IN SOIL QC OIL VKI BATCH: Use. and the sum. same. assess the. Analysis Extract and. analyse the. al growth and. humidity absorption.

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Eurofins Miljø A/S Smedeskovvej 38 DK-8464 Galten CERTIFICATE FOR QC OIL IN SOIL SEMI-VOLATILE HYDROCARBONS BATCH: VKI-24-1-0299 USE OF THE REFERENCE MATERIAL Description, Quantity and Preservation

1 Eurofins Miljø A/S Smedeskovvej 38 DK-8464 Galten CERTIFICATE FOR QC OIL IN SOIL SEMI-VOLATILE HYDROCARBONS BATCH: VKI USE OF THE REFERENCE MATERIAL Description, Quantity and Preservation This reference material consists of 100 g of driedd soil slightly polluted withh oil and without significant content of volatile compounds. It has been certified for the content of the oil fractionss >nc 10 -nc 25 5, >nc 25 -nc 35 5 and the sum of hydrocarbons, by analysis mainly according too the method which the Danish D Environmental Protection Agency has had elaborated for analysis of polluted soil /3/. The material has beenn stabilised by drying, homogenisationn and γ-irradiation Use The reference material is intended for f control of the accuracy and precision of analyses. The reference material is typically intended for the internal quality control of analyses of the hydrocarbons of the oil fractions >nc 10 -nc 25, >nc 25 -nc 35 and the sum of hydrocarbons in soil.. It may also be used for the t implementation and optimisation of analytical methods. It is important that the batch numbers of the referencee material and on the certificate are the same. Preparation for Use Begin the determinationn with an extraction. Since the material is dried soil, it is recommended that the amount of aqueous pyrophosphate be increased as described in the method recommended by the Danish EPA /3/. For example; add 30 ml of aqueous pyrophosphatee and 20 ml of pentane too 50 g of soil.. Make sure that t the extraction technique chosen is sufficiently efficient. In case of doubt as too the quality of the extraction technique, assess the suspension visually. Analysis Extract and analyse the reference sample at thee same time and in the same manner as the other samples. Storage and Durability Store the reference material in the original unopened packing at room temperature or r in a refrigerator. The certificate is valid until 1st of March 2020 provided the material is stored under the recommendedd conditions. When the sample has been opened, its durability may be limited due to microbiologicam al growth and humidity absorption. PRODUCTION OF THE REFERENCE MATERIAL AND DOCUMENTATION Production The material consists of an oil-polluted clay soil supplied by Bioteknisk Jordrens (now: Soilrem A/S), Kalundborg, Denmark in December The soil was dried slightly at approx. 100 CC and coarse-crushed, the soil was ground in a mill until approx. 99% of the material had a particle size less than 90 µm. In connection with this grinding the material whereupon branches and stones larger than approx. 25 mmm were removed. Subsequently, was This certificate is prepared in accordance with the international ISO guidelines for f certificationn of referencee materials /1/.

2 mixed. The material was subjected to γ-irradiation at two times 15 kgrey, after which it was filled aseptically into metal tins. The material has been produced in accordance with the quality management procedures of VKI (now: Eurofins Miljø A/S), with the aim to obtain the intended quality of the material. Documentation of Content The documentation of the oil content of the material is mainly based on an extraction with aqueous pyrophosphate and pentane or dichloromethane. All analyses were performed on samples without drying, immediately after opening of the tin, when the dry matter content of the sample is higher than 99%. Internal control Homogeneity: The homogeneity of the oil fractions >nc 10 -nc 25, >nc 25 -nc 35 and of the sum of hydrocarbons in the reference material have been examined. The test for homogeneity has been performed by testing the standard deviation between reference samples against the standard deviation of duplicate determinations of individual containers (F-test, 95%). No signs of heterogeneity were detected. Stability: The stability is being followed and no signs of instability were detected at the date of this certificate. External documentation For the external documentation the laboratories were requested to analyse the reference material in duplicate in the same series of analysis. In addition, the laboratories were requested to analyse a control sample consisting of soil material spiked with a concentrate of a known amount of diesel oil and fuel oil. The statistics of the external control values have been calculated in accordance with the international standard ISO Guide 35 /1/. The following calculations have been made on the basis of the analytical results submitted by the laboratories: Y : average, calculated in accordance with ISO Guide 35, s L : standard deviation between the laboratories, calculated in accordance with ISO Guide 35, : 1 p 1 ( Y i Y) 2 The 95% confidence interval of the true mean value of the analysis results is: where Y ± t 0,025 ν sl ( ). p p: number of laboratories included in the calculations ν: p-1, number of degrees of freedom t 0,025 (ν): t value of level at ν degrees of freedom. The selection of results for the calculation of the content of the reference material is based on the laboratories: - having routine - achieving results of the parameter in question which are neither Cochran or Grubbs outliers - the recovery of the results, e.g. obtained by the analyses of the control samples consisting of soil spiked with diesel oil and fuel oil, lies within ± 20% of the assigned value. The statistical parameters according to ISO 5725 /4/, the analytical methods used as well as the number of laboratories having used each analytical method are listed in the table below. The laboratories selected for certification and the data included in the external laboratory documentation are Certificate QC Oil in Soil 2 Batch VKI

3 listed in an annex to this certificate. Certified Values The content of benzene, toluene, ethylbenzene and xylenes as well as the fraction of benzene nc 10 is close to or below the limit of detection for the participating laboratories, and have therefore not been certified. PARAMETER UNIT AVERAGE BETWEEN LABORATORY STANDARD DEVIATION Y 95% CONFIDENCE LIMITS OF THE AVERAGE Y ± t 0,025 ν sl ( ). p NUMBER OF LABORATORIES IN THE CALCULATIONS/ METHOD s L Lower Upper (p) >nc 10 nc A 2B 1C 1D >nc 25 nc A 3B 2D EXCLUDED SETS OF RESULTS AFTER CALCULA- TION G = Grubbs C = Cochran - - Sum of hydrocarbons A 3B 2D - Methods A: "Bestemmelse af olie i jord. Gaschromatografisk metode" ( Determination of oil in soil. Gas chromatographic method ), elaborated by the Reference Laboratory, VKI, of the Danish Environmental Protection Agency, July B: Like reference A, but extraction with dichloromethane C: Like reference A, but determination by GC-MS D: Other methods Use of the Certified Values For laboratories with an analytical quality that is comparable with the laboratories that have contributed with the external control data of this certificate, the following applies: 1) For single determinations, analytical results will with a probability of 95% be in the interval: Y ± t ( ν 0,025 ).s L 2) Analytical results, calculated as the average of a double determination will with a probability of 95% be in the interval: Y ± t 0,025 ν sl ( ). 2 Batch VKI Certificate QC Oil in Soil

4 REFERENCES /1/ ISO guide 35:2006. Certification of reference materials - General and statistical principles for certification. /2/ ISO guide 31:2000. Reference materials - Contents of certificates and labels /3/ "Bestemmelse af olie i jord. Gaschromatografisk metode" ( Determination of oil in soil. Gas chromatographic method ), elaborated by the Reference Laboratory of the Danish Environmental Inspection Agency, VKI, July /4/ ISO/DIS , 1994, Accuracy (trueness and precision) of measurement methods and results. Date of issue: January 2014 DIRECTOR RESPONSIBLE SCIENTIST Karsten Jørgensen Eurofins Miljø A/S DK-8464 Galten Ulla Lund, PhD Eurofins Miljø A/S DK-8464 Galten QUALITY MANAGER Jette Groth Eurofins Miljø A/S DK-6600 Vejen Certificate revision history: January 2014 (expiry date added); August 2004 (original certificate date, English version); October 2002 (certificate date, Danish version) Certificate QC Oil in Soil 4 Batch VKI

5 ANNEX TO CERTIFICATE QC OIL IN SOIL Laboratory Measurements m i s ri >nc 10 nc 25 >nc 25 nc 35 n ri Method m i s ri A A D D C B A B A A A A B B B D A A A A A A n ri Method m i Sum of hydrocarbons s ri n ri Method A D B B A A A B D A A A m i : average of laboratory i s ri : standard deviation of laboratory i the series of analysis n ri : number of results for determination of s ri Methods: See explanation on page 3 Batch VKI Certificate QC Oil in Soil

6 ANNEX TO CERTIFICATE QC OIL IN SOIL Certifying Laboratories Denmark AnalyCen A/S, Fredericia Dansk Chemex Eurofins Danmark A/S, Albertslund Eurofins Danmark A/S, Viborg Højvang Miljølaboratorium, Dianalund Milana Miljølaboratoriet, Elsinore Miljøcenter Vestjylland, Holstebro Miljølaboratoriet Storkøbenhavn, Glostrup PC Laboratoriet A/S, Fjerritslev ROVESTA Miljø, Holbæk Technological Institute, Tåstrup Technological Institute, Kemiteknik, Århus Norway Miljøkemi, Norsk Miljø Senter A/S, Oslo Certificate QC Oil in Soil 6 Batch VKI

BATCH: VKI least 97%. Use. Analysis For quality ples. Production. in accordance

BATCH: VKI least 97%. Use. Analysis For quality ples. Production. in accordance Smedeskovvej 39 DK-8464 Galten CERTIFICATE FOR QC ENDOCRINE DISRUPTORS IN MUNICIPAL SLUDGE S ORGANIC MATERIAL BATCH: VKI-27-1-0297 INSTRUCTION FOR USE OF THE REFERENCE MATERIAL L Description, Quantity