It is important that the batch numbers of the reference material and on the certificate are identical.

Transcription

1 Eurofins Miljø A/S Smeeskovvej 38 DK-8464 Galten CERTIFICATE FOR QC DWB MAJOR COMPONENTS IN DRINKING WATER BATCH: VKI an VKI INSTRUCTIONS FOR USE OF THE REFERENCE MATERIAL Description This reference material consists of two ifferent ampoules with concentrates for preparation of one reference sample for quality control after ilution with water. The certificate inclues ocumentation for the analytical parameters soium, potassium, calcium, magnesium, chlorie, fluorie, sulphate, hyrogen carbonate, conuctivity, ph an total issolve solis. Quantity an Preservation For practical reasons, QC DWB consists of 2 types of ampoules packe separately: QC DW1B an QC DW2B. 1 L reference sample is prouce by ilution of 10 ml of each of the two concentrates. The concentrates are preserve by autoclaving. Use The reference material is intene for quality control, i.e. measurement an control of the accuracy an precision of analyses. It is typically intene for analyses of major components in rinking water. It may also be use in the quality control of other types of water samples an for the implementation an optimisation of analytical instruments an analytical methos. It is important that the batch numbers of the reference material an on the certificate are ientical. Preparation for Use Stabilise the ampoules at room temperature (approx. 20 C). Break the ampoule neck of DW1B an DW2B open at the mark, withraw the concentrate with a pipette, an ilute as follows: Distille water (or water of equivalent purity) 500 ml QC DW1B 10,0 ml QC DW2B 10,0 ml Distille water (or water of equivalent purity) up to 1000 ml The reference material is only certifie for sample preparation using both ampoule concentrates. The certifie concentrations are given in the table on page 3 of this certificate. Analysis For quality control the reference material is analyse at the same time an in the same manner as other samples. This certificate is prepare in accorance with the international ISO guielines for certification of reference materials /1/ an /2/.

2 Storage an Durability Store the ampoules protecte from sunlight, e.g. in the ampoule boxes, an at room temperature or in a refrigerator. The certificate is vali until 1 st of October 2019 provie the material is store uner the recommene conitions. PRODUCTION OF THE REFERENCE MATERIAL AND DOCUMENTATION Prouction The prouction of this reference material is in accorance with the quality management proceures of Eurofins, with the aim of obtaining the intene quality of the material. Documentation of Content All ocumentation for the reference material has been performe after ilution of the ampoule concentrates as escribe above. Internal control The analytical quality of Eurofins has been ocumente an foun satisfactory by regular participation in international proficiency tests. Homogeneity: The homogeneity has been investigate by measurements of soium, potassium, calcium, magnesium, chlorie an sulphate in ranomly selecte ampoules of QC DWB. Tests for homogeneity have been performe by comparing the stanar eviation between the reference material units with the within batch stanar eviation obtaine from uplicate measurements of the reference material in the same sample (Ftest, 95%). In aition, homogeneity testing in accorance with ISO Guie 35 /1/ was inclue in the external control. No inication of heterogeneity was foun. Stability: The stability of the reference material is being followe at 5 C, 20 C an 37 C, an no inication of instability was observe at the ate of this certificate. External control The concentration of major components in the reference material was etermine by selecte laboratories in an external ocumentation in September The participating laboratories are skille an have ocumente goo analytical quality by participation in interlaboratory comparisons an by analysis of a control sample in the certification. The laboratories were requeste to analyse five samples of QC-DWB: three samples in the same analytical series, one by uplicate etermination, an two samples in two ifferent analytical series as single eterminations. The statistics are in accorance with the international stanar: ISO Guie 35 /1/. On the basis of the analytical results submitte by the laboratories the following statistical parameters have been calculate: Y : average, calculate in accorance with ISO Guie 35 (section ): s L : stanar eviation between the laboratories, calculate in accorance with ISO Guie 35 (section ): 1 p 1 Y i Y 2 The 95% confience interval of the true mean value of analytical results is: Y ± t 0,025 sl ( ). p where p: number of laboratories inclue in calculations ν: p-1, egrees of freeom Certificate QC DWB 2 Batch VKI an VKI

3 t 0,025 (ν): t value of 0,025 level at ν egrees of freeom. The criteria for selection of laboratories were as follows: the laboratory results in proficiency tests iverge less than 2 stanar eviations from the nominal value, an the laboratory analyses more than 20 analytical series each year or hols accreitation for the parameter. the laboratory result for the control sample in the certification stuy eviate less than 10% (0.2 phunits) from the nominal value, an the laboratory results in the certification stuy are not Cochran outliers or Grubbs outliers or eeme to be an outlier base on a scientific evaluation. The ata inclue in the external control an names of the participating laboratories are liste in an annex to this certificate. On the basis of the selecte results, the following has been calculate: Certifie Values DETERMINAND UNIT AVERAGE BETWEEN LABORATORY STANDARD DEVIATION 95% CONFIDENCE LIMITS OF THE AVERAGE VALUE Y ± t 0,025 sl ( ). p NUMBER OF DATA SETS IN CALCULATIONS/ METHOD Y s L Lower Upper (p) Soium 51 2, /A 4/B 5/D EXCLUDED DATA SETS C: Cochran outlier G: Grubbs outlier 1C Potassium 5,12 0,054 5,08 5,17 Calcium 25,7 0,92 25,2 26,2 Magnesium 5,0 0,19 4,9 5,2 Chlorie 60,4 1,5 59,5 61,2 Fluorie 0,99 0,036 0,96 1,02 Sulphate 60 1, /A 4/B 3/D 3/A 3/B 2/C 6/D 3/A 3/B 1/C 6/D 2/A 9/B 3/C 2/A 5/B 1/A 6/B 1/C 1C, 1G 2C 3C Hyrogen carbonate (HCO 3) mmol/l* 62,9 1,03 1,4 0,023 62,1 1,02 63,8 1,05 1/A 6/B 3/C 1/D 1/E 1/X 2C Conuctivity ( 25) ms/m 44,8 0,37 44,6 45,1 11/A 3/B 5C, 2G ph (25 C) 8,84 0,073 8,81 8,88 18/A 3C Total issolve solis 247 4, /A 3C * : The results are measure in ; the concentrations in mmol/l are calculate on this basis. Batch VKI an VKI Certificate QC DWB

4 s Soium, potassium: A F-AAS (DS 258:1985, SFS 3017, NS 4775, SS , SM 19. e Na D / K D) B ICP-AES (EN ISO an others) C Ion chromatography (EN ISO an others) D ICP-MS (EN ISO an others) Calcium, magnesium: A F-AAS (DS 238:1985, SFS 3018, NS 4776, SS ) B ICP-AES (EN ISO an others) C Ion chromatography (EN ISO an others) D ICP-MS (EN ISO an others) Chlorie: A Potentiometric titration with silver nitrate (DS 239:1984, SFS 3006, NS 4756, SS ) B Ion chromatography (EN ISO an others) C Flow analysis with photometric or potentiometric etection (EN ISO 15682, SM 17. e. 4500Cl - E) Fluorie: A Potentiometric measurement with ion selective elektroe (DS 218, SFS 3037, NS 4740, SS ) B Ion chromatography (EN ISO an others) Sulphate: A Measurement of turbiity after precipitation with barium (DS 286:1990, SS , EPA 375.4) B Ion chromatography (EN ISO an others) C Measurement of turbiity after precipitation with barium (SM 17. e F - E) Hyrogen carbonate: A Potentiometric measurement (DS 253:1977) B Potentiometric measurement (EN ISO ) C Potentiometric measurement (EN ISO ) D Titrimetric measurement (SS ) E Titrimetric measurement (SM 20. e. 2320A) Conuctivity: A Electrometric measurement (EN 27888, ISO 7888) B Electrometric measurement (DS 288, SS ) ph: A Potentiometric measurement (DS 287:1978, SFS 3021, NS 4720, SS ) Total issolve solis: M Drying of the evaporate sample for > 2 hours at 105 C 3 C (DS 204:1980, SFS 3008, NS 4764, SS ) X Other methos Use of the Certifie Values For laboratories with an analytical quality that is comparable to that of the laboratories who have contribute to the external control ata of this certificate, the following applies: 1) For single eterminations, analytical results will with a probability of 95% be in the interval: Y ± t ( 0,025 ).s L 2) Analytical results, calculate as the average of two eterminations will with a probability of 95% be in the interval: Y ± t 0,025 sl ( ). 2 Certificate QC DWB 4 Batch VKI an VKI

5 REFERENCES /1/ ISO guie 35:2006. Certification of reference materials - General an statistical principles for certification. /2/ ISO guie 31:2000 Reference materials - Contents of certificates an labels. Date of issue: January 2016 DIRECTOR RESPONSIBLE SCIENTIST Karsten Jørgensen Eurofins Miljø A/S DK-8464 Galten Ulla Lun, PhD Eurofins Miljø A/S DK-8464 Galten QUALITY DIRECTOR Jette Groth Eurofins Miljø A/S DK-6600 Vejen Certificate revision history: January 2016 (expiry ate extene); December 2013 (expiry ate ae); September 2011 (original certificate ate) Batch VKI an VKI Certificate QC DWB

6 ANNEX TO CERTIFICATE QC DWB Laboratory Measurements Soium Calcium 55,6 1,28 4 2,90 3 D 51,1 0,39 4 1,03 3 A 50,7 0,79 4 0,58 3 B 49,2 1,01 4 0,94 3 D 51,1 0,70 4 0,10 3 B 54,9 0,52 4 0,82 3 A 52,4 0,32 4 1,83 3 B 48,6 0,39 4 1,42 3 D 50,3 1,18 4 0,32 3 B 49,8 0,81 4 0,98 3 D 50,3 0,40 4 1,00 3 A 52,7 0,35 4 1,45 3 D 27,2 0,34 4 2,15 3 D 24,9 1,82 4 1,13 3 C 26,9 0,51 4 0,80 3 A 25,1 0,20 4 0,46 3 C 25,2 0,54 4 0,32 3 D 26,2 0,93 4 0,15 3 B 24,5 0,30 4 0,38 3 A 27,3 0,10 4 0,44 3 B 25,5 0,13 4 0,13 3 D 24,5 0,36 4 1,59 3 B 25,6 0,42 4 0,15 3 D 26,2 0,36 4 0,55 3 D 25,4 0,10 4 0,49 3 A 25,3 0,14 4 1,07 3 D Potassium Magnesium 5,09 0, ,081 3 A 5,06 0, ,074 3 B 5,13 0, ,034 3 D 5,19 0, ,009 3 B 5,22 0, ,076 3 B 5,08 0, ,042 3 D 5,13 0, ,015 3 B 5,09 0, ,044 3 D 5,5 0, ,40 3 D 5,0 0, ,06 3 A 5,0 0, ,05 3 C 5,0 0, ,16 3 D 5,2 0, ,01 3 B 5,0 0, ,18 3 A 5,3 0, ,13 3 B 4,8 0, ,09 3 D 4,8 0, ,02 3 B 4,9 0, ,16 3 D 4,9 0, ,19 3 D 5,1 0, ,04 3 A 5,0 0, ,28 3 D Certificate QC DWB 6 Batch VKI an VKI

7 Chlorie Sulphate 60,1 0,20 4 0,48 3 A 62,5 0,16 4 1,55 3 B 59,2 0,19 4 0,13 3 B 60,8 0,10 4 0,67 3 B 56,6 1,30 4 0,48 3 C 60,2 0,30 3 0,89 3 C 61,7 0,74 4 0,60 3 B 60,4 0,24 4 0,25 3 B 60,5 0,13 4 0,03 3 B 61,6 0,88 4 0,67 3 B 60,2 0,22 4 0,86 3 B 59,1 0,34 4 1,14 3 B 62,3 0,47 4 1,17 3 C 60,1 0,35 4 0,41 3 A 59 0,08 4 0,06 3 B 61 0,10 4 0,68 3 B 58 0,17 4 0,49 3 C 61 0,19 4 0,23 3 B 60 0,13 4 0,04 3 B 62 0,79 4 0,21 3 B 60 0,05 4 0,50 3 B 61 0,77 4 0,94 3 A Fluorie Hyrogen carbonate 0,94 0, ,017 3 B 0,98 0, ,055 3 A 1,02 0, ,013 3 B 0,98 0, ,000 3 B 1,05 0, ,019 3 B 0,97 0, ,010 3 B 0,99 0, ,001 3 A 62,6 0,59 4 1,42 3 B 64,7 0,60 4 0,79 3 E 63,0 0,00 4 0,72 3 C 62,4 0,28 4 0,15 3 B 64,7 1,00 4 0,86 3 D 65,5 0,07 4 0,18 3 B 62,8 1,01 4 0,22 3 C 63,2 0,25 4 0,28 3 C 62,3 1,20 4 1,30 3 B 60,9 0,23 4 0,98 3 B 61,1 0,75 4 0,38 3 B 62,5 0,08 4 A 62,6 0,58 4 0,49 3 X Batch VKI an VKI Certificate QC DWB

8 Conuctivity Total issolve solis ms/m ms/m ms/m 44,6 0,10 4 0,26 3 A 44,9 0,17 4 0,34 3 A 44,5 0,10 4 0,30 3 A 45,1 0,13 4 0,08 3 B 44,3 0,21 4 0,24 3 A 44,5 0,10 4 0,33 3 A 45,4 0,08 4 0,20 3 B 44,9 0,06 4 0,10 3 B 45,2 0,00 4 0,12 3 A 45,2 0,09 4 0,10 3 A 44,7 0,06 4 0,08 3 A 44,3 0,27 4 0,21 3 A 45,4 0,05 4 A 44,9 0,14 4 A ph 8,81 0, ,11 3 A 8,78 0,021 2 A 8,78 0, ,10 3 A 8,79 0, ,037 3 A 8,74 0, ,091 3 A 8,87 0, ,025 3 A 8,99 0,016 4 A 8,88 0, ,038 3 A 8,93 0, ,034 3 A 8,87 0, ,012 3 A 8,92 0, ,010 3 A 8,87 0, ,010 3 A 8,93 0, ,023 3 A 8,79 0, ,071 3 A 8,72 0, ,025 3 A 8,82 0,012 4 A 8,83 0, ,090 3 A 8,86 0, ,005 3 A 254 0,58 3 5,43 3 A 241 4,27 4 1,30 3 A 246 1,83 4 1,73 3 A 246 0,58 4 1,61 3 A 242 4,57 4 0,52 3 A 246 0,61 4 2,74 2 A 253 5,00 4 A External Control Values : average for laboratory i : stanar eviation for laboratory i within an analytical series : number of results for etermination of : stanar eviation for laboratory i between analytical series : number of results for etermination of s: See explanation on page 4. Certificate QC DWB 8 Batch VKI an VKI

9 ANNEX TO CERTIFICATE QC DWB Certifying Laboratories Denmark Eurofins Miljø A/S, Vejen Lab Vest I/S, Holstebro Milana AS, Humlebæk R. Dons' Vananalytisk Laboratorium A/S, Værløse Faroe Islans Heilsufrøiliga Starvsstovan, Tórshavn Finlan FCG Finnish Consulting Group Oy, Helsinki Metropolilab Oy, Helsinki Ramboll Analytics, Lahti Water an Environment Research of South-West Finlan, Turku Norway Eurofins Norsk Miljøanalyse AS, Moss Haranger Miljøsenter AS, Oa Norges Geologiske Unersøkelse, Tronheim Vestfollab A/S, Sem Sween ALcontrol AB, Karlsta ALcontrol AB, Linköping ALS Scaninavia AB, Luleå Eurofins Environment Sween AB, Liköping Göteborg Vatten, Lackarebäcksverket, Angere Motala Kommun, Tekniska Förvaltningen Vatten, Motala Nynäshamns Kommun, VA-avelingen, Nynäshamn Tekniska Verken i Linköping AB (publ), Linköping Ålan Islans Ålans miljö och hälsoskysmynighet, Laboratoriet, Jomala Batch VKI an VKI Certificate QC DWB