EN ISO 11885:1997
(Main)Water quality - Determination of 33 elements by inductively coupled plasma atomic emission spectroscopy (ISO 11885:1996)
Water quality - Determination of 33 elements by inductively coupled plasma atomic emission spectroscopy (ISO 11885:1996)
Wasserbeschaffenheit - Bestimmung von 33 Elementen durch induktiv gekoppelte Plasma-Atom-Emissionsspektrometrie (ISO 11885:1996)
Diese Internationale Norm legt en Verfahren zur Bestimmung der gelösten oder partikulären Anteile sowie eine Gesamtbestimmung der folgenden Elemente in Roh-, Trink- und Abwasser fest: Alumium, Antimon, Arson, Beryllium , Bismut, Bor, Cadmium, Calcium, Chrom, Cobalt, Kupfer, Eisen, Blei, Lithium, Magnesium, Mangan, Molybdän, Nickel, Kalium, Selen, Silicium, Silber, Natrium, Strontium,Schwefel, Zinn, Titan, Wolfram, Vanadium, Zink und Zirconium
Qualité de l'eau - Dosage de 33 éléments par spectroscopie d'émission atomique avec plasma couplé par induction (ISO 11885:1996)
Kakovost vode - Določevanje 33 elementov z atomsko emisijsko spektroskopijo z induktivno sklopljeno plazmo (ISO 11885:1996)
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Wasserbeschaffenheit - Bestimmung von 33 Elementen durch induktiv gekoppelte Plasma-Atom-Emissionsspektrometrie (ISO 11885:1996)Qualité de l'eau - Dosage de 33 éléments par spectroscopie d'émission atomique avec plasma couplé par induction (ISO 11885:1996)Water quality - Determination of 33 elements by inductively coupled plasma atomic emission spectroscopy (ISO 11885:1996)13.060.50VQRYLExamination of water for chemical substancesICS:Ta slovenski standard je istoveten z:EN ISO 11885:1997SIST EN ISO 11885:1998en01-januar-1998SIST EN ISO 11885:1998SLOVENSKI
STANDARD
SIST EN ISO 11885:1998
SIST EN ISO 11885:1998
SIST EN ISO 11885:1998
SIST EN ISO 11885:1998
SIST EN ISO 11885:1998
INTERNATIONAL STANDARD IS0 11885 First edition 1996-12-15 Water quality - Determination of 33 elements by inductively coupled dasma atomic emission sDectroscow Qua/it6 de Yea u - Dosage de 33 Mments par spectroscopic d’6mission atomique avec plasma coup16 par induction Reference number IS0 11885: 1996(E) SIST EN ISO 11885:1998
ISO11885:1996(E) Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through IS0 technical committees. Each member body interested in a subject for which a technical committee has been estabiished has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. IS0 collaborates closely bkth the Enternationai Ekctrotechnicai Commission (IEC) on all matters of ekctrstechnical standardization. Draft International Standards adopted 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 I1 885 was prepared by Technical Committee lSO/TC 147, W&W quaMy, Subcommittee SC 2, Physical, chemical and biochemical methods. Annex A of this International Standard is for information only. 0 IS0 1996 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. International Organization for Standardization Case postale 56 l CH-1211 Geneve 20 l Switzerland Internet central @ isocs.iso.ch x.400 c=ch; a=400net; p=iso; o=isocs; s=central Printed in Switzerland ii SIST EN ISO 11885:1998
INTERNATIONAL STANDARD o IS0 IS0 11885: 1996(E) Water quality - Determination of 33 elements by inductively coupled plasma atomic emission spectroscopy 1 Scope 1.1 Field of application This International Standard specifies a method for the determination of dissolved, particulate or total elements in raw, potable and waste water for the following elements: aluminium, antimony, arsenic, barium, beryllium, bismuth, boron, cadmium, calcium, chromium, cobalt, copper, iron, lead, lithium, magnesium, manganese, molybdenum, nickel, phosphorus, potassium, selenium, silicon, silver, sodium, strontium, sulfur, tin, titanium, tungsten, vanadium, zinc, zirconium. Table 1 lists these elements along with the recommended wavelengths and typical estimated instrumental detection limits using conventional pneumatic nebulization. Actual working detection limits are sample-dependent and as the sample matrix varies, these concentrations can also vary. Because of the differences between various makes and models of satisfactory instruments, no detailed instrumental operating instructions can be provided. Instead, the analyst will need to refer to the instructions provided by the manufacturer of the particular instrument. 1.2 Interferences Table 2 lists elements and the most important spectral interferences at the wavelengths recommended for analysis. Several types of interference effects can contribute to inaccuracies in the determination of trace elements. They can be summarized as follows. a) Spectral interferences, categorized as: 1) overlap of a spectral line from another element; these effects can be compensated by utilizing computer correction of the raw data; 2) unresolved overlap of molecular band spectra; these effects can possibly be overcome by selection of an alternative wavelength. If the appropriate equipment is available, wavelength scanning can be performed to detect potential spectral interferences. b) Background influences, categorized as: 2) background contribution from continuous or recombination phenomena; 3) background contribution from stray light from the line emission of elements in high concentration. The effect of background interferences can usually be compensated by background correction adjacent to the analyte line. 1 SIST EN ISO 11885:1998
IS0 11885:1996(E) 0 IS0 Table 1 - Recommended wavelengths and typical detection limits Element Ag Al As B Ba Bi Ca Cd Wavelength nm 328,068 338,289 308,215 396,152 167,08 193,696 197,197 189,042 208,959 249,678 247,773 233,527 455,403 493,409 313,042 234,861 313,107 223,061 306,772 315,887 317,933 393,366 214,438 226,502 228,802 Limit of detection mg/l 0,02 0,02 W W 0,04 091 011 0,08 0,005 0,006 0,Ol 0,004 0,002 0,003 0,002 0,005 0,04 0,08 091 0,Ol 0,002 0,Ol 0,Ol 0,Ol Element MO Na Ni P Pb S Sb Se Si Sn Wavelength nm 202,030 204,598 589,592 588,995 330,237 231,604 178,287 213,618 214,914 177,428 220,353 283,306 182,036 180,669 206,833 217,581 196,026 203,985 251,611 212,412 288,158 235,848 189,980 Limit of detection mg/l 0,03 0,05 03 0,02 0,02 095 091 091 OS 02 0,07 095 OS 091 091 091 031 0,02 0,02 0,03 a1 61 co 228,616 0,Ol Sr 407,771 0,0005 421,552 0,Ol Cr 205,552 0,Ol 460,733 091 267,716 0,Ol 283,563 0,Ol Ti 334,941 0,005 284,325 0,Ol 336,121 0,Ol 337,280 0,Ol cu 324,754 0,Ol 368,520 0,Ol 327,396 0,Ol v 290,882 0,Ol Fe 259,940 0,02 292,402 0,Ol 238,20 310,230 0,Ol 311,071 0,Ol K 766,490 769,90 2 W 207,911 0,03 209,860 0,06 Li 460,286 099 239,709 0,06 670,784 0,002 222,589 0,06 202,998 0,06 MCI 279,079 0,03 279,553 0,0005 Zn 206,191 0,Ol 285,213 0,001 213,856 0,005 Mn 257,610 0,002 Zr 343,823 0,Ol 293,306 0,02 354,262 0,05 339,198 2 SIST EN ISO 11885:1998
0 IS0 IS0 11885: 1996(E) Table 2 - Spectral interferences Element Ag Wavelength nm 328,068 338,289 Interfering elements Cr Element MO Wavelength nm 202,030 204,598 Interfering elements Al, Fe Al 308,215 Mn, V, Fe 396,152 MO, Cu 167,08 Fe Na 589,592 588,995 330,237 Ar As B Ba Bi Ca Cd 193,696 197,197 189,042 208,959 249,678 247,773 233,527 455,403 493,409 313,042 234,861 313,107 223,061 306,772 315,887 317,933 393,366 214,438 226,502 228,802 Fe, Al Fe, Al Al Al, MO Fe, Cr Fe Fe, V V Fe cu Fe, V co Fe, V Fe Fe As, Co Ni P Pb S Sb Se Si Sn Sr Ti V W Zn 231,604 178,287 213,618 214,914 177,428 220,353 283,306 182,036 180,669 206,833 217,581 196,026 203,985 251,611 212,412 288,158 235,848 189,980 co I Cu, Fe, MO, Zn Cu, Al, Mg cu Al, Co, Ti Cr, MO Ca Cr, Mg, Co, Mn MO, Co co Cr cu Fe K Li Mg 228,616 205,552 267,716 283,563 284,325 324,754 327,396 259,940 238,20 766,490 769,90 460,286 670,784 279,079 279,553 285,213 Ti Fe, MO Mn, V Fe, MO Fe Ti, Fe co Mg, Ar Fe Fe 407,771 421,552 460,733 334,941 336,121 337,280 368,520 290,882 292,402 310,230 311,071 207,911 209,860 239,709 222,589 202,998 206,191 213,856 Ca, Cr, Si Co, Cr Fe, MO Fe, MO, Cr Fe, Mn, Ti, Cr cu Cr Cu, Ni, Fe Mn 257,610 Fe, MO, Cr Zr 343,823 293,306 Al, Fe 354,262 339,198 SIST EN ISO 11885:1998
IS0 11885:1996(E) 0 IS0 Physical interferences are generally considered to be effects associated with the sample nebulization and transport processes. Such properties as change in viscosity and surface tension can cause significant inaccuracies, especially in samples which may contain high concentrations of dissolved solids and/or acid. If these types of interference are operative, they will be reduced by dilution of the sample and/or utilization of standard addition techniques. Chemical interferences are characterized by molecular compound formation, ionization effects and solute vaporization effects. These effects are overcome by buffering of the sample matrix and by standard addition procedures (see 8.1.3.2). Whenever a new or unusual sample matrix is encountered, a series of tests should be performed prior to reporting concentration data for analyte elements. When investigating a new sample matrix, comparison tests can be performed using other analytical techniques, such as atomic absorption spectrometry. Serial dilution - If the analyte concentration is sufficiently high (minimally IO x the instrumental detection limit after dilution), an analysis of a dilution needs to agree within 5 % of the original determination (or within some acceptable control limit that has been established for that matrix). If not, a chemical or physical interference effect could be responsible. Calibration by standard addition (see 8.1.3.2) - A spike added to the original determination at a minimum level of 10 x the instrumental detection limit (maximum 100 x) needs to be recovered to within 90 % to 110 %, or within the established control limit for that matrix. If not, a matrix effect should be suspected. The use of a standard addition analysis procedure can usually compensate for this effect. 2 Normative reference The following standard contains provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the edition indicated was valid. All standards are subject to revision, and parties to agreements based on this standard are encouraged to investigate the possibility of applying the most recent edition of the standard indicated below. Members of IEC and IS0 maintain registers of currently valid International Standards. IS0 5667-3:1994, Water quality - Sampling - Par? 3: Guidance on the preservation and handling of samples. 3 Definitions For the purposes of this International Standard, the following definitions apply: 3.1 dissolved metals: Those metals in a water sample which will pass through a 0,45 pm membrane filter. 3.2 particulate metals: Those metals in a water sample which are retained by a 0,45 pm membrane filter. 3.3 total metals: Concentration of metals determined on an unfiltered sample following digestion (see 8.1.3), or the sum of the dissolved (see 8.1 .l) plus particulate metal concentrations (see 8.1.2). 3.4 instrumental detection limit: Concentration, equivalent to a signal due to the analyte, which is equal to three times the standard deviation of a series of ten replicate measurements of a reagent blank signal at the same wavelength. 3.5 sensitivity: Slope of the curve of the relationship between signal emission intensity and sample concentration. 3.6 instrument check standard: Multielement standard of known concentrations prepared by the analyst to monitor and verify instrument performance on a daily basis (see 5.7). 4 SIST EN ISO 11885:1998
0 IS0 IS0 11885: 1996(E) 3.7 interference check sample: Solution containing both interfering and analyte elements of known concentration that can be used to verify background and interelement correction factors. 3.8 independent calibration check: Solution, obtained from an outside source, having known concentration values to be used to verify the calibration standards. 3.9 reference standards: Series of known standard solutions used by the analyst for calibration of the instrument (i.e. preparation of the calibration curve). 3.10 linear dynamic range: Concentration range over which the analytical response remains linear. 3.11 reagent blank: Deionized water, containing the same acid matrix as the calibration standards, which is carried through the entire analytical scheme. 3.12 calibration blank: Deionized water acidified with nitric or hydrochloric acid. 3.13 method of standard addition: Analytical technique involving the use of the unknown analyte and the unknown analyte plus a known amount of standard analyte (see 8.1.3.2). 3.14 sample duplication: Analysis of two portions of the same sample. 4 Principle The basis of the method is the measurement of atomic emission by an optical spectroscopic technique. Samples are nebulized and the aerosol that is produced is transported to the plasma torch where excitation occurs. Characteristic atomic-line emission spectra are produced by a radio-frequency inductively coupled plasma (ICP). The spectra are dispersed by a grating spectrometer and the intensities of the lines are monitored by detectors. The signals from the detectors are processed and controlled by a computer system. A background correction technique is used to compensate for variable background contributions to the determination of trace elements. 5 Reagents WARNING - The toxicity of each reagent used in this method has not been precisely defined; however, each chemical compound needs to be treated as a potential health hazard. From this viewpoint, exposure to these chemicals to the lowest possible level by whatever means available is recommended. Preparation methods involve the use of strong acids, which are corrosive and cause burns. Laboratory coats, gloves and safety spectacles should be worn when handling acids. Toxic fumes are evolved by nitric acid. Always carry out digestion in a fume cupboard, as well as addition of acid to samples because of the possibility of toxic gases being released. The exhaust gases from the plasma should be ducted away by an efficient fume extraction system. 51 . General requirements NOTE - Standard stock solutions may be purchased or prepared from ultrahigh-purity grade chemicals. The content of the determinants in the water and reagents shall be negligibly low, compared with the concentrations to be determined. 5 SIST EN ISO 11885:1998
IS0 11885:1996(E) 0 IS0 All salts shall be dried for 1 h at 105 “C unless otherwise specified. 5.2 Nitric acid, p(HN0,) = 1,40 g/ml 5.3 Dihydrogen dioxide (hydrogen peroxide), H,O,, volume fraction 30 %. NOTE - On the determination of phosphorus, attention should be paid to a possible stabilization of hydrogen peroxide with phosphoric acid, as this will affect the phosphorous determination. 5.4 Sulfuric acid, p(H,SO,) = 184 g/ml. 5.5 Hydrochloric acid, c(HCI) = 0,2 mol/l. 5.6 Ammonium sulfate, (NH&SO,. 5.7 Element stock solutions Ag, Al, As, B, Ba, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, MO, Na, Ni, P, Pb, S, Sb, Se, Si, Sn, Sr, Ti, V, W and Zn at mass concentrations of 1 000 mg/l each. NOTE - ICP-AES element standard reference solutions with respective specifications which can be used as stock solutions are commercially available. They have been prepared according to particulars of the manufacturer. Normally, these stock solutions contain hydrochloric acid or nitric acid and have a shelf life of several months. Formulations for the preparation of element stock solutions are identified below. 5.8 Intermediate mixed standard solutions Prepare these as mixed element standards in 5 % nitric acid or 5 % hydrochloric acid (volume fraction). To ensure chemical compatibility use the combinations given in 5.8.1 to 5.8.6. On composing multielement reference solutions, the chemical compatibility and the possible hydrolysis of the initial compounds, as well as spectral interferences, shall be taken into account. In order to avoid interferences, the digestion reagents (e.g. nitric acid, sulfuric acid, aqua regia) shall be added to the reference solutions. 5.8.1 Multielement reference solution I p(Al, Be, Cd,
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