ESG & scientific Environmental Scientifics Group Test Report: EJ7813 Report on the Measurement of Uranium Isotopes and 45 Elements Scan in Soil and Oil Samples Prepared for Chris Busby Green Audit August 2010S ©& Scientifics IN scientifics Analysis of Soil and Oil Samples for Uranium Isotopes and 45 Elements Scan Client: Testing Facility Laboratory Reference: Customer Reference: Quote Number: Samples Received: ‘Sample Condition: Analysis Completed: Approved by: Date: Approver's name: Job Title: Report Date: Or Chris Busby Green Audit Castle Cottage Sea View Place Aberystwyth SY23 1DZ Scientifics Harwell Laboratory 551 South Becquerel Avenue Harwell Science and Innovation Campus Chilton Didcot Oxfordshire Ox11 OTB EJ7813 Riga 4 MET-HAR-6415 19 July 2010 Good 24 August 2010 22S 2sf¥|> Sarah James Laboratory Manager 25 August 2010 Test Report £J7813; Page 1 of 12S oO scientifics Scienttcs Introduction Six samples of soil and one sample of oil were received for the measurement of *°Uranium, 28Uranium and total Uranium by ICP-MS and 45 Elements Scan by ICP-AES. On receipt the samples were logged into our system then stored in a secure sample store at room temperature prior to analysis. {tis noted that the samples arrived in good condition. Experimental Analysis was carried out using the following methods. The samples were analysed according to methods: + HS/WI/1075 ‘Operation and Maintenance of Perkin Elmer Optima 4300 Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES), issue 8 * HS/WI1002 ‘Operation and maintenance of inductively coupled plasma mass spectrometers (ICP-MS)', issue 19. The samples were digested in triplicate in concentrated nitric and hydrofluoric acids in fluoropolymer vessels by microwave. Following digestion, the samples were made to a known volume with demineralised water having a resistivity of 18.2 M&cm. The digested samples were diluted as necessary prior to measurement by ICP-MS (Agilent 7500ce). Calibration was achieved using the method of standard addition from a certified uranium standard. Bismuth was added as an internal standard to monitor and correct for instrumental drift. Quality contro! standards at 5.0, 10 and 20 yg.L" total uranium (0.22% *U) were prepared from an alternative source stock solution from that used to prepare the calibration standard and the results are detailed in the table under the heading "QC Standard”. ‘The 45 elements scan was performed by ICP-AES, which was calibrated using certified standards. Results The results obtained are reported in the tables attached in total mg.kg’ in the samples as received and as the ratio °U/5U, The suffixes ‘A, B and C’ after the laboratory reference indicate three independent preparations of each sample respectively. The suffixes ‘1, 2 and 3° after the laboratory reference indicate the independent sample measurements of the same sample digest solutions respectively. LOD is the limit of detection and is defined as three times the standard deviation obtained from the measurement of a series of at least five instrument blanks. Measurement uncertainty for those results significantly above the LOD is typically estimated to be + 20%. Results within an order of magnitude of the LOD have a higher uncertainty. Test Report EJ7813: Page 2 of 12oN S oO scientifics > Scientifies It appears from the variations in the data, that the Uranium 235 concentration is the main factor in affecting the measured ratio. When Uranium 235 concentrations are close to the instrumental LOD, the variation in the measured isotope ratio is large as is shown in the following tables. This is due to the instrument used (conventional quadropole ICP-MS), and to improve these ratios, a more sensitive technique, such as a sector field ICP-MS (High Resolution or Multicollector) would be required, To aid in estimating measurement uncertainty for Uranium analysis, all data are reported to 3 significant figures. Additionally the RSD % for the isotope ratios is presented; this has been calculated on unrounded data Results for Boron in 45 Element Scan are marked as ‘NM’ means Not Measured due to the sample preparation used, where the addition of Boric Acid was required for sample digestion. Although the laboratory holds UKAS accreditation for the measurement of analytes in solution by \CP-AES and ICP-MS, UKAS accreditation is not claimed on these samples. Any opinion and interpretation contained herein is not UKAS accredited. Test Report £J7813: Page 3 of 12\ S & scien ifics Scientifics Results from the Analysis of Oil Sample for *5U and **U by ICP-MS Customer Laboratory 235 238) 2261 225 Reference Reference 7 u aoe ac LOD 0.0007 0.002 NA NA__| EJ7819A1 <0.0007 0.065 0.065 NA EJ7B19A2 0.004 0.081 0.082 NA EJ7B19A3 0.0007 0.064 0.084 NA Cee en (emrsidden NA. NA\ NAL NA\ Mean NA NA NA NA RSD % NA NA NA NA EJ7619AT <0.0007 0.065 0.085 NA EJ7B19A2 0.001 0.081 0.082 37.9 EJ7819A3 <0.0007, 0.064 0.084 150 ee Sid dev NA NA NA\ NA Mean NA NA NA NA, RSD % NA NA NA NA, EJ7819B1 0.007 0.057 0.059 379 J7819B2 0.007 0.059 0.059 77.2 £J7819B3 <0.0007 0.059 0.059 726 Se Std dev NA NA NA NA Mean NA NA NA NA RSD % NA NA NA NA EJ7819C1 0.0007 0.076 0.076 NA EJ7819C2 0.003 0.087 0.070 26.2 EJ7819C3. <0.0007 0.074 0.075 151 ee Std dev NA NA NA NA ‘Mean NA NA NA NA RSD % NA NA NA NA QC Standard 0.23/48 wo. 0.25, 0.26 55,56 NA NA QC Standard 0.45/9.5 wa. 0.51, 0.51 14,14 NA NA QC Standard 0.90/1: 19 ug.L* 0.89, 0.99 20, 22 NA NA 1. Results ore expressed in mg.kg inthe samples as received. 2. The suffix'A, 8 and C' indicates three preparations of each sample respectively. +3. The suffix", 2 and 3"ingicales three measurements of each sample digest solution respectively “4 Results ove’ an order of magnitude above the LOD are estimated to have an uncertainty of = 20%. '5. The expecied results forthe QC Standards are 0.23, 0.45 9° 0.90 ug. (®"U) and 4.8, 9.5 or 19 ugLL" (™U)+ 20% 6, Rallo calculated on normalised biank corrected courts of "UU 7. See notes on page 3 for addional information Test Report EJ7813: Page 8 of 12cN S oO scientifics ° Scientifies The Analysis of Soil Samples for 45 elements Customer Reference Riga 1 Riga 2 Riga 3 Laboratory Reference EJ7813 EJ7814 EJ7815 LoD Ag 4 <1 <1 <1 Al 0.05 29000 16000 25000 As 1 <1 <1 <1 B NM NM NM NM Ba 0.002 230 110 240 Be 0.004 on 0.21 0.59 Bi 02 <0.2 <0.2 <0.2 Ca 0.02 67000 80000 74000 ca 0.04 <0.04 <0.04 <0.04 Co 04 27 67 19 Cr 0.02 140 62 93 cu 0.02 110 <0.02 30 Fe 0.03 40000 41000 26000 Ga 0.05 14 16 1" Ge 0.2 <02 <0.2 <0.2 Hf 0.05 <0.05 <0.05 <0.05 Hg 02 <02 <0.2 <0.2 In 02 <0.2 <0.2 <0.2 K 01 6400 3400 6200 Li 0.05) <0.05 <0.05 <0.05 Mg 0.004 19000 8900 44000 Mn 0.005 500 210 370 Mo 0.2 <0.2 <0.2 <02 4, Results are expressed as mg ka’ Inthe sample as received. 2, Resulls ver an order of magnitude above the LOD are estimated lo have an uncertainty of 420%. 3. Results within an order of magnitude of Ure LOD have a high uncertainty and are reported to one significant igure, “4, Resulls for Boron are marked as NM means" Not Measured! Test Report EJ7813: Page 9 of 12ry S oO scientifics” Scientifics The Analysis of Soil Samples for 45 elements Customer Reference Riga 1 Riga 2 Riga 3 Laboratory Reference £7813 E7814 E7815 Lop Na 0.03 <0.03 <0.03 2100 Nb 0.02 <0.02 <0.02 <0.02 Ni 0.05 65 37, 75 P 05 960 960 560 Pb 0.3 200 <0.3 34 Rb 0.4 87 32 24 s 5 <6 <5 8300 Sb 03 <0.3 <0.3 <0.3 Sc 0,002 6.5 3.3 55 Se 2 <2 <2 <2 Si 04 140000 140000 120000 Sn 03 <0.3 <0.3 <0.3 Sr 0.05 180 110 300 Ta 0.05 <0.05 <0.05 <0.05 Te 06 <0.6 <0.5 <05 Ti 0.003 2800 1200 2300 Tl 04 <0.4 <0.4 <0.4 v 0.01 61 32 50 w 0.4 <0.4 <0.4 <0.4 Y 0,002 99 59 77 Zn 0.1 2600 <0. 49 zr 0.03 40 7 41 4, Results are expressed as mg kg" in the sample as received. 2. Results over an order of magnitude above the LOD are estimated to have an uncertainty of 420%, except for Si where ies 250%, 3, Results within an order of magnitude ofthe LOD have @ high uncertainty anc are reported to one significant figure. Test Report EJ7813: Page 10 of 12S OC scientifics” Scientifics The Analysis of Soil Samples for 45 elements Customer Reference Riga 4 Riga 5 Riga 6 Laboratory Reference EJ7816 £J7817 £/7818 Lop Ag 1 <1 <1 <1 Al 0.05 21000 15000 23000 As 1 <1 42 <1 B NM NM NM NM Ba 0.002 190 7 290 Be 0.001 oat 0.18 0.41 Bi 02 <0.2 <0.2 <0.2 Ca 0.02 95000 62000 63000 cd 0.04 <0.04 <0.04 <0.04 Co of 130 44 5A cr 0.02 7 95 81 cu 0.02 60 33 <0.02 Fe 0.03 20000 8900 15000 Ga 0.05 5 82 4 Ge 02 <0.2 <0.2 <0.2 HF 0.05 <0.05 <0.05 <0.05 Hg 02 <02 <02 <0.2 in 02 <0.2 <0.2 <02 K 4 5200 3400 6500 ui 0.05 <0.05 <0.05 <0.05 Mg 0.004 13000 6200 13000 Mn 0.005 340 160 290 Mo 02 <0.2 <02 <0.2 Results are expressed as mg kg" inthe sample as received. Results aver an order of magnitude above the LOD are estimated to have an uncertainty of 420%. Resulls wilhin an order of magnitude ofthe LOD have a high uncerinty and are reported o one signicant igure, Resulls for Boron are marked as NM means ' Not Measured. 1 2 3 4 Test Report £7813: Page 11 of 12S © scientifies > Scientifies The Analysis of Soil Samples for 45 elements Customer Reference Riga 4 Riga 5 Riga 6 Laboratory Reference E7816 E7817 Ev7618 Lop Na 0.03 7.6 10000 47 Nb 0.02 <0.02 <0.02 <0.02 Ni 0.05 45 27 38 P 05 910 120 470 Pb 03 98 <0.3 <0.3 Rb 04 47 26 24 s 5 <5 37000 <5 Sb 0.3 <0.3 <0.3 <0.3 Se 0.002 47 34 48 Se 2 <2 <2 <2 Si 04 120000 120000 73000 Sn 0.3 <0.3 39 <0.3 ‘st 0.05 280 370 200 Ta 0.05 <0.05 <0.05 <0.05 Te 05 <0.5, <0.5 <0.5 Ti 0.003 2700 1000 1500 TI 04 <0.4 <0.4 <0.4 v 0.01 45 32 40 w 0.4 <0.4 <0.4 <0.4 Y 0.002 73 36 84 Zn o4 510 <0.4 <0.4 Zr 0.03 19 "1 26 4. Resuls ae expressed as mg kg" inthe sample as received, 2. Results over an order of magritude above the LOD are estimated to have an uncertainty of 220%, except for Si where itis 250%, 3, Results within an order of magnitude ofthe LOD have a high unce ly and are reported to one significant figure. Test Report £J7813: Page 12 of 12 1018