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COMPLETED FOR:

AQA Quimica S.A.

Membrane #7
01/10/22 WO#120921-1
Table of Contents
Executive Summary 1
Inspection 2
Membrane Surfaces 2
Feed Spacers 4
Foulant Analysis 5
Foulant Density Measurement and Composition Testing 5
Microscope Analysis 6
Biological Activity Testing 7
Testing for Carbonates and Metals 8
Fourier Transform Infrared Spectroscopy (FT-IR) Analysis 9
Membrane Surface Imaging and Elemental Composition Testing 10
Flat Sheet Performance and Cleaning Study 13
Flat Sheet Cleaning Study 13
Testing for Flat Sheet Damage 15
Fujiwara Testing 15
Dye Testing 15
Certification by Laboratory 16
Appendix I. Membrane Construction Diagrams 17
Appendix II. Biological Activity Ratings 18
E XE CUTIVE SUMMARY
Background AQA Quimica S.A. provided (2) Filmtec BW30XFR400/34i reverse osmosis (RO)
membrane samples to Avista for full membrane autopsies. The flat sheets were identified as Membrane
#1 and Membrane #7. The remainder of this report pertains to Membrane #7. Below is a summary of the
analysis.

Foulant Analysis Low aerobic bacteria activity was observed. Microscope analysis identified mainly
amorphous crystalline material,. The bulk of the foulant was confirmed to be silica scale.

Flat Sheet Performance and Cleaning Study Flat sheet samples harvested from samples received
produced no permeability. Flat sheet permeability was restored and complete visual foulant removal was
achieved using RoClean P112 (2% by weight in RO/DI water, heated to approximately 35 degrees
Celsius and circulated) for 6 hours.

Flat Sheet Damage Fujiwara testing was negative for the presence of halogens in the membrane
structure.

Autopsy Conclusion The flat sheets were fouled with mainly silica scale. Although permeability could
be restored to normal, membrane rejection could not be completely recovered due to abrasion of the
membrane surface.

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INSPECT ION
Membrane Surfaces should be uniform and shiny. They are inspected for:

• Foulant – can cause elevated differential pressures, loss in permeate flow and loss in rejection
• Creasing of the membrane surface – more common in the presence of gapping, feed spacer
extrusion and telescoping, can cause loss in rejection
• Delamination – lifting of the thin-film membrane from the support layer which is often caused by
positive pressure on the permeate side of the element, causes loss in rejection

Results: The membrane displayed a thin, translucent white-colored foulant layer which adhered tightly to
the membrane surface. Smooth, tan-colored foulant material was also very lightly coating the exposed
membrane surfaces of the sample.

Exposed membrane surface of Membrane #7

The following key will be used throughout the report to demonstrate whether the observation is
within or outside normal conditions or if the test was not carried out.

Within normal conditions Outside normal conditions Not tested

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Foulant scraped on Membrane #7 sheet

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Feed Spacers are composed of plastic net material designed to separate the membrane leaves, forming
a flow path, and to promote turbulence within the feed water channels. They are inspected for:

• Foulant – can block the feed channels, causing elevated differential pressure
• Damage – fouling can cause deformation of the material, disrupting the hydraulics of the
membrane and increasing cleaning difficulty

Results: The feed spacers were in good condition.

Feed spacer of Membrane #7

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FOULANT ANALY SIS
Foulant Density Measurement and Composition Testing is performed to quantify degree of fouling,
which contributes to full element differential pressure, and determine the composition of the foulant:

• Moisture Content – the portion of the foulant that is water. Biological materials tend to have higher
moisture contents (>95%)
• Organic Content – the portion of the foulant composed of carbon, which ignites during testing
• Inorganic Content – the portion of the foulant not composed of carbon and does not ignite during
testing

Results: Foulant composition testing could not be performed due to the scarcity of harvestable foulant
material.

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Microscope Analysis is performed on Gram-stained foulant samples using a light microscope at 1000x
using an oil immersion lens. Gram-positive bacteria are stained purple while Gram-negative bacteria are
stained pink. The following organic and inorganic components can be identified:

• Organics: Bio-slime, humic/fulvic acid, bacteria, yeast, mold, nematodes, microorganism shells
• Inorganics: inorganic material (e.g. metals, clays), translucent crystals, particles

Results: Microscope analysis identified amorphous crystalline material. Lesser amounts of bio-slime,
inorganic deposits and other particulate material were also present.

Light microscope images (1000x) of foulant scraped from Membrane #7

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Biological Activity Testing gives a semi-quantitative result for live aerobic bacteria and yeast/mold
content of a sample. Greater colony density, measured in colony-forming units (CFU)/ml, indicates a
more biologically active sample.

• Higher biological activity is associated with more biological fouling


• The biological activity rating references are available in Appendix II on page 18.

Results: Highlighted in the table below.

Biological Activity Rating Aerobic Bacteria Yeast/Mold


Low 0-100 0-100
Moderate 100-10,000 100-10,000
High 10,000-1,000,000 10,000-100,000
Very High 1,000,000-TNTC 100,000-TNTC

Before Incubation After Incubation

Aerobic Bacteria

Yeast/Mold

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Testing for Carbonates and Metals is performed by applying several drops of dilute hydrochloric acid
(HCl) to the foulant surfaces.

• Effervescing (bubbling) – positive for carbonates


• Yellow color change – positive for the presence of metals.

Results: Acid testing displayed neither effervescing nor yellow color change.

Before HCl After HCl

Acid test reaction

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Fourier Transform Infrared Spectroscopy (FT-IR) Analysis produces a spectrum for the foulant that
is compared to an extensive FT-IR library of known foulants to identify specific compounds (functional
groups). FT-IR is performed on either a harvested sample of the foulant or directly on the membrane
surface if sufficient harvestable material is not present.

Results: FT-IR identified peaks associated with silica.

Compound Wavelength (cm-1)

Silica 1000

FT-IR spectral image of foulant removed from the membrane surface of Membrane #7

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Membrane Surface Imaging and Elemental Composition Testing is used to identify foulants and the
degree of fouling. This is accomplished using Chromatic Elemental ImagingSM (CEISM) and Energy
Dispersive Spectroscopy (EDS) Analysis.

• CEI – high-resolution imaging technique that assigns elements colors to show the spatial
distribution, interaction and relative concentration of elements in sample
• EDS – provides the relative concentrations of elements present in a sample

Results: CEI confirmed the bulk of the foulant layer to be comprised of silica (light blue). Lesser patches
of clay (aluminum silicates – combination of yellow and light blue) and bio-slime (carbon – dark blue)
were also identified. The element representative of the membrane surface (sulfur – red) was partially
visible in areas absent of foulant.

CEI image (150x) of the membrane surface with labels

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CEI image (1500x) of the membrane surface with labels

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Results: EDS analysis confirmed silica as the dominant inorganic element present. A small amount of
aluminum was also identified. The low sulfur weight percentage indicates a relatively thick foulant layer.

Membrane #7 New Membrane


Elements (Weight Percent, wt%)
(Weight Percent, wt%)

Carbon 22.17 40.00-60.00

Oxygen 43.85 30.00-40.00

Sulfur 3.72 5.00-9.00

Silica 28.11 --

Aluminum 2.14 --

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FLAT SHEET PE RFORMANCE AND CLEANING ST UDY
Flat Sheet Cleaning Study is performed in a cell test apparatus to determine the most effective cleaning
regimen for overall improvement in permeability, rejection and visual foulant removal.

• Flat sheet normalized permeability and rejection before and after cleaning are calculated and
compared to the manufacturer’s specification for new membranes of the same model
• Calculations are performed using industry standard water passage coefficient (A value) and salt
passage coefficient (B value) and converted for ease of understanding. A and B values are
available upon request

Results: The following regimen achieved complete visual foulant material, improving permeability and
rejection:

1) RoClean P112 (2% by weight in RO/DI water, 35 degrees Celsius and circulated) for 6 hours

Filmtec BW30XFR400/34i Permeability Rejection (%)

Pre-Clean Flat Sheet No Permeability

Post-Clean Flat Sheet Normal 97.0

Manufacturer’s Specification 8.61 to 1.16E-04 99.6 to 99.8

Permeability (% of Normal)

Pre-Clean
Post-Clean

0% 25% 50% 75% 100% 125% 150% 175% 200% >200%

Rejection (%)

Pre-Clean Post-Clean

<95% 96% 97% 98% 99% 100%

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Pre-clean flat sheet

Post-clean flat sheet

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TE STING FOR FLAT SHEET DAMAGE
Fujiwara Testing is a qualitative analysis which determines if a polyamide (PA) thin-film membrane has
been exposed to halogen (e.g. chlorine, bromine, or iodine) oxidation. Exposure to halogens is
progressively damaging to PA membranes, causing increases in flow and losses in permeate quality.

Results: Fujiwara testing was negative for the presence of halogens (e.g. chlorine) in the membrane
structure.

Dye Testing is used to identify the presence and extent of chemical and/or physical damage to
membrane flat sheet samples.

• Uneven dye uptake – indicates physical damage


• Even dye uptake – indicates chemical damage
• Dye penetration to the membrane backing – indicates severe damage

Results: Dye testing showed even unuptake with increased uptake in the feed spacer contact points. This
is indicative of physical damage (e.g. abrasion). The damage was severe in some areas, with partial dye
penetration observed on the membrane backing.

Membrane Surface Membrane Backing

Dye test results

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CERT IFICATION BY LABORAT ORY

Report Number Report Content Membrane Number Report Date

Membrane #1
WO#120921-1 Standard Spiral Autopsy 01/10/22
Membrane #7

We the undersigned being the technical specialists in membrane autopsy and related testing procedures
and protocol for Avista Technologies certify to the best of our knowledge and belief that the tests listed
in this report have been conducted following Avista’s standard testing practices and that the results are
accurate and complete.

By signing this certificate neither the laboratory employees nor their employer makes any warranty,
expressed or implied, concerning the cleaning study results.

Date: 01/10/22

Signed:

Jessica Foster Jenna Neel


Laboratory Services Supervisor Laboratory Services Chemist

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APPENDIX I. MEMBRANE CONST RUCTION DIAGRAMS

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APPENDIX II. BIOLOGICAL ACT IV ITY RATINGS

Aerobic Bacteria Yeast Mold

Low

Moderate

High

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