1、BSI Standards PublicationBS ISO 16000-31:2014Indoor airPart 31: Measurement of flame retardants and plasticizers based on organophosphorus compounds Phosphoric acid esterBS ISO 16000-31:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO16000-31:2014.The UK pa
2、rticipation in its preparation was entrusted to TechnicalCommittee EH/2/5, Emissions to internal environments.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users
3、 are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 73399 4ICS 13.040.20Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of the
4、Standards Policy and Strategy Committee on 31 May 2014.Amendments issued since publicationDate Text affectedBS ISO 16000-31:2014 ISO 2014Indoor air Part 31: Measurement of flame retardants and plasticizers based on organophosphorus compounds Phosphoric acid esterAir intrieur Partie 31: Mesurage des
5、ignifugeants bass sur des composs organophosphors Ester dacide phosphoriqueINTERNATIONAL STANDARDISO16000-31First edition2014-05-01Reference numberISO 16000-31:2014(E)BS ISO 16000-31:2014ISO 16000-31:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2014All rights reserved. Unle
6、ss 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 either ISO at the a
7、ddress 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 SwitzerlandBS ISO 16000-31:2014ISO 16000-31:2014(E) ISO 2014 All rights reserved iiiCont
8、ents PageForeword ivIntroduction vi1 Scope . 12 Normative references 13 Occurrence 14 Indoor air . 34.1 Measurement planning 34.2 Apparatus and materials for sampling and sample preparation . 34.3 Sampling . 64.4 Sample preparation 65 Test chamber air . 65.1 General . 65.2 Apparatus and materials fo
9、r sampling . 75.3 Sampling . 75.4 Sampling procedure . 85.5 Sample preparation 86 Calibration 86.1 Internal standard solutions and calibration solutions . 86.2 Internal standard solutions 86.3 Calibration solutions for low resolution . 96.4 Calibration solutions for high resolution 107 Identificatio
10、n and quantification .117.1 General 117.2 Analysis apparatus 117.3 Analysis with GC/LR-MS 117.4 Analysis with GC/HR-MS . 117.5 Calculation result interpretation and presentation .138 Performance characteristics .148.1 Performance characteristics of the air analyses .149 Quality assurance .1410 Inter
11、ferences .14Annex A (informative) Nomenclature and physical characteristics .16Annex B (informative) Example chromatograms for standard solutions .19Bibliography .21BS ISO 16000-31:2014ISO 16000-31:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of n
12、ational 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. Inter
13、national 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.The procedures used to develop this document and those inte
14、nded 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 documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www
15、.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 for identifying any or all such patent rights. Details of any patent rights identified during the development of the document w
16、ill 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 convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expres
17、sions 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: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 146, Air quality, Subcommittee SC 6, Ind
18、oor air.ISO 16000 consists of the following parts, under the general title 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
19、Part 4: Determination of formaldehyde Diffusive sampling method Part 5: 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
20、 or MS-FID Part 7: Sampling strategy for determination of airborne asbestos 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 furni
21、shing Emission test chamber method Part 10: Determination of the emission 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 samp
22、les and preparation of test specimens Part 12: Sampling strategy for polychlorinated biphenyls (PCBs), polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and polycyclic aromatic hydrocarbons (PAHs)iv ISO 2014 All rights reservedBS ISO 16000-31:2014ISO 16000-31:2014(E) P
23、art 13: Determination of total (gas and particle-phase) polychlorinated 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 (
24、PCBs) and polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs) 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: Det
25、ection and enumeration of moulds Culture-based method Part 18: Detection and enumeration of moulds Sampling by impaction Part 19: Sampling strategy for moulds Part 21: Detection and enumeration of moulds Sampling from materials Part 23: Performance test for evaluating the reduction of formaldehyde c
26、oncentrations by sorptive building materials Part 24: Performance test for evaluating the reduction of volatile organic compound (except formaldehyde) concentrations by sorptive building materials Part 25: Determination of the emission of semi-volatile organic compounds by building products Micro-ch
27、amber method Part 26: Sampling strategy for carbon dioxide (CO2) Part 28: Determination of odour emissions from building products using test chambers Part 29: Test methods for VOC detectors Part 30: Sensory testing of indoor air Part 31: Measurement of flame retardants and plasticizers based on orga
28、nophosphorus compounds Phosphoric acid ester Part 32: Investigation of buildings for pollutants and other injurious factors InspectionsThe following parts are under preparation: Part 33: Determination of phthalates with gas chromatography/mass spectrometry (GC/MS) Part 34: Strategies for the measure
29、ment of airborne particles (PM 2,5 fraction) Part 35: Measurement of polybrominated diphenylether, hexabromocyclododecane and hexabromobenzene Part 36: Test method for the reduction rate of airborne bacteria by air purifiers using a test chamber ISO 2014 All rights reserved vBS ISO 16000-31:2014ISO
30、16000-31:2014(E)IntroductionIn general terms, phosphoric acid esters are formed by the reaction of alcohols or phenols with phosphoryl chloride (POCl3). A distinction is made between mono-, di-, and triesters (see Figure 1). The triesters with aryl and alkyl groups, as well as with mixed halogenated
31、 and halogen-free ester groups serve as plasticizers and flame retardants in plastics and varnishes. Parallel therewith, phosphoric acid esters are incorporated in hardeners and accelerants, in mordant and adhesion boosting agents, and serve as cleaning, corrosion inhibition, and adhesion-facilitati
32、ng substances by the treatment of metal surfaces. They are used as auxiliary means in paper and textiles, as wetting and defoaming agents, emulsifiers, and stabilizers, as additives to cleaning agents and detergents, as not readily flammable hydraulic liquids, and as oil and fuel additives (see Tabl
33、e 1). Not considered in this regard are the groups of the thio- and dithiophosphoric acid esters (pesticides), as well as the phosphoric acid esters with cyanide and halogen groups, with a special impact as acetylcholinesterase inhibitors (nerve gases).3KeyR aryl, alkyl, halogenated, and halogen-fre
34、e ester groupsFigure 1 Structural formula of the phosphoric acid estersSuch multiplex applicability of the organophosporus compounds (OPCs) leads to the effect that large indoor areas with OPC-containing building materials, varnishes, paints, floor care products, or fire protection coatings can be e
35、ncountered. Due to their varying physical and physical-chemical properties, OPC can also be detected in the indoor transfer media (dust and air). As a rule, OPCs boiling at high temperatures such as tris(2-butoxyethyl) phosphate (TBEP, see Annex A) can be found in relevant concentrations in indoor a
36、ir only if the emission source reaches elevated temperatures. In the case of such sources (e.g. screens or roller blinds for sun protection), the importance of higher temperatures must be taken into consideration when emission chamber tests are carried out.There is an increasing public interest in t
37、he possible health effects of OPCs indoors. For indoor air, a Guideline Value II of 0,05 mg/m3was published for TCEP and, in simplified terms, for the sum of TCEP, TCPP, TBP, TBEP, TEHP, and TPP as well. The Guideline Value I derived there amounts to 0,005 mg/m3.4A review article on the occurrence a
38、nd evaluation of OPC in an indoor environment is available.5This part of ISO 16000 is based on VDI 4301 Part 5.vi ISO 2014 All rights reservedBS ISO 16000-31:2014INTERNATIONAL STANDARD ISO 16000-31:2014(E)Indoor air Part 31: Measurement of flame retardants and plasticizers based on organophosphorus
39、compounds Phosphoric acid ester1 ScopeThis part of ISO 16000 specifies a test method for the sampling and analysis of the phosphoric acid esters in indoor air and in test chamber air through gas chromatography/mass spectrometry. Both principle methods of the low-resolution mass spectrometry and the
40、high-resolution mass spectrometry are described.The methods described in this part of ISO 16000 are not suitable for the determination of the phosphoric acid esters in materials.NOTE ISO 16000-6 can be applied for the determination of the more volatile compounds covered by this standard.2 Normative
41、referencesThe following documents, 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) applie
42、s.ISO 16000-1, Indoor air Part 1: General aspects of sampling strategyISO 16000-9, Indoor air Part 9: Determination of the emission of volatile organic compounds from building products and furnishing Emission test chamber methodISO 16000-13, Indoor air Part 13: Determination of total (gas and partic
43、le-phase) polychlorinated dioxin-like biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins/dibenzofurans (PCDDs/PCDFs) Collection on sorbent-backed filters3 OccurrenceThe following compounds belonging to the halogen-free organophosphates are frequently detected in indoor air: triphenyl phosphate (
44、TPP); tris(2-butoxyethyl) phosphate (TBEP); tri-n-butyl phosphate (TBP); tris(2-ethylhexyl) phosphate (TEHP); cresyl diphenyl phosphate (CDP); triethyl phosphate (TEP); tricresyl phosphate (TCP). ISO 2014 All rights reserved 1BS ISO 16000-31:2014ISO 16000-31:2014(E)The following halogenated phosphor
45、ic acid esters are detected predominantly in house dust and indoor air: tris(2-chloroethyl) phosphate (TCEP); tris(chloropropyl) phosphate (TCPP); tris(1,3-dichloro-2-propyl) phosphate (TDCPP).Bridged diphosphates based on resorcinol- and bisphenol-A are also increasingly implemented as flame retard
46、ants, e. g. tetraphenyl resorcinol diphosphate (RDP) or tetraphenyl bisphenol-A diphosphate (BDP).So far, there is little information about the release of these compounds from primary sources.Table 1 provides an overview of the organophosphates frequently detected in indoor air. The nomenclature and
47、 the chemical and physical data on the organophosphates are listed in Annex A.Table 1 Organophosphates and their intended use (see References5and6)OPC Abbrevia-tionOrganophosphates Intended use as flame retardant and plasticizerCDP Cresyl diphenyl phosphateFlame retardant coatingsRDP Tetraphenyl res
48、or-cinol diphosphateCasing materials, special cablesTBEP Tris(2-butoxyethyl) phosphateFloor care products, floor wax, additives in elastomers, solvents for resins, antifoaming agents, additives for plastic, synthetic rub-ber, and varnishesTBP Tri-n-butyl phos-phateDefoaming agents for concrete addit
49、ives, wall paper, dispersion paints, varnishes, rubber, plastic, and vinyl resins, antifoaming agentsTCEP Tris(2-chloroethyl) phosphatePaints, coatings, soundproofing ceilings, fibre glass wall paper, expanding foam, casing materialsTCPP Tris(1-chloro-2-propyl)-phos-phateaSound-absorbing polyurethane foam, expansion foam, soft foam (seats, mattresses), rear lining of textile, casing materialsTDBPP Tris(2,3-dibromo-propyl) phosphateFoamed rubber, varnis
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