1、PD ISO/TS 17951-1:2016 Water quality Determination of fluoride using flow analysis (FIA and CFA) Part 1: Method using flow injection analysis (FIA) and spectrometric detection after off- line distillation BSI Standards Publication WB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06PD ISO/TS 179
2、51-1:2016 PUBLISHED DOCUMENT National foreword This Published Document is the UK implementation of ISO/TS 17951-1:2016. The UK participation in its preparation was entrusted to Technical Committee EH/3/2, Physical chemical and biochemical methods. A list of organizations represented on this committe
3、e can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2016. Published by BSI Standards Limited 2016 ISBN 978 0 580 94113 9 ICS 13.060
4、.50 Compliance with a British Standard cannot confer immunity from legal obligations. This Published Document was published under the authority of the Standards Policy and Strategy Committee on 30 September 2016. Amendments issued since publication Date Text affectedPD ISO/TS 17951-1:2016 ISO 2016 W
5、ater quality Determination of fluoride using flow analysis (FIA and CFA) Part 1: Method using flow injection analysis (FIA) and spectrometric detection after off-line distillation Qualit de leau Dosage des fluorures par analyse en flux (FIA et CFA) Partie 1: Mthode par analyse avec injection en flux
6、 (FIA) et dtection spectromtrique TECHNICAL SPECIFICATION ISO/TS 17951-1 Reference number ISO/TS 17951-1:2016(E) First edition 2016-07-01PD ISO/TS 17951-1:2016ISO/TS 17951-1:2016(E)ii ISO 2016 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2016, Published in Switzerland All rights reserved. Un
7、less otherwise specified, no part of this publication may be reproduced or utilized otherwise 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
8、 address below or ISOs member body in the country of the requester. ISO copyright office Ch. de Blandonnet 8 CP 401 CH-1214 Vernier, Geneva, Switzerland Tel. +41 22 749 01 11 Fax +41 22 749 09 47 copyrightiso.org www.iso.orgPD ISO/TS 17951-1:2016ISO/TS 17951-1:2016(E)Foreword iv Introduction v 1 Sco
9、pe . 1 2 Normative references 1 3 Principle 1 4 Interferences 2 5 Reagents 2 6 Apparatus . 4 7 Sampling and sample preparation 4 8 Procedure. 5 8.1 Distillation . 5 8.2 Setting up the system 5 8.3 Reagent blank measurement 5 8.4 Adjustment of sensitivity . 5 8.5 Confirmation of repeatability . 5 8.6
10、 Calibration 5 8.7 Measurement of samples . 6 9 Calculation 6 10 Expression of results 6 11 Test report . 7 Annex A (informative) Example of flow injection analysis (FIA) system 8 Annex B (informative) Example of a distillation apparatus and procedure 9 Annex C (informative) Results of the interlabo
11、ratory trial 11 Bibliography .12 ISO 2016 All rights reserved iii Contents PagePD ISO/TS 17951-1:2016ISO/TS 17951-1:2016(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Internationa
12、l 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. International organizations, governmental and non-governmental, in liaison with ISO,
13、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 intended for its further maintenance are described in the ISO/IEC Directives, Part
14、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 (see www.iso.org/directives). Attention is drawn to the possibility that some of the el
15、ements 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 in the Introduction and/or on the ISO list of patent declarations recei
16、ved (see www.iso.org/patents). Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement. For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs ad
17、herence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information The committee responsible for this document is ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods. ISO 17951 consists of the follow
18、ing parts, under the general title Water quality Determination of fluoride using flow analysis (FIA and CFA): Part 1: Method using flow injection analysis (FIA) and spectrometric detection after off-line distillation Technical Specification Part 2: Method using continuous flow analysis (CFA) with au
19、tomated in-line distillation Technical Specificationiv ISO 2016 All rights reservedPD ISO/TS 17951-1:2016ISO/TS 17951-1:2016(E) Introduction Fluorine compounds in waters and effluents exist in various chemical forms, such as fluoride ion, complexes of iron, aluminium, boron and etc., as well as inso
20、luble forms, such as calcium and magnesium fluorides. Excess fluoride can cause bone damage and fluorosis. The manual steam distillation method can be troublesome because of its complexity. It is necessary to ensure conversion of any insoluble fluorides into soluble fluoride for measurement. Flow an
21、alysis with colourimetric detection is a rapid cost-effective method of determining of soluble (dissolved) fluoride in the method distillate. This part of ISO 17951 describes FIA methods for flow analysis of fluoride. ISO 2016 All rights reserved vPD ISO/TS 17951-1:2016PD ISO/TS 17951-1:2016Water qu
22、ality Determination of fluoride using flow analysis (FIA and CFA) Part 1: Method using flow injection analysis (FIA) and spectrometric detection after off-line distillation WARNING Persons using this part of ISO 17951 should be familiar with normal laboratory practice. This part of ISO 17951 does no
23、t 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. IMPORTANT It is absolutely essential that tests conducted in a
24、ccordance with this part of ISO 17951 be carried out by suitably qualified staff. 1 Scope This part of ISO 17951 specifies a method for the determination of fluoride in waters, waste waters and effluents by flow injection analysis (FIA). Any insoluble or complexed fluoride is converted to fluoride i
25、on by a manual distillation procedure from sulfuric/phosphoric acid. Fluoride ion in the distillate is measured using flow analysis with lanthanum alizarin complexone and spectrometric detection. This method is applicable to industrial waste waters, effluents, surface waters, ground waters, leachate
26、s. It is not recommended for drinking waters where a distillation step is not required. In this part of ISO 17951, two working ranges are described: working range I: 0,1 mg/l to 1 mg/l; working range II: 1 mg/l to 10 mg/l. The specification of the calibration solutions are to be adapted accordingly.
27、 2 Normative references The following documents, in whole or in part, are normatively referenced in this document 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 amen
28、dments) applies. ISO 3696, Water for analytical laboratory use Specification and test methods ISO 6353-2, Reagents for chemical analysis Part 2: Specifications First series ISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1
29、: Statistical evaluation of the linear calibration function ISO 8466-2, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 2: Calibration strategy for non-linear second-order calibration functions 3 Principle Prior to the introduction of
30、 sample solution into the FIA system, the sample solution is manually distilled (see Annex B). Then, the distillate is introduced into a continuous carrier stream (water) TECHNICAL SPECIFICATION ISO/TS 17951-1:2016(E) ISO 2016 All rights reserved 1PD ISO/TS 17951-1:2016ISO/TS 17951-1:2016(E) by mean
31、s of injection valve and is mixed with a continuously streaming flow of lanthanum alizarin complexone solution. The formed blue colour is measured by spectrometric detection around 620 nm. Without the distillation, fluoride ion in water samples is determined. 4 Interferences Without distillation, la
32、nthanum alizarin complexone spectrometric method suffers from the interferences by aluminium, cadmium, cobalt, iron, nickel, beryllium, lead, etc. However, these interferences are removed by the distillation. 5 Reagents Use only reagents of recognized analytical grade. The prepared solution is degas
33、sed, if necessary. 5.1 Water, grade 1, as specified in ISO 3696. 5.2 1,2-Dihydroxyanthraquinonyl-3-methylamine-N,N-diacetic acid dihydrate (alizarin complexone), C 19 H 15 NO 8 2H 2 O. 5.3 Ammonia solution I, c(NH 3 ) = 15 mol/l, as specified in ISO 6353-2. 5.4 Hydrochloric acid I, c(HCl) = 12 mol/l
34、, as specified in ISO 6353-2. 5.5 Ammonium acetate, C 2 H 7 NO 2 , as specified in ISO 6353-2. 5.6 Sodium acetate trihydrate, C 2 H 3 O 2 Na3H 2 O, as specified in ISO 6353-2. 5.7 Acetic acid, C 2 H 4 O 2 , as specified in ISO 6353-2. 5.8 Lanthanum(III) oxide, La 2 O 3 . 5.9 Acetone, C 3 H 6 O, as s
35、pecified in ISO 6353-2. 5.10 Sodium fluoride, NaF. 5.11 Sulfuric acid, c(H 2 SO 4 ) = 18 mol/l. 5.12 Phosphoric acid, c(H 3 PO 4 ) = 14,6 mol/l. 5.13 Carrier solution, water (5.1). 5.14 Ammonia solution II. Mix 10 ml of ammonia solution I (5.3) and 100 ml of water (5.1). 5.15 Ammonium acetate soluti
36、on, (C 2 H 7 NO 2 ) = 200 g/l. Dissolve 200 g of ammonium acetate (5.5) in about 800 ml of water (5.1). Make up to 1 000 ml with water (5.1). 5.16 Sodium acetate solution. Dissolve 41 g of sodium acetate trihydrate (5.6) in 400 ml of water (5.1) and add 24 ml of acetic acid (5.7).2 ISO 2016 All righ
37、ts reservedPD ISO/TS 17951-1:2016ISO/TS 17951-1:2016(E) 5.17 Hydrochloric acid II, c(HCl) = 2 mol/l. Mix 20 ml of hydrochloric acid (5.4) and 100 ml of water (5.1). 5.18 Lanthanum(III) solution, c(La(III) = 0,1 mol/l. Add 0,163 g of lanthanum(III) oxide (5.8) to 10 ml of hydrochloric acid II (5.17)
38、and dissolve it by heating of the solution. 5.19 Lanthanum-alizarin complexone solution. Dissolve 0,192 g of alizarin complexone (5.2) to 4 ml of ammonia solution II (5.14) and 4 ml of ammonium acetate solution (200 g/l) (5.15). Add this solution into 425 ml of sodium acetate solution (5.16) with st
39、irring, and add 400 ml of acetone (5.9) gradually. Then, add 10 ml of lanthanum(III) solution (5.18) to the solution and mix it. After cooling, adjust the pH of the solution to 4,7 with acetic acid (5.7) or ammonia solution I (5.3), then make it up to 1 000 ml with water (5.1). Lanthanum-alizarin co
40、mplexone solution (5.19) can be prepared by using alfusone. 1)In that case, after dissolving 1,2 g of alfusone to small amount of water (5.1), add 90 ml of acetone (5.9) and mix the solution. Make up the solution to 300 ml with water (5.1). The solution shall be prepared at the time of analysis. 5.2
41、0 Fluoride stock solution ion, (F) = 100 mg/l. Take sodium fluoride (5.10) in a platinum plate and dry at 105 C at least 1 h. Then cool it in a desiccator. Dissolve 0,221 g of NaF (5.10) in water in a 1 000 ml volumetric flask. Make up to volume with water (5.1). This solution is stable for one mont
42、h at room temperature in a polyethylene bottle. 5.21 Fluoride standard solution, (F) = 10 mg/l. Take 10 ml of the fluoride stock solution (5.20) to a 100 ml volumetric flask and make up to volume with water (5.1). This solution is stable for one week in the dark at 2 C to 8 C in a polyethylene bottl
43、e. 5.22 Calibration solutions. Prepare at least five calibration solutions with fluoride concentrations roughly regularly distributed over the working range, by dilution of the appropriate fluoride standard solution or the fluoride stock solution. Examples of calibration solutions for two possible w
44、orking ranges are given in 5.22.1. For other working ranges, prepare calibration solutions appropriate to cover a decade of concentrations, accordingly. 5.22.1 General Prepare at least five calibration solutions to cover a decade of concentration, accordingly. 5.22.2 Calibration solutions I for work
45、ing range 0,1 mg/l to 1 mg/l For example, six calibration solutions should be prepared as follows. Pipette, into 100 ml volumetric flasks, 1 ml, 2 ml, 4 ml, 6 ml, 8 ml and 10 ml respectively, of the fluoride standard solution I (5.21) and make up to volume with water (5.1). 1) Alfusone is a product
46、commercially available. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of this product. ISO 2016 All rights reserved 3PD ISO/TS 17951-1:2016ISO/TS 17951-1:2016(E) These solutions contain 0,1 mg/l, 0,2 mg/l, 0,4 mg/l
47、, 0,6 mg/l, 0,8 mg/l and 1 mg/l fluoride, respectively. 5.22.3 Calibration solutions II for working range 1 mg/l to 10 mg/l For example, six calibration solutions should be prepared as follows. Pipette, into 100 ml volumetric flasks, 1 ml, 2 ml, 4 ml, 6 ml, 8 ml and 10 ml respectively, of the fluori
48、de standard solution I (5.20) and make up to volume with water (5.1). These solutions contain 1 mg/l, 2 mg/l, 4 mg/l, 6 mg/l, 8 mg/l and 10 mg/l fluoride, respectively. 6 Apparatus Usual laboratory equipment and, in particular, the following. 6.1 Flow injection analysis system. A suitable example of
49、 the system contains the components as specified in 6.1.1 to 6.1.5 (see Figure A.1). 6.1.1 Low pulsation pump. Use a multichannel quantitative pump with a low pulsation. 6.1.2 Sample introduction system. Use an injector for introducing samples. Select the appropriate amount of sample. Automatic sample introduction device can be used, if necessary. 6.1.3 Reaction manifold, consists of fluorocarbon polymer tubes, such as polytetrafluoroethylene (PTFE) with the internal diameter of 0,5 mm to 0,8 mm,
