DIN EN 16693-2015 Water quality - Determination of organochlorine pesticides (OCP) in whole water samples - Method using solid phase extraction (SPE) with SPE-disks combined with g.pdf

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1、December 2015 English price group 15No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 13.060.50!%Ir+“2387908www.din.d

2、eDIN EN 16693Water quality Determination of organochlorine pesticides (OCP) in whole water samples Method using solid phase extraction (SPE) with SPE-disks combined with gas chromatography-mass spectrometry (GC-MS);English version EN 16693:2015,English translation of DIN EN 16693:2015-12Wasserbescha

3、ffenheit Bestimmung von Organochlorpestiziden (OCP) in Gesamtwasserproben Verfahren mittels Festphasenextraktion (SPE) mit SPE-Disks in Verbindung mit Gaschromatographie-Massenspektrometrie (GC-MS);Englische Fassung EN 16693:2015,Englische bersetzung von DIN EN 16693:2015-12Qualit de leau Dosage des

4、 pesticides organochlors (POC) dans la totalit de lchantillon deau Mthode par extraction en phase solide (SPE) avec disques SPE, avec couplage chromatographie en phase gazeuse-spectromtrie de masse (CG-SM);Version anglaise EN 16693:2015,Traduction anglaise de DIN EN 16693:2015-12www.beuth.deDocument

5、 comprises 33 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.11.15 DIN EN 16693:2015-12 2 A comma is used as the decimal marker. National foreword This document (EN 16693:2015) has been prepared by Technical Committee CEN/TC 2

6、30 “Water analysis” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was DIN-Normenausschuss Wasserwesen (DIN Standards Committee Water Practice), Working Committee NA 119-01-03-02 UA Organische Verbindungen of NA 119-01-03 AA Wasseruntersuchung. Designation of th

7、e method: Determination of organochlorine pesticides (OCP) in whole water samples Method using solid phase extraction (SPE) with SPE-disks combined with gas chromatography-mass spectrometry (GC-MS): Method DIN EN 16693 F 51 This standard has been prepared under mandate M/424, which was given to CEN

8、by the European Commission for the development and enhancement of standard methods in support of the Water Framework Directive (WFD) (Directive 2000/60/EC). The method specified in this standard supports the requirements given in Annex X of the Water Framework Directive (WFD). The DIN Standard corre

9、sponding to the International Standard referred to in this document is as follows: ISO 5725-2 DIN ISO 5725-2 DIN EN 16693:2015-12 3 Expert assistance and specialized laboratories will be required to perform the analyses described in this standard. Existing safety requirements are to be observed. Dep

10、ending on the objective of the analysis, a check shall be made on a case-by-case basis as to whether and to what extent additional conditions will have to be specified. This standard has been prepared by the DIN-Normenausschuss Wasserwesen (DIN Standards Committee Water Practice) in collaboration wi

11、th the Wasserchemische Gesellschaft - Fachgruppe in der Gesellschaft Deutscher Chemiker (Water Chemistry Society - Division of the German Chemical Society). It is part of the series Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlammuntersuchung (German standard methods for the examination

12、 of water, waste water and sludge): Determination of organochlorine pesticides (OCP) in whole water samples Method using solid phase extraction (SPE) with SPE-disks combined with gas chromatography-mass spectrometry (GC-MS) (F 51). Standard methods published as DIN Standards are obtainable from Beut

13、h Verlag GmbH, either individually or grouped in volumes. The standard methods included in the loose-leaf publication entitled Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlammuntersuchung will continue to be published by Beuth Verlag GmbH and Wiley-VCH Verlag GmbH yigis the measured val

14、ue of the target substance i in the water sample, e.g. in area units; yIgis the measured value of internal standard I in the water sample, the unit depending on the evaluation, e.g. area unit; Igis the mass concentration of internal standard I in the water sample, in micrograms per litre (g/l); biIg

15、, miIgsee Formula (2). DIN EN 16693:2015-12 EN 16693:2015 (E) 17 11 Expression of results The mass concentration, in micrograms per litre (g/l) or nanograms per litre (ng/l), of the individual compounds listed in Table 1 shall be reported to two significant figures. EXAMPLES Alachlor 11 g/l 1,2,3-TC

16、B 1,2 g/l Hexachlorobutadiene 0,14 g/l Endrin 0,021 g/l Endosulfan-II (beta) 0,000 34 g/l Endosulfan-II (beta) 0,34 ng/l 12 Test report The test report shall contain at least the following information: a) the applied test method, with a reference to this European Standard (EN 16693); b) all informat

17、ion necessary for the complete identification of the water sample; c) sample preparation and extraction; d) expression of the results, according to Clause 11; e) any details not specified in this European Standard or which are optional, as well as any factor which may have affected the results. DIN

18、EN 16693:2015-12 EN 16693:2015 (E) 18 Annex A (informative) Suitable gas chromatographic conditions and example chromatograms GC-conditions of example chromatograms in Figure A.1 GC equipment: Agilent 6890 A1), Gerstel MPS 21)Injection: 1 l, glass-liner (straight, desactivated, with 1 notch); I.D: 1

19、,0 mm, Gerstel CIS 41), 60 C; 10 C/s to 300 C; 10 min; splitless Capillary column: Phenomenex Zebron ZB 5ms1), 30 m 0,25 mm 0,25 m Concentration: 10 ng/ml Carrier gas: helium (5.0); 0,9 ml/min Temperature programme: 65 C; 10 C/min to 300 C; 10 min MS detector: Agilent 5973 C MSD1), quadrupole-MS, EI

20、, 70 eV, SIM 1) Agilent 6890 A, Gerstel MPS 2, Gerstel CIS 4 Phenomenex Zebron ZB 5ms and Agilent 5973 C MSD are examples of suitable products which are commercially available. These examples are given only as information for the users of this European Standard and do not constitute an endorsement b

21、y CEN of these products. DIN EN 16693:2015-12 EN 16693:2015 (E) 19 a) ion 180 b) ion 225 c) ion 250 d) ion 183 e) ion 284 DIN EN 16693:2015-12 EN 16693:2015 (E) 20 f) ion 160 g) ion 265 h) ion 193 i) ion 195 j) ion 246 DIN EN 16693:2015-12 EN 16693:2015 (E) 21 k) ion 263 l) ion 235 m) ion 185 n) ion

22、 231 o) ion 290 DIN EN 16693:2015-12 EN 16693:2015 (E) 22 p) ion 200 q) ion 237 r) ion 247 Key t Time in minutes (min) Y Abundance, signal intensity 1 1,3,5-TCB 15 pp-DDE 2 1,2,4-TCB 16 Dieldrin 3 1,2,3-TCB 17 Endrin 4 Hexachlorobutadiene (HCBD) 18 Endosulfan-II (beta) 5 Pentachlorobenzene 19 pp-DDD

23、 6 alpha-HCH 20 op-DDT 7 Hexachlorobenzene (HCB) 21 pp-DDT 8 beta-HCH IS 1 1,2,4-TCB (d3) 9 gamma-HCH IS 2 HCBD (13C3) 10 delta-HCH IS 3 HCB (13C6) 11 Alachlor IS 4 Alachlor (d13) 12 Aldrin IS 5 Endosulfan-I (alpha) (d4) 13 Isodrin IS 6 pp-DDT (13C12) 14 Endosulfan-I (alpha) Figure A.1 Example gas c

24、hromatograms of OCP DIN EN 16693:2015-12 EN 16693:2015 (E) 23 Annex B (informative) Repeatability and reproducibility data The performance data on repeatability and reproducibility given in Tables B.1, B.2 and B.3 were determined in a European interlaboratory trial for validation carried out in June

25、 2014 on surface water. The water used was taken from an urban and industrialized area (river Ruhr in Muelheim, Germany). Three samples (sample 1, 2 and 3, see Tables B.1, B.2 and B.3) were spiked with OCP listed in Table 1. Sample 2 and 3 were additionally spiked with different amounts of suspended

26、 particulate matter (SPM). The SPM used was an OCP-containing certified reference material (CRM). Evaluation according to ISO 5725-2. DIN EN 16693:2015-12 EN 16693:2015 (E) 24 Table B.1 Performance data for OCP spiked surface water, sample 1 Compound l n o X x sR CV,R sr CV,r % g/l g/l % g/l % g/l %

27、 Alachlor 8 16 11,1 0,162 5 0,138 1 85,0 0,027 6 20,0 0,014 0 10,1 Aldrin 10 20 0,0 0,015 0 0,012 6 83,7 0,002 6 21,1 0,001 0 7,9 Dieldrin 12 23 0,0 0,020 0 0,021 3 106,3 0,006 4 30,1 0,001 8 8,5 Endrin 10 20 9,1 0,020 0 0,019 9 99,3 0,006 5 33,0 0,001 0 5,2 Isodrin 8 16 11,1 0,020 0 0,016 6 83,1 0,

28、003 8 23,0 0,000 8 4,8 op-DDT 12 24 0,0 0,036 0 0,038 9 108,0 0,016 6 42,7 0,003 4 8,7 pp-DDT 12 24 0,0 0,022 7 0,026 5 116,6 0,009 8 37,2 0,002 1 7,8 pp-DDD 10 20 16,7 0,036 1 0,036 5 101,1 0,011 8 32,4 0,003 0 8,4 pp-DDE 11 22 8,3 0,045 0 0,039 1 86,9 0,012 3 31,5 0,002 4 6,2 Hexachlorobenzene (HC

29、B) 10 20 0,0 0,024 0 0,020 7 86,0 0,007 7 37,3 0,001 5 7,4 Hexachlorobutadiene (HCBD) 9 18 0,0 0,113 4 0,070 6 62,3 0,019 5 27,6 0,005 6 7,9 alpha-HCH 11 22 8,3 0,029 9 0,024 6 82,2 0,010 4 42,3 0,001 6 6,4 beta-HCH 12 24 0,0 0,030 3 0,028 8 94,9 0,012 1 42,2 0,002 0 7,1 delta-HCH 11 22 0,0 0,037 4

30、0,039 1 104,6 0,010 9 27,9 0,001 8 4,7 gamma-HCH 12 23 0,0 0,029 9 0,026 6 89,0 0,013 9 52,2 0,002 2 8,4 Pentachlorobenzene 9 18 0,0 0,015 1 0,015 6 103,0 0,009 5 60,8 0,002 8 18,1 1,2,3-TCB 7 14 12,5 0,324 7 0,249 1 76,7 0,069 5 27,9 0,007 2 2,9 1,2,4-TCB 7 14 12,5 0,257 3 0,223 9 87,0 0,058 7 26,2

31、 0,010 9 4,9 1,3,5-TCB 8 16 11,1 0,270 0 0,210 9 78,1 0,053 2 25,2 0,008 8 4,2 Endosulfan-I (alpha) 10 20 0,0 0,013 1 0,011 8 89,7 0,003 9 33,5 0,001 9 15,8 Endosulfan-II (beta) 10 20 0,0 0,013 2 0,010 2 77,3 0,003 6 35,1 0,000 9 9,3 l number of laboratories after outlier rejection n number of indiv

32、idual test results after outlier rejection o percentage of outliers X assigned value xoverall mean of results (without outliers) recovery rate sR reproducibility standard deviation CV,R coefficient of variation of reproducibility sr repeatability standard deviation CV,r coefficient of variation of r

33、epeatability DIN EN 16693:2015-12 EN 16693:2015 (E) 25 Table B.2 Performance data for OCP spiked surface water, additionally spiked with 20 mg/l of suspended particulate matter (SPM), sample 2 Compound l n o X x sR CV,R sr CV,r % g/l g/l % g/l % g/l % Alachlor 8 16 11,1 0,325 1 0,266 3 81,9 0,047 0

34、17,6 0,022 0 8,3 Aldrin 9 18 10,0 0,020 3 0,017 3 85,1 0,004 6 26,4 0,002 3 13,6 Dieldrin 10 20 16,7 0,026 5 0,027 9 105,3 0,003 8 13,6 0,002 1 7,6 Endrin 11 22 0,0 0,027 5 0,032 0 116,2 0,008 4 26,4 0,003 9 12,1 Isodrin 10 20 0,0 0,030 0 0,024 8 82,5 0,012 0 48,3 0,002 8 11,3 op-DDT 11 22 8,3 0,054

35、 0 0,045 5 84,2 0,010 8 23,8 0,005 2 11,4 pp-DDT 11 22 8,3 0,030 6 0,030 6 100,0 0,009 3 30,3 0,004 5 14,8 pp-DDD 10 20 16,7 0,049 7 0,045 8 92,2 0,014 0 30,5 0,003 4 7,4 pp-DDE 12 24 0,0 0,058 4 0,053 0 90,8 0,016 6 31,2 0,003 7 7,0 Hexachlorobenzene (HCB) 10 20 0,0 0,030 0 0,024 9 82,8 0,007 4 29,

36、7 0,001 6 6,4 Hexachlorobutadiene (HCBD) 9 18 0,0 0,170 1 0,093 8 55,1 0,030 9 33,0 0,010 3 11,0 alpha-HCH 11 22 8,3 0,049 3 0,042 4 85,9 0,016 5 38,9 0,002 4 5,7 beta-HCH 12 24 0,0 0,052 3 0,054 3 103,9 0,025 4 46,7 0,007 1 13,2 delta-HCH 11 22 0,0 0,061 2 0,063 3 103,4 0,021 7 34,4 0,009 8 15,6 ga

37、mma-HCH 12 24 0,0 0,051 6 0,046 3 89,6 0,018 7 40,4 0,003 7 7,9 Pentachlorobenzene 8 16 11,1 0,018 9 0,014 9 79,0 0,005 2 35,1 0,001 3 8,4 1,2,3-TCB 8 16 0,0 0,405 9 0,292 1 72,0 0,130 4 44,6 0,074 0 25,3 1,2,4-TCB 8 16 0,0 0,385 9 0,332 4 86,1 0,088 0 26,5 0,061 0 18,4 1,3,5-TCB 9 18 0,0 0,324 0 0,

38、276 8 85,4 0,109 5 39,6 0,072 2 26,1 Endosulfan-I (alpha) 10 20 0,0 0,013 9 0,013 7 98,6 0,004 7 34,6 0,002 0 14,8 Endosulfan-II (beta) 10 20 0,0 0,015 0 0,013 4 89,3 0,004 5 33,8 0,001 2 9,1 For explanation of symbols see Table B.1. DIN EN 16693:2015-12 EN 16693:2015 (E) 26 Table B.3 Performance da

39、ta for OCP spiked surface water, additionally spiked with 200 mg/l of suspended particulate matter (SPM), sample 3 Compound l n o X x sR CV,R sr CV,r % g/l g/l % g/l % g/l % Alachlor 7 14 22,2 0,433 4 0,365 2 84,3 0,072 9 19,9 0,024 0 6,6 Aldrin 11 22 0,0 0,185 0 0,151 1 81,7 0,032 6 21,6 0,011 4 7,

40、5 Dieldrin 12 24 0,0 0,125 0 0,132 3 105,8 0,044 2 33,4 0,009 0 6,8 Endrin 11 22 8,3 0,183 4 0,183 0 99,8 0,076 2 41,7 0,012 1 6,6 Isodrin 10 20 0,0 0,180 0 0,147 8 82,1 0,041 7 28,2 0,012 7 8,6 op-DDT 9 18 25,0 0,240 0 0,196 8 82,0 0,070 5 35,8 0,008 3 4,2 pp-DDT 11 22 8,3 0,161 2 0,171 5 106,4 0,0

41、66 3 38,7 0,013 9 8,1 pp-DDD 10 20 16,7 0,340 6 0,302 8 88,9 0,103 5 34,2 0,021 2 7,0 pp-DDE 11 22 8,3 0,205 6 0,206 9 100,6 0,058 5 28,3 0,013 8 6,7 Hexachlorobenzene (HCB) 10 20 0,0 0,108 0 0,090 6 83,9 0,021 9 24,2 0,007 0 7,7 Hexachlorobutadiene (HCBD) 9 18 0,0 0,396 9 0,218 1 55,0 0,092 9 42,6

42、0,008 6 4,0 alpha-HCH 10 20 16,7 0,224 3 0,175 1 78,0 0,068 6 39,2 0,010 2 5,8 beta-HCH 10 20 16,7 0,216 4 0,194 6 89,9 0,073 0 37,5 0,011 6 5,9 delta-HCH 10 20 9,1 0,252 7 0,218 5 86,5 0,061 4 28,1 0,018 1 8,3 gamma-HCH 11 22 8,3 0,227 4 0,195 7 86,1 0,064 7 33,1 0,006 3 3,2 Pentachlorobenzene 8 16

43、 11,1 0,090 6 0,074 9 82,7 0,016 7 22,3 0,005 6 7,4 1,2,3-TCB 7 14 12,5 0,487 1 0,361 4 74,2 0,129 5 35,8 0,024 5 6,8 1,2,4-TCB 7 14 12,5 0,506 5 0,375 4 74,1 0,135 7 36,1 0,019 0 5,1 1,3,5-TCB 8 16 11,1 0,486 0 0,351 8 72,4 0,159 8 45,4 0,012 7 3,6 Endosulfan-I (alpha) 11 22 0,0 0,087 1 0,081 4 93,4 0,030 4 37,4 0,007 4 9,1 Endosulfan-II (beta) 10 20 9,1 0,062 1 0,062 3 100,3 0,038 1 61,2 0,005 4 8,7 For explanation of symbols see Table B.1. DIN EN 16693:2015-12