ISO-16200-1-2001.pdf

Reference number ISO 16200-1:2001(E) ©ISO 2001 INTERNATIONAL STANDARD ISO 16200-1 First edition 2001-08-15 Workplace air quality Sampling and analysis of volatile organic compounds by solvent desorption/gas chromatography Part 1: Pumped sampling method Qualité de l'air des lieux de travail Échantillonnage et analyse des composés organiques volatils par désorption au solvant/chromatographie en phase gazeuse Partie 1: Méthode d'échantillonnage par pompage Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/12/2007 23:04:36 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 16200-1:2001(E) PDF disclaimer This PDF file may contain embedded typefaces. 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Unless otherwise specified, no part of this 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 ISO's member body in the country of the requester. ISO copyright office Case postale 56 ? CH-1211 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 2001 All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/12/2007 23:04:36 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 16200-1:2001(E) © ISO 2001 All rights reservediii ContentsPage Foreword.iv 1Scope 1 2Normative references1 3Principle2 4Reagents and materials 2 5Apparatus.4 6Sampling.6 7Procedure.7 8Calculations8 9Interferences 9 10Precision and bias.9 11Storage and transport .9 12Test report10 13Quality control10 Annex A (informative) Description of sorbent types.23 Annex B (informative) Equivalence of gas chromatographic stationary phases.24 Annex C (informative) Determination of breakthrough volume .25 Bibliography27 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/12/2007 23:04:36 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 16200-1:2001(E) iv© ISO 2001 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 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 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. 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 of this part of ISO 16200 may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 16200-1 was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee SC 2, Workplace atmospheres. ISO 16200 consists of the following parts, under the general title Workplace air quality Sampling and analysis of volatile organic compounds by solvent desorption/gas chromatography: ?Part 1: Pumped sampling method ?Part 2: Diffusive sampling method Annexes A, B and C of this part of ISO 16200 are for information only. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/12/2007 23:04:36 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARDISO 16200-1:2001(E) © ISO 2001 All rights reserved1 Workplace air quality Sampling and analysis of volatile organic compounds by solvent desorption/gas chromatography Part 1: Pumped sampling method 1Scope This part of ISO 16200 gives general guidance for the sampling and analysis of volatile organic compounds (VOCs) in air by solvent desorption/gas chromatography using pumped sampling. This part of ISO 16200 is applicable to a wide range of VOCs, including hydrocarbons, halogenated hydrocarbons, esters, glycol ethers, ketones and alcohols. A number of sorbents are recommended for the sampling of these VOCs, each sorbent having a different range of applicability. However, activated coconut shell charcoal is frequently used. Very polar compounds may require derivatization; very low boiling compounds will only be partially retained by the sorbents and can only be estimated qualitatively. Semi-volatile compounds will be fully retained by the sorbents, but may only be partially recovered. The upper limit of the useful range is set by the sorptive capacity of the sorbent used and by the linear dynamic range of the gas chromatograph column and detector or by the sample-splitting capability of the analytical instrumentation used. The lower limit of the useful range depends on the noise level of the detector and on blank levels of analyte and/or interfering artefacts on the sorbent tubes or in the desorption solvent. Artefacts are typically subnanogram for activated charcoal, but higher levels of aromatic hydrocarbons have been noted in some batches. The concentration range for which this part of ISO 16200 is valid for the measurement of airborne vapours of VOCs is dependent on the volume sampled. For example, for a 10-litre sample of air, the range is approximately 1 mg/m3 to 1000 mg/m3individual organic compound. For a 1-litre sample of air, the range is approximately 10 mg/m3to 10 000 mg/m3individual organic compound, and pro rata. 2Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this part of ISO 16200. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this part of ISO 16200 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 registers of currently valid International Standards. EN 1232, Workplace atmospheres Pumps for personal sampling of chemical agents Requirements and test methods EN 1540, Workplace atmospheres Terminology Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/12/2007 23:04:36 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 16200-1:2001(E) 2© ISO 2001 All rights reserved 3Principle A measured volume of sample air is drawn through one (or more) sorbent tubes in series; an appropriate sorbent (or sorbents) being selected for the compound or mixture to be sampled. Provided suitable sorbents are chosen, volatile organic components are retained by the sorbent tube and thus are removed from the flowing air stream. The collected vapour is desorbed by a solvent, typically carbon disulfide, and the solution is analysed with a gas chromatograph equipped with a flame ionization detector, mass spectrometer or other selective detector. 4Reagents and materials During the analysis, use only reagents of analytical reagent grade. 4.1Volatile organic compounds A wide range of VOCs are required as reagents for calibration purposes. 4.2Desorption solvent The desorption or elution solvent, commonly carbon disulfide, should be of chromatographic quality. It shall be free from compounds co-eluting with the substances of interest. Tables 1 and 2 give recommended desorption solvents for particular vapours (see 7.5). Where necessary (see Note 2), a desorption solvent modifier should be added at a sufficient concentration to result in a homogeneous solution in desorbed samples. Dimethylformamide may be suitable for this purpose. NOTE 1Carbon disulfide is normally recommended for the desorption of non-polar compounds from activated carbon. For polar compounds and mixtures of polar and non-polar compounds there is no ideal universal desorption solvent. Dichloromethane, methanol, higher alcohols, dimethylformamide and acetonitrile have been used as eluents, either singly or mixed with each other or carbon disulfide. OSHA methods 07 and 100 1 and the NIOSH methods 1301, 1400, 1401, 1402, 1403 for ketones and alcohols 2 give examples of suitable desorption solvents other than pure carbon disulfide. NOTE 2The use of carbon disulfide desorption solvent can result in problems when polar analytes are collected from humid atmospheres. Polar analytes may be soluble in a water phase which forms following desorption with carbon disulfide when sufficient water is collected with the sample. 4.3Sorbents 4.3.1Activated charcoal Tubes prepacked by the manufacturer with preconditioned charcoal are available and do not require further conditioning. Alternatively, tubes may be prepared by the user. A particle size of 0,35 mm to 0,85 mm is recommended. Before packing the tubes, the charcoal shall be heated in an inert atmosphere, e.g. high-purity nitrogen, at approximately 600 °C for 1 h. To prevent recontamination of the charcoal, it shall be kept in a clean atmosphere during cooling to room temperature, storage, and loading into the tubes. The sorptive capacity and desorption efficiency of different batches of activated charcoal may vary. Commercial tubes, if used, should be purchased from the same batch and in sufficient number to provide consistent performance for a definite period of time. NOTEActivated charcoal is usually processed from coconut shells. For some applications, petroleum-based charcoal is preferred (see Tables 1 and 2). Some manufacturers recommend synthetic carbons as alternatives to charcoal of biological origin. 4.3.2Other sorbents Sorbents other than charcoal may be used for certain applications (see Tables 1 and 2). NOTEA description of sorbent types is given in annex A. Equivalent sorbents may be used. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/12/2007 23:04:36 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 16200-1:2001(E) © ISO 2001 All rights reserved3 4.4Calibration standards Calibration blend solutions are required in order to compare the concentrations of desorbed solutions (7.3) with those calibration standards in the gas chromatographic analysis. Such solutions should be prepared in a way that is traceable to national standards. An internal standard is optional. If used, it should not interfere with the compounds of interest and it should not be removed from the elution solvent by the sorbent. In the context of this method, the purpose of the internal standard is to correct for small variations in the injection volume. The use of an internal standard as a surrogate to correct for desorption efficiency (e.g. n-propyl acetate in the analysis of n-butyl acetate) is not recommended. Desorption efficiency should be determined directly with the compounds of interest (7.5). Storage times for calibration solutions vary according to application. Typically, carbon disulfide dilutions should be prepared fresh weekly, or more frequently if evidence is noted of decomposition or evaporation. NOTEIn the analysis of complex mixtures, calibration blends of the pure compounds may be prepared before dilution with the elution solvent. Examples of three calibration blends are listed here. These have been used in the analysis of mixed solvents in paints, thinners, adhesives, cleaning fluids and miscellaneous commercial products. The components are arranged to give resolved peaks on both BP-1 and BP-10 phases1?. Other blends may be more appropriate on different columns or in other applications. In the examples below, calibration blends 1-3 are stable for at least one year when stored in dark glass bottles with PTFE-lined screw-caps at less than 4 °C. a)Blend 1 consists of: n-hexane, n-heptane, n-octane, n-decane, n-undecane, n-dodecane, benzene, toluene, o-xylene, p-xylene, n-propylbenzene, isopropylbenzene, o-ethyltoluene, m-ethyltoluene, p-ethyltoluene, 1,2,4-trimethylbenzene, 1,3,5-trimethylbenzene, n-propyl acetate, n-butyl acetate, isobutyl acetate, butoxyethyl acetate. b)Blend 2 consists of: isopropanol, isobutanol, n-butanol, 1-methoxy-2-propanol, butoxyethanol, toluene, ethylbenzene, 1,2,3-trimethylbenzene, ethyl acetate, ethoxyethyl acetate. c)Blend3consistsof:acetone,2-butanone,4-methylpentan-2-one,cyclohexanone,2-methylcyclohexanone, 3-methylcyclohexanone, 4-methylcyclohexanone, isopropyl acetate, n-nonane, toluene. 4.4.1Solution containing approximately 10 mg/ml of each liquid component Weigh 1 g of the substance or substances of interest into a 100 ml volumetric flask, starting with the least volatile substance. Make up to 100 ml with desorption solvent (4.2), stopper and shake to mix. 4.4.2Solutions containing approximately 1 mg/ml of liquid components Introduce 50 ml of desorption solvent into a 100 ml volumetric flask. Add 10 m