Testing procedures January 30, 2014 1|2

Migliore Waste Solutions Ltd Address Telephone Web Business ID 2524247-9 Valtakatu 35 A 4 +358 5 5354 198 www.migliore.fi 45700 Kuusankoski – Finland +358 400 550 823

Testing Procedures

1. Migliore’s  technology  was,  such  as  it  was  then,  tested  and  proven  already  in  the  year  2007.  By  that  time,  we had developed our technology up to a phase, where it was possible, appropriate and important to carry out serious tests on oil & gas drilling waste. The small-scale testing equipment was built.

2. We received two sets of materials from the North Sea oil drilling platforms and areas, altogether three

barrels. The first batch came from MI-SWACO’s  drilling  area,  and  the  other  one  was  sent  by  OTT  (Onsite  Treatment Technologies AS, Norway) from two different drilling areas. All the dispatched material represented the worst possible (the absolutely dirtiest) local drilling waste.

3. The received material was treated with our small-scale equipment in Finland. The small-scale treatment equipment is a rotating kiln, and can reach as high treatment temperatures as 1300 C. The testing was carried out by using batches of 30 kilos at a time. Altogether more than 40 test drives were run. All the test runs produced exactly the kinds of lightweight clay aggregate granules we expected. The following laboratory analyses were overwhelmingly better than anticipated.

4. Six sets of those testing results (the granules) were analysed by the laboratory of Jyväskylä University. The whole contents of the granules were examined, and special attention was paid to their non-solubility.

Testing procedures January 30, 2014 2|2

Migliore Waste Solutions Ltd Address Telephone Web Business ID 2524247-9 Valtakatu 35 A 4 +358 5 5354 198 www.migliore.fi 45700 Kuusankoski – Finland +358 400 550 823

5. As to the leaching characteristics of the end product, i.e. the granules, no leaching could be appreciated. All the hazardous substances, such like heavy metals, were encapsulated into the granules. The outcome of the laboratory test was that the granules were cleaner than the average soil in the Finnish forest, and that the end product is suitable for a multitude of purposes. The end product does NOT contain any hydrocarbons or other organic substances. The organic coal was turned into CO2 during the test. With our newest technology the emissions remain under the EU norms for industry.

6. Migliore’s   treatment  process   is  based  on  super-high temperatures and a rotating double-kiln. A similar principle (though much lower temperature) is applied to e.g. asphalt plant kiln technology. However, Migliore’s  technology  is  much  further  developed  since  2007 and thus we can fully use the existing energy in the material to be treated as its process energy, i.e. NO external energy is needed, provided that the waste contains 4 – 6 % of hydrocarbons (which it normally does). If not, for instance waste oil can be used. The inner lining for the kilns enables a quick start-up and shutdown (from 12 to 24 hours when the equipment arrives in the site). The design and materials make the equipment extremely vibration resistant, it tolerates rough handling, and it is thus suitable for moving from one place to another, by air, sea or land. Our contract manufacturer Amomatic Oy makes similar kinds of kilns for asphalt plants, and we utilise their decades of experience in the basic parts of our kilns. The inner structure of the drum and the double-kiln technology, both patented by us, utilise to a great extent already proven materials and components. Our equipment is mobile (built and fitted into seven intermodal shipping containers, no need for any additional facility for treatment). Its energy efficiency is exponentially better than with those current traditional solutions using rotation incinerator technology, although they may reach same high temperatures as our method.

INSTITUTE FOR ENVIRONMENTAL

UNIVERSITY OF JYVÄSKYLÄ RESEARCH

Postal address: Telephone: E-mail: P.O. Box 35 (YAD) +358 14 260 3830 firstname.lastname@ymtk.jyu.fi FI-40014 University of Jyväskylä Telefax: Internet: Street address: +358 14 260 3831 www.jyu.fi/ymtk Survontie 9 Ambiotica, Building D, 4th floor

Migliore Oy REPORT Pulkkanen AnteroValtakatu 35 A 4 17.9.2007 45700 Kuusankoski

PRELIMINARY CHARACTERISATION OF LEACHING BEHAVIOUR OF SOLID GRANULAR WASTE MATERIAL

Samples of six different ceramic granulate materials were analysed for total acid leach-able metal content and for organic matter as loss on ignition. The release of soluble con-stituents upon contact with water was tested according to standard SFS-EN 12457-2:2002. These tests cannot be used alone to determine the leaching behaviour of a mate-rial.

SAMPLES, PRE-TREATMENT AND TESTS

Samples were received from Migliore Oy 29.08.2007. In the laboratory samples were crushed when necessary (granulate size > 4 mm) and a separate sub sample was used to analyse dry matter content (105 °C).

Total acid leachable metal content was analysed by ICP-OES according to standard SFS-EN ISO 11885:1998 following micro wave acid extraction with concentrated nitric acid according to EPA 3051:1998. Loss on ignition (550 °C) was analysed according to SFS 3008:1990.

In the leaching test SFS-EN 12457 a portion of the sample with particle size below 4 mm (originally or after pre-treatment) was brought into contact with water (liquid to solid ratio 1:10) in a shaking device for 24 h. The solid residue was separated by filtra-tion and the eluate was analysed in addition to pH (SFS 3021: 1979) and conductivity (SFS-EN 27888: 1994), for chlorides and sulphates by ion chromatography (SFS-EN ISO 103014-1:1995) and for metals by ICP-MS (SFS-EN ISO 17294-2:05).

RESULTS

Results of the analysis with associated uncertainty values and analysis dates are pre-sented in the attachment (Analysis report 2007-3643). A summary of the results are also presented in the following tables (table 1 & table 3).

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TOTAL CONCENTRATIONS

Table 1. Total acid leachable metal content, and DM (dry matter), and LOI (loss on ignition) in the samples.

Parameter Unit 3643-1Solid sample MI-100

3643-2Solid sample MI-100 II

3643-3Solid sample RAO-HOT

3643-4Solid sample RA-00

3643-5Solid sample TORE-100

3643-6Solid sample S 50 D 50

DM % 99,9 99,9 99,9 99,9 99,9 99,9 LOI % 0,0 0,0 0,0 0,0 0,0 0,0 Sb mg/kg < 5 < 5 < 5 < 5 < 5 < 5 As mg/kg 5 6 < 3 4 6 3 Ba mg/kg 8 800 13 000 13 000 9 900 13 000 9 000 Cd mg/kg < 0,5 < 0,5 < 0,5 < 0,5 < 0,5 < 0,5 Cr mg/kg 11 13 8 10 13 11 Cu mg/kg 9 11 7 6 18 8 Pb mg/kg < 3 < 3 < 3 < 3 < 3 < 3 Mo mg/kg < 1 < 1 < 1 < 1 < 1 < 1 Ni mg/kg 11 16 6 12 12 10 S mg/kg 1 500 1 400 1 300 1 600 1 300 1 800 Se mg/kg < 3 < 3 < 3 < 3 < 3 < 3 Zn mg/kg 24 29 13 18 31 21

The tested samples consists entirely of inorganic matter and the elemental concentrations are very similar in the different materials. These values can be compared with the guidelines given by the Fin-nish Environmental Administration for assessment of soil contamination (table 2) /1/.

Table 2. Guidelines given by the Finnish Environmental Administration for assessment of soil con-tamination (Ministry of the Environment, 2007).

Parameter Unit Background value in soil

Threshold value

Lower guideline value

Upper guideline value

Sb mg/kg 0,02 (0,01-0,2) 2 10 50

As mg/kg 1 (0,1-25) 5 50 100Ba mg/kg - - - -Cd mg/kg 0,03 (0,01-0,15) 1 10 20Cr mg/kg 31 (6-170) 100 200 300Cu mg/kg 22 (5-110) 100 150 200Pb mg/kg 5 (0,1-5) 60 200 750Ni mg/kg 17 (3-100) 50 100 150Zn mg/kg 31 (8-110) 200 250 400

With the exception of barium, the total acid leachable concentration values in the samples are low, comparable to natural background values in Finnish soil. No threshold and guideline values are given for barium, but the concentration values are clearly higher than natural background values in soil.

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SOLUBLE CONCENTRATIONS

Table 3. Soluble concentrations of the material in the leaching test compared to acceptance criteria for waste at landfills /2/..

Parameter Unit 3643-1Eluate MI-100

3643-2Eluate MI-100 II

3643-3Eluate RAO- HOT

3643-4Eluate RA-00

3643-5Eluate TORE- 100

3643-6Eluate S 50 D 50

Accept. crit. - landfill for stable waste (class A)

Accept. crit. - landfill for conventional inorganic waste and treated haz-ardous waste (class B1b)

Accept. crit. - landfill for hazardous waste (class C)

As mg/kg 0,2 0,3 0,1 0,4 0,1 0,3 0,5 2 25 Ba mg/kg 1,4 0,9 3,2 0,9 1,3 1,8 20 100 300 Cd mg/kg < 0,001 < 0,001 < 0,001 < 0,001 < 0,001 < 0,001 0,04 1 5 Cr mg/kg 0,02 0,03 0,03 0,08 0,02 0,02 0,5 10 70 Cu mg/kg < 0,01 < 0,01 < 0,01 < 0,01 < 0,01 < 0,01 2 50 100 Mo mg/kg 0,18 0,17 0,08 0,02 0,03 0,02 0,5 10 30 Ni mg/kg < 0,01 < 0,01 < 0,01 < 0,01 < 0,01 < 0,01 0,4 10 40 Pb mg/kg < 0,01 < 0,01 < 0,01 < 0,01 < 0,01 < 0,01 0,5 10 50 Sb mg/kg < 0,01 < 0,01 < 0,01 < 0,01 < 0,01 < 0,01 0,06 0,7 5 Se mg/kg < 0,01 < 0,01 < 0,01 < 0,01 < 0,01 < 0,01 0,1 0,5 7 Zn mg/kg < 0,01 < 0,01 < 0,01 < 0,01 < 0,01 < 0,01 4 50 200 Cl- mg/kg 4 26 4 23 180 6 800 15 000 25 000 SO4 mg/kg 1 700 3 000 800 2 500 1 400 1 100 1 000 20 000 50 000 pH 9,3 1,4 4,3 9,0 5,0 8,5 - > 6 - Cond. mS/m 39,6 2 070 21,5 51,0 34,8 28,9 - - -

Eluate pH-values varied in a wide range from 1,4 to 9,3. The solubility of metals in the materials was low but sulphate was noticeably leached from the materials. With the exception of sulphate, concen-trations of the parameters under investigation remained below the threshold values for acceptability of waste for non-hazardous waste landfill (class A). The low pH of certain materials should be taken into consideration when disposing of the materials. Even if there was almost no indication of increased leachability in the material itself, the acidity may enhance the leachability of metals in adjacent mate-rials.

Allan Witick Laboratory manager

References:

1. Ministry of the Environment 2007: Assessment of soil contamination and the remediation need. Environmental Administration Guidelines 2 /2007 (in Finnish).

2. Margareta Wahlström, Jutta Laine-Ylijoki, Elina Vestola, Kati Vaajasaari, Anneli Joutti 2006: Ac-ceptance Procedures for Waste at Landfills. Environmental Administration Guidelines 2/2006 (in Fin-nish).