1、PD ISO/TS 17951-2:2016 Water quality Determination of fluoride using flow analysis (FIA and CFA) Part 2: Method using continuous flow analysis (CFA) with automated in-line distillation BSI Standards Publication WB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06PD ISO/TS 17951-2:2016 PUBLISHED
2、DOCUMENT National foreword This Published Document is the UK implementation of ISO/TS 17951-2:2016. 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 committee can be obtained on
3、 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 94114 6 ICS 13.060.50 Compliance with
4、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 17951-2:2016 ISO 2016 Water quality Determi
5、nation of fluoride using flow analysis (FIA and CFA) Part 2: Method using continuous flow analysis (CFA) with automated in-line distillation Qualit de leau Dosage des fluorures par analyse en flux (FIA et CFA) Partie 2: Mthode par analyse en flux continu (CFA) avec distillation in situ automatique T
6、ECHNICAL SPECIFICATION ISO/TS 17951-2 Reference number ISO/TS 17951-2:2016(E) First edition 2016-07-01PD ISO/TS 17951-2:2016ISO/TS 17951-2:2016(E)ii ISO 2016 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2016, Published in Switzerland All rights reserved. Unless otherwise specified, no part o
7、f 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 address below or ISOs member body
8、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 17951-2:2016ISO/TS 17951-2:2016(E)Foreword iv Introduction v 1 Scope . 1 2 Normative references 1 3 P
9、rinciple 2 4 Interferences 2 5 Reagents 2 6 Apparatus . 5 7 Sampling and sample preparation 5 8 Procedure. 5 8.1 Setting up the system 5 8.2 Reagent blank measurement 5 8.3 Adjustment of sensitivity . 6 8.4 Confirmation of repeatability . 6 8.5 Calibration 6 8.6 Measurement of samples . 6 9 Calculat
10、ion 7 10 Expression of results 7 11 Test report . 7 Annex A (informative) Example of continuous flow analysis (CFA) with an in-line distillation unit and spectrometric detection 8 Annex B (informative) Determination of fluoride by automatic distillation continuous flow analysis (CFA) and ion selecti
11、ve detection . 9 Annex C (informative) Examples of flow systems .12 Annex D (informative) Results of interlaboratory trial .13 Annex E (informative) Recovery test for fluoride 14 Annex F (informative) Analytical precision of fluoride 15 Bibliography .16 ISO 2016 All rights reserved iii Contents Page
12、PD ISO/TS 17951-2:2016ISO/TS 17951-2:2016(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each memb
13、er 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, also take part in the work. ISO collaborates closely with the International Ele
14、ctrotechnical 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 1. In particular the different approval criteria needed for the different types
15、 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 elements of this document may be the subject of patent rights. ISO shall not be h
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18、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 following parts, under the general title Water quality Determination of fluoride usin
19、g 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 automated in-line distillation Technical Specificationiv ISO 2016 All rights rese
20、rvedPD ISO/TS 17951-2:2016ISO/TS 17951-2:2016(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 insoluble forms, such as calcium and magnesium fluorides. Excess fluoride can cause
21、 bone damage and fluorosis. In order to ensure conversion of any insoluble fluorides into soluble fluoride for measurement, steam distillation is necessary. This part of ISO 17951 describes a CFA method for flow analysis of fluoride with integrated in-line distillation and spectrometric detection. A
22、 CFA method with ion-selective detection is described in Annex B. ISO 2016 All rights reserved vPD ISO/TS 17951-2:2016PD ISO/TS 17951-2:2016Water quality Determination of fluoride using flow analysis (FIA and CFA) Part 2: Method using continuous flow analysis (CFA) with automated in-line distillatio
23、n WARNING Persons using this part of ISO 17951 should be familiar with normal laboratory practice. This part of ISO 17951 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
24、 and to ensure compliance with any national regulatory conditions. IMPORTANT It is absolutely essential that tests conducted in accordance 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 wa
25、ters, waste waters and effluents by continuous flow analysis (CFA). Any insoluble or complexed fluoride is converted to fluoride ion by an automated continuous flow distillation procedure from sulfuric/phosphoric acid. Fluoride ion in the distillate is measured using flow analysis with lanthanum ali
26、zarin complexone and spectrometric detection. This method is applicable to industrial waste waters, effluents, surface waters, ground waters, leachates. When this method is applied to the analysis of drinking water, a heater and a distillation unit is unnecessary. Some drinking water contains high c
27、oncentration of aluminium and iron. In the case of drinking water, this part of ISO 17951 is appropriate to drinking water with low interferences. It is not applicable to samples which contain large amount of suspended matter. In this part of ISO 17951, two working ranges are described: working rang
28、e I: 0,1 mg/l to 1,0 mg/l; working range II: 1,0 mg/l to 10 mg/l. The specification of the calibration solutions are to be adapted accordingly. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application.
29、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 methods ISO 6353-2, Reagents for chemical analysis Part 2: Specificatio
30、ns First series ISO 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical evaluation of the linear calibration function ISO 8466-2, Water quality Calibration and evaluation of analytical methods and estimation of perf
31、ormance characteristics Part 2: Calibration strategy for non-linear second-order calibration functions TECHNICAL SPECIFICATION ISO/TS 17951-2:2016(E) ISO 2016 All rights reserved 1PD ISO/TS 17951-2:2016ISO/TS 17951-2:2016(E) 3 Principle Sample, water and mixture of sulfuric acid and phosphoric acid
32、are gas-segmented and mixed in a reaction coil. The mixture is transported through a heating device and a distillation unit. The distillate is mixed with collection solution and lanthanum alizarin complexone solution. The mixture is transported to a reaction coil and the formed blue colour is measur
33、ed by spectrometric detection around 620 nm. 4 Interferences Without distillation, lanthanum alizarin complexone spectrophotometric method suffers from the interferences by aluminium, cadmium, cobalt, iron, nickel, beryllium, lead, etc. However, these interferences are removed by the distillation. I
34、n the case of sample containing high chloride, the recovery of fluoride decreases. For example, in a sea water sample, the response decreases to about 70 %. Thus, recovery test is necessary for the analysis of such samples. 5 Reagents Use only reagents of recognized analytical grade. The prepared so
35、lution is degassed, 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(
36、HCl) = 12 mol/l, as specified in ISO 6353-2. 5.5 Ammonium acetate, CH 3 COONH 4 , as specified in ISO 6353-2. 5.6 Sodium acetate trihydrate, CH 3 COONa3H 2 O, as specified in ISO 6353-2. 5.7 Acetic acid, CH 3 COOH, as specified in ISO 6353-2. 5.8 Lanthanum(III) oxide, La 2 O 3 . 5.9 Acetone, CH 3 CO
37、CH 3 , as specified in ISO 6353-2. 5.10 Sodium fluoride, NaF. 5.11 Ethanol (95), C 2 H 5 OH(95). (95) = volume fraction. 5.12 Sulfuric acid, c(H 2 SO 4 ) = 18 mol/l. 5.13 Imidazole, C 3 H 4 N 2 . 5.14 Poly(oxyethylene)octylphenylether, C 14 H 22 O(C 2 H 4 O) n .2 ISO 2016 All rights reservedPD ISO/T
38、S 17951-2:2016ISO/TS 17951-2:2016(E) 5.15 Phosphoric acid, c(H 3 PO 4 ) = 14,6 mol/l. 5.16 Ammonia solution II. Mix 10 ml of ammonia solution I (5.3) and 100 ml of water (5.1). 5.17 Ammonium acetate solution, (C 2 H 7 NO 2 ) = 200 g/l. Dissolve 200 g of ammonium acetate (5.5) to about 800 ml of wate
39、r (5.1). Make up to 1 000 ml with water (5.1). 5.18 Sodium acetate solution. Dissolve 41 g of sodium acetate trihydrate (5.6) to 400 ml of water, and add 24 ml of acetic acid (5.7). 5.19 Hydrochloric acid II, c(HCl) = 2 mol/l. Mix 20 ml of hydrochloric acid I (5.4) and 100 ml of water (5.1). 5.20 La
40、nthanum(III) oxide 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 (5.19) and dissolve it by heating of the solution. 5.21 Lanthanum-alizarin complexone solution (solution A). Dissolve 0,192 g of alizarin complexone (5.2) to 4 ml of ammonia
41、 solution II (5.16) and 4 ml of ammonium acetate solution (200 g/l) (5.17). Add this solution into 425 ml of sodium acetate solution (5.18) with stirring, and add 400 ml of acetone (5.9) gradually. Then, add 10 ml of lanthanum(III) oxide solution (5.20) to the solution and mix it. After cooling, adj
42、ust 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 complexone solution (solution A) (5.21) can be prepared by using alfusone. 1)In that case, after dissolving 1,2 g of alfusone to small amount of wate
43、r (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. 5.22 Lanthanum-alizarin complexone solution (solution B). Dissolve 10 g of imidazole (5.13) to about 200 ml of water (5.1). Add 40 ml of
44、acetic acid (5.7), 45 ml of acetone (5.9) and 0,5 ml of fluoride stock solution I (5.23). Make up the solution to 300 ml with water (5.1). Add 200 ml of lanthanum-alizarin complexone solution (solution A) (5.21) and 5 ml of ethanol solution of poly(oxyethylene)octylphenylether (5.25) and mix the sol
45、ution. Lanthanum-alizarin complexone solution (solution B) (5.22) can be prepared with alfusone. In that case, dissolve 2,5 g of alfusone to about 300 ml of water (5.1). Add 40 ml of acetic acid (5.7), 10 g of imidazole (5.13), 125 ml of acetone (5.9) and 0,5 ml of fluoride stock solution I (5.23),
46、and mix the solution. After making up the solution to 500 ml with water (5.1), add 5 ml of ethanol solution of poly(oxyethylene) octylphenylether (5.25) and mix the solution. This solution shall be prepared at the time of analysis. 5.23 Fluoride stock solution, (F) = 100 mg/l. Take sodium fluoride (
47、5.10) in a platinum plate and heat it at 105 C at least 1 h. Then cool it in a desiccator. Dissolve 0,221 g of NaF (5.10) in water (5.1) and in a 1 000 ml volumetric flask and make up to volume with water (5.1). Store the solution in a polyethylene bottle. 1) Alfusone is a product commercially avail
48、able. 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 17951-2:2016ISO/TS 17951-2:2016(E) This solution is stable for one month at room temperature. 5.24 Fluori
49、de standard solution, (F) = 10 mg/l. Take 10 ml of fluoride stock solution (5.23) to a 100 ml volumetric flask and make up to volume with water (5.1). Store the solution in a polyethylene bottle. This solution is stable for one week in the dark at 2 C to 8 C. 5.25 Ethanol solution of poly(oxyethylene)octylphenylether. Dissolve 50 g of poly(oxyethylene)octylphenylether (5.14) in ethanol (95) (5.11) and make up to 100 ml with ethanol (95) (5.11). This solution is stable for one month at room temperat
