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1、BRITISH STANDARD BS EN ISO 14402:1999 BS 6068-2.68:1999 Water quality Determination of phenol index by flow analysis (FIA and CFA) The European Standard EN ISO 14402:1999 has the status of a British Standard ICS 13.060.50 Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006
2、, Uncontrolled Copy, (c) BSI BS EN ISO 14402:1999 This British Standard, having been prepared under the direction of the Health and Environment Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 November 1999 BSI 04-2000 ISBN 0 580 35101 7 Amen
3、dments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 14402:1999 BSI 04-2000i Contents Page National forewordii Foreword2 Forewordiii Text of ISO 144021 Licensed Copy: sheffieldun shef
4、fieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 14402:1999 ii BSI 04-2000 National foreword This British Standard reproduces verbatim ISO 14402:1999 and implements it as the UK national standard. The UK participation in its preparation was entrusted by Technical
5、 Committee EH/3, Water quality, to Subcommittee EH/3/2, Physical, chemical present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulg
6、ate them in the UK. A list of organizations represented on this subcommittee can be obtained on request to its secretary. BS EN ISO 14402 is one of a series of standards on water quality, others of which have been, or will be, published as Sections of BS 6068. This standard has therefore been given
7、the secondary identifier BS 6068-2.68. The various Sections of BS 6068 are comprised within Parts 1 to 7, which, together with Part 0, are listed below. Part 0: Introduction; Part 1: Glossary; Part 2: Physical, chemical and biochemical methods; Part 3: Radiological methods; Part 4: Microbiological m
8、ethods; Part 5: Biological methods; Part 6: Sampling; Part 7: Precision and accuracy. NOTEThe tests described in this British Standard should only be carried out by suitably qualified persons with an appropriate level of chemical expertise. Standard chemical procedures should be followed throughout.
9、 Cross-references The British Standards which implement international publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catal
10、ogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comp
11、rises a front cover, an inside front cover, pages i and ii, the EN ISO title page, page 2, the ISO title page, pages ii to iv, pages 1 to 14, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in
12、 the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14402 September 1999 ICS English version Water quality Determination of phenol index by
13、flow analysis (FIA and CFA) (ISO 14402:1999) Qualit de leau Dtermination de lindice phnol par analyse en flux (FIA et CFA) (ISO 14402:1999) Wasserbeschaffenheit Bestimmung des Phenolindex mit der Flieanalytik (FIA und CFA) (ISO 14402:1999) This European Standard was approved by CEN on 23 July 1999.
14、CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on a
15、pplication to the Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Central Secretariat h
16、as the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European C
17、ommittee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1999 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 14402:1999 E Licensed Copy
18、: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 14402:1999 BSI 04-2000 2 Foreword The text of the International Standard ISO 14402:1999 has been prepared by Technical Committee ISO/TC 147 “Water quality” in collaboration with Technical Committee C
19、EN/TC 230 “Water analysis”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by March 2000, and conflicting national standards shall be withdrawn at the latest
20、 by March 2000. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherla
21、nds, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. NOTE FROM CEN/CS: The foreword is susceptible to be amended on reception of the German language version. The confirmed or amended foreword, and when appropriate, the normative Annex ZA for the references to international publi
22、cations with their relevant European publications will be circulated with the German version. Endorsement notice The text of the International Standard ISO 14402:1999 was approved by CEN as a European Standard without any modification. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29
23、GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 14402:1999 ii BSI 04-2000 Contents Page Forewordiii Introduction1 1Scope1 2Normative references1 3Determination of phenol index (without distil
24、lation) after extraction1 3.1Principle1 3.2Interferences2 3.3Reagents2 3.4Apparatus3 3.5Sampling5 3.6Procedure6 3.7Calculation of results7 4Determination of phenol index (without extraction) after distillation7 4.1Principle7 4.2Interferences7 4.3Reagents7 4.4Apparatus8 4.5Sampling11 4.6Procedure11 4
25、.7Calculation of results11 5Expression of results12 6Precision and accuracy12 7Test report12 Annex A (informative) Statistical data13 BibliographyInside back cover Figure 1 Example of a flow injection system for the determination of 0,01 mg/l to 1,0 mg/l phenol index without distillation and with ex
26、traction4 Figure 2 Example of a continuous flow system for the determination of 0,01 mg/l to 1,0 mg/l of phenol index without distillation and with extraction5 Figure 3 Example of a combined FIA/CFA-system for the determination of 0,01 mg/l to 1,0 mg/l phenol index with distillation and without liqu
27、id-liquid extraction9 Figure 4 Example of a continuous flow system for determination of 0,01 mg/l to 1,0 mg/l of phenol index with distillation and without liquid-liquid extraction10 Table A.1 Statistical data for the determination of phenol index after extraction with continuous flow analysis (CFA)
28、13 Table A.2 Statistical data for the determination of phenol index after extraction with flow injection analysis (FIA)13 Table A.3 Statistical data for the determination of phenol index after extraction with flow analysis (combined evaluation of data, obtained from FIA- and CFA-systems)14 Table A.4
29、 Statistical data for the determination of phenol index after distillation with flow analysis (only CFA systems)14 Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 14402:1999 BSI 04-2000iii Foreword ISO (the International Organization
30、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 member body interested in a subject for which a technical committee has been established has t
31、he 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 Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Interna
32、tional Standards are drafted in accordance with the rules given 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 memb
33、er bodies casting a vote. International Standard ISO 14402 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical biochemical methods. Annex A of this International Standard is for information only. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18
34、01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 14402:1999 BSI 04-20001 Introduction Methods for determination of water quality using flow analysis and automatic wet chemica
35、l procedures are particularly suitable for the processing of large sample series at a high analysis frequency. Differentiation is needed between flow injection analysis (FIA) 1, 2 and continuous flow analysis (CFA) 3. Both methods include automatic dosage of the sample into a flow system (manifold)
36、where the analytes in the sample react with the reagent solutions on their way through the manifold. The sample preparation may be integrated in the manifold. The reaction product is measured in a flow detector. Phenol index is an analytical convention. It represents a group of aromatic compounds wh
37、ich under the specific reaction conditions form coloured condensation products. The analytical result is expressed in terms of phenol concentration. This International Standard describes two methods: the determination of phenol index (without distillation) after extraction, and the determination of
38、phenol index (without extraction) after distillation. It should be investigated whether and to what extent particular problems will require the specification of additional marginal conditions. 1 Scope This International Standard specifies two methods for the determination of the phenol index in wate
39、rs of different origin (such as ground waters, surface waters, seep waters, and waste waters) in mass concentrations of 0,01 mg/l to 1 mg/l (in the undiluted sample). In particular cases, the range of application may be adapted by varying the operating conditions. Clause 3 describes the determinatio
40、n of phenol index (without distillation) after extraction, and in clause 4 the determination of phenol index (without extraction) after distillation is given. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of t
41、his International Standard. For dated references, subsequent amendments to, or revisions 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
42、 documents indicated below. For undated references, the latest edition of the normative 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 5667-3:19
43、94, Water quality Sampling Part 3: Guidance on sample handling and preservation. ISO 6439:1990, Water quality Determination of phenol index 4-Aminoantipyrine spectrometric methods after distillation. 3 Determination of phenol index (without distillation) after extraction 3.1 Principle The sample is
44、fed into a continuously flowing carrier stream and mixed with also continuously flowing solutions of 4-aminoantipyrine and potassium peroxodisulfate. Phenolic compounds in the sample are oxidized by potassium peroxodisulfate, and the resulting quinones react with 4-aminoantipyrine, forming coloured
45、condensation products. These are extracted in a flow extraction unit from the aqueous phase into chloroform. The chloroform phase is separated by a suitable phase separator (e.g. a hydrophobic semipermeable membrane), and the absorbance of the organic phase is measured spectrometrically in a flow sp
46、ectrometer at 470 nm to 475 nm. More information on this analytical technique is given in the references 6 to 9. It is absolutely essential that the test described in this International Standard be carried out by suitably qualified staff. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:48:
47、29 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 14402:1999 2 BSI 04-2000 3.2 Interferences 3.2.1 Chemical interferences Under the prevailing reaction conditions, aromatic amines will also form condensation products with 4-aminoantipyrine, leading to positive bias. Interferences can occur when t
48、he sample, after the addition of the reagent solutions, does not reach a pH of 10,0 to 10,5. In particular this may occur in the cases of strongly acidic, strongly alkaline and buffered samples. In these cases, the sample is adjusted to a pH between 5 and 7 prior to addition of the reagent solutions
49、. Further information on interferences is given in 5. 3.2.2 Physical interferences arising from applying CFA and FIA If the samples contain particulate matter, refer to 3.5 (last paragraph). Turbid samples do not cause interferences with the determination. In the event of coloured samples, check whether the colour can be extracted with chloroform, and determine the sample blank without the addition of reagents R1 and R2. The difference in response between the two measurements shall be taken into account