Fa =EL IPPC Application Form

Attachment N’ D

Attachment D contains all the relevant infrastructural and operational information

pertaining to the change in the activity.

Completed IPPC Application Form 2005 Page 51 of 53

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Attachment N”- D

Attachment D contains all the relevant infYastructura1 and

operational information pertaining to the new activity, i.e the

acceptance of waste solvent Tom other sites for solvent recovery

on the Pfizer Ringaskiddy site.

Attachment D [Section 1 l] also provides proposed alterations

(which have previously been agreed between the licensee and the

Agency as part of the current licence Reg No. 542) to be

considered for inclusion to the text of the new license.

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INTRODUCTION 3

DETAILS OF EXISTING SOLVENT RECOVERY FACILITIES 5

CONTENTS

1. I

2.

3.

4.

5.

6.

ABATEMENT OF EMISSIONS OF VOLATILE ORGANIC COMPOUNDS 17

FUGITIVE EMISSIONS ARISING FROM SOLVENT RECOVERY ACTIVITIES 21

WASTES ARISING FROM SOLVENT RECOVERY ACTIVITIES 26

CAPABiLITY OF EXISTING SOLVENT RECOVERY FACILITIES 30

7. UNIT OPERATIONS LINKED WITH RECOVERY OF SOLVENTS FROM OTHER SITES 33

8. DETAILS OF RECEPTION PROTOCOL FOR INCOMING SOLVENTS FOR RECOVERY 35

9.

10.

11.

TRACEABILITY OF SOLVENTS FOR RECOVERY 36

TESTING OF SOLVENTS FOR RECOVERY 39

MANAGEMENT OF EXISTING LICENCE 40

ATTACHMENT D.l SITE LAYOUT

Drawing No. EIR-2-IOO-C4857, Rev. A

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I. INTRODUCTION

Pfizer Ireland Pharmaceuticals (PIP) Ringaskiddy Active Pharmaceutical Ingredient (API) Plant first was issued with an Integrated Pollution Control (IPC) Licence, Register Number 13, in 1995. This was revised to IPC Licence Register Number 370 in 1998 to allow for the operation of a new Milling and Blending Plant on site. This was further revised to IPC Licence Register Number 542 in 2000 to allow for the operation of a new organic synthesis plant, OSP4. In 2000, Pfizer Inc. acquired the Warner-Lambert company, and in 2003 it acquired Pharmacia. Sites at Loughbeg and Little Island in Cork and Pottery Road in Dublin that previously belonged to these companies are now part of Pfizer Ireland Pharmaceuticals.

Detailed descriptions of the site activities and facilities have been provided in the previous two licence review applications and in the original licence application mentioned above. The current licence review application is driven by the following:

The Ringaskiddy site has facilities for the recovery of solvents from waste streams which it uses to recover a large proportion of the solvents used onsite. Pfizer wishes to extend solvent recovery activities at the Ringaskiddy site to include the recovery of solvent from other sites. It is Pfizer’s understanding that this requires a change in the IPPC licence to include activity class 11.1 of the First Schedule of the Protection of the Environment Act, 2003 (The recovery or disposal of waste in a facility, within the meaning of the Act of 1996, which facility is connected or associated with another activity specified in this Schedule in respect of which a licence or revised licence under Part IV is in force or in respect of which a licence under the said Part is or will be required), in addition to IPPC activity class 5.16 (The use of a chemical or biological process for the production of basic pharmaceutical products). It is important to note at the outset that this activity will utilise technology and processes already in use on the site and will not result in a significant impact on the environment.

In addition, the Protection of the Environment Act, 2003, brought into force a requirement that all IPC licences be reviewed by the EPA and changed to IPPC (Integrated Pollution Prevention and Control) licences by 29” October, 2007. The IPPC licensing regime takes into account changes in EU environmental legislation between 1996 and 2003 and places additional conditions on the licensee not previously covered by the IPC licence. It is our understanding that the Agency may take this opportunity to review the site’s licence in respect of these changes.

This review also provides an opportunity to incorporate details previously agreed between the licensee and the Agency as part of the current licence.

Consultation with the Environmental Protection Agency established that a full application form was not required, but that the review application documentation should address the following:

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1. Details of the existing solvent recovery facilities (refer to Section 2 of this document);

2. Capabiiities of existing solvent recovery facilities and how incoming wastes will be proven to be capable of recovery in these facilities (refer to Section 6 of this document);

3. Traceability of accepted wastes (refer to Section 9 of this document);

4. Details of the reception protocol for incoming wastes (refer to Section 8 of this document);

5. Testing of accepted wastes (refer to Section IO of this document);

6. Issues previously agreed with the Agency by letter and issues foreseen by the licensee (refer to Section 11 of this document)

The proposed new operation of the recovery of solvent from other sites would have the following environmental benefits:

1.

2.

3.

4.

5.

The proposed new arrangement would greatly facilitate progress towards a more integrated waste management structure for Pfizer in Ireland.

There would be proportionately fewer loads of waste solvent exported by PIP from the State for recovery or disposal abroad.

There would be proportionately fewer loads of virgin solvent required by PIP to be imported from abroad, thereby minimising the depletion of non-renewable natural resources

The proposed new arrangement would facilitate management of waste solvent by a recovery route (R-code) rather than by a disposal route (D-code).

The new activity would be transport neutral in the Cork region, i.e. there would be no net increase or decrease in the number of road tankers used by PIP. It would significantly reduce the number of longer journeys required and thereby reduce vehicle emissions.

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2.

2.1

DETAILS OF EXISTING SOLVENT RECOVERY FACILITIES

Introduction The production of pharmaceuticals involves the use of organic solvents, which must be disposed of efficiently or recovered. Where feasible at the Ringaskiddy facility, solvents are recovered and reused in the manufacturing process to minimise the amount of solvent sent for disposal. Solvents are well-defined materials whose physical and chemical properties are well known and for which analytical methods exist that enable them to be specified to very tight limits (down to ppm levels in most cases). With the appropriate test regime and qualification protocols in place, the quality of recovered solvent can be assured, enabling it to be reused in a highly controlled, but flexible way.

Solvent recovery is undertaken on this site by the use of distillation towers and pervaporation. See Figure 1 for a basic flow diagram of solvent recovery operations. Solvents are recovered in three areas on site: OSP3 has two recovery towers; OSP4 has two recovery towers; and Production Services has four recovery towers and one pervaporation unit. The solvent recovery areas are shown in Attachment D.1. The technologies associated with distillation and pervaporation are discussed below in Section 2. Solvent recovery operations on the site are the responsibility of the Production Department.

In 2004, 15,078 Tonnes of solvents (nineteen in number) were introduced into the site for use. The fate of these solvents is shown in the Figure 2 below. Onsite recovery and re-use accounts for a large proportion (25%) of the solvent used onsite in 2004.

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ISOLVENT WASTESTREAM

SOLVENT RECOVERY I I

r-4 PRE-TREATMENT/ NEUTRALISATION

l-l

DISTILLATION A

I 1 bj PERVAPORATIONF

-/RECOVERED sowers>

OFF SITE DISPOSAL

FIGURE 1: UNIT OPERATIONS SOLVENT RECOVERY

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Figure 2: Solvent Fate Percentages (2004)

2.2 Pre-treatment Certain streams may require pre-treatment (e.g. pH neutralisation) prior to entry to a distillation column. Such pre-treatment may be performed at the originating site or in existing onsite vessels. In the future, pre-treatment vessels may be provided onsite to allow more efficient pre- treatmenffneutralisation as required.

2.3 Distillation Distillation is used to separate a mixture of liquids. The basis for this separation is the differing volatilities of the components. Separation is achieved by the redistribution of the components between the liquid and the vapour phases. The more volatile component(s) concentrates in the vapour phase while the less volatile component(s) concentrates in the liquid phase. The two phases are generated by vaporisation and condensation of the feed mixture within a distillation column. The derived product is withdrawn from a particular point in the distillation tower.

Distillation column

A distillation column IS a tall cylindrical-shaped vessel. The column encloses a contacting device which is used to bring the liquid and vapour phases into intimate contact. The contacting device used in a distillation column may be packing, trays or plates. The distillation process is illustrated in Figure 3.

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DISTILLATION COLUMN

FEED

CONDENSER

VENT

REFLUX DIVIDER

REFLUX 4

- A , __--_-----+’

-

IRE-BOILER

FIGURE 3: PFD FOR DISTALLATION

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The feed material which is to be separated into its components is introduced at one or more points along the column shell, or, in certain recoveries, is fed directly to the main pot. The heat within the column causes the more volatile part of the feed to enter the vapour phase. Because of the difference in gravity between the vapour and the liquid phases, the liquid runs down the column while the vapour goes up the column contacting the downcoming liquid and causing it to vaporise. This partial vaporisation of the downcoming liquid and partial condensation of the rising vapour is repeated along the length of the column. The liquid reaching the bottom of the column enters the reboiler where it is partially vaporised and sent back up the column. Part of the remaining liquid may be withdrawn as bottom product. The vapour reaching the top of the column is cooled and condensed to a liquid in the overhead condenser and diverted to a reflux pot/decanter where water can be removed by decanting. Part of this liquid is returned to the column as reflux. The remainder of the overhead stream is withdrawn as the overhead or distillate product. Any non-volatile solids are left in the pot of the column and disposed of by incineration or sent for treatment in the onsite waste water treatment plant (WWTP).

Control Eauipment

All distillation columns are fully automated and are controlled by a number of pre-programmed sequences which are initiated and run on the plant distributed control systems (DCS). The DCS also displays the current parameter status including any alarms. Thus the operation of any distillation column can be monitored fully in the control room via the DCS.

Figure 4 shows the control equipment typically associated with a distillation column. Among the features to note are the following:

l The distillation towers and associated equipment have actuated valves which are controlled by the plant DCS system.

l There are level transmitters on the main pots, reflux pots, decanters and recovered product test-tanks which allow level control.

0 There are control valves on the feed, reflux and product lines which allow the flowrates to be controlled based on a set points stated in the DCS recipes.

0 There are a number of temperature transmitters on the distillation towers and associated equipment. The temperature transmitters are used to control the recovery of solvents and also as a non- specific indication of distillate product quality.

0 In the case of OSP3 and OSP4, all equipment on the distillation towers are vented into the VOC abatement systems.

s There are high level switches on the main pots, reflux pots and decanters to protect against overfilling. If activated, the distillation tower is shutdown automatically.

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l There are pressure relief valves or rupture discs on the distillation columns, main pots, reflux pots and decanters to protect against overpressure.

l There are flame arrestors on the distillation columns and associated equipment.

Calibration and Maintenance of Kev equipment

Written procedures are in place for the inspection, calibration, maintenance and recording of all key items of plant and instrumentation, and these procedures are compiled in the Engineering Calibration and Preventative Maintenance manuals.

All work is carried out within the confines of Pfizer Engineering Standards.

Any work carried out by outside contractors is done within strict guidelines and conforms to Pfizer standards.

Records of all inspections, calibrations and the certificates of test/master calibrating equipment are held in the Maintenance offices.

The records of calibrations indicate which test/master instrument was used for the calibration.

Instrumentation calibration and inspection record sheets are retained in the Maintenance offices. The scheduling of calibrations is achieved with a software package and calibrations are carried out on a planned basis in accordance with the availability of the equipment. The frequencies at which calibrations and inspections are carried out vanes between individual plant items, but is based on experience, good manufacturing and engineering practices, and the service history of the instrument.

Certain instrumentation is deemed to be critical, from a safety, quality or environmental perspective. All critical instrumentation is inspected and calibrated at least annually.

Emissions from a distillation column

Normal operation

Gaseous emissions: During normal operation of the distillation column vapours generated during distillation are condensed in the overhead condenser or in the vent condenser. In Production Services, those vapours that are not condensed are emitted to atmosphere through the vent. In OSP3 the recovery tower emissions are ducted to the OSP3 volatile organic compound (VOC) abatement system: this comprises acid and caustic scrubbers, a guard scrubber and an absorption column containing a non- volatile liquid which traps any non-condensable organic compounds (refer to Section 3.1 below). In OSP4 the emissions from solvent recovery towers are ducted to the Thermal Oxidiser (refer to Section 3.2 below).

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Liquid emissions: Liquids are emitted from the distillation column as distillate product and bottoms product.

Solid emissions: Some residual solids could be entrained in the liquid wastes.

Fugitive emissions: Fugitive emissions may occur through flanges and seals. Any liquid spillages are contained in bunded areas and sent to the waste water treatment plant for processing.

In Production Services Solvent Recovery, some volatile materials that do not condense may be lost to atmosphere from the top of the distillation column. Such fugitive emissions are discussed in Section 4 below.

In OSP3 Solvent Recovery the emissions from the towers are removed by the VOC plant, so fugitive emissions are minimised. VOC absorption is discussed below in Section 3.1.

In OSP4 Solvent Recovery emissions from the towers are fed into the Thermal Oxidiser, and are thus minimised. Thermal oxidation is discussed below in Section 3.2.

Stat+up/shutdown

Emissions during start-up and shutdown are similar to those during normal operation.

Cleaning

Emissions during cleaning will be similar to those during normal operation.

Process Malfunction

Any process malfunction which gives rise to overpressure in the reboiler, distillation column or in the reflux pot may also give rise to emissions to the atmosphere. If the overpressure exceeds the set pressures of the emergency relief valves and bursting discs, then the relief valves will open and the bursting discs will rupture to allow liquid, vapour or a two-phase mixture to discharge to atmosphere. Overpressure could be caused from the following process malfunctions:

l Pressure build-up due to abnormal heat input through the steam- heated reboiler bundle.

l Pressure build-up due to external fire. l Pressure build-up due to blockages or restrictions in pipelines.

Any over-pressurisation of the system will be detected by the high pressure alarm on the column. This automatically shuts the steam valve to the reboiler and allows immediate action to be taken to reduce the pressure safely.

Power Failure

In the event of a power failure, the actuated valves will fail safe. Thus the steam supply to the reboiler will be stopped, allowing the column to cool and halting the formation of solvent vapours. Any vapours which do not condense

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2.4

within the column will be discharged to atmosphere or the relevant abatement system through the vent system.

In the event of loss of cooling water to the condensers, the vapours emitted from the column will be discharged to the atmosphere or the relevant abatement system through the vent system. However, such an event will be detected by the control system, which would allow immediate action to be taken to correct the problem.

Pervaporation Pervaporation is a membrane-based process for the separation of water from a liquid organics stream. It is used at Ringaskiddy to dehydrate solvent-based distillate recovered from production waste streams. This separation was previously carried out by performing a number of distillations. Now only one distillation is required prior to the pervaporation operation, to remove solids and adjust pH as necessary. This distillation may also remove water down to the azeotropic point.

The pervaporation system, as shown in Figure 5 separates the ‘wet” solvent into a “dry” product stream and an aqueous waste or permeate stream. A typical feed may contain 10% water. The product stream may have water percentages reduced to typically less than 0.5% and the permeate stream will be 95% water and 5% solvent.

Pervaporation is carried out by passing the wet solvent over a hydrophilic membrane, which preferentially allows water to pass through, while retaining the solvent. The feed stream is pressurised and heated to near the boiling point of the contaminant (water) and the down stream side of the membrane is placed under a high vacuum. The net effect of the vacuum and the heat is to cause the water to vaponse as it passes through the membrane. On the vacuum side of the membrane, the vapour is condensed and collected as permeate. As a small percentage of solvent passes through the membrane, the permeate is not pure water. The permeate may be recycled for further treatment to minimise the solvent loss, or it may be sent to the WVVTP for treatment.

Control Philosophy

The overall system control is by means of a PLC, which provides the various loop controls as well as a number of operating sequences such as those for long or short term shutdown, cleaning, solvent selection, etc. Figure 6 illustrates the control equipment associated with the pervaporation system.

The feed solvent to the unit is analysed and filtered beforehand to ensure that there are no materials present which can damage the membranes or attack the materials of construction.

Calibration and Maintenance of Kev equipment

The calibration and maintenance of key equipment is in accordance with the procedures outlined in Section 2.3 above.

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EXCHANGER EXCHANGER

PUMP

< WATER PERMEATE

-lEAT

VACUUM VESSEL

Ji XV 1 PERMEATE VESSEL

FIGURE 5: SCHEMATIC OF PERVAPORATION PLANT

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L---

----

--L-

----

----

----

----

--

--.

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Emissions

Normal operation

Gaseous emissions: The pervaporation unit itself is essentially a closed system. The gases leaving the system are mainly non-condensables drawn through the vacuum pump. Any vapours passing through the pump are passed through a glycol-cooled condenser to further remove solvents and the discharge is then fed to the OSPI VOC absorption plant where any remaining VOCs are removed.

Liquid emissions: The liquid waste stream from the pervaporation unit consists of the water extracted from the solvent plus a small percentage of solvent carried over through the membrane. This stream is returned to storage from which it may be m-distilled and run through the pervaporation unit again, as part of a new batch of distillates. Alternatively, it may be sent to the site WWTP for treatment.

Solids emissions: There are no solids emissions from the unit.

Fugitive emissions: The permeate pumps on the unit are of the seal-less type so there will be no running losses. Normal working losses from the storage tank are discussed in Section 4.2.2. Any non-condensable from the vacuum pump are ducted to the OSPI VOC plant.

Start-up/shutdown

At the start of a new recovery campaign, the first portion of solvent through the pervaporation unit is sent for disposal.

Cleaning

As the unit is multipurpose, there is a comprehensive cleaning cycle, which involves isolating the solvent supply to the unit. On completion of a recovery campaign, nitrogen is used to blow the remaining solvent in the lines back to the feed tank. The waste solvent from cleaning is reworked to separate and recover the solvents, or is disposed of offsite.

Process Ma/function

All critical functions are monitored by the PLC which upon detection of a malfunction sends the unit into a short-term shutdown mode where it puts unit operations on hold until the fault has been corrected. In this mode, the steam is shut off and the product stream is redirected to the feed tank. The glycol remains on to condense any vapours remaining in the system. If the glycol were to fail, the vent from the vessels feeds to the OSPI VOC absorption plant.

Failure of the feed solvent pump will result in the unit going into short-term shut down as outlined above, based on a low feed flow switch.

Power failure

If the power supply to the PLC is interrupted, the system goes into short-term shut down mode. Similarly, a power failure in the field on a pump or instrument will also drive the system to short-term shut down.

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3.0

3.1

ABATEMENT OF EMISSIONS OF VOLATILE ORGANIC COMPOUNDS

Full details of the site’s volatile organic compound (VOC) abatement systems were included in the site’s IPC Licence Applications of 1994 and 2000. Please refer to these documents for details of these systems. A summary description of these systems is provided herein. VOC monitoring remains in accordance with the site’s IPC Licence Register Number 542.

WC Absorption There are absorption plants for the removal of VOCs from the emissions to air from three plants on site: OSPI, OSP2 and OSP3.

Process emissions from each plant are minimised by condensation. The combined process emissions are then treated in an emission treatment system comprising scrubbers and a VOC absorption unit. The emissions from each plant are monitored continuously and discharged to the atmosphere at the licensed emission points V3 (OSP?), V2 (OSP2) and V5 (OSP3).

A typical flow diagram for an absorption system is shown in Figure 7 attached. The principal elements of the system are two columns: an absorption column and a desorption column. Both columns are packed with a high performance structured packing.

Waste process vapour, having been treated by an acid or caustic scrubber, followed by a guard scrubber, is fed to the base of the absorption column. As the VOC-laden vapour passes up through the column it is washed counter- currently with an organic liquid absorbent (currently polyethylene glycol dibutyl ether). The absorbent absorbs VOCs from the vapour stream with the result that the treated vapour discharged to atmosphere from the top of the column is in compliance with the IPC Licence Register Number 542.

The absorbent collected at the base of the absorption column, now containing VOCs, is pumped to the desorption column to be regenerated. In the desorption column, which is operated under vacuum, the VOCs are separated from the absorbent using steam stripping. The steam and stripped VOCs pass from the top of the desorption column to a condenser where they are collected. Purified absorbent is pumped from the base of the desorption column, via a heat exchanger and a cooler, to the top of the absorption column.

Absorbent is continually circulating between the absorption and desorption columns. Therefore, the waste vapour passing through the absorption column is continuously contacted with pure absorbent. Consequently, the removal of VOCs from the vapour stream is maximised.

Each VOC absorption system is fully automated and ties into the plant control systems.

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PROCESS AIR FROM SCRUBBER

TREATED AIR TO ATMOSPHERE

CONDENSER

CAUSTIC

I=- ~

CA% RECIRCUL

Pub

GUARD

SCRUBBER

.I. 3 ;TIC .ATI AP

ON

I/ -F

ABSOR PUI\

ABSORPTION COLUMN

WATER TO \ WASTEWATER

DECANTER TREATMENT PLANT/

I \

EXCHANGER EXCHANGER

STEAM

ABSORBENT PUMP

BESORPTION COLUMN

1 FIGURE 7: PFD FOR VOC ABSORPTION SYSTEM

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3.2 Flameless Thermal Oxidation

Flameless thermal oxidation (FTO or Thermatrix Thermal Oxidiser) is the end-of-line abatement technique used in OSP4 to remove VOCs from process exhaust vapour prior to release to atmosphere. The OSP4 solvent recovery towers vent to the thermal oxidiser. Figure 8 shows the FTO process schematic.

The gaseous stream from the plant passes through vent condensers and appropriate scrubbers prior to entering a “knock-out” pot that removes entrained particulate matter and liquid droplets and acts as a buffer tank. The stream is diluted with air on entry to the reaction chamber. The fume oxygen content and lower explosive limit (LEL) are monitored continuously to ensure that the mixture fed to the FTO system does not enter the flammable range.

As the amount of solvent vapour in the process emission is variable, it is generally not sufficient to supply all the energy to maintain the reaction chamber at its optimal operating temperature. Natural gas is used as a supplemental fuel to maintain the operating temperature.

Thermal oxidation of organic compounds in the gas stream takes place in a refractory-lined reactor filled with inert heat-resistant ceramic packing. The typical operating temperature is approximately 1040 OC. The VOC-rich gas stream and natural gas are premixed and then passed into the reactor via a dip-tube. Midway through the reactor the mixture reaches a reaction zone where the temperature rises rapidly. The organic compounds react at a concentration below their lower flammability limit so a high temperature flame does not occur. The ceramic matrix stores heat and enables the reaction to occur in stable conditions right across the reactor. Any organic compounds in the stream are oxidised thermally to primarily carbon dioxide and water vapour. As all the solvent mixture passes through the reaction zone, the thermal reaction is essentially complete. This results in a VOC destruction efficiency of greater than 99.99%.

The reaction zone temperature is measured by thermocouples. The natural gas input varies depending on the fuel level in the gas from the header to maintain a constant enthalpy level.

The outlet gases are cooled from approximately 1040 OC to approximately 290 OC by a waste heat boiler that generates steam for use on site. This means that a large proportion of the energy from the VOC stream and the additional natural gas is recovered for use. The hot gases then pass through a fine water droplet quench to cool them further to approximately 55 - 60 OC, followed by a final caustic scrubber to remove any remaining acid gases, if present. The final treated air stream then passes through a plume suppression system so that no visible plume exists at ambient conditions.

The thermal oxidiser is fully automated and ties into the plant control systems.

The final emission to atmosphere from the thermal oxidiser is at the licensed emission point VI 3.

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TO&imphere

I 1

I dOWJS22t4 OxKBser Fume Blow% Bmass

*tern smass

* FAA.2214 F&?Water Tank

ONE.2214 FeerpwaterPumps

Figure 8: PFD of the Therrnatrix Thermal Oxidiser OAOE.22I4

auencn RecIIcUIobon

Pump

OAFlo-221 4 Scrubbar

ROClrtUIabbn Pump

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4.1

i=UGlTlVE EMISSIONS ARISING FROM SOLVENT RECOVERY

ACTIVITIES

Fugitive emissions (general) Fugitive emissions are defined as “low-level diffuse volatile organic compound emissions that occur when process fluid (either gaseous or liquid) escapes from the plant equipment”. By their nature, fugitive emissions are difficult to track, although there are a number of calculation methodologies for their estimation.

The total estimated worst-case fugitive emission of solvent as calculated in the site’s Pollution Emissions Register for 2004 was 75 Tonnes, i.e. 0.51% of total solvent input. This arose from all operations utilising solvent, not merely solvent recovery activities. This is calculated using conservative worst-case methodologies, primarily based on a US-EPA average emission factors approach. Full details are given in the site’s Pollution Emissions Register, submitted annuallv to the Agency as part of the site’s Annual Environmental Report.

4.2 Sources of fugitive activities

emissions arising from solvent recovery

The sources of fugitive emissions of solvent arising from solvent recovery activities on site are as shown in Table 1 below:

Table 1: Potential sources of fugitive emissions in each solvent recovery area

Note that the pervaporation unit in Production Services is connected to the OSPI VOC plant; the OSP3 recovery towers are connected to the OSP3 VOC plant, and the OSP4 solvent storage tanks and recovery towers are connected to the Thermatrix, thus fugitive emissions from these items of plant are minimised.

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4.2.1 Abatement of fugitive emissions from storage tanks in Production Services Solvent storage tanks in Production Services are fitted with conservation vents, abatement systems designed to minimise fugitive emissions of solvent vapour to atmosphere from the tanks.

The conservation vent is normally closed and so prevents emissions to air from the storage tank. Pallets in the conservation vent housing allow intake of air and escape of vapours as the tank normally breathes in and out. The pallets open and close to permit only that intake or outlet relief necessary to remain within permissible working pressures.

4.2.2 Estimation of fugitive emissions from storage tanks The US EPA provides a software model, TANKS 4.0, which calculates the fugitive emissions from storage tanks. In this model are entered the following details on each tank: shape (e.g. horizontal/vertical); dimensions; capacity; volume; solvent composition; annual throughput; and number of turnovers of solvent in the year. The TANKS 4.0 model then uses vapour pressure methodologies to work out the emissions: The total losses from fixed roof tanks are equal to the sum of the standing storage (breathing) losses and the working losses.

Results from the TANKS 4.0 model are used regularly to estimate fugitive emissions from working losses and breathing losses. These estimates contribute to the total figure for fugitive emissions reported on an annual basis in the Pollution Emissions Register in the Annual Environmental Report. In 2004, the total fugitive emissions from those storage tanks in Production Services associated with solvent recovery are estimated to have amounted to approximately 2.93 Tonnes, i.e. less than 0.08% of the total amount of solvent recovered.

4.3 Emissions during solvent recovery operations (distillation) During the distillation process, solvent is heated by the application of steam to the pot still. It evaporates and then condenses and is collected. Vapours from the distillation equipment pass through a second vent condenser. The condenser operates at a cooling water inlet temperature of 18OC. Solvent enters the still as a liquid at ambient temperature (assumed to be 12OC) and exits as a fugitive emission as vapour at a maximum of 22OC. An estimate of the solvents recovered onsite during 2004 shows that a total of approximately 413 Kg was lost as fugitive emissions from the distillation process during solvent recovery (26 Kg during heat-up; 149 Kg due to transfers in and out of the solvent recovery equipment and 238 due to transfers into test tanks).

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4.4 Leaks from valve seals, pump seals and flanges Fugitive emissions arising due to leaks from seals and flanges are difficult to quantify, however engineering standards and controls on the site keep these to a minimum.

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Valve Seals: Valves are specified within the Pfizer Ireland Pharmaceuticals engineering standards in line with specific applications. All valves utilized have been deemed technically acceptable and their performance is monitored on an ongoing basis. These valves have two sealing mechanisms. The primary seal is the valve ball or plug, against the PTFEITFM (Modified PTFE) seats, with an additional spindle seal on the shaft.

The failure of the primary seal is normally detected as part of the normal operational performance of the valve, thus repair is instigated at an early stage, without excessive reliance on the secondary seal.

Pump Seals: Single and double mechanical seals are utilized on site. Single seal pumps are utilized in Production Services. The main type of seal utilized on site is a double mechanical seal, with a sealing fluid pressurizing the space between the seals. Thus it is necessary for two seals to fail before any emission can occur.

Dry running seals are utilized in applications where pure fluids are being pumped. These have proved to be reliable, with low failure rates.

A major category of pumps on site are seal-less pumps. These pumps are totally enclosed, and cannot leak because of seal failure.

Nitrogen Gas Seals for use on Agitators: These seal units admit a controlled flow rate of filtered nitrogen, at a pressure in excess of the process equipment pressure between the seal faces. This is done in order to provide a very small amount of seal face separation to maintain sealing and cooling.

Flanges: All gaskets utilized to seal flanges are in accordance with the Pfizer Ireland Pharmaceuticals engineering standards. Gasket material is identified in each piping specification. These gasket materials have been technically verified and tested and in turn deemed to be fit for purpose. The primary protection against leaking flanges is system testing for leaks before use in a process.

4.5 Total fugitive emissions from solvent recovery activities (2004) The total estimated fugitive emissions from solvent recovery activities onsite during 2004 is as follows in Table 2.

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Table 2: Estimated fugitive emissions from solvent recovery activities in 2004

Amount of solvent recovered in 2004 1 3,784,200 Kg

Note: Fugitive emission calculations associated with filling of road tankers o recovered

Emissions from solvent recovery towers

Total fugitive emissions due to solvent recovery activities

413 Kg

3343 Kg

Estimated Emissions from storage tanks associated with solvent recovery

solvent, destined for return back to other sites, are not included as this activity did not take place in the past.

Fugitive emissions from solvent recovery are therefore estimated to be 0.09% of total solvent recovered onsite.

4.6 Projected future fugitive emissions from solvent recovery activities The site has a capability to recover a maximum of approximately 12 million litres of solvent per annum (see Section 6.1 below). Of this, 6 million litres would be expected to involve the recovery of material generated onsite for re- use on site, whilst 6 million litres could be solvent from other sites recovered at Ringaskiddy.

This is a theoretical maximum recovery. However, it is not anticipated that solvent recovery would typically achieve these volumes onsite. The projected recovery volumes for 2006, for example, are for 4.8 million litres of solvent originating at Ringaskiddy and 2.3 million litres of solvent recovered originating at other sites.

Table 3 below shows the estimated fugitive emissions arising from two scenarios: the projected recovery volumes for 2006, and the maximum recovery possible.

For these purposes, an average solvent density of 0.9 is assumed.

Filling/emptvinq of road tankers

Solvent from other sites recovered at the Ringaskiddy site may be returned to the other sites for re-use. This is an additional operation not currently performed on site. During filling of road tankers, a certain amount of solvent vapour is lost from the tanker headspace via the vent. It is assumed that such emissions contain solvent vapour at 25% saturation in air.

Furthermore, a small amount of solvent is expected to be lost from flexible hoses as a result of emptying and filling of road tankers. The solvent contained in one flexible hose (6m in length) has been calculated as

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approximately 2OKg, of which 1-2 % would evaporate, i.e. 200-4OOg of solvent. The remainder will be washed down through the weak effluent system in the waste water treatment plant. It is assumed for these purposes that solvent is moved both on and offsite in 20,OOOL lots.

Table 3: Estimated future fugitive emissions from solvent recovery activities*

*These figures assume that 20% of solvent recovery/storage will take place in OSP4 and will result in no resulting fugitive emissions

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5.0 WASTES ARISING FROM SOLVENT RECOVERY ACTIVITIES Wastes arising from recovery of solvent from other sites will be dealt with in the same manner as wastes from current solvent recovery operations. All wastes generated onsite will continue to be reported annually to the Agency in the site’s Annual Environmental Report. As the new activity, i.e the acceptance of solvent from other sites for the purposes of solvent recovery onsite at Pfizer Ringaskiddy, is to recover as much solvent as possible, waste generation will be minimised. The quantity of waste arising from each recovery process will vary dependent on the recovery yield. For example, the recovery process for a toluene based waste stream from Pfizer Loughbeg is estimated at 85%. This implies that 15% of the incoming toluene based stream will remain as a waste stream. In 2006, it is envisaged that 2.3 million litres of solvent will be accepted from other Pfizer sites for recovery onsite at Ringaskiddy. Based on an 85% recovery yield this will give rise to approximately 345,000 litres of waste. Where possible the waste streams will be treated in the onsite wastewater treatment plant. Those that require to be sent offsite for incineration will be shipped in accordance with the Pfizer Ringaskiddy waste management procedures. Typically waste streams from this site are sent for disposal under one of the following EWC codes:

070501 Aqueous washing liquors and other liquors

070503 Organic halogenated solvents, washing liquids and mother liquors

070504 Non-halogenated organic solvents

070508 Other still bottoms and reaction residues

5.1 Pre-treatment Before a waste solvent stream may be distilled, it may require some pre-treatment, e.g. pH neutralisation, decant of aqueous layer, pervaporation, or filtration. Any resulting wastes arising will be sent to the wastewater treatment plant or sent for disposal offsite.

5.2 Still heels During the distillation process, the higher boiling materials become concentrated in the still pot while the lower boiling (more volatile) materials evaporate off and are condensed and collected in a receiver. The material which remains in the pot, called the “still heel”, generally contains water, possibly some solvent, and any non-volatile solids. Depending on the nature of the components, this still heel may be treated in the site wastewater treatment plant or sent for disposal offsite.

5.3 ‘Aqueous decants Water collected from the pre-distillation decanter is sent to the WWTP. Also, the vapours reaching the top of the distillation columns are cooled and condensed to a liquid in the overhead condenser and diverted to a reflux pot/decanter where water can be removed by decanting. This water is also sent for treatment in the onsite WWTP.

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5.4 Permeate As described in Section 2.4 above, the pervaporation system separates the “wet” solvent into a “dry” product stream and an aqueous waste or permeate stream. As a small percentage of solvent passes through the membrane, the permeate is not pure water. However, the permeate is usually recycled for further treatment to minimise the solvent loss. The final permeate stream contains approximately 95% water and 5% solvent. This will be sent to the wastewater treatment plant or sent for disposal offsite.

5.5 Condensate Condensate from the boilers is recycled back to the boiler intake or directed to the WWTP.

5.6 Cleaning Aqueous boilouts and washings from cleanouts of the recovery towers between solvent runs are sent to the VWVTP.

Solvent flushes of equipment are typically sent for disposal offsite.

5.7 Summary of the site’s wastewater treatment plant Full details of the site wastewater treatment plant were included in the IPC Licence Applications of 1994 and 2000 and subsequent updates to the Agency. There follows below a brief summary of the WWTP operation.

Figure 9 is a schematic process flow diagram for the WVVTP. The activated sludge treatment process is as follows:

Strong wastewater streams from the production plants, that contain solvent which is treatable in the WVVTP, are collected in holding tanks which allow for satisfactory balancing of effluent composition. From there, strong effluent is pumped at a controlled rate to two equalisation tanks at the head of the treatment plant where neutralisation (pH adjustment) takes place. The weak process effluent streams, consisting of wash water, pump seal water and other dilute aqueous streams including rainwater collected in bunded areas, are also fed to these equalisation tanks.

From the equalisation tanks the combined process wastewater is pumped to a splitter box which allows parallel feed to three first-stage aeration basins. Nutrient addition (phosphoric acid and urea) is made as required by in-line metering to the pumpout from the equalisation tanks. Stormwater (if contaminated) can be added to the equalisation tanks. Domestic effluent is added to the second stage aeration basins.

Following first-stage treatment by the activated sludge process, the flows from the first-stage aeration basins are directed to two first-stage clarifiers. Overflow from these clarifiers flows by gravity to a splitter box for parallel feed to the two second-stage aeration basins. One of the second-stage aeration basins is linked to a hollow-fibre membrane filtration system. Treated effluent emerges from the membrane as permeate, and sludge can be recycled back to the basin. The remaining second-stage aeration basin is linked to second- stage clarifiers, again to facilitate sludge separation. Sludge from these clarifiers can be recycled back to the aeration basins. Overflow from these clarifiers combines with membrane permeate to form final treated effluent.

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Combined final treated effluent is pumped via a pipeline into the Cork County Council sewer pipe linked to a marine outfall.

The equalisation tanks and the aeration basins are roofed to minimise odour and VOC emissions. The headspace air from the first-stage basins is passed through biofilters packed with peat fibre material for odour control.

Surplus activated sludge is dewatered to approximately 15% dry solids in mechanical belt presses and sent offsite for treatment and disposal. Filtrate from the belt presses is returned to the WWTP.

Final treated effluent is monitored in accordance with the requirements of the site’s IPC licence (Reg No. 542).

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6.0 CAPABILITY OF EXISTING SOLVENT RECOVERY FACILITIES

6.1 Solvent recovery volumes In 2004, approximately 15,000 Tonnes of solvent was used in processes on the site. Of this, approximately 3,800 Tonnes or 25% of this solvent input was recovered on site. This comprised eight different solvents from a number of processes.

There are five large recovery towers on site and three smaller towers. A maximum recovery yield on each larger tower is estimated to be 3 million litres per annum, and on each smaller tower is estimated to be 1 million litres per annum. These figures are dependent on the composition of the streams to be treated and the supply volumes generated. In general, these figures represent the maximum estimated capabilities. In combination they give a projected maximum recovery yield for the site of 18 million litres per annum, if all were running at 100% capacity all year round. However, there is a certain amount of down-time in the equipment due to, for example, waiting for test results, cleaning of equipment, boil outs, etc. A maximum recovery yield for the site of 12 million litres of solvent per annum is a more realistic figure. Half of this amount, i.e. 6 million litres, is expected to be used for recovery of solvent generated on site, with the other 6 million litres of capacity available for the recovery of solvent received from other sites. This is an estimated realistic maximum projection and is dependent on product mix and volume.

6.2 Assessment of Recovery Capability Before any new waste stream for recovery will be accepted on site it will be subjected to a Site Solvent Recovery Assessment. This assessment procedure is documented in the Technical Services Standard Operating Procedure RNG-TS-SOP-015 The principal elements of this assessment procedure are as follows:

6.2.1 Selection of waste streams for recovery Streams for recovery are identified on the basis of volume, cost, technical feasibility, complexity and potential yield. Process streams are generally waste solvent streams, distillate streams or decant streams. A proposed method of recovery is identified.

6.2.2 Initial Laboratory Investigation A sample of the solvent stream proposed for recovery is obtained from the plant by the Development Chemist. If the required solvent is unavailable from the plant, a laboratory pilot is performed and the solvent stream is collected.

The Development Chemist/Technician concentrates down a portion of the sample to 20-30% and arranges, if necessary, for shipment of the concentrated sample for process safety testing (thermal stability).

The Development Chemist and Production Services Team Leader identify any pm-treatment that may be required before distillation, e.g. pH neutralisation, decant of aqueous layer, pervaporation, and filtration. The

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Development Chemist performs a trial distillation on the sample and records any relevant observations.

The Development Chemist/Technician concentrates down a portion of the sample to dryness and any observations are recorded. The distillation flask is examined and weighed to measure the dissolved solids content. A sample of any remaining residue may be sent for process safety testing.

The Development Chemist/Production Services Team Leader at the site planning to use the recovered solvent determines the value of completing a laboratory use test on the recovered solvent. The Development Chemist completes initial critical quality testing on the lab-recovered solvent to determine its suitability for use-test (a laboratory-scale pilot reaction using the recovered solvent). A use-test should only be completed if the solvent recovered in the lab is of similar quality to that expected to be recovered on the plant.

6.2.3 Agreement and Approval of Initial Solvent Recovery Assessment Protocol A protocol is agreed at this stage between Technical Services, Production Services and QA as to what additional data, if any, is required before commencing plant recovery trials. This protocol should also outline the objectives of the recovery trial and the trial recovery specification.

6.2.4 Process Modelling (not an SOP requirement) A computer simulation may be conducted. Into this are input the feed stream composition and product expected, the number of stages in the recovery tower, the reflux ratio and the condenser duties. This calculates a theoretical separation obtainable from the recovery equipment, and may be used in the development of Operating Instructions.

6.2.5 Solvent Recovery Preparations The Production/Production Services Supervisor ensures that the Operating Instructions and Distributed Control System (DCS) recipe for the plant-scale recovery trial are prepared. These instructions are reviewed by Technical Services and Production Services and approved by the QA Chemist, along with the relevant Production Manager/Team Leader.

6.2.6 Process Safety Review A Process Safety Review is carried out to confirm that the process is safe to run on the selected site recovery units. Any process safety information from tested samples is used in this review.

6.2.7 Solvent Recovery Trial If the recovery is on a solvent from another site, the appropriate volume is transported onto the Ringaskiddy site. A limited solvent recovery trial is carried out on plant-scale. This is supervised by the assigned Production/Production Services Supervisor to generate representative samples of recovered solvent. The recovery method used and relevant data such as operating instructions, processing notes and tower conditions are maintained. Any amendments to the DCS recipe and Operating Instructions

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as a result of the trial are implemented. The volumes recovered should be sufficient for laboratory testing and use-testing.

6.2.8 Laboratory Use-test and Specification Setting A sample of the plant scale trial solvent is submitted to the In-Process Control Lab for analysis to the quality regulatory or appropriate specification.

Pending successful analysis, appropriate laboratory use-tests are performed by the Development Chemistrrechnician using a sample of the plant-scale trial solvent.

The requirement for a quality regulatory filing is assessed by the QA Chemist. If a quality regulatory change is required, local site procedures are followed.

Once the laboratory-scale use-testing has been successfully completed, a specification for the recovered solvent is set; the recovered solvent is approved by the QA Chemist for use in typically a three-batch production plant trial.

6.2.9 Large-scale Recovery and Process Qualification A sufficient quantity of solvent is recovered using the approved Operating Instructions and DCS recipe to perform typically a three-batch trial campaign at full scale. The recovered solvent is tested by the In-Process Control Lab. The recovered solvent may be transported to the site where it is to be re- used. The solvent recovered in this full-scale recovery is used in a production three-batch trial. Plant performance and product quality are closely monitored during this trial. Any other testing deemed necessary by the Development Chemist is also performed on these three batches.

6.2.10 Approval of Recovery Process Once completed, the production plant trial is reviewed by the Development Chemist, the Production Supervisor and the QA Chemist.

It is the combined responsibility of the assigned Development Chemist and Production/Production Services Supervisor to compile a report detailing the significant steps outlined above in the development of the solvent recovery process. This report, the Solvent Recovery Development Report, is reviewed by Technical Services, Production Services and approved by the Quality Assurance Manager as final authorisation for reuse of the recovered solvent. The site intending to use the recovered solvent must be involved in this final approval process.

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7.

7.1

7.2

UNIT OPERATIONS LINKED WITH RECOVERY OF SOLVENTS FROM OTHER sms The principal unit operations associated with recovery of solvents from other sites are:

1. Reception and Storage

2. Solvent recovery, including the operations of

e Distillation

B Petvaporation

3. Storage and Dispatch.

Reception and storage The following steps will be completed to control the reception of solvents for recovery from other sites:

Pfizer Ringaskiddy Production personnel ensure that the waste type incoming is approved for acceptance onto the Pfizer Ringaskiddy site before the tanker leaves the originating site.

Pfizer Ringaskiddy Production personnel will ensure that storage tanks are available for incoming solvent for recovery from the other site.

Incoming solvent will be weighed at the weighbridge. The shipment will be recorded on the weighbridge system and on the solvent waste information management system.

The shipment will be offloaded to the tank and the unwashed tanker is returned to the originating site as an “empty unclean” tanker, with the appropriate paperwork. All loading and unloading operations take place in bunded and contained areas.

The Cl-form will be completed and copies sent to the originating site, the local authority and the haulier, and a copy will be retained on file.

Standard Operating Procedure PS4-001 defines the manner by which a tanker of waste solvent is received, sampled and offloaded.

Solvent recovery operations Certain streams may require pretreatment (e.g. pH neutralisation) prior to entry to the recovery equipment. Once the recovery equipment becomes free, the recovery process will be initiated by Production personnel.

A generic flow diagram of the Solvent Recovery unit operations and how they are related is shown in Figure 1. Distillation and Pervaporation are discussed in further detail in Section 2 above.

Recovered solvent lots on site are tracked using a solvent allocation management system. Only approved, recovered lots of solvent are stored in the storage tanks. As lots are added to the top of a storage tank and removed through the bottom outlet, solvent lots are dispatched on a “first-in, first-out” basis. Recovered solvent is sampled and analysed.

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7.3 Storage and dispatch Recovered solvent is stored in dedicated solvent storage tanks until used on site or sent off site for reuse at another site. All storage tanks are adequately bunded and reside in contained areas to contain any spillages that may occur.

Production personnel will order a road tanker to transport the recovered solvent to the destination site. It is the intention that either a dedicated tanker or a certified clean tanker will be used.

Production personnel will generate the appropriate transport documentation to accompany the load. A consignment note (Cl-form) is not required as the solvent is no longer a waste.

Production personnel dispatch the recovered solvent to the destination site.

The volume of solvent sent offsite is recorded on the solvent allocation management system.

Site Core Standard Operating Procedure PS4-002 defines the manner by which solvent tankers are loaded with recovered solvent and sent off-site.

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8 DETAILS OF RECEPTION PROTOCOL FOR INCOMING SOLVENTS FOR RECOVERY The site Standard Operating Procedure PS4-001 (Acceptance of Waste Solvent Tankers) defines the manner by which a waste solvent tanker is received and offloaded. The Environmental Management System Procedure EMS-J3 (Management of hazardous wastes) gives a high-level overview of the procedure by which waste solvent may be accepted onto the site for recovery, and refers out to the more detailed Standard Operating Procedures.

In summary, the following steps are followed:

1. The road tanker is weighed in at Security and the load details are recorded, then it is directed to the appropriate area for off-loading.

2. The documentation accompanying the load is checked. This must include the Cl-form and its accompanying Annex detailing the analysis of the waste by the originating site, and the TREM card. The Cl-form is completed and copies are given to the driver, Cork County Council and the consignor (site where the waste solvent originated). On completion of the documentation for the road tanker, a record of the load is recorded in the solvent waste information management system.

3. A sample of the tanker contents is taken and retained until the solvent load has been recovered. A record that a retained sample has been taken is made in the Waste Solvent Tanker Acceptance Record log sheet, kept in the relevant Control Room.

4. The waste solvent is offloaded to the appropriate solvent storage tank. All loading and unloading operations take place in bunded and contained areas.

5. The volume transferred is recorded in the Waste Solvent Tanker Acceptance Record log sheet.

6. Once the tanker has been accepted and offloaded for recovery, a Disposal/Recovery Certificate can be issued to the waste originator.

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9 TRACEABILITV OF SOLVENTS FOR RECOVERY

9.1 Reception of waste solvent for recovery Waste solvents for recovery will be brought onto the site by road tanker (typically 18,000 - 28,000 L capacity). Each load will be accompanied by the relevant documentation, i.e. consignment note (Cl-form), record of analysis from the originating site, and TREM card. When the load arrives at the Pfizer Ringaskiddy security gate, it will be weighed in. Security personnel will record the tanker container number, load description, load date, waste haulier and weight received on the site’s bulk delivery weighbridge system. When the waste solvent is offloaded, the tanker will be weighed out and second weight will be entered in the bulk delivery weighbridge system.

The bulk delivery weighbridge system is linked to the site’s solvent waste information management system, so the information entered will be transferred across. Production personnel will enter additional information on each load in the solvent waste information management system: Cl-number, UN number, waste origin, EWC code, recovery code, any comments on the load, analytical data supplied by the originating site, and the tag number of the tank to which it was offloaded. At this point, if the analytical data indicates that the waste material is not suitable for recovery at Ringaskiddy, the load can be returned to the originating site.

The waste will be offloaded into a dedicated and segregated tank on site, which may contain previous loads of the same material. It may be mixed with other loads of material that have been previously approved for the process under the Technical Services Standard Operating Procedure RNG-TS-SOP- 015. At this point, the solvent waste information management system will be used to generate a certificate of disposal/recovery for the waste load, dated for the date of receipt of the load. This certificate of disposal/recovery will be returned by production personnel to the originating site.

Solvent storage tanks have a typical capacity of 4O,OOOL, so there will be at least two loads of received solvent for recovery in each full storage tank. These will be fed on a continuous or batchwise basis to the dedicated recovery towers.

Waste solvent for recovery will be offloaded into designated storage vessels. Records will be retained for each waste solvent load received; identifying which specific solvent storage vessel it was offloaded into. Storage vessels containing waste solvent for recovery will forward-feed to assigned distillation columns (or pervaporation unit) on a continuous or batchwise basis. Full traceability is thereby achieved for each waste solvent load, from receipt of the road tanker through off-loading, storage, and subsequent recovery.

9.2 Recovered solvent The fate of recovered solvent is depicted in Figure IO. Solvent is collected from the recovery process and sent to a test tank (typically 7,000 - 10,OOOL capacity). Each test tank of recovered solvent collected is dealt with as a separate lot of recovered solvent. A sample is taken from the test tank and assigned a sample number from the laboratory information management system. The sample is tested in the In-Process Control Laboratory against an approved specification. If the solvent lot passes the specification, it is

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9.3

released to a dedicated solvent storage tank. If it fails specification, depending on the nature of contaminant, it may be reworked in the recovery equipment or sent for disposal off-site. At this point it is recorded on the solvent allocation management system and the sample number from the laboratory information management system becomes the lot number on the solvent allocation management system. The lot volume transferred and the destination tank identity are recorded on the solvent allocation management system. As the solvent storage tanks have a typical capacity of 40,000 L, there are usually four or five recovered solvent lots stored in a storage tank. At any given time, the solvent allocation management system can identify what lots of solvent are stored in each of the solvent storage tanks.

To transfer recovered solvent offsite, a delivery number will be generated. The solvent allocation management system will allocate an appropriate volume of recovered solvent from storage and allocate the appropriate lot numbers to that delivery number. Lot numbers from storage tanks are assigned on a ‘first in, first out” basis, i.e. the most recent lot transferred into a storage tank will only be emptied from the tank once all the earlier lots have been emptied. The details of the tanker used (weight, tanker number) from the bulk delivery weighbridge system at Security will be linked to the delivery number in the solvent allocation management system. The solvent allocation management system will generate a delivery docket that will contain the following: delivery number, solvent, volume, lot numbers, and test results from individual lots. The tanker will be weighed out to provide a check weight. The solvent allocation management system will be able to provide reporting details for any given period. Full traceability is thereby achieved between the recovery process and the recovered solvent, thus completing the traceability and tracking of the material, from incoming waste solvent to outgoing recovered solvent.

Waste from Solvent Recovery The recovery process may give rise to residual material which must be disposed of offsite (see Section 5 above). Such material will be recorded on the solvent waste information management system, in the same manner in which all wastes arising on the site are recorded. Aqueous waste arising from the recovery process will be directed to the WVVTP.

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Recovered Solvent ’

Sample taken for testing in the IPC laboratory. I

1 Sample number assigned by laboratory information management

system (LIMS)

LIMS sample # becomes Solvent lot # on solvent

First lot # into the tank will be

FIGURE 10: THE FATE OF SOLVENT POST RECOVERY

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40. TESTING OF SOLVENTS FOR RECOVERY Waste solvents for recovery will be tested by the originating site for parameters agreed with the Ringaskiddy site before the solvent stream is dispatched to Ringaskiddy. As a minimum, the pH, water content and identity of the solvent(s) will be analysed. The test results will be attached as an Annex to the consignment note (Cl-form) that accompanies the load of waste dispatched for recovery to the Ringaskiddy site.

The contents of the road tanker will be sampled at Ringaskiddy prior to offloading. As the contents have previously been tested at the originating site, the Annex will be accepted as legitimate evidence of testing, and additional testing of this sample will not generally be repeated at Ringaskiddy. This sample is retained for a period of time as a contingency sample.

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11. MANAGEMENT OF EXISTING LICENCE Some technical adjustments have been taken into account in correspondence between the licensee and the Agency during the period of the current and earlier licences. Such changes and adjustments included, for example, permissions for the use of new waste disposal and recovery methods, adjustments to monitoring test frequencies, offsite archiving of records, etc. Such written approvals were issued by the Agency under the conditions of the existing and earlier licences. Written guidance has also been received from the Agency regarding, for example, the submission of monitoring data, the structure and content of the Annual Environmental Report, etc. Pfizer considers that such written permissions and guidance received from the Agency shall continue to apply unless specifically withdrawn in revised licences.

In addition, several approvals and updates identified during the preparation of this application which may be pertinent to the text of the revised licence are shown in Table 4 below.

Table 4: Approvals and updates applicable to the revised licence.

3 July 2003 13 August 2003

Various

M542Iap32mo

DisposaliRecovery methods for wastes have been added or modified with the approval of the Agency in accordance with Notes 1-3 to Schedule 3(i) of Licence 542. The current consolidated list is provided in Tables 6 and 7 below.

Notification of the change of the site name to” Pfizer Ireland Pharmaceuticals Ringaskiddy Active Pharmaceutical Ingredient Plant”.

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Table 4 (continued): Approvals and updates applicable to the revised licence.

24 November 2003

24 March 2004; section 2 therein

24 March 2004; section 4 therein

31 March 2004; section 1 therein

6 September 2004

EPA response on 3-Dee-2003; additional information thereupon supplied by Pfizer to EPA on 8 March 2004.

Correspondence dated 23 April 2004;

Correspondence dated 28 April 2004.

22 April 2004 M542/ap36mo

Site Inspection Report of 3 September 2004

Site Inspection Report of 3 September 2004

M542/gc44ew- Internal Intra-group chonam.doc corporate restructuring

M5421gc47mo (23Apr-2004)

M542lap37mo (28-Apr-2004)

Inspection Ref. Particulates monitoring No. (IRN) in Schedule l(iii) to be 54204Sl02MO; adjusted from annual Section 2(3) monitoring to a 3-year therein rotating programme.

Inspection Ref. No. (IRN) 54204Sl02MO; section 2(5) therein

Revision of some parts of the reporting timetable for monitoring results for emissions to air and to sewer as required under conditions 5.7 and 6.3 of the current licence.

Use of groundwater well 409 as a substitute for well 6

Adjustment to Condition 12.4 of licence -Waste records to be now stored for 2yrs onsite; with facility to transfer to offsite document storage for a further 5 years.

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Furthermore, the Licensee takes this opportunity to propose that the textual adjustments shown in Table 5 below be taken into account in the new licence.

Table 5: Proposed Licence Adjustments

Schedules l(ii) and 2(ii)

Schedule

2 (ii)

Schedule

2 (iii)

Reference to “Daily sampling” in the monitoring frequency for the Biological treatment $I:! to be replaced with “ Daily as per other IPPC Licences where Note 1 is interpreted as the following “On each day when laboratory facilities are available and not less than 5 days per week, except during holidays and process shut-down periods”

l TOC Analysis Method/Technique should read “Automatic TOC”.

l Total Ammonia Analysis Method/Technique should read “distillation/titration”.

To accurately reflect the current system and allow for possible future upgrades.

Daily Sampling is not necessary over weekends for the parameters listed in Schedule 2(ii) as there is at least an 8 - day hydraulic residence time in the WWTP. Sampling at weekends and public holidays does not achieve additional environmental protection

To reflect current analytical practice/ methodologies

None of the adjustments presented in Tables 4 and 5 above or those presented in Tables 6 and 7 below have an environmental impact - rather these details are listed in order to assist in preparation of a licence that will accurately reflect the details of the activity.

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Product s*mnrac nr samples f,,,,, %,I- II

51,I ,,,,Gs ,,ld intermediate ‘mm +hn r=rboratory

and protective clothing naterials of nroduction

I -I- I Offsite incineration/ Incineration withgy

recovery/ Use as a fuel

Offsite incineration/ Incineration with Energy recovery/ Use as a fuel

Packaging material contaminated with r. .___. .-..- _. ,. -~~ ~.. - I I

I I I Offsite incineration/ Incineration with Energy Obsolete chemicals and stock

Waste oil

Medical waste from onsite first aid

Spent catalyst containing precious metals

Fluorescent tubes

Lead-acid batteries

Ni-Cd batteries

Discarded electrical and electronic equipment

Other

-- recovery/ Use as a fuel

Offsite incineration/ Incineration with Energy recovery/ Use as a fuel/ Offsite reclamation

Approved hazardous waste contractor

Offsite Recovery/Regeneration

Offsite Recycling

Offsite Recycling

Offsite Recycling

Offsite Recycling

* Table 6 outlines only hazardous waste types which are recovered onsite or recovered/disposed offsite.

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Table 7: Consolidated List of Approved Disposal and Recovery Routes for Non-Hazardous Waste

Sludge from the wastewater treatment Offsite Composting followed by beneficial reuse as landfill cover

Alkaline batteries

Mixed construction and demolition wastes

Wooden packaging

Plastic packaging Glass

Recycle Reuse/Recycle

Recycle Reuse/Recycle

Recycle Reuse/Recycle

Recycle Reuse/Recycle

Recycle Reuse/Recycle

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Table 8 below provides a summary of the correspondence between this site and the Agency with respect to various licence notifications and updates. None of the correspondences listed in Table 8 require any amendment to the text of the existing IPC licence Reg No. 542, with the exception of those which are also listed in Table 4 above.

Table 8: Approvals and updates applicable to the existing IPC licence, Reg.No. 542.

Change of Team Leader Environment

Use of AVR-Safeway as new waste disposal contractor

Notification of new minor vents 179MOO6 and 185M016

Update on status of OSP4 Thermal Oxidiser Test Programme

Update on production of atorvastatin and UK-338,003-27

Notification of new minor vents 178M031, 179MOO7 and 163MO45

Use of Glancre as sludge disposal contractor

Submission in respect of OSP4 Hydrogenation Building

Use of Tank Trans as new waste hauliers

08-Apr-02 Use of Atlas Ireland for sludge drying

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Table 8 (Continued): Approvals and updates applicable to the existing IPC licence, Reg.No. 542.

Notification of change to selected shutdown dates

Notification of use of EcoSafe for medical waste

Update on flnalised shutdown dates

Modifications to vent V38

Notification of new minor emission point 17OMO23 and new potential emission point 163PO77

Notification of utilisation of temporary boiler

Notification of use of Heraeus as recovery facility for spent catalyst containing precious metals

Upgrade of continuous emissions monitors on V2, V3 and V5

Notification of use of SRM (Morecambe) as a cemfuel facility

Notification of use of Irish Lamp Recycling as contractor for fluorescent tubes, disused electrical goods and non-hazardous wastes

Notification of use of Betrem and lnnovatherm for sludge treatment and disposal

Update of Inventory of Materials : for manufacture of Eletriptan Hemisulphate ; UK-390,957 ; CP-703,458

1 I 1 1 1 1 I 1 1 1 3 I I 1

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Table 8 (Continued): Approvals and updates applicable to the existing IPC licence, Reg.No. 542.

Notification of use of RWE for hazardous waste treatment and disposal

Notification of use of Nickelhuette for spent catalyst recovery

Notification of minor emission points 163MO47 and 163MO48

Notification of extension to OSPI to install new goods lift, covered drum laydown area

20-Jun-03

24-Jun-03

Notification of use of Eurosource Europe for the recycling of ink/toner cartridges

Proposed test protocol for OSP4 weak effluent drains

Notification of minor emission points 190M019 and 190M020

Notification of annual shutdown dates

Notification of site name change Ringaskiddy Active Pharmaceutical Ingredient Plant

Notification of Apparec for obsolete electrical equipment including those containing refrigerant gases

Notification of use of Ashgrove Recycting

Notification of Meridian Technical Services

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Table 8 (Continued): Approvals and updates applicable to the existing IPC licence, Reg.No. 542.

Use of larger temporary boiler, extension of use

Use of O’D Recycling [McGill Tipperaryj for composting of sludge

Notification of minor emission point 178MO32 [mobile mill]

Update of Inventory of Materials : for manufacture of [S&S]-Reboxetine ; UK-427,857 ; Varenicline [CP-526,555]

Programme of environmental communications with external interested parties

Modification to licensed emission point V37

Resubmission of existing temporary boiler, extension of use

Notification of use of Cork Confidential Shredding

Update on shutdown dates

Notification of use of John Butler and Dan Sheahan reclamation sites for builders rubble

Notification of use of Minane Bridge sludge handling facility

OSP3 shutdown dates

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Table 8 (Continued): Approvals and updates applicable to the existing IPC licence, Reg.No. 542.

Internal restructuring : new PIP partnership

9

Air dispersion modelling methodology for third boiler notification

17-Dee-03 Use of Coolrec to recycle electronic goods

24Mar-041 Agreements from onsite meeting of l&Mar-04

!zFl

(i) Proposal for mitigation of dust vent monitoring; (ii) Proposal to manage number of H2 vents; (iii) Response to PK-2313 magnahelic - - ww

22-Apr-04 New boiler submission

- -

!!!!!!I

Notification of shutdown dates

09-Jun-04 Update of Inventory of Materials : for manufacture of AG-1859 ; Pregabalin Asymmetric ; Triton RX-100

07-Jul-041 Submission of environmental policy for information only

7

(i) OSP4 Small Equipment Group minor emission points; (ii) Use of Macroom Haulage, Transbound, Cork County Council Landfill,

05Aug-04 Bottlehill, Cara Waste Management Ltd. Transfer Station, National Document Management Group Ltd, Shred-it and Glyntown Enterprises; (iii) Use of new materials ; sodium phosphate, trichickenfootphos catalyst, argon; (iv) Temporary boiler extension; (v) Upgrade of OSP3 DCS to Delta V); (vi) Cornposting of spent Bord na Mona peat biofilters; (vii) Sludge trial using Ultraclay;

Storage of waste records onsite [reduced from seven years to two years]

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I!

Table 8 (Continued): Approvals and updates applicable to the existing IPC licence, Reg.No. 542.

Update of Inventory of Materials : for manufacture of iNOS ; Torcetrapib ; Asenapine ; also notification of cyanomonoester and bromine deactivation materials

Summary of understandings re: PER ; waste facility notification and approval [cf. Dow Halterman] ; noise monitoring programme

Update on calibration of magnahelic gauges, notification of sutent and notification of temporary transfer of 170 M 031 from DC 768 in OSP3 to DC 1704 in OSP4

Notification of OSP4 shutdown dates

Summary of understandings re: meeting with Agency Inspector on 1 O-Mar-05 : including hydrogen vent approval transfer system ; solvent recovery trials for PIP sites ; use of Midland 466, 424 and sodium tartrate ; PER restructure

Use of Novian International Ltd trading as Healthcare Waste Management Services for the collection of medical waste

Use of Gandon Enterprises Ltd transfer station and storage facility for hazardous and non hazardous waste

Notification of OSPI ,2,3 shutdown dates

(i) Notification of Solvent Recovery Trial in RKY; (ii) Use of Watetford City Council cornposting facility for food wastes

7

(i) Carbon beds on VOC Plants ; (ii) Minor Emission Point 191M016 from FGB jet mill isolators ; (iii) New materials for Torcetrapib l-

30-Sep-05 2, PD-200390, Cooling Tower cleaning , MIBK ; (iv) Request for guidance and consultation on EES air report ; (v) Solvent Recovery trial on MTBE from LI ; (vi) Confirmation regarding fish tainting requirements ;(vii) Request for update on status of licence review application ; (viii) Sludge disposal route Shanks Vlaanderen - Ciment D’Obourg

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Table 8 (Continued): Approvals and updates applicable to the existing IPC licence, Reg.No. 542.

(i) Use Atlas Environmental as a waste contractor for canteen cooking oil, (ii) use of Waterford City Council Cornposting facility at Carrignard, Water-ford City for cornposting of non-hazardous waste, (iii) Intention to send 3 aqueous waste streams from the manufacture of Toracetrapib Step 3/4 to the onsite Waste Water Treatment Plant, (iv) Reduce the low TOC diversion setting on the system for automatic diversion of surface water to the site retention pond.(v) Request for Agency guidance on implementation of the WEEE directive, (vi) Notification of change of Seveso status for the Pfizer Ringaskiddy site.

] I 1

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.a T2!B -

~__

IPPC Application Form

Attachment N” D.1

SITE LAYOUT

DRAWING NO. EIR-2-l OO-C4857, REV. A

Completed IPPC Application Form 2005 Page 52 of 53

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