American Water Chemicals, Inc.

9203 King Palm Dr. Suite A, Tampa FL 33619

Tel: 1-813-621-3932 Fax: 1-813-621-4085
WWW.MEMBRANECHEMICALS.COM

Membrane Autopsy Report

Date
Nov/19/2008

Tests performed for

Minera Yanacocha

Tests Performed by
Di Yu

Table of Content
Table of Content................................................................................................................ 2
Introduction....................................................................................................................... 3
Membrane information ................................................................................................... 3
Membranes autopsy tracking information .................................................................. 3
Background information ............................................................................................. 3
Procedure of autopsy....................................................................................................... 5
Shipping and Package: ..................................................................................................... 6
External inspection ........................................................................................................... 7
Fiberglass wrap ............................................................................................................... 7
Brine Seal and Anti Telescoping Device (ATD) ............................................................ 8
Weight Test...................................................................................................................... 10
ATD and Fiberglass Removal........................................................................................ 11
Membrane Sleeves and Spacer Inspection ................................................................... 12
Dye Test ........................................................................................................................... 13
Fujiwara Test .................................................................................................................. 14
Foulant and Scalant Collection...................................................................................... 15
Advanced foulant/scalant analysis ................................................................................ 16
SEM imaging and EDS analysis ................................................................................... 16
FTIR analysis ................................................................................................................ 19
Results Discussion ........................................................................................................... 20
Findings and discussion ................................................................................................ 20
Conclusion and recommendation.................................................................................. 20
Release of Liability.......................................................................................................... 21
Attachment ...................................................................................................................... 22

Introduction
A membrane that was severely scaled during operation was submitted for autopsy
analysis.

Membrane information
Membranes autopsy tracking information
Element manufacturer: HW Process Technologies, Inc.
Model: HWATFE 8040
SN: 8008519
Client and client address: Minera Yanacocha SRL, Lima Peru.
Client Contact Person: Gustavo Escobar
Client Contact Phone Number: +51-1-215-2600
Client Contact E-mail: Gustavo.escobar@newmont.com
Date Autopsy Initiated: Nov. 19th 2008
Date Shipped: Nov. 7th 2008
Date Received: Nov. 14th 2008
Carrier: Senores International Millenium Cargo
AWC Lab Reference Number: 20081119MA
Autopsy performer: Di Yu

Background information
1. Describe the feed water source for the RO Unit in question?
See AWC water chemistry projection attachment.
2. List the equipment in the Pretreatment System in the order they appear in the process.
Make the description as specific as possible. Provide chemical manufacture and
dosage level if possible.
Merrill Crowe plant press filter barren tank Antiscalant dosing Nalco 9714
Bag filter hp pump for RO membrane system.

3. Describe the configuration of the RO system:

1st Stage

2nd Stage

Array, number of
36
24
pressure vessel
Pressure drops
-13
6
(PSI)
Elements per
6
6
pressure vessel
Types of
membrane
HWATFE 8040
HWATFE 8040
elements in each
vessel and stage
Insert a chart of the RO system configuration if necessary.

3rd Stage
12
-2
6

HWATFE 8040

4. Describe the position of the membrane element sent for autopsy:

RO Skid:
Stage:
Position:
5. Describe the problem of the membrane (pressure build up, performance degrading,
reduced production, increased maintenance cost, etc.):
Pressure build up and reduced production.

Procedure of autopsy
Based on the pre-diagnosis, certain autopsy tests will be determined to be performed at
the AWC Laboratory. This section contains a brief description of the tests; the ones to be
performed on this specific autopsy report are marked with . Photographs are taken
throughout the autopsy to record the progress. Any sign of abnormal condition of the
membrane element will be reported on this document.
1.
2.

Examination of the shipping container for damage incurred during shipment.

Examination of the external construction of the element, including the
fiberglass shell, ATDs, and brine seal, for damage incurred during operation
and/or shipping.
3.
Weight measurement and bubble test to estimate scale problem and integrity.
4.
Examination of the feed and concentrate ends of the element before and after
removal of the ATDs.
Removal of the fiberglass shell.
5.
6.
Examination of each individual membrane sheet for evidence of channeling,
fouling, and/or manufacturer defects.
7.
Examination of glue lines.
Measurements of active membrane area, for comparison against the
8.
manufacturers specifications.
9.
Testing of three membrane samples with flat sheet testing setup, representing
the feed, middle, and concentrate portions of the element, for determination of
membrane damage.
Perform dye testing to verify the integrity of the membrane sample
10.
11.
Perform Fugiwara tests for membrane samples to identify chlorine damage if
such damage is suspected.
Perform SEM, EDS and FTIR analysis for samples of the membrane sheet if
12.
ordered by customer.
13.
Collect and extract foulant and/or scalant found on the membrane surface.
14.
Perform at least but not limited to, acid test, SEM, EDS, XRD and FTIR
analysis for the foulant and/or scalant.
Perform BART (Biological Activity Reaction Test) for the foulant materials to
15.
determine presents of bio-fouling..

Shipping and Package:

Description of the shipping and package condition:
Delivery date and time: Nov. 14th afternoon
Package materials: paper box
Packaging Description: Box was broken and membrane was exposed.
Sealing: A plastic cover wrapped the membrane. Part of the plastic cover was broken.
Is the membrane wet or dry? : Half dry
Additional observations (appearance, damage observed, etc):

Membrane package was broken as delivered.

Membrane was wrapped with a plastic cover.

External inspection
Fiberglass wrap
1. Manufacturer, Model and SN:
Element manufacturer: HW Process Technologies, Inc.
Model: HWATFE 8040
SN: 8008519
2. Gel coat (crack or deformation observation):
Gel coat cracked on feed side.
3. Finish (Fiberglass manufacture quality)
Fiberglass surface is covered with scale.
4. Additional note (attach photos if available)

Fiberglass close to feed side cracked

Fiberglass close to concentrate side cracked

Membrane fiberglass was partially covered with scale.

Brine Seal and Anti Telescoping Device (ATD)

1. Brine Seal condition (sign of degradation and leakage):
Brine seal is dirty with badly scaled surface.
2. Upstream ATD (integrity and make)
Upstream feed side ATD cracked. The element sleeves formed telescope from the feed
side.
3. Downstream ATD (integrity and make)
Dent in two places and cracked in one area.
4. Odor and touch
Light smell, dry to touch.
5. Additional notes (attach photos if available)

Crack on feed side ATD

Crack on concentrate side ATD

Weight Test
1. Testing condition Dry/Wet:
Half dry

2. Testing results in Pound or Kg

85 lbs or 38.5 Kg

3. Additional notes (attach photo if available)

Clean membrane should have a weight of approximately 35 lbs or 19.5 Kg.

10

ATD and Fiberglass Removal

1. Remove upstream and downstream ATDs.
See attached photo.
2. Inspect the feed side and concentrate end of the element.
Heavily scaled and telescoping is visible.
3. Remove fiberglass wrap.
See attached photo.
4. Additional notes. (attach photo if available)

Feed side ATD removal

Concentrate side ATD removal

Fiberglass was partially removed

11

Membrane Sleeves and Spacer Inspection

1. Number of sleeves and spacers
20 sleeves and 20 spacers
2. Condition of the sleeves
Severely scaled
3. Condition of the spacers
Severely scaled
4. Active membrane area and glue line (check the glue line condition and measure
the glue line width, estimate active membrane area)
The glue line is not uniform.
5. Additional notes (smell, touch, foulant, scale, attach photo if available)

Severely scaled membrane surface

Severely scaled spacer

Scale collection from spacer

Uneven membrane sleeve glue line

12

Dye Test
Three sections of membrane were cut from the feed end, middle and concentrate end of
the element. Each was tested with a dye solution to determine if the membrane had been
damaged. A blue green dye solution is applied to the feed side of the membrane sheet. If
the membrane is damaged, dye color can be observed from the permeate side of the
membrane. Photos of the dye at feed side and permeate side are provided for
comparison.

The dye was applied to the feed side of membrane samples collected from feed, middle
and concentrate end.

The dye was observed from the permeate side of the membrane. The penetration of the
dye indicated structural damage of the membrane; this is probably caused by growth of
scale to a thickness exceeding the available space between the membrane leaves thereby
prying them apart and tearing into the membrane.

13

Fujiwara Test
A sample of the membrane was subjected to a Fujiwara test. A positive reaction
indicated halogen damage to the membrane surface. Examples of Halogens are
chemicals such as chlorine and bromine. The tests are carried out for samples from feed
end, middle and concentrate end of the membrane element. The photos of the test results
are insert below and all the tests were carried out with a blank (test tube with colorless
solution) for comparison.

Tube A is 100% negative results with blank, tube B is 100% positive results, tube C is the
membrane sample which has negative results, tube D is a virgin membrane sample with
negative results for comparison. The Fujiwara tests showed no chlorine damage.

14

Foulant and Scalant Collection

1. Record the procedure of collecting foulant and/or scalant.
Large amount of half dry salt deposited on the surface of membrane sleeve and spacer.
2. Appearance of foulant and/or scalant
Yellow color dry solids
3. Odor of the foulant and/or scalant
No strong odor.
4. Viscosity of foulant
The scale is solid and dry and not viscous.
5. Additional notes (attach photos if available)
Collected scale did not dissolve in 10% HCl. Neither did it dissolve in 10% NaOH
solution. However, it was dissolved in a special cleaning procedure that adopted AWC
products that specifically designed to remove CaSO4 scale.

From Left to Right: Left: scale was added in 2%C238 solution at natural pH and 45
degree C. Middle: scale was stirred overnight in the solution and was dispersed by C238.
Right: then 2%C239 was added and the pH was adjusted to 12.5, the dispersed scale
particles were dissolved.

15

Advanced foulant/scalant analysis

SEM imaging and EDS analysis
SEM (Scanning Electronic Microscopy) is used to determine topography, morphology
and crystallographic orientation of a sample. The SEM shows very detailed images at
magnifications up to 200 thousand times. EDS (Energy Dispersive Spectroscopy)
analysis is a standard procedure for identifying and quantifying elemental composition of
a sample. The material is bombarded with electrons from a SEM and the X-rays
produced are measured by an X-ray dispersive spectrometer. Every element has its own
characteristic wavelength and can be identified accordingly.
The scale collected from the membrane is examined with SEM and EDS analysis. SEM
images and EDS spectrums, together with composition reporting tables are attached in
the section.

Minera Yanacocha scale image at 5000X magnification.

16

Minera Yanacocha scale image at 200X magnification.

17

EDS spectrum showed the elementary compositions of the Minera Yanacocha scale.
Element
C
O
Na
Si
S
Pd
Ca
Fe
Au
Total

Wt %
9.89
37.11
0.64
1.84
18.86
2.06
22.98
0.71
5.9
100

At %
18.47
52.01
0.62
1.47
13.18
0.43
12.86
0.29
0.67
100

The quantitative ratio of the elements in the scale

The scale is mainly CaSO4 with small amount of Si and Fe.

18

FTIR analysis
Fourier Transform Infrared spectrometer (FTIR) is a powerful tool for identifying types
of chemical bonds (functional groups). The wavelength of light absorbed is characteristic
of the chemical bond. The spectrum of an unknown material can be identified by
comparison to a library of known compounds. FTIR test is carried out for the scale after
it was dried at 80 degree C for 3 hours. FTIR analysis indicates functionality associated
with a hydrated metal salt or oxide exclusively. The sample is therefore likely mainly a
hydrated calcium and sulfur salt. The spectrum is shown below:
101

90

80

70

%T
60

50

40

30
25
4000

3500

3000

2500

2000

1500

1000

650

cm-1

FTIR spectrum of scale dried at 80 degree C for 3 hours.

100.0
95
90
2209.35

85

1425.47

80
75

1681.91

70
65
60
%T 55

1617.87
3391.76

50
45
40
35
30

666.31

25

1097.26

20
15.8
4000.0

3000

2000

1500
cm-1

FTIR spectrum of a CaSO4 standard

19

1000

600.0

Results Discussion
The customer of Minera Yanacocha had a very severe membrane scaling problem. The
membrane was autopsied at AWC and the composition of the scale was identified.

Findings and discussion

The scale was mainly CaSO4. The scale had grown so severely that the membrane
sleeves had been damaged mechanically as shown in dye testing. This particular
membrane element was scaled and damaged beyond the limits of repair. The cause of
CaSO4 scale growth was that the antiscalant in use was not able to control the formation
of CaSO4 scale. Tube testing in the lab of AWC antiscalants showed successful control
of CaSO4 scale when dosed as recommended in the antiscalant projection program.

Conclusion and recommendation

The tested membrane was severely scaled and damaged. If the membrane elements were
scaled to such extend, it should be replaced with new membrane elements. To clean the
elements with less scale and damage, combination of AWC C238 and C239 can be an
efficient method. For future operation, acid should be added to reduce LSI - due to the
excessively high feed pH of the system, it is not possible to operate without acid dosing.
AWC antiscalant A104 should be used to control CaCO3 and CaSO4 scale formation for
the RO system.

Reviewed by

Mohannad Malki
Technical Director

20

Release of Liability
The Membrane Autopsy Service (The Service) was performed in accordance with the
standards of care, skill, and diligence normally provided by a professional in the
performance of similar services. American Water Chemicals, Inc. makes no warranty of
any kind with the respect to The Service and will not be liable for any damages resulting
from the use or misuse of The Service. In no event shall American Water Chemicals, Inc.
have any liability for The Service, including, but not limited to, special, indirect,
incidental, consequential, or other direct damages whether such liability arises in
contract, negligence, strict liability, or otherwise, and the Client hereby agrees to release
and indemnify American Water Chemicals, Inc. against same.

21

Attachment
AWC antiscalant projection program report:

22

23