1、BRITISH STANDARD Water quality - Determination of phenol index by flow analysis (FIA and CFA) The European Standard EN IS0 14402:1999 has the status of a British Standard ICs 13.060.50 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BS EN IS0 14402: 1999 BS 6068-2.68: 1999 BS
2、EN IS0 14402:1999 Environment Sector Committee, bd. No. Date authority of the Standards Committee and comes into effect on 15 November 1999 1 was published under the National foreword Comments O BSI 11-1999 ISBN O 680 36101 7 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN IS0 14402 September 1
3、999 ICs English version Water quality - Determination of phenol index by flow analysis (FIA and CFA) (IS0 14402:1999) Qualit de leau - Wtennlnation de lindice phend par analyse en flux (FIA et CFA) (IS0 10402:1Q99) Wasserbeschaffenheit - Besfimmung des Phenolindex mit der Flieanalytik (FIA und CFA)
4、(IS0 14402:1999) This European Standard was approved by CEN on 23 July 1999. CEN members are bound to comply with the CEWCENELEC Intemal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteraon. Up-to-date lists and bibliogra
5、phical 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, Geman). A version in any other language made by translation under the responsibility of a CE
6、N member into its own language and notified to Me Central Secretariat has the same status as ihe official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, enmark, Finland, France, Germany, Greece, Iceland, Ireland. Italy, Luxembourg, Netherlands, Norway, P
7、ortugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITIEE FOR STANDARDIZATION COMITE EUROPEEN DE NORMALISATION EUROPISCHES KOMITEE FUR NORMUNG Central Secrotariit: rue de Stassart, 36 6-1050 Brussels Q 1999 CEN All rights of exploitation in any form and by any means resewed worldwid
8、e for CEN national Members. Ref. No. EN IS0 14402:1999 E STD=BSI BS EN IS0 111402-ENGL 11999 Ip Lb211bbS 08311029 0311 EN IS0 14402:1999 Foreword The text of the International Standard IS0 14402:1999 has been prepared by Technical Committee iSO/TC 7 47 “Water qualiy“ in collaboration with Technical
9、Committee CEN/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
10、 the latest by March 2000. According to the CENKENELEC Internai 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
11、, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. NOTE FROM CENKS: 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 internatio
12、nal publications with their relevant European publications will be circulated with the German version. Endorsement notice The text of the International Standard IS0 14402:1999 was approved by CEN as a European Standard without any modification. STD-BSI BS EN IS0 LLILIUZ-ENGL 1999 Lb24bb9 08LL030 85b
13、 U EN IS0 14402:1999 INTERNATIONAL STAN DARD IS0 14402 First edition 1999-09-01 Water quality - Determination of phenol index by flow analysis (FIA and CFA) Qualit de leau - Dtermination de lindice phnol par analyse en flux (FIA et CFA) Reference number IS0 14402:1999(E) STD*BSI BS EN IS0 14402-ENGL
14、 1999 Is Lb24bbS OB11031 792 = EN IS0 14402:1999 Contents Page 1 scope 1 3 Determination of phenol index (without distillation) after extraction 3.1 Principle . 1 3.3 Reagents 2 2 Nomative references . 1 1 3.2 Interferences 1 3.4 Apparatus 4 3.5 Sampling 6 3.6 Procedure 7 3.7 Calculation of results
15、. 8 4 Determination of phenol index (without extraction) after distillation 9 4.1 Principle . 9 4.2 Interferences . 9 4.3 Reagents 9 4.4 Apparatus 10 4.5 Sampling 13 4.6 Procedure 13 4.7 Calculation of results . 14 5 Expression of results 14 6 Precision and accuracy . 14 7 Test report 14 Annex A (in
16、formative) Statistical data . 15 Bibliography 17 STD*BSI BS EN IS0 LqLi02-ENGL 1999 M Lb24bb7 0811032 b27 9 EN IS0 14402:1999 Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member bodies). The work of preparing Internatio
17、nal 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. International organizations, governmental and non-governmental, in liaison with SO,
18、 also take pari in the work. IS0 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISOAEC Directives, Part 3. Draft International Standards ad
19、opted 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. International Standard IS0 14402 was prepared by Technical Committee ISO/TC 147, Water quahty, Subcommitt
20、ee SC 2, Physical, chemical biochemical methods. Annex A of this International Standard is for information only. iii STD-BSI BS EN IS0 34402-ENGL 1997 1b24bbS 08LL033 5b5 EN IS0 14402:1999 Introduction Methods for determination of water quality using flow analysis and automatic wet chemical procedur
21、es are par- ticularly suitable for the processing of large sample series at a high analysis frequency. Differentiation is needed between flow injection analysis (FIA) l , 21 and continuous flow analysis (CFA) 3. Both methods include automatic dosage of the sample into a flow system (manifold) where
22、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 which un
23、der the specific reaction conditions form coioured condensation products. The analytical resuii 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 phenol
24、 index (without extraction) after distillation. It should be investigated whether and to what extent particular problems will require the specification of additional marginal conditions. iv - STDOBSI BS EN IS0 L4402-ENGL 3999 m 3ib211bb9 0833034 4T1 = EN IS0 14402:1999 Water quality - Determination
25、of phenol index by flow analysis (FIA and CFA) 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 of 0,Ol mgA to 1 mgA (in the
26、undiluted sample). In particular 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 clause 4 the determination of phenol index (without extraction) after distillation
27、 is given. 2 Normative 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 revisions of, any of these publications do not apply. However, partie
28、s 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 normative document referred to applies. Members of IS0 and IEC maintai
29、n registers of currently valid International Standards. IS0 3696:1987, Water for analytical laboratory use - Specification and test methods. IS0 5667-3:1994, Water qualify - Sampling - Part 3: Guidance on sample handling and preservation. IS0 6439: 1 990, Water quality - Determination of phenol inde
30、x - 4-Aminoantipyrine spectromefdc methods ater 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 pero
31、xodisulfate. Phenolic compounds in the sample 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 sepa
32、rated by a suitable phase separator (e.g. a hydrophobic semipermeable membrane), and the absorbance of the organic phase is measured spectrometrically in a flow spectrometer at 470 nm to 475 nm. More information on this analytical technique is given in the references 6 to 91. It is absolutely essent
33、ial that the test described in this International Standard be carried out by suitably qualified staff. 3.2 Interferences 32.1 Chemical interferences Under the prevailing reaction conditions, aromatic amines will also form condensation products with 4-aminoanti- pyrine, leading to positive bias. 1 -
34、STD-BSI BS EN IS0 111402-ENGL 1999 M Lb211bbS 0811035 338 M EN IS0 14402:1999 Interferences can occur when the sample, after the addition of the reagent solutions, does not reach a pH of 10,O to 105 in particular this may occur in the cases of strongly acidic, strongly alkaline and buffered samples.
35、 In these cases, the sample is adjusted to a pH between 5 and 7 prior to addition of the reagent solutions. Further information on interferences is given in 5. 39.2 Physical interferences arising from applying CFA and FIA if the samples contain particulate matter, refer to 3.5 (last paragraph). Turb
36、id 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 Fi1 and R2. The difference in response between the two measurements shall be take
37、n into account with the evaluation (according to 3.7). The interiaboratory trial (see clause 6 and annex A) has 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 p
38、henols (phenol index after distillation, see clause 4, and on the other hand the phase segmentation and phase separation procedures (phenol index after extraction, see clause 3). In general such interferences can easily be discovered. In the case of significant detergent content, this International
39、Standard is only applicable for phenol mass concentrations above 0,l mg/i. 3.3 Reagents Use only reagents of recognized analytical grade quality. The reagent blank value shall regularly be checked (see 3.6.3). The solutions used for the flow system shall be degassed. If not stated otherwise, it is r
40、ecommended 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 appropri
41、ately. 3.3.1 3.3.2 3.3.3 3.3.4 3.3.5 3.3.6 3.3.7 3.3.8 3.3.9 Water, of grade 1 in accordance with IS0 3696 Potassium hydroxide, KOH Sodium hydrogencarbonate, NaHC03 LEaminoantipyrine (4-amino-2,3-dimethyl-l -phenyl-3-pyrazolin-5-one), C1 fH13N30 Potassium peroxodisulfate, K2S208 Phenol, C6H50H Boric
42、 acid, H3B03 Ethanol, C2H50H, 96 Y mass fraction BPropanol, C3H70H, 100 % mass fraction 3.3.10 Sulfuric acid, p(H2S0,) = 1,84 mi 3.3.1 1 Hydrochloric acid, HCI, 50 % mass fraction 3.3.12 Potassium hydroxide solution, c(K0H) = 1 ,O moM 3.3.13 Buffer solution Dissolve in a 1 o00 ml graduated flask in
43、approximately 500 ml of water (3.3.1): 23 g of sodium hydrogencarbonate (3.3.3), 27 g of boric acid (3.3.7), and 35 g of potassium hydroxide (3.3.2) and make up to volume with water. The pH of the buffer solution is approximately 10,3. The solution is stable for 1 month. 2 STDOBSI BS EN IS0 14402-EN
44、GL 1449 9 Lb24bb9 OBL103b 27q EN IS0 14402:1999 3.3.14 Carrier solution (symbol C in Figure 1) Use water (3.3.1) degassed under reduced pressure. 3.3.15 4-Aminoantipyrine solution I (symbol R1 in Figures 1 and 2) Dissolve in a 100 ml graduated flask 0,5 g of 4-aminoantipyrine (3.3.4) in approximatel
45、y 50 ml of buffer solution (3.3.13), and make up to volume with buffer solution (3.3.13). Degas the solution, e.g. by membrane filtration. Prepare fresh solution every day. 3.3.16 Potassium peroxodisulfate solution (symbol R2 in Figures 1 and 2) Dissolve in a 100 ml graduated flask 5 g of potassium
46、peroxodisulfate (3.3.5) in approximately 90 ml of water (3.3.1), adjust to pH 11 with potassium hydroxide solution (3.3.12) and make up to volume with water. Degas the solution, e.g. by membrane filtration. Prepare fresh solution daily. 3.3.17 Chloroform, CHCI3 (symbol Org in Figures 1 and 2) Degas
47、the chloroform solution either by membrane filtration or for 3 min in an ultrasonic bath. 3.3.18 Phenol stock solution, p = 1 O00 mgA Dissolve in a 1 O00 ml graduated flask 1,000 g of phenol (3.3.6) in water (3.3.1) and make up to volume with water. Use only colourless phenol crystals. The cooled so
48、lution (2 OC to 5 OC) is stable for one month. 3.3.19 Phenol standard solution I, p = 10 mgA Pipette 1 mi of the stock solution (3.3.18) into a 100 ml graduated flask, and make up to volume with water (3.3.1). The cooled solution (2 OC to 5 OC) is stable for one week. 3.3.20 Phenol standard solution
49、 II, p = 1 mgA Pipette 10 ml of the standard solution I (3.3.19) into a 100 ml graduated flask, and make up to volume with water (3.3.1). The cooled solution (2 OC to 5 OC) is stable for one week. 3.3.21 Calibration solutions Prepare the calibration solutions according to the origin of the sample and the expected concentrations by diluting the phenol standard solution I or II respectively (3.3.1 9 or 3.3.20). Prepare a minimum of at least five calibration solutions per working range. Proceed as follows for working ranges I and II, if using e.g.
