Chemical & Biological Survey at Baltray October 2016

Produced by

AQUAFACT International Services Ltd

On behalf of

Premier Periclase Ltd.

December 2016

For inspection purposes only. Consent of copyright owner required for any other use.

AQUAFACT INTERNATIONAL SERVICES LTD., 12 KILKERRIN PARK, GALWAY . www.aquafact.ie [email protected] tel +353 (0) 91 756812

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Table of Contents

1. Introduction ...... 1

2. Summary ...... 2

3. Materials & Methods ...... 2

3.1. Biological Sampling ...... 3 3.2. Sediment Sampling ...... 4 3.3. Water Sampling ...... 4

4. Results ...... 5

4.1. Biological Results ...... 5 4.2. Sediment Results ...... 6 4.3. Water Results ...... 7

5. Discussion ...... 9

5.1. Biology ...... 9 5.2. Sediment ...... 9 5.3. Seawater ...... 10

List of Figures Figure 3.1: Sample stations, 14th October 2016 ...... 3 For inspection purposes only. Consent of copyright owner required for any other use.

List of Tables

Table 3.1: Station coordinates ...... 3 Table 4.1: Biological results from grab stations ...... 5 Table 4.2: Sediment results ...... 6 Table 4.3: Seawater sample results - Flood tide ...... 7 Table 4.4: Seawater sample results - Ebb tide ...... 8 Table 4.5: Resulst from effluent analysis ...... 9 Table 5.1: Comparison on metals levels from Irish ports and harbours with Baltray 2016 results. ... 10

List of Appendices

Appendix 1 Species List Appendix 2 Sediment ALS Lab Report Appendix 3 Water NLS Lab Report; TelLab Lab Report Appendix 4 Effluent NLS Lab Report

EPA Export 29-03-2017:23:50:59 Chemical & Biological Survey, Premier Periclase Ltd. Baltray, Co. Louth, October 2016 December 2016

1. Introduction

Premier Periclase Ltd. commissioned AQUAFACT to carry out a chemical and biological survey of the area surrounding the effluent outfall pipe from their magnesite production plant in Drogheda. Previous monitoring, since 1980, has measured the chemical characteristics of the seawater in the vicinity of the effluent plume and the results have shown that, based on the parameters measured, there has been little or no measurable impact on water quality as a result of the discharge.

AQUAFACT conducted a survey of water, sediment chemistry and sediment biology on the 14th October 2016, the results of which are contained in this report.

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2. Summary

A faunal, sediment and water quaality survey was carried out in the vicinity of the Premier Periclase outfall in October 14th 2016.

The faunal survey showed that the species encountered were sensitive or indifferent to pollution and very typical for that environment on the east coast of Ireland. Community type and diversity was similar to previous years.

Analysis of sediments from the vicinity of the outfall for metals content showed that the levels of calcium, magnesium, nickel, zinc and chromium were lower than the levels found in sediment at the control site 2km east of the outfall. The metal levels at all sites sampled were at the lower end of the range found in Irish ports and harbours.

The results of the seawater quality survey show that the range of the results from the outfall site were comparable to the ranges observed at the sites further afield. There were slight increases in the following parameters at the outfall site on the ebb tide compared to the flood tide: pH, Nitrogen, Phosphorus, Carbonate, Bicarbonate, Nickel, Zinc and Chromium. These increases are not environmentally significant.

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3. Materials & Methods

All sampling took place on the 14th October 2016. Figure 3.1 shows the locations of the sample stations and the parameters sampled at each location. Table 3.1 contains the station coordinates.

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Figure 3.1: Sample stations, 14th October 2016.

Table 3.1: Station coordinates.

Station Longitude Latitude Parameter Outfall -6.22923 53.72915 Fauna, Water 100 N - 6.22923 For inspection53.73003 purposes only.Fauna, Sediments, Water Consent of copyright owner required for any other use. 200 N -6.22924 53.73092 Fauna, Sediments, Water 300 N -6.22923 53.7318 Fauna 100m S -6.22923 53.72827 Fauna, Sediments, Water 200m S -6.22923 53.72738 Fauna, Sediments, Water 300m S -6.22923 53.7265 Fauna Control -6.19877 53.72908 Sediments

3.1. Biological Sampling

The biological samples were collected using a 0.1m2 van Veen grab sampler at the following 7 stations: Outfall, 100m N, 200m N, 300m N, 100m S, 200m S and 300m S. All grab returns were sieved on a 1mm mesh sieve, stained with Eosin-briebrich scarlet and fixed in 4% w/v buffered formaldehyde solution upon returning to the laboratory.

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All faunal samples were placed in an illuminated shallow white tray and sorted first by eye to remove large specimens and then sorted under a stereo microscope (x 10 magnification). Following the removal of larger specimens, the samples were placed into Petri dishes, approximately one half teaspoon at a time and sorted using a binocular microscope at x25 magnification.

The fauna was sorted into four main groups: Polychaeta, Mollusca, Crustacea and others. The ‘others’ group consisted of echinoderms, nematodes, nemerteans, cnidarians and other lesser phyla. The fauna were maintained in stabilised 70% industrial methylated spirit (IMS) following retrieval and identified to species level where practical using a binocular microscope, a compound microscope and all relevant taxonomic keys. After identification and enumeration, specimens were separated and stored to species level.

3.2. Sediment Sampling

The sediment samples were collected using a 0.1m2 van Veen grab sampler at the following 5 stations: 100m N, 200m N, 100m S, 200m S and Control. The sediment samples were stored in plastic containers and sent to ALS Laboratories in Loughrea (INAB No. 173T) for the analysis of Nickel, Zinc, Chromium, Calcium and Magnesium using the Ultra trace ME-MS61 48 element four acid ICP-MS procedure. Fractions of the samples were also analysed in-house by AQUAFACT for % moisture and % solids.

For inspection purposes only. Consent of copyright owner required for any other use. 3.3. Water Sampling

Water samples were collected using a Niskin water sampler at 5 stations: Outfall, 100m N, 200m N, 100m S and 200m S. The samples were collected from 1m below the surface and 1m above the seabed. Samples were collected on the ebb and flood tide. High water on the day was at 10:43am. One sample of final effluent was provided by Premier Periclase Ltd.

All water samples plus the effluent were sent to NLS in the UK (UKAS No. 0754) and analysed for:  pH  Total Nitrogen  Total Phosphorus  Sulphate

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 Zinc  Nickel  Chromium  Calcium  Magnesium

Water samples from each station (except the effluent sample) were also sent to T.E. Labs in Carlow (INAB Registration No. 106T) for the analysis of bicarbonate and carbonate.

4. Results

4.1. Biological Results

Table 4.1 shows the results of the biological sampling. A full phylogenetic species list can be found in Appendix 1.

Table 4.1: Biological results from grab stations.

Station 100m S 200m S 300m S Outfall 100m N 200m N 300m N Turbellaria 1 Nemertea 1 1 Sigalion mathildae 1 1 1 1 1 Eteone longa agg. 1 Phyllodoce groenlandica For inspection purposes1 only. 1 1 Consent of copyright owner required for any other use. Glycera oxycephala 1 Glycera tridactyla 2 6 1 1 3 3 Nephtys sp. (juv) 1 Nephtys caeca 1 Scoloplos (Scoloplos) armiger 1 Spiophanes bombyx 2 Magelona mirabilis 2 5 1 4 7 Capitella sp. complex 1 Chaetozone setosa 1 Tharyx sp. 1 Amphictene auricoma 1 Perioculodes longimanus 1 Ampelisca brevicornis 1 Iphinoe trispinosa 1 1 1 1 3 Diastylis bradyi 1 Crangon crangon 1 Pagurus bernhardus 1 Brachyura (juv) 1 Euspira nitida 2 1 1

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Station 100m S 200m S 300m S Outfall 100m N 200m N 300m N Nucula nitidosa 6 7 2 14 1 10 Mytilidae (juv) 1 Kurtiella bidentata 1 1 Fabulina fabula 3 Donax vittatus 77 11 21 74 38 37 53 Abra sp. (juv) 1 1 Abra alba 1 Phaxas pellucidus 1 Chamelea striatula 2 1 1 Thracia phaseolina 1 1 3 Acrocnida brachiata 1 Ophiura ophiura 12 2 1 3 2 1 Total 111 36 24 90 69 50 86

4.2. Sediment Results

Table 4.2 shows the results of the sediment analyses. Appendix 2 shows the lab report from ALS Laboratories. Solids ranged from 76.43% at the Control to 81.91% at 100m S. Moisture ranged from 18.09% at 100m S to 23.57% at the Control. Calcium ranged from 26100 mg/kg at 100m N to 34800 mg/kg at the Control. Chromium ranged from 23 mg/kg at 100mN to 43 mg/kg at the Control. Magnesium ranged from 3900 mg/kg at 100m N to 5200 mg/kg at the Control. Nickel ranged from 7.4 mg/kg at 100m N to 11.2 mg/kg at the Control. Zinc ranged from 26 mg/kg at 200m S to 44 mg/kg at the Control.

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Table 4.2: Sediment results.

Parameter 100m N 200m N 100m S 200m S Control LOD* % Solids 81.16 80.30 81.91 76.47 76.43 - % Moisture 18.84 19.70 18.09 23.53 23.57 - Calcium (mg/kg) 26100 28100 29100 29200 34800 100 Chromium (mg/kg) 23 31 38 27 43 1 Magnesium (mg/kg) 3900 4500 4300 4300 5200 100 Nickel (mg/kg) 7.4 7.8 7.9 7.8 11.2 0.2 Zinc (mg/kg) 28 27 28 26 44 2 * Limits of Detection

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4.3. Water Results

Table 4.3 shows the results from the water samples collected on the flood tide and Table 4.4 shows the water results from samples collected on the ebb tide. Appendix 3 shows the lab reports containing these results. On the flooding tide ranged from 8.03 (200m N B, Outfall S, 100m S B) to 8.04 (all other samples). Nitrogen ranged from 398 mg/l (Outfall S) to 625 mg/l (200m S B). Total phosphorus ranged from 21.8 mg/l (200m S B) to 32.1 mg/l (100m N S). Sulphate ranged from 2490 mg/l (100m S S) to 2710 mg/l (100m N B). Carbonate ranged from 5 mg/l at 200m N (Bottom) to 20 mg/l at 200m N (Surface) and 100m N (Bottom). Bicarbonate ranged from 120 mg/l at 200m N (Surface) and 100m N (Bottom) to 140 mg/l at 200m N (Bottom) and 200m S (Bottom). Nickel ranged from 0.84 µg/l (100m N S) to 18.8 µg/l (200m S B). Zinc ranged from 2.48 µg/l (100m N S) to 374 µg/l (200m N B). Calcium ranged from 366 mg/l (100m S S) to 419 mg/l (200m N B). Magnesium ranged from 1200 mg/l (100m S B) to 1310 mg/l (100m S S). Chromium ranged from <0.5 µg/l (100m N S) to 1.86 µg/l (200m N B).

Table 4.3: Seawater sample results - Flood tide

Parameter 200m N 100m N Outfall 100m S 200m S LOD S B S B S B S B S B pH 8.04 8.03 8.04 8.04 8.03 8.04 8.04 8.03 8.04 8.04 0.05 Nitrogen as 489 408 443 479 398 467 482 529 449 625 100 N (mg/l) Total 26.3 29.8 32.1 25.3 29.2 27.4 25.9 24.8 28.5 21.8 20 Phosphorus (mg/l) For inspection purposes only. Sulphate as 2630 2650 2600Consent of 2710copyright owner2520 required 2540for any other2490 use. 2550 2690 2570 5

SO4 (mg/l) Carbonate as 20 5 10 20 10 10 10 10 10 10 1

CaCO3 (mg/l) Bicarbonate 120 140 130 120 135 125 130 135 130 140 1

as CaCO3 (mg/l) Nickel (µg/l) 0.859 9.32 0.84 6.1 0.872 4.15 0.914 9.05 1.07 18.8 0.3 Zinc (µg/l) 3.61 374 2.48 147 2.76 108 6.01 206 12.4 213 0.4 Calcium 390 419 401 403 410 387 366 400 390 410 10 (mg/l) Magnesium 1240 1230 1230 1290 1210 1210 1310 1200 1270 1220 3 (mg/l) Chromium 0.523 1.86 <0.5 0.931 0.572 0.694 0.586 0.822 0.734 0.919 0.5 (µg/l) S = 1m below surface B = 1m above bottom LOD = Limits of Detection

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On the ebbing tide ranged from 8.03 (200m N S, 200m N B, 100m N B) to 8.31 (100m S S). Nitrogen ranged from 325 mg/l (Outfall S) to 640mg/l (200m S B). Total phosphorus ranged from 21.2 mg/l (200m N B) to 39.1 mg/l (200m S B). Sulphate ranged from 2390 mg/l (100m N S) to 2710 mg/l (100m S B). Carbonate ranged from 10 mg/l at 200m N (Bottom) and 100m N (Surface) to 40 mg/l at Outfall (Surface) and 100m N (Surface and Bottom). Bicarbonate ranged from 105 mg/l at 100m S (Surface and Bottom) to 135 mg/l at 200m N (Bottom). Nickel ranged from 1.04 µg/l (100m N S, 100m S S) to 22.7 µg/l (200m N B). Zinc ranged from 3.47 µg/l (Outfall S) to 1620 µg/l (200m N B). Calcium ranged from 378 mg/l (200m S S) to 447 mg/l (100m S B). Magnesium ranged from 1140 mg/l (100m N S) to 1270 mg/l (Outfall B). Chromium ranged from 0.866 µg/l (100m N S) to 3.25 µg/l (200m N B).

Table 4.4: Seawater sample results - Ebb tide.

Parameter 200m N 100m N Outfall 100m S 200m S LOD S B S B S B S B S B pH 8.03 8.03 8.04 8.03 8.21 8.05 8.31 8.2 8.04 8.08 0.05 Nitrogen as N 485 619 551 548 325 574 526 511 474 640 100 (µg/l) Total 30.1 21.2 29.7 30.6 32.4 27.6 32.1 28 29.6 39.1 20 Phosphorus (µg/l) Sulphate as 2560 2590 2390 2580 2550 2660 2650 2710 2430 2610 5

SO4 (mg/l) Carbonate as 20 10 10 30 40 20 40 40 20 30 1

CaCO3 (mg/l) Bicarbonate as 130 135 130 115 125 110 105 105 120 115 1

CaCO3 (mg/l) For inspection purposes only. Consent of copyright owner required for any other use. Nickel (µg/l) 1.33 22.7 1.04 5.93 1.06 8.99 1.04 6.34 1.11 5.32 0.3 Zinc (µg/l) 4.37 1620 4.83 317 3.47 364 3.83 181 4.4 222 0.4 Calcium (mg/l) 395 400 405 403 417 399 416 447 378 431 10 Magnesium 1220 1200 1140 1230 1210 1270 1220 1230 1200 1240 3 (mg/l) Chromium 0.908 3.25 0.866 1.57 1.03 2.32 1.23 2.86 0.789 3.09 0.5 (µg/l) S = 1m below surface B = 1m above bottom LOD = Limits of Detection

Table 4.5 shows the results from the effluent analysis. Appendix 4 shows the lab reports containing these results.

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Table 4.5: Results from effluent analysis.

Parameter Effluent LOD pH 10.7 0.05 Nitrogen as N (µg/l) <100 100 Total Phosphorus (µg/l) <10 10

Sulphate as SO4 (mg/l) 2510 5 Nickel (µg/l) <5 1 Zinc (µg/l) <30 5 Calcium (mg/l) 2220 1 Magnesium (mg/l) 45.7 0.3 Chromium (µg/l) 34 0.5 Iron (µg/l) 36.8 30

5. Discussion

5.1. Biology

All faunal species encountered are typical of the sediment type in the area. The community was dominated by the bivalve molluscs Donax vittatus and Nucula nitidosa, the brittlestar Ophiura ophiura and the polychaetes Magelona mirabilis and Glycera tridactyla. All of these species are For inspection purposes only. Consent of copyright owner required for any other use. typical of the sandy environment found along the east coast of Ireland and all of these species are either very sensitive to pollution or indifferent to it. No distinction could be made between the faunal community in the location of the outfall and those from the sites further afield. The species encountered were similar to previous years.

5.2. Sediment

Analysis of sediments from the vicinity of the outfall for metals content showed that the levels of calcium, magnesium, nickel, zinc and chromium were lower than the levels found in sediment at the control site 2km east of the outfall. Table 5.1 shows a comparison of metal results from Irish ports with those from Baltray. The metal levels at all sites sampled were at the lower end of the range found in Irish ports and harbours.

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Table 5.1: Caparison on metals levels from Irish ports and harbours with Baltray 2016 results.

Parameter Irish Ports (mg/kg dry wt.) Baltray 2016 (mg/kg dry wt.) Zinc 20 - 480 26-44 Chromium 4.3 - 118 23 - 43 Nickel 3 - 56 7.4 - 11.2

5.3. Seawater

While the range of the results from the outfall site were comparable to the ranges observed at the sites further afield, there were slight increases in the following parameters at the outfall site on the ebb tide compared to the flood tide: pH, Nitrogen, Phosphorus, Carbonate, Bicarbonate, Nickel, Zinc and Chromium. These increases are not environmentally significant.

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Appendix 1 Species List

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Station Aphia 100m S 200m S 300m S Outfall 100m N 200m N 300m N Id. PLATYHELMINTHES 793 Turbellaria 794 1 NEMERTEA 152391 Nemertea 152391 1 1 ANNELIDA 882 POLYCHAETA 883 PHYLLODOCIDA 892 Sigalionidae 943 Sigalion mathildae 131072 1 1 1 1 1 Phyllodocidae 931 Eteone longa agg. 130616 1 Phyllodoce groenlandica 334506 1 1 1 Glyceridae 952 Glycera oxycephala 130126 1 Glycera tridactyla 130130 2 6 1 1 3 3 Nephtyidae 956 Nephtys sp. (juv) 129370 1 Nephtys caeca 130355 1 ORBINIIDA 884 Orbiniidae 902 Scoloplos (Scoloplos) 334772 1 armiger SPIONIDA 889 Spionidae 913 Spiophanes bombyx 131187 2 Magelonidae 914 Magelona mirabilis 130271 2 5 1 4 7 CAPITELLIDA 890 Capitellidae 921 Capitella sp. complex 129211 1 For inspection purposes only. TEREBELLIDA Consent900 of copyright owner required for any other use.

Cirratulidae 919 Chaetozone setosa 129955 1 Tharyx sp. 129249 1 Pectinariidae 980 Amphictene auricoma 152448 1 ARTHROPODA 1065 CRUSTACEA 1066 AMPHIPODA 1135 Oedicerotidae 101400 Perioculodes longimanus 102915 1 Ampeliscidae 101364 Ampelisca brevicornis 101891 1 CUMACEA 1137 Bodotriidae 110378 Iphinoe trispinosa 110462 1 1 1 1 3 Diastylidae 110380 Diastylis bradyi 110472 1 DECAPODA 1130 Crangonidae 106782

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Station Aphia 100m S 200m S 300m S Outfall 100m N 200m N 300m N Id. Crangon crangon 107552 1 Paguridae 106738 Pagurus bernhardus 107232 1 BRACHYURA 106673 Brachyura (juv) 106673 1 MOLLUSCA 51 GASTROPODA 101 CAENOGASTROPODA 382204 Naticidae 145 Euspira nitida 151894 2 1 1 BIVALVIA 105 NUCULIDA 382247 Nuculidae 204 Nucula nitidosa 140589 6 7 2 14 1 10 MYTILIDA 210 Mytilidae 211 Mytilidae (juv) 211 1 IMPARIDENTIA 869600 Montacutidae 225 Kurtiella bidentata 345281 1 1 CARDIIDA 869602 Tellinidae 235 Fabulina fabula 146907 3 Donacidae 236 Donax vittatus 139604 77 11 21 74 38 37 53 Semelidae 1781 Abra sp. (juv) 138474 1 1 Abra alba 141433 1 ADAPEDONTA 869601 Pharidae 23091 For inspection purposes only. Phaxas pellucidus 140737Consent of copyright owner required for any other use. 1

VENERIDA 217 Veneridae 243 Chamelea striatula 141908 2 1 1 ANOMALODESMATA 254 Thraciidae 256 Thracia phaseolina 152378 1 1 3 ECHINODERMATA 1806 OPHIUROIDEA 123084 OPHIURIDA 123117 Amphiuridae 123206 Acrocnida brachiata 236130 1 Ophiuridae 123200 Ophiura ophiura 124929 12 2 1 3 2 1

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Appendix 2

Sediment

ALS Lab Report

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Appendix 3

Water

NLS Lab Report TelLab Lab Report

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EPA Export 29-03-2017:23:50:59 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

Caroline Roche AQUAFACT International Services Ltd 12 Kilkierrin Park Liosbaun Galway

Dear Caroline

Please find attached the results for the batch of 20 samples described below.

Samples Registered on: 19-Oct-2016 Analysis Started on: 20-Oct-2016 Analysis Completed on: 31-Oct-2016 Results for Batch Number 20100593 Your Purchase Order Number: None Supplied You will be invoiced shortly by our accounts department.

If we can be of further assistance then please do not hesitate to contact us.

Yours sincerely

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Vici Morgan Customer Services Team Leader Tel: (0113) 231 2177 [email protected]

Opinions and interpretations expressed herein are outside the scope of UKAS Accreditation. Details of analytical procedures and performance data are available on request. The date of sample analysis is available on request.

The Environment Agency carries out analytical work to high standards and within the scope of its UKAS accreditation, but has no knowledge of whether the circumstances or the validity of the procedures used to obtain the samples provided to the laboratory were representative of the need for which the information was required. The Environment Agency and/or its staff does not therefore accept any liability for the consequences of any acts or omissions made on the basis of the analysis or advice or interpretation provided.

NLS Leeds NLS Nottingham NLS Starcross Olympia House Meadow Lane Staplake Mount Gelderd Lane Nottingham Starcross Gelderd Road NG2 3HN Exeter Leeds LS12 6DD EX6 8FD Page 1 of 22

EPA Export 29-03-2017:23:50:59 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655471 Sampled on: 14-Oct-16 @ 09:50 Comments: 200S Bottom Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.625 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0218 mg/l 0.02 None SX 868 pH 8.04 pH Units 0.05 UKAS SX 9 Nickel 18.8 ug/l 0.3 UKAS SX 89 Zinc 213 ug/l 0.4 UKAS SX 89 Calcium 410 mg/l 10 UKAS SX 95 Magnesium 1220 mg/l 3 UKAS SX 95 Sulphate as SO4 2570 mg/l 5 UKAS SX 95 Chromium 0.919 ug/l 0.5 UKAS SX 92

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NLS Leeds NLS Nottingham NLS Starcross Olympia House Meadow Lane Staplake Mount Gelderd Lane Nottingham Starcross Gelderd Road NG2 3HN Exeter Leeds LS12 6DD EX6 8FD Page 2 of 22

EPA Export 29-03-2017:23:50:59 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655472 Sampled on: 14-Oct-16 @ 09:50 Comments: 200S Surf Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.449 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0285 mg/l 0.02 None SX 868 pH 8.04 pH Units 0.05 UKAS SX 9 Nickel 1.07 ug/l 0.3 UKAS SX 89 Zinc 12.4 ug/l 0.4 UKAS SX 89 Calcium 390 mg/l 10 UKAS SX 95 Magnesium 1270 mg/l 3 UKAS SX 95 Sulphate as SO4 2690 mg/l 5 UKAS SX 95 Chromium 0.734 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:50:59 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655473 Sampled on: 14-Oct-16 @ 09:40 Comments: 100mS Bot Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.529 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0248 mg/l 0.02 None SX 868 pH 8.03 pH Units 0.05 UKAS SX 9 Nickel 9.05 ug/l 0.3 UKAS SX 89 Zinc 206 ug/l 0.4 UKAS SX 89 Calcium 400 mg/l 10 UKAS SX 95 Magnesium 1200 mg/l 3 UKAS SX 95 Sulphate as SO4 2550 mg/l 5 UKAS SX 95 Chromium 0.822 ug/l 0.5 UKAS SX 92

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NLS Leeds NLS Nottingham NLS Starcross Olympia House Meadow Lane Staplake Mount Gelderd Lane Nottingham Starcross Gelderd Road NG2 3HN Exeter Leeds LS12 6DD EX6 8FD Page 4 of 22

EPA Export 29-03-2017:23:50:59 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655474 Sampled on: 14-Oct-16 @ 09:40 Comments: 100mS Surf Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.482 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0259 mg/l 0.02 None SX 868 pH 8.04 pH Units 0.05 UKAS SX 9 Nickel 0.914 ug/l 0.3 UKAS SX 89 Zinc 6.01 ug/l 0.4 UKAS SX 89 Calcium 366 mg/l 10 UKAS SX 95 Magnesium 1310 mg/l 3 UKAS SX 95 Sulphate as SO4 2490 mg/l 5 UKAS SX 95 Chromium 0.586 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:50:59 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655475 Sampled on: 14-Oct-16 @ 09:51 Comments: Outfall Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.467 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0274 mg/l 0.02 None SX 868 pH 8.04 pH Units 0.05 UKAS SX 9 Nickel 4.15 ug/l 0.3 UKAS SX 89 Zinc 108 ug/l 0.4 UKAS SX 89 Calcium 387 mg/l 10 UKAS SX 95 Magnesium 1210 mg/l 3 UKAS SX 95 Sulphate as SO4 2540 mg/l 5 UKAS SX 95 Chromium 0.694 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:50:59 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655476 Sampled on: 14-Oct-16 @ 09:51 Comments: Outfall Surf Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.398 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0292 mg/l 0.02 None SX 868 pH 8.03 pH Units 0.05 UKAS SX 9 Nickel 0.872 ug/l 0.3 UKAS SX 89 Zinc 2.76 ug/l 0.4 UKAS SX 89 Calcium 410 mg/l 10 UKAS SX 95 Magnesium 1210 mg/l 3 UKAS SX 95 Sulphate as SO4 2520 mg/l 5 UKAS SX 95 Chromium 0.572 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:50:59 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655477 Sampled on: 14-Oct-16 @ 10:00 Comments: 100N Bot Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.479 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0253 mg/l 0.02 None SX 868 pH 8.04 pH Units 0.05 UKAS SX 9 Nickel 6.10 ug/l 0.3 UKAS SX 89 Zinc 147 ug/l 0.4 UKAS SX 89 Calcium 403 mg/l 10 UKAS SX 95 Magnesium 1290 mg/l 3 UKAS SX 95 Sulphate as SO4 2710 mg/l 5 UKAS SX 95 Chromium 0.931 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:50:59 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655478 Sampled on: 14-Oct-16 @ 10:00 Comments: 100m N Surf Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.443 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0321 mg/l 0.02 None SX 868 pH 8.04 pH Units 0.05 UKAS SX 9 Nickel 0.840 ug/l 0.3 UKAS SX 89 Zinc 2.48 ug/l 0.4 UKAS SX 89 Calcium 401 mg/l 10 UKAS SX 95 Magnesium 1230 mg/l 3 UKAS SX 95 Sulphate as SO4 2600 mg/l 5 UKAS SX 95 Chromium <0.5 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:50:59 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655479 Sampled on: 14-Oct-16 @ 10:10 Comments: 200m N Bot Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.408 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0298 mg/l 0.02 None SX 868 pH 8.03 pH Units 0.05 UKAS SX 9 Nickel 9.32 ug/l 0.3 UKAS SX 89 Zinc 374 ug/l 0.4 UKAS SX 89 Calcium 419 mg/l 10 UKAS SX 95 Magnesium 1230 mg/l 3 UKAS SX 95 Sulphate as SO4 2650 mg/l 5 UKAS SX 95 Chromium 1.86 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655480 Sampled on: 14-Oct-16 @ 10:10 Comments: 200m N Surf Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.489 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0263 mg/l 0.02 None SX 868 pH 8.04 pH Units 0.05 UKAS SX 9 Nickel 0.859 ug/l 0.3 UKAS SX 89 Zinc 3.61 ug/l 0.4 UKAS SX 89 Calcium 390 mg/l 10 UKAS SX 95 Magnesium 1240 mg/l 3 UKAS SX 95 Sulphate as SO4 2630 mg/l 5 UKAS SX 95 Chromium 0.523 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655481 Sampled on: 14-Oct-16 @ 12:30 Comments: 200m N Bot Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.619 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0212 mg/l 0.02 None SX 868 pH 8.03 pH Units 0.05 UKAS SX 9 Nickel 22.7 ug/l 0.3 UKAS SX 89 Zinc 1620 ug/l 0.4 UKAS SX 89 Calcium 400 mg/l 10 UKAS SX 95 Magnesium 1200 mg/l 3 UKAS SX 95 Sulphate as SO4 2590 mg/l 5 UKAS SX 95 Chromium 3.25 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655482 Sampled on: 14-Oct-16 @ 12:30 Comments: 200m N Surf Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.485 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0301 mg/l 0.02 None SX 868 pH 8.03 pH Units 0.05 UKAS SX 9 Nickel 1.33 ug/l 0.3 UKAS SX 89 Zinc 4.37 ug/l 0.4 UKAS SX 89 Calcium 395 mg/l 10 UKAS SX 95 Magnesium 1220 mg/l 3 UKAS SX 95 Sulphate as SO4 2560 mg/l 5 UKAS SX 95 Chromium 0.908 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655483 Sampled on: 14-Oct-16 @ 12:40 Comments: 100m N Bot Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.548 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0306 mg/l 0.02 None SX 868 pH 8.03 pH Units 0.05 UKAS SX 9 Nickel 5.93 ug/l 0.3 UKAS SX 89 Zinc 317 ug/l 0.4 UKAS SX 89 Calcium 403 mg/l 10 UKAS SX 95 Magnesium 1230 mg/l 3 UKAS SX 95 Sulphate as SO4 2580 mg/l 5 UKAS SX 95 Chromium 1.57 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655484 Sampled on: 14-Oct-16 @ 12:40 Comments: 100m N Surf Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.551 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0297 mg/l 0.02 None SX 868 pH 8.04 pH Units 0.05 UKAS SX 9 Nickel 1.04 ug/l 0.3 UKAS SX 89 Zinc 4.83 ug/l 0.4 UKAS SX 89 Calcium 405 mg/l 10 UKAS SX 95 Magnesium 1140 mg/l 3 UKAS SX 95 Sulphate as SO4 2390 mg/l 5 UKAS SX 95 Chromium 0.866 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655485 Sampled on: 14-Oct-16 @ 12:45 Comments: Outfall Bottom Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.574 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0276 mg/l 0.02 None SX 868 pH 8.05 pH Units 0.05 UKAS SX 9 Nickel 8.99 ug/l 0.3 UKAS SX 89 Zinc 364 ug/l 0.4 UKAS SX 89 Calcium 399 mg/l 10 UKAS SX 95 Magnesium 1270 mg/l 3 UKAS SX 95 Sulphate as SO4 2660 mg/l 5 UKAS SX 95 Chromium 2.32 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655486 Sampled on: 14-Oct-16 @ 12:45 Comments: Outfall Surf Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.325 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0324 mg/l 0.02 None SX 868 pH 8.21 pH Units 0.05 UKAS SX 9 Nickel 1.06 ug/l 0.3 UKAS SX 89 Zinc 3.47 ug/l 0.4 UKAS SX 89 Calcium 417 mg/l 10 UKAS SX 95 Magnesium 1210 mg/l 3 UKAS SX 95 Sulphate as SO4 2550 mg/l 5 UKAS SX 95 Chromium 1.03 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655487 Sampled on: 14-Oct-16 @ 12:50 Comments: 100m S Bot Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.511 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0280 mg/l 0.02 None SX 868 pH 8.20 pH Units 0.05 UKAS SX 9 Nickel 6.34 ug/l 0.3 UKAS SX 89 Zinc 181 ug/l 0.4 UKAS SX 89 Calcium 447 mg/l 10 UKAS SX 95 Magnesium 1230 mg/l 3 UKAS SX 95 Sulphate as SO4 2710 mg/l 5 UKAS SX 95 Chromium 2.86 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655488 Sampled on: 14-Oct-16 @ 12:50 Comments: 100m S Surf Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.526 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0321 mg/l 0.02 None SX 868 pH 8.31 pH Units 0.05 UKAS SX 9 Nickel 1.04 ug/l 0.3 UKAS SX 89 Zinc 3.83 ug/l 0.4 UKAS SX 89 Calcium 416 mg/l 10 UKAS SX 95 Magnesium 1220 mg/l 3 UKAS SX 95 Sulphate as SO4 2650 mg/l 5 UKAS SX 95 Chromium 1.23 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655489 Sampled on: 14-Oct-16 @ 12:55 Comments: 200m S Bot Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.640 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0391 mg/l 0.02 None SX 868 pH 8.08 pH Units 0.05 UKAS SX 9 Nickel 5.32 ug/l 0.3 UKAS SX 89 Zinc 222 ug/l 0.4 UKAS SX 89 Calcium 431 mg/l 10 UKAS SX 95 Magnesium 1240 mg/l 3 UKAS SX 95 Sulphate as SO4 2610 mg/l 5 UKAS SX 95 Chromium 3.09 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Seawater Samples Folder No: 003655490 Sampled on: 14-Oct-16 @ 12:55 Comments: 200m S Surf Quote No: 13458 Matrix: Saline Water Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen as N 0.474 mg/l 0.1 UKAS SX 375 Phosphorus : Total 0.0296 mg/l 0.02 None SX 868 pH 8.04 pH Units 0.05 UKAS SX 9 Nickel 1.11 ug/l 0.3 UKAS SX 89 Zinc 4.40 ug/l 0.4 UKAS SX 89 Calcium 378 mg/l 10 UKAS SX 95 Magnesium 1200 mg/l 3 UKAS SX 95 Sulphate as SO4 2430 mg/l 5 UKAS SX 95 Chromium 0.789 ug/l 0.5 UKAS SX 92

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100593 - 1 0754 Batch description: Seawater Reported on: 31-Oct-2016

Method Description Summary for all samples in batch Number 20100593 9 SX I pH EC Turbidity; Conductivity; Turbidity - determined by automated electrode probe system 89 SX M ICPMS Saline - Metals - saline matrix elimination; determined by ICPMS 92 SX M Misc Cr - Chromium - acid digested; determined by GF-AAS 95 SX M ICPOES Saline - Metals; Sulphate - acid digested; determined by ICPOES 375 SX I Saline Total N - digested, determined colorimetrically by autoanalyser 868 SX I Saline Total Phosphorus - digested; determined colorimetrically by autoanalyser

James Trout Laboratory Site Manager

All reporting limits quoted are those achievable for clean samples of the relevant matrix. No allowance is made for instances when dilutions are necessary owing to the nature of the sample or insufficient volume of the sample being available. In these cases higher reporting limits may be quoted and will be above the MRV. Minimum Reporting Value (MRV). A minimum concentration selected for reporting purposes (i.e. the less than value), which is higher than the statistically derived method limit of detection. Solid sample results are determined on a "dried" sample fraction except for parameters where the method description identifies that "as received" sample was used. Uncertainty of Measurement information relating to sample results is supplied upon request. Uncertainty is estimated from the performance of routine quality control standards, using the calculation 2 X Relative Standard Deviation + Bias. This is based on the guidance issued by the UKTAG Chemistry task team - Guidance on the implementation of the Quality Assurance/Quality Control requirements’ associated with Commission Directive 2009/90/EC, Article 4 (UoM = 2 X %RSD), with a contribution added for the bias.

The analysis start date specified is the date of the first test, dates for other analysis are available on request. Please note all samples will be retained for 10 working days for aqueous samples and 30 working days for solid samples after reporting unless otherwise agreed with Customer Services Key to Accreditation: UKAS = Methodology accredited to ISO/IEC 17025:2005, MCertS = Methodology accredited to MCertS Performance Standard for testing of soils, none = Methodology not accredited Key to Lab ID: LE = Leeds, NM = Nottingham, SX = Starcross, SC = Sub-Contracted outside NLS, FI = Field Data - outside NLS, NLS = Calculated Any subsequent version of this report denoted with a higher version For number inspection will purposes supersede only. this and any previous versions END OF TEST REPORT Consent of copyright owner required for any other use.

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EPA Export 29-03-2017:23:51:00 T.E. LABORATORIES LIMITED Trading as

Loughmartin Business Park, Tullow, Co. Carlow Phone: 059-9152881 Fax: 059-9152886

CERTIFICATE OF ANALYSIS Page 1 of 3

Project Description: Analysis of Aqueous Samples

Attention: Ms. Caroline Roche Lab ID: 132817 - 132836

Company: Aquafact Date Sampled: 14/10/2016 Address: 12 Kilkerrin Park, Liosbaun Industrial Estate, Tuam Road, Galway, Certificate No: L/16/1955 Date Rec’d: 17/10/2016 For inspection purposes only. Consent of copyright owner required for any other use. Issue Date: 02/11/2016 Our Ref: WS-42020

Project Summary: Twenty samples were analysed for a range of determinands. Please see page 2-3 for results. Terms & Conditions and methods used are outlined in the attached appendix.

No. of Pages: Results page 2-3 plus 4 page appendix

Mr. Peter O'Byrne Ms Breda Moore Quality Manager Technical Manager

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ANALYSIS OF AQUEOUS SAMPLES.

Date Sampled:14/10/2016 Date Rec'd: 17/10/2016 Date Analysis Commenced: 28/10/2016 Our Ref: WS-42020 Certificate No: L/16/1955

Sample ID 200m S BOT 9:30 200m S SURF 9:30 100m S BOT 9:40 100m S SURF 9:40 Outfall BOT 9:51 Outfall SURF 9:51 100m N BOT 10:00 100m N SURF 10:00 200m N BOT 10:10 200m N SURF 10:10

Determinand Lab ID 132817 132818 132819 132820 132821 132822 132823 132824 132825 132826

Bicarbonate as CaCo3 n/a 140 130 135 130 125 135 120 130 140 120

Carbonate as CaCo3 n/a 10 10 10 10 10 10 20 10 5 20

Concentrations expressed as mg/l (ppm) unless stated otherwise ** = INAB Accredited Tests ++ = Subcontracted Tests n/a = Non-INAB Accredited Tests

The above results relate only to the sample tested This report should not be regenerated except in full and with the consent of T.E. Laboratories Ltd. For inspection purposes only. Consent of copyright owner required for any other use.

T.E. Laboratories

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ANALYSIS OF AQUEOUS SAMPLES.

Date Sampled:14/10/2016 Date Rec'd: 17/10/2016 Date Analysis Commenced: 28/10/2016 Our Ref: WS-42020 Certificate No: L/16/1955

Sample ID 200m N BOT 12:30 200m N SURF 12:30 100m N BOT 12:40 100m N SURF 12:40 Outfall BOT 12:45 Outfall SURF 12:45 100m S BOT 12:50 100m S SURF 12:50 200m S BOT 12:55 200m S SURF 12:55

Determinand Lab ID 132827 132828 132829 132830 132831 132832 132833 132834 132835 132836

Bicarbonate as CaCo3 n/a 135 130 115 130 125 110 105 105 115 120

Carbonate as CaCo3 n/a 10 20 30 10 20 40 40 40 30 20

Concentrations expressed as mg/l (ppm) unless stated otherwise ** = INAB Accredited Tests ++ = Subcontracted Tests n/a = Non-INAB Accredited Tests

T.E. Laboratories

EPA Export 29-03-2017:23:51:00

Appendix 4

Effluent

NLS Lab Report

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100591 - 1 0754 Batch description: Trade Effluent Reported on: 02-Nov-2016

Caroline Roche AQUAFACT International Services Ltd 12 Kilkierrin Park Liosbaun Galway

Dear Caroline

Please find attached the results for the batch of 1 samples described below.

Samples Registered on: 19-Oct-2016 Analysis Started on: 20-Oct-2016 Analysis Completed on: 02-Nov-2016 Results for Batch Number 20100591 Your Purchase Order Number: None Supplied You will be invoiced shortly by our accounts department.

If we can be of further assistance then please do not hesitate to contact us.

Yours sincerely

For inspection purposes only. Consent of copyright owner required for any other use.

Vici Morgan Customer Services Team Leader Tel: (0113) 231 2177 [email protected]

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100591 - 1 0754 Batch description: Trade Effluent Reported on: 02-Nov-2016

1 Client: AQUAFACT International Services Ltd Project: 13458 Sediment and Aqueous Analysis Quote Description: Trade Effluent Samples Folder No: 003655493 Sampled on: 14-Oct-16 @ 09:00 Comments: Effluent Quote No: 13458 Matrix: Trade to Controlled Waters Analyte Result Units Flag MRV Accred Lab ID Testcode Nitrogen : Total as N <0.100 mg/l 0.1 UKAS SX 1389 Phosphorus : Total as P <0.0100 mg/l 0.01 UKAS SX 1389 pH 10.7 pH Units 0.05 UKAS SX 9 Sulphate as SO4 2510 mg/l 5 UKAS SX 1192 Chromium 34.0 ug/l 0.5 UKAS SX 34 Nickel <5 ug/l 1 UKAS SX 34 ELEVATED_MRV : Matrix interference Zinc <30 ug/l 5 UKAS SX 34 ELEVATED_MRV : Matrix interference Calcium 2220 mg/l 1 UKAS SX 38 Iron 36.8 ug/l 30 UKAS SX 38 Magnesium 45.7 mg/l 0.3 UKAS SX 38

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EPA Export 29-03-2017:23:51:00 Analytical Report

Final Report

Report ID - 20100591 - 1 0754 Batch description: Trade Effluent Reported on: 02-Nov-2016

Method Description Summary for all samples in batch Number 20100591 9 SX I pH EC Turbidity - pH; Conductivity; Turbidity - by automated electrode probe system 34 SX M ICPMS Routine - Metals - acid digested; determined by ICPMS 38 SX M ICPOES Routine - Metals - acid digested; determined by ICPOES 1192 SX I Sulphate by Ion Chromatography 1389 SX I Total N and P - digested, determined colorimetrically by autoanalyser

James Trout Laboratory Site Manager

The analysis start date specified is the date of the first test, dates for other analysis are available on request. Please note all samples will be retained for 10 working days for aqueous samples and 30 working days for solid samples after reporting unless otherwise agreed with Customer Services Key to Accreditation: UKAS = Methodology accredited to ISO/IEC 17025:2005, MCertS = Methodology accredited to MCertS Performance Standard for testing of soils, none = Methodology not accredited Key to Lab ID: LE = Leeds, NM = Nottingham, SX = Starcross, SC = Sub-Contracted outside NLS, FI = Field Data - outside NLS, NLS = Calculated Any subsequent version of this report denoted with a higher version number will supersede this and any previous versions END OF TEST REPORT For inspection purposes only. Consent of copyright owner required for any other use.

NLS Leeds NLS Nottingham NLS Starcross Olympia House Meadow Lane Staplake Mount Gelderd Lane Nottingham Starcross Gelderd Road NG2 3HN Exeter Leeds LS12 6DD EX6 8FD Page 3 of 3

EPA Export 29-03-2017:23:51:00