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1、BRITISH STANDARD BS EN ISO 13395:1996 Water quality Determination of nitrite nitrogen and nitrate nitrogen and the sum of both by flow analysis (CFA and FIA) and spectrometric detection The European Standard EN ISO 13395:1996 has the status of a British Standard ICS 13.060 Licensed Copy: sheffieldun
2、 sheffieldun, na, Sat Nov 18 01:41:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 13395:1996 This British Standard, having been prepared under the direction of the Health and Environment Sector Board, was published under the authority of the Standards Board and comes into effect on 15 Novem
3、ber 1996 BSI 10-1998 The following BSI references relate to the work on this standard: Committee reference EH/3/2 Draft for comment 94/501676 DC ISBN 0 580 26092 5 Committees responsible for this British Standard The preparation of this British Standard was entrusted by Technical Committee EH/3, Wat
4、er quality, to Subcommittee EH/3/2, Physical, chemical and biochemical methods, upon which the following bodies were represented: British Agrochemicals Association Ltd. British Ceramic Research British Gas plc British Soft Drinks Association Ltd. Chemical Industries Association Convention of Scottis
5、h Local Authorities Department of the Environment (Her Majestys Inspectorate of Pollution) Department of the Environment (Water Directorate) Department of Trade and Industry (Laboratory of the Government Chemist) GAMBICA (BEAMA) Ltd. Industrial Water Society National Rivers Authority Royal Society o
6、f Chemistry Soap and Detergent Industry Association Society of Chemical Industry Swimming Pool and Allied Trades Association Ltd. Water Companies Association Water Research Centre Water Services Association of England and Wales Amendments issued since publication Amd. No.DateComments Licensed Copy:
7、sheffieldun sheffieldun, na, Sat Nov 18 01:41:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 13395:1996 BSI 10-1998i Contents Page Committees responsible Inside front cover National foreword ii Foreword 2 1Scope3 2Normative references 3 3Principle3 4Reagents3 5Apparatus6 6Checking the flow
8、system7 7Sampling and sample preparation7 8Interferences7 9Procedure7 10Evaluation9 11Expression of results9 12Precision9 13Test report13 Annex A (informative) Examples of flow injection systems (5.1) for the determination of nitrite(N) and nitrite/nitrate(N)14 Annex B (informative) Examples of cont
9、inuous flow systems (5.2) for the determination of nitrate(N) and nitrite/nitrate(N) 15 Annex C (informative) Example of a continuous flow system (so-called “macroflow”) (5.2) for the determination of 0,2 mg/l to 2 mg/l nitrite/nitrate(N)16 Annex D (informative) Bibliography17 Figure A.1 14 Figure B
10、.1 15 Figure C.1 16 Table 1 Options for preparing the solutions C and B in Figure A.1, Figure B.1 and Figure C.1 4 Table 2 Preparation of the calibration solutions for nitrite(N) 5 Table 3 Preparation of the calibration solutions for nitrite/nitrate(N) 6 Table 4 Statistical data for the determinatio
11、n of nitrite(N) with flow injection analysis (FIA) 10 Table 5 Statistical data for the determination of nitrite(N) with continuous flow analysis (CFA) 11 Table 6 Statistical data for the determination of nitrite/nitrate(N) with flow injection analysis (FIA)12 Table 7 Statistical data for the determi
12、nation of nitrite/nitrate(N) with continuous flow analysis (CFA) 13 List of referencesInside back cover Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:41:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 13395:1996 ii BSI 10-1998 National foreword This British Standard has been prep
13、ared by Subcommittee EH/3/2 and is the English language version of EN ISO 13395:1996 Water quality Determination of nitrite nitrogen and nitrate nitrogen and the sum of both by flow analysis (CFA and FIA) and spectrometric detection published by the European Committee for Standardization (CEN). It i
14、s identical with ISO 13395:1996 published by the International Organization for Standardization (ISO). 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 fol
15、lowed throughout. 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. Cross-references Public
16、ation referred toCorresponding British Standard ISO 3696:1987BS EN ISO 3696:1995 Water for analytical laboratory use. Specification and test methods BS EN 25667 Water quality. Sampling ISO 5667-1:1980Part 1:1994 Guidance on the design of sampling programmes ISO 5667-2:1991Part 2:1993 Guidance on sam
17、pling techniques ISO 5667-3:1994BS 6068 Water quality Part 6 Sampling Section 6.3:1996 Guidance on the preservation and handling of samples ISO 6777:1984BS EN 26777:1993 Water quality. Physical, chemical and biochemical methods. Determination of nitrite: molecular absorption spectrometric method Sum
18、mary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN title page, pages 2 to 18, 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 the amendment t
19、able on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:41:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 13395 July 1996 ICS:13.060.00 Descriptors: Water, quality, water pollution, water tests, chemical analys
20、is, determination of content, nitrogen, nitrates, nitrites. English version Water quality Determination of nitrite nitrogen and nitrate nitrogen and the sum of both by flow analysis (CFA and FIA) and spectrometric detection Qualit de leau Dtermination de lazote nitreaux et de lazote nitrique et de l
21、a somme des deux par analyse en flux (CFA et FIA) et dtection spectromtrique (ISO 13395:1996) This European Standard was approved by CEN on 1996-06-09. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the statu
22、s of a national 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 ve
23、rsion in any other 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, Denmark, Finland, France, Germany, G
24、reece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1996 Copyright r
25、eserved to CEN members Ref. No. EN ISO 13395:1996 E Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:41:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 13395:1996 BSI 10-1998 2 Foreword The text of the International Standard ISO 13395:1996 has been prepared by Technical Committee ISO/T
26、C 147, Water quality, in collaboration with Technical 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 January 1997 an
27、d conflicting national standards shall be withdrawn at the latest by January 1997. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Gr
28、eece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:41:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 13395:1996 BSI 10-19983 1 Scope This International Standard speci
29、fies a method for the determination of nitrite(N) (see note 2), nitrate(N) or the sum of both nitrite/nitrate(N), in various types of waters (such as ground, drinking, surface, and waste waters) in mass concentrations ranging from 0,01 mg/l to 1 mg/l for nitrite(N) and from 0,2 mg/l to 20 mg/l for n
30、itrite/nitrate(N), both in the undiluted sample. The range of application can be changed by varying the operating conditions. NOTE 1Seawater may be analysed with changes in respect to sensitivity and adaptation of the carrier solution and calibration solutions to the salinity of the samples. NOTE 2T
31、he following concise terms are used in the text of this International Standard: 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid
32、. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Stan
33、dards. ISO 3696:1987, Water for analytical laboratory use Specification and test methods. ISO 5667-1:1980, Water quality Sampling Part 1: Guidance on the design of sampling programmes. ISO 5667-2:1991, Water quality Sampling Part 2: Guidance on sampling techniques. ISO 5667-3:1994, Water quality Sam
34、pling Part 3: Guidance on the preservation and handling of samples. ISO 6777:1984, Water quality Determination of nitrite Molecular absorption spectrometric method. 3 Principle 3.1 Sum of nitrite(N) and nitrate(N), nitrite/nitrate(N) With flow injection analysis (FIA), the sample is fed into a conti
35、nuously flowing buffer solution (carrier stream) by means of an injection valve, or, with continuous flow analysis (CFA) being applied, it is continuously mixed with this buffer solution. Nitrate in the sample is reduced with metallic cadmium to nitrite4. Then, a phosphoric acid reagent solution tha
36、t is also flowing continuously is admixed. Nitrite that is initially present and nitrite resulting from the reduction of nitrate will diazotize sulfanilamide in acid solution to the diazonium salt which is then coupled with N-(1-naphthyl)ethylenediamine to form a red dye 567. Waste containing cadmiu
37、m in liquid or solid form shall be removed appropriately. 3.2 Nitrite(N) Nitrite(N) is determined, omitting the cadmium reduction, directly by the above-mentioned diazotization and coupling reaction8. The chemical reactions of the nitrite are identical with those in the manual procedure (see ISO 677
38、7). 3.3 Nitrate(N) The mass concentration of nitrate(N) is given by the difference: nitrite/nitrate(N) nitrite(N). 4 Reagents If not stated otherwise, only reagents of recognized analytical grade and water according to grade 1 of ISO 3696 shall be used. The blank value of the reagents shall be check
39、ed regularly (see 9.3). 4.1 Phosphoric acid (H3PO4), r = 1,71 g/ml. 4.2 Sulfanilamide (4-aminobenzenesulfonamide, C6H8N2O2S). 4.3 N-(1-naphthyl)ethylenediaminedihydrochloride N-(1-naphthyl)-1,2- diaminoethanedihydrochloride), C12H16N2Cl2. 4.4 Sodium nitrite (NaNO2), dried to constant mass at, for ex
40、ample, 150 C. 4.5 Potassium nitrate (KNO3), dried to constant mass at, for example, 150 C. 4.6 Imidazole (C3H4N2), for synthesis, or alternatively ammonium chloride (NH4Cl), dried to constant mass at 105 C (see note 3). 4.7 Hydrochloric acid I (HCl) concentrated, w = 37 %. nitrite(N):(mass concentra
41、tion of) nitrite, expressed as nitrogen nitrate(N):(mass concentration of) nitrate, expressed as nitrogen nitrite(N)/nitrate(N):(mass concentration of) the sum of nitrite(N) and nitrate(N) Licensed Copy: sheffieldun sheffieldun, na, Sat Nov 18 01:41:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN I
42、SO 13395:1996 4 BSI 10-1998 4.8 Hydrochloric acid II, c(HCl) = 1 mol/l. 4.9 Copper sulfate solution I, r(CuSO45H2O) = 2,5 g/l; this solution is stable. 4.10 Copper sulfate solution II, r(CuSO45H2O) = 20 g/l; this solution is stable. 4.11 Polyethyleneglycol dodecyl ether HO (CH2CH2 O)n C12H21, surfac
43、tant, u = 33 C to 41 C, solution, w = 30 %. The solution is stable for approximately 4 weeks. 4.12 Cadmium granulate (Cd), grain size, for example 0,3 mm to 1,5 mm (a minimum reduction capacity of 90 % shall be reached; see 5.1 and 5.2). 4.13 Imidazole stock solution, c = 0,25 mol/l. Dissolve, in a
44、beaker of nominal capacity 1 litre, 17,0 g of imidazole (4.6) in approximately 900 ml of water. While stirring with a magnetic stirrer, add hydrochloric acid I (4.7) and adjust, with the help of a pH electrode, the pH to 7.5. Transfer to a volumetric flask, of nominal capacity 1 000 ml, and dilute t
45、o volume with water. The solution is stable for 4 weeks if kept in a brown glass bottle at room temperature. 4.14 Buffer solution Mix 100 ml of the imidazole stock solution (4.13) with 100 l of copper sulfate solution I (4.9). Prepare the solution freshly before use. NOTE 3Alternatively an ammonium
46、buffer solution can be used, for example: 85 g of ammonium chloride (NH4Cl) should be dissolved in water and diluted to a volume of 1 000 ml, and the pH should be adjusted to approximately 7,5. 4.15 Carrier or dilution solutions, C and B in Figure A.1, Figure B.1 and Figure C.1. Table 1 shows some w
47、ell-known options for preparing these solutions. Prepare the solutions, containing the surfactant (4.11), freshly before use. Prior to use, solutions C and B for FIA shall be degassed, for example by membrane filtration (vacuum). Table 1 Options for preparing the solution C and B in Figure A.1, Figu
48、re B.1 and Figure C.1 4.16 Buffered copper sulphate solution Mix 20 ml of the copper sulfate solution II (4.10) and 20 ml of the imidazole stock solution (4.13) in a beaker of nominal capacity 50 ml. Prepare the solution freshly before use. 4.17 Reagent solution, R1 (in Figure A.1, Figure B.1 and Fi
49、gure C.1). Dissolve, in a volumetric flask of nominal capacity 500 ml, 5 g of sulfanilamide (4.2), 0,5 g of N-(1-naphthyl)ethylenediaminedihydrochloride (4.3) in water, add 50 ml of phosphoric acid (4.1), and dilute to volume. Stored in a brown glass bottle, the solution is stable for at least one week. NOTE 4For the preparation of this reagent solution, hydrochloric acid (4.7, 4.8) may be used instead of phosphoric acid, provided equivalent performance characteristics are obtained. The soluti