1、DEUTSCHE NORM Julv 2001 Water quality - Determination of hydrocarbon oil index Part 2: Method using solvent extraction and gas chromatography (IS0 9377-2 2000) Enalish version of DIN EN IS0 9377-2 DIN - EN IS0 9377-2 ICs 13.060.50 Wasserbeschaffenheit - Bestimmung des Kohlenwasserstoff-Index - Teil
2、2: Verfahren nach Lsemittelextraktion und Gaschromatographie (IS0 9377-2 : 2000) European Standard EN IS0 9377-2 : 2000 has the status of a DIN Standard. A comma is used as the decimal marker. This standard is part of the series Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlamm- untersuc
3、hung - Summarische Wirkungs- und Stoffkenngren (Gruppe H) (German standard methods for the examination of water, waste water and sludge - Parameters characterizing effects and substances (group HI. National foreword This standard has been published in accordance with a decision taken by CEN/TC 230 t
4、o adopt, without alteration, International Standard IS0 9377-2 as a European Standard. The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Committee). Expert assistance and specialized laboratories will be required to perform the anal
5、ysis described in this standard. Depending on the objective of the analysis, a check shall be made on a case-by-case basis as to whether and to what extent additional conditions will have to be specified. Standard methods published as DIN Standards are obtainable from Beuth Verlag GmbH, either indiv
6、idually or grouped in volumes. The standard methods included in the loose-leaf publication entitled Deutsche Einheitsvetfahren zur Wasser-, Abwasser- und Schlammuntersuchung will continue to be published by Wiley-VCH Verlag and Beuth Verlag GmbH. Standard methods or draft standards bearing the group
7、 title German standard methods for the examination of water, waste water and sludge are classified under the following categories (main titles): General information (group A) (DIN 38402) Sensory analysis (group B) (DIN 38403) Physical and physicochemical parameters (group C) (DIN 38404) Anions (grou
8、p D) (DIN 38405) Cations (group E) (DIN 38406) Substance group analysis (group F) (DIN 38407) Gaseous constituents (group G) (DIN 38408) Parameters characterizing effects and substances (group H) (DIN 38409) Biological-ecological methods of analysis (group M) (DIN 3841 O) Microbiological methods (gr
9、oup K) (DIN 3841 1) Continued overleaf. EN comprises 21 pages. No pari of this standard may be reproduced without the prior permission of Ref. No. DIN EN IS0 9377-2 : 2001 -0 V Deutsches Institut fur Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany, s the exclusive right of sale for G
10、erman Standards (DIN-Normen). English price group O9 Sales No. 1109 11 .o1 Page 2 DIN EN IS0 9377-2 : 2001 -07 Bio-assays (group L) (DIN 3841 2) Individual constituents (group P) (DIN 3841 3) Sludge and sediments (group S) (DIN 3841 4) Bio-assays with microorganisms (group T) (DIN 3841 5) In additio
11、n to the methods described in the DIN 38402 to DIN 38415 series of standards, there are a number of European Standards available, which also form part of the collection of German standard methods. Information on Parts of these series of standards that have already been published can be obtained from
12、 the offices of the Normenausschuss Wasserwesen, telephone (030) 26 O1 -25 49, or from Beuth Verlag GmbH, Burggrafenstrae 6, D-10787 Berlin. DIN EN IS0 5667-3 is the standard corresponding to International Standard IS0 5667-3 referred to in clause 2 of the EN. National Annex NA Standard referred to
13、(and not included in Normative references and Annex ZA) DIN EN IS0 5667-3 Water quality - Sampling - Part 3: Guidelines on preserving and handling water samples (IS0 5667-3 : 1994) EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN IS0 9377-2 October 2000 ICs 13.060.50 English version Water qualit
14、y - Determination of hydrocarbon oil index Part 2: Method using solvent extraction and gas chromatography (IS0 9377-2 : 2000) Qualit de leau - Dtermination de lindice hydrocarbure - Partie 2: Mthode par extraction au solvant et chromatographie en phase gazeuse Wasserbeschaffenheit - Bestimmung des K
15、ohlenwasserstoff-Index - Teil 2: Verfahren nach Lsemittelextraktion und Gaschromatographie (IS0 9377-2 : 2000) (IS0 9377-2 : 2000) This European Standard was approved by CEN on 2000-1 0-04. CEN members are bound to comply with the CENKENELEC Internal Regulations which stipulate the conditions for gi
16、ving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national stand- ards may be obtained on application to the Management Centre or to any CEN member. The European Standards exist in three official vers
17、ions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, th
18、e Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, the Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, and the United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Management
19、 Centre: rue de Stassart 36, 8-1050 Brussels O 2000. CEN - All rights of exploitation in any form and by any means reserved worldwide for CEN national members. Ref. No. EN IS0 9377-2 : 2000 E Page 2 EN IS0 9377-2 : 2000 Foreword International Standard IS0 9377-2 : 2000 Water quality - Determination
20、of hydrocarbon oil index - Part 2: Method using solvent extraction and gas chromatography, which was prepared by ISO/TC 147 Water quality of the International Organization for Standardization, has been adopted by Technical Committee CEN/TC 230 Water analysis, the Secretariat of which is held by DIN,
21、 as a European Standard. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, and conflicting national standards withdrawn, by April 2001 at the latest. In accordance with the CENKENELEC Internal Regulations, the natio
22、nal standards organizations of the follow- ing countries are bound to implement this European Standard: Austria, Belgium, the Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, the Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, and the United
23、Kingdom. Endorsement notice The text of the International Standard IS0 9377-2 : 2000 was approved by CEN as a European Standard without any modification. NOTE: Normative references to international publications are listed in Annex ZA (normative). Con tents Page Foreword 2 1 Scope 3 2 Normative refer
24、ences 3 3 Term and definition . 3 4 Interferences 4 5 Principle 4 6 Reagents . 4 7 Apparatus . 6 8 Sampling and sample preservation . 7 9 Procedure . 7 10 Test report . 1 1 I I Precision . 12 Annex A (informative) Example of a column and a microseparator 13 Annex C (informative) Determination of boi
25、ling range of a mineral oil from the gas chromatogram 20 Annex B (informative) Examples of gas chromatograms of mineral oil standard and water samples 15 Bibliography 21 Page 3 EN IS0 9377-2 : 2000 1 Scope This part of IS0 9377 specifies a method for the determination of the hydrocarbon oil index in
26、 waters by means of gas chromatography. The method is suitable for surface water, waste water and water from sewage treatment plants and allows the determination of a hydrocarbon oil index in concentrations above 0,l mg/l. The method is not applicable to the quantitative determination of the content
27、 of volatile mineral oil. However, on the basis of the peak pattern of the gas chromatogram, certain qualitative information on the composition of the mineral oil contamination can be derived. NOTE 1 For the determination of the mineral-oil content of soils and sediment. see ISO/TR 11046. NOTE 2 hig
28、her values the adsorption capacity of the clean-up column packing may not be sufficient. The mass concentration of animal and vegetable fat in the test sample should not exceed 150 mgll, because at NOTE 3 may occur. In the case of highly polluted waste water, especially if containing a high amount o
29、f surfactants, a loss in recovery 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this part of IS0 9377. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply
30、. However, parties to agreements based on this part of IS0 9377 are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of IS0 and
31、IEC maintain registers of currently valid International Standards. IS0 5667-3: 1994, Water quality - Sampling - Part 3: Guidance on the preservation and handling of samples. IS0 8466-1 :1990, Water quality - Calibration and evaluation of analytical methods and estimation of performance characteristi
32、cs - Part 1: Statistical evaluation of the linear calibration function. 3 Term and definition For the purposes of this part of IS0 9377, the following term and definition applies. Page 4 EN IS0 9377-2 : 2000 3.1 hydrocarbon oil index by GC-FID the sum of concentrations of compounds extractable with
33、a hydrocarbon solvent, boiling point between 36 OC and 69 OC, not adsorbed on Florisill) and which may be chromatographed with retention times between those of n-decane (C10H2*) and n-tetracontane (C40H82) NOTE Substances complying with this definition are long-chain or branched aliphatic, alicyclic
34、, aromatic or alkyl- substituted aromatic hydrocarbons. 4 Interferences Compounds of low polarity (e.g. halogenated hydrocarbons) and high concentrations of polar substances can interfere with the determination. Surface-active substances interfere with the extraction step. 5 Principle The water samp
35、le is extracted with an extracting agent. Polar substances are removed by clean-up on Florisil. The purified aliquot is analysed by capillary chromatography using a non-polar column and a flame ionization detector (FID). The total peak area between n-decane and n-tetracontane is measured. The concen
36、tration of mineral oil is quantified against an external standard consisting of two specified mineral oils, and the hydrocarbon oil index is calculated. It is absolutely essential that the test described in this part of IS0 9377 be carried out by suitably qualified staff. It should be investigated w
37、hether and to what extent particular problems will require the specification of additional marginal conditions. 6 Reagents All reagents shall be reagent grade and suitable for their specific purpose. The suitability of the reagents and solutions shall be checked by carrying out a blank test. 6.1 Wat
38、er for the preparation of solutions. Distilled water, or water from a generator of purified water capable of removing organic traces, for example using activated carbon. shall be used. 6.2 Extracting agent. Single hydrocarbon solvent or technical mixture of hydrocarbons, boiling range 36 “C to 69 “C
39、. In case of a change of extracting agent, repeatability tests are necessary 6.3 Sodium sulfate, anhydrous, Na2S04. 6.4 Magnesium sulfate heptahydrate, MgS04 . 7H20. 1) Florisil is a trade name for a prepared diatomaceous substance, mainly consisting of anhydrous magnesium silicate. This information
40、 is given for the convenience of users of this part of IS0 9377 and does not constitute an endorsement by IS0 of this product. Page 5 EN IS0 9377-2 : 2000 6.5 Mineral acid, e.g. hydrochloric acid , c(HCI) = 12 moll1 (p= 1,19 ghl). 6.6 Acetone, C3H60. 6.7 desiccator. Florisill), grain size 150 pm to
41、250 pm (60 mesh to 100 mesh), heated to 140 OC for 16 h and stored in a 6.8 Mixture of mineral oils. 6.8.1 Standard*) mixture. Weigh accurately equal amounts of two different types (type A and type B, both containing no additives) of mineral oil and add enough extraction solvent (6.1 1.2) to give a
42、total hydrocarbon concentration of about 10 mg/ml. Type A should show discrete peaks in the gas chromatogram. An example is diesel fuel without any additives. See EN 590 for further information. Type B should have a boiling range higher than that of type A and should have unresolved signals in the g
43、as chromatogram. An example of this type is a lubricant without any additives, boiling range 325 OC to 460 OC. 6.8.2 Calibration mixture. Prepare at least five different calibration solutions by diluting aliquots of standard mixture (6.8.1) with the extraction solvent (6.1 1.2). The following concen
44、trations may be suitable: O (blank), 0,2 mglml, 0,4 mglml, 0,6 mglml, 0,8 mg/ml and 1 ,O mglml. Higher concentrations may be advisable for other applications. Store the calibration mixture tightly sealed in a refrigerator (4 OC to 8 OC). The calibration mixtures are stable for up to six months. 6.8.
45、3 Quality Control (QC) standard. Prepare a standard solution according to 6.8.1 in acetone (see 6.6) with a mass concentration of e.g. 1 mglml. The exact concentration should be about a thousand times the desired application range. NOTE in acetone about tenfold before spiking the QC water. When usin
46、g a lubricant for QC, the stock solution is easily prepared in extracting agent (6.2), which is further diluted Store the solution tightly sealed in a refrigerator (4 “C to 8 OC). It is stable for up to six months. 6.9 Standard mixture of n-alkanes for system performance test. Dissolve n-alkanes wit
47、h even carbon numbers (Cz0, C40 and at least three further n-alkanes) in extracting agent (6.2) to give concentrations of approximately 50 pglrnl of the individual components. It may be necessary to use a different solvent, e.g. heptane, for the first solution; in this case dilute this first solutio
48、n with extracting agent (6.2). Store the standard mixture tightly sealed in a refrigerator. It is stable for up to six months 2) Standards are available from Fachgruppe 1.2 Bundesanstalt fr Materialforschung und -Prfung Richard-Willsttter-Strasse 1 I D-12489 Berlin, Germany This information is given
49、 for the convenience of users of this pari of IS0 9377 and does not constitute an endorsement by IS0 of these products. Page 6 EN IS0 9377-2 : 2000 NOTE 1 well as for the detector response. NOTE 2 the sample. This solution is used to verify the suitability of the gas chromatographic system for the resolution of n-alkanes as This solution is used to give information on the retention times of the n-alkanes to characterize the hydrocarbons in 6.10 Reference compounds. 6.10.1 n-Decane, C10H22. 6.1 0.2 n-Tetracontane, C40H82. 6.10.3 n-Eicosane, C20H42. 6.1 I Extraction solv
