1、BRITISH STANDARDBS EN ISO 18856:2005 BS 6068-2.94: 2005Water quality Determination of selected phthalates using gas chromatography/ mass spectrometryThe European Standard EN ISO 18856:2005 has the status of a British StandardICS 13.060.50g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g4
2、4g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN ISO 18856:2005This British Standard was published under the authority of the Standards Policy and Strategy Committee on 17 October 2005 BSI 17 October 2005I
3、SBN 0 580 46760 0National forewordThis British Standard is the official English language version of EN ISO 18856:2005. It is identical with ISO 18856:2004.The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH/3/2, Physical, chemical and
4、biochemical methods, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary.Cross-referencesThe British Standards which implement international or European publications referred to in this document may be found in the BSI
5、 Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for it
6、s correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests i
7、nformed; monitor related international and European developments and promulgate them in the UK.Summary of pagespage, the EN foreword page, the ISO title page, pages ii to v, a blank page, pages 1 to 32, an inside back cover and a back cover.The BSI copyright notice displayed in this document indicat
8、es when the document was last issued.Amendments issued since publicationAmd. No. Date CommentsThis document comprises a front cover, an inside front cover, the EN title EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 18856August 2005ICS 13.060.50English VersionWater quality - Determination of
9、selected phthalates using gaschromatography/mass spectrometry (ISO 18856:2004)Qualit de leau - Dosage de certains phtalates parchromatographie en phase gazeuse/spectromtrie demasse (ISO 18856:2004)Wasserbeschaffenheit - Bestimmung ausgewhlterPhthalate mittelsGaschromatographie/Massenspektrometrie (I
10、SO18856:2004)This European Standard was approved by CEN on 20 July 2005.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliograph
11、ical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN me
12、mber into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithu
13、ania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All right
14、s of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 18856:2005: EForeword The text of ISO 18856:2004 has been prepared by Technical Committee ISO/TC 147 “Water quality“ of the International Organization for Standardization (ISO) and has been take
15、n over as EN ISO 18856:2005 by Technical Committee CEN/TC 230 “Water analysis”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by February 2006, and conflict
16、ing national standards shall be withdrawn at the latest by February 2006. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finl
17、and, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 18856:2004 has been approved by CEN as EN ISO 18856:2005
18、without any modifications. EN ISO 18856:2005Reference numberISO 18856:2004(E)INTERNATIONAL STANDARD ISO18856First edition2004-09-15Water quality Determination of selected phthalates using gas chromatography/mass spectrometry Qualit de leau Dosage de certains phtalates par chromatographie en phase ga
19、zeuse/spectromtrie de masse EN ISO 18856:2005ii iiiContents Page Foreword iv Introduction v 1 Scope 1 2 Normative references . 2 3 Principle . 2 4 Interferences 3 5 Reagents 3 6 Apparatus. 5 7 Sampling and sample pre-treatment. 7 8 Procedure. 7 9 Calibration 10 10 Calculation. 13 11 Expression of re
20、sults 15 12 Precision 15 13 Test report 15 Annex A (informative) List of phthalates 16 Annex B (informative) General remarks . 18 Annex C (normative) Precision data. 19 Annex D (informative) Examples of solutions (overview) 22 Annex E (informative) Example of equipment to avoid contaminations. 25 An
21、nex F (informative) Examples of suitable capillary columns 29 Annex G (informative) Example of gas chromatographic conditions. 30 Bibliography . 32 EN ISO 18856:2005iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member
22、 bodies). 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
23、 and 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 Directiv
24、es, Part 2. The main task of technical committees is to prepare International Standards. 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
25、casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 18856 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee
26、 SC 2, Physical, chemical and biochemical methods. EN ISO 18856:2005vIntroduction The user should be aware that particular problems could require the specification of additional marginal conditions. EN ISO 18856:2005blank1Water quality Determination of selected phthalates using gas chromatography/ma
27、ss spectrometry WARNING Persons using this International Standard should be familiar with normal laboratory practice. This International Standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate saf
28、ety and health practices and to ensure compliance with any national regulatory conditions. IMPORTANT It is absolutely essential that tests conducted according to this International Standard be carried out by suitably trained staff. 1 Scope This International Standard specifies a method for the deter
29、mination of phthalates in water after solid phase extraction and gas chromatography/mass spectrometry. This method is applicable to the determination of phthalates (see Table 1) in ground water, surface water, wastewater and drinking water in mass concentrations ranging from above 0,02 g/l up to 0,1
30、50 g/l, depending on the individual substance and the value of the blank. The applicability of this method to other phthalates not specified in Table 1 is not excluded, but it is necessary to determine its applicability in each case (see Annex A for the list of phthalates). General remarks concernin
31、g the recovery and use of internal standards is given in Annex B. Table 1 Phthalates determined by this method No Name Formula Abbreviation Molar mass g/mol CASanumber 1 Dimethyl phthalate C10H10O4DMP 194,2 131-11-3 2 Diethyl phthalate C12H14O4DEP 222,24 84-66-2 3 Dipropyl phthalate C14H18O4DPP 250,
32、3 131-16-8 4 Diisobutyl phthalate C16H22O4DiBP 278,4 84-69-5 5 Dibutyl phthalate C16H22O4DBP 278,4 84-74-2 6 Butyl benzyl phthalate C19H20O4BBzP 312,4 85-68-7 7 Dicyclohexyl phthalate C20H26O4DCHP 330,4 84-61-7 8 Di(2-ethylhexyl) phthalate C24H38O4DEHP 390,6 117-81-7 9 Di(n-octyl) phthalate C24H38O4
33、DOP 390,6 117-84-0 10 Didecyl phthalate C28H46O4DDcP 446,7 84-77-5 11 Diundecyl phthalate C30H50O4DUP 474,4 3648-20-2 aCAS: Chemical Abstracts System. EN ISO 18856:20052 2 Normative references The following referenced documents are indispensable for the application of this document. For dated refere
34、nces, only the edition cited applies. For undated references, the latest edition of the reference document (including any amendments) applies. ISO 5667-1, Water quality Sampling Part 1: Guidance on the design of sampling programmes ISO 5667-2, Water quality Sampling Part 2: Guidance on sampling tech
35、niques ISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples 3 Principle Extraction of the compounds from the water by solid-phase extraction. Then separation is accomplished using capillary columns by gas chromatography and followed by identification
36、and quantification of the phthalates by mass spectrometry. The principle of this method is outlined in Figure 1. Figure 1 Flowchart of the analysis EN ISO 18856:200534 Interferences IMPORTANT Due to their use as plasticizer agents, phthalates are ubiquitous. Therefore, pay special attention to avoid
37、 any contamination. 4.1 Interferences during sampling In order to avoid interferences and cross-contamination, do not use plastics materials (pipes, etc.). 4.2 Interferences during enrichment Commercially available adsorbent materials are often of varying quality. Considerable batch-to-batch differe
38、nces in quality and selectivity of this material are possible. The recovery of single substances may vary with concentration. Therefore, check the recovery regularly at different concentration levels and whenever new batches are used. Perform calibration and analysis with material from the same batc
39、h. Cross-contamination is likely to occur with laboratory air. Therefore, remove, as far as possible, plastics materials from the laboratory. Cleaning agents often contain phthalates and may severely contaminate the laboratory air if in use regularly. Therefore, refrain from using these agents durin
40、g application of this procedure. The use of plastics gloves during pre-treatment may increase the contamination. The maximum allowed blank level for each phthalate is 80 ng/l with reference to water (see Annex C). 4.3 Interferences in gas chromatography Phthalates may bleed from the septa of the inj
41、ector into the gas chromatograph, therefore use septa that are not likely to contaminate the system. Fittings of syringes, for example, or equipment and septa of the sampling bottles (see 6.7) may as well contain phthalates. Therefore make sure that uncontaminated septa are used. 5 Reagents Use, as
42、far as available, reagents of analytical quality, or better. Use only reagents with negligibly low concentrations of phthalates and verify by blank determinations and, if necessary, apply additional cleaning steps. 5.1 Water, having a negligibly low concentration of phthalates. In some cases, it may
43、 be preferable to use surface water instead of distilled water, because the concentration levels of the blank of surface water can be lower (9.3). Other waters with negligibly low concentrations of phthalates may be used as well. 5.2 Nitrogen, N2of high purity, at least a volume fraction of 99,9 %,
44、for drying and eventually for concentration by evaporation. 5.3 Helium, He of high purity, at least a volume fraction of 99,999 %. 5.4 Operating gases for gas chromatography/mass spectrometry, of high purity and in accordance with manufacturers specifications. 5.5 Ethyl acetate, highest purity, C4H8
45、O2. 5.6 Methanol, CH3OH. EN ISO 18856:20054 5.7 Isooctane, C8H18(2,2,4-trimethylpentane). 5.8 Quartz wool, heated to 400 C for at least 4 h. 5.9 Reversed-phase C18 (RP-C18) material. Alternative material and commercial glass cartridges may be used, provided the properties are similar to the material
46、 described in this International Standard and the properties are checked in accordance with 4.2. Check break-through rates prior to starting the analysis and each time a new batch of RP-C18 is used. 5.10 Aluminium oxide, alumina, Al2O3, neutral, 50 m to 200 m, heated to 400 C for at least 4 h. Bring
47、 the aluminium oxide to ambient temperature within 6 h. Store in a covered flask. Use within 5 d after baking. Alternative materials, such as Florisil1)or silica may be used, provided their properties and capacity to separate are similar to aluminium oxide and their properties are checked in accorda
48、nce with 4.2. 5.11 Internal standards, for example diallyl phthalate, DAlP, C14H14O4; D4-ring-deuterated dibutyl phthalate, “D4-DBP”, D4-C16H22O4; D4-ring-deuterated di(n-octyl) phthalate, “D4-DOP”, D4-C24H38O4, 13C(6 to 12)-labelled standard (as far as available). 5.12 Reference substances of the p
49、hthalates, mentioned in Table 1, with defined mass concentrations, for the preparation of reference solutions for the gas chromatographic procedure. 5.13 Solutions of single substances. In a 10 ml volumetric flask (6.15), dissolve, for example, 10 mg of each of the reference substances in ethyl acetate (5.5) and bring to volume with ethyl acetate (mass concentration: 1 g/l). Store the solutions in glass bottles at 18 C, protected from light, and check the concentration at least every three months. 5.14 Stock solution. In a 10 ml volumet
