DIN ISO 15923-1-2014 Water quality - Determination of selected parameters by discrete analysis systems - Part 1 Ammonium nitrate nitrite chloride orthophosphate sulfate and silicat.pdf

1、July 2014 Translation by DIN-Sprachendienst.English price group 14No 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 1

2、3.060.50!%7B#“2203100www.din.deDDIN ISO 15923-1Water quality Determination of selected parameters by discrete analysis systems Part 1: Ammonium, nitrate, nitrite, chloride, orthophosphate, sulfate andsilicate with photometric detection (ISO 15923-1:2013),English translation of DIN ISO 15923-1:2014-0

3、7Wasserbeschaffenheit Bestimmung von ausgewhlten Parametern mittels Einzelanalysensystemen Teil 1: Ammonium, Nitrat, Nitrit, Chlorid, Orthophosphat, Sulfat und Silikat durchphotometrische Detektion (ISO 15923-1:2013),Englische bersetzung von DIN ISO 15923-1:2014-07Qualit de leau Dtermination de para

4、mtres slectionns par des systmes danalyse discrte Partie 1: Ammonium, nitrate, nitrite, chlorure, orthophosphate, sulfate et silicate pardtection photomtrique (ISO 15923-1:2013),Traduction anglaise de DIN ISO 15923-1:2014-07www.beuth.deDocument comprises 33 pagesIn case of doubt, the German-language

5、 original shall be considered authoritative.07.14 A comma is used as the decimal marker. Contents Page National foreword .4 National Annex NA (informative) Bibliography 7 Introduction .8 1 Scope 9 2 Normative references 9 3 Principle 9 4 Interferences 10 5 Reagents .10 6 Apparatus .10 7 Sampling and

6、 sample preparation .10 8 Calibration 11 8.1 Calibration function .11 8.2 Calibration validity check .11 9 Procedure .11 10 Calculation 12 11 Expression of results 12 12 Test report 13 Annex A (normative) Correction for inherent colour .14 A.1 General 14 A.2 Sample blanking 14 A.3 Use of a compensat

7、ing solution 14 Annex B (normative) Determination of ammonium .15 B.1 Principle 15 B.2 Interferences 15 B.3 Reagents .15 B.4 Procedure .16 Annex C (normative) Determination of the sum of nitrate and nitrite by the hydrazine method 17 C.1 Principle 17 C.2 Interference 17 C.3 Reagents .17 C.4 Procedur

8、e .18 Annex D (normative) Determination of nitrite 20 D.1 Principle 20 D.2 Interference 20 D.3 Reagents .20 D.4 Procedure .21 Annex E (normative) Determination of chloride by the thiocyanate method 22 E.1 Principle 22 E.2 Interference 22 E.3 Reagents .22 E.4 Procedure .23 DIN ISO 15923-1:2014-07 2 A

9、nnex F (normative) Determination of orthophosphate . 24 F.1 Principle . 24 F.2 Interference 24 F.3 Reagents 24 F.4 Procedure . 25 Annex G (normative) Determination of sulfate by the turbidimetric method . 27 G.1 Principle . 27 G.2 Interference 27 G.3 Reagents 27 G.4 Procedure . 27 Annex H (normative

10、) Determination of silicate 29 H.1 Principle . 29 H.2 Interference 29 H.3 Reagents 29 H.4 Procedure . 30 Annex I (informative) Performance data . 31 Bibliography 33 DIN ISO 15923-1:2014-07 3 National foreword This document (ISO 15923-1:2013) has been prepared by Technical Committee ISO/TC 147 “Water

11、 quality” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Committee), Working Committee NA 119-01-03-01-23 AK Einzelanalysensysteme of NA 119-01-03 AA Wasseruntersuchung. Attention is drawn to the poss

12、ibility that some of the elements of this document may be the subject of patent rights. DIN and/or DKE shall not be held responsible for identifying any or all such patent rights. Designation of the method: Determination of selected parameters by discrete analysis systems Part 1: Ammonium, nitrate,

13、nitrite, chloride, orthophosphate, sulfate and silicate with photometric detection (D 49): Method DIN ISO 15923-1 D 49 As a result of national implementation in Germany, the following action has been taken: ISO 15923-1:2013 has been taken over as DIN ISO 15923-1 without any modifications. Editorial

14、remarks concerning ISO 17155:2012: Re Clause 5: Commercially available and ready-made reagents may be used, provided their composition and properties meet the requirements of the International Standard. The conversion factors for ammonia given in Clause 11, Table 1, are incorrect. The correct factor

15、s are given below: Table 1 Conversion factors Parameter Units Conversion factor Converted units Ammonia mg/l N 1,287 8 mg/l NH4Ammonia mg/l NH40,776 5 mg/l N Re C.3.3: Further experience has shown that this solution needs to be made fresh every day. DIN ISO 15923-1:2014-07 4 The DIN Standards corres

16、ponding to the International Standards referred to in this document are as follows: ISO 3696 DIN ISO 3696 ISO 5663 DIN EN 25663 ISO 5667-3 DIN EN ISO 5667-3 ISO 5725-2 DIN ISO 5725-2 ISO 6777 DIN EN 26777 ISO 6878 DIN EN ISO 6878 ISO 8466-1 DIN 38402-51 ISO 8466-2 DIN ISO 8466-2 ISO 13395 DIN EN ISO

17、 13395 ISO 15682 DIN EN ISO 15682 DIN ISO 15923-1:2014-07 5 DIN ISO 15923-1:2014-07 6 Expert assistance and specialized laboratories will be required to perform the analyses described in this standard. Existing safety requirements are to be observed. Depending on the objective of the analysis, a che

18、ck 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 Normenausschuss Wasserwesen (Water Practice Standards Committee) in collaboration with the Wasserchemische Gesellschaft Fachgruppe in der

19、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 of water, waste water and sludge): Determination of selec

20、ted parameters by discrete analysis systems Part 1: Ammonium, nitrate, nitrite, chloride, orthophosphate, sulfate and silicate with photometric detection (D 49): Standard methods published as DIN Standards are obtainable from Beuth Verlag GmbH, either individually or grouped in volumes. The standard

21、 methods included in the loose-leaf publication entitled Deutsche Einheits-verfahren zur Wasser-, Abwasser- und Schlammuntersuchung will continue to be published by Beuth Verlag GmbH and Wiley-VCH Verlag GmbH general information (group A) Calibration of analytical methods, evaluation of analytical r

22、esults and linear calibration functions used to determine the performance characteristics of analytical methods (A 51) DIN EN 25663, Water quality Determination of Kjeldahl nitrogen Method after mineralization with selenium DIN EN 26777, Water quality Determination of nitrite Molecular absorption sp

23、ectrometric method DIN EN ISO 6878, Water quality Determination of phosphorus Ammonium molybdate spectrometric method DIN EN ISO 5667-3, Water quality Sampling Part 3: Preservation and handling of water samples DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN ISO

24、5725-2, 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 DIN ISO 8466-2, Water quality Calibration and evaluation of analytical methods and estimation of performance c

25、haracteristics Part 2: Calibration strategy for non-linear second-order calibration functions DIN EN ISO 13395, Water quality Determination of nitrite nitrogen and nitrate nitrogen and the sum of both by flow analysis (CFA and FIA) and spectrometric detection DIN EN ISO 15682, Water quality Determin

26、ation of chloride by flow analysis (CFA and FIA) and photometric or potentiometric detection DIN ISO 15923-1:2014-07 7 IntroductionMany photometric determinations can be automated with a discrete analysis system. With one single apparatus, a large number of different parameters can be determined, an

27、d the parameters to be determined can be specified for each sample. Working with small volumes requires less sample material and reagent.Samples that fall beyond the normal measuring range can either be automatically diluted or measured again with a different measuring range.This part of ISO 15923 s

28、pecifies methods for the automatic determination of ammonium, nitrate, nitrite, chloride, orthophosphate, and silicate with photometric detection and a turbidimetric determination of sulfate using a discrete analysis system. The field of application is water (ground, potable, surface, waste, eluates

29、, and boiler water).Water quality Determination of selected parameters by discrete analysis systems Part 1: Ammonium, nitrate, nitrite, chloride, orthophosphate, sulfate and silicate with photometric detection DIN ISO 15923-1:2014-07 8 WARNING Persons using this part of ISO 15923 should be familiar

30、with normal laboratory practice. This part of ISO 15923 does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.

31、 IMPORTANT It is absolutely essential that tests conducted in accordance with this part of ISO 15923 be carried out by suitably qualified staff.1 ScopeThis part of ISO 15923 specifies methods for the automatic performance of spectrophotometric and turbidimetric analyses with a discrete analysis syst

32、em for determining ammonium, nitrate, nitrite, chloride, orthophosphate, sulfate, and silicate. The field of application is ground, potable, surface, waste, eluates, and boiler water.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and a

33、re indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 3696, Water for analytical laboratory use Specification and test methodsISO 5667-3, Water quality S

34、ampling Part 3: Preservation and handling of water samplesISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical evaluation of the linear calibration functionISO 8466-2, Water quality Calibration and evaluation of

35、analytical methods and estimation of performance characteristics Part 2: Calibration strategy for non-linear second-order calibration functions3 PrincipleA discrete analysis system is an automated system for spectrophotometric and turbidimetric determinations.The colour reactions take place in react

36、ion cells, which may be cuvettes, in an incubator. For each determination, a separate reaction cell is used. Preset volumes of the sample and the reagents are pipetted into the cells and mixed.After expiry of the incubation period, the absorbance of the solution is measured at the wavelength applica

37、ble to the determination. This is done by passing the cuvettes through the photometer or by transferring the measuring solution from the reaction cells to a photometer with a flow-through cell.DIN ISO 15923-1:2014-07 9 4 InterferencesParticles present in the sample can lead to blockages and will int

38、erfere with the photometric measurement. Filtration of all samples through a 0,45 m membrane filter is recommended, except for the determination of total phosphate and Kjeldahl nitrogen digests (see Annexes B and F). Particles can also be removed by settlement, centrifugation, or dialysis.This metho

39、d is applicable to samples in a pH range from 5 to 9, which covers most natural waters. Samples outside this range may require pH correction.Inherent colour or turbidity of the sample interferes with the analysis. On the prevention of such interference, see Annex A. Interferences specific to each pa

40、rameter are discussed in Annexes B to H.NOTE Interference by inherent colour shall be compensated by measuring the absorbance of the sample before the addition of the chromogenic reagent (sample blanking) or by making use of a compensating solution (measuring solution without a chromogenic compound)

41、. For further details, see Annex A. A safe procedure for the correction of turbidity cannot really be given. The Lambert-Beer law does not apply to turbid solutions. Furthermore, many chromogenic reagents and coloured complexes are adsorbed on particles.5 ReagentsReagents for each parameter are spec

42、ified in Annexes B to H. Use only reagents of recognized analytical grade, unless otherwise specified in the relevant annex. Dry all solid reagents for at least 1 h at (105 5) C, provided that they are thermally stable. Store the dried solid in a desiccator before weighing. Reagent volumes specified

43、 in Annexes B to H may be adjusted to suit local requirements or different instrument specifications.5.1 Water, complying with grade 1 as defined in ISO 3696.6 Apparatus6.1 Discrete analysis system, generally consisting of the following components:6.1.1 Sample injection device, for automated or manu

44、al operation.6.1.2 Sample container.6.1.3 Reagent container, refrigerated or not.6.1.4 Incubator with temperature control, capable of maintaining a constant temperature of e.g. 37 C.6.1.5 UV/VIS detector, e.g. spectrophotometer, suitable for a wavelength range usually between 340 nm and 880 nm.6.1.6

45、 Control and data processing unit.6.1.7 Recording device, e.g. PC with software for data acquisition and evaluation.7 Sampling and sample preparationUse clean vessels for sampling.Turbidity or particulates interfere with spectrophotometric detection. Clarify samples by filtration through a 0,45 m me

46、mbrane (settlement, centrifugation, or dialysis may also be used). To avoid DIN ISO 15923-1:2014-07 10 contamination by the filter membrane, discard the first 20 ml to 30 ml of filtrate. Samples for the determination of total phosphate should not be filtered. Refer to Annex F.Prepare and store the s

47、ample in accordance with Annexes B to H or with ISO 5667-3 if no specific guidance is given in the relevant annex.Prepare a sample of water (5.1) in the same way as the sample, to be used as a blank.Prepare a control standard solution from the primary control standard containing a level of analyte s

48、imilar to the samples. Run as a sample at appropriate intervals in the batch, according to local requirements. A minimum interval of once every 20 samples is recommended.8 Calibration8.1 Calibration functionWhen the analytical system is first evaluated and at intervals afterwards, establish a calibration function for each parameter (see ISO 8466-1 or ISO 8466-2) as follows:Using the primary calibration standard, prepare an appropriate series of calibration solutions for the respecti