1、CEN EN*ISO 99b3-II 95 111 3404589 0326282 375 RBISH STANDARD Water quality Determination of alkalinity - Part 1. Determination of total and composite al kalini t y The European Standard EN IS0 9963-1 : 1995 has the status of a British Standard ICs 13.060.40 BS EN IS0 BS 6068 : Section 2.51 : 1996 99
2、63-1 : 1996 CEN ENUISO 99b3-3 95 = 3404589 O326283 O03 AmdNo. BS EN IS0 9963-1 : 1996 Date Text affected Committees responsible for this British Standard The preparation of this British Standard was entrusted by Technical Committee Em, Water quality, to Subcommittee EHBE, Physical, chemical and bioc
3、hemical methods, upon which the following bodies 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 Author
4、ities Department of the Environment (Water Directorate) Department of Me and industry (Laboratory of the Government Chemist) GAMBICA (BEAMA) Ltd. Industrial Water Society Insitution of Water and Environmental Management National Rivers Authority Royal Society of Chemistry Soap and Detergent Industry
5、 Association Society of Chemical Industry Swimming Pool and Allied Mes Association Ltd. Water Companies Association Water Research Centre Water Services Association of England and Wales This British Standard, having been prepared under the direction of the Health and hvironment Sector Board, was pub
6、lished under the authority of the Standards Board and comes into effect on 15 May 1996 O BSI 1996 The following BSI references relate to the work on this standard Committee reference EWZ Draft for comment 92150314 DC ISBN O 680 26293 O CEN EN*ISO 9963-1 95 3404587 OL2b284 T48 BS EN IS0 9963-1 : 1996
7、 Contents Committees responsible National foreword Page Inside front cover 11 Foreword 2 Method 1 Scope 2 Normative references 3 Definitions 4 Principle 6 Reagents 7 Sampling and sample treatment 8 Procedure 9 Expression of results 10 Testreport 6 APP- 3 3 3 4 4 5 5 5 6 7 Annexes A (informative) Inf
8、ormation on factors for the conversion of a3kalinity values to alteniative units 8 ZA (normative) Nonnative references to international publications with their relevant European publications 9 O BSI 1996 I CEN EN*ISO 9963-1 95 = 3404589 0126285 984 BS EN IS0 9963-1 : 1996 National foreword This Brit
9、ish Standard has been prepared by Subcommittee EH/3/2 and is the English language version of EN IS0 9963-1 : 1995 Water quality - Determination of alkalinity - Part 1 : Determination of total and composite alkalinity published by the European Committe for Standardization (GEN). It is identical with
10、IS0 9963-1 : 1994, published by the International Organization for Stanardization (ISO). Cross-references Publication referred to IS0 3696 : 1987 EN 25667-1 : 1993 (IS0 5667-1 : 1980) EN 25667-2 : 1993 (Is0 5667-2 : 1991) IS0 6107-2 : 1989 IEC 7462 : 1982 Corresponding British Standard BS 3978 : 198
11、7 Specification for water for laboratory use BS EN 25667 : 1993 Water quality. Sampling BS EN 25667-1 1994 Guidance on the des of sampling Prnmn=S BS EN 25667-2 : 1993 Guidume on sampling techniques BS 6068 Water quality Part 1 Glossary Section 1.2 : 1990 Additioncd terms relating to tgpes of watq a
12、nd treatment and storage of water and waste water) and terms used in sampling and analysis of water BS 6438 Electrochemical analyzers Part 2 : 1984 Method for specifying per$omnce of pH value analyzers Compliance with a British Standard does not of itself confer immunity from legal obligations. ii O
13、 BSI 19% CEN EN*ISO 9963-1 95 3404589 0326286 810 EXROPEAN flmm NORME EUROPENNE EuROP to assess the equivalent hydrogen carbonate, carbonate and hydroxide concentration of water. 3.3 phenolphthalein endpoint alkalinity; com- posite alkalinity (Ap): The measurement by titration to the phenolphthalein
14、 endpoint (pH 8,3) of that por- tion of alkalinity arbitrarily attributed to all the hydroxyl and half the carbonate content of a water. IS0 6107-21 NOTE 1 The alkalinity of water is primarily a function of the hydrogen carbonate, carbonate and hydroxide concen- CEN EN*ISO 9963-1 95 m 3404589 032628
15、9 52T m Page 4 EN IS0 9963-1 : 1995 trations. Other buffering substances D 90 % (VA4 ethanol and dilute with water to 200 ml f 4 ml. Mix well. 5.6 Bromocresol green-methyl red indicator sol- ution. Dissolve 0,200 g f 0,005 g of bromocresol green and 0,015 g i 0,002 g of methyl red in 100 ml f 4 ml o
16、f ethanol 90 % (VA4 ethanol. Store in an amber glass bottle. 5.7 Sodium thiosulfate solution, c(Na2S203.5H,0) x 0,l molll. Dissolve 2,5 g f 0,2 g of sodium thiosulfate pentahydrate (Na,S,O3.5H2O) in 100 mi f 5 ml of water. Store in an amber glass bottle in the refrigerator for a maximum of six month
17、s. 6 Apparatus Usual laboratory equipment and, in particular, the fol- lowing should be used. 6.1 Magnetic stirrer, and plastics-coated stirring bar. 6.2 pH-meter, with a compatible electrode system suitable for the measurement of pH to within f 0,05 pH units over the range 4 to IO, and a suitable t
18、itration vessel designed so that contact with air is minimized. The equipment shall be set up, calibrated (preferably using buffers with pH values 4, 7 and 91, and used according to IEC 746-2. 6.3 Precision burette, of capacity 10 ml, graduated in divisions of 0,02 ml, and conforming to the re- quir
19、ements of IS0 385-1. 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 remains inside the bottle. Ideally analyse the samples immediate
20、ly after collection. If this is not possible, store in a cool place. In order to avoid nitrification or scaling. Many types of samples are little affected during storage. Test for any effects of storage on the type of samples analysed. (See IS0 5667-1 and IS0 5667-2.) 8 Procedure Strongly coloured o
21、r turbid samples should be ana- lysed by the potentiometric method. 8.1 Potentiometric method Calibrate the pH-meter according to 6.2. NOTE 3 The potentiometric titration is free from interfer- ence caused by oxidizing agents, although difficulties in endpoint detection may be experienced in the pre
22、sence of organic substances. Soaps, oily substances, etc. may coat the glass electrode and cause a sluggish response. Addi- tional time should be allowed between titrant additions to let the electrode come to equilibrium, and the electrodes should be cleaned frequently. CEN EN*ISO 99b3-II 95 Page 6
23、EN IS0 9963-1 : 1995 8.1.1 Determination of composite alkalinity titratable to pH 8.3 (phenolphthalein alkalinity) NOTE 4 the titration of composite alkalinity can lower the results. Absorption of atmospheric carbon dioxide during Pipette 100 mi f 1 ml of sample (volume V4) into the titration vessel
24、. Place the vessel on a magnetic stirrer and dip a plasticscoated stirring bar and pHelectrodes into the solution. Start the stirrer motor and stir at a rate at which a vortex is just not perceptible. Measure the pH value of the sample and, if it is found to be 8,3 or less, record the composite alka
25、linity titratable to pH 8,3 as zero. If the alkalinity is in the range 4 mmol/l to 20 mmol/l, use 0.1 mol/l hydrochloric acid (5.3). If the alkalinity is in the range 0,4 mmol/l to 4 mmol/l, use 0,02 mol/l hydrochloric acid (5.4). Titrate the sample with the appropriate acid and note the volume V, i
26、n millilitres, of acid con- sumed. Retain the solution for use in the determination of the total alkalinity. 8.1.2 Determination of total alkalinity Continue to titrate the solution reserved from the de- termination of composite alkalinity titratable to pH 8,3 (see 8.1.1) with the appropriate hydroc
27、hloric acid sol- ution until the meter reads pH 4,5 f 0,05 (in the vi- cinity of pH 4,5, add the titrant drop by drop and allow at least 30 s for the electrodes to attain equilibrium with the solution). Note the total volume V6, in milli- litres, of acid required. 8.2 Visual method NOTE 5 Remove any
28、 free chlorine present by adding 0.1 mi of sodium thiosulfate colution (5.7) per 200 mi of sample. This procedure removes up to 1.8 mg/l of chlorine. 8.2.1 Determination of composite alkalinity titratable to pH 83 (phenolphthalein alkalinity) NOTE 6 the titration of composite alkalinity can lower th
29、e results. Absorption of atmospheric carbon dioxide during Pipette 100 ml f 1 mi of sample (volurne V4) into a 250 ml Erlenmeyer flask and add 0,l ml f 0,02 ml of phenolphthalein indicator solution (5.5). If a pink col- our is not obtained, regard the composite alkalinity titratable to pH 8,3 as zer
30、o. Titrate pinkcoloured samples with acid until the pink colour disappears. If the alkalinity is in the range 4 mmol/l to 20 mmol/l, use 0,l mol/l hydrochloric acid (5.3). If the alkalinity is in the range 0,4 mmol/l to 4 mmol/l, use 0,02 mol/l hydrochloric acid (5.4). Note the volume V, in milli- l
31、itres, of acid consumed. Retain the solution for use in the determination of the total alkalinity. 8.2.2 Determination of total alkalinity Add 0,l mi f 0,02 ml of bromocresol green-methyl red indicator solution (5.6) to the solution reserved from the determination of composite alkalinity titratable
32、to pH 8,3 (see 8.2.1). Continue to titrate with the appropriate hydrochloric acid solution until the colour changes from greenish-blue to grey. Note the total volume V, in millilitres, of acid consumed. 9 Expression of results 9.1 Calculation 9.1.1 Composite alkalinity titratable to pH 8,3 (phenolph
33、thalein alkalinity) c(HC1) x V5 x 1 O00 Ap = v4 where AP is the capacity to react with hydro- gen ions, expressed in millimoles per litre, of composite alkalinity titratable to pH 8,3; c(HCI) is the actual concentration, ex- pressed in moles per litre, of the hydrochloric acid solution (5.3 or 5.4)
34、used; v4 is the volume, in millilitres, of the test portion (normally 1 O0 mi); v5 is the volume, in millilitres, of hydrochloric acid solution (5.3 or 5.4) consumed to reach pH 8.3. 9.1.2 Total alkalinity c(HC1) x V, x 1 O00 AT = v4 where AT is the capacity to react with hydro- gen ions, expressed
35、in millimoles per litre, of total alkalinity titratable to PH 45; CEN EN*ISO 9963-3 95 3404589 O326292 O34 D Page 7 EN IS0 9963-1 : 1995 c(HCI) is the actual concentration, ex- pressed in moles per litre, of the hydrochloric acid solution (5.3 or 5.4) used; v4 is the volume, in millilitres, of the t
36、est portion (normally 1 O0 mi); v6 is the volume, in millilitres, of hydrochloric acid solution (5.3 or 5.4) consumed to reach pH 4,5. 10 Test report The test report shall include the following information: a) a reference to this part of IS0 9963; b) precise identification of the sample; c) the resu
37、lts, expressed in millinoles (H) per litre; d: any departure from the procedure specified or any other circumstmce that may have affected the results. CEN ENrISO 9963-3 95 3404589 0326293 T50 Page 8 EN IS0 9963-1 : 1995 Annex A (informative) Information on factors for the conversion of alkalinity va
38、lues to alternative units Alkalinity values may be expressed in alternative units. Factors for the conversion from millimoles per litre are given in table A.l. Table A.l b I Alternative unit for the expression of factor I results mmol/l CaCO, mg/l CaCO, mg/i HCO; Partc/l O0 O00 English degree (= 1 C
39、lark degree) German degree French degree U.S. degree 0.50 50 61 5.0 3.50 2,80 5.0 2,90 CEN EN*ISO 9963-1 95 = 3404587 0126274 997 Page 9 EN IS0 9963-1 : 1995 Annex ZA (normative) Normative references to international publications with their relevant European publications This European Standard incor
40、porates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate piaces in the text and the publications are iisted hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this Euro
41、pean Standard only when incorporated in it by amendment or revision For undated references the kst edition of the publication referred to applies (including amendments). IEC publication Year Title ENmD Year IS0 5667-1 1980 Water quality - Sampling - Part 1: Guidance EN 25667-1 1993 IS0 5667-2 1991 W
42、ater qualitp - Sampling - Part 2: Guidance EN 25667-2 1993 on the design of sampling programm on sampling !?chniques - CEN EN+ISO 99b3-1 95 m 3404589 0326275 823 m BS EN IS0 9963-1 : 1996 List of references See national foreword. O BSI 19% CEN EN+ISO 9963-3 95 3404589 0326296 7bT BS EN IS0 BS 6068 :
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