1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN ISO 9377-2:2000 BS
2、6068-2.72:2000 Incorporating Corrigenda Nos. 1 and 2 The European Standard EN ISO 9377-2:2000 has the status of a British Standard ICS 13.060.50 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Water quality Determination of hydrocarbon oil index Part 2: Method using solvent ex
3、traction and gas chromatographyThis British Standard, having been prepared under the direction of the Health and Environment Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 December 2000 BSI 5 October 2001 ISBN 0 580 36664 2 BS EN ISO 9377-2
4、:2000 Amendments issued since publication Amd. No. Date Comments 13023 corrigendum No. 1 February 2001 13416 corrigendum No. 2 5 October 2001 Incorporating annex ZA. National foreword This British Standard is the official English language version of EN ISO 9377-2:2000. It is identical with ISO 9377-
5、2:2000. The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH/3/2, Physical, chemical and biochemical methods, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European commi
6、ttee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-re
7、ferences Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding European publications. The British Standards which implement international or European publications referred to in
8、this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. U
9、sers of British Standards are responsible for their correct application. This is one of a series of standards on water quality, others of which have been, or will be, published as Sections of BS 6068. The various Sections of BS 6068 are comprised within Parts 1 to 7, which, together with Part 0, are
10、 listed below. Part 0 Introduction Part 1 Glossary Part 2 Physical, chemical and biochemical methods Part 3 Radiological methods Part 4 Microbiological methods Part 5 Biological methods Part 6 Sampling Part 7 Precision and accuracy NOTE. The tests described in this British Standard should only be ca
11、rried out by suitably qualified persons with an appropriate level of chemical expertise. Standard chemical procedures should be followed throughout. Compliance with a British Standard does not itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an i
12、nside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to iv, pages 1 to 19, the annex ZA page, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued.EUROPEANSTANDARD NORMEEUROP
13、ENNE EUROPISCHENORM ENISO93772 October2000 ICS13.060.50 Englishversion WaterqualityDeterminationofhydrocarbonoilindexPart2: Methodusingsolventextractionandgaschromatography(ISO 93772:2000) QualitdeleauDterminationdelindicehydrocarbure Partie2:Mthodeparextractionausolvantet chromatographieenphasegaze
14、use(ISO93772:2000) WasserbeschaffenheitBestimmungdes KohlenwasserstoffIndexTeil2:Verfahrennach LsemittelextraktionundGaschromatographie(ISO9377 2:2000) ThisEuropeanStandardwasapprovedbyCENon4October2000. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgiv
15、ingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyo
16、therlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,N
17、etherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2000CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers
18、. Ref.No.ENISO93772:2000EgaPe2 INESO3977:20020 CORRECTED20010328 Foreword ThetextoftheInternationalStandardISO93772:2000hasbeenpreparedbyTechnical CommitteeISO/TC147“Waterquality“incollaborationwithTechnicalCommitteeCEN/TC 230“Wateranalysis“,thesecretariatofwhichisheldbyDIN. ThisEuropeanStandardshal
19、lbegiventhestatusofanationalstandard,eitherbypublication ofanidenticaltextorbyendorsement,atthelatestbyApril2001,andconflictingnational standardsshallbewithdrawnatthelatestbyApril2001. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimp
20、lementthisEuropeanStandard:Austria,Belgium, CzechRepublic,Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy, Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandtheUnited Kingdom. Endorsementnotice ThetextoftheInternationalStandardISO93772:2000wasapprovedbyCENasaEuropean Stan
21、dardwithoutanymodification. NOTE:NormativereferencestoInternationalStandardsarelistedinannexZA(normative). ENISO93772:2000Reference number ISO 9377-2:2000(E) INTERNATIONAL STANDARD ISO 9377-2 First edition 2000-10-15 Water quality Determination of hydrocarbon oil index Part 2: Method using solvent e
22、xtraction and gas chromatography Qualit de leau Dtermination de lindice hydrocarbure Partie 2: Mthode par extraction au solvant et chromatographie en phase gazeuse ENISO93772:2000ii ENISO93772:2000ISO -77392:(0002)Eiii Contents Page Foreword.iv 1 Scope 1 2 Normative references 1 3 Term and definitio
23、n .1 4 Interferences 2 5 Principle2 6 Reagents.2 7 Apparatus .4 8 Sampling and sample preservation .5 9 Procedure .5 10 Test report .9 11 Precision.10 Annex A (informative) Example of a column and a microseparator 11 Annex B (informative) Examples of gas chromatograms of mineral oil standard and wat
24、er samples 13 Annex C (informative) Determination of boiling range of a mineral oil from the gas chromatogram 18 Bibliography19 ENISO93772:2000ISO -77392:(0002)E iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bo
25、dies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental an
26、d non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives,
27、 Part 3. 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. Attention is drawn to the possibility that some of the elements
28、of this part of ISO 9377 may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 9377-2 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical method
29、s. ISO 9377 consists of the following parts, under the general title Water quality Determination of hydrocarbon oil index: Part 1: Method using solvent extraction and gravimetry Part 2: Method using solvent extraction and gas chromatography Annexes A, B and C of this part of ISO 9377 are for informa
30、tion only. ENISO93772:2000INTENRATIONAL TSANDADR ISO -77392:(0002)E1 Water quality Determination of hydrocarbon oil index Part 2: Method using solvent extraction and gas chromatography 1 Scope This part of ISO 9377 specifies a method for the determination of the hydrocarbon oil index in waters by me
31、ans 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 0,1 mg/l. The method is not applicable to the quantitative determination of the content of volatile
32、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 The mass concent
33、ration of animal and vegetable fat in the test sample should not exceed 150 mg/l, because at higher values the adsorption capacity of the clean-up column packing may not be sufficient. NOTE 3 In the case of highly polluted waste water, especially if containing a high amount of surfactants, a loss in
34、 recovery may occur. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this part of ISO 9377. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, pa
35、rties to agreements based on this part of ISO 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 ISO and IEC maintain
36、registers of currently valid International Standards. ISO 5667-3:1994, Water quality Sampling Part 3: Guidance on the preservation and handling of samples. ISO 8466-1:1990, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistica
37、l evaluation of the linear calibration function. 3 Term and definition For the purposes of this part of ISO 9377, the following term and definition applies. ENISO93772:2000ISO -77392:(0002)E 2 3.1 hydrocarbon oil index by GC-FID the sum of concentrations of compounds extractable with a hydrocarbon s
38、olvent, boiling point between 36 Ca n d 69 C, not adsorbed on Florisil 1) and which may be chromatographed with retention times between those of n-decane (C 10 H 22 ) and n-tetracontane (C 40 H 82 ) NOTE Substances complying with this definition are long-chain or branched aliphatic, alicyclic, aroma
39、tic 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. 5P r i n c i p l e The water samp
40、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
41、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 ISO 9377 be carried out by suitably qualified staff. It should be investigated w
42、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
43、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 Cto6 9 C. I
44、n case of a change of extracting agent, repeatability tests are necessary. 6.3 Sodium sulfate, anhydrous,Na 2 SO 4 . 6.4 Magnesium sulfate heptahydrate,Mg S O 4 7H 2 O. 1) Florisil is a trade name for a prepared diatomaceous substance, mainly consisting of anhydrous magnesium silicate. This informat
45、ion is given for the convenience of users of this part of ISO 9377 and does not constitute an endorsement by ISO of this product. ENISO93772:2000ISO -77392:(0002)E3 6.5 Mineral acid, e.g. hydrochloric acid , c(HCl) = 12 mol/l ( = 1,19 g/ml). 6.6 Acetone,C 3 H 6 O. 6.7 Florisil 1) ,g r a i ns i z e1
46、5 0 mt o2 5 0 m (60 mesh to 100 mesh), heated to 140 C for 16 h and stored in a desiccator. 6.8 Mixture of mineral oils. 6.8.1 Standard 2) 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
47、 (6.11.2) to give a 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 unresol
48、ved signals in the gas chromatogram. An example of this type is a lubricant without any additives, boiling range 325 Cto4 60 C. 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 (6.11.2). The following concentrations may be suitable: 0 (blank), 0,2 mg/ml, 0,4 mg/ml, 0,6 mg/ml, 0,8 mg/ml and 1,0 mg/ml. Highe
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