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1 Proficiency test SPIL-4 (2012) Nitrogen parameters in wastewater (effluent) Quality Documentation May 2013
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3 Proficiency test SPIL-4 (2012) Quality documentation Smedeskovvej 38, DK-8464 Galten, Denmark May 2013 Tel: Fax: Web: Client Environmental laboratories Client s representative Project Proficiency test SPIL-4 (2012) Project No Authors Ulla Lund Date Approved by Carsten Theisen Pedersen Quality Documentation UOL CTP Revision Description Key words Analytica quality, assigned value, precision, accuracy, homogeneity, stability, total nitrogen, ammonium, nitrite+nitrate, conductivity, ph, wastewater By Approved Classificationn Open Internal Proprietary Date Distribution DANAK Eurofins: Ulla Lund, Carsten Theisenn Pedersen No of copies File File
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5 1 CONTENTS 1 INTRODUCTION FEATURES OF THE PROFICIENCY TEST Sample preparation Statistical analysis of participants data Assigned and spike value Assigned and spike values Test of spike values Test of assigned values HOMOGENEITY AND STABILITY OF SAMPLES CONCLUSION REFERENCES... 6 APPENDICES A List of participants... A-1 B Sample preparation... B-1 C Control of spike value... C-1 D Control of recovery... D-1 E Concentration level... E-1 F Homogeneity and stability... F-1
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7 1 INTRODUCTION A proficiency test on the analysis of nitrogen parameters in wastewater was conducted on 8 November The proficiency test was organised by Eurofins Miljø A/S. The present report contains Eurofins documentation for the quality of the proficiency test. Results of the proficiency test including data from participating laboratories and statistical analysis of these data were issued in a report to all participants and DANAK /1/ on 10 December
8 2 FEATURES OF THE PROFICIENCY TEST Participants in the proficiency test were a total of 77 laboratories from Denmark, Norway and Sweden. A list of participants is shown in Appendix A. The closing date for submission of results was 26 November All participants had submitted their results before the dead-line. 2.1 Sample preparation The parameters covered in the proficiency test are listed in Table 2 as are the abbreviations used in this report. Four samples were dispatched for the proficiency test. The samples were sample pairs covering the parameters as described in Table 1. The matrix of the samples represented wastewater, in this case effluent. Sample preparation is described in Appendix B. Table 1 Samples in the proficiency test Sample name Parameters A1/B1 TN, NH 4, NO 2+3, γ 25 A2/B2 ph 2.2 Statistical analysis of participants data A split-level design was used. The data analysis was performed in accordance with ISO 5725: Accuracy (trueness and precision) of measurement methods and results (1994) /2/ and as described in detail in Spliid (1992) /3/. A short introduction to the statistics and a list of symbols and abbreviations used is given in Eurofins document Schedule for a proficiency test, which is available at Eurofins home page /4/. The statistical model used is based on the assumption that the variances for the two samples in a sample pair are identical. The assumption was tested (F-test, 95% confidence level) and the result was that the two variances may be assumed to be identical for all parameters. 2.3 Assigned and spike value An overview of the concentrations in the samples (the assigned values) and the difference in concentration between the two samples of a sample pair (spike value) are shown in Table 2 compared to the range of concentrations normally encountered in effluent. The table also gives the expanded uncertainty of the assigned values. 2
9 Table 2 Assigned and spike value Parameter Abbreviation Unit Typical Range Assigned value Uncertainty of assigned value Spike value Total nitrogen TN mg/l N Ammonium NH 4 mg/l N Nitrite+nitrate NO 2+3 mg/l N Conductivity γ 25 ms/m ph ph Assigned and spike values The content of each parameter in each sample is given an assigned value for the sample with the lower content and a spike value, the spike value being the difference in concentration between the two samples of the sample pair. In order to ensure optimal use of the data, the assigned value is calculated as the average of the median for both samples in the sample pair after subtraction of the spike value. The spike values are calculated from sample preparation except for γ 25 where the spike value is the difference between median values for the two samples in the sample pair. The assigned value for TN is operationally defined and is a consensus value based upon the median for method no. 2. A list of method identification numbers is found in the report to participants /1/. A number of laboratories submitted results for conductivity that were obviously in another unit than specified. These results were excluded before estimation of the assigned value. Assigned values for NH 4, NO 2+3 and ph are consensus values for all laboratories based on the median Test of spike values A comparison was made (t-test, 95% confidence level) between the spike value and the difference in concentration between the two samples in the sample pair found from the laboratories results, see Appendix C. The tests showed no significant difference between the two Test of assigned values The assigned value and the average of the results obtained from all laboratories were also compared (t-test, 95% confidence level), see Appendix D. The test showed no significant difference between the two for most parameters and the control of assigned value at Eurofins confirmed the value (Appendix E). The exception is TN. Average recovery for TN was 98.5%. The difference could be attributed to influence from laboratories using methods other than those prescribed by the Danish EPA. The test was repeated after exclusion of the results for method no. 6, 62, 71, 710, 71A, 72 and 9 and now showed no significant difference and an average recovery of 99.8%. Furthermore, the results of control measurements at Eurofins confirmed the assigned value (Appendix E). The assigned value is therefore kept unchanged. 3
10 3 HOMOGENEITY AND STABILITY OF SAMPLES The homogeneity and stability of samples were tested using the following parameters as indicators: NH4 NO3 ph Homogeneity test Combined homogeneity and stability test Homogeneity test The results of control measurements are shown in Appendix F. The appendix also gives the results of the statistical evaluation of the control data. The data are analysed by analysis of variance (ANOVA) giving: 1. the standard deviation/variance for replicates (the contribution from analytical variability), 2. the between bottle standard deviation/variance (the contribution from heterogeneity) and 3. the between days concentration difference (the contribution from instability). Homogeneity is evaluated by comparing the between bottle variance to 0.15 * the maximum tolerated deviation from the assigned value specified by the Danish EPA /5/ ( sigma in the calculations is 0.5 times the maximum tolerated deviation), whereas the stability is evaluated by comparing the concentration change of the samples to 0.15 * the maximum tolerated deviation from the assigned value specified by the Danish EPA /5/. This test ensures that heterogeneity and instability will not have negative influence on the evaluation of participant performance /6/. The appendix also shows the standard deviation within and between laboratories from the proficiency test to allow comparison between tests performed and average quality from participating laboratories. The tests for stability and homogeneity show that the samples are stable and homogeneous. 4
11 4 CONCLUSION The quality control performed, including test of sample stability and homogeneity as well as test of recovery of spike and assigned values, shows that the samples and their assigned values are suitable for testing the proficiency of the participating laboratories for all parameters. The results are also suitable for estimation of the general quality of analyses among all participating laboratories. For total nitrogen the participants did not recover the assigned value. Eurofins scrutiny of the combined evidence gave the conclusion that the assigned value is correct. The assigned value is therefore kept unchanged and it is recommended as the basis for evaluation of participating laboratories. 5
12 5 REFERENCES /1/ Eurofins A/S, Proficiency test SPIL-4 (2012), Report to participants, December /2/ ISO , Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method, /3/ Spliid, H., Procedure and analysis of data for proficiency tests and environmental analyses, Report to Danish Environmental Protection Agency, 1994 (in Danish). /4/ Eurofins A/S, Schedule for a proficiency test, document may be downloaded from /5/ Ministry of Environment regulation no. 900 on quality criteria for environmental measurements, 17 August 2011 (in Danish). /6/ ISO 13528, Statistical methods for use in proficiency testing by interlaboratory comparison,
13 APPENDICES
14 APPENDIX A List of participants
15 Laboratory Town Country Eurofins Miljø A/S Vejen Danmark Højmarklaboratoriet Lem St. Danmark Vandsamarbejdet A/S Holstebro Danmark CP Kelco ApS, Spildevandslaboratoriet Ll. Skensved Danmark Sun Chemicals, E30 Køge Danmark AquaDjurs - Fornæs Renseanlæg Grenaa Danmark Bjergmarken R/A, Roskilde Forsyning Roskilde Danmark Faxe Spildevand Faxe Danmark Faxe Spildevand Faxe Danmark Fredericia Spildevand A/S Fredericia Danmark Greve Solrød Forsyning Greve Danmark Hach Lange ApS Brønshøj Danmark Halsnæs Kommunale Forsyning A/S Liseleje Danmark Hedensted Spildevand A/S Daugård Danmark Hedensted Spildevand A/S Daugård Danmark Holstebro Centralrenseanlæg, Vestforsyning A/S Holstebro Danmark Ikast-Brande Spildevand Ikast Danmark Kerteminde Forsyning - Spildevand A/S Kerteminde Danmark Kolding Spildevand A/S Bjert Danmark Køge-Egnens Renseanlæg Køge Danmark Lynettefællesskabet I/S København K Danmark Mølleåværkets Driftslaboratorium Lyngby Danmark Nyborg Renseanlæg Nyborg Danmark Næstved Centralrenseanlæg Næstved Danmark Provas Haderslev Forsyningsservice Haderslev Danmark Randers Spildevand A/S Randers NØ Danmark Rensningsanlæg Øst, Esbjerg Esbjerg Danmark Rensningsanlæg Øst, Esbjerg, Spildevandslaboratoriet Esbjerg Danmark Ringkøbing-Skjern Forsyning A/S, Spildevand Skjern Danmark Ringsted Renseanlæg Ringsted Danmark Rønne Renseanlæg Rønne Danmark SK Forsyning, Slagelse Renseanlæg Slagelse Danmark SK Forsyning, Slagelse Renseanlæg Slagelse Danmark SK Forsyning, Slagelse Renseanlæg Slagelse Danmark SK Forsyning, Slagelse Renseanlæg Slagelse Danmark Svendborg Centralrenseanlæg Skårup Fyn Danmark Sønderborg Renseanlæg Sønderborg Danmark Vandrens - Stigsnæs Industripark A/S Skælskør Danmark A-1
16 Laboratory Town Country Vejen Renseanlæg Vejen Danmark Vejle Spildevand A/S Vejle Danmark Ålborg Renseanlæg Vest Ålborg Danmark Ålborg Renseanlæg Øst Ålborg Øst Danmark Dianalund Renseanlæg Dianalund Danmark Norges Geotekniske Institutt Oslo Norge Statoil Petroleum AS, Snøhvit Melkøya, drift Hammerfest Norge Eurofins Environment Testing Sweden AB Lidköping Sverige Arctic Paper Munkedals AB Munkedal Sverige Holmen Paper Norrköping Sverige Ineos Sverige AB Stenungsund Sverige Preem AB Göteborg Göteborg Sverige Preemraff Lysekil Lysekil Sverige Rottneros Bruk AB Rottneros Sverige Smurfit Kappa Kraftliner Piteå Sverige St1 Refinery AB Göteborg Sverige Stora Enso Publication Paper Hyltebruk Sverige Södra Cell AB Mönsterås Mönsterås Sverige Trollhättan Energi AB, Arvidstorps Lab. Trollhättan Sverige Yara AB Köping Sverige Ernemar Laboratoriet Oskarshamn Sverige GRYAAB AB Göteborg Sverige Kalmar Vatten AB, VA-lab, Avloppsreningsverket Kalmar Sverige Kristianstad Kommun, C4 Teknik, Kommunteknik Kristianstad Sverige Käppalaverket Lidingö Sverige Laboratoriet vid Smedjeholms Arv Falkenberg Sverige Mjölby Kommun Mjölby Sverige Motala Kommun Motala Sverige Skellefteå Kommun, Tekniska kontoret VAA-avd. Skellefteå Sverige Tekniska förvaltningen, Verksamhetsstöd VA, Laboratoriet Örebro Sverige Uddebo Laboratorium Luleå Sverige Uppsala Vatten o. Avfall AB, Vattenlaboratoriet Uppsala Sverige VA SYD Klaghamns Avloppsreningsverket Malmö Sverige VA SYD Källby Avloppsreningsverk Malmö Sverige VA SYD Sjölundalaboratoriet Malmö Sverige VA-SYD, Ellingelaboratoriet Malmö Sverige VIVAB Varberg Sverige Västerviks Miljö & Energi AB, Vattenlaboratoriet Västervik Sverige A-2
17 Laboratory Town Country Vallviks Bruk AB Vallvik Sverige A-3
18 APPENDIX B Sample preparation
19 Stock solution Prepared from Concentration Stock NH g Ammonium chloride (NH 4 Cl) milli-q water up to g NH 4 : mg/kg N Stock NO g Potassium nitrate (KNO 3 ) milli-q water up to g NO 3 : mg/kg N B-2 Sample Sample prepared from A g stock NH kg Milli-Q water Filtered effluent from Darum wastewater treatment plant up to 70,00 kg B g stock NH 4 0 g stock NO 3 0 g stock TN Sample A1 up to kg TN mg/l N NH 4 mg/l N NO 3 mg/l N Conductivity ms/m c a b d (c+0.748) (a+0.748) b e Sample Sample prepared from A2/B2 Filtered effluent from Darum wastewater treatment plant ph f B-1
20 APPENDIX C Control of spike value
21 Total nitrogen, mg/l N Control of differences within sample pairs Laboratory Difference AB A B A B UC UC UC A B A B A - 74B No of labs., p 72 No of repl., n 2 d s² s t = p (d/s) Sign. level, p(t) No test statistics were found to be significant UC denotes a Cochran outlier C-1
22 Ammonium, mg/l N Control of differences within sample pairs Laboratory Difference AB UC 3A B - 4A B UC UG A B A B A UC 74B UC No of labs., p 66 No of repl., n 2 d s² s t = p (d/s) Sign. level, p(t) No test statistics were found to be significant UC denotes a Cochran outlier UG denotes a Grubbs outlier C-2
23 Nitrite+nitrate, mg/l N Control of differences within sample pairs Laboratory Difference AB A B - 4A B UC UC UC A B A B A - 74B No of labs., p 59 No of repl., n 2 d s² s t = p (d/s) Sign. level, p(t) No test statistics were found to be significant UC denotes a Cochran outlier C-3
24 Conductivity, ms/m Control of differences within sample pairs Laboratory Difference AB A - 3B - 4A - 4B U U U UG UC U U U U U A - 69B - 70A B A B No of labs., p 23 No of repl., n 2 d 0.00 s² 0.01 s 0.10 t = p (d/s) Sign. level, p(t) No test statistics were found to be significant UC denotes a Cochran outlier UG denotes a Grubbs outlier U denotes data excluded from the data file due to an error in units C-4
25 ph, Control of differences within sample pairs Laboratory Difference AB A B - 4A B UC UC A B - 70A B A B No of labs., p 70 No of repl., n 2 d s² s t = p (d/s) Sign. level, p(t) No test statistics were found to be significant UC denotes a Cochran outlier C-5
26 APPENDIX D Control of recovery
27 Total nitrogen, mg/l N Control of recovery, average of results Laboratory Sample pair AB A B A B UC UC UC A B A B A - 74B No of labs., p 72 No of repl., n 2 m s² s Assigned value, µ 5.7 Recovery, % 98.5 t = p (m-µ)/s Sign. level, p(t) * * denotes that there is a significant difference (t-test, 5%-level) ** denotes that there is a significant difference (t-test, 1%-level) *** denotes that there is a significant difference (t-test, 0.1%-level) UC denotes a Cochran outlier D-1
28 Ammonium, mg/l N Control of recovery, average of results Laboratory Sample pair AB UC 3A B - 4A B UC UG A B A B A UC 74B UC No of labs., p 66 No of repl., n 2 m s² s Assigned value, µ Recovery, % 99.9 t = p (m-µ)/s Sign. level, p(t) No test statistics were found to be significant UC denotes a Cochran outlier UG denotes a Grubbs outlier D-2
29 Nitrite+nitrate, mg/l N Control of recovery, average of results Laboratory Sample pair AB A B - 4A B UC UC UC A B A B A - 74B No of labs., p 59 No of repl., n 2 m s² s Assigned value, µ 4.52 Recovery, % 99.9 t = p (m-µ)/s Sign. level, p(t) No test statistics were found to be significant UC denotes a Cochran outlier D-3
30 Conductivity, ms/m Control of recovery, average of results Laboratory Sample pair AB A - 3B - 4A - 4B U U U UG UC U U U U U A - 69B - 70A B A B No of labs., p 23 No of repl., n 2 m s² 0.08 s 0.28 Assigned value, µ Recovery, % t = p (m-µ)/s Sign. level, p(t) No test statistics were found to be significant UC denotes a Cochran outlier UG denotes a Grubbs outlier U denotes data excluded from the data file due to an error in units D-4
31 ph, Control of recovery, average of results Laboratory Sample pair AB A B - 4A B UC UC A B - 70A B A B No of labs., p 70 No of repl., n 2 m s² s Assigned value, µ 7.27 Recovery, % 99.6 t = p (m-µ)/s Sign. level, p(t) No test statistics were found to be significant UC denotes a Cochran outlier D-5
32 APPENDIX E Concentration level
33 Concentration level SPIL-4 (2012) Parameter Unit Sample Bottle no. I II Bottle Sample Assigned Spike Average Average value Measured Assigned Total nitrogen mg/l N A1 50 5,62 5,70 5,66 5,66 5,7-0,61 0,6 B1 87 6,29 6,24 6,27 6,27 6,3 Ammonium mg/l N A1 50 0,746 0,735 0,741 0,741 0,758 0,003 0,000 B1 87 0,740 0,734 0,737 0,737 0,758 E-1 Nitrite+nitrate mg/l N A1 50 4,42 4,43 4,43 4,43 4,52-0,61 0,6 B1 87 5,03 5,03 5,03 5,03 5,12 ph A2 79 7,18 7,18 7,18 7,27-0,05 0 B2 86 7,23 7,23 7,23 7,27
34 APPENDIX F Homogeneity and stability
35 PT: SPIL Parameter: NH4 Unit: mg/l N Sigma: 0,050 6,5% of level Responsible for tests: agk/kms 6,5% of level or 1,3*S T max Homogeneity test Date: Stability test Date: Sample x(a) x(b) average sd sd^2 Sample x(a) x(b) B-1 0,775 0,775 0,775 0,0000 0,000 B-9 0,771 0,768 0,770 0,0021 0,000 B-18 0,781 0,777 0,779 0,0028 0,000 B-27 0,778 0,789 0,784 0,0078 0,000 B-36 0,782 0,785 0,784 0,0021 0,000 B-45 0,785 0,773 0,779 0,0085 0,000 For stability B-54 0,783 0,785 0,784 0,0014 0,000 General average (y): B-63 0,776 0,785 0,781 0,0064 0,000 /x-y/ = B-72 0,774 0,78 0,777 0,0042 0,000 B-81 0,771 0,776 0,774 0,0035 0,000 B-90 0,773 0,768 0,771 0,0035 0,000 B-94 0,767 0,764 0,766 0,0021 0,000 Conclusions ss = 0, *sigma= 0,015 For homogeneity /x-y/ = General average (x) 0,777 Analytical Is s w < 0,15*sigma Sample average sd (s x ) 0,0060 quality YES Within-sample sd (s w ): 0,0045 Between-samples sd (ss): 0,0051 Homogeneity: Is ss < 0.3*sigma? S L in the Proficiency Test: 0,0378 YES S R in the Proficiency Test: 0,0387 Stability: /x-y/ < 0.3*sigma? No data F-1
36 PT: SPIL Parameter: NO2+3 Unit: mg/l N Sigma: 0,33 6,5% of level Responsible for tests: kma/agk 6,5% of level or 1,3*S T max Homogeneity test Date: Stability test Date: Sample x(a) x(b) average sd sd^2 Sample x(a) x(b) B-1 4,96 5,08 5,02 0,085 0,007 B-87 5,03 B-9 4,95 5,03 4,99 0,057 0,00 B-18 5,00 5,02 5,01 0,014 0,000 B-27 4,94 5,05 5,00 0,078 0,006 B-36 5,02 5,09 5,06 0,049 0,002 B-45 4,99 4,98 4,99 0,007 0,000 For stability B-54 4,97 5,04 5,01 0,049 0,002 General average (y): 5,03 B-63 4,98 5,07 5,03 0,064 0,004 /x-y/ = 0,015 B-72 5,03 4,99 5,01 0,028 0,001 B-81 4,96 5,04 5,00 0,057 0,003 B-90 5,04 5,07 5,06 0,021 0,000 B-94 5,01 5,04 5,03 0,021 0,000 Conclusions ss = 0 0.3*sigma= 0,10 For homogeneity /x-y/ = 0, General average (x) 5,01 Analytical Is s w < 0,15*sigma Sample average sd (s x ) 0,023 quality NO Within-sample sd (s w ): 0,050 Between-samples sd (ss): 0 Homogeneity: Is ss < 0.3*sigma? S L in the Proficiency Test: 0,151 YES S R in the Proficiency Test: 0,154 Stability: /x-y/ < 0.3*sigma? YES F-2
37 PT: SPIL Parameter: ph Unit: 1,3*s T Sigma: 0,065 max Responsible for tests: agk/kms 6,5%of level or 1,3*S T max Homogeneity test Date: Stability test Date: Sample x(a) x(b) average sd sd^2 Sample x(a) x(b) B-1 6,96 B-10 7,01 7,01 B-20 7,02 7,02 B-30 7,04 7,04 B-41 7,06 7,06 B-52 7,04 7,04 For stability B-62 7,05 7,05 General average (y): B-72 7,06 7,06 /x-y/ = B-83 7,04 7,04 B-94 7,06 7,06 B-104 7,03 7,03 B-106 7,04 7,04 Conclusions ss = 0, *sigma= 0,020 For homogeneity /x-y/ = General average (x) 7,04 Analytical Is s w < 0,15*sigma Sample average sd (s x ) 0,016 quality No data Within-sample sd (s w ): Between-samples sd (ss): 0,016 Homogeneity: Is ss < 0.3*sigma? S L in the Proficiency Test: 0,149 YES S R in the Proficiency Test: 0,157 Stability: /x-y/ < 0.3*sigma? No data F-3
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