1、BSI Standards PublicationBS ISO 17299-4:2015Textiles Determination ofdeodorant propertyPart 4: Condensation sampling analysisBS ISO 17299-4:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 17299-4:2015.The UK participation in its preparation was entrusted t
2、o TechnicalCommittee TCI/80, Chemical testing of textiles.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 are responsible for its correctapplication. The Bri
3、tish Standards Institution 2015. Published by BSI StandardsLimited 2015ISBN 978 0 580 76088 4ICS 59.080.01Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 Januar
4、y 2015.Amendments issued since publicationDate Text affectedBS ISO 17299-4:2015 ISO 2015Textiles Determination of deodorant property Part 4: Condensation sampling analysisTextiles Dtermination des proprits du dodorant Partie 4: Analyse par condensation dchantillonnageINTERNATIONAL STANDARDISO17299-4
5、First edition2015-01-15Reference numberISO 17299-4:2015(E)BS ISO 17299-4:2015ISO 17299-4:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2015All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by a
6、ny 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 address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Ge
7、neva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 17299-4:2015ISO 17299-4:2015(E)Contents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Reagents 16 Apparatus and materials
8、 27 Test method . 37.1 Sampling of test specimen 37.2 Preparation of container 47.3 Preparation of odour chemical solution or master gas 47.4 Testing procedure . 47.4.1 Take three specimens from the sample for one test as shown in Table 1. . 47.5 Measurement of odour gas concentration 67.5.1 General
9、 67.6 Testing without specimen . 68 Calibration 69 Test result 69.1 Calculation of the concentration of the odour chemical . 69.2 Calculation of reduction rate for odour chemical . 710 Test report . 7Annex A (informative) Actual application of the thermal desorption GC-MS to the measurement of indol
10、e, isovaleric acid, and nonenal . 8Annex B (informative) Actual application of ion chromatography to the measurement of hydrogen sulfide 15Annex C (informative) Actual application of ion chromatography to the measurement of methyl mercaptan 19Annex D (informative) Practical example 22 ISO 2015 All r
11、ights reserved iiiBS ISO 17299-4:2015ISO 17299-4:2015(E)ForewordISO (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.
12、 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 Interna
13、tional Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the differ
14、ent 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.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
15、not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will 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 i
16、nformation given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT), s
17、ee the following URL: Foreword Supplementary information .The committee responsible for this document is ISO/TC 38, Textiles.ISO 17299 consists of the following parts, under the general title of Textiles Determination of deodorant property Part 1: General principle Part 2: Detector tube method Part
18、3: Gas chromatography method Part 4: Condensation sampling analysis Part 5: Metal-oxide semiconductor sensors method iv ISO 2015 All rights reservedBS ISO 17299-4:2015ISO 17299-4:2015(E)IntroductionThis part of ISO 17299 describes condensation sampling analyses to measure the very low concentration
19、of the odour chemicals which is assumed at the level of human olfactory perception threshold. ISO 2015 All rights reserved vBS ISO 17299-4:2015BS ISO 17299-4:2015Textiles Determination of deodorant property Part 4: Condensation sampling analysis1 ScopeThis part of ISO 17299 specifies a deodorant tes
20、ting method using analytical instruments after using condensation sampling methods for all textile products. This method is applicable to gaseous odour chemicals, such as indole, methyl mercaptan, hydrogen sulfide, isovaleric acid, and nonenal.2 Normative referencesThe following documents, in whole
21、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) applies.ISO 17299-1, Textiles Determination of deo
22、dorant property Part 1: General principle3 Terms and definitionsFor the purpose of this document, the following terms and definitions apply.3.1condensation samplingmethod for collecting gaseous odour chemicals at very low concentration levels, which are then condensed by analytical methods to higher
23、 concentration levels to facilitate detections of the chemicals4 PrincipleThe concentration of a gaseous odour chemical in a container with or without a textile specimen after a designated elapsed time is measured by instrumental devices. The reduction rate of concentration of gaseous odour chemical
24、s is calculated from the difference of average concentration data obtained from the container with specimen and from that without specimen. The test shall be done for each chemical individually.5 ReagentsUnless otherwise specified, analytical grade reagents are used.5.1 Ethanol, reagent with concent
25、ration of 99,5 %.5.2 Odour chemicals.5.2.1 Indole (C8H7N), reagent.5.2.2 Methyl mercaptan, at a certified concentration of 2,0 l/l 3 % in nitrogen diluent.5.2.3 Hydrogen sulfide (H2S), at a certified concentration of 2,0 l/l 3 % in nitrogen diluent.INTERNATIONAL STANDARD ISO 17299-4:2015(E) ISO 2015
26、 All rights reserved 1BS ISO 17299-4:2015ISO 17299-4:2015(E)5.2.4 Isovaleric acid (CH3)2CHCH2COOH, reagent with a purity of 98,0 %.5.2.5 Nonenal (C9H16O), reagent with a concentration of 95,0 % in ethanol solution.5.3 Diluent gas, nitrogen gas from nitrogen gas cylinder with a purity of at least 99,
27、99 %.6 Apparatus and materials6.1 Plastic bags, with a volume of 3 l, at least six plastic bags for one test (see ISO 17299-1).6.2 Micro syringe, capable of delivering 10 l of solution by an accuracy of 0,1 l.6.3 Heat sealer, used to seal open edge of plastic bag. The adhesive tape can be used as an
28、 alternative.NOTE A sealing attachment such as a linear binder can be used.6.4 Aspirator or vacuum pump, capable of evacuating remaining air from 3 l sealed plastic bag (refer to Figure 1, item 1).6.5 Adsorption tube, capable of being mounted on a thermal desorption instrument, and absolving condens
29、ed samples of testing chemicals.6.6 Thermal desorption instrument, capable of mounting an adsorption tube and baking it for cleaning at a temperature over 280 C with flow of inert gas.6.7 Impinger, capable of putting absorbing solution and condensing odour chemical of the gas sample supplied from th
30、e plastic bag (refer to Figure 1, item 2).6.8 Air pump, capable of drawing approximately 0,2 l per minute of a sample gas from a plastic bag into adsorption tube, impinger, etc. (refer to Figure 1, item 3).2 ISO 2015 All rights reservedBS ISO 17299-4:2015ISO 17299-4:2015(E)Key1 plastic bag with spec
31、imen2 impinger3 air pumpFigure 1 Sampling set-up6.9 Thermal desorption gas chromatography (GC) equipment, coupled with a thermal desorption instrument which can be heated up a temperature higher than 280 C and equipped with a flame photometer detector (FPD), a flame ionization detector (FID), or mas
32、s spectrometer (MS).6.10 Ion chromatography (IC) equipment, to analyse the testing solution of condensed sample in impinger.The detectors used are Conductivity Detector (CD).7 Test method7.1 Sampling of test specimenThe dimension or mass of specimen for textile products is shown in Table 1.Table 1 D
33、imension or mass of specimenKind Dimension or massFabrics (woven, knit, non-woven, and tapes) 250 cm2 12,5 cm2Yarns, fibres, and feather 2,5 g 0,125 gFor multi-layer products, the edge and the untreated layer (or the “not targeted” layer) may be covered with an aluminium sheet or the test specimen m
34、ay be folded in two with the untreated layers inward, in order to avoid contact of untreated layer with odorous atmosphere.Condition the specimen as specified in ISO 17299-1. ISO 2015 All rights reserved 3BS ISO 17299-4:2015ISO 17299-4:2015(E)7.2 Preparation of container7.2.1 Prepare six plastic bag
35、s with the capacity of 3 l, three plastic bags for testing with a specimen and three plastic bags for the control test without a specimen. Place adhesive tape on the plastic bag at the insertion point of the odour chemical.NOTE The capacity of plastic bag is 3 l for all testing methods.7.2.2 Clean t
36、he plastic bags used in this test using nitrogen gas or clean air, more than five times of taking gas in and out by filling gas of the plastic bag volume just before testing.7.3 Preparation of odour chemical solution or master gasPerform the test for each odour chemical independently. Prepare the od
37、our chemical solutions for the testing as indicated below.7.3.1 Indole solution.Dissolve 0,6 g of the indole reagent (5.2.1) in 100 ml of ethanol (5.1).7.3.2 Methyl mercaptanPrepare the master gas with 1 l/l of methyl mercaptan concentration by using the standard methyl mercaptan gas (5.2.2) and dil
38、uent gas (5.3).7.3.3 Hydrogen sulfidePrepare the master gas with 0,2 l/l of hydrogen sulfide concentration by using the standard hydrogen sulfide gas (5.2.3) and diluent gas (5.3).7.3.4 Isovaleric acid.7.3.4.1 Dilute isovaleric acid reagent (5.2.4) of 5 ml and make up to 100 ml by ethanol (5.1). 7.3
39、.4.2 Dilute the diluted solution of 1 ml and make up to 100 ml by ethanol (5.1).7.3.5 Nonenal.7.3.5.1 Dilute nonenal reagent (5.2.5) of 3,5 ml and make up to 100 ml by ethanol (5.1).7.3.5.2 Dilute the diluted solution of 0,6 ml and make up to 100 ml by ethanol (5.1).Perform the test for each odour c
40、hemical separately.7.4 Testing procedureThis is a test with specimens.7.4.1 Take three specimens from the sample for one test as shown in Table 1.7.4.2 Place the specimens in the plastic bag one by one, so as to spread them out as much as possible. See Figure 2.NOTE Curling and creasing of specimen
41、might be unavoidable.4 ISO 2015 All rights reservedBS ISO 17299-4:2015ISO 17299-4:2015(E)Figure 2 Specimen in a plastic bag7.4.3 Hold the specimen by clips from outside of bag to make easier operation. Then, seal the opened edge of the bag for insertion of specimen by using heat sealer (6.3).7.4.4 D
42、eaerate from the plastic bag as much as possible by using an aspirator or a vacuum pump (6.4).7.4.5 Insert 2,5 l of nitrogen gas or the odour testing gas prepared. Then, add the odour testing solution by using micro syringe into the dilution nitrogen gas. The injection needle is stung at the point o
43、f the attached adhesive tape. The insertion quantity is indicated in Table 2.7.4.6 When inserting the solution or gas, be careful not to touch the specimen. After inserting the chemical, close the hole of the needle with adhesive tape.Table 2 Insertion quantity of odour testing solution or gasIndole
44、Methyl mercaptanHydrogen sulfide Isovaleric acid NonenalOdour testing solution 2,5 l 2,5 l 2,5 lOdour testing gas - 2,5 l (1 l/l) 2,5 l (0,2 l/l) 7.4.7 Knead the bag 20 times.7.4.8 Place the plastic bag still for 2 h as a reaction time.7.4.9 After 2 h have elapsed, knead the bag 20 times.7.4.10 Conn
45、ect the outlet of the testing bag to either a plug of adsorption tube, or an impinger. ISO 2015 All rights reserved 5BS ISO 17299-4:2015ISO 17299-4:2015(E)7.4.11 Extract 2 l of the testing gas from the plastic bag using the air pump (6.8) at a rate of 0,2 l/min and deliver the testing gas into a con
46、densation sampling device as shown in Table 3.Lie the testing bag sprawled during delivery of the testing gas.Table 3 Testing gas sampling method and amountIndole Methyl mercaptanHydrogen sulfide Isovaleric acid NonenalGas condensation sampling methodadsorption tube impinger impinger adsorption tube
47、 adsorption tubeTesting gas amount 2,0 lIf using the activated carbon type adsorption tube, clean the tube by baking prior to testing.7.5 Measurement of odour gas concentration7.5.1 GeneralMount an adsorption tube after sampling of the odour chemical on a thermal-desorption GC, then measure the gas
48、concentration of the odour chemical. FID, FPD, or MS are available as the detector of GC.If using methyl mercaptan and hydrogen sulfide, the absorbing solution after sampling by impinger could be measured by an ion chromatography.7.6 Testing without specimenThis is a control test which is performed
49、following the instructions in 7.4 and 7.5 without a specimen. The number of tests shall be same as that for the testing with specimen, i.e. three.8 CalibrationPrepare three different concentration gases from the standard solution or master gas.Measure the standard solutions or gases using either thermal-desorption GC or ion chromatography. Then, plot the peak area data on a graph against the inserted quantity of the odour chemical which is calculated from the concentration. More
