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Acknowledgements
The authors of this report would like to thank all other CSIRO team members who have
provided input into this project: Roger OHalloran, Grace Tjandraatmadja, Michelle Critchley and
Yesim Gozukara.
The project team would like to thank Smart Water Fund and the water companies represented
by this body: City West Water, South East Water, Yarra Valley Water and Melbourne Water
Corporation, for their financial support in this project.
Everwater, Sampford and Sons, and New Water are gratefully acknowledged for providing
technologies to test and the resources to commission them.
CSIRO would also like to thank the EPA (Environment Protection Authority Victoria) and DHS
(Department of Human Services) for their contributions to the development of this protocol,
Ecowise for information on field testing of greywater technologies and other manufacturers who
provided greywater quality data.
Page iii
Executive Summary
This report provides details of a proposed laboratory based greywater technology testing
protocol and details the recommended procedures, methods and analysis techniques for this
process. This is a draft methodology and should be viewed as such, its purpose being a
discussion document to be circulated to regulatory bodies, councils, system manufacturers and
other stakeholders for comment and discussion. The report includes a description of the
protocol as well as details of the processes that were followed during protocol development and
the rationale of decisions and recommendations.
The protocol was developed by testing three small scale greywater treatment systems (Table A
and (Diaper C. and Toifl M. 2006; Diaper C. et al. 2006; Diaper C. and Toifl M. 2007)) which
combined different chemical, physical and biological processes to achieve performance
requirements. The technologies were selected on the basis of these unit processes in order to
ensure the protocol was appropriate for the different process types.
Table A: Technologies tested during protocol development
Technology Process
type
Treatment process
Disinfection
process
Semi batch
UV
Batch
UV
Semi batch
Chemical (Cl/Br)
The testing was undertaken in a PC2 (Physical Containment Level 2) laboratory under
controlled conditions. The following basic equipment was required for testing:
The technologies were fed with a synthetic greywater which mimicked an average combined
laundry and bathroom greywater from an Australian residential dwelling. The components of the
greywater included a range of market share household products, some laboratory grade
chemicals and secondary sewage effluent sourced from a local wastewater treatment plant
(Eastern Treatment Plant, Melbourne). The quality parameter ranges for suspended solids,
biological oxygen demand (BOD), temperature, pH, turbidity, sodium, zinc, total phosphorous
total Kjeldahl nitrogen (TKN), conductivity, chemical oxygen demand (COD), total organic
carbon (TOC), total coliforms and E.coli were selected following review of Australian and
international literature and analysis of data collected from Australian case studies. Whilst
calcium and magnesium were analysed in the synthetic greywater, parameter ranges were not
specified as these will vary and is dependent on mains water quality. Aluminium was also
measured but has no specific parameter range as this will be highly dependent on the
household products used.
Page iv
Tracer study
Chemical testing
Microbiological testing.
The tracer study provided a profile of technology flow conditions and was used to develop flow
and dosing regimes for chemical and microbiological testing. The tracer used in the testing of
the three greywater technologies was sodium chloride, as simple monitoring of outlet
concentrations was possible and the concentrations used did not affect biological treatment.
The parameters selected for chemical testing were based on a literature review of components
of greywater and investigation of greywater components likely to have detrimental impacts on
soils, plant life and other water bodies. The water quality parameters analysed in the feed and
product streams during chemical testing were the same as those for the synthetic greywater
with the addition of nitrate and F.Enterococci, and the exception of temperature. The basic
micro-organism analysis was carried out during chemical testing as secondary effluent was
added to the synthetic greywater and the performance of the technology could be clarified prior
to dosing high micro-organism concentrations.
The purpose of the microbiological testing was to prove a log removal of bacterial, protozoan
and viral surrogates. The micro-organisms selected were in accordance with those suggested in
national water recycling guidelines (Environment Protection and Heritage Council et al. 2006).
During protocol development a helminth surrogate, latex fluorospheres, was trialled but analysis
techniques were time consuming and of limited accuracy, and the proof of log removal was
inconclusive. As helminth ova are unlikely to be prevalent in greywater in Australia it is
recommended this surrogate is rejected as a testing requirement.
The bacterial surrogates used were Escherichia coli (ATCC 25772) and Enterococcus faecalis
(ATCC 19433) as both are recommended strains for use with Colilert tests kits (IDEXX
Laboratories), the selected analysis technique. Inoculum concentrations of > 106 cfu/100mL
were required in order to prove a 7 log removal (minimum detection 100 cfu/100mL).
The viral surrogates selected were the bacteriophages MS-2 and X174, a somatic and an fspecific RNA phage respectively. Although the phages are similar in size (24 and 27 nm
respectively), they have different isoelectric points (X174 pI = 6.6 and MS-2 pI = 3.9) (Dowd
S.E. et al. 1998; Dowd et al. 1998). The reason for basing selection on charge rather than size
was that, for the greywater treatment technologies currently on the market in Australia, removal
at the molecular level will be predominantly influenced by charge rather than size. Product water
samples were assayed for MS2 and X174 phage, either in-house or by a NATA accredited
laboratory, using the ISO standard methods for MS-2 (International Standard Organisation
1995) and X174 (International Standard Organisation 2000). The concentrations of each
phage had to be at least 106 so that log 7 removal could be proven by any system tested.
Clostridium perfringens was selected as the surrogate for Cryptosporidium oocysts. The spores
were prepared from frozen stocks obtained from the culture collection held by the University of
NSW and product samples were analysed using the method described in AS/NZS 4276.17.1
(2000) (Australian Standard 2000). One litre sample volumes were used, as previous work had
indicated that the product samples collected required concentration, rather than the dilution,
described in the standard method. Concentrations of spores in the inoculum were in the range
of 105 to 106 spores/100mL so that 7 log removal could be proven.
Technologies are challenged with repeated high feed concentrations of the different microorganism surrogates, the number of repetitions and product sample analysis dependent on the
technology and the results of the tracer study. Collection of proportional volume feed and
product samples, rather than spot samples, is recommended.
The three stages of testing outlined in the protocol provided:
Page v
As such, the protocol is appropriate for testing technologies for High Exposure Risk end uses,
such as residential dual reticulation, multi-unit dwellings and unrestricted access urban
irrigation, as outlined in the National Water Recycling Guidelines (Environment Protection and
Heritage Council et al. 2006)
Page vi
Table of Contents
Introduction .............................................................................................................. 1
1. Rationale............................................................................................................ 2
2. Experimental set up.......................................................................................... 5
System requirements............................................................................................................ 5
3.
Synthetic greywater.......................................................................................... 7
3.1.
3.2.
3.3.
4.
5.
6.
Method .................................................................................................................... 13
Results .................................................................................................................... 14
Microbiological testing................................................................................... 16
6.1.
6.2.
6.3.
6.4.
6.5.
7.
8.
9.
Recipe....................................................................................................................... 7
Procedure ................................................................................................................. 7
Quality....................................................................................................................... 9
Reporting......................................................................................................... 20
Discussion and recommendations ............................................................... 21
Future work ..................................................................................................... 23
TABLES
Table 1: Summary of technologies tested during protocol development ......................................3
Table 2: Final synthetic greywater recipe (formulation 4) .............................................................8
Table 3: Parameter ranges and quality of synthetic greywater ...................................................10
Table 4: NATA laboratory results of chemical and bacterial testing ...........................................14
Table 5: Example results of micro-organism log removal for Technology C...............................19
Table 6: Example of HAZOP assessment method .....................................................................23
Table 7: Synthetic greywater parameter ranges compared to Australian greywater data ..........31
Table 8: Australian greywater quality data..................................................................................32
Page vii
FIGURES
Figure 1: Technologies tested during protocol development (L to R, Technology A, B and C) ....6
Figure 2: Schematic of the system layout .....................................................................................6
Figure 3: Tracer study outlet Electrical conductivity Technology A..........................................12
Figure 4: Tracer study outlet Electrical conductivity Technology C .........................................12
Page viii
Introduction
The first section of this report introduces the background to the project and the reasons for
and the requirements of the greywater testing protocol development in the Rationale (Section
1). The experimental set up is then described, providing details of equipment and facilities
used in the testing of three greywater treatment technologies (Section 2).
The synthetic greywater recipe is then described, with details of component contributions,
procedures for the generation of synthetic greywater and the results of water quality analysis
of large scale batches of greywater (Section 3).
The next three sections describe the testing protocol and its components. The testing
protocol comprised of three analytic processes:
Tracer study
Chemical testing
Microbiological testing.
Section 4 describes the tracer study testing that was required for each technology prior to
starting performance testing. The tracer study was required in order to understand the flow
profiles of the technology being testing and to develop the subsequent chemical and
microbiological testing regimes.
The chemical testing requirements are then described (Section 5), followed by experimental
details of the microbiological dosing with Escherichia coli and Enterococcus faecalis, MS2
and X174 coliphages and protozoa surrogates (Section 6).
Section 7 outlines possible reporting requirements for the testing of greywater systems,
developed from the summary reports of the three technologies tested during the
development of the protocol.
Section 8 provides recommendations for the future development of the protocol to a national
standard. Section 9 describes a proposed desk-based risk assessment to be carried out in
conjunction with the laboratory based testing which will provide a more complete assessment
of technologies under a range of operating conditions.
1. Rationale
The aim of this project was to develop a practical, robust and reproducible method for testing
greywater treatment technologies to Australian recycled water standards, proving log
removal of bacteria, virus, protozoa and helminth surrogates. There is no standard national
testing method for greywater technologies in Australia and the research undertaken aids in
the development of appropriate protocols and procedures for different scales of treatment
and end uses of greywater. The processes used are in line with the risk assessment
approach of the National Water Recycling Guidelines (Environment Protection and Heritage
Council et al. 2006). The work was funded by Smart Water Fund and CSIRO Water for a
Healthy Country Flagship.
There is currently much focus, both nationally and internationally, on water saving measures,
better management of water supplies and implementation of policies to reduce wastewater
discharges to receiving waters. The use of alternative source waters, such as greywater, is
being investigated and there are a wide range of technologies commercially available for
greywater treatment. In Australia, numerous strategies that include greywater treatment
systems for water recycling in the home are being supported by government agencies
(Victorian Government Department of Sustainability and Environment 2004; New South
Wales Government 2006). This has led to an increased interest in developing new greywater
recycling technologies.
Despite the perceived innocuous nature of greywater, it can contain enteric bacteria, viruses
and intestinal parasites which may be pathogenic (Casanova et al. 2001; Birks and Hills
2007; Winward et al. 2007). Previous studies have found increased risks to human health
from viral, but not bacterial, pathogens when using greywater for accidental direct contact,
sportsfield irrigation and groundwater recharge with greywater (Ottoson and Stenstroem
2003). However, before widespread adoption of domestic greywater systems is approved, it
is essential that thorough, robust and reproducible testing procedures are developed in order
to ensure that there is no increase in human health risk.
In Australia, there are no national guidelines for testing of household greywater systems, and
different states have different protocols and procedures for testing. At the single household
scale there are prescriptive standards for technology accreditation (New South Wales Health
Department 2005). It is often recommended that the accreditation be used in conjunction with
guidance documents for greywater use in single household residential premises (New South
Wales Department of Energy Utilities and Sustainability 2007). The NSW single household
domestic greywater accreditation is based on a 26 week field monitoring period of greywater
treatment systems in a household of eight to ten people (or 720 to 900 L/day greywater flow)
and includes thermotolerant coliform (TC), Biological Oxygen Demand (BOD5), suspended
solids (SS), free chlorine, total Kjeldahl nitrogen (TKN), total nitrogen (TN) and total
phosphorus (TP) analysis. However, there is currently no recommended testing for
pathogenic micro-organisms.
For multi-dwelling premises, guidance (New South Water Health 2005) is in the form of a
framework for the assessment of recycled water schemes, and is not prescriptive in testing
requirements (New South Wales Department of Water and Energy 2007). The NSW
guideline recommends validation, verification and operational monitoring requirements based
on the exposure risk level of the end use of the recycled water. Monitoring is recommended
for the highest exposure risk level (for internal use and unrestricted irrigation) of BOD5; pH;
SS; turbidity; free chlorine (or other disinfection system efficiency); and the micro-organisms
E.coli, coliphages and Clostridia.
The monitoring programs suggested for both single residential and multi-dwelling premises
do not necessarily validate the performance of the technology for pathogen removal. The
recommended field testing will not necessarily challenge the technology with high
concentrations of pathogenic micro-organisms in the feed stream, therefore maximum log
removal cannot be assessed.
In order to address this potential issue of system performance validation and to enable a
wide range of likely conditions to be assessed, the approach taken in this study was to use a
laboratory based testing process rather than field tests, to validate the performance of
greywater treatment technologies. Three different greywater treatment technologies were
used in the development of the protocol. Technologies were selected based on their method
of processing: one semi-batch biological and UV disinfection process, a batch chemical and
physical separation process with UV disinfection and a semi-batch biological process with
chemical disinfection (Table 1). This range of process types allowed investigation of the
appropriateness of selected surrogate micro-organisms and the suitability of the protocol to
different process types.
Table 1: Summary of technologies tested during protocol development
Technology Process
type
Treatment process
Disinfection
process
Maximum Flow
rate (L/day)
Semi
batch
UV
600
Batch
UV
1000
Semi
batch
Chemical
(Cl/Br)
300
Victorian EPA, DHS and Smart Water Fund. The use of surrogate organisms had the
advantage of reduced Occupational Health and Safety requirements compared with the use
of viable pathogens. This means testing facilities did not have to comply with high levels of
microbiological containment and allowed simpler, more easily transferable testing methods to
be developed. Development of a robust and reproducible testing protocol will depend on the
ease of use and quantification of the microbial species and surrogates used. Surrogates
have been used in previous studies with greywater (Rose et al. 1991; Ottoson and
Stenstroem 2003).
The test method was developed as a three-stage process: tracer study testing, chemical
testing and microbiological testing. The tracer study allowed assessment of the hydraulic
integrity of the technology and provided the basis for flow, inoculum dosing and sample
collection frequency requirements of the chemical or microbiological testing. The chemical
testing included a range of physical, chemical and microbiological parameters which
provided an indication of potential environmental and human health risks, as well as an
assessment of system operational performance. The microbiological testing was designed to
prove compliance with the log removal requirements for the selected surrogates
recommended in recycled water guidelines (Environment Protection and Heritage Council et
al. 2006). This three-stage approach allowed verification of system performance prior to the
more complex and costly microbiological testing.
2. Experimental set up
System requirements
The basic testing system components were (Figure 2):
Feed tank
Online monitoring of pH, conductivity and turbidity were suggested in order to allow
continuous monitoring of synthetic greywater feed. However, spot samples could be taken
and analysed to ensure consistency in feed quality.
The micro-organisms used for testing the greywater technologies are listed as Class 2 in the
AS/NZ Standard 2243.3:2002, Safety in laboratories - Microbiological aspects and
containment facilities and a PC2 (Physical Containment Level 2) facility was required for the
testing process.
For the development of the synthetic greywater and testing of three greywater treatment
technologies used to develop and validate the protocol, a 1000 L custom built feed tank was
used. A tank of this volume was required so large scale batches of the greywater could be
produced and tested. A submersible pump (a Grundfos AP12 40 04A1V with vortex impellor
was used in this study) in the feed tank was used to continually mix the synthetic greywater
for a minimum nine hour period prior to use. A T-piece pipe was connected to the outlet of
the pump in order to ensure flows were tangential to the walls of the tank to aid in surface
scouring and reduce foam generation. Mixing of the greywater prior to use increased the
temperature of the greywater and lowered the pH to the required parameter range (Table 3,
Section 3.3)
The flow of the greywater feed to the technology was monitored using a rotameter or an
online mag-flow meter (a Turbo KP-G polypropylene lined meter was used in this study).
Flows were adjusted using two valves and a recycling loop back to the feed tanks. The feed
pump used in this study was a Davey M3061-0 with Torrium priming and a maximum flow of
5000 l/hr and 69 m maximum head. Volumes of synthetic greywater fed to the technology
during testing were monitored via a simple level measurement of the feed tank and
crosschecked with the rotameter or flowmeter. Temperature, pH, conductivity and turbidity
were monitored online prior to a sampling point, installed between the feed tank and the
technology.
The three technologies (Figure 1) were installed by manufacturers and distributors and were
tested as installed. Any operational or maintenance issues during the testing were addressed
by the manufacturer.
Product samples were taken as spot samples or as a proportion of the total outlet flow,
depending on the technology. A peristaltic pump was used for taking the proportional
samples. This is the recommended method for sample collection, providing details of outlet
flow are available and outlet flows are relatively constant.
One technology tested had a final product storage tank as an integral component of the
technology (Figure 1, Technology A). (It is recommended that product samples are taken
prior to any final storage of treated greywater in order to test technology performance, rather
than the effect of storage, on treated greywater.)
Clay,
effluent and
microorganism
dosing point
using dosing
pump
Mixing tank
(1000 L)
Online
monitoring of
pH, conductivity,
temperature
Feed
pump
Sampling
point
Submersible
mixing pump
Rotameter
or flow
meter
Technology to
be tested or
holding tank
3. Synthetic greywater
The synthetic greywater formulation was a modified version of a recipe developed and used
for testing greywater systems in the UK (Brown R. and Palmer A. 2002). The composition of
greywater has been found to vary significantly between countries and regions (Siegrist R.L.
et al. 1976; Brandes 1978; Walpole and Hartley 1993; Eriksson et al. 2002). There are a
number of reasons for this variability: use of different household products (and the different
composition of products); varying tap water qualities and water usages; different householder
behaviours; and the inclusion or exclusion of various waste streams in the greywater, laundry
only, bathroom only or laundry and bathroom combined. These factors suggest that careful
consideration needs to be given before using a formulation that has been developed in
another country or region.
There were a number of requirements for synthetic greywater formulation for technology
testing:
Be reproducible and provide consistent quality between batches and between users.
3.1. Recipe
To meet the above requirements the formulation developed contained products expected to
be found in average Australian households, including personal care products and detergents
and additional laboratory chemicals in order to achieve the concentration ranges of various
parameters as required. Market share products were used where data was available
(Appendix 1 Synthetic greywater components). Estimations of amount of products used
were made and combined with average water usage data in order to calculate the amount of
product to be used in the recipe (Appendix 2).
3.2. Procedure
To prepare the synthetic greywater all ingredients, except the clay and secondary effluent,
were weighed and mixed with 500 mL warm water in a blender at low speed for one minute.
The quantities given in the table below are for 100 L of greywater. The feed tank was filled
with the required amount of tap water and the concentrated ingredient mixture added. A
submersible pump in the feed tank was used to mix the greywater overnight or for at least
nine hours. Mixing the greywater for at least nine hours was found to decrease the pH into
the correct range (Table 2) and also brought the temperature of the greywater into the
desired range of 25-35C. The outlet of the pump in the feed tank required some modification
to direct the outlet towards the feed tank walls to reduce entrainment of air and foaming in
the feed tank.
Product used
Sunscreen
1.5
UV TripleGuard
Moisturiser
Dove
Toothpaste
3.25
Deodorant
Mum
Na2SO4
3.5
Analytical grade
NaHCO3
2.5
Analytical grade
Na2PO4
3.9
Analytical grade
Clay (Unimin)1
Industrial grade
Vegetable Oil
0.7
Shampoo/hand wash
72
Palmolive
Laundry
15
Boric acid2
0.14
Analytical grade
Lactic acid
2.8
Analytical grade
Secondary effluent3
2L
OR
Secondary effluent was stored (< 4C) and used within 2 weeks of collection
The clay and secondary effluent were mixed together and stirred using a magnetic stirrer for
at least 15 mins prior to and during feed of the greywater technology. The clay and
secondary effluent mixture was added inline via a peristaltic pump, as adding clay to the
feed tank increased adhesion of clay to the feed tanks walls and fitting. Any micro-organism
inocula (bacteria, virus, protozoa and helminth surrogates) used for testing the greywater
technologies were also added to the effluent and clay prior to dosing. Secondary effluent was
allowed to reach room temperature prior to dosing or addition of microbial inocula in order to
reduce the potential for damage to the micro-organisms due to a rapid change in
temperature.
This mix of freely suspended micro-organisms and micro-organisms associated with
particulate material provided an assumed worst case scenario for testing; the microorganisms not bound to particulate being the smallest and more likely to pass through
filtration process, the bound micro-organisms being shielded from chemical and physical
disinfection process if they are not removed by filtration. Further analysis of the ratio of
Greywater Technology Testing Protocol
3.3. Quality
Table 3 shows the expected water quality parameter ranges for the synthetic greywater
produced using the recipe given in Table 2. The target parameter ranges (Table 3) used for
the synthetic greywater formulation were based primarily on Australian greywater quality
data. Initially data from the Smart Water Fund Testing Protocol for proposed technologies
treating greywater was used to set parameter ranges (source data from (Jeppesen 1996))
but there were limitations in using this data, primarily that it was over ten years old. Thus, the
data sources were extended to other current Australian data collected from system
technology manufacturers and Ecowise (Appendix 4) and international literature (Eriksson et
al. 2002). Following this review, the median of the parameters ranges for BOD, turbidity,
sodium and conductivity were reduced. Further investigation of total-N and total-P ranges is
required as the median and averages for the current data analysed were significantly
different from the initial parameter ranges suggested by Smart Water Fund (see Appendix 4).
The results of the analysis of initial large scale batch testing showed that several parameters
were outside of the desired range. Several new ingredients were added and the quantities of
some of the existing ingredients in the recipe were adjusted on subsequent batches until the
results from the final large scale batch testing showed that the chemical and physical
parameters were all within the expected range (Table 3). The adjustments to the recipe are
shown in Appendix 5 and the results of the corresponding large scale batches are shown in
Appendix 6. The chemical components of the recipe were found to be reproducible between
batches, with the results in Table 3 showing the average and standard deviation for the final
formulation (presented in Table 2). Results are an average of five batches for the
formulation.
The microbiological parameters were more difficult to adjust and were largely dependent on
the concentration of micro-organisms present in the secondary treated effluent, which can
vary. Whilst the E.coli concentrations were in the desired range, the total coliform
concentration was 103 times the desired range. Coliforms are abundant in the environment
and are commonly found in the faeces of warm blooded animals, in aquatic environments, in
soil and on vegetation. This abundance of coliforms in the environment may account for the
higher than expected levels of total coliforms in the synthetic greywater.
Updated range
Appendix 3 (mg/L
unless otherwise stated)
Suspended solids
60 - 80
60 - 80
59.0 3.3
BOD
150 - 200
130 - 180
146.7 5.0
Temperature
20 - 30C
25 - 35C
pH
6.5 8.0
6.5 8.0
7.4 0.1
Turbidity
60 80 NTU
50 70 NTU
52.1 4.6
Boron
0.1 0.5
0.1 0.5
Sodium
80 130
50 90
65.3 1.0
Calcium
7.6 0.3
Magnesium
1.3 0.1
Aluminium
Zinc
0.1 0.5
0.1 0.5
Total phosphorous-P
10 20
10 20
17.8 0.4
3.0 5.0
3.0 5.0
3.0 0.1
Parameter
1.6 0.4
Nitrate
<0.2
Nitrite
<0.003
Conductivity (S/cm)
450 - 550
300 - 400
322.2 6.7
COD
250 - 400
250 - 400
276.7 21.0
TOC
50 - 150
50 - 150
62.6 12.7
Total coliforms
(cfu/100mL)
10 10
E.coli (cfu/100mL)
101 - 102
F.Enterococci
(cfu/100mL)
106 107
102 103
102 103
10 10
1-100
10
4. Tracer study
A tracer study was used to determine the profile of flow for each technology prior to
commencing chemical and microbiological testing. The choice of tracer was discussed with
the technology manufacturers prior to commencing the tracer studies to ensure that it would
not interfere with the process of the technology or damage any media or bacterial growth on
any media utilised. The tracer selected for the three technologies tested during the
development of the protocol was sodium chloride.
Initially, the sampling and run-time procedures of the testing protocol were to be based on
the theoretical hydraulic retention time (HRT), S (where S= VT/Q, and VT is the total volume
of greywater storage within a technology and Q is the rate of feed to the technology).
However, the different types of treatment technology to be tested used numerous filtration
and media types, which made estimation of greywater storage volume difficult and so the
tracer study technique was utilised.
The tracer studies were carried out by adding a salt dose to the first batch of water fed to the
technology and then feeding further batches of clean water until the conductivity at the outlet
of technology returned to background levels. The sodium chloride concentrations used did
not affect the treatment processes and conductivity probes were used to continuously
monitor and record the effluent during the tracer study. Other tracers could be used, such as
Rhodamine B, if there were concerns regarding the effects on the process.
The results of two technology tracer studies are presented in order to demonstrate the use of
the method in developing sampling and run time protocols. Figure 3 shows tracer study
testing results from Technology A, the semi-batch process greywater treatment technology,
to which one 150 L batch of high salt content feed was added. The technology was then fed
with ten subsequent 150 L batches of potable water per day over a period of three days. The
technology maximum daily flow rate was stated as 600 L/day (N.B. The constant conductivity
readings observed between the first and second and the second and third days are due to
the technology being shut down overnight.
The results show conductivity breakthrough observed at outlet at ~ 6 hours, during the
second feed batch of potable water to the technology. The maximum concentration at the
outlet was observed after 9.5 hours, or an additional batch time. This information was then
used to determine the feed inoculum and product sample collection to be used when testing
the performance of the technology in the removal of micro-organisms. From examining the
tracer study outlet profile the proposed microorganism test method for this first technology
was:
Feed high inoculum dose until the tracer study peak product concentration is achieved
i.e. feed high inoculum dose for three 150 L batches
Continue to analyse product samples until the tracer study concentration returns to
background levels i.e. collect product samples for a minimum of ten 150 L greywater
batches
Operating the testing in this manner aids in proof of log removal during testing and ensures
that all potentially contaminated product is analysed. Further statistical analysis of the
number of samples and replicates is required to ensure the testing regime demonstrates log
removal.
The results of a salt tracer study for Technology C, operating on a batch cycle, is shown in
Figure 4. The design of this technology was such that there was a small residual storage at
the end of processing, therefore the conductivity does not return to zero after the first batch.
After three consecutive salt-free feeds, the conductivity of product returns to background
levels.
11
1200
Unit on
standby
overnight
Feed 3
Conductivity (S/cm)
1000
Feed 4
800
Feed 6
Feed 5
600
400
Feed 7
Unit on
standby
overnight
Feed 1
Feed 10
Feed 11
Feed 12
200
Feed 8
Feed 9
Feed 2
0
0.00
12.00
24.00
36.00
48.00
60.00
Time (hours)
Figure 3: Tracer study outlet Electrical conductivity Technology A
1400
1200
Feed 1 - 100
Feed 2 - 100
Feed 3 - 100
1000
800
600
400
200
0
0
10
12
14
16
18
20
Time (hours)
When testing this system for removal of micro-organisms, inoculum was dosed for three feed
cycles and product was collected for a total of six feed cycles (twice the number observed for
the tracer study outlet concentration to return to background levels). This was done to ensure
any micro-organisms that may be entrained in the technology media would be detected and
was a different rationale to that used for the first technology.
12
5. Chemical testing
5.1 Method
Chemical components analysed for all of the technologies tested are shown in Table 4. The
parameters were selected based on a literature review of components of greywater and
investigation of greywater components likely to have detrimental impacts on soils, plant life
and other water bodies (Jeppesen 1996). The soil type to which the greywater is applied will
have an effect on the impacts of different chemical constituents. In general, clayey soils are
more affected by high salinity, sodicity and metals, and there is the possibility of
eutrophication of surface waters. On the other hand, in sandy soils all these parameters are
more likely to affect the groundwater.
Analysis of suspended solids was carried out as part of the chemical testing for each
technology as it provided an indication of the propensity of the treated greywater to cause
physical blockage of soil pores or blockage of irrigation systems. Turbidity was also
measured, as this is an easy way to measure indicators of colloidal and suspended residual
material, and provides a quick check of technology performance.
The electrical conductivity was measured as a surrogate measure for total dissolved solids,
which provides a measure of the dissolved salt content or salinity. Salinity will effect both
plant growth and soil structure. pH can also impact plant growth and soil structure and also
provides an easy check that a technology is operating correctly.
The total organic carbon (TOC), chemical oxygen demand (COD) and biological oxygen
demand (BOD5) were included as they provide a good surrogate measurement of biologically
degradable, organic and non biologically degradable components.
Total phosphorous and total nitrogen were analysed during testing as these parameters
provide a measure of the nutrient content of the treated water. Both nitrogen and
phosphorous are required for plant growth but can cause detrimental effects to both plants
and open water bodies if present in excessive quantities. In addition, both parameters
provide an indication of the propensity for biological regrowth in the treated water. Nitrate
was also measured as this provides an indication of technology performance. The
measurement of calcium and magnesium in conjunction with nitrogen and phosphorous will
give an indication of the potential benefits of greywater use to plant growth.
Testing for calcium, magnesium and sodium was undertaken in order to obtain a value for
sodium adsorption ratio (SAR), an indicator used to assess the impacts of treated water on
soil infiltration. Zinc was also included as levels approaching or above the guideline values
for irrigation have been found in greywater (Christova-Boal, 1996; Hypes, 1974). Aluminium
is often present in personal care products so was also included in the testing.
Total coliforms, E.coli and F.Enterococci, were also monitored during chemical testing, as
secondary effluent was added to the feed. This gave a preliminary indication of technology
performance for bacteria removal and ensured the technology was operating correctly.
13
Chlorine and bromine residual analysis was undertaken in-house where necessary.
Transport times to the external laboratory made NATA testing of chlorine and bromine
impracticable. Results are not reported here as they are not NATA accredited, but the
inclusion of these parameters for analysis when the tested technology utilises chemical
disinfection, is recommended.
5.2 Results
Testing for chemical and physical parameters was carried out for each technology on the
feed and product water and included suspended solids, biological oxygen demand (BOD),
conductivity, pH and turbidity (see Table 4 for full list). The samples were analysed by a
NATA accredited laboratory. The pH, conductivity, temperature and turbidity of the greywater
feed were also monitored throughout all trials using on-line probes. Boron was included in
initial analysis as it may be present in laundry detergents and is known to have acute toxicity
to plants. Boron concentrations found in greywater (Friedler 2004) are often above the
recommended maximum value for irrigation waters (Environmental Protection Authority
Victoria 1991). However, the boron analysis method selected by the laboratory employed to
carry out the sample analysis was not particularly sensitive and was not able to detect levels
below 1.2 ppm. As the levels of boron in the greywater were below this limit they were not
detected and therefore results for boron are not available.
Table 4: NATA laboratory results of chemical and bacterial testing
Parameter
Units
Average product
(mg/L)
<5
Max
product
13
% Removal
(mg/L)
Average feed
(mg/L)
105.0
BOD
Suspended Solids
(mg/L)
67.0
3.2
95
COD
(mg/L)
238
104
190
56
TKN
(mg/L)
5.2
5.51
11
Nitrate
(mg/L)
0.2
0.43
Total P
(mg/L)
16.9
16.6
18
TOC
(mg/L)
43
29
50
33
Conductivity
(uS/cm)
324
339
350
7.1
6.7
6.8
pH
>95
Turbidity
(NTU)
46.1
10.7
18
77
Total coliforms
(cfu/100mL)
>2419.6
E.coli
(cfu/100mL)
67
F.Enterococci
(cfu/100mL)
850
Calcium
(mg/L)
7.4
6.82
7.9
Magnesium
(mg/L)
1.4
1.5
1.7
Sodium
(mg/L)
64
67
68
Zinc
(mg/L)
0.02
0.07
0.14
Aluminium
(mg/L)
1.5
0.48
1.4
57
*increase observed
14
The results presented in Table 4 are for the semi-batch Technology C, a biological process
with fixed media and chemical disinfection. Results show average feed and product
concentrations and the maximum observed value in all product samples. The technology
removed a high percentage of BOD and SS and all bacterial sampling found no detectable
micro-organisms in the product sample. Full details of the results for the three technologies
tested can be found in the Technology Testing Reports (Diaper and Toifl 2006; Diaper et al.
2006; Diaper and Toifl 2007). Statistical analysis of the results requires further discussion.
15
6 Microbiological testing
During the microbiological testing of each technology, random samples of product water
were analysed in house for pH and turbidity to provide a quick check of technology
performance. Should these parameters be outside the expected range, further chemical
testing is recommended in order to assess whether the technology is operating correctly.
Should the chemical analysis prove the technology is not operating correctly, it is
recommended that microbiological testing is suspended.
16
cfu/100mL were required in order to prove a 7 log removal (minimum detection 100
cfu/100mL).
For dosing a greywater technology, 75 mL each of E. Coli and E. faecalis inocula was mixed
with secondary treated effluent and clay, and then added to the greywater feed using a
dosing pump (a Prominent gamma/4-W was used in this study). The amount of effluent
dosed with each feed was 1% of the volume of greywater fed each time (e.g. 1 L of
secondary treated effluent with 100 L of greywater). Feed volumes varied between 100 L and
225 L depending on the feed volume for each technology. Feed samples were taken as a
proportion of the total inlet flow from the sample point prior to the technology. The number of
feeds for which bacteria were dosed was determined by the results of the tracer study for
each technology.
Product samples were taken after processing by the technology and analysed for E Coli and
E. faecalis using Colilert and Enterolert Quantitray analysis.
17
Organisation 2000) was carried out to ensure that the concentration range was correct prior
to dosing. The concentrations of each phage had to be at least 106 so that log 7 removal
could be proven by any system tested.
Phage dosing was carried out in the same way as the bacteria dosing using 75 mL of each
phage mixed with secondary treated effluent and clay, then dosed to the technology via
dosing pump for the duration of the feed. The amount of effluent dosed with each feed was
1% of the volume of greywater fed.
Product water samples were assayed for MS2 and X174 phage either in house or by a
NATA accredited laboratory. In house analysis used the ISO standard methods for MS-2
(International Standard Organisation 1995) and X174 (International Standard Organisation
2000).
18
and some methodologies changed throughout the development of the protocol, the direct
comparison of technology is not meaningful at this stage.
The results for the fluorospheres were the same for all technologies, with no fluorospheres
being detected in any product samples and all technologies providing a log 4 removal. The
visual fluorescence detection method used for analysis of samples was problematic as it was
difficult to see the fluorospheres in samples where the product water was turbid. Additionally,
large volumes of samples needed to be processed in order to determine that no
fluorospheres could be detected which was difficult for the turbid samples as the filters
became blocked very quickly. Further method calibration would be required in order to
validate the procedure if helminth testing were included.
However, it is recommended that a helminth surrogate is NOT incorporated in any future
testing protocol because:
C.perfringens spores are 1-3 m (Lovins W.A. et al. 2002) and, if size exclusion is the
expected removal method, will provide a worst case compared to 90 m fluorospheres.
Table 5: Example results of micro-organism log removal for Technology C
Microorganism or
surrogate
Technology C
(Biological + Chemical
disinfection)
E. coli
>7
Faecal enterococci
>7
Bacteriophage MS-2
Coliphage X174
C. perfringens spores
Fluorospheres
19
7. Reporting
The reports from the three technologies tested are available on the Smart Water Fund
website (www.smartwater.com.au). The report contents are similar for all technologies and
incorporate a Protocol and methodology refinements section in addition to the description
and results from the technology testing. If this testing protocol is to be developed as a
national standard, reporting requirements will need to be specified. A suggested report
template is provided below. Incorporation of feedback and comment from regulatory
authorities is required to progress and finalise these reporting requirements.
System operation
o
Tracer study
Chemical testing
Results
Comment
Micro-biological testing
o
Bacteria
Results
Phages
Results
Clostridium perfringens
Results
20
Should the chemical analysis prove the technology is not operating correctly, it is
recommended that microbiological testing is suspended
Boron analysis is not included in the feed or product analysis following further
investigation of its likely presence in greywater. The concentrations of boron in greywater
would need to be confirmed by sending samples to a laboratory that has a very low limit
of detection.
When dosing micro-organism inocula, secondary effluent is not added to the synthetic
greywater, due to the potential competition between organisms in the effluent and
inocula, which could lower the number of organisms present.
Another recommendation for the testing protocol is that the feed sample point is located
closer to the technology (current setup has 4-5 m of pipework and flowmeter prior to
technology). Micro-organisms can attach to particulate material and particulate material can
settle or adhere to feed pipework and so there may be some removal of micro-organisms in
the pipework prior to the technology. Locating the sample point as close to the technology as
practically possible will allow these effects to be taken into consideration.
Furthermore, there are some requirements for additional research work which will ensure the
protocol is robust, reliable and applicable to a range of technologies. Suggested additional
work includes:
Investigation of the use of other viral surrogates for other technology types which may be
based primarily on size exclusion. The surrogate selection for these trials was based on
the charge of the surrogates rather than size as this was more relevant for the
technologies that we were investigating. However for a membrane based technology, for
example, surrogates based on size would be more appropriate.
Investigate the use of other tracers, such as Rhodamine B, if there are concerns
regarding the effects of sodium chloride on the greywater treatment process.
21
Further investigation of Total-N and Total-P ranges is required as the median and
averages for the current data analysed, were significantly different from the initial
parameter ranges suggested by Smart Water Fund. The original parameter ranges
suggested by SWF (1996) showed Total-P levels in greywater are greater than Total-N
levels. However, data collected recently from industry sources and some literature
suggests that P levels are actually lower than N levels in the greywater. This could be
due to changes in detergent formulations with many manufacturers beginning to produce
low phosphate detergents to be more environmentally friendly.
22
9. Future work
The proposed testing protocol outlined in this document does not provide a complete
assessment of technology performance and it is recommended that this protocol is combined
with a desk-based risk assessment and field testing. In field situations, greywater treatment
systems will operate long term and be subject to large variations in greywater quantity and
quality and particular householder behaviours. In the laboratory based testing protocol, these
issues are not assessed and a structured risk-based assessment is recommended in order to
understand the likely impacts of these variations.
Preliminary development of the desk-based risk assessment has been undertaken and a
Hazard and Operability (HAZOP) (Kletz 1999) type approach is recommended. This
approach requires an understanding of the possible causes of failure of the technology and
an assessment of their frequency and consequences. As such, the assessment team should
be multi-disciplinary in order to provide expertise in all potential health and environmental
risks and include someone with knowledge and expertise in system operation (often the
technology manufacturer).
The HAZOP process requires that the system be assessed component by component and
utilises keywords, such as NO, LESS and MORE to assess the impact of variations in
system operation on each component. These keywords are used to identify causes and
consequences for each deviation from normal operation. A quantitative scale can then be
used to rank the consequences i.e. Major (3), Moderate (2) and Minor (1), and the
frequencies of the causes i.e. Almost certain (3), Likely (2) and Unlikely (1) (highlighted in
yellow in Table 6). High, medium and low risks can then be identified and appropriate
controls can be suggested for high/medium risks if required i.e. frequency x consequence
score 6 (highlighted in red in Table 6).
Table 6: Example of HAZOP assessment method
Deviation
Potential
causes
Consequences
No flow into
system for
extended period
Normal
operation i.e.
Holidays (3)
Nuisance odours as
untreated greywater
stored in tank (2)
(6)
Redesign system
to allow complete
emptying of tanks
Blockage in
collection
pipework (1)
No drainage of greywater
from supply point (2)
(2)
None
(2)
None
(6)
No level sensing
Incorrect
installation (2)
This assessment method is not yet fully developed for specific application to greywater
technologies and further definition of keywords and deviations is required to ensure the
Greywater Technology Testing Protocol
23
24
Anionic and non-ionic surfactants (Commonly used are alcohol ethoxylates and alkyl
phenol ethoxylates)
Optical brightener/fluorescer
Enzyme (commonly used is proteinase)
Alkalis
Sodium polyphosphate
Zeolite (synthetic ion-exchanging zeolites are commonly used)
Polymer
25
Perfume
Colour.
Palmolive Soft Wash Milk and Honey 500 mL, made in Thailand (Customer info: 1800 802
307)
Ingredients as per package:
Water
Sodium Laureth sulphate
Cocamidopropylbetaine
Cocaminde DEA
Lauryl glucoside
Polyquaternium 7
Fragrance
Glycol distearate
Laureth-4
Sodium chloride
Sodium sulphate
Citric acid
Poloxamer 124
Sodium styrene/acrylates copolymer
DMDM Hydantoin
Methylchloroisothiazolinone
Methylisothiazolinone
Tetrasodium EDTA
Honey
Dry milk powder
Ci 19140
Ci 16035.
Anti-perspirant Mum Dry Active, 24h by Procter and Gamble (Customer info: 1800 226 524)
Active ingredients as per package:
Binders
pH agents.
26
Toothpaste Colgate Maximum Cavity Protection, regular flavour, 140 g by Colgate (Customer
info: Colgate Oral Care 1800 802 307)
Active ingredients as per package:
Abrasives: used to provide cleaning power, common compounds used are calcium
carbonate, silica, calcium phosphate, and alumina.
Detergents: used to create the foaming action and keep it from dribbling. The most
common detergent is sodium lauryl sulphate.
Humectants: to provide texture and retain moisture. Common humectants are Glycerin,
sorbitol, and water. Xylitol is a superior humectant but not commonly used.
Thickeners: Common thickeners are Carrageenan, cellulose gum and xanthan gum.
Preservatives: used to prevent growth of microorganisms in toothpaste. Common
examples are sodium benzoate, methyl paraben, triclosan and ethyl paraben. Common
preservatives include sodium benzoate, methyl paraben, and ethyl paraben.
Flavouring agents: Used to improve the taste of toothpaste. Most toothpaste sweeteners
are artificial and contribute very little to cavity formation. A common sweetener used is
Saccharin.
Colouring agents: used to improve the appearance of toothpaste. Artificial dyes are used
to colour red, green, and blue toothpastes. Titanium dioxide is used to make some
toothpastes white.
Tartar control: toothpaste that are designed for tartar control commonly contain
pyrophosphate.
27
Also contains:
Methylparaben
Propylparaben
Phenoxyethanol
Iodopropynyl butylcarbamate
Fragrance.
28
29
30
Original
range
Suspended
solids (mg/L)
60 - 80
Updated range
(mg/L unless
otherwise stated)
60 - 80
BOD (mg/L)
150 - 200
130 - 180
172
109
Turbidity (NTU)
60 80
50 70
52
43.6
Sodium (mg/L)
80 130
50 90
96
73
Total
phosphorous
P (mg/L)
10 20
10 20
5.9
3.12
Total Kjeldahl
nitrogen N
(mg/L)
3.0 5.0
3.0 5.0
11.1
11.6
Conductivity
(S/cm)
450 - 550
300 - 400
361
290
Total coliforms
(cfu/100mL)
103 104
103 104
68200
23500
201
202
Faecal coliforms
(cfu/100mL)
Average of collected
data
Median of collected
data
76
45.5
31
Comments
BOD
SS
Median
97
48
130
43
TKN
Total - N
Turbidity
EC
6.6
3.5
3.5
TP
0.7
82
290
144
39
43.6
332
Average 5 to 10
samples
Median
34
33.8
189
52.5
79.5
14
15
2.75
Median
180
73.5
9.1
9.1
3.5
Laundry only
Max and min
only
Sullage
Median
787
100.6
159
210
113
335
11.6
12.6
Average
Average
Average
Median
57
68.5
109.25
38
25
21.5
90
23
5.53
15.53
21.67
6.6
5.57
15.53
21.67
AVERAGE
MEDIAN
172
109.25
76
45.5
11.1
11.6
10.3
9.1
385
1.5
170
1.35
1037
21.5
177.9
601
8.1
73
21.5
103.5
10.13
10.2
10.37
0.28
52
43.6
361
290
5.9
3.125
51.4
11.9
100
180000
100
202
33.8
4.25
FC
>2000
39
Average
TC
0.14
Average 5 to 10
samples
Average 9 to 15
samples
Average
Na
38
988
300
<1
23500
96
73
68163
23500
201
202
32
Product used
Formulation 1
Formulation 2
Formulation 3
Sunscreen
UV triplegaurd
1.5
1.5
1.5
Toothpaste
Colgate
3.25
3.25
3.25
Deoderant
Mum
0.5
1.0
1.0
Na2SO4
Analytical Grade
3.5
3.5
Unimin Clay
Industrial Grade
5.0
5.0
1 ml
Urine
Vegetable Oil
0.7
0.7
0.7
Shampoo
Palmolive
72
72
72
Laundry
Detergent
Omo High
Performance/
Omomatic
concentrate
15
15
15
Antifoam
Silfoam SEA39
1.5
As required
Secondary
Effluent
Carrum STP
1L
1L
1L
Boric Acid
Analytical grade
0.14
0.14
Urea
Analytical Grade
0.5
0.5
NAHCO3
Analytical Grade
2.5
2.5
Na2PO4
Analytical grade
3.9
33
Original
range
(Jeppesen
1996)
Suspended solids
60 - 80
Updated
range
Appendix 3
(mg/L
unless
otherwise
stated)
60 - 80
Results from
large scale
batches Formulation 1
Results from
large scale
batches Formulation 2
Results from
large scale
batches Formulation 3
51.4 17.9
70.3 14
67 47.1
BOD
150 - 200
130 - 180
84.2 28.2
125 11
105 13.3
Temperature
20 - 30C
25 - 35C
pH
6.5 8.0
6.5 8.0
6.9 0.2
8.2 0.7
7.1 0.1
Turbidity
60 80
NTU
50 70 NTU
32.8 17.7
27.3 5.2
46.1 25.4
Boron
0.1 0.5
0.1 0.5
0.8 0
<1.5
< 2.0
Sodium
80 130
50 90
57.7 5
56.4 1.2
64.5 1.1
Calcium
6.7 0.6
7.4 0.4
7.4 0.3
Magnesium
1.3 0.1
1.5 0.04
1.4 0.1
Aluminium
Zinc
0.1 0.5
0.1 0.5
0.08 0.01
<0.01
0.02 0
Total phosphorousP
10 20
10 20
9.7 0.6
9.1 0.2
16.9 1.5
Total Kjeldahl
nitrogen-N
3.0 5.0
3.0 5.0
4.5 1.1
5.4 0.4
5.2 0.1
Nitrate
<0.2
0.2
Nitrite
0.014 0.005
0.007 0.004
1.5 1.0
Conductivity
(S/cm)
450 - 550
300 - 400
298 29.5
281 7.4
324 12.6
COD
250 - 400
250 - 400
171.1 35.5
224 15
238 11.4
TOC
50 - 150
50 - 150
35.1 5.9
Total coliforms
(cfu/100mL)
10 10
E.coli (cfu/100mL)
101 - 102
48.5 12
43 6.4
>2419.6
>2419.6
102 103
83 113
67 100
7.8 5.1
850 1111
10 10
F.Enterococci
(cfu/100mL)
Highlighted cells show out of range parameters
34
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36