ISO-10304-2-1995.pdf
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1、INTERNATIONAL STANDARD IS0 10304-2 First edition 1995-04-01 Water quality - Determination of dissolved anions by liquid chromatography of ions - Part 2: Determination of bromide, chloride, nitrate, nitrite, orthophosphate and sulfate in waste water Qualit de I eau - Dosage des anions dissous par chr
2、omatographie des ions en phase liquide - Partie 2: Dosage des ions bromure, chlorure, nitrate, nitrite, orthophosphate et sulfate dans /es eaux u) 0.1 to 50 CD or UV (200 nm to 215 nm) Nitrite (NO,) 0,05 to 20 CD or UV (200 nm to 215 nm) Orthophosphate (PO:-) 0,l to 20 CD Sulfate CSO-) 0.1 to 100 CD
3、 NOTE - The working range is limited by the exchange capacity of the columns. 1.2 Interferences 1.2.1 Organic acids, such as monocarboxylic or dicarboxylic acids, can interfere with the determi- nation of inorganic anions. 1.2.2 In a buffered eluent (e.g. carbonate/hydrogen carbonate), the determina
4、tion will not be influenced by the sample pH in the range of pH 2 to pH 9. 1.2.3 Large concentration differences between the anions Br-, Cl-, NO, NO, PO:- and SOi- may lead to typical cross-sensitivity interferences caused by an insufficient separation. The respective concentrations given in table2
5、were typical for conductivity detectors and UV-detectors; no interferences could be observed with a sample volume of 50 1. The data given are valid only when the quality requirements specified for the columns are met (see clause 6). The determi- nation of chloride may be subject to interference from
6、 high fluoride concentrations. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/19/2007 05:54:27 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 10304-2:1995
7、(E) 0 IS0 Table 2 - Cross-sensitivity of anions Detection: conductivity (CD) and direct UVI Maximum Ratio of the mass tolerable absolute concentrations concentration of solute/interfering ion interfering ionsl) t-w/l Br-/Cl- I:500 Cl- 500 Br-/PO:- I:100 PO;- 100 Br-/NO; I:50 NO, 100 Br-/SO:- I:500 s
8、o:- 500 Br-/SO:- 1:502) Cl-/NO, I:50 NO, 5 Cl-/NO, 1:500 NO, 500 cl-/so:- I:500 so:- 500 NO;/Br- I:100 Br- 100 NO,/CI- I:500 (CD) Cl- 500 I:2 000 (UV) cl- 500 NO,/SO:- I:500 (CD) so:- 500 1 :I 000 (UV) so:- 500 NO,/SO:- 1:502) NO,/CI- I:250 (CD) Cl- (CD) 100 1 :lO 000 (UV) cl- (UV) 500 NO;/PO;- I:50
9、 PO;- 20 NO;/NO, I:500 NO, 500 NO;/SO:- I:500 (CD) so:- 500 I:1 000 (UV) so;- 500 PO:-/Br- I:100 Br- 100 Po;-/cI- I:500 Cl- 500 PO;-/NO, I:500 NO, 400 PO;-/NO, I:100 NO, 100 PO;-/so;- 1:500 so:- 500 PO;-/so;- 1:502) so;-/cl- I:500 Cl- 500 SO:-/NO, I:500 NO, 400 so:-/so;- 1:502) so:-/s,o;- I:500 so;-
10、/I- I:500 1) Dilute the sample if the interfering concentration is exceeded. 2) When it is present, SO:- will always interfere. 1.2.4 The determination of sulfate may be subject to interference by high iodide or thiosulfate concen- trations. Relations: SOi-/I- or SO:-/S,O:- or I-/S,Oz- = I:500 Cross
11、-sensitivities to other anions, such as Br-, Cl-, NO, NO, PO:- and SO:-, may occur, especially in the presence of sulfite ions whose retention strongly depends on the selectivity of the separating column used. Inorganic anions such as fluoroborate or chlorite can interfere with the determination of
12、the named in- organic anions. NOTE 1 The identification of some anions (e.g. nitrite) or the detection of interferences (e.g. fatty acids) can be fa- cilitated by using a conductivity detector and UV-detector placed in series. Anion combinations (e.g. Cl-/l-) which are not listed in table2 will not
13、interfere in the specified range of application. Solid particles and organic compounds (such as min- eral oils, detergents and humic acids) shorten the lifetime of the separating column and are therefore eliminated before the analysis is started (see clause 7). Sulfide ions can cause errors during t
14、he determination of sulfate; they are eliminated according to clause 7. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this part of IS0 10304. At the time of publication, the editions indicated were valid. All standar
15、ds are subject to revision, and parties to agreements based on this part of IS0 10304 are encouraged to investi- gate the possibility of applying the most recent edi- tions of the standards indicated below. Members of IEC and IS0 maintain registers of currently valid International Standards. IS0 566
16、7-l :1980, Water quality - Sampling - Part 1: Guidance on the design of sampling pro- gfammes. IS0 5667-2:1991, Water quality - Sampling - Part 2: Guidance on sampling techniques. IS0 5667-3:1994, Water quality - Sampling - Part 3: Guidance on the preservation and handling of samples. Copyright Inte
17、rnational Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/19/2007 05:54:27 MDTNo reproduction or networking permitted without license from IHS -,-,- Q IS0 IS0 10304-2: 1995(E) IS0 8466-1:1990, Water quality - C
18、alibration and evaluation of analytical methods and estimation of performance characteristics - Part 1: Statistical evaluation of the linear calibration function. IS0 10304-l : 1992, Water quality - Determination of dissolved fluoride, chloride, nitrite, orthophosphate, bromide, nitrate and sulfate
19、ions, using liquid chro- matography of ions - Part 1: Method for water with low contamination. 3 Principle Liquid chromatographic separation of ions by means of a separating column. Use of an anion exchanger as the stationary phase, and usually, aqueous solutions of salts of weak monobasic and dibas
20、ic acids as mo- bile phases (eluent, see 4.17). Conductivity and UV-detectors are used within this part of IS0 10304. When using conductivity detectors, it is essential that the eluents have a sufficiently low conductivity. For this reason, conductivity detectors are often com- bined with a suppress
21、or device (e.g. a cation exchanger) which decreases the conductivity of the eluent and converts the separated anions into their corresponding acids. UV-detection either measures the absorption directly (see table 1) or, in the case of anions which are transparent in the UV-range, measures the decrea
22、se in the background absorption caused by a UV-absorbing eluent (indirect measurement). If in- direct UV-detection is used, the measuring wave- length depends on the composition of the eluent. The concentration of the respective anions is deter- mined by a calibration of the overall procedure. Par-
23、ticular cases may require calibration by means of standard addition (spiking). If no suppressor device is used, it is essential that the conductivity of the eluent be as low as possible. NOTE 2 References covering this analytical technique are summarized in annex A of IS0 10304-I :I 992. 4 Reagents
24、Use only reagents of recognized analytical grade. Weigh with an accuracy of 1 % of the nominal mass. The water shall have an electrical conductivity of 0,45 pm. The increase of the elec- trical conductivity due to an uptake of carbon dioxide does not interfere with the determination. 4.1 Sodium hydr
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