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1、 Reference number ISO 15009:2002(E) ISO 2002 INTERNATIONAL STANDARD ISO 15009 First edition 2002-10-15 Soil quality Gas chromatographic determination of the content of volatile aromatic hydrocarbons, naphthalene and volatile halogenated hydrocarbons Purge-and-trap method with thermal desorption Qual
2、it du sol Dtermination par chromatographie en phase gazeuse des teneurs en hydrocarbures aromatiques volatils, en naphtalne et en hydrocarbures halogns volatils Mthode par purge et pigeage avec dsorption thermique ISO 15009:2002(E) PDF disclaimer This PDF file may contain embedded typefaces. In acco
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5、ting. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. ISO 2002 All rights reserved. Unless otherwise specified, no part of this
6、publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211
7、Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.ch Web www.iso.ch Printed in Switzerland ii ISO 2002 All rights reserved ISO 15009:2002(E) ISO 2002 All rights reserved iii Contents Page Foreword iv 1 Scope 1 2 Normative references 1 3 Principle . 1 4 Reagents 2 5 Preparati
8、on of standard solutions. 4 6 Apparatus. 4 7 Sampling, preservation and sample pretreatment 7 8 Procedure. 7 8.1 Blank determination 7 8.2 Dry matter content 7 8.3 Extraction. 7 8.4 Purge-and-trap. 8 8.5 Gas chromatographic analysis 8 9 Calculation. 10 9.1 Principle . 10 9.2 Procedure. 10 10 Express
9、ion of results 11 11 Precision 11 12 Test report 11 Annex A (informative) Relative retention times with respect to ethylbenzene-D10 of volatile aromatic hydrocarbons and volatile halogenated hydrocarbons on CP-Sil 5 CB and CP-Sil 13 CB columns 12 Annex B (informative) Validation 15 Bibliography 18 I
10、SO 15009:2002(E) iv ISO 2002 All rights reserved Foreword ISO (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
11、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 and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International
12、 Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. The main task of technical committees is to prepare International Standards. Draft International Standards
13、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 of this International Standard may be t
14、he subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 15009 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics. Annexes A and B of this International Standard are for i
15、nformation only. -,-,- INTERNATIONAL STANDARD ISO 15009:2002(E) ISO 2002 All rights reserved 1 Soil quality Gas chromatographic determination of the content of volatile aromatic hydrocarbons, naphthalene and volatile halogenated hydrocarbons Purge-and-trap method with thermal desorption 1 Scope This
16、 International Standard specifies a method for quantitative gas-chromatographic determination of volatile hydrocarbons, naphthalene and volatile halogenated hydrocarbons in soil. This International Standard is applicable to all types of soil. Under the conditions specified in this International Stan
17、dard, the following limits of determinations apply (expressed on basis of dry matter): volatile hydrocarbons and naphthalene: 0,1 mg/kg; volatile halogenated hydrocarbons: 0,01 mg/kg. The lower limit of determination is dependent on the equipment used and the quality of the methanol grade used for t
18、he extraction of the soil sample. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not
19、 apply. However, parties to agreements based on this International Standard 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
20、 of ISO and IEC maintain registers of currently valid International Standards. ISO 4799, Laboratory glassware Condensers ISO 10381-1, Soil quality Sampling Part 1: Guidance on the design of sampling programmes ISO 10381-2, Soil quality Sampling Part 2: Guidance on sampling techniques ISO 11465, Soil
21、 quality Determination of dry matter and water content on a mass basis Gravimetric method Technical corrigendum 1 3 Principle From an untreated field-moist soil sample, test samples are taken. The test sample is extracted with methanol. After centrifugation, part of the methanol extract is brought i
22、nto a purge vessel filled with water. The volatile compounds are purged with nitrogen or helium and adsorbed on a suitable adsorbing agent. The adsorbed compounds are desorbed thermally and, by means of a carrier gas flow, optionally via a cold trap, brought into a gas chromatograph. The various com
23、pounds are separated using a capillary column -,-,- ISO 15009:2002(E) 2 ISO 2002 All rights reserved with an immobile phase of low polarity. Volatile aromatic hydrocarbons are detected with a flame ionization detector (FID). Volatile halogenated hydrocarbons are detected with an electron capture det
24、ector (ECD). Volatile aromatic hydrocarbons and volatile halogenated hydrocarbons can be determined in one gas chromatographic run. Part of the effluent is brought to the FID and part to the ECD, e.g. via an effluent splitter. Identification and quantification takes place by comparison of retention
25、times and peak heights (or peak areas) of an internal standard added with the corresponding variables of an external standard solution. The efficiency of the procedure depends on the composition of the soil that is investigated. The described procedure does not take into account incomplete extractio
26、n caused by structure and composition of the soil sample. Extraction with methanol is preferred to the use of acetone because acetone extracts are not suitable for “purge- and-trap”. For confirmation of the identity of detected compounds and the concentrations found, further investigation is recomme
27、nded. Confirmation can be done by repeating the gas chromatographic analysis using a column of different polarity and/or by using gas chromatography-mass spectrometry (GC-MS). 4 Reagents All reagents shall be of recognized analytical grade. Verify whether the reagents are applicable for this specifi
28、c purpose and free of interfering compounds. 4.1 Water, free of volatile aromatic and halogenated hydrocarbons. Usually boiler water with a temperature of at least 80 C and 1 day old can be used. Purging with an inert gas, e.g. nitrogen at a flowrate of 10 ml/min for 30 min, is another way to remove
29、 interfering compounds from water. Sufficient water from the same batch should be available to complete each batch of analyses, including all preparations. 4.2 Internal standards. 4.2.1 For the determination of volatile aromatic hydrocarbons, preferably two internal standards should be selected that
30、 do not interfere with compounds present in the sample extract. Examples of suitable internal standards are: Toluene-D8 (CAS No. 2037-26-5); Ethylbenzene-D10 (CAS No. 25837-05-2). 4.2.2 For the determination of volatile halogenated hydrocarbons, preferably two internal standards should be selected t
31、hat do not interfere with compounds present in the sample extract. Examples of suitable internal standards are: 1,4-dichlorobutane (CAS No. 110-56-5); ,-trifluorotoluene (CAS No. 98-08-8); 2-bromofluorobenzene (CAS No. 1072-85-1). 4.3 Volatile aromatic hydrocarbons. Compound CAS No. benzene 71-43-2
32、toluene 108-88-3 ethylbenzene 100-41-4 o-xylene 95-47-6 -,-,- ISO 15009:2002(E) ISO 2002 All rights reserved 3 m-xylene 108-38-3 p-xylene 106-42-3 styrene 100-42-5 naphthalene 91-20-3 4.4 Volatile halogenated hydrocarbons. Compound CAS No. dichloromethane 75-09-2 trichloromethane 67-66-3 tetrachloro
33、methane 56-23-5 1,1-dichloroethane 75-34-3 1,2-dichloroethane 107-06-2 1,1,1-trichloroethane 79-01-6 1,1,2-trichloroethane 79-00-5 1,2-dichloropropane 78-87-5 1,2,3-trichloropropane 98-18-4 cis-1,3-dichloropropene 10061-01-5 trans-1,3-dichloropropene 10061-02-6 cis-1,2-dichloroethene 156-59-2 trans-
34、1,2-dichloroethene 156-60-5 3-chloropropene 107-05-1 trichloroethene 79-01-6 tetrachloroethene 127-18-4 monochlorobenzene 108-90-7 1,2-dichlorobenzene 95-50-1 4.5 Methanol (CAS No. 67-56-1) The methanol used shall not contain more than 100 g/l of the individual volatile aromatic compounds and not mo
35、re than 10 g/l of the volatile halogenated hydrocarbons that are to be analysed. 4.6 Adsorbing agent, polymer of 2,6-diphenyl-p-phenoxide1) (40 60 mesh) of a grade suitable for thermal desorption. Other adsorbing agents may be used provided that their suitability has been tested. 4.7 Cooling water f
36、or purge-and-trap. 1) Tenax TA is an example of a suitable product available commercially. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by ISO of this product. -,-,- ISO 15009:2002(E) 4 ISO 2002 All rights reserved The t
37、emperature of the cooling water depends on the dimensions of the purge-and-trap equipment (6.1). A temperature of about 10 C is recommended. A cryostat shall be used if the temperature of the cooling water is too high. 4.8 Inert carrier gas for the gas chromatograph. 4.9 Nitrogen as inert gas for th
38、e purge equipment. 5 Preparation of standard solutions 5.1 Primary standard solutions for volatile aromatic and halogenated compounds in methanol, 4 g/l. Weigh about 100 mg of the individual standard compounds (4.3 and 4.4) to an accuracy of 0,1 mg into a closed septum flask containing 25 ml methano
39、l. Transfer the standard compounds into the flask using a syringe. 5.2 Internal standard solutions in methanol, 4 g/l. Weigh about 100 mg of the individual internal standard compounds (4.2.1 and 4.2.2) to an accuracy of 0,1 mg into a closed septum flask containing 25 ml of methanol. Using a syringe,
40、 transfer the standard compounds into the flask. 5.3 Calibration solutions containing 0 mg/l to 200 mg/l of each primary standard (5.1) and the selected internal standard(s) (5.2), 200 mg/l. Prepare the calibration solutions in methanol. Dilute the amounts indicated in Table 1 of the solutions obtai
41、ned according to 5.1 and 5.2 with methanol (4.5) to 100 ml. Table 1 Preparation of calibration solutions Calibration solution Internal standard solution (5.2) ml Primary standard solution (5.2) ml Concentration in the calibration solution mg/l Quantity in g/5 l calibration solution in 100 ml (sample
42、) water 5.3.1 5 0 0 0 5.3.2 5 1 40 0,2 5.3.3 5 2 80 0,4 5.3.4 5 3 120 0,6 5.3.5 5 4 160 0,8 5.3.6 5 5 200 1,0 6 Apparatus Use the usual laboratory glassware, free of interfering compounds. All glassware shall be cleaned according to the usual procedures for this type of analysis. 6.1 Purge-and-trap
43、apparatus. An example of an off-line purge-and-trap system is given in Figure 1. NOTE 1 This International Standard follows the description of an “off-line purge-and-trap” method. The use of commercially available online instruments is allowed provided that equivalent results are obtained during val
44、idation of this equipment. With such an instrument, purge-and-trap occurs on-line with gas chromatography and detection. Follow the manufacturers instruction manual especially regarding items 6.1.1 to 6.1.9 NOTE 2 This method is only validated for the off-line procedure. ISO 15009:2002(E) ISO 2002 A
45、ll rights reserved 5 Key 1 Round-bottom flask, 100 ml (6.1.1) 2 Inlet tube for thermocouple (6.1.5) 3 Tip of sintered glass 4 Gas inlet tube (6.1.2) 5 Spherical joint, in accordance with ISO 641, with PTFE ring (6.1.3) 6 Conical joint 14/23 in accordance with ISO 383 7 Condenser (6.1.6) 8 Screwcap (
46、6.1.7) 9 Adsorption tube (6.1.8) 10 Conical joint 14/23 in accordance with ISO 383 Figure 1 Example of off-line purge-and-trap apparatus -,-,- ISO 15009:2002(E) 6 ISO 2002 All rights reserved 6.1.1 Round-bottom flask with three angled side necks, volume 100 ml. 6.1.2 Gas inlet tube with a tip of sin
47、tered glass. 6.1.3 Spherical joint, with PTFE. 6.1.4 Flow adjustment mechanism. The nitrogen flowrate shall be (40 2) ml/min. 6.1.5 Inlet tube for the thermocouple. 6.1.6 Allin- or Graham-type condenser, in accordance with ISO 4799. 6.1.7 Screwcap with cut-off ring made of silicone rubber with PTFE
48、inlay. 6.1.8 Adsorption tubes, made of glass or stainless steel, filled with at least 240 mg of adsorbing agent (4.6). The adsorbent is kept in place using inert material, e.g. silanized glass fibre. The tubes shall be suitable for direct use in connection with the apparatus for thermal desorption. The tubes shall be marked on one side. The tubes shall be provided with caps of inert material, e.g. polyethylene or metal, with screwcaps and PTFE ring, allowing tight closing after purging. Before use, the adsorbent shall be activated and purified by slowly heat