1、- - STD*BSI BS EN L233-ENGL 1777 Lb24bbS 0585478 111111 BRITISH STANDARD Water quality - Determination of chromium - Atomic absorption spectrometric methods it it rn The European standard EN 1233 : 1996 has the status of a British Standard ICs 13.060.01 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PE
2、RMITTED BY COPYRIGHT LAW BS EN 1233 : 1997 BS 68: Section 2.38 : 1997 STD-BSI BS EN 1233-ENGL I997 Lb2Libb9 0585Li79 380 D AmdNo. Date BS EN 1233 : 1997 Text affected Committees responsible for this British Standard The preparation of this British Standard was entrusted by Technical Committee Ew3, W
3、ater qmty, to Subcommittee Ew3/2, Physical, chemical and biochemical methods, upon which the following bodies were represente3 British Agrochemicals Association Ltd. British Ceramic Research British Gas pic British Soft Drinks Association Ltd. Chemical Indusries Association Convention of Scottish Lo
4、cal Authorities Department of the Environment (Water Directorate) Environment agency GAMBICA (BEAMA LM.) Indusird Water Society Laboratory of the Government Chemist Royal Society of Chemistry Soap and Detergent Industry Association Society of Chemical Industty Swimming Pool and AUied “kades Associat
5、ion Ltd. Water Companies Association Water Research Centre Water Services Association of England and Waies This British Standard, having been prepared under the direction of the Health and Environment Sector Board, was pubiished under the authority of the Standards i3oard and comes inta effect on 16
6、 January 1997 O BSI 1997 The foiiowing BSI references reiate ta the work on this Standard: Committee reference EHMZ Draft for comment 93/508226 DC ISBN O 680 26789 X * M * STD-BSIBS EN 1233-ENGL I777 162Libb9 0585500 722 BS EN 1233 : 1997 Contents Committees responsibe page inside hnt cover Nationai
7、 foreword ii Foreword 2 Method introduction 1 scope 2 Normative references 3 Determination of chromium by flame atomic absorption spectromebiy 4 Annex A sediment samples 8 hbles 1 precision daa for clause 3 5 Determination of chromium by eledrothermai atomization atomic absorption spectrometry 6 (in
8、formative) information on prekatment and digestion of sludge and 2 Interferingions 3 Precision data for clause 4 5 7 Q BSI 1997 i STD.BSI BS EN 1233-ENGL I777 M Ibi9bb7 0585501 8b7 M BS EN 1233 : 1997 National foreword This British Standard has been prepared by Technid committee EH and is the Englis
9、h language version of EN 1233 Water quuLity - DetemLinat.ion of chmium - Atomic absolption spectrmne methods, published by the European Committee for Standardization (CEN). It supersedes BS 6068 : Section 2.38 : 1990, which is withdrawn. NOTE. The tests described in this British Standard should oniy
10、 be carried out by suitably qualied persons with an appropriate level of chemical expertise. Standard chemical procedures should be followed throughout Cross-references Publication referred to Corresponding British Standard BS 6068 Water quality Part 6 Sampling Section 6.2 : 1991 Guidance on samplin
11、g techniques Section 6.3 : 1996 Guidame on ule pre-sermtm and handling of samples EN 25667-2 : 1993 Is0 56673 : 1994 Compliance with a British Standard does not of itself confer immunity from legal obligations. ii O BSI 1997 STD.BSI BS EN 1233-ENGL L777 Lb24bbS 0585502 7T5 EUROPEAN SIANDARD NORME EU
12、R0PEE”E EUROP- NOEWI EN 1233 July 1996 ICs 13.060.40 Descriptors: water, quality, chemical analysis, determination of content, chromium, atomic absorption spedmmetry Eh- for example: pipette 1,0 ml, 2,6 ml, 5,O ml, 10,O ml and 20,O ml of chromium standard solution (see 3.2.7.2) into a series of 100
13、ml volumetric flasks. Add to each fhsk depending on the pretreatment (see 3.4.2 and 3.4.3) 10 ml or 2 ml of nitric acid (see 3.2.3) respectiveiy and 10 ml of lanthanum chIoride solution (see 3.2.6), dilute to the mark with water and mix These solutions correspond to chromium concentmiions of 0,50 mg
14、/i, 1,25 mgil, 2,50 ma, 5,00 mg/l and 10,O mg/i respectively Proceed accordingly for other concentration ranges of interest. 3.6.3 Cdbration Set up the instrument in accordance with the manufacturers instructions (at wavelength A = 357,9 nm) using a nitrous oxiddacetylene flame. Aspirate a calibrati
15、on solution (see 3.6.2) and optimize the aspiration, the burner height and the flame conditions. Aust the response of the instrument to zero absorbance with wateE In tum, aspirate the set of calibration solutions (see 3.6.2) and the blank solution (see 3.6.1). Plot a graph having the chromium concen
16、trations of the calibration solutions in milligrams per litre as abscissa and the corresponding absorbance dues as ordinate. Alternatively, data processing facilities can be used to equate the concentnition against the absorbance. 3.6.4 lht portiun measurement Aspirate the prepared test portion (see
17、 3.4.2 or 3.4.3) into the flame and measure the absorbance for chromium. After each measurement aspirate water and readjust the zero, if necessarJT O BSI 1997 STD-BSI BS EN L233-ENGL 1777 Lb24bb7 O58550b 390 Ion Mate Chioride sodium Potassium Magnesium Calcium 3.6 Expression of results 3.6.1 By refe
18、rence to the calibration graph obtained (see 3.6.3) or data processing faciities used, determine the concentration of chromium corresponding to the absorbances of the test portion (see 3.6.4) and of the biank solution (see 3.6.1). Calculate the concenimiion of chromium of the sample using the equati
19、on (As - AS0)VW VFJJ P= where: Concentration Ion Concentration mg/i mp/i 10 000 Iron 500 12000 Nickel 100 9OOO Copper 100 9000 Cobalt 100 2000 Aluminium 100 2000 zinc 100 p As is the absorbance of the test portion; Asois the absorbance of the blank; Vp is the volume of the acidified sample in accord
20、ance with 3.4.2 or 3.4.3, respectively, in millilitres; b is the sensitivity (slope of the calibration graph) in litres per milligram; Vw is the volume of the test portion according to 3.4.2 or 3.4.3 respectiva, in mjililitres. is the chromium concentration of the sample, in milligrams per litre; Ty
21、pe of sample Standard solution Water with added concentration 3.6.2 Precision data An interlaboratory test carried out in January 1985 yielded the data given in table 1. The standard solution used was made hm deionized water, spiked with chromium. The water used was a municipai, biologia is the numb
22、er of measured dues (without outliers); is the concentration of samples, in micrograms per litre; is the overall mean, in micrograms per litre; is the recovery rate, in percent; is the repeatability standard deviation, in micrograms per litre; is the repeaiabiity variation coefficient, in percent3 i
23、s the reproducibility standard dewon, in micrograms per iit1-6 is the reproducibility variation coefficient, in percent. O BSI 1997 STD-BSI BS EN L233-ENGL 1997 Lb24bby 0585507 05T Page 8 ENl233:1996 Annex A (Mormative) Information on pretreatment and digestion of sludge and sediment samples A.l Pre
24、treatment of sludge and sediment samples After sampling, the sludge and sediment samples are stred in the original bottles (see 3.4.1) in a refrigerator, or frozen until further treatment. If the determination is to be carried out on a dry residue, the sample is preferably freeze dried, or aiternati
25、vely dried at 105 C f 2 “C for about 24 h The dried sample is homogenized. NOTE. Dried sludges and sediments may be hygroscopic, and should therefore be dried again prior to anaiysis if stored for a very long time. A2 Digestion As an aiternative for the digestion described in 3.4.2, the following me
26、thod can be used. ilansfer a precisely weighed amount of the samples to the dgestion flask (a colourless bottle made of heat-resistant glass or an equivalent glass quality), volume about 100 mL The bottle and the screw cap shail withstand at least a pressure of 200 kpa (120 OC). The largest permissi
27、ble amount of sample is 1 g of dried material, or the equivalent amount of wet sample. Add 20 ml of nitric acid (see 3.2.3). Close the digestion flask tight Fax: O181 996 7048. Subscribing members of BSI are kept up to date with standards developments and receive subslmtial discounts on the purchase
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29、odies. Except as pennittixi under the Copyright, Designs and Patents Act 1988 no errtract may be reproduced, stored in a retried system or transmitted in any form or by any means - electronic, photocopying, recording or otherwise - without prior written permission from BSI. This does not preclude th
30、e j-ee use, in the com of implementing the standard, of necessary details such as symbols, and size, type or grade designations. If these details are to be used for any other purpose than impiementalion then the prior written permission of BSI must be obtained. if permision is granted, the terms may include royaity payments or a licensing rgreement. Details and advice can be obtained from the Copyright Manager, BSI, 389 Chiswick High Road, London W4 4A.L otherwiserequ ISBN O 680 26789 X EW2