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 13.060.50BSENISO14402:1999 This British Standard, having been prepared under the directi
2、onof the Health and Environment Sector Committee,was published underthe authorityof the Standards Committee and comesintoeffecton 15November1999 BSI 04-2000 ISBN 0 580 35101 7 Amendments issued since publication Amd. No. Date CommentsBSENISO14402:1999 BSI 04-2000 i Contents Page National foreword ii
3、 Foreword 2 Foreword iii Text of ISO 14402 1BSENISO14402:1999 ii BSI 04-2000 National foreword This British Standard reproduces verbatim ISO14402:1999 and implements it as the UK national standard. The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality, to S
4、ubcommittee 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 promulgate them in the UK. A list of organi
5、zations 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 BS6068. This standard has therefore been given the secondary identifier BS6068-2.68.
6、 The various Sections of BS6068 are comprised within Parts1 to7, 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 methods; Part 5: Biological methods; Part
7、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. Cross-references The British Standards w
8、hich 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 Catalogue. A British Standard does not purport
9、 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 comprises a front cover, an inside front cove
10、r, pagesi andii, theENISO title page, page 2, the ISO title page, pages ii to iv, pages1 to14, aninside 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 the amendment table on the inside front cover.E
11、UROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM ENISO 14402 September1999 ICS English version Water quality Determination of phenol index by flowanalysis (FIA and CFA) (ISO 14402:1999) Qualit de leau Dtermination de lindice phnol par analyse en flux (FIA et CFA) (ISO14402:1999) Wasserbeschaffenheit
12、 Bestimmung des Phenolindex mit der Flieanalytik (FIA und CFA) (ISO 14402:1999) This European Standard was approved by CEN on23July1999. 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
13、 standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any ot
14、her language made by translation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, G
15、reece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and UnitedKingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1999 CEN All righ
16、ts of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 14402:1999 EENISO14402:1999 BSI 04-2000 2 Foreword The text of the International Standard ISO14402:1999 has been prepared by Technical Committee ISO/TC147 “Water quality” in collaboration wit
17、h Technical Committee CEN/TC230 “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 March2000, and conflicting national standards shall be wi
18、thdrawn at the latest by March2000. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, L
19、uxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the UnitedKingdom. 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 i
20、nternational publications with their relevant European publications will be circulated with the German version. Endorsement notice The text of the International Standard ISO14402:1999 was approved by CEN as a European Standard without any modification.ENISO14402:1999 ii BSI 04-2000 Contents Page For
21、eword iii Introduction 1 1 Scope 1 2 Normative references 1 3 Determination of phenol index (without distillation) after extraction 1 3.1 Principle 1 3.2 Interferences 2 3.3 Reagents 2 3.4 Apparatus 3 3.5 Sampling 5 3.6 Procedure 6 3.7 Calculation of results 7 4 Determination of phenol index (withou
22、t extraction) after distillation 7 4.1 Principle 7 4.2 Interferences 7 4.3 Reagents 7 4.4 Apparatus 8 4.5 Sampling 11 4.6 Procedure 11 4.7 Calculation of results 11 5 Expression of results 12 6 Precision and accuracy 12 7 Test report 12 Annex A (informative) Statistical data 13 Bibliography Inside b
23、ack 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 extraction 4 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 extra
24、ction 5 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 liquid-liquid extraction 9 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 wit
25、hout liquid-liquid extraction 10 Table A.1 Statistical data for the determination of phenol index after extraction with continuous flow analysis (CFA) 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
26、 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 Statistical data for the determination of phenol index after distillation with flow analysis (only CFA systems) 14ENISO14402:1999 BSI 04-2000 iii
27、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 member body interested in a subject for which a t
28、echnical 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 Electrotechnical Commission (IEC) on all matters
29、 of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard re
30、quires approval by at least75% of the member bodies casting a vote. International Standard ISO 14402 was prepared by Technical Committee ISO/TC147, Water quality, Subcommittee SC2, Physical, chemical biochemical methods. Annex A of this International Standard is for information only.iv blankENISO144
31、02:1999 BSI 04-2000 1 Introduction Methods for determination of water quality using flow analysis and automatic wet chemical 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,
32、 2 and continuous flow analysis (CFA) 3. Both methods include automatic dosage of the sample into a flow system (manifold) 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 produ
33、ct is measured in a flow detector. Phenol index is an analytical convention. It represents a group of aromatic compounds which under the specific reaction conditions form coloured condensation products. The analytical result is expressed in terms of phenol concentration. This International Standard
34、describes two methods: the determination of phenol index (without distillation) after extraction, and the determination of phenol index (without extraction) after distillation. It should be investigated whether and to what extent particular problems will require the specification of additional margi
35、nal conditions. 1 Scope This International Standard specifies two methods for the determination of the phenol index in waters of different origin (such as ground waters, surface waters, seep waters, and waste waters) in mass concentrations of0,01mg/l to1mg/l (in the undiluted sample). In particular
36、cases, the range of application may be adapted by varying the operating conditions. Clause 3 describes the determination of phenol index (without distillation) after extraction, and in clause4 the determination of phenol index (without extraction) after distillation is given. 2 Normative references
37、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 revisions of, any of these publications do not apply. However, parties to agreements based on this Inte
38、rnational 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 normative document referred to applies. Members of ISO and IEC maintain registers of currently valid Int
39、ernational Standards. ISO 3696:1987, Water for analytical laboratory use Specification and test methods. ISO 5667-3:1994, Water quality Sampling Part3: Guidance on sample handling and preservation. ISO 6439:1990, Water quality Determination of phenol index 4-Aminoantipyrine spectrometric methods aft
40、er distillation. 3 Determination of phenol index (without distillation) after extraction 3.1 Principle The sample is 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
41、are oxidized by potassium peroxodisulfate, and the resulting quinones react with 4-aminoantipyrine, forming coloured 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 hy
42、drophobic semipermeable membrane), and the absorbance of the organic phase is measured spectrometrically in a flow spectrometer at470nm to475nm. 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 S
43、tandard be carried out by suitably qualified staff.ENISO14402:1999 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 whe
44、n the sample, after the addition of the reagent solutions, does not reach a pH of10,0 to10,5. 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 between5 and7 prior to addition of the reagent solutions.
45、 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 to3.5 (last paragraph). Turbid samples do not cause interferences with the determination. In the event of coloured samples, check wheth
46、er 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 with the evaluation (according to3.7). The interlaboratory trial (see clause 6 and Annex A) h
47、as shown that detergents in waste water can strongly influence the determination, because the foam produced in the flow system can disturb on the one hand the steam distillation of volatile phenols (phenol index after distillation, see clause4, and on the other hand the phase segmentation and phase
48、separation procedures (phenol index after extraction, see clause3). In general such interferences can easily be discovered. In the case of significant detergent content, this International Standard is only applicable for phenol mass concentrations above0,1mg/l. 3.3 Reagents Use only reagents of reco
49、gnized analytical grade quality. The reagent blank value shall regularly be checked (see3.6.3). The solutions used for the flow system shall be degassed. If not stated otherwise, it is recommended to degas the solutions under reduced pressure, because by this procedure the solutions are simultaneously purified. WARNING Phenol is toxic and can easily be absorbed through the skin. Chloroform is toxic and cancerogenic. Waste containing these substances should be disposed of appropriately. 3.3.1 Water, of
