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1、Reference number ISO 15061:2001(E) ISO 2001 INTERNATIONAL STANDARD ISO 15061 First edition 2001-07-01 Water quality Determination of dissolved bromate Method by liquid chromatography of ions Qualit de leau Dosage du bromate dissous Mthode par chromatographie des ions en phase liquide Copyright Inter
2、national Organization for Standardization Provided by IHS under license with ISO Licensee=Shell Global Solutions International B.V./5924979112 Not for Resale, 04/17/2007 10:56:02 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15061:2001(E) PDF disclaimer This PDF file
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5、tion parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. ISO 2001 All rights reserved. Unles
6、s otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO co
7、pyright office Case postale 56 ? CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.ch Web www.iso.ch Printed in Switzerland ii ISO 2001 All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Shell
8、Global Solutions International B.V./5924979112 Not for Resale, 04/17/2007 10:56:02 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15061:2001(E) ISO 2001 All rights reservediii ContentsPage Foreword.iv Introduction.v 1Scope 1 2Normative references1 3Interferences 1 4Pri
9、nciple2 5Essential minimum requirements2 6Reagents.3 7Apparatus.4 8Quality requirements for the separator column.6 9Sampling and sample pretreatment.8 10Procedure.10 11Calculation12 12Expression of results 12 13Test report12 Annex A (informative) Eluents.13 Annex B (informative) Regeneration solutio
10、ns15 Annex C (informative) Example of column-switching technique.16 Annex D (informative) Interlaboratory trial.18 Annex E (informative) Checked interferences20 Bibliography21 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Shell Global Soluti
11、ons International B.V./5924979112 Not for Resale, 04/17/2007 10:56:02 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15061:2001(E) iv ISO 2001 All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide federation of national st
12、andards 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. International o
13、rganizations, 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. International Standards are drafted in accordance with the rules giv
14、en in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibili
15、ty that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. InternationalStandardISO 15061waspreparedbyTechnicalCommitteeISO/TC 147,Waterquality, Subcommittee SC 2, Physical, chemica
16、l and biochemical methods. Annexes A, B, C, D and E of this International Standard are for information only. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Shell Global Solutions International B.V./5924979112 Not for Resale, 04/17/2007 10:56:
17、02 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15061:2001(E) ISO 2001 All rights reservedv Introduction The essential minimum requirements of an ion chromatographic system applied within the scope of this International Standard for the determination of dissolved bro
18、mate are given in clause 5. The diversity of the appropriate and suitable assemblies, and the procedural steps depending on them, permit a general description only. Further information on the analytical technique can be found in the normative references (clause 2) and the bibliography. Copyright Int
19、ernational Organization for Standardization Provided by IHS under license with ISO Licensee=Shell Global Solutions International B.V./5924979112 Not for Resale, 04/17/2007 10:56:02 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyright International Organization for Stan
20、dardization Provided by IHS under license with ISO Licensee=Shell Global Solutions International B.V./5924979112 Not for Resale, 04/17/2007 10:56:02 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARDISO 15061:2001(E) ISO 2001 All rights reserved1 Water q
21、uality Determination of dissolved bromate Method by liquid chromatography of ions 1Scope This International Standard specifies a method for the determination of dissolved bromate in water (e.g. drinking water, raw water, surface water, partially treated water or swimming pool water). Appropriate pre
22、treatment of the sample, for example by elimination of chloride, sulfate, metals, preconcentration or dilution, gives a range of applicability of 0,5 g/l to 1 000 g/l dissolved bromate. The working range is restricted by the ion-exchange capacity of any preconcentration columns used and that of the
23、separator column. Dilution of the sample to the working range may be necessary. 2Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or r
24、evisions of, any of these publications do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the no
25、rmative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 3696:1987, Water for analytical laboratory use Specification and test methods. ISO 5667-1:1980, Water quality Sampling Part 1: Guidance on the design of sampling programmes
26、. ISO 5667-2:1991, Water quality Sampling Part 2: Guidance on sampling techniques. ISO 5667-3:1994, Water quality Sampling Part 3: Guidance on the preservation and handling of samples. ISO 8466-1:1990, Water quality Calibration and evaluation of analytical methods and estimation of performance chara
27、cteristics Part 1: Statistical evaluation of the linear calibration function. ISO 8466-2:1993, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 2: Calibration strategy for non-linear second order calibration functions. 3Interferences 3
28、.1The presence of nitrate, chloride, carbonate and sulfate may affect the capacity of the concentrator column and lead to poor recovery of bromate (9.2.1). 3.2The presence of chloride, sulfate, carbonate and hydrogen carbonate can cause interference with the determination of bromate (9.2.1). Dependi
29、ng on the column utilized, other ions may interfere; this should be checked. 3.3Metals present (e.g. barium and silver ions released from sample pretreatment steps) will bind to the resin material of concentrator and separator columns, resulting in a loss of performance. Metal ions may be eliminated
30、 with the aid of a metal clean-up column or special exchangers (see Figure 1 and clause 9). Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Shell Global Solutions International B.V./5924979112 Not for Resale, 04/17/2007 10:56:02 MDTNo reproduc
31、tion or networking permitted without license from IHS -,-,- ISO 15061:2001(E) 2 ISO 2001 All rights reserved 3.4The interference of some organic acids with the determination of bromate was checked and found not to be significant to the concentrations tested (annex E). 3.5Solid particles and organic
32、compounds such as mineral oils, detergents and humic acids shorten the life-time of the concentrator and separator column. 4Principle 4.1Sample pretreatment is carried out in order to remove ozone (9.1.3) and solids, and to reduce chloride, sulfate, carbonate, hydrogen carbonate and metals present b
33、y use of cation exchangers (9.2). 4.2Measurement of bromate is made in the range 0,5 g/l to 1 000 g/l, with or without preconcentration (10.3). 4.3Liquid chromatographic separation of bromate is carried out either by means of a separator column or after elution of bromate from a concentrator column,
34、 if used. An anion exchange resin is used as the stationary phase, and usually, aqueous solutions of salts of weak mono- and dibasic acids as eluent (see 6.10 and annex A). 4.4A conductivity detector (CD) with chemical suppression is used. A UV detector (?= 190 nm to 205 nm) is suitable to confirm t
35、he CD results only. NOTEWhen using conductivity detectors it is essential that the eluents have a sufficiently low conductivity. For this reason, conductivity detectors are combined with a suppressor device (cation exchanger) which reduces the conductivity of the eluent and transforms the sample spe
36、cies into their respective acids. UV detection measures absorbance directly. 4.5Strongly retained ions (e.g. nitrate, phosphate, sulfate) are removed from the separator column, e.g. by flushing the separator column with a more concentrated eluent. 4.6The concentration of bromate is determined after
37、calibration of the overall procedure. 5Essential minimum requirements a)Preconcentration For low bromate concentrations the use of a concentrator column may be required. On-line techniques can be used (see 10.3 and annex C). Ensure that recovery is within 80 % to 120 %. b)Resolution power of the col
38、umn It is essential that the peak resolution R shall not fall below 1,3 (clause 8, Figure 4) between bromate and the nearest peak, which is usually chloride. c)Method of detection Measurement of the electrical conductivity (CD) with a chemical suppressor device, and UV if confirmation is required. d
39、)Applicability of the method: 0,5 g/l to 1 000 g/l. e)Calibration shall be carried out in accordance with ISO 8466-1 or ISO 8466-2 (10.2). f)Guarantee of analytical quality Control is necessary for the validity of the calibration function (10.5). Replicate determinations may be necessary. Use of the
40、 method of standard addition may be required when matrix interferences are expected (10.3). Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Shell Global Solutions International B.V./5924979112 Not for Resale, 04/17/2007 10:56:02 MDTNo reproduc
41、tion or networking permitted without license from IHS -,-,- ISO 15061:2001(E) ISO 2001 All rights reserved3 6Reagents Use only reagents of recognized analytical grade. Carry out weighing of the reagents with an accuracy of?1 % of the nominal mass, unless stated otherwise. 6.1Water, complying with gr
42、ade 1 as defined in ISO 3696. 6.2Sodium hydrogen carbonate, NaHCO3. 6.3Sodium carbonate, Na2CO3. 6.4Disodium tetraborate decahydrate, Na2B4O7?10 H2O. 6.5Boric acid, H3BO3. 6.6Potassium bromate, KBrO3. 6.7Nitric acid, c(HNO3) = 0,1 mol/l. 6.8Sulfuric acid,?(H2SO4) = 1,84 g/ml. 6.9Ethylenediamine, C2H
43、8N2. 6.10Eluents. Degas all water used for eluent preparation. Take steps to avoid any renewed air pick-up during operation (e.g. by helium sparging). In order to minimize the growth of bacteria or algae, store the eluents in the dark and renew every 3 d. See annex A for examples of eluents. Two dif
44、ferent types of eluent are used. 6.10.1Eluent of Type 1, of a lower concentration level (for examples see clause A.1) to be applicable for the separation of bromate and 6.10.2Eluent of Type 2, of a higher concentration level (for examples see clause A.2) to be applicable to remove strongly retained
45、ions (e.g. nitrate, phosphate) from the concentrator and separator column. The choice of eluent is dependent on the choice of column and detector; seek advice from the column supplier. The chosen combination of separator column and eluent shall conform to the resolution requirements stated in clause
46、 8. A selection of reagents for common eluents is presented in 6.2 to 6.5. 6.11Bromate stock standard solution,?(BrO3?) = 1 000 mg/l Dry approximately 1,5 g of potassium bromate (6.6) for at least 1 h at 105 C?5 C. Store the dried solid in a desiccator. Dissolve 1,306 g?0,001 g of the dried potassiu
47、m bromate in approximately 800 ml of water (6.1) in a 1 000 ml volumetric flask, and dilute to volume with water (6.1). Store the solution at 2 C to 6 C in polyethylene or glass bottles and renew it every 12 months. Alternatively, use commercially available stock solutions of the required concentrat
48、ion. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=Shell Global Solutions International B.V./5924979112 Not for Resale, 04/17/2007 10:56:02 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15061:2001(E) 4 ISO 2001 All rights reserved 6.12Bromate standard solutions. 6.12.1General Depending upon the concentrations expected, prepare the