1、- CEN EN*ISO 99b3-2 95 3404589 DL24000 493 I BS EN IS0 BS 6068 BRITISH STANDARD 9963-2 : 1996 I Section 2.52 : 11996 Water quality Determination of alkalinity - Part 2. Determination of carbonate alkalinity The European Standard EN IS0 %W2 : 1995 has the status of a British Standard I ICs 13.060.40
2、NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGH LAW CEN ENxISO 9963-2 95 m 3404589 OI12400L 32T m BS EN IS0 9963-2 : 1996 This British Standard, having been prepared under the direction of the Health and Environment Sector Board, was published under the authority of the Standards B
3、oard and comes into effect on 15 April 1996 O BSI 1996 Cornmittees responsible for this British Standard The preparation of this British Standard was entrusted by Technical Committee Ew3, Water quaity, to Subcommittee Ew312, Physical, chemical and biochemical methods, upon which the following bodies
4、 were represented: The Association of the Laboratory Supply Industry British Agrochemicals Association Ltd. British Ceramic Research British Gas plc British Soft Drinks Association Ltd. Chemical Industries Association Convention of Scottish Local Authorities Department of the Environment (Water Dire
5、ctorate) Department of We and Industry (Labomq of the Government Chemist) GAMBICA (BElMA) Ltd. Industrial Water Society Institution of Water and Environmental Management Nationai Rivers Authority Royal Society of Chemistry Soap and Detergent Industry Association Society of Chemical Indw Swimming Poo
6、l and Alied Wes Association Ltd. Water Companies Association Water Research Centre Water SeMces Association of England and Wales Amendments issued since publication Amd. No. Date I Te*affected I l The following BSI references reiate to the work on this standard Committee reference EW2 Draft for comm
7、ent 92/53921 ISBN O 580 26292 2 I I CEN EN*ISO 99b3-2 95 3404589 03i2La092 2bb BS EN IS0 9963-2 : 1996 Contents page Committees responsible Inside front cover Nationai foreword ii Foreword 2 Guide 1 Scope 2 Normative references 3 Definition 4 Principle 6 Reagents 4 6 APP- 7 Sampling and sample treat
8、ment 8 Procedure 5 5 6 9 Expression of results 6 10 l is the mass, in grams, of sodium carbonate taken for the preparation of solution 5.4; is the volume, in millilitres, of sodium carbonate solution (5.4) taken for titration (normally 2,O mi); is the volume, in millilitres, of hydrochloric acid sol
9、ution (5.5) con- sumed in the titration of the sodium carbonate solution (5.4); is the volume, in millilitres, of hydrochloric acid solution (5.5) con- sumed in the blank titration. 6 Apparatus Usual laboratory equipment and, in particular, the fol- lowing should be used. 6.1 Burette, preferably of
10、total capacity 10 ml, graduated in divisions of 0.02 ml, and conforming to the requirements of IS0 385-1. 6.2 Titration vessel, use either a glass filter funnel with a porosity of 2-3 and a volume of about 75 ml, or a gas distribution tube for dipping into the titration vessel (an Erlenmeyer flask w
11、ith a volume of 100 ml). 6.3 pH-meter, with a compatible electrode system suitable for the measurement of pH to within - + 0,05 pH units over the range 3 to 10, for use when the endpoint determination is to be made using a pH-meter. The equipment shall be set up, calibrated, and used according to IE
12、C 746-2. Alternatively, a titrator fulfilling these specifications can be used. 7 Sampling and sample treatment Collect samples in clean polyethylene or borosilicate glass bottles with a volume of at least 100 ml. Fill the bottle completely with the sample and insert the stopper so that no air remai
13、ns inside the bottle. Ana- lyse the samples immediately after collection. If this is not possible, store the samples at a temperature of 4 “C to 8 OC in order to avoid nitrification or scaling. (See IS0 5667-2.) Page 6 EN IS0 9963-2 : 1996 8 Procedure Mount the components according to figure 1. NOTE
14、 1 Coloured samples interfere with the indicator endpoint determination. Such samples should be analysed using a pHmeter. 8.1 Endpoint detection with a pH-meter Set the gas flow (5.2) to the titration vessel (6.2) at a rate that produces abundant bubbles and transfer 50,O ml f 0,l ml of sample (volu
15、me V4) to the vessel. Inseri the pH electrodes and titrate slowly with hydrochloric acid (5.5) to a pH value of 5,4. The pH value has to be stable for at least 30 s, if not continue the titration. Note the volume V, in millilitres, of acid consumed. If the volume of acid consumed exceeds 10 ml, take
16、 a smaller volume of the sample (Vs) and dilute to 50 ml f 5 ml with water (5.1). In this case, the vol- ume of acid consumed shall be not less than 3 ml. 8.2 Endpoint detection with indicator Set the gas flow (5.2) to the titration vessel (6.2) at a rate that produces abundant bubbles and transfer
17、50,O ml f 0.1 ml of sample (volume V4) to the vessel. Add three drops of indicator and titrate slowly with hydrochloric acid (5.5) until the colour changes to grey with a trace of red. The colour has to remain for at least 30 s, if not continue the titration. Note the vol- ume V5, in millilitres, of
18、 acid consumed. If the volume of acid consumed exceeds 10 ml, take a smaller portion of the sample and dilute to 50 ml f 5 ml with water (5.1). In this case, the vol- ume of acid consumed shall be not less than 3 mi. 8.3 Blank sample Titrate 50 ml of water (5.1 in the same way as for the sample. Per
19、form at least three titrations and calculate the mean value (volume Ve). 9 Expression of results 9.1 Calculation Calculate the concentration of alkalinity, expressed in millimoles per litre, using the equation c(HCI)(V5 - Va) x 1 O00 v4 A= where A is the alkalinity of the sample, ex- pressed in mill
20、imoles per litre; c(HCI) is the concentration, expressed in moles per litre, of the hydrochloric acid (5.5); is the volume, in millilitres, of the sample; is the volume, in millilitres, of hydrochloric acid (5.5) consumed by the sample; is the volume, in millilitres, of hydrochloric acid (5.5) consu
21、med by the blank sample (8.3). Report the result; expressed in millimoles per litre, to two significant digits. 9.2 Precision Two interlaboratory tests performed in 1988 and 1992 gave the results shown in table 1. In two international interlaboratory calibrations this method was used by one laborato
22、ry, with the results shown in tablez. At one laboratory, a control solution with a concen- tration of 0,200 mmol/l gave a mean value of 0,201 rnmol/l and a coefficient of variation of 2,O % (number of measuring values = 49). 10 Test report The test report shall include the following information: a r
23、eference to this part of IS0 9963; precise identification of the sample; the result, expressed in millimoles per litre to two significant digits; the endpoint detection used; any departure from the procedure specified or any other circumstance that may have affected the resu Its. CEN EN*ISO 9963-2 .
24、95 E 3404589 042YOLO 332 Number of laboratories 70 Drinking water SNV 3535 69 69 1 O0 1 o1 1 O0 1 o1 Type of water Reference Natural water ITM i993 Page 7 EN IS0 9963-2 : 1996 Mean cooffiC/.nt of mmol/l % 2 2.984 3.6 3 4,480 3.6 4 0,933 4.0 2 1,142 34 1 0,884 3.4 1 1,406 3,O 1 1,188 3.5 Of concentra
25、tion variation outliefs Table 1 - Preddon data Tvpe of water 91 05 Sample A Sample B 9206 Sample A Sample B Number of Number of Concentration, mmol/l laboratories outliers This method All methods R0fW.W NIVA 1991 20 1 0,298 0,300 20 1 0,358 0,358 NIVA 1992 20 13 0,042 0,047 20 13 0.1 51 O, 1 55 Tabl
26、e 2 - Comparison of resuits using this method with other methods for the determination of alkalinity CEN EN*ISO 99b3-2 95 = 3404589 02240LL 279 m Page 8 EN IS0 9963-2 : 1995 Alternative unit for the expression of rnUItS mmol/l Caco3 mg/l CaCO, English degree (= 1 Clark degree) German degree French d
27、egree U.S. degree Annex A (informative) Conversion factor 0,50 50 3.50 2.80 5,O 2.90 Information on factors for the conversion of alkalinity values to alternative units Alkalinity values may be expressed in alternative units. Factors for the conversion from millimoles per litre are given in tableA.l
28、. Table A.l CEN EN*ISO 9963-2 95 3404589 83214032 LO5 m Page 9 EN IS0 9963-2 : 1996 Annex B (informative) Bibliography l Convention on long-range transboundary air pol- lution, Infercalibrafion 9105. Programme Centre, Norwegian Institute for Water Research, Oslo. 2) Convention on long-range transbou
29、ndary air pol- lution, Infercalibrarion 9206. Programme Centre, Norwegian Institute for Water Research, Oslo. 3 STUMM, W. and MORGAN, J.J. Aquatic Chemis- try. J. Wiley (1981). 4 ITM 1993. Comparison of testing 1992-1. ton balance. (in Swedish with English summary.) Institute of Applied Environmenta
30、l Research, University of Stockholm, Sweden. 5 SNV 3535. Intercalibration 1988-1. Chemical analysis of drinking water. (in Swedish with English summary.) Swedish National Environ- mental Protection Agency. Annex ZA (normative) Normative references to international publications with their relevant Eu
31、ropean publications This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions
32、 of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including amendments). Publication Year Titie EN Year IS0 5667-1 1980 Water quality - Shmpling - EN 2
33、5667-1 1993 Part 1 : Guidance on the design of sampling Programmm Part 2 : Guidance on sampling techniques IS0 5667-2 1991 Water quality - Sampling - EN25667-2 1993 CEN EN*ISO 9963-2 95 D 3404589 01i240L4 T88 D BS EN IS0 9963-2 : 1996 List of references See national foreword O BSI 1996 CFM ENxISO 77
34、63-2 95 m 3404589 0324035 914 m BS EN IS0 BS 668 : Section 2.52 : 1996 9963-2 : 1996 BSI 389 Chiswick High Road London w4 4AL BSI - British Standards Institution BSI is the independent national body responsible for preparing British Standards. t presents the UK view on standards in Europe and at the
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