Communication from the Agent of Argentina commenting on the response given by Uruguay to the question put to the latter by Judge Bennouna at the end of the hearing held on 29 September 2009

Argentina's written comments to Uruguay's reply to Judge Bennouna's question "JVhat
process and products are used by the Botnia plant for its cleaning?"

1. At the end of the hearings held on 29 September 2009 Judge Bennouna asked

the following question:

JVhatprocess and products are used by the Botnia plant for its cleaning?
Uruguay was asked to provide a reply by 9 October 2009, and Argentina was

provided with an opportunity to respond by 19 October 2009.

2. Uruguay provided an oral response during the hearings on 2 October 2009 (CR

2009/23, pp. 14-15, paras. 6-8 (Mr. Reichler), and made available a copy of an

affidavit dated 30 September 2009, as written by Mr Gervasio Gonzalez
Sirneonoff. By letter dated 8 October 2009 Uruguay merely reaffmned the

response it had given on 2 October 2009, without adding anything new.

3. Argentina is pleased to have an opportunity to respond to the new evidence

provided by Uruguay. As set out below, Argentina notes that Uruguay has

provided an incomplete response to the question posed by Judge Bennouna, and
subrnits that the evidence before the Court points decisively to the fact that the

Botnia plant has used nonylphenols that are banned in the pulp and paper

industry in the European Union. Before addressing the statement of Mr.

Gonzalez, it is appropriate to place it in the context in which it was prepared.

4. Argentina raised the issue of nonylphenols in its new written documents

submitted on 30 June 2009 after monitoring the Uruguay River for more than a

· year. Specifically, this monitoring identified the presence of elevated levels of

nonylphenols in the waters, clams, in the algal bloom of February 2009 and in

sediments around the Botnia plant, as weil as the presence of nonylphenols in

pulp samples from the plant which matched the nonylphenols identified
elsewhere. This monitoring and analysis points direct!y and unambiguously to

the use of nonylphenols at the Botnia plant. Uruguay has bad ample opportunity

1NewDocumentsSubmittedby Argentinaon30June2009,Chapter3: UruguayRiverEnvironrnental
SurveillanceProgramBiogeochemicalStudies,in particularExecutiveSummarya4 andsection3.4.1
and3.5.

• Ibidem to respond to the evidence submitted by Argentina. It could have introduced its

own evidence but it has not done so. Consequently, the unchallenged evidence

before the Court shows that (1) pulp produced at the Botnia plant is

contaminated by the presence of significant levels of nonylphenols, and (2) the
waters, clams, the algal bloom and the sediments in the immediate vicinity of the

plant's effluent discharge pipe show significantly elevated levels of

nonylphenols as compared with samples taken in other places on the river. Both

factors point conclusive!y to the use of nonylphenols ethoxylates (NPEs) at the

plant, the presence of which is reflected in degraded nonylphenols in pulp,

waters, clams, algal blooms and sediments.

5. Against this background, instead of addressing the issue by way of testing or

monitoring by its competent authorities, Uruguay has served two affidavits that

are part of the evidence before the Court and made inconsistent arguments by

way of submission that go beyond what its own evidence will support. This has
3
been fully addressed by Argentina during the hearings, and need not here be
repeated. On 15 July 2009 Uruguay served a first affidavit by Ing. Alicia

Torres.4 Ing. Torres has no apparent expertise on the subject of the production of

pulp, includirigissues of cleaning, or on nonylphenols. Her affidavit raised more

questions than it answered, and was conspicuous by its failure to address the

cleaning of the eucalyptus wood chips or the cleaning of the plant itself, the
process in which nonylphenols could be expected to be used. Despite Ing. Torres

affidavit, and an affidavit dated 20 September 2009 by Mr Gonzalez (which was

referred to in part in a letter submitted by Uruguay to the Court on 28 September

2009 but which Argentina has not seen in full), on 22 September 2009 counsel

for Uruguay told the Court that although Uruguay was "convinced" that there

"is" no use of nonylphenols - he did not say there "has never been" any use of
nonylphenols - if the plant was using nonylphenols then Uruguay would put a

stop to it (CR 2009/17, p. 24, para. 38 (Mr. Reichler). Itwas readily apparent

>See CR 2009112 14 September 2009, p. 59, para. 24 (Prof Wbeater); CR 2009/14 16 September 2009,
pp.-45-47, paras. 15-17 and 18-23, and p. 51, paras. 26-28 (Prof Colombo); CR 2009/15 17 September
2009, pp. 16-18, paras. 12-16 (Prof Sands) and p. 24, para. 7 (Prof Wbeater); CR 2009/20 28 September
2009, pp. 50-51, paras. 21-23 (Prof Colombo);, CR 2009/21 29 September 2009, p. 21, para. 32 (Prof
4ands).
Affidavit of Agr. Eng. Alicia Torres, Director of DINAMA, l3 July 2009, Uruguay's Comments on
Argentina's New Documents, 15July 2009, Annex C24. · that the state of knowledge and certainty of Uruguay as to what was being
5
discharged into the river was less than complete.

6. On 2 October 2009, nearly three months after this issue was first raised by

Argentina to the Court in its 30thJune 2009 Report, Uruguay revisited the issue

for a third time, submitting a further affidavit dated 30 September 2009 and

written also by Mr Gonzalez. Mr Gonzalez works for Botnia and therefore Iacks

independence. Once again, the affidavit is incomplete, in failing to address all

aspects of the cleaning of the eucalyptus wood chips. It is ambiguous and

contains errors of fact that suggest that its author lacks technical expertise.

7. Argentina has obtained a report on Mr Gonzalez's affidavit, by providing a copy

to Dr Bruce Sithole, an expert on the use of nonylphenols in the pulp and paper

industry. As can be seen from his curriculum vitae, which is attached to his

report, Dr Sithole worked for 22 years at FPinnovations - Paprican (the Pulp and

Paper Research Institute of Canada), where he \'\rasa Principal Scientist and

Group Leader. He has prepared a detailed report dated 16 October 2009 on the

use of nonylphenols in pulp mills in general and at the Botnia Mill, a copy of
which is attached. His report sets out inter alia the context and processes by

which it is necessary to remove lipophilic extractives from the hardwood

eucalyptus chips in order to produce high quality and commercially valuable

pulp. Those processes constitute a cleaning process, and relate to matters that are

addressed by Judge Bennouna's question. Dr Sithole states at paragraph 31 that

the mere addition of defoamer (even one incorrect/y described as a

'surfactant'by Mr. Gonzalez in his affidavit) in the washing process will

not be sufficient to achieve pulp of the quality which is produced at the

5 Argentina notes that the subject of nonylphenols is not the only one on which Uruguay's submissions
and evidence are incomplete. Uruguay bas challenged Argentina's interpret oa~ ieonword
'oxidabilidad's used in OSE monitoring data for the period from 19 April 2007 to 13 May 2009 (CR
2009/23, pp. 17-19, paras. 12-17, referring to Argentina's arguments made at CR 2009/21, p. 29, para.
33). Uruguay's preferred interpretation is that 'oxidabilidad' means 'oxides' (CR p. 18, para.
15),yet the terrn 'oxides'ot one that bas meaning in this context and is not usually associated with the
measurement of water qua1ity. In any event, the evidence before the Court indicates serious problems
with biochemical oxygen demand(BOD) and shows that "continued recordings of the buoys confirmed

recurrent oxygendeficits the Uruguay River relative to the Bay which presented more oxic conditions":
New Documents submitted by Argentina on 30 June 2009, Volume 1, Scientific and Technical Report,
Chapter 3, Executive Summary,p. 2, second paragraph, and Section 3.2.3. This evidence has not been
challenged by Uruguay.

3 mill. The very fact that a defoamer is required, indicates to me that a

surfactant is indeed used in the washing process.

Dr Sithole concludes at paragraph 23 of his report that, contrary to the claim

made by Uruguay during the hearings (CR 2009/23, p. 14), a 2008 AMEC report

(included at Annex 48 of Uruguay's Reply) does not specifically describe the
principal cleaning chemicals used by the Fray Bentos mill. At paragraph 34 of

his report, Dr Sithole concludes that Mr Gonzalez's affidavit of 30 September

2009

does not provide a complete answer to the question and does not jully

describe the "process and products ... used by the Botnia plant for its

cleaning".
His report further concludes at paragraph 33 that a number of factors point

stronglyto the use of nonylphenols at theplant:

1 am not able to express an absolutely definitive view. However, there

are a number of factors that are significant: the eucalyptus hardwood

used to produce the pulp at the plant; the absence of easily available
alternatives to clean the eucalyptus or its wood chips to remove

lipophilic material; the issues·of cost, taking into account the type of

pulp produced at the mill; the repeated failure on the parr of Uruguay

and Botnia to provide detailed information on the cleaning processes

used at the Botnia plant or the compounds thar are u,sed; the strong

evidence of NP Es in higher concentrations in the waters into which the
plant's effluent discharges are made; the evidence of NPEs in sample of

sediments, clams, algal blooms; and the evidence of NPEs in samples of

pulp produced by the mill. Thesefactors point strongly towards the clear

conclusion that NPEs have been used at the Botnia plant in one or more

cleaning processes associated with the production of wood pulp. In the
lightof my professional experience, 1 would be very surprised if NPEs

had not been used. If 1were asked to quanti/y my leve/ of certainty that

NPEs had been used, lwouldput itat 95%.

8. Argentina adopts Dr Sithole's conclusions. These conclusions will not have

come as a surprise to Uruguay. Uruguay was familiar with the issues he has
raised, and had ample opportunity to address them by way of detailed evidence,

4 including by way of complete affidavit. Argentina submits that the fact that

Uruguay has not addressedthe issues raised by Dr Sithole,has not provided full
information as to the sUrfactants that are used to remove the lipophilic

extractives, and has not provided any evidence as to its o·wntesting for the

presence of nonylphenols, points conclusively to the use of nonylphenols

ethoxylates(NPEs)by theBotniaplant.

9. Uruguay accepts the dangers posed by nonylphenols, including the irreversible

damage that they may cause to plant, animal and human life. In the
circumstances, this_is exactly the kind of issue for which the principles of

prevention and precaution play an important role. Argentina submits that the

evidence before the Court indicates that the burden ison Uruguay to establish

conclusivelythat it does not use, and has not used, nonylphenols.t has not met
that burden. Specifically,n response to Judge Bennouna's question, by failing

to provide a complete account of the "process and products ... used by the

Botnia plant for itscleaning" Uruguay's actions require the Court to conclude

that the evidence before the Court points compellingly to the use of
nonylphenols ethoxylates (NPEs) at the plant, in particular for the purpose of

removing Iipophilic extractives from the eucalyptus hardwood chips that are

used at the plant.

Buenos Aires, 19October2009

Agentof the ArgentineRepublic

5 Report into: (1) the Use ofNonylphenols in Pulp Mills in General and
(2) at the Botnia Mill, Uruguay

Dr B Sithole, Quebec, 16 October 2009

Personal background and professional experience

1. 1 am a research chemist and 1 hold a Ph.D. in Environmental Analytical Chemistry

from the Trace Analysis Research Center, Department of Chemistry, Dalhousie

University, Halifax, Nova Scotia, Canada, 1983. As indicated in my Curriculum
Vitae, which is attached as Annex 1, my research experience includes extensive

analysis of nonylphenol ethoxylate surfactants ('NPEs') as used in pulp and paper

samples and for the removal of lipophilic extractives in pulp and paper making

processes.

2. From 1987 to 2009, 1 was employed at FPinnovations -Paprican (formerly the Pulp

and Paper Research lnstitute of Canada), Quebec, where 1 was a Principal Scientist

and Group Leader. My work at Paprican involved methods development and analysis

of phytosterols, wood extractives, deposits and additives in pulp and paper matrices.
The developed methods are used to solve production problems, assess environmental

pollution, improve mill production, and for reverse-engineering studies to help in new

product development. The analytical techniques used include LC-MS, GC/MS,

pyrolysis-GC/MS, FTIR, HPLC, GPC, SPE and ion chromatography. 1 was also
involved in troubleshooting environmental and wet-end issues in pulp and paper mills.

3. My publications on NPEs include the following (see further the full list as set out at

Annex 1to this report):

1 B.B. Sitholé and L.H. Allen, 1989. Determination of nonionic nonylphenol

ethoxylate surfactants in pulp and paper mill process samples by

spectrophotometry and HPLC, J ASSOC. OFF. ANAL. CHEM, 72, 273-276.

B.B. Sitholé, B. Zvilichovsky, C. Lapointe and L.H. Allen, 1990. Adsorption

of nonylphenol ethoxylate surfactants on metal surfaces: effect on quantitation

by liquid chromatography, J ASSOC. OFF. ANAL. CHEM, 73(2), 322-324.

B.B. Sitholé and E.J. Pimente!, 2009. Determination of nonylphenol and
nonylphenol ethoxylates in pulp samples by Py-GC/MS, J ANAL. APPL.

PYROLYSIS, 85(1-2): 465-469.

Consultation report: Deresination of aspen in sulphite dissolving pulps: comparison

ofNPE and non-NPE surfactants, FPinnovations Confidential Internai Report, 2008.

4. My professional memberships and related activities are set out in full in my

Curriculum Vitae at Annex 1. In 1997 I was elected Fellow ofthe Chemical Institute

of Canada. I was the Chair of the Fine and Coated Papers Committee, Pulp & Paper

Technical Association of Canada, from 1998-2002. In 2002, I was awarded a

Certificateof Appreciation by the Pulp & Paper Technical Association of Canada,

2002, Such certificates are given "To recognise individuals who have provided

exceptional services toAPTAC and/or the Canadian pulp and paper industry".

Terms of Reference

5. I have been asked by the Government of Argentina to prepare an independent report,

on the basisof materials provided to me or which I obtained myself, on the following

issues:

1. The use ofNPEs in pulp mills;

2 2. Whether it is possible or likely that NPEs are being used at the Botnia plant;

3. The information that would be needed to reach a definitive conclusion on

the use ofNPEs at the Botnia plant.

In addressing these issues, I have been asked to respond to the question posed to

Uruguay by Judge Bennouna during the hearing, taking into account also the response

given by Uruguay to the question, during the hearing and on 9 October 2009. The
question asked by Judge Bennouna was:

"What process and products are used by the Botnia plant for its cleaning?"

I understand Judge Bennouna's question to address the cleaning of the plant itself and
the eucalyptus wood chips, which process would include the removal of lipophilic

extracts.

Materials Considered in the Preparation of this Report

6. In preparing this report 1have drawn on my professional experience and expertise in

the field. In addition, the materials which 1have used in preparing this report include:

(i) A copy of the 'Rio Uruguay Environmental Surveillance Program (Chapter III,

Biogeochemical Studies - November/08-April/09)' report, pages 1 through 42
provided by Argentina".

(ii) An English translationf the Affidavit of Agr. Eng. Alicia Torres, director of the

National Environmental agency, provided by Argentina.

(iii) A technical report attached to the Affidavitf Ing. Torres: Nonylphenol and its

Ethoxylates in Environmental matrices. Case study Uruguay. Soledad Andrade

B.S., Sandra Castro Scarone, B.S., Natalia Barboza, B.S., May 2008, produced by

DINAMA, provided by Argentina ("DINAMA Report").

3 (iv)A copy of Tables 1-5 indicating individual Nonylphenol (NPI to NP6) and total
concentrations in settling particles, water samples, pulp and technical product,

entitled 'Data_Table_Nonylphenols [1], provided by Argentina.

(v) A case study from the USA entitled 'Pulp and Paper industry Voluntarily Reduces

Use of Nonylphenol Ethoxylates', available at
http://www.deg.state.mi.us/documents/deg-ead-p2-p5-npe.pdf

(vi)A fact sheet on the pulp mill project published by Botnia available at

http://w3.upm­

kymmene.com/upm/internet/cms/upmmma.nsfllupgraphics/Botnia%20Uruguay%20f
act%20sheet
ENG.pdf/$file/Botnia%20Uruguay%20fact%20sheetENG.pdf

(vii) A press release available at http://w3.upm-

kymmene.com/upm/internet/cms/upmcms.nsf/pkv!UPM and Botnia's Fray Bent

os pulp mill in Uruguay?OpenDocument

(viii) The current published priee for Botnia's FRB EUCA (effective 1 October

2009) source: http://www.botnia.com/en/default.asp?path=204,21 0,211,2672,3058

(ix) Arguments made by Counsel for Uruguay in the course of the hearing held at the

International Court of Justice on Tuesday 22 September 2009 (CR 2009/17) (in
particular at paragraphs 22 to 28 on pages 8-9).

(x) A September 2007 AMEC Report, included as Annex 48 to Uruguay's Reply in
the court proceedings.

(xi) A copy of the affidavit of Mr. Gervasio Gonzalez, Environmental Manager at the

Fray Bentos pulp mill, dated 30 September 2009, together with annexed
attachments.

Other material which 1would have liked to have seen

7. lt would have been helpful in preparing this report to have had access to other

material. Specifically, it would be very useful to be provided with a document setting

out in detail the list of ali additives used at the Botnia plant, together with their MSDS
information. This information would allow me to understand the composition of ail

4 the chemical formulations used at the plant. For example, a case study conducted in

Michigan, USA, in 2000, found that of the 780 process chemicals used by 17 mills in

the state,

• 604 products were NPE-free;

• 60 products were identified by their vendors as containing NPE (at 1-6%

levels);

• 31 products were no longer sold by vendors;

• 85 products were identified as having unknown NPE content.

The vendors were pressured to change the 60 NPE-laden products and the results

were:

• 28 products were re-formulated to NPE-free products

• 2 products did not have the potential for waste water discharge, and so were
not converted

• 6 products were no longer sold by vendors

• 24 products could not be re-formulated

If such a case study had been condueted in Uruguay I am certain that the results

would demonstrate that many additives used in Uruguay also contain NPEs. Thus it

is, in my view, very likely that a significant number of products sold by vendors in

Uruguay to the pulp and paper industry will contain NPEs, considering that the sale of

such products is not banned in the country.

8. The DINAMA Report to which I have been referred (paragraph 6 above, document

3), shows that significant amounts of products having NPE concentrations are used in

Uruguay and would be likely to result in industrial discharges. lt is striking, however,
that the industries referred to in the report do not include the pulp and paper industry,

and that no reference is made to data on pulp and paper mill effluents, which I

understand to be a major industry in Uruguay. This raises the question, to my mind,

as to why this industry was not included in the study?

59. The DINAMA Report shows that NPEs are widely used in Uruguay, including in the
wool industry. Raw wool contains lipophilic materials that impart undesirable

properties to the final products and thus need to be removed. Lipophilic materials are

natural fats and fatty compounds that are presentn animais and plants and are soluble

in organic solvents. These materials are also presentn wood and need to be removed
as they interfere with the pulp and papermaking process, since they impart poor

quality to the final product. The more lipophilic material there is in the pulp and

paper, the lower is its quality and bence its commercial value. There are therefore

good financial reasons for removing lipophilic materials from pulp. Estimates are that
the North American industry spends $750 million annually to tackle problems caused

by lipophilic extractives. NPE cleaning agents are cheap and very effective in the

removal of these lipophilic materials, and that is why they have been widely used in

the pulp and paper industry throughout the world. In my opinion it is very probable

that Uruguayan vendors of NPE-containing cleaning agents to the wool industry in
Uruguay would also be in a position to sell the same products to the pulp and paper

industry, since they could be used in that industry. They would be relatively cheap

and easily available.

Description of the process, and the point at which, NPEs would be introduced

1O.The terminologies used with respect to NPEs may be confusing and warrant a brief

explanation as sorne people incorrectly use them interchangeably. Nonylphenol

ethoxylates (NPEs) are ethoxylated products of nonylphenol (NP)- that is, they are

manufactured from NP. They are the major components in the NPE formulations sold

for industrial use. However, NPEs degrade in the environment to form NP which is
very toxic to aquatic biota.

11. There are many unit operations or stages in the manufacture of pulp. From the
materials to which 1have been referred, and in particular the Affidavit of Ing Torres,

she seems to focus on just two of the unit operations, namely production (which

would be the cooking process) and bleaching. Her affidavit does not refer expressly

6 to pulp washing operations (where the pulp bas already been produced) orto cleaning
operations (where dirt and contaminants are removed from the pulp), which are the

processes in which NPE are typically used. Also,n many instances, high amounts of

extractives and lipophilic extractives lead to what we cali deposition problems on mill

machinery. Fully bleached kraft pulp like the one produced at the Botnia plantis sold

on the basis of kappa number and lipophilic extractives content. Kappa number is an

indicationof the residual lignin in the pulp that affects the whiteness of the pulp. The
lipophilic extractives threshold values are around% using dichloromethane as the

extraction solvent. Final pulps that have high extractives values will cause severe

problems for customers when they convert the pulp to final products such as

photocopy paper. The problems include sticky deposits on paper machines,

unacceptable odours when the paper is used on photocopiers (the fats in the

extractives become rancid and emit objectionable smells), slippage on the paper on
copier machines (paper sticking in and jamming copier machines). The deposits that

are caused by the extractives require cleaning with alkali and surfactants, and NPEs

may also be present in these industrial cleaners. NPEs may be present in products

used to clean the plant itself. Sorne mills add surfactants in the digester - during the

cooking stage to solubilise the problematic lipophilic extractives but not where
eucalyptus is used for pulpproduction because of cost issue.

12.An extensive series of unit operations are utilised in the production of fully bleached

pulp, e.g., debarking, chipping, cooking, brownstock washing, pressing, bleaching,
etc. These unit operations function to produce/convert wood into pulp. Cleaning

ope~ati suchsas boil outs, serve to clean the system and ensure the production of

good quality pulp. They are not directly involved in the conversion of wood into

pulp.

13. In Kraft pulping, the stage of the process at which NPEs are introduced is in the

washing of the pulp after cooking (high amounts will impair the bleaching process

and cause sticky deposits on mill equipment) and after bleaching to remove

extractives that have been affected by the bleaching process. 1 would have expected

lng. Torres to have mentioned thisn her Affidavit. They can also be introduced in

7 pulp storage tanks where surfactants (dispersing agents) are added to disperse the

lipophilic extractives thereby preventing them from agglomerating to form the sticky

deposits. Ing. Torres does mention the addition of dispersing agents but gives no

indication on the chemistry of the surfactants used. NPEs can be effective dispersing
agents at dosages similar to those mentioned by Ing. Torres.

14.In Kraft pulping, as practiced at the Botnia plant, the produced brown pulp is washed
in brownstock operations to remove lignin and the lipophilic materials mentioned

earlier Surfactants are used at this stage as they solubilise the lignin and lipophilic

extractives. The surfactants function just like soap that is used to wash out dirt in

laundry. Alkali washing alone can be effective in softwood pulps because the
components in their lipophilic are easily solubilised and washed out. However, the

components in eucalyptus and other hardwoods are not easily solubilised by alkali and

thus remain with the pulp. Addition of NPEs to the wash water is effective in

solubilising and removing these components. Extensive studies have shawn that
surfactants thatdo not contain NPEs are not effective in removing the problematic

components in hardwood extractives. The washed brown pulp is then bleached in the

bleaching operations to remove residual lignin and tum the fibres white. A series of

washing operations are used including sorne that operate in alkaline conditions, where
surfactants are also used to effect removal of residual lipophilic extractives. The

lipophilic materials are effectively removed under alkaline conditions and in the

presence of surfactants. If the lipophilic materials are not removed, they can build up

and accumulate on mill equipments, e.g., even blocking pipes in serious cases. Mills
that use hardwoods - such as eucalyptus - need to periodically shut down and clean

the whole process to remove the lipophilic materials, a process termed "boil-out".

This entails filling the lines with a series of cleaning agents that include alkaline and

surfactants at elevated temperatures. Here again NPEs have been the traditional
choice, due to their effectiveness and low cost. However, when the cleaning

chemicals are discharged into the mill effluents, there is a dramatic rise in the

concentration of NPEs in the receiving waters. Surfactants containing NPEs are also

sometimes added as lubricants on the pulp machine.

8Type of NPEs used: the difficulties of using hardwood (eucalyptus) and why

opera tors of such mills are more likely to need NPEs.

15. Pulps made from softwoods are easy to clean with alkali and surfactants, in general

due to the composition of the lipophilic materials that is easy to solubilise. The

lipophilic components in hardwoods, on the other band, are recalcitrant and difficult

to remove. lt has been ascertained that NPEs are very effective in the removal of

these lipophilic materials. 1 have done extensive studies over many years on NPE­
free surfactants and, so far, have not found any that are as good and effective as

NPEs. lndeed, 1 have worked with a North American mill that had planned to use

aspen hardwood in the manufacture of a certain grade of chemical pulp, but

abandoned the idea as good quality pulp could not be achieved without the use of
washing surfactants containing NPE. The removal of NPEs in cleaning agents has

necessitated the implementation of long and expensive procedures such as extra

washing at higher alkali charges and higher operating temperatures. These procedures

have drawbacks in terms of cost of using extra chemicals, cost of energy to operate at
higher temperatures, and possible damage to the fibres exposed to more alkali. Since

the Botnia plant uses hardwood, and claims not to use NPEs, it would be useful to get

information about the procedures used to achieve low and acceptable levels of

extractives in the final products made at the mill. 1understand that such information

has not been made publicly available, and have not been able to find such information
on the basis of web-based research.

The dangers posed by NPEs and why NPEs are banned in many places across the
world.

16. NPEs are highly toxic to fish and other water dwelling organisms and are considered
to be hormone disrupting substances, mimicking oestrogen. They degrade relatively

readily in the environment to form the even more harmful nonylphenol (NP). For

example, concentrations of nonylphenol as low as 0.017 mg/L (17 Jlg/L) have been

shawn to be lethal to winter flounder in 96 hour exposures. Nonylphenol is not

9 readily biodegradable and takes months or even longer to degrade in surface waters or

in soils and sediments, (where it tends to be easily immobilised). Non-biological

degradation is negligible. Bioconcentration and bioaccumulation is significant in
water dwelling organisms and birds, where it has been found in internai organs at

between 10 and 1000 times greater than the surrounding environment. Nonylphenols

are not broken down effectively in sewage treatment plants. Because of the

bioaccumulation and persistence of nonylphenol (the primary degradation product of
NPE), it is possible that it could be transported significant distances, and so have a

potentially global reach in its effects.

17. Due to these concerns, the use of NPE-laden products has been banned in pulp and

papermaking operations in the European Community. As far as I am aware, no such

restrictions exist in Uruguay.

18.Current commercial products used as surfactants contain concentrations of more than

0.1% of NPE by mass. They therefore cannot be used for the manufacturing of pulp

and paper, in accordance with EU Directive 2003/53. The levels vary from 1 to 6%.
Sorne NPE surfactants are sold as 100% actives and are added to the wash water at 1-

5 kg/tonne.

19.Possible alternatives to not using NPEs include: pulping softwoods instead of

hardwoods (supply limitations for the Botnia mill); wood seasoning to reduce the

amount of lipophilic extractives in the wood by natural means by leaving eut logs for

3-4 months (or in chip form for 3-6 weeks) before processing them for pulping; and
good debarking (bark contains 6 times more extractives than wood). I believe that the

Botnia mill is not implementing these alternatives because there is no ready

availability of softwoods in Uruguay. Wood seasoning is expensive as it ties up

capital and requires a lot land. Also, wood seasoning causes wood darkening and
fungal growths that then would result in extra costs for the mill due to higher

consumption of cooking and bleaching chemicals. Non NPE surfactants such as

alcohol ethoxylates (AEs) have been developed to replace NPEs in North America in

10 the past 5 years, but they are not effective for hardwood extractives. 1am not aware

oftheir use in South American mills.

20. NPEs are commodity products and therefore relatively cheap. The newly-developed

AEs are specialty products that are 3-4 times more expensive than NPEs.

Overall assessment and conclusions as to use of NPEs in sorne way at or on the

Botnia plant on the basis of the material to which 1have been referred.

21. 1have reviewed the data submitted by the Argentine Government. Assuming it to be

accurate, it provides convincing evidence of the presence of NPEs and their

degradation product, NP, in the matrices collected from the Uruguay River and an
analyzed pulp sample. The analytical protocols used are sound and have been

carefully carried out according to international standards. The data is consistent with

the conclusion that the Botnia plant is the source of the NPEs that have been detected.

This conclusion is considerably strengthened by the observation that the amounts of
NPEs in the analysed samples are highest at the mill effluent discharge points, and

there is no evidence of discharges in material quantities from other sources (other than

the mill) that may have contributed to the measured NPEs at such levels.

22. The prevalence of NPE-using industries that have similar problems as the pulp mill

and the lack of formai NPE prohibition in Uruguay lead me to believe that the high

quality hardwood pulp at the Botnia mill is most likely manufactured with aid of
additives that contain NPEs.

23. From data published by Botnia, it seems that the plant produces fully bleached
eucalyptus Kraft pulp. This type of pulp is weil known to require extensive removal

of extractives and lipophilic matter, and eucalyptus is notorious for difficulty in

achieving very low levels of the extractives in the final pulp. Cost considerations

11 would point strongly to the use ofNPE, since alternative cleaning processes are much

more expensive. Having carried out a general review of material that is publicly

available on the Botnia plant, I have not been able to find any information on the

cleaning process. I have been provided with a copy of Annex 48 to Uruguay's Reply,
a report by AMEC from September 2007. In the course of the oral arguments

Uruguay has claimed that this includes information on chemicals that are used as

cleaning materials at the plant. The AMEC report does not address the use of

surfactants and nonylphenol ethoxylates at the mill. The information at page 22 of the

AMEC report only refers to the defoamer. lt does so by reference to US
Environmental Protection Agency (EPA) Cluster Rule Requirements Related to

Emissions to Water, which do not regulate NPEs (see http://www.epa.gov/EPA­

TOX/2007/September/Day-05/t17542.htm). ltappears to me that if the AMEC report

had referred to European regulations on this issue then the mill would have had to
address the NPE issue. Accordingly, Uruguay was wrong to state that the AMEC

report had "specifically described the principal cleaning chemical used by the Fray

Bentos mill" (CR 2009/23, p. 14).

24. My comments on the information pxovidedin the affidavit ofMr. Gonzalez are set out

below.

25. I note that at paragraph25 of the arguments presented to the Court on 22 September

(CR 2009/17, p. 23), Uruguay addresses issues of monitoring, but has not challenged
the presence of elevated levels of nonylphenols in the vicinity of the plant's

discharges and has not provided any satisfactory explanation for such elevated levels.

Itis important to point out that the reason why European and Canadian mills do not

use NPEs is due to pressure from regulatory authorities and/or from customers.

Whether or not the mills are 'modern' has no bearing whatsoever on the use ofNPEs.
In the case of the Uruguay mill therefore, I would ask: is there evidence that the mill

is required to demonstrate that no NPEs are used? Canadian mills selling to Europe

for example have to demonstrate or certify that noNPEs were used in the mills.

26. At paragraph 27 of its submissions presented on 22 September (CR 2009/17, p. 24),

Uruguay accepts that there are nonylphenols in the river and addresses the question of

where else could they have come from. ltis my professional opinion, based on the

12 evidence obtained from the monitoring programme conducted by Argentina, that it

appears that the highest concentrations of NPEs are at the mill effluent discharge

point. 1would ask how this can be explained, other than by the suspicion that the mill

emits NPEs. Such suspicion is strengthened in my view by the fact that NPEs have

been detected in the pulp sample. 1am surprised that Uruguay bas not addressed this
point at ali, which seems to me to provide the clearest possible evidence confirming

the use of nonylphenols.

The statement produced by Ing Torres on 13 July 2009, in particular paragraph 4

27. 1 have read with interest the affidavit prepared by Ing. Torres on 13 July 2009. She

states that "The use of etoxilated nonylphenol in the paper manufacture industry can

be identified, but it is not directly identified with the wood pulp industry" (paragraph
4). lt is not exactly clear to me what this means. If it is intended to suggest that the use

of NPE is not associated with the wood pulp industry then it is inaccurate: for the

reasons 1describe above, NPEs have been extensively used in and are associated with

the production of wood pulp, especially from hardwoods such as eucalyptus. She

states that "Nonylphenol and its ethoxylates are not inherent elements in wood pulp
manufacture processes by the Kraft method or its bleaching by ECF (elementary

chlorine free)" (paragraph 1). lt is not clear to me what she means by "inherent": the

fact is that NPEs are extensively used in these activities around the world. She states

that "the plant of Botnia ... does not use nonylphenol nor its derivative etholixates in
any of its production and wood pulp bleaching processes" (paragraph 1). lt is not clear

to me what is meant by "production and wood pulp bleaching processes". NPEs are

not used in the pulp bleaching process or in the production process as such: they are

used in the cleaning processes 1 described above. It would be helpful if lng. Torres

had described by what methods the Botnia plant carries out its cleaning processes, and
if she were to provide a list of the commercial products and compounds used in those

cleaning processes. This information would be more definitive. She states that the

Botnia plant "does not generate nonylphenol nor its etholixate derivatives in any of its

processes" (paragraph 2). lt is not clear to me what is meant by the word "generate".
Typically the cleaning process does not "generate" NPEs, but rather it uses products

13 that contain NPEs, which would typically be discharged into the effluent. In sum, the

affidavit is very ambiguous, and uses terms that are strange. The useofNPEs in pulp

and papermaking is weil documented.

28. At paragraph 23 of its submissions made on 22 September (CR 2009/17, p. 23),

Uruguay relies on the affidavit of Dr. Alicia Torres to support the claim that the
Botnia plant does not use nonylphenols for any process, including the "cleaning of

pulp". As 1read the statement that is not what she says. Uruguay could have provided

concrete evidence on ail the chemicals used for the cleaning of the wood chips and the

plants itself, but apparently has not done so, with the exception of Mr. Gonzalez's

statement which 1 comment on below. Notwithstanding the limited and in sorne

particulars, incorrect, information provided by Mr. Gonzalez (describing a defoamer

as a 'surfactant' for example), the question that arises is this: how does the plant

address the problems encountered in producing clean and high quality pulps from

eucalyptus hardwood that is high in lipophilic content? Uruguay has provided no

explanation.

29. 1 note that at paragraph 28 of the submissions presented on 22 September (CR

2009/17, p. 24), Uruguay states that "it is convinced that there is no use of [NPEs] by

Botnia", adding that "At any rate, both Parties agree that Botnia should not use any

nonylphenols in its production, cleaning, or any otherprocesses". Uruguay then states

that: "If, if, contrary to everything Uruguay believes to be true, Botnia is using

nonylphenols, Uruguay will put a stop to it. ... " It appears from this statement that

Uruguay was, at that date at !east, unable to confirm that it was not using

nonylphenols. Indeed, it appears from the statement that Uruguay did not know at that

date whether NPEs were being used in any processes at the plant. My response to

these comments by Uruguay is to ask: Why is there no mill data relating to the use of

NPEs in the DINAMA report? Was this information left out on purpose? 1would have

assumed that DINAMA would have precise data from such an important industry.

The statement produced by Mr. Gonzalez, Environmental Manager at the Botnia

mill, dated 30 September 2009

1430. I have reviewed the affidavit of Mr. Gonzalez. In particular, I have noted the

comments on chemicals used at the Botnia mill made by Mr. Gonzalez in paragraphs

3, 5 and 6 of his affidavit. In my view, his comments do not explain or shed light on

how high quality eucalyptus pulp can be produced at the Botnia mill without the use

ofNPE surfactants. The pulp produced by the mill is reported to include FRB EUCA

which is described in Botnia's handbook on the mill as "a superior quality pulp of

even quality and high flexibility" (Sowing the seeds of sustainability, Botnia and the
Fray Bentos Pulp Mill", at page 101). The current published priee for Botnia's FRB

EUCA is USD 590 (effective 1 October 2009) which would confirm that this is not a

low grade pulp (source:

http://www .botnia.com/en/default.asp?path=204,21 0,211,2672,3058).

31. In my professional opinion, the mere addition of defoamer (even one incorrectly

described as a 'surfactant' by Mr. Gonzalez in his affidavit) in the washing process

will not be sufficient to achieve pulpof the quality which is produced at the mill. The

very fact that a defoamer is required, indicates to me that a surfactant is indeed used

in the washing process. I do not know of any surfactants other than NPE that can do

the job of effectively cleaning the pulp, unless the mill is implementing other

expensive cleaning strategies._ It. is striking that Uruguay bas still provided no

information on such strategies in the documents to which I have been referred. Thus,

given the strong evidence of NPEs in higher concentrations in the waters into which

the mill's effluent discharges are made, and given the failure by Uruguay or Botnia to

explain how the mill is able to produce good quality pulp using only the materials

referred to in Mr. Gonzalez's statement, I am bound to conclude that the evidence
points strongly to the conclusion that NPEs have been used - or are being used - at

the mill.

32. My detailed comments on Mr. Gonzalez's affidavit are as follows:

In relation to paragraph 3 of his affidavit, 1 wonder if Mr. Gonzalez is familiar with

the pulp making process? He states that "the brown stock" is "then subjected to in­

digester washing followed by severa! washing stages ... " This statement does not

make sense to anyone with familiarity with these processes, because wood chips are

converted to pulp in the digester after which they go to a blow tank and then to the

washing stages. Thus I do not understand what he means by "in-digester washing".

15Even more significantly, paragraph 3 of the affidavit does not give details on how the

lipophilic extractives are removed from the eucalyptus chips (as described above,

these extractives have to be removed to produce high quality pulp). It would be

useful, indeed essential in my view, in order to answer Judge Bennouna's question,
for Uruguay to have provided detailed information on this key issue. The fact that it

has not done so gives rise to even greater suspicion that it is at this stage in the

process that NPEs are used.

In relation to paragraph 5, I note that Uruguay claims to have supplied information on

"cleaning" chemicals used at the mill and that Mr. Gonzalez claims that the

extractives are removed by a "washing process that uses a surfactant...called BIM AF

4151". However BIM AF 4151 is a defoamer, it is not a surfactant (a cleaner).
Chemicals such as BIM AF 4151 are used to counteract the foam that results when a

surfactant is used. Thus, the fact the mill uses a defoamer indicates that there are

foaming problems at the mill, and the key question is: what is causing the foam? In ali

probability the foam is caused by the use of a surfactant. This raises the further
question as to the identity of the surfactant that is used in the washing process that

necessitates the need for a defoamer?

At paragraph 5, Mr. Gonzalez states that "surfactants help to remove air out of the
washing water/liquor." This is not correct: surfactants exacerbate foaming problems;

defoamers are used to remove foam, and not the other way round! Mr. Gonzalez

appears to be confused or Jackknowledge about processes and chemical products.

Also at paragraph 5 Mr. Gonzalez states that: "Extractives removed from the pulp
during the washing end in the 'black liquor"'. This is not entirely true. Sorne

extractives will come out with the black liquor in the early stages of the washing

when the concentrated black liquor is removed. After this, the wash liquid is not

mixed with the concentrated black liquor to avoid dilution: diluted black liquor is not
good for recovery boilers as its burning efficiency is reduced. Such wash liquids are

treated to remove the extractives by severa! means such as floatation or purging into

mill effluents. One of the main reasons for an effluent treatment system is to remove

the extractives. Since Mr. Gonzalez is in charge of environmental issues at the
Botnia mill, it puzzles me why he would say that wash liquids are not discharged to

the effluent. Where else can they go? Only mills that are 100% closed can claim this,

16 but the Fray Bentos mill is not one of them, so there must be wash process liquids that

are discharged into the effluent system and then into the river.

In relation to paragraph 6, I note that Mr. Gonzalez mentions the use of three

chemicals. '211' is an alcohol ethoxylate surfactant that, according to Mr. Gonzalez,
is used for hand cleaning equipment at the mill. As mentioned above, alcohol

ethoxylates are not as efficient as NPEs in removing hardwood lipophilic extractives,

and presumably this is why Mr. Gonzales does not state that this product is used in the

washing process at the Fray Bentos mill. The other two chemicals - PROFLOC 1408
and PROFLOC 2903 - are not surfactants at ali. They are flocculants or coagulants,

having an entirely different purpose.

The upshot of ali this is that despite the passage of time since Argentina first raised

this issue on 30 June 2009, Uruguay and Botnia have still not explained how the
lipophilic extractives are removed from the eucalyptus hardwood chips.

Conclusion

33. I am not able to express an absolutely definitive view. However, there are a number of

factors that are significant: the eucalyptus hardwood used to produce the pulp at the
plant; the absence of easily available alternatives to clean the eucalyptus or its wood

chips to remove lipophilic material; the issues of cost, taking into account the type of

pulp produced at the mill; the repeated failure on the part of Uruguay and Botnia to

provide detailed information on the cleaning processes used at the Botnia plant or the
compounds that are used; the strong evidence ofNPEs in higher concentrations in the

waters into which the plant's effluent discharges are made; the evidence of NPEs in

sample of sediments, clams, algal blooms; and the evidence of NPEs in samples of

pulp produced by the mill. These factors point strongly towards the clear conclusion

that NPEs have been used at the Botnia plant in one or more cleaning processes
associated with the production of wood pulp. In the light of my professional

experience, 1 would be very surprised if NPEs had not been used. If I were asked to

quantify my level of certainty that NPEs had been used, 1would put it at 95%.

1734. In conclusion, the arguments of Uruguay presented to the Court at the hearing are

contradicted by the evidence I have seen. relation to the question posed by Judge

Bennouna, the affidavit relied upon by Uruguay does not provide a complete answer
to the question and does not fully describe the "process and products ... used by the

Botnia plant for its cleaning". The failure to provide a complete answer reinforces the

conclusion that NPEs have been used at the mill.

35. I would be pleased to assist the Court in seeking to answer any further questions that

it might have.

,,

η6{-,Le~.:

Bruce Sitholé,B.Sc.(Hons), M.Sc., Ph.D., FCIC

18 Annex 1: Curriculum vitae

B. Bruce Sitholé

Address: 12Manor Crescent, Pointe Claire, Quebec, CANADA, H9R 4S9

Telephone: Home: 514-630-4824 E-mail: [email protected]

Citizenship: Canadian

SUMMARY

• Proven track record in developing innovative analytical methods to help solve
production problems and improve productivity
• Application ofFDA protocols in the analysis of food packaging
• Analysis of food additives and contaminants in food packaging
• Extensive interactions with both internai and external clients

• Very good communicator to both technical and non-technical audiences
• Well-versed in a variety of analytical techniques including LC-MS, HPLC, GPC,
GC, GC/MS, Py-GC/MS, ion chromatography, and FTIR
• Very good at building collaborations with personnel from other departments and

groups.
• Experience with washing and process aids
• Experience with use of surfactants in pulping and papermaking
• Consultations to pulp and paper mills in North America, South Africa and Brazil

WORK EXPERIENCE

Principal Scientist and Group Leader, Analytical Chemistry, 1987- 2009: Analytical
Sciences, Paprican, Pointe Claire, Quebec. Methods development and analysis of

phytosterols, wood extractives, deposits and additives in pulp and paper matrices. The
developed methods are used to solve production problems, assess environmental
pollution, improve mill production, and for reverse-:engineering studies to helpin new

product development. The analytical techniques used include LC-MS, GC/MS,
pyrolysis-GC/MS, FTIR, HPLC, GPC, SPE and ion chromatography. Troubleshooting
environmental and wet-end issues in paper mills.

Research Chemist: ONTARIO WASTE MANAGEMENT CORPORATION, May 1986
- June 1987. Characterization of and methods development for analysis of hazardous
industrial wastes.

Research Officer: NATI ONAL RESEARCH COUNCIL, Ottawa, October 1984 -April
1986.Research on in-door air pollution by GC/MS.

19Post-Doctoral Visiting Fellow: Environmental Health Center, HEALTH AND

WELFARE CANADA, Ottawa, December 1983 - September 1985. Analysis of
halogenated phenols in drinking water by GC and GC/MS.

Research Chemist: United Kingdom Atomic Energy Authority, Dounreay, Scotland,

1978 - 1979. Characterization of soluble organic matter by GPC, fluorescence
spectroscopy and ultrafiltration.

AWARDS AND HONOURS

United Nations Development Programme scholarship at the University of Sierra Leone,

1973-1977.

Third prize in an essay-writing contest held by the British Broadcasting Corporation in 1977.

Commonwealth scholarship at the University of Aberdeen, 1977-1978.

Commonwealth fellowship at Dalhousie University, 1979-1983.

NSERC Visiting Fellowship at Health and Welfare Canada, 1983-1985.

Presidential Citation, Pulp & Paper Research Institute of Canada, "For sustained leadership

and innovation in developing analytical chemical procedures for the pulp and paper industry",
1993.

Director, Papricourse (2 week course on the science of pulp and papermaking), Pulp & Paper

Research Institute of Canada, 1994-1998.

Elected Fellow ofthe Chemical Institute ofCanada, 1997.

W.A.E. McBryde Award for work in analytical chemistry, The Chemical Institute of Canada,
1999.

Section Editor, Pulp & Paper, Encyclopedia of Analytical Chemistry, John Wiley & Sons,
2000.

Chair, Fine and Coated Papers Committee, Pulp & Paper Technical Association of Canada,
1998-2002.
Certificate of Appreciation, Pulp & Paper Technical Association of Canada, 2002, "To
recognise individuals who have provided exceptional services to PAPTAC and/or the

Canadian pulp and paper industry".

Member, Editorial Board, TAPPSA Journal (South Africa) since 2008.

20International Scientific Committee Member, ISWFPC conferences (since 1997).

PROFESSIONAL MEMBERSHIPS
Chemical Institute of Canada

American Chemical Society

Association of Official Analytical Chemists

Pulp and Paper Technical Association of Canada

Technical Associationof the American Pulp and Paper Industry

PUBLICATIONS

• 72 reports and publications in refereed joumals
• 4 chapters in books

• 25 oral presentations at national and international conferences

EDUCATION

1) Ph.D. in Environmental Analytical Chemistry

Trace Analysis Research Center, Department of Chemistry, DALHOUSIE UNIVERSITY,

Halifax, Nova Scotia, Canada, 1983.

Thesis Title: The Analysis and Chemistry of Antibiotics and Amines in Model

Environmental Systems.

2) M.Sc. by course-work and thesis in Analytical Chemistry

Department of Chemistry, UNIVERSITY OF ABERDEEN, Scotland, 1978

Thesis title: Determinationf Antimony in Organo-antimony Compounds by AA and Flame
Emission Spectroscopy

3) B.Sc. (Hons.) Chemistry, UNIVERSITY OF SIERRA LEONE, Freetown, Sierra Leone,
1977

REFERENCES

Available upon request.

21PUBLICATIONS

1. B.B. Sitholé, 1980. Pollution - a growing problem in developing countries, YOUR

WORLD: INTERNATIONAL EDUCATION CENTRE NEWSLETTER, 2(2), 15 - 16.

2. J.W. Parsons, M.G. Kibblewhite, B.B. Sitholé and E.H. Voice, 1980. The chemistry

of soluble organic material in the Dounreay water supply from Loch Shurrey, In
WATER CHEMISTRY OF NUCLEAR REACTOR SYSTEMS, Proceedings of the
British Nuclear EnergySociety, Bournemouth, 2, 145- 150.

3. 3. I.L. Marr, J. Anwar and B.B. Sitholé, 1982. Micro-determination of antimony in
organo-antimony compounds by atomic absorption spectrophotometry, ANALYST,
107, 1212-1217.

4. B.B. Sitholéand R.D. Guy, 1985. The interaction of secondary amines with bentonite
clay and humic acid in dilute aqueous systems, ENVIRONMENT

INTERNATIONAL, 11,499-504.

5. B.B. Sitholé and D.T. Williams, 1986. A survey of halogenated phenols at forty

Canadian potable water treatment plants, J.SOC. OFF. ANAL. CHEM., 69, 807-
810.

6. B.B. Sitholé, D.T. Williams, C. Lastoria and J. Robertson, 1986. Determination of
halogenated phenols in raw and potable water by selected ion monitoring GC-MS, J.
ASSOC. OFF. ANAL. CHEM., 69,466-473.

7. B.B. Sitholé and R.D. Guy, 1986. Determination of alkyl amines by indirect
photometrie chromatography, ANALYST, 111, 395 -397.

8. B.B. Sitholé and R.D. Guy, 1986. The formation of N-nitrosodibutylamine from
precursors in model environmental systems,SCL TOTAL ENVIRONMENT, 50, 227-

235.

9. B.B. Sitholé and R.D. Guy, 1986. Separation of nitroimidazoles by high-pressure

Iiquid chromatography, TALANTA, 33, 95 - 97.

JO.B.B. Sitholéand R.D. Guy, 1987. Models for tetracycline in aqueous systems. Part 1.

Interaction with clay materials, WATER, AIR, SOIL POLLUT., 32, 303- 314.

11. B.B. Sitholéand R.D. Guy, 1987. Models for tetracycline in aqueous systems. Part 2.

Interaction with humic substances, WATER, AIR, SOIL POLLUT., 32,315-321.

2212. B.B. Sitholéand L.H. Allen, 1989. Determination ofnonionic nonylphenol ethoxylate
surfactants in pulp and paper mill process samples by spectrophotometry and HPLC,
J. ASSOC. OFF. ANAL. CHEM, 72, 273-276.

13. B.B. Sitholé, 1990. Interfacing a personal computer to a gas chromatograph for
complex organic analysis, The ANALYST (London), 115, 237-241.

14. B.B. Sitholé, B. Zvilichovsky, C. Lapointe and L.H. Allen, 1990. Adsorption of

nonylphenol ethoxylate surfactants on metal surfaces: effect on quantitation by liquid
chromatography, J. ASSOC. OFF. ANAL. CHEM, 73(2), 322-324.

15. L.H. Allen, B.B. Sitholé,J.M. MacLeod, C.L. Lapointe and F.J. McPhee, 1991. The

importance of seasoning and barking in kraft pulping of aspen, J. PULP and PAPER
SC!., 17(3), J85-J91.

16. B.B. Sitholé, P. Vollstaedt and L.H. Allen, 1991. Comparison of Soxtec versus

Soxhlet systems for the determination of wood extractives (lipids)TAPPI J., 74(11),
187-191.

17. B.B. Sitholé,J.L. Sullivan and L.H. Allen, 1992. Identification and quantitation of

wood acetone extractives (lipids) by gas chromatography and Lotus 1-2-3,
HOLZFORSCHUNG, 46(5), 409-416.

18. B.B. Sitholé,1992. Modern methods for the analysis of wood extractives: a review,

APPITA, 45(4), 260-264.

19. B.B. Sitholé, 1993. A rapid spectrophotometric procedure for the determination of
total free resin and fatty acids in pulp and paper matriTAPPI J. 76(10), 123-127.

20. B.B. Sitholéand L.H. Allen, 1994. Quantitative determination of synthetic polymers
in pitch deposits by pyrolysis gas chromatography, J. PULP PAP. SC!., 20(6):J168-
J171.

21. S. Nyarku and B.B. Sitholé, 1994. Analysis of alkyl ketene dimer (AKD) by
potentiometric titratioCAN. J. CHEM, 72:274.

22. B.B. Sitholéand K. Kingsland, 1994. Generation of slide-quality outputs from data
collected on HP Chemstation software, CANADIAN CHEMICAL NEWS, 46(8):8-9.

2323. B.B. SitholéandE. Milanova, 1994. A toxicity database on additives used in pulp and
paper manufacturing, PAPRICAN PULP & PAPER MISCELLANEOUS REPORT#
287.

24. B.B. Sitholé, S. Nyarku, and L.H. Allen, 1995. Chromatographie methods and

procedures for the determination of alkyl ketene dimer and its hydrolysis product in
pulp and paper matrices, THEANALYST, 120(4):1163-1169.

25. B.B. Sitholé, 1995. Application Reviews: Pulp and Paper, ANALYTICAL

CHEMISTRY, 67(12):87R-95R.

26. B.B. Sitholé, 1995. A novel spectrophotometric procedure for determining the acid
number oftall oilsJ.WOOD CHEM, 29(3):177-181.

27. B.B. Sitholé,T. Tran and L.H. Allen, 1996. Quantitative determination of aluminum
soaps in pitch deposits, NORDIC PULP PAP. RES. J.,11(2):64-69.

28. E. Milanova and B.B. Sitholé, 1997. A simple method for estimation of newsprint

dyes in effluents by solid phase extraction, TAPPJ.,80(5):113-118.

29. E. Milanova, S. Wood and B.B. Sitholé,1997. Toxicity ofnewsprint dyes to rainbow
trout and activated sludge, TAPPIJ.,80(5):113-18.

30. L.H. Allen, C.L. Lapointe, B.B. Sitholé and R. Truitt, 1997. Press roll pitch
deposition problems associated with the use of certain clay products in newsprint
manufacture, J.PULP PAP. SCl, 23(4):J157-160.

31. E. Milanova and B.B. Sitholé, 1997. Acute toxicity to fish and solution stability of
sorne biocides used in the pulp and paper industry, WAT. SCl TECH 35(2-3): 373-
380.

32. R. Jonasson, B. Fuhr, B. Sitholéand L. Allen, 1997. Studies on the occurrence of
glycosides in aspen wood and kraft pulp, Proceedings, 8h !NT. SYMP. WOOD &
PULPING CHEM., CPPA, Montreal, pp. 43:1-43:6.

33. M.J. Rocheleau, B.B. Sitholéand L.H. Allen, 1998. Fungal treatment of aspen for
wood resin reduction: a laboratory evaluation,.PULP PAP. SCl, 24(2): 37-42.

2434. L.H. Allen, C.L. Lapointe, B.B. Sitholé,R.E. Truitt and P.E. Sennett, 1998. Pitch
deposition in newsprint mills using certain kaolin pigments, TAPP1J.,81(7): 137-

138.

35. E. Milanova and B.B. Sitholé, 1998. Determination of methylene-bis-thiocyanate
biocide in effluents and in extracts of fortified tissue paper samples, J. PULP PAP.
SCl, 24(6): 173-177.

36. A.N. Serreqi, R. Leone, C. Breuil, B. Sitholéand B. Ambayec, 1998. Identification of
steryl esters in aspen wood by capillary GC, Proceedingih !NT CONF. BIOTECH
PULP PAPER INDUSTRY, CPPA, Montreal, pp. B11-B14.

37. B.B. Sitholé,D. Filion and S. Fletcher, 1998. Determination and classification of

contaminants in recycled pulp furnishes by screening techniques, PROG. PAP.
RECYC., 8(1): 34-44.

38. M.J. Rocheleau, B.B. Sitholéand L.H. Allen, 1999. Fungal treatment of aspen for
wood resin reduction: effect on aged aspen at room temperature and at 5°C,
HOLZFORSCHUNG, 53(1): 16-20.

39. B.B. Sitholé,D. Filion and L.H. Allen, 1999. A laboratory test to measure deposition
in recycled papermaking, PAPER TECH, 40(1): 26-30.

40. E. Milanova, S. Ellis and B.B. Sitholé, 1999. Aquatic toxicity and degradation of
products ofsome dithiocarbamate biocides, PULP PAP. CAN., 100(3): T92-93.

41. B.B. Sitholé and B. Ambayec, 2000. Identification and determination of surface
sizing agents on sized papers, PULP PAP CAN 101(9): 53-57.

42. B.B. Sitholé, 2000. Pulp and paper matrices analysis: Introduction, in

"ENCYCLOPEDIA OF ANALYTICAL CHEMISTRY: Applications, Theory and
Instrumentation", R.A. Meyers (ed), Vol. 9, John Wiley & Sons, New York, pp.
8337-8345.

43. B.B. Sitholé, 2000. Applications of analytical pyrolysis in the pulp and paper
industry, in "ENCYCLOPEDIA OF ANALYTICAL CHEMISTRY: Applications,

Theory and Instrumentation", R.A. Meyers (ed), Vol. 10, John Wiley & Sons, New
York, p. 8443-8481.

2544.B.B. Sitholé, 2000. Analysis and characterization of resin deposits, in "FITCH
CONTROL, WOOD RESIN & DERESINATION', E. Back & L.H. Allen (editors),
TAPPI PRESS, Atlanta, ch 12.

45.B.B. Sitholé & W. Kamutzki, 2000. Contaminants in recycled papers, in "FITCH
CONTROL, WOOD RESIN & DERESINATION", E. Back & L.H. Allen (editors),
TAPPI PRESS, Atlanta, ch. 14.

46.M. Polverari, B.B. Sithol& L.H. Allen, 2001. Effects of system ciosure on retention
aids for SC-Grade manufactureTAPPI J 84 (3): 56.

47. M. Polverari, L.H. Allen, B.B. Sitholé,P. Gagno& J.-F. Samuel, 2001. The effects
on retention and drainage of converting from 100% OCC to 50% OCC: 50% NSSC in
a closed-cycle paperboard milTAPPI J, 84(1): 99-104.

48. E. Milanova, S.M. Elli& B.B. Sitholé,2001. Aquatic toxicity and solution stability
of two organic corrosion inhibitors: 2-mercaptobenzothiazole and 1,2,3-benzotriazole,
NORDIC PULP PAP RESJ., 16(3): 215-218.

49. B. Aikawa, R. Burk & B.B. Sitholé,2001. Dechlorination of chlorinated mode] wood
resin compounds in supercritical carbon dioxide: implications for improved analysis
of chlorinated pitch deposiAPPLIED CATALYSIS B: ENVIRONMENTAL, 848, 1-

12.

50. B.B. Sitholé,2001. Scale deposition problems in pulp and paper millProceedings,
7TH BRAZILIAN SYMPOSIUM ON THE CHEMISTRY OF WOOD & OTHER

COMPONENTS, Belo Horizonte, Brazil.

51. M. Polverari, L.H. Allen and B. B. Sitholé, 2001. Effects of system closure on
retention and drainage aid performance in TMP manufacture. Part TAPPI J., 82(4):

188-192.

52. B.B. Sitholé& L.H. Allen, 2002. Impact of wood extractives on system closure,

TAPPSA J, Sept 2002: 22-28.

53. B.B. Sitholé, M-J. Rocheleau, R.W. Berlyn, C. Heitner and L.H. Allen, 2002. Is
fungal treatment of aspen chips beneficiai for CTMP? Proceedings, 11 TH

INTERNATIONAL CONFERENCE & EXHIBITION, TAPPSA, Durban, South Africa.

54. B.B. Sitholé,D. Filion, and J. Pimente], J., 2002. Is seasonal variability in mechanical
pulp quality due to variation in extractPAPRJCAN RESEARCH REPORT 1602.

2655.B. Aikawa, R. C. Burk, and B. B. Sitholé, 2003. Catalytic hydrodechlorination of 1-
chlorooctadecane, 9,10-dichlorostearic acid, and 12,14-dichlorodehydroabietic acid in
supercritical carbon dioxide,PPLIED CATALYSIS B: ENVIRONMENTAL, 43(4):
371-387.

56.M. Polverari, J. Hamel, B. Sitholé & L.H. Allen, 2003. A new retention aid for the
production of SC printing grades: pilot paper machine results,TAPPI JOURNAL,
2(9): 3-7.

57. B.B. Sitholé, B. Ambayec, and R. Beaudoin, 2003. Aplicao de pirolise-CG/EM
(cromatogarfia de gas/espectronetrai de mass) na industria de cellulose e papel:
analises de agentes de colagem fluoroquimicos no pape!, Special Supplement on

Paprican, 0 PAPEL, Ano LXIV (9): 10-19.

58. J.R. Wood, K.B. Miles, D.F. Wong, and B.B. Sitholé, 2003. Wood quality variations
in black spruce and balsam fir: Do they explain seasonal variations in pulp properties?

PRR 1638.

59. M. Douek, B.B. Sitholéand S. Banerjee, 2003. Survey of deposits and contaminants
in mills using recycled fibre,G. PAP. RECYCLING,13(1): 12-22.

60. B.B. Sitholéand L.H. Allen, 2003. A rapid method for estimating wood seasoning in
logs and wood chips by enzymatic colorimetrie determination of glycerides,
Proceedings, TAPPI 2003 SPRING TECHNICAL CONFERENCE PROCEEDINGS.

61. E. Milanova and B.B. Sitholé,2004. Migration of fluorescent whitening agents from
food packaging made from recycled paper, PAPER, FILM & FOIL CONVERTER,
78(3): 78-83, 2004.

62. B.B. Sitholé, B. Ambayec and R. Beaudoin, 2004. Analysis of fluorochemical sizing
additives in paper and mill deposits by Py-GC/MS, CAN J. ANAL. SCL
SPECTROSCOPY, 49(3), 148-155.

63. B.B. Sitholé and D. Filion, 2005. Determination of silicone defoamers in mill pitch
deposits,TAPPSA J.,Jan 2005.

64. B.B. Sitholé, 2005. A new method to measure the pH of wood chips, PULP PAP.
CAN, 106(11): T235-T238.

2765. B.B. Sitholé,2006. A new method to measure the pH of wood chips, TAPPSA J.,
February 2006.

66. B.B. SitholéJ. Pimentel, B. Ambayec, A. Gagne, M. Douek, and Larry Allen, 2008.
Evidence for the occurrence of polymerised wood resin in pulp and paper samples by
various analytical techniques, PROCEEDINGS, TAPPI 2008 ENGINEERING,

PULPING AND ENVIRONMENTAL CONFERENCE.

67. B.B. Sitholé, B. Ambayec, L. Lapierre, and L. H. Allen, 2009. A study of

polymerization of aspen (Populus) wood lipophilic extractives by SEC and Py­
GC/MS, PROCEEDINGS, ANNUAL MEETING, PAPTAC, MONTREAL.

68. B.B. Sitholéand E.J. Pimentel, 2009. Determination ofnonylphenol and nonylphenol

ethoxylates in pulp samples by Py-GC/MS, J. ANAL. APPL. PYROLYSIS, 85(1-2):
465-469.

69. B.B. Sitholéand P. Abbyad, 2009. Analysis of aluminum soaps in pitch deposits by
gas chromatography, inpress, TAPPI JOURNAL.

70. B.B. Sitholé, S. Shirin, X. Zhang, L. Lapierre, J. Pimentel, and M. G. Paice, 2009.
Deresination options in sulphite pulping, accepted, BIORESOURCES.

71. B.B. Sitholé, S. Shirin and B. Ambayec, 2009. Analysis and fate of lîpophilic
extractivesn sulphite pulps, accepted, J. WOOD CHEM TECHN.

72. B. B. Sitholé,B. Ambayec, 2009. Determination of silicone defoamers in pulp fibres

and deposits byPy-GC/MS, FPINNOVATIONS-PAPRICAN, PRR # 1899.

73. B.B. Sitholé, M. Doucette and R. Fiolet, Troubleshooting and controlling barium

sulphate scale deposition problems in an unbleached kraft paper mill, PAPRICAN
SPECIAL REPORT# 633.

74. B.B. Sitholéand B. Ambayec, Comparison analysis of fluorescent whitening agents in
formulations and paper samples byPy-GC/MS and LC/MS, under internai review.

75. B.B. Sitholé,J.Pimentel and S. Gibbons, Using Py-GC/MS to troubleshoot toxicity
problems in mill effluents, under internai review.

28 Consultation report:

Deresination of aspen in sulphite dissolving pulps: comparison of NPE and non-NPE

surfactants,conjidential interna! report, 2007.

29