1、BSI Standards PublicationBS EN 13999-2:2013Adhesives Short termmethod for measuring theemission properties of low-solvent or solvent-freeadhesives after applicationPart 2: Determination of volatile organiccompoundsBS EN 13999-2:2013 BRITISH STANDARDNational forewordThis British Standard is the UK im
2、plementation of EN 13999-2:2013.It supersedes BS EN 13999-2:2007 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PRI/52, Adhesives.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not
3、 purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2013. Published by BSI StandardsLimited 2013ISBN 978 0 580 78121 6ICS 83.180Compliance with a British Standard cannot confer immunity fromlegal obligatio
4、ns.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 December 2013.Amendments issued since publicationDate Text affectedBS EN 13999-2:2013EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13999-2 December 2013 ICS 83.180 Supersedes EN 1399
5、9-2:2007English Version Adhesives - Short term method for measuring the emission properties of low-solvent or solvent-free adhesives after application - Part 2: Determination of volatile organic compoundsAdhsifs - Mthode de mesurage rapide des caractristiques missives des adhsifs teneur faible ou nu
6、lle en solvants aprs application - Partie 2: Dosage des composs organiques volatils Klebstoffe - Kurzzeit-Verfahren zum Messen der Emissionseigenschaften von lsemittelarmen oder lsemittelfreien Klebstoffen nach der Applikation - Teil 2: Bestimmung flchtiger organischer Verbindungen This European Sta
7、ndard was approved by CEN on 19 October 2013. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concernin
8、g such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into it
9、s own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germa
10、ny, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR
11、NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13999-2:2013: EBS EN 13999-2:2013EN 13999-2:2013 (E) 2 Contents Page Foreword 3 1 Scope 4 2 Normative ref
12、erences 4 3 Principle 4 4 Reagents and materials 4 5 Apparatus .5 6 Procedure .6 7 Identification and calculation .9 8 Precision and bias 11 9 Test report . 11 10 Quality control . 11 Bibliography . 13 BS EN 13999-2:2013EN 13999-2:2013 (E) 3 Foreword This document (EN 13999-2:2013) has been prepared
13、 by Technical Committee CEN/TC 193 “Adhesives”, the secretariat of which is held by AENOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by June 2014, and conflicting national standards shall be wi
14、thdrawn at the latest by June 2014. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 13999-2:2007. EN 13999
15、-2:2013 includes the following significant technical changes with respect to EN 13999-2:2007: a) change in the calculation of total VOC; b) harmonization of the testing conditions to EN ISO 16000-9. EN 13999, under the general title Adhesives Short -term method for measuring the emission properties
16、of low-solvent or solvent-free adhesives after application, consists of the following parts: Part 1: General procedure Part 2: Determination of volatile organic compounds Part 3: Determination of volatile aldehydes Part 4: Determination of volatile diisocyanates SAFETY STATEMENT Persons using this d
17、ocument should be familiar with the normal laboratory practice, if applicable. This document 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 wit
18、h any regulatory conditions. ENVIRONMENTAL STATEMENT It is understood that some of the material permitted in this European Standard may have negative environmental impact. As technological advantages lead to acceptable alternatives for these materials, they will be eliminated from this European Stan
19、dard to the extent possible. At the end of the test, the user of this European Standard should take care to carry out an appropriate disposal of the wastes, according to local regulation. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countri
20、es are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Polan
21、d, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 13999-2:2013EN 13999-2:2013 (E) 4 1 Scope This European Standard specifies a method for the determination of single volatile organic compounds (VOC) and of the total amount of volatile organic
22、compounds (TVOCEN13999) in the exhaust air of an emission test chamber after application of a low-solvent or solvent-free adhesive as defined in EN 923:2005+A1:2008. The method is based on use of a solid sorbent with subsequent desorption and gas chromatographic analysis. The method is applicable to
23、 measurement of non-polar and slightly polar VOC. 2 Normative references The 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 editi
24、on of the referenced document (including any amendments) applies. EN 1232, Workplace atmospheres - Pumps for personal sampling of chemical agents - Requirements and test methods EN 13999-1, Adhesives - Short term method for measuring the emission properties of low-solvent or solvent-free adhesives a
25、fter application - Part 1: General procedure EN ISO 16000-9, Indoor air - Part 9: Determination of the emission of volatile organic compounds from building products and furnishing - Emission test chamber method (ISO 16000-9) EN ISO 16017-1, Indoor, ambient and workplace air - Sampling and analysis o
26、f volatile organic compounds by sorbent tube/thermal desorption/capillary gas chromatography - Part 1: Pumped sampling (ISO 16017-1) ISO 16000-6, Indoor air - Part 6: Determination of volatile organic compounds in indoor and test chamber air by active sampling on Tenax TA sorbent, thermal desorption
27、 and gas chromatography using MS or MS-FID 3 Principle A sufficient volume of test chamber air is drawn with an appropriate flow through a sorbent tube (or several tubes in series) containing a solid sorbent. Volatile organic compounds (VOC) are retained by the sorbent tube, which is subsequently an
28、alysed in the laboratory. The VOC are desorbed from the sampling tube and transferred by a flow of inert carrier gas into a capillary gas chromatograph coupled to a mass spectrometric detector (MS) and to a flame ionisation detector (FID) or only to a mass spectrometric detector. 4 Reagents and mate
29、rials 4.1 Volatile organic compounds for calibration Compounds of gas chromatographic grade. 4.2 Methanol Methanol of gas chromatographic grade. BS EN 13999-2:2013EN 13999-2:2013 (E) 5 4.3 Sorbent material For general purpose, poly(2,6-diphenyl-p-phenylene oxide, particle size (0,18 to 0,25) mm i.e.
30、 (60 to 80) mesh (Tenax1)TA 1 or equivalent sorbent materials) shall be used. For the determination of very volatile carcinogenic organic compounds (e.g. vinyl chloride), Carbopack X 1)or equivalent sorbent materials as described in EN ISO 16017-1 shall be used. 4.4 Carrier gas Helium, argon or nitr
31、ogen with a purity 99,999 % or better. 5 Apparatus 5.1 Sorbent tubes Sorbent tubes made from stainless steel or glass that can be filled with at least 200 mg of Tenax TA sorbent (4.3) are used. For example, tubes with 6 mm external diameter, 5 mm internal diameter and 90 mm long fulfil the requireme
32、nt and are used in many commercial thermal desorbing devices. It is recommended to use unsilanised glass wool or other suitable mechanism, e.g. stainless steel frit to retain the sorbent in the tube and metal screw caps and polytetrafluoroethylene (PTFE) ferrules for closing the sorbent tube. Carbop
33、ack X (4.3) or equivalent tubes are filled as described in EN ISO 16017-1. 5.2 Sorbent tube unions Two sorbent tubes may be connected in series during sampling with metal screw cap couplings with PTFE ferrules. 5.3 Syringes A precision 10 l liquid syringe readable to 0,1 l. 5.4 Sampling pump The pum
34、p shall fulfil the requirements of EN 1232 or equivalent. 5.5 Tubing PE poly(ethylene) or PTFE tubing of appropriate diameter to ensure a leak-proof fit to both pump and sample tube. Sampling tubes shall not be used with plastic tubing other than PTFE upstream of the sorbent to avoid interference fr
35、om contaminants. 5.6 Flow meter calibrator Bubble meter or other appropriate suitable device for gas flow calibration. 5.7 Gas chromatograph A capillary gas chromatograph coupled to a mass spectrometric detector and to a flame ionisation detector or only to a mass spectrometric detector shall be use
36、d in accordance with EN ISO 16017-1 and ISO 16000-6. 1) Carbopack X and Tenax TA are examples of suitable products available commercially. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of this product. BS EN 13999-2:201
37、3EN 13999-2:2013 (E) 6 5.8 Thermal desorption apparatus Apparatus for two-stage thermal desorption of sorbent tubes and transfer of desorbed vapours via an inert gas flow into a gas chromatograph is required. A typical apparatus contains a mechanism for holding the tubes to be desorbed whilst they a
38、re heated and purged simultaneously with inert carrier gas. The desorption temperature and time is adjustable, as is the carrier gas flow rate. The apparatus may also incorporate additional features, such as automatic sample tube loading, leak testing, and a cold trap or another suitable device to c
39、oncentrate the desorbed sample. The desorbed sample, contained in the purge gas, is routed to the gas chromatograph and capillary column via a heated transfer line. 5.9 Injection facility for preparing standards by liquid spiking Use a commercially available unit for preparation of calibration stand
40、ards or any other device allowing reproducible preparation of calibration standards. 5.10 Emission test chamber An emission test chamber as described in EN 13999-1 or in EN ISO 16000-9 shall be used. 6 Procedure 6.1 Preparation of sampling tubes 6.1.1 Preconditioning Use commercially pre-cleaned sam
41、pling tubes containing Tenax TA or sampling tubes that are preconditioned and filled in the laboratory as described for Tenax TA in this clause. For special purposes such as determination of specific carcinogenic volatile organic compounds as foreseen in EN 13999-1, other sorbent materials as descri
42、bed in EN ISO 16017-1 can be taken. Remove trace impurities of manufactured Tenax TA before using it for VOC sampling. The success of the cleaning procedure is checked by performing analysis of the blank sorbent. Tube blanks are acceptable if no individual interfering artefact peaks exceed 2 ng and
43、if TVOC levels do not exceed 20 ng after subtraction of non-interfering VOC artefacts. NOTE Usually keeping the tubes at a temperature of (320 10) C for at least 3 h using carrier gas flow of 50 ml/min to 100 ml/min is sufficient. Pack one end of the sampling tubes with unsilanised glass wool or sta
44、inless steel gauze. Weigh the appropriate amount of adsorbent. Transfer the adsorbent into the tube e.g. using suction. Prior to storage or conditioning seal the open end of the tube in the same manner as was done with the other end. To maintain the sorption capacity of the sampling tube, use no les
45、s than 200 mg of sorbent per tube. 6.1.2 Conditioning Recondition the pre-cleaned sampling tubes prior to each use at temperature of (320 10) C for 30 min (Tenax TA) under inert carrier gas flow of 50 ml/min to 100 ml/min to remove trace organic volatiles possibly trapped on the tube. Analyse the tu
46、bes, using routine analytical parameters, to ensure that the thermal desorption blank is sufficiently small. If the blank is unacceptable, repeat the conditioning procedure. The tube blank is acceptable if no individual interfering artefact peaks exceed 2 ng and if TVOC levels do not exceed 20 ng af
47、ter subtraction of non-interfering VOC artefacts. If the blank is unacceptable, recondition the tubes by desorbing them for 10 min under a 50 ml/min to 100 ml/min flow rate of inert carrier gas at a BS EN 13999-2:2013EN 13999-2:2013 (E) 7 temperature 20 C higher than that used for analysis and then
48、repeat the analysis. If after repeated conditioning, the blank is still unacceptable, the tubes shall be re-packed. It is recommended to seal the conditioned sorbent tubes with metal screw caps fitted with PTFE ferrules and store the tubes in an emission free container at room temperature. Condition
49、ed sampling tubes should be used within two weeks. Tubes stored for more than two weeks should be reconditioned before sampling. If other sealing material than PTFE/metal is used then the tubes should be used for sampling within 1 week. 6.2 Test chamber air sampling Assemble the sampling line. Prepare the test chamber sampling port as described in EN 13999-1 or EN ISO 16000-9. If the sampling flow rate is determined with a calibrator, start the pump, note and record the sampling flow rate. Connect the sampler to the chamber sampling port,
