ISO-10304-1-1992.pdf
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1、INTERNATIONAL STANDARD IS0 10304-I First edition 1992-11-15 Water quality - Determination of dissolved fluoride, chloride, nitrite, orthophosphate, bromide, nitrate and sulfate ions, using liquid chromatography of ions - Part 1: Method for water with low contamination Qua/it6 de I eau - Dosage des i
2、ons fluorure, chlorure, nitrite, orthophosphate, bromure, nitrate et sulfate dissous, par chromatographie des ions en phase liquide - Partie I: Mkthode applicable pour les eaux faiblement contaminkes Reference number IS0 10304-1:1992(E) Copyright International Organization for Standardization Provid
3、ed by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 08:41:57 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 10304-1:1992(E) Foreword IS0 (the International Organization for Standardization) is a worldwide federatio
4、n of national standards bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 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.
5、 International organizations, govern- mental and non-governmental, in liaison with ISO, also take part in the work. IS0 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the techn
6、ical committees are circulated to the member bodies for voting. Publication as an Inter- national Standard requires approval by at least 75 % of the member bodies casting a vote. International Standard IS0 10304-I was prepared by Technical Commit- tee ISO/TC 147, Water qualify, Sub-Committee SC 2, P
7、hysical, chemical, biochemical methods, IS0 10304 consists of the following parts, under the general title Water quality - Determination of dissolved fluoride, chloride, nitrite, orthophosphate, bromide, nitrate and sulfate ions, using liquid chro- matography of ions: - Part 1: Method for water with
8、 low contamination - Part 2: Method for waste water - Part 3: Determination of chromate, thiocyanate and thiosulfate Annex A of this pat-t of IS0 10304 is for information only. 0 IS0 1992 All rights reserved. No part of this publication may be reproduced or utilized in any form or by any means, elec
9、tronic or mechanical, including photocopying and microfilm, without permlsslon In writing from the publisher. International Organization for Standardization Case Postale 56 l CH-1211 Gen sample injection system (e.g. sample loop, 50 PI); precolumn (see clause 7); separating column with the required
10、separating performance (see clause 6); conductivity detector, with or without a suppressor device; recording device (e.g. integrator with plotter). Table 4 - Concentrations of the calibration solutions Anion F NO2 PO4 Br Cl NO3 so4 Concentrations of the calibration solutions w/l Working range 0,l mg
11、/l to 1 ,O mg/l %I; Q2; 0,3; 0,4; 0,5; 0,6; 0,7: O o,9; I,0 0,l: 0,2; 0,3; 0,4; 0,5: 0,6; 0,7: 0,a; o,9; I,0 0,l: 0,2; 0,3; 0,4; 0,5; 0,6: Q,7; 0,a; o,9: I,0 0,1: 0,2; 0,3: 0,4: 0,5; 0,6: 0,7; 0,a; 0,9: I,0 Working range I,0 mg/l to IO,0 mg/l 1; 2; 3; 4; 5: 6; 7; 8: 9: 10 1; 2: 3; 4; 5; 6; 7; a; 9;
12、10 1; 2; 3; 4; 5; 6; 7: 8; 9; 10 NOTE - The addition of lml of the eluent concentrate solution decreases the concen- tration of the calibration solution. However, this deviation is compensated by the equal treatment of the sample (see clause 7). 5 Copyright International Organization for Standardiza
13、tion Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 08:41:57 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 10304-1:1992(E) Sample Q InJectIon t Separating Eluent - Pump Precolumn Figure 1 - Schematic di
14、agram of an ion chromatography system 5.2 Additional equipment, including the following: drying oven; desiccator; graduated flasks, of nominal capacities 100 ml, 1 000 ml, and 5 000 ml; graduated flasks, of nominal capacity 100 ml, plastics, to be used for low concentrations (e.g. -c 0,1 ms/k gradua
15、ted pipettes, of nominal capacity 1 ml to IO ml or microlitre syringes; membrane filtering apparatus with membrane filters of mean pore size 0,45 pm. Quality requirements of the separating column The separating column is the essential part of the ion chromatographic system. Its separating per- forma
16、nce depends on several operating factors, such as column material and type of eluents. Within the scope of this part of IS0 10304, use only those separating columns that yield a baseline resolved separation of all the components of the injected standard solution containing seven anions (F, Cl, NO, P
17、O, Br, NO, and SO,), at a concentration level of 1 mg/l, (see figure2). If only some of the anions shown in figure2 have to be determined, this re- quirement is applicable for those anions. Therefore, the peak resolution shall not fall below R= I,3 (see equation 1 and figure3). Calculate the peak re
18、solution R using the equation R = 2(tR* - fd w, + w* . . . (1) where tRt tR2 is the retention time, in seconds, of the 1st peak; is the retention time, in seconds, of the 2nd peak; is the peak width, in seconds, of the 1st peak; is the peak width, in seconds, of the 2nd peak. 7 Sampling and sample p
19、retreatment Use vessels made of polytetrafluoroethylene (PTFE) or polyethylene for sampling. Use only new vessels or those that have been rinsed thoroughly with wa- ter (see clause 4). To prevent the risk of contam- ination of the sample, do not use strong mineral acids or alkaline detergent solutio
20、ns for cleaning the vessels. After the arrival of the sample in the laboratory, filter it through a membrane filter (of pore size 0,45 pm) to prevent adsorption of the anions on particulate matter or conversion of anions by bacterial growth. Prevent the risk of contamination of the sample by the mem
21、brane (e.g. filter the sample and discard the first portion of the filtrate). Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/21/2007 08:41:57 MDTNo reproduction or networking permitted
22、without license from IHS -,-,- IS0 10304-1:1992(E) Concentration of standard solution s 1 mg/l Sample volume 8 50 FL NOTE - Elution sequences and retention times rk may vary, depending on the type of column and the eluent composition. Figure 2 - Example of a chromatogram of a column conforming to th
23、is part of IS0 10304 tR2 Component i! :omponent 1 ! ! I Tlme (s) c N I Figure 3 - Idealized representation of the chromatographic separation Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale,
24、04/21/2007 08:41:57 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 10304-1:1992(E) Stabilize the sample by cooling it to between 4 “C and 6 “C or by deepfreezing until the analysis is performed, Where nitrite is to be determined, fill the sample vessel completely. Carr
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