1、 ISO 2014 Textiles Determination of deodorant property Part 5: Metal-oxide semiconductor sensor method Textiles Dtermination de la proprit de dodorant Partie 5: Mthode par capteur semi-conducteur mtal-oxyde INTERNATIONAL STANDARD ISO 17299-5 First edition 2014-04-15 Reference number ISO 17299-5:2014
2、(E) ISO 17299-5:2014(E)ii ISO 2014 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2014 All rights reserved. Unless 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
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4、iso.org Web www.iso.org Published in Switzerland ISO 17299-5:2014(E) ISO 2014 All rights reserved iii Contents Page Foreword iv Introduction v 1 Scope . 1 2 Normative references 1 3 T erms and definitions . 1 4 Principle 2 5 Reagents 2 6 Apparatus and materials 3 7 Preparation of the odour test gas
5、. 3 7.1 Master gas . 3 7.2 Preparation of the test quasi unpleasant odours 4 8 Sensor response check . 5 9 Preparation of calibration curve . 5 9.1 Initial concentration . 5 9.2 Odour unit concentration for quasi unpleasant odours 5 9.3 Creation of calibration curve for quasi unpleasant odours 6 10
6、Deodorant test 7 10.1 Preparation of test specimen 7 10.2 Conditioning of the specimen 7 10.3 Test procedure . 7 11 Calculation of the odour unit concentration . 8 12 Calculation of reduction rate . 8 13 Test report . 9 Annex A (informative) Example of the test .10 Annex B (informative) Specificatio
7、ns of the odour t est instrument .14 Annex C (informative) Practical testing results .17 Bibliography .26 ISO 17299-5:2014(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Internatio
8、nal 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
9、, 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 intended for its further maintenance are described in the ISO/IEC Directives, Par
10、t 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.iso.org/directives). Attention is drawn to the possibility that some of the
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12、eived (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 expressions related to conformity assessment, as well as information about ISOs
13、adherence to the WTO principles in the Technical Barriers to Trade (TBT) see 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 Textiles Determination of deodo
14、rant property: Part 1: General principle Part 2: Detector tube method Part 3: Gas chromatography method Part 4: Condensation sampling analysis Part 5: Metal-oxide semiconductor sensor methodiv ISO 2014 All rights reserved ISO 17299-5:2014(E) Introduction This part of ISO 17299 describes a test metho
15、d using a testing instrument equipped with multiple metal- oxide semiconductor sensors against composite odours for all textiles. The multiple sensors improve accuracy for several kinds of composite odours. ISO 2014 All rights reserved v Textiles Determination of deodorant property Part 5: Metal-oxi
16、de semiconductor sensor method 1 Scope This part of ISO 17299 specifies a deodorant test method using an odour analyser equipped with multiple metal-oxide semiconductor sensors against composite odours. The artificial composite odours used in this part of ISO 17299 are a quasi sweat odour, a quasi b
17、ody odour (nonenal mixture odour) and a quasi excrement odour. This part of ISO 17299 applies to all kinds of textile products, such as woven fabrics, knits, threads, yarns, fibres, braids, cords, etc. 2 Normative references ISO 17299-1, Textiles Determination of deodorant property Part 1: General p
18、rinciple 3 T erms a nd definiti ons For the purposes of this document, the following terms and definitions apply. 3.1 quasi unpleasant odour artificial composite odour used to simulate an unpleasant odour Note 1 to entry: Artificial composite odours for the purpose of this part of ISO 17299 are as f
19、ollows: quasi sweat odour: ammonia, acetic acid, isovaleric acid; quasi body odour (nonenal mixture odour): ammonia, acetic acid, isovaleric acid, nonenal; quasi excrement odour: ammonia, acetic acid, hydrogen sulfide, methyl mercaptan, indole. 3.2 odour unit concentration concentration defined as t
20、he rate of the odour chemical concentration in l/l against the olfactory threshold concentration Note 1 to entry: It is expressed in OU/m 3 . 3.3 olfactory threshold concentration minimum concentration at which human could perceive Note 1 to entry: Olfactory threshold concentration value of the odou
21、r chemical substances used in this part of ISO 17299 is shown in Table 1. Note 2 to entry: See Reference 1 in the Bibliography. INTERNATIONAL ST ANDARD ISO 17299-5:2014(E) ISO 2014 All rights reserved 1 ISO 17299-5:2014(E) Table 1 Olfactory threshold concentration Unpleasant odour components Ammonia
22、 Acetic acid Isovaleric aicid Nonenal Hydrogen sulfide Methyl mer- captan Indole Olfactory threshold concentration l/l 1,5 0,006 0,000 078 0,000 08 0,000 41 0,000 07 0,000 3 3.4 metal-oxide semiconductor sensor sensor using a metal-oxide semiconductor made of e.g. tin dioxide Note 1 to entry: The re
23、sponse of sensors corresponds to gas chemical concentration. The blend recipe of the constituent metal-oxide gives different response trend to chemicals. 3.5 odour test instrument instrument equipped with multiple metal-oxide semiconductor sensors Note 1 to entry: This instrument is built up with th
24、e inlet of the testing gas, sensors, and cleaning system of sensor head. 3.6 response value value obtained as outputs from sensors 3.7 response vector vector for a quasi unpleasant odour consisting of response value obtained from each sensor separately 3.8 response vector length length obtained as v
25、ector sum which is calculated as square-root of sum of squares of response values Note 1 to entry: The length represents a proportional amount of chemical concentration. 3.9 calibration curve curve that determines odour unit concentration corresponding to response vector length Note 1 to entry: The
26、quadratic curve is used for this calibration curve derived from Reference 2 as proximity. 4 Principle The quasi unpleasant odour gas is inserted in plastic bags with test specimen or without specimen. After 2 h reaction time, the odour unit concentration of remained gases is obtained by using an odo
27、ur test instrument with 10 metal-oxide semiconductor sensors. The reduction rate in odour chemical concentration is calculated from the odour unit concentration with and without specimen. 5 Reagents Unless otherwise specified, analytical grade reagents shall be used in this test. 5.1 Ammonia water,
28、reagent of 28 % in concentration of ammonia (NH 3 ) in water. 5.2 Acetic acid, reagent of 99,7 % in concentration of acetic acid (CH 3 COOH) in water. 5.3 Methyl mercaptan, 100 l/l in concentration of standard gas by nitrogen dilution. 5.4 Hy d r o g en s u l f i d e, 100 l/l in concentration of sta
29、ndard gas by nitrogen dilution.2 ISO 2014 All rights reserved ISO 17299-5:2014(E) 5.5 Indole, indole (C 8 H 7 N) reagent. 5.6 Isovaleric acid, 98,0 % solution. 5.7 Nonenal, 2-nonenal (C 9 H 16 O) reagent (95,0 % solution). 5.8 Diluent gas, dry air obtained from nitrogen - oxygen mixture cylinder wit
30、h purity of at least 99,999 9 % or, nitrogen gas from nitrogen gas cylinder with purity of at least 99,999 9 %. 6 Apparatus and materials Unless otherwise specified, the following shall be used in this test. 6.1 Plastic bag, 3 l in capacity with a glass tube as inlet of gas. 6.2 Air pump, with a flo
31、w meter or an integrating flow meter for 3 l/min flow rate. 6.3 Oven, capable of operating at 80 C. 6.4 Micro-syringe, with a capacity of 10 l. 6.5 Syringe, with a capacity of 200 ml. 6.6 Detector tube, with a concentration measurement range of 50 l/l to 500 l/l for ammonia. 6.7 Heat seal, capable o
32、f sealing a plastic bag. 6.8 Aspirator or vacuum pump. 6.9 Odour test instrument, with 10 metal-oxide semiconductor sensors. 7 Preparation of the odour test gas The odour test gases are prepared just before the test. Master gases and the quasi unpleasant odours may be prepared by permeator or gas cy
33、linder. 7.1 Master gas 7.1.1 Clean 3 l of plastic bags (6.1) by using the diluent gas, then the preparation of master gases of odour component chemicals is as described in 7.1.2 to 7.1.4. 7.1.2 Ammonia, acetic acid, isovaleric acid, and nonenal 7.1.2.1 Inject 2,5 l of the diluent gas into the plasti
34、c bags (7.1.1). 7.1.2.2 Inject the chemical solution with the amount according to Table 2 into plastic bags prepared in 7.1.2.1. 7.1.2.3 Keep the plastic bags with the prepared gas under the test environment for 30 min. 7.1.3 H y d r o g e n s u l f i d e a n d m e t h y l m e r c a p t a n 7.1.3.1
35、Inject the chemical standard gases with the amount according to Table 2 into plastic bags. 7.1.4 Indole 7.1.4.1 Put the specified amount of indole powder into a plastic bag (6.1) according to Table 2. 7.1.4.2 Inject 2,5 l of dilute gas in the plastic bag. 7.1.4.3 Heat the plastic bag for sublimation
36、 at 80 C for 10 min. ISO 2014 All rights reserved 3 ISO 17299-5:2014(E) 7.1.4.4 Transfer all gas of 7.1.4.3 to new plastic bag. Table 2 Master gas concentration of unpleasant odour components and manufacture method Master gas Ammonia Acetic acid Isovaleric acid Nonenal Hydrogen sulfide Methyl mer- c
37、aptan Indole Master gas target concentration l/l 1 500 500 50 15 100 100 6 Diluent gas quantity ml 2 500 2 500 2 500 2 500 0 0 2 500 Materials of odour components chemi- cals Ammonia water (5.1) Acetic acid (5.2) Isovaleric acid (5.6) Nonenal (5.7) Hydrogen sulfide (5.4) Methyl mer- captan (5.3) Ind
38、ole rea- gent (5.5) Quantity of injection odour component chemicals 10 l 5 l 2 l 5 l 2 500 ml 2 500 ml 0,3 g powder Inspection Dilute to 1/10 and use detec- tor tube No action 7.2 Preparation of the test quasi unpleasant odours The compositions of the quasi unpleasant odours are shown in Table 3. Th
39、e compositions give the initial concentration of odour chemicals for test. Table 3 Composition of chemicals in the quasi unpleasant odours Unpleasant odour com- ponents Composition of chemicals for master gas (ml) Tot al (ml) Ammonia Acetic acid Isovaleric acid Nonenal Hydrogen sulfide Methyl mercap
40、tan Indole Diluent gas Quasi unpleasant odour Sweat odour 50 250 500 - - - - 1 700 2 500 Body odour (nonenal mixture odour) 50 250 500 830 - - - 870 2 500 Excrement odour 50 250 - - 100 200 1 250 650 2 500 Initial concentration of components l/l 30 50 10 5 4 8 3 7.2.1 Preparation of the quasi sweat
41、odour 7.2.1.1 Clean a plastic bag (6.1) by using the diluent gas (5.8). 7.2.1.2 Inject 1,7 l of the diluent gas into the plastic bag by using the air pump (6.2). 7.2.1.3 Inject 500 ml of isovaleric acid master gas, 250 ml of acetic acid master gas and 50 ml of ammonia master gas in order into the pl
42、astic bag by using the syringe (6.5) according to Table 3. See Figure 1.4 ISO 2014 All rights reserved ISO 17299-5:2014(E) Figure 1 Injection of master gases 7.2.2 Preparation of quasi body odour (nonenal mixture odour) 7.2.2.1 Clean a plastic bag (6.1) by using the diluent gas (5.8). 7.2.2.2 Inject
43、 870 ml of the diluent gas into the plastic bag by using the air pump (6.2). 7.2.2.3 Inject 830 ml of nonenal master gas, 500 ml of isovaleric acid master gas, 250 ml of acetic acid master gas and 50 ml of ammonia master gas in order into the plastic bag by using syringe ( 6.5) according to Table 3.
44、 7.2.3 Preparation of quasi excrement odour 7.2.3.1 Clean a plastic bag (6.1) by using the diluent gas (5.8). 7.2.3.2 Inject 650 ml of the diluent gas into the plastic bag by using the air pump (5.2). 7.2.3.3 Inject 1 250 ml of indole master gas, 200 ml of methyl mercaptan master gas, 100 ml of hydr
45、ogen sulfide master gas, 250 ml of acetic acid master gas and 50 ml of ammonia master gas in order into the plastic bag by using syringe (6.5) according to Table 3. 8 Sensor response check To confirm the response of the sensors, the measurements are performed with all odour chemicals by using the od
46、our test instrument (6.9). If a sensor shows no response, replace the sensor and check again. 9 Preparation of calibration curve 9.1 Initial concentration The initial odour chemical concentrations of the test are shown in Table 3 for all component chemicals. 9.2 Odour unit concentration for quasi un
47、pleasant odours 9.2.1 Odour unit concentration for the initial concentration The odour unit concentration value is simply calculated by the initial concentration (b) divided by the olfactory threshold concentration (a) as shown in Table 4. ISO 2014 All rights reserved 5 ISO 17299-5:2014(E) Table 4 O
48、dour unit concentration for the component chemicals Unpleasant odour components Ammonia Acetic acid Isovaleric aicid Nonenal Hydrogen sulfide Methyl mer- captan Indole Olfactory thresh- old concentration l/l (a) 1,5 0,006 0,000 078 0,000 08 0,000 41 0,000 07 0,000 3 Initial concentra- tion of compo-
49、 nents l/l (b) 30 50 10 5 4 8 3 Odour unit concen- tration (b)/(a) 20 8 333 128 205 62 500 9 756 114 286 10 000 9.2.2 Odour unit concentration for the quasi unpleasant odour The largest odour unit concentration value of the component chemicals is selected as the odour unit concentration of the quasi unpleasant odour as shown in Table 5. Table 5 Odour unit concentration of the quasi unpleasant odours Quasi unpleasant odour Odour unit concentration for selection quasi un
