1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 16000-4:2011Indoor airPart 4: Determination of formaldehyde Diffusive sampling methodBS ISO 16000-4:2011 BRITISH STANDARDNational forewordThis British Standard is the UK i
2、mplementation of ISO 16000-4:2011.It supersedes BS ISO 16000-4:2004 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee EH/2/3, Ambient atmospheres.A list of organizations represented on this committee can beobtained on request to its secretary.This publica
3、tion does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 68687 0ICS 13.040.20Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the autho
4、rity of theStandards Policy and Strategy Committee on 31 December 2011.Amendments issued since publicationDate Text affectedBS ISO 16000-4:2011Reference numberISO 16000-4:2011(E)ISO 2011INTERNATIONAL STANDARD ISO16000-4Second edition2011-12-01Indoor air Part 4: Determination of formaldehyde Diffusiv
5、e sampling method Air intrieur Partie 4: Dosage du formaldhyde Mthode par chantillonnage diffusif BS ISO 16000-4:2011ISO 16000-4:2011(E) COPYRIGHT PROTECTED DOCUMENT ISO 2011 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by
6、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 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mai
7、l copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2011 All rights reservedBS ISO 16000-4:2011ISO 16000-4:2011(E) ISO 2011 All rights reserved iiiContents Page Foreword iv Introduction vi 1 Scope 1 2 Normative references 1 3 Principle . 2 4 Reagents 2 5 Apparatus . 3 6 Sampling 4 7 P
8、rocedure . 4 7.1 Desorption and sample preparation 4 7.2 Calibration 4 7.3 HPLC analysis 5 7.4 Determination of sample concentration 6 7.5 Storage . 6 7.6 Determination of desorption efficiency . 6 8 Calculation . 6 8.1 Mass of DNPH-formaldehyde on the filter 6 8.2 Concentration of formaldehyde in a
9、ir . 7 9 Precision and uncertainty of the method 7 10 Quality assurance/quality control 8 11 Test report 8 Annex A (informative) Typical designs of diffusive samplers 9 Bibliography 11 BS ISO 16000-4:2011ISO 16000-4:2011(E) iv ISO 2011 All rights reservedForeword ISO (the International Organization
10、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 t
11、he 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. Interna
12、tional Standards are drafted in accordance with the rules given in the ISO/IEC Directives, 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. Publicatio
13、n 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 document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights
14、. ISO 16000-4 was prepared by Technical Committee ISO/TC 146, Air quality, Subcommittee SC 6, Indoor air. This second edition cancels and replaces the first edition (ISO 16000-4:2004), which has been technically revised, especially 7.2. ISO 16000 consists of the following parts, under the general ti
15、tle Indoor air: Part 1: General aspects of sampling strategy Part 2: Sampling strategy for formaldehyde Part 3: Determination of formaldehyde and other carbonyl compounds in indoor air and test chamber air Active sampling method Part 4: Determination of formaldehyde Diffusive sampling method Part 5:
16、 Sampling strategy for volatile organic compounds (VOCs) Part 6: Determination of volatile organic compounds in indoor and test chamber air by active sampling on Tenax TAsorbent, thermal desorption and gas chromatography using MS or MS-FID Part 7: Sampling strategy for determination of airborne asbe
17、stos fibre concentrations Part 8: Determination of local mean ages of air in buildings for characterizing ventilation conditions Part 9: Determination of the emission of volatile organic compounds from building products and furnishing Emission test chamber method Part 10: Determination of the emissi
18、on of volatile organic compounds from building products and furnishing Emission test cell method Part 11: Determination of the emission of volatile organic compounds from building products and furnishing Sampling, storage of samples and preparation of test specimens Part 12: Sampling strategy for po
19、lychlorinated biphenyls (PCBs), polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and polycyclic aromatic hydrocarbons (PAHs) BS ISO 16000-4:2011ISO 16000-4:2011(E) ISO 2011 All rights reserved v Part 13: Determination of total (gas and particle-phase) polychlorinated
20、dioxin-like biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs) Collection on sorbent-backed filters Part 14: Determination of total (gas and particle-phase) polychlorinated dioxin-like biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs)
21、Extraction, clean-up and analysis by high-resolution gas chromatography and mass spectrometry Part 15: Sampling strategy for nitrogen dioxide (NO2) Part 16: Detection and enumeration of moulds Sampling by filtration Part 17: Detection and enumeration of moulds Culture-based method Part 18: Detection
22、 and enumeration of moulds Sampling by impaction Part 19: Sampling strategy for moulds Part 23: Performance test for evaluating the reduction of formaldehyde concentrations by sorptive building materials Part 24: Performance test for evaluating the reduction of volatile organic compound (except form
23、aldehyde) concentrations by sorptive building materials Part 25: Determination of the emission of semi-volatile organic compounds by building products Micro-chamber method Part 26: Sampling strategy for carbon dioxide (CO2) Part 28: Determination of odour emissions from building products using test
24、chambers The following parts are under preparation: Part 21: Detection and enumeration of moulds Sampling from materials Part 27: Determination of settled fibrous dust on surfaces by SEM (scanning electron microscopy) (direct method) Part 29: Test methods for VOC detectors Part 30: Sensory testing o
25、f indoor air Part 31: Measurement of flame retardants and plasticizers based on organophosphorus compounds Phosphoric acid ester Part 32: Investigation of constructions on pollutants and other injurious factors Inspections BS ISO 16000-4:2011ISO 16000-4:2011(E) vi ISO 2011 All rights reservedIntrodu
26、ction Formaldehyde has a high potential toxicity, and therefore, its determination is of interest as an indoor air pollutant. Formaldehyde is an irritant that may cause allergic reactions and other health issues. Formaldehyde is the simplest carbonyl compound, with one carbon, one oxygen and two hyd
27、rogen atoms. In its monomolecular state, it is a colourless, pungent, reactive gas. It has been used in the production of urea-formaldehyde resins, adhesives and insulating foams. Emissions from particle (chip) board and wall insulation are the major sources of formaldehyde in indoor air. This part
28、of ISO 16000 is intended to be used for characterizing indoor air following the sampling strategy for formaldehyde specified in ISO 16000-2. ISO 16000-1 gives general requirements for the measurement of indoor air pollutants and the important conditions to be observed before or during the sampling o
29、f individual pollutants or groups of pollutants. An active formaldehyde measurement procedure (reference method) is specified in ISO 16000-3. Aspects of the determination (sampling and analysis) and the sampling strategy of specific pollutants or groups of pollutants are specified in the other parts
30、 of ISO 16000. ISO 1601767and ISO 1221915also focus on volatile organic compound (VOC) measurements. BS ISO 16000-4:2011INTERNATIONAL STANDARD ISO 16000-4:2011(E) ISO 2011 All rights reserved 1Indoor air Part 4: Determination of formaldehyde Diffusive sampling method WARNING Persons using this part
31、of ISO 16000 should be familiar with normal laboratory practice. This part of ISO 16000 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 safety and health practices and to ensure compliance with any
32、 national regulatory conditions. 1 Scope This part of ISO 16000 specifies a determination of formaldehyde in indoor air using a diffusive sampler with solvent desorption and high performance liquid chromatography (HPLC). The test method is applicable to the measurement of formaldehyde1 )in indoor ai
33、r over the range from 0,001 mg/m3to 1,0 mg/m3for a sampling period of between 24 h and 72 h. For sampling periods of 24 h, the applicable concentration range is 0,003 mg/m3to 1 mg/m3, and for 72 h it is 0,001 mg/m3to 0,33 mg/m3. NOTE Confirmed samplers with respect to measurement sensitivity and pre
34、cision can apply to short-term sampling (less than 24 h). The method is suitable for measurements in atmospheres with conventional indoor air relative humidity and for monitoring at air velocities as low as 0,02 m/s. The chromatographic step in the method is designed to eliminate potential interfere
35、nces, including those due to the presence of other carbonyl compounds. The sampling method gives a time-weighted average result. NOTE There are several diffusive samplers with various designs and shapes commercially available. They are all based on the reaction of 2,4-dinitrophenylhydrazine with for
36、maldehyde. They are not specifically described in this part of ISO 16000 to avoid any impression that ISO favours one model over another. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited app
37、lies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 16000-2, Indoor air Part 2: Sampling strategy for formaldehyde ISO 16000-3:2011, Indoor air Part 3: Determination of formaldehyde and other carbonyl compounds in indoor air and test ch
38、amber air Active sampling method ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories EN 13528-2, Ambient air quality Diffusive samplers for the determination of concentrations of gases and vapours Requirements and test methods Part 2: Specific requirements
39、and test methods 1) Instead of systematic IUPAC nomenclature, traditional names are used in this part of ISO 16000, e.g. “formaldehyde” is used instead of “methanal”. BS ISO 16000-4:2011ISO 16000-4:2011(E) 2 ISO 2011 All rights reserved3 Principle The diffusive sampler is exposed to air for a define
40、d time period. The rate of sampling depends on the diffusion coefficient of formaldehyde, and is proportional to the cross-sectional area of the opening of the monitor and inversely proportional to the length of the diffusion zone of the monitor. This rate is known as the diffusive uptake rate of th
41、e sampler, and has been determined by prior calibration in a standard atmosphere. The formaldehyde vapour migrates into the sampler by diffusion and is collected on a strip of cellulose paper loaded with silica gel, which has been coated with 2,4-dinitrophenylhydrazine (DNPH) and phosphoric acid. A
42、stable hydrazone is formed which can be desorbed by acetonitrile and the solution analysed by means of a high performance liquid chromatograph (HPLC) equipped with an ultraviolet (UV) detector. The diffusive sampler may also be used for personal sampling, for which purpose it is attached to the clot
43、hing of the person being monitored. 4 Reagents During the analysis use only chemicals of recognized grade. 4.1 2,4-Dinitrophenylhydrazine, recrystallized at least twice with UV-grade acetonitrile (4.2) before use. 4.2 Acetonitrile, HPLC UV grade (each batch of solvent should be tested before use). 4
44、.3 Concentrated hydrochloric acid, 36,5 % to 38 % (mass fraction), 1,19 kg/l. 4.4 Nitrogen, high-purity grade (best source). 4.5 Water, HPLC grade. 4.6 Formaldehyde, 37 % solution (mass fraction). 4.7 Ethanol, 95 % (mass fraction). 4.8 Methanol, HPLC grade. 4.9 Phosphoric acid, 85 % (mass fraction).
45、 4.10 Glycerin, 20 % (volume fraction). 4.11 Formaldehyde dinitrophenylhydrazone (DNPH-formaldehyde). WARNING 2,4-Dinitrophenylhydrazine is explosive in the dry state. Handle with extreme care. It is also toxic (in the rat, LD50 654 mg/kg), has been shown to be mutagenic in some tests, and is irrita
46、ting to the eyes and skin. Weigh 2 g of 2,4-dinitrophenylhydrazine (4.1) and place in a 500 ml flask. Add 10 ml of concentrated hydrochloric acid (HCI) (4.3) with stirring. Dissolve the yellow precipitate formed in 200 ml of ethanol (4.7). Filter the solution to remove undissolved hydrazine hydrochl
47、oride (DNPHHCl). To the filtered solution, add 0,8 ml of formaldehyde. Collect by filtration the yellowish DNPH-formaldehyde precipitate formed, and wash with 5 ml cold ethanol. Recrystallize the precipitate twice from hot ethanol and allow to dry in air. Check the purity of the DNPH-formaldehyde de
48、rivative by melting-point determination (166 C) or HPLC analysis (purity 99 % mass fraction). If the impurity level is not acceptable, recrystallize the derivative in ethanol. Repeat the purity check and recrystallization, as necessary, until an acceptable level of purity (e.g. 99 % mass fraction) i
49、s achieved. The DNPH-formaldehyde derivative should be stored under refrigeration (4 C) and protected from light. It should be stable for at least 6 months. NOTE Storage under nitrogen or argon further prolongs the lifetime of the derivative. DNPH derivatives of formaldehyde for use as standards are commercially available both in the form of pure crystals and as individual or mixed stock solutions in acetonitrile. BS ISO
