BS ISO 15923-1-2013 Water quality Determination of selected parameters by discrete analysis systems Ammonium nitrate nitrite chloride orthophosphate sulfate and silicate with photo.pdf

1、BSI Standards PublicationBS ISO 15923-1:2013Water quality Determinationof selected parameters bydiscrete analysis systemsPart 1: Ammonium, nitrate, nitrite, chloride,orthophosphate, sulfate and silicate withphotometric detectionBS ISO 15923-1:2013 BRITISH STANDARDNational forewordThis British Standa

2、rd is the UK implementation of ISO 15923-1:2013.The UK participation in its preparation was entrusted to TechnicalCommittee EH/3/2, Physical chemical and biochemical methods.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not pur

3、port to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2013. Published by BSI StandardsLimited 2013ISBN 978 0 580 70683 7ICS 13.060.50Compliance with a British Standard cannot confer immunity fromlegal obligation

4、s.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 December 2013.Amendments issued since publicationDate Text affectedBS ISO 15923-1:2013 ISO 2013Water quality Determination of selected parameters by discrete analysis systems Part 1: Ammoniu

5、m, nitrate, nitrite, chloride, orthophosphate, sulfate and silicate with photometric detectionQualit de leau Dtermination de paramtres slectionns par des systmes danalyse discrte Partie 1: Ammonium, nitrate, nitrite, chlorure, orthophosphate, sulfate et silicate par dtection photomtriqueINTERNATIONA

6、L STANDARDISO15923-1First edition2013-12-15Reference numberISO 15923-1:2013(E)BS ISO 15923-1:2013ISO 15923-1:2013(E)ii ISO 2013 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2013All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise

7、 in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase p

8、ostale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 15923-1:2013ISO 15923-1:2013(E) ISO 2013 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Principle 14 Interfere

9、nces 25 Reagents 26 Apparatus . 27 Sampling and sample preparation 28 Calibration 38.1 Calibration function 38.2 Calibration validity check 39 Procedure. 310 Calculation 411 Expression of results 412 Test report . 4Annex A (normative) Correction for inherent colour . 6Annex B (normative) Determinati

10、on of ammonium 7Annex C (normative) Determination of the sum of nitrate and nitrite by the hydrazine method 9Annex D (normative) Determination of nitrite .12Annex E (normative) Determination of chloride by the thiocyanate method 14Annex F (normative) Determination of orthophosphate .16Annex G (norma

11、tive) Determination of sulfate by the turbidimetric method .19Annex H (normative) Determination of silicate 21Annex I (informative) Performance data 23Bibliography .25BS ISO 15923-1:2013ISO 15923-1:2013(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of n

12、ational standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. Inter

13、national organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those inte

14、nded for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2. www.iso

15、.org/directivesAttention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be

16、 in the Introduction and/or on the ISO list of patent declarations received. www.iso.org/patentsAny trade name used in this document is information given for the convenience of users and does not constitute an endorsement.The committee responsible for this document is ISO/TC 147, Water quality, Subc

17、ommittee SC 2, Physical, chemical and biochemical methods.ISO 15923 consists of the following parts, under the general title Water quality Determination of selected parameters by discrete analysis systems: Part 1: Ammonium, nitrate, nitrite, chloride, orthophosphate, sulfate and silicate with photom

18、etric detectioniv ISO 2013 All rights reservedBS ISO 15923-1:2013ISO 15923-1:2013(E)IntroductionMany photometric determinations can be automated with a discrete analysis system. With one single apparatus, a large number of different parameters can be determined, and the parameters to be determined c

19、an 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 specifies methods for the automatic

20、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, and boiler water). ISO 2013 All r

21、ights reserved vBS ISO 15923-1:2013BS ISO 15923-1:2013Water quality Determination of selected parameters by discrete analysis systems Part 1: Ammonium, nitrate, nitrite, chloride, orthophosphate, sulfate and silicate with photometric detectionWARNING Persons using this part of ISO 15923 should be fa

22、miliar 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 cond

23、itions. 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 analys

24、is system 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 documen

25、t and are 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 qu

26、ality Sampling 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 evaluat

27、ion of 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 i

28、n reaction 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

29、applicable 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.INTERNATIONAL STANDARD ISO 15923-1:2013(E) ISO 2013 All rights reserved 1BS ISO 15923-1:2013ISO 1592

30、3-1:2013(E)4 InterferencesParticles present in the sample can lead to blockages and will interfere 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

31、 and F). Particles can also be removed by settlement, centrifugation, or dialysis.This method 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 anal

32、ysis. On the prevention of such interference, see Annex A. Interferences specific to each parameter 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

33、by making use of a compensating solution (measuring solution without a chromogenic compound). 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

34、 coloured complexes are adsorbed on particles.5 ReagentsReagents for each parameter are specified 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 therma

35、lly stable. Store the dried solid in a desiccator before weighing. Reagent volumes specified 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

36、 consisting of the following components:6.1.1 Sample injection device, for automated or manual 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

37、. spectrophotometer, suitable for a wavelength range usually between 340 nm and 880 nm.6.1.6 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 in

38、terfere with spectrophotometric detection. Clarify samples by filtration through a 0,45 m membrane (settlement, centrifugation, or dialysis may also be used). To avoid 2 ISO 2013 All rights reservedBS ISO 15923-1:2013ISO 15923-1:2013(E)contamination by the filter membrane, discard the first 20 ml to

39、 30 ml of filtrate. Samples for the determination of total phosphate should not be filtered. Refer to Annex F.Prepare and store the sample 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 th

40、e sample, to be used as a blank.Prepare a control standard solution from the primary control standard containing a level of analyte similar 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 recommend

41、ed.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 soluti

42、ons for the respective parameter as described in Annexes B to H, including a zero-concentration solution.Analyse the calibration solutions according to Clause 9 and the instrument manufacturers instructions.Confirm the validity of the data obtained and use to calculate the regression line as specifi

43、ed in ISO 8466-1 or ISO 8466-2.Verify the continuing validity of the established calibration function by analysing an appropriate calibration standard solution, at regular intervals according to the accuracy requirements or at least at the end of the batch.Recalibrate if necessary.8.2 Calibration va

44、lidity checkIf the full calibration function is not established daily, carry out an initial calibration validity check by analysing two calibration standard solutions in the lower and upper third of the calibrated working range after the setup procedure (see Clause 9).Verify the continuing validity

45、of the established calibration function by analysing an appropriate calibration standard solution at regular intervals according to the accuracy requirements or at least at the end of the batch.Recalibrate if necessary.9 ProcedureSet up the discrete analysis system according to the instrument manufa

46、cturers instructions.Calibrate the system according to Clause 8 and the instrument manufacturers instructions.Prepare the samples according to Clause 7 and Annexes B to H. A consistent incubation temperature and time are essential for the stability of the absorbance measurements. For guidance on rec

47、ommended incubation temperatures and times, refer to Annexes B to H. Note that the incubation times given in Annexes B to H are recommendations, which may be varied according to experience.Measure the absorbance of the samples using the conditions in Annexes B to H and the instrument manufacturers i

48、nstructions. Measure the blank according to Annex A and the instrument manufacturers instructions. ISO 2013 All rights reserved 3BS ISO 15923-1:2013ISO 15923-1:2013(E)If the absorbance of the sample exceeds that of the top calibration solution, dilute the sample, or reduce the sample intake by an ap

49、propriate factor to bring it into the upper half of the calibration range, and reanalyse. If necessary, blank correct the sample absorbances (see Annex A).The procedures in Annexes B to H may be modified for different instruments or to change the range or sensitivity of the method for different parameter concentrations or sample types.10 CalculationCalculate the mass concentration, , of the parameter in question in micrograms per litre (g/l) or milligrams per litre (mg/l) from the calibration line (see Claus