap and filling to the

required level (shoulder, top, no headspace) without overflowing. Samples collected for SGS were

rinsed with the sample before collection and stored with frozen cooler bricks. Grab samples from the



autosampler were collected in a clean, rinsed glass beaker and decanted into sample bottles. This was

to minimise the risk of overflowing or spilling the sample due to the water spurting out from the

autosampler.

Composite samples were collected in a 20L glass bottle packed with cooler bricks, or four 10L

containers in a refrigerator. The sample was poured into a clean glass beaker through a clean glass

funnel, and decanted into the final sample containers.

Samples for Hg for CCWA and nutrients and FRP for SGS required filtering, The sample was filtered

though a 0.45um syringe filter into the final sample bottle.

Sample labels will be filled out on site with the following information:

• sample name;

• sample date; and

• sample analyses required

Laboratory the sample will be delivered to for analysis

Field and Trip Blanks

Field and trip blanks monitor contamination during sampling. Trip blanks are sealed bottles of

deionised water that are transported along the field trip to each site but are not opened. Field blanks

are treated in the same manner as samples, but bottles are filled with deionised (DI) water, instead of

samples from the site.

Field Blanks

One field blank is taken at each sample site, for each analysis method. Field blanks will be routinely

analysed alongside samples and will indicate if any contamination has occurred in the field or during

transportation of the empty sample bottles. Bottles that have been cleaned and prepared in the

same manner as the sampling bottles are filled on site with DI water. The water used will be taken

from the DI water supply from CSIRO and transported in clean pre-rinsed 20 L glass containers. Filled

field blanks are provided by Curtin for all analysis and by CCWA for pesticides. These are opened at

the pre-micro filtration sampling locations.

Trip Blanks

One trip blank is collected for each trip, for each analysis method. Trip blanks are not routinely

analysed, but are instead kept as a back up monitor, should either field blanks or samples

demonstrate unreasonably high analyte concentrations or contamination. One set of bottles, cleaned

and prepared in the same manner as the other samples bottles, are supplied filled by Curtin and

CCWA. NMI and SGS are filled with DI water from CSIRO. The bottles are sealed at CSIRO and then

transported along side the samples during the field trip. The bottles should be labelled with the dates

by the personnel carrying out the sampling. The samples are not opened during the trip.

Sample homogeneity

To ensure that comparison of trends in different chemical parameters is valid, it is important that all

sub-samples delivered to individual analytical laboratory are representative of the original bulk

sample.

Composite samples are collected in either a single 20 L container or four 10 L containers, over a

twenty four hour period. Sample homogeneity before sub-sampling is ensured through vigorously

shaking the container.

Grab samples are collected by (tipping water into a big vat??) Sample homogeneity before

subsampling is ensured by (mixing? Stirring?).



Field Replicates

Field replicates are two or more samples taken simultaneously at the same site, representative of the

same environmental conditions. They provide information about environmental heterogeneity and

the reproducibility of field sampling.

Ideally duplicates of all samples would be taken; however in this project doubling the number of

samples is impractical with respect to the total number of samples and analytes and also the sample

volume available for analysis. In addition, limitations on the total volume of sample collected by the

compositing autosampler mean that there is insufficient water for duplicate composite samples.

Replicates can be obtained for the grab samples, however due to the low number of samples, results

may not be meaningful.

Field replicates will be considered in 2008 when the analyte list should have decreased (on the basis

of repeated non-detection) and there is time and sample volume available for duplicate analysis.

3.4 On-line Measurements

Online measurements are recorded as per Table 2. CSIRO are responsible for the recording of these

during the sampling event.

Table 2: Online Measurements available at the sampling sites

Sample Site Online Measurement

pH

free ammonia

turbidity KWRP Panel 1

conductivity

pH

free ammonia

turbidity

conductivity

total chlorine

KWRP Panel 6

ORP

pH

conductivity KWRP Panel 7

total chlorine

Beenyup Post MF pH

conductivity

Beenyup Post RO conductivity

3.5 Field Measurements

CSIRO will be responsible for ensuring the collection of the following Field Measurements from each

sampling site (where applicable):

• time;

• sample temperature;

• pH;

• electrical conductivity;

• dissolved Oxygen (DO); and

• ambient temperature

3.6 Sample Distribution



CSIRO will deliver samples to the laboratories, as labelled on the bottles. If delivery of samples is not

possible on the day of collection, samples will be stored chilled (4 °C) and delivered the next day.

CSIRO will notify the laboratories that the samples will not arrive on the day of collection.

A signed copy of the sample form will act as a chain of custody form. A copy will be given to each

laboratory as well as a copy kept by CSIRO.

QA/QC samples for NMI NSW will be delivered to Curtin, where they will undergo spiking and

splitting. Curtin will be responsible for the delivery of the QA/QC samples to NMI WA. NMI WA will

send samples to NMI NSW.

Radiation samples are to be delivered to CCWA. CCWA will deliver these to APRENSA and Radiation

Health respectively.

3.7 Reporting

Sampling Forms will act as Chain of Custody forms. Furthermore these forms will detail information

on any problems, breakages etc that occurred during the Sampling Event. Copies of these will be

forwarded to Department of Health (c/o Clemencia Rodriguez) to be inputted into the Master

Database. Additionally copies of the completed forms will be attached to the WIR in Appendix E.

At the completion of each sampling event, the PCRP Technical Group will meet to discuss the

sampling event. A Review of Sampling Event will be completed and will be attached to the WIR in

Appendix F, with a hard copy kept by the Water Corporation Technical Representative.

Results from each sampling event will be forwarded to the Department of Health (c/o Clemencia

Rodriguez) for addition to the Master Database, with copies to be provided to Department of Water

and Water Corporation. The Water Corporation Technical Representative will store hard copies of

results on a Project File. NMI NSW will provide results to Curtin, for forwarding to the Department of

Health (c/o Clemencia Rodriguez).

Curtin and Chemistry Centre will provide results in the template developed by the Department of

Health (Appendix G). NMI will report results using its own reporting format.

Where results are delivered in stages, spreadsheets should not be updated, until a substantial amount

of data is received in order to maintain an audit trail. Results will be randomly audited by the Water

Corporation by following results from the laboratory reports into the database.

3.8 Contingencies

In the event of unforeseen circumstances on sampling (e.g. autosampler failure), the Water

Corporation Technical Representative will decide on whether to proceed with sampling and analysis,

or whether samples are cancelled and inform laboratories ASAP as below.

Organisation Contact Number

Water Corporation Palenque Blair 9420 3328

CSIRO Simon Higginson 0429 186 609

Curtin Andrew Chan 0412 257 782

Chemistry Centre Karyn Courtney 9222 3578

NMI Paula McLay 9368 8425



4 MEASUREMENT AND ANALYSIS

SPECIFICATIONS

4.1 Sample Analysis

The analysis to be completed by each laboratory is detailed in Appendix A. Table 2 summarises the

methods used for each group of analytes.

Table 2: Summary of Analytes

Laboratory Analyte Method

VOCs Purge and trap GC-MS, plus other GC-

MS methods for specific compounds

Trihalomethanes Purge and trap GC-MS

Haloacetic acids LLE and derivatization GC-MS

Haloacetonitriles LLE-GC-MS

Other DBP IC

Haloaldehydes LLE-GC-MS

Haloketones LLE-GC-MS

NitrosoDBP SPE-GC-MS

PAHs SBSE-GC-MS

Brominated flame retardants SBSE-GC-MS

Phenols Derivatization and SBSE-GC-MS

Alkyl phenols Derivatization and SBSE-GC-MS

Alkyl phenol polyethoxylates SPE-LC-MS/MS or Derivatization and

SBSE-GC-MS

Hormones SPE-LC-MS/MS

Chelating Agents LLE and derivatization GC-MS

Organotines LLE and derivatization GC-MS

Pharmaceuticals SPE-LC-MS/MS (4 methods) or SBSE-

GC-MS

Curtin University

Other To be confirmed

NMI Dioxins HRGC/HRMS

PCBs HRGC/HRMS

Metals ICP-OES; colorimetric

Selected hormones and antibiotics for

comparison with Curtin results

Chemistry Centre Pesticides GC-ECD/NPD or GC-MS

Mercury

Metals

Radiation Preparation

ARPANSA Radium Liquid Scintillation Countin High

resolution gamma-ray spectrometry

Gross α particle activity

SGS Standard wastewater parameters

4.2 Analytical Quality Assurance

Each laboratory (Curtin, CCWA, NMI, SGS) will follow in-house quality assurance guidelines. In

addition to concentration data, laboratories will report an uncertainty for each result. Limits of

Detection and Quantitation, precision, and recovery for each method will also be reported.



Method Validation

Generally, analytical methods used by NMI, CCWA and SGS are nationally accredited and validation

studies have been undertaken as part of this process. In contrast, the methods used by Curtin have

been developed specifically for the PCRP project and therefore will undergo validation during the

project. It is acknowledged that the non-routine nature of these analyses means that accreditation is

unlikely. However, method validation will incorporate the following minimum criteria:

• Each method will be documented in a Standard Operation Procedure (SOP). The SOP will

report on acceptable criteria for method precision (repeatability) and bias (recovery), the

range of linearity, method detection limits and uncertainty budgets. The SOP will also

comment on the robustness of the method, the effect of variations in certain parameters,

and method sensitivity and selectivity.

• Where possible, newly developed methods from Curtin will be validated using certified

reference materials (CRM). In the absence of appropriate CRM, where appropriate

capabilities exist, methods will be tested by inter-laboratory testing for validation. The inter-

laboratory testing schemes participated in will be documented in Appendix J.

Curtin will also ensure the developed methods are scrutinized through appropriate peer review

processes including consultation with leading international experts and publication of methods in

peer reviewed journals.

5 Documentation

5.1 Master Database

Department of Health representative (Clemencia Rodriguez) will be responsible for the Master

Database. After a major addition of data to the Master Database, the database will be provided to

each organisation.

Water Corporation will audit the database, through comparing selected data received from the

laboratories to the data contained in the database.

5.2 Sampling Form

Water Corporation’s technical representative will be the custodian for the Sampling Form. This form

will detail information on:

• samples required;

• measurements required;

• laboratories samples will be delivered to; and

• act as chain of custody for samples.

Two weeks prior to each sampling event, Sampling Forms will be forwarded to CSIRO. Appendix E will

contain the completed Sampling Forms.

5.3 Review of Sampling Event

Water Corporation’s technical representative will be the custodian for the Review of Sampling Event.

This document will detail any differences that occurred from the planned Sampling Event. Appendix F

will contain the Review of Sampling Event.

Curtin Results Reporting Template

The Department of Health will be the custodian for the template Curtin and CCWA will use to report



results. This is contained in Appendix G.

6 DATA MANAGEMENT

6.1 Data organisation and layout

In order to ensure agreement in the reporting of analytical results between laboratories, an Excel

spreadsheets with all the relevant information, data checking and data verification is attached in

Appendix H.

6.2 Data storage system

Electronic and hard copies of all raw instrumental and quantification will be stored by the analysing

laboratory. Both Electronic and hard copies of the Final sample results will be stored retained in two

separate locations, one at the Department of Health (c/o Clemencia Rodriguez) and Water

Corporation (c/o Project Manager).

6.3 Data management protocols

Suggested content:

• The need to properly register the project, sites and sampling regime information in the database.

• The process for managing completed forms and generated data, e.g. storage of local copies,

transfer of copies to central database for processing, etc

• How and by whom data will be captured.

7 DATA ANALYSIS AND REPORTING

7.1 Removing Analytes from List of Analytes

It is expected that many parameters will not be analysed over the full term of the project. If eight

samples are recorded at an individual sample location below the detection limit, then the Research

Steering Team will review whether future sampling for this parameter at this location is necessary and

submit this to the Steering Committee for approval. Other parameters may also be reviewed for

potential removal from analysis after 8 sample results from a single sample location. The variability of

results recorded from the initial eight samples will be an important factor in these decisions. NB:

Eight samples in most cases will equate to two sampling seasons – with four samples per season.

However, a few parameters will only be monitored once per season (as marked on attached

spreadsheet).

8 PROJECT ASSESSMENT

Generally it would be assessment against aims (from memory key outcomes include scientific papers

(or PhD) including results, indirect potable reuse regulations for WA and capability to assess safety of

an aquifer recharge scheme from a chemical perspective), however some aims have been modified

since first outline of aims (e.g. agreement that not focussing on both Beenyup and Subiaco at once,

only one at a time, so only one years worth of data, and agreement that Subiaco would be dropped if

necessary, so need to make sure the modified scope is used. Also we will be assessed by the PCRP

presumably.



I’d suggest talking to Deanne about this. Perhaps there should be assessment against the starting

Project objectives/overview (e.g. 4.2 of the Project Plan)?



APPENDIX A – LIST OF ANALYTES

CCWA

ID CAS Parameter Reporting

Units LOR

Analysis

Method Notes:

Metals

500 7429-90-5 Aluminium

501 7440-36-0 Antimony

502 7440-38-2 Arsenic

503 7440-39-3 Barium

504 Beryllium

505 7440-42-8 Boron

506 Cadmium

507 7440-43-9 Chromium (Total)

508 7440-50-8 Copper

509 7439-92-1 Lead

510 7439-96-5 Manganese

511 7439-97-6 Mercury

512 7439-98-7 Molybdenum

513 7440-02-0 Nickel

514 7782-49-2 Selenium

515 7440-22-4 Silver

516 7440-28-0 Thallium

517 7440-61-1 Uranium

518 7439-89-6 Iron

519 7440-48-4 Cobalt

520 7439-93-2 Lithium

521 7440-24-6 Strontium

522 7440-62-2 Vanadium

523 7440-66-6 Zinc

524 7440-31-5 Tin

Pesticides

525 309-00-2 Aldrin

526 57-74-9? Chlordane (total isomers)

527 60-57-1 Dieldrin

528 72-20-8 Endrin

529 76-44-8 Heptachlor & Hp Epoxide

530 959-98-8 Endosulfan I (alpha)

531 33213-65-9 Endosulfan II (beta)

532 1031-07-8 Endosulfan sulfate

533 115-32-2 Dicofol (1,1-bis(chlorophenyl)-2,2,2-

trichloroethanol)

534 50-29-3 DDT and metabolites (total isomers)

p,p-DDE

(only requires analyse if

DDT above LOR)

535 72-43-5 Methoxychlor

536 58-89-9 Lindane [gamma

hexachlorocyclohexane (HCH)]

537 56-38-2 Parathion (Parathion-ethyl)

538 298-00-0 Parathion methyl (Methyl paration)

539 23505-41-1 Pirimiphos-ethyl


540 29232-93-7 Azinphos-Methyl

541 60-51-5 Dimethoate

542 122-14-5 Fenitrothion

543 121-75-5 Malathion (maldison)

544 62-73-7 Dichlorvos

545 563-12-2 Ethion

546 950-37-8 Methidathion

547 4824-78-6 Bromophos-ethyl

548 470-90-6 Chlorfenvinphos

549 299-84-3 Fenchlorphos (ronnel)

550 115-90-2 Fensulfothion

551 2540-82-1 Formothion

552 13457-18-6 Pyrazophos

553 35400-43-2 Sulprofos

554 3383-96-8 Temephos

555 6923-22-4 Monocrotophos

556 22224-92-6 Fenamiphos

557 786-19-6 Carbophenothion (Thrition)

558 41198-08-7 Profenofos

559 13071-79-9 Terbufos

560 22248-79-9 Tetrachlorvinphos

561 298-04-4 Disulfoton

562 13194-48-4 Ethoprophos

563 640-15-3 Thiometon

564 333-41-5 Diazinon

565 30560-19-1 Acephate

566 52-68-6 Trichlorfon

567 7786-34-7 Mevinphos

568 2921-88-2 Chlorpyrifos

569 62-73-7 Dichlorvos

570 5234-68-4 Carboxin

571 1897-45-6 Chlorothalonil

572 60168-88-4 Fenarimol

573 60207-90-1 Propiconazole

574 43121-43-3 Triadimefon

575 17804-35-2 Benomyl

576 10605-21-7 Carbendazim (MCB)

577 23564-06-9 Thiophanate

578 40487-42-1 Pendimethalin

579 82-68-8 Quintozene (PentaChloroNitroBenzene,

PCNB)

580 51338-27-3 Diclofop-methyl

581 957-51-7 Diphenamid

582 27314-13-2 Norflurazon

583 15299-99-7 Napropamide

584 1861-32-1 Propanil (3′,4′-dichloropropionanilide)

585 23950-58-5 Propyzamide

586 4726-14-1 Nitralin

587 19044-88-3 Oryzalin

588 1582-09-8 Trifluralin (tifluralin)

589 2312-35-8 Propargite

590 1918-16-7 Propachlor

591 51218-45-2 Metolachlor


592 1912-24-9 Atrazine

593 122-34-9 Simazine

594 886-50-0 Terbutryn

595 139-40-2 Propazine

596 834-12-8 Ametryn (Ametryne)

597 21725-46-2 Cyanazine (Bladex)

598 51235-04-2 Hexazinone

599 21087-64-9 Metribuzin

600 1982-47-4 Chloroxuron

601 64902-72-3 Chlorsulfuron

602 330-54-1 Diuron

603 2164-17-2 Fluometuron

604 74223-64-6 Metsulfuron-methyl

605 25057-89-0 Bentazone (Bentazon)

607 314-40-9 Bromacil

608 5902-51-2 Terbacil

609 94-75-7 2,4-D (2,4-dichlorophenoxyacetic acid)

610 1702-17-6 Clopyralid

611 1918-00-9 Dicamba

612 122-39-4 DPA (Diphenylamine)

613 94-74-6 MCPA ((4-chloro-2-

methylphenoxy)acetic acid)

614 7085-19-0 Mecoprop (MCPP)

615 93-72-1 Fenoprop (Silvex, 2,4,5-TP)

616 52756-25-9 Flamprop-methyl

617 1918-02-1 Picloram

618 93-76-5 2,4,5-T or (2,4,5-trichlorophenoxyacetic

acid)

619 55335-06-3 Triclopyr

620 145-73-3 Endothall (Endothal)

621 75-99-0 Dalapon (2,2-Dichloro propanoic acid)

622 1689-84-5 Bromoxynil

623 1194-65-6 Dichlobenil

624 43222-48-6 Difenzoquat methyl sulfate

625 85-00-7 Diquat

626 1910-42-5 Paraquat

627 28434-01-7 Bioresmethrin

628 51630-58-1 Fenvalerate

629 52645-53-1 Permethrin

630 23135-22-0 Oxymal (Oxamyl, Vydate)

631 116-06-3 Aldicarb

632 63-25-2 Carbaryl (Sevin)

633 1563-66-2 Carbofuran

635 2032-65-7 Methiocarb

636 16752-77-5 Methomyl

637 23103-98-2 Pirimicarb

638 28249-77-6 Thiobencarb (Bolero)

639 2631-37-0 Promecarb

640 759-94-4 EPTC (s-ethyl-dipropylthiocarbamate)

641 2212-67-1 Molinate (Ordram)

642 1114-71-2 Pebulate

643 1929-77-7 Vernolate

644 51-03-6 Piperonyl butoxide


645 1071-83-6 Glyphosate

646 61-82-5 Amitrole

647 3337-71-1 Asulam

648 2593-15-9 Etridiazole

649 25954-13-6 Fosamine ammonium salt

650 137-26-8 Thiram (TMTD)

Method not developed

as at July 2007. Once

analyte list has been

reduced will develop

methods.

651 77-47-4 Hexachlorocyclopentadiene (HCCPD)

652 298-02-2 Phorate

653 55-38-9 Fenthion

654 10265-92-6 Methamidophos (O,S-dimethyl

phosphoramidothioate)

655 67747-09-5 Prochloraz





methods.

656 6190-65-4 Atrazine-desethyl





methods.

657 34014-18-1 Tebuthiuron

658 330-55-2 Linuron

659 18691-97-9 Methabenzthiazuron

660 35367-38-5 Diflubenzuron

661 1861-32-1 Dacthal (Chlorthal Dimethyl, DCPA)

662 887-54-7 DCPA mono-acid degradate





methods.

663 2136-79-0 DCPA di-acid degradate





methods.

664 94-81-5 4-(4-chloro-2-methylphenoxy)butanoic

acid (MCPB)

665 55512-33-9 Pyridate





methods.

666 52918-63-5 Deltamethrin

667 52315-07-8 Cypermethrin

668 66230-04-4 Esfenvalerate





methods.

669 82657-04-3 Bifenthrin

670 1646-87-3 Aldicarb Sulfoxide





methods.

671 1646-88-4 Aldicarb Sulfone





methods.


672 204-043-8 Propoxur (2-isopropoxyphenyl

methylcarbamate, Baygon)

673 33089-61-1 Amitraz





methods.

674 105827-78-9 Imidacloprid

675 86479-06-3 Hexaflumuron

676 64628-44-0 Triflumuron

677 120068-37-3 Fipronil

678 94-82-6 2,4-DB acid

679 95737-68-1 Pyriproxifen





methods.

680 133-06-2 Captan

681 101-21-3 Chlorpropham (CIPC)

682 137-42-8 Metham Sodium (metam/sodium

methyldithiocarbamate)





methods.

Alachor

beta-BHC

Chllorpyrifos methyl

Demeton-S methyl

Curtin University

ID CAS Parameter Units LOR Analysis

Method Notes

VOCs

100 71-43-2 Benzene PT-GC-G1

101 56-23-5 Carbon tetrachloride PT-GC-G1

102 108-90-7 Chlorobenzene (monochlorobenzene) PT-GC-G1

103 95-50-1 1,2-dichlorobenzene (orto) PT-GC-G1

104 106-46-7 1,4-dichlorobenzene (pDCB, 1,4-DCB) PT-GC-G1

105 75-34-3 1,1-dichloroethane PT-GC-G1

106 107-06-2 1,2-dichloroethane (1,2-DCA, Ethylene

dichloride) PT-GC-G1

107 75-35-4 1,1-dichloroethene (1,1-DCE) PT-GC-G1

108 156-59-2 1,2-dichloroethene, cis PT-GC-G1

109 156-60-5 1,2-dichloroethene, trans PT-GC-G1

110 75-09-2 Dichloromethane (methylene chloride) PT-GC-G1

111 100-41-4 Ethyl benzene PT-GC-G1

112 87-68-3 Hexachlorobutadiene PT-GC-G1

113 100-42-5 Styrene (vinylbenzene) PT-GC-G1

114 79-34-5 1,1,2,2-Tetrachloroethane PT-GC-G1

115 127-18-4 Tetrachloroethene (tetrachloroethylene,

perchloroethylene, PCE) PT-GC-G1

116 108-88-3 Toluene PT-GC-G1

117 71-55-6 1,1,1-Trichloroethane (TCA) PT-GC-G1

118 79-00-5 1,1,2-Trichloroethane PT-GC-G1

119 120-82-1 1,2,4-Trichlorobenzene PT-GC-G1


120 79-01-6 Trichloroethene (trichloroethylene, TCE) PT-GC-G1

121 75-69-4 Trichlorofluoromethane (Freon 11, CFC-

11) PT-GC-G1

122 76-13-1 1,1,2-Trichloro-1,2,2-trifluoroethane

(CFC-113, Freon 113) SU

123 1330-20-7 Xylenes PT-GC-G1

124 106-93-4 Ethylene Dibromide (1,2-

Dibromoethane, EDB) PT-GC-G1

125 96-12-8 Dibromochloropropane (1,2-dibromo-3-

chloropropane (DBCP)) PT-GC-G1

126 78-87-5 1,2-Dichloropropane (1,2-DCP) PT-GC-G1

127 542-75-6 1,3-Dichloropropene PT-GC-G1

128 630-20-6 1,1,1,2-Tetrachloroethane PT-GC-G1

129 87-61-6 1,2,3-Trichlorobenzene PT-GC-G1

130 96-18-4 1,2,3-Trichloropropane (TCP) PT-GC-G1

131 526-73-8 1,2,3-trimethylbenzene PT-GC-G1

132 95-63-6 1,2,4-trimethylbenzene (pseudocumene) PT-GC-G1

133 108-67-8 1,3,5-trimethylbenzene (mesitylene) PT-GC-G1

134 541-73-1 1,3-dichlorobenzene (meta) PT-GC-G1

135 142-28-9 1,3-Dichloropropane PT-GC-G1

136 594-207 2,2-Dichloropropane (sec) PT-GC-G1

137 95-49-8 2-Chlorotoluene (ortho) PT-GC-G1

138 106-43-4 4-Chlorotoluene (para) PT-GC-G1

139 593-60-2 Bromoethene (Vinyl bromide) PT-GC-G1

140 75-00-3 Chloroethane (ethyl chloride) PT-GC-G1

141 74-87-3 Chloromethane (methyl chloride) PT-GC-G1

142 75-71-8

Dichlorodifluoromethane

(Diflurorodichloromethane, CFC-12,

Freon 12)

PT-GC-G1

143 67-72-1 Hexachloroethane PT-GC-G1

144 98-82-8 Isopropyl benzene (cumene) PT-GC-G1

145 104-51-8 n-butyl benzene PT-GC-G1

146 103-65-1 n-propyl benzene (isocumene,

propylbenzene) PT-GC-G1

147 99-87-6 p-Isopropyltoluene (p-cymene) PT-GC-G1

148 135-98-8 sec-butyl benzene PT-GC-G1

149 98-06-6 tert butyl benzene PT-GC-G1

150 25551-13-7 Trimethylbenzenes (mixed isomers) PT-GC-G1

151 107-02-8 Acrolein LLE-Der-GC-G4

152 107-13-1 Acrylonitrile SPME-GC-G5

DBP

153 NO CAS Total Trihalomethanes (TTHM)

154 67-66-3 Chloroform (Trichloromethane) PT-GC-G1

155 75-27-4 Bromodichloromethane

(Dichlorobromomethane) PT-GC-G1

156 124-48-1 Chlorodibromomethane

(dibromochloromethane) PT-GC-G1

157 75-25-2 Bromoform (Tribromomethane) PT-GC-G1

158 74-95-3 Dibromomethane PT-GC-G1

159 74-97-5 Bromochloromethane PT-GC-G1

160 NO CAS Haloacetic acids (HAA9)

161 79-11-8 Chloroacetic acid (monochlororacetic

acid; MCA) LLE-Der-GC-G2

162 79-43-6 Dichloroacetic acid (DCA) LLE-Der-GC-G2

163 650-51-1 Trichloroacetic acid (TCA) LLE-Der-GC-G2

164 79-08-3 Bromoacetic acid (monobromoacetic LLE-Der-GC-G2


acid; MBA)

165 631-64-1 Dibromoacetic acid (DBA) LLE-Der-GC-G2

166 71133-14-7 Dichlorobromoacetic acid (DCBA;

bromodichloroacetic acid) LLE-Der-GC-G2

167 5589-96-8 Bromochloroacetic acid (BCA) LLE-Der-GC-G2

168 5278-95-5 Dibromochloroacetic acid (DBCA;

Chlorodibromoacetic acid) LLE-Der-GC-G2

169 75-96-7 Tribromoacetic acid (TBA) LLE-Der-GC-G2

170 76-06-2 Chloropicrin (Trichloronitromethane) LLE-GC-G6

171 15541-45-4 Bromate IC-G3

172 7758-19-2 Chlorite IC-G3

173 7775--09-9 Chlorate IC-G3

174 506-68-3 Cyanogen bromide

175 108-86-1 Bromobenzene (Phenyl bromide;

Bromobenzol) PT-GC-G1

176 NO CAS Haloacetonitriles (7)

177 3252-43-5 Dibromoacetonitrile (DBAN) LLE-GC-G6

178 3018-12-0 Dichloroacetonitrile (DCAN) LLE-GC-G6

179 107-14-2 Monochloroac

Documents

PCRP Appendices FINAL 29062010 - WA Health/media/Files/Corporate... · 2016. 6. 28. · CAS No Parameter Units LOR 3-Jun-05 3-Jun-05 10-Jun-05 10-Jun-05 9-Jun-05 20-Jun-05 DBP NO