BS PD ISO TS 17182-2014 Soil quality Determination of some selected phenols and chlorophenols Gas chromatographic method with mass spectrometric detection《土质 某些选定的酚和氯酚的测定 气相色谱与质谱检测.pdf

1、BSI Standards PublicationSoil quality Determination of some selected phenols and chlorophenols Gas chromatographic method with mass spectrometric detectionPD ISO/TS 17182:2014National forewordThis Published Document is the UK implementation of ISO/TS 17182:2014.The UK participation in its preparatio

2、n was entrusted to TechnicalCommittee EH/4, Soil quality.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisions ofa contract. Users are responsible for its correct application. The Bri

3、tish Standards Institution 2014.Published by BSI Standards Limited 2014ISBN 978 0 580 76247 5ICS 13.080.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This Published Document was published under the authority of theStandards Policy and Strategy Committee on 31 Dece

4、mber 2014.Amendments issued since publicationDate Text affectedPUBLISHED DOCUMENTPD ISO/TS 17182:2014 ISO 2014Soil quality Determination of some selected phenols and chlorophenols Gas chromatographic method with mass spectrometric detectionQualit du sol Dosage de quelques phnols et chlorophnols slec

5、tionns Mthode par chromatographie en phase gazeuse avec dtection par spectromtrie de masseTECHNICAL SPECIFICATIONISO/TS17182Reference numberISO/TS 17182:2014(E)First edition2014-12-15PD ISO/TS 17182:2014ISO/TS 17182:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2014All right

6、s reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from eit

7、her ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandPD ISO/TS 17182:2014ISO/TS 17182:2014(E)Contents PageForeword

8、 iv1 Scope . 12 Normative references 33 Principle 34 Interferences 34.1 Interference with sampling and extraction 34.2 Interference with GC-MS determination 45 Reagents 45.1 Products used in their commercially available form 45.2 Aqueous solutions 45.3 Standard solutions of phenols . 56 Apparatus an

9、d equipment 57 Sampling 68 Procedure. 68.1 Test portion 68.2 Dry matter content 68.3 Blank sample 68.4 Standard sample 68.5 Extraction 68.6 Acetylation 78.7 Gas chromatographic analysis . 78.8 Calibration 79 Calculation 89.1 Calculation of the content of substance i in the extract . 89.2 Calculation

10、 of the content of selected phenol soil sample per dry matter (mg/kg dry matter) . 910 Test report . 9Annex A (informative) Typical concentrations of the standard solutions .10Annex B (informative) Example of gas chromatographic conditions 11Bibliography .15 ISO 2014 All rights reserved iiiPD ISO/TS

11、 17182:2014ISO/TS 17182:2014(E)ForewordISO (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 ISO technical committees. Each member body interes

12、ted in a subject for which a technical committee has been established 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. ISO collaborates closely with the International Electrotechnical C

13、ommission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO document

14、s should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).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 f

15、or identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the

16、convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Fore

17、word - Supplementary information.The committee responsible for this document is ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics.iv ISO 2014 All rights reservedPD ISO/TS 17182:2014Soil quality Determination of some selected phenols and chlorophenols Gas chromato

18、graphic method with mass spectrometric detectionWARNING Phenols and chlorophenols are both toxic and corrosive and should be handled with care. Methanol and acetonitrile are toxic and acetic acid is corrosive. Latex or nitrile gloves and eye protection should be worn at all times. Spills should imme

19、diately be wiped up with adsorbent tissue and placed in sealed containers used for the disposal of toxic chemicals. Samples should be treated as toxic and harmful. Extreme care shall be taken through all steps of the extraction procedure, which shall be performed in a fume hood. All solvent wastes s

20、hall be collected and treated as hazardous waste. Thus, there is a contamination risk in the laboratory.1 ScopeThis International Standard describes the gas chromatographic determination of phenols, methyl phenols, di-methylphenols and tri-methylphenols (see Table 1) and selected chlorophenols (see

21、Table 2) by using mass spectrometric detection in soil samples. This method can also be used for other solid samples, such as sediments and solid wastes. This International Standard describes an acidic liquid extraction of soil, followed by acetylation and then liquid/liquid extraction. Determinatio

22、n takes place by gas chromatography and mass spectrometric detection.With this method, phenols and chlorophenols can be determined at the lowest of mass concentrations ranging from approximately 0,01 mg/kg to 0,1 mg/kg depending on the component sensitivity and the quantity of sample used. In some c

23、ases, complete separation of isomers cannot be achieved. Then the sum is reported.NOTE With this method, other higher methylated phenols can also be analysed provided that the suitability and the validity of the method is proven.Table 1 Target phenolic compounds with relevant mass fractions of respe

24、ctive acetylated compounds for MS-detectionCompound CAS-RNaChemical formulaAcetylated compoundsFragmentationb1stmass Relative intensity %2ndmass Relative intensity %phenol 108-95-2 C6H6O 94 100 66 262-methylphenol (o-cresol)95-48-7 C7H8O 108 100 107 683-methylphenol (m-cresol)108-39-4 C7H8O 108 100

25、107 854-methylphenol (p-cresol)106-44-5 C7H8O 108 100 107 922,3-dimethylphenol 596-75-0 C8H10O 122 90 107 1002,4-dimethylphenol 105-67-9 C8H10O 122 100 107 852,5-dimethylphenol 95-87-4 C8H10O 122 100 107 902,6-dimethylphenol 576-261-1 C8H10O 122 100 107 92aChemical abstract service registry number.b

26、Spectral database for organic compounds (SDBS).TECHNICAL SPECIFICATION ISO/TS 17182:2014(E) ISO 2014 All rights reserved 1PD ISO/TS 17182:2014ISO/TS 17182:2014(E)Compound CAS-RNaChemical formulaAcetylated compoundsFragmentationb1stmass Relative intensity %2ndmass Relative intensity %3,4-dimethylphen

27、ol 95-65-8 C8H10O 122 99 107 1003,5-dimethylphenol 108-68-9 C8H10O 122 100 107 682,3,5-trimethylphenol 697-82-5 C9H12O 136 87 121 1002,3,6-trimethylphenol 2416-94-6 C9H12O 136 90 121 1002,4,6-trimethylphenol 527-60-6 C9H12O 136 10 121 853,4,5-trimethylphenol 527-54-8 C9H12O 136 70 121 1002-ethylphen

28、ol 90-00-6 C8H10O 107 100 122 483-ethylphenol 620-17-7 C8H10O 122 48 107 1004-ethylphenol 123-07-9 C8H10O 107 100 122 354-propylphenol 645-56-7 C9H12O 107 100 136 254-isopropylphenol 99-89-8 C9H12O 121 100 136 282-hydroxybiphenyl 90-43-7 C12H10O 170 100 141 23Internal standards2-fluorophenol 367-12-

29、4 C6H5FO 112 100 64 584-fluorophenol 371-41-5 C6H5FO 112 100 64 183-fluoro-2-methyl-phenol452-72-2 C7H7FO 126 100 97 294-fluorocatechol 367-32-8 C6H5FO2128 100 75 28aChemical abstract service registry number.bSpectral database for organic compounds (SDBS).Table 2 Target chlorophenolic compounds with

30、 relevant mass fractions of respective acetylated compounds for MS-detectionCompound CAS-RNaChemical formulaAcetylated compoundsFragmentation1stmass Relative intensity %2nd mass Relative intensity %2-chlorophenol 95-57-8 C6H5OCl 128 100 130 343-chlorophenol 108-43-0 C6H5OCl 128 100 130 294-chlorophe

31、nol 106-48-9 C6H5OCl 128 100 130 352,6-dichlorophenol 87-65-0 C6H4OCl2162 100 164 672,4-dichlorophenol 120-83-2 C6H4OCl2162 100 164 662,5-dichlorophenol 583-78-8 C6H4OCl2162 164 3,5-dichlorophenol 591-35-5 C6H4OCl2162 100 164 662,3-dichlorophenol 576-24-9 C6H4OCl2162 100 164 663,4-dichlorophenol 95-

32、77-2 C6H4OCl2162 100 164 662,4,6-trichlorophenol 88-06-2 C6H3OCl3196 100 198 98aChemical abstract service registry number.Table 1 (continued)2 ISO 2014 All rights reservedPD ISO/TS 17182:2014ISO/TS 17182:2014(E)Compound CAS-RNaChemical formulaAcetylated compoundsFragmentation1stmass Relative intensi

33、ty %2nd mass Relative intensity %2,3,6-trichlorophenol 933-75-5 C6H3OCl3196 100 198 1002,3,5-trichlorophenol 933-78-8 C6H3OCl3196 100 198 1002,4,5-trichlorophenol 95-95-4 C6H3OCl3196 96,1 198 1002,3,4-trichlorophenol 15950-66-0 C6H3OCl3196 100 198 983,4,5-trichlorophenol 609-19-8 C6H3OCl3196 100 198

34、 1002,3,4,5-tetrachlorophenol 4901-51-3 C6H2OCl4230 232 2,3,5,6-tetrachlorophenol 935-95-5 C6H2OCl4230 79 232 1002,3,4,6-tetrachlorophenol 58-90-2 C6H2OCl4230 78 232 100pentachlorophenol 87-86-5 C6HOCl5264 66 266 100aChemical abstract service registry number.2 Normative referencesThe following docum

35、ents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 3696, Water for analyti

36、cal laboratory use Specification and test methodsISO 10381-1, Soil quality Sampling Part 1: Guidance on the design of sampling programmesISO 11465, Soil quality Determination of dry matter and water content on a mass basis Gravimetric methodISO 14507, Soil quality Pretreatment of samples for determi

37、nation of organic contaminantsISO 18512, Soil quality Guidance on long and short term storage of soil samplesISO 22892, Soil quality Guidelines for the identification of target compounds by gas chromatography and mass spectrometry3 PrincipleThe method described here is based on two steps. The first

38、step includes a solid/liquid extraction: the phenols are extracted from field moist soil with methanol at low pH. The second step is the derivatization of phenols obtained in an aliquot of methanol in aqueous carbonate solution with acetic anhydride; the derivatives formed are extracted from this sa

39、mple with cyclohexane. The cyclohexane fraction is analyzed by gas chromatography with mass spectrometric detection.4 Interferences4.1 Interference with sampling and extractionStandard laboratory glassware, appropriately cleaned and free of interfering compounds. Do not use any kind of plastic conta

40、iners, since phenols can be adsorbed to these. Plastic materials can also contribute their impurities to the sample material. Surfactants, present in the sample, might disturb the proper extraction of phenols.Table 2 (continued) ISO 2014 All rights reserved 3PD ISO/TS 17182:2014ISO/TS 17182:2014(E)4

41、.2 Interference with GC-MS determinationSubstances which have the same or nearly the same retention time of the target analytes and which give the same mass fragments (i.e. isomeric phenols other than stated in the table) might interfere with the determination.5 ReagentsDuring the analysis, unless o

42、therwise stated, use only reagents of recognized analytical grade and water of at least grade 1 as defined in ISO 3696.Only commercially available certified standards of high purity shall be used.5.1 Products used in their commercially available form5.1.1 Gas chromatography gases, of a purity as rec

43、ommended by the gas chromatography manufacturer.5.1.2 Methanol, CH3OH, with a mass fraction of 99,5 %.5.1.3 Cyclohexane, C6H12or other hydrocarbon solvent like heptane.5.1.4 Hydrochloric acid, HCl, concentrated, with a mass fraction of 37 %.5.1.5 Sodium hydroxide, NaOH.5.1.6 Potassium carbonate, K2C

44、O3.5.1.7 Acetic anhydride, (CH3CO)2O, anhydrous.5.1.8 Sodium sulfate, Na2SO4, anhydrous.Weigh portions of 2 g of sodium sulfate into test tubes with polytetrafluoroethylene (PTFE) lined caps. Dry the test tubes at (550 20) C for 4 h 30 min without caps. Take them to a desiccator and let them cool. W

45、hen cooled, put on the caps and store the tubes at room temperature. Sodium sulfate can also be dried in bigger portions and stored in a desiccator after cooling. Weigh portions of 2 g into tubes when needed.5.1.9 Selected phenol and chlorophenol standards, listed in Table 1 and Table 2.5.1.10 Selec

46、ted fluorophenol standards, listed in Table 1 as internal standard.NOTE Other compounds such as isotopic and deuterated phenols which might not interfere with the GC-MS measurement can also be used as internal standards.5.2 Aqueous solutions5.2.1 Sodium hydroxide solution, NaOH, c(NaOH) = 0,1 mol/l.

47、5.2.2 Sodium hydroxide solution, NaOH, c(NaOH) = 0,5 mol/l.5.2.3 Potassium carbonate solution, K2CO3, c(K2CO3) = 0,1 mol/l.5.2.4 Potassium carbonate solution, K2CO3, c(K2CO3) = 5,2 mol/l.4 ISO 2014 All rights reservedPD ISO/TS 17182:2014ISO/TS 17182:2014(E)5.3 Standard solutions of phenols5.3.1 Inte

48、rnal standard solution5.3.1.1 GeneralFluorophenols can be used as suitable internal standard.5.3.1.2 Stock solutionPrepare the stock solution by weighing fluorophenols (5.1.10) and dissolving it in methanol (5.1.2). A suitable concentration is 1 mg/ml. Divide the stock solution into 5 ml bottles wit

49、h tight caps, 1,5 ml to each, and store at 18 C.NOTE Stock solutions are stable for at least half a year when stored in the dark at 4 C. They are stable at least one year at 18 C.5.3.1.3 Working solutionPrepare this working solution by diluting the stock solution (5.3.1.2) with distilled water. A suitable concentration is 100 g/ml.5.3.2 Individual standard phenol solutions5.3.2.1 GeneralTypical concentrations of standard solutions are given in Annex A.5.3.2.2 Stock solutionWeigh out each of t