ISO 17299-5:2014

Textiles — Determination of deodorant property — Part 5: Metal-oxide semiconductor sensor method

ISO 17299-5:2014 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 ISO 17299-5:2014 are a quasi sweat odour, a quasi body odour (nonenal mixture odour) and a quasi excrement odour. ISO 17299-5:2014 applies to all kinds of textile products, such as woven fabrics, knits, threads, yarns, fibres, braids, cords, etc.

Textiles — Détermination des propriétés de neutralisation d'odeurs — Partie 5: Méthode par capteur à semi-conducteur métal-oxyde

General Information

• Status: Published
• Publication Date: 16-Apr-2014
• ICS: 59.080.01 - Textiles in general
• Technical Committee: ISO/TC 38 - Textiles
• Drafting Committee: ISO/TC 38/WG 23 - Biological properties of textiles
• Current Stage: 9093 - International Standard confirmed
• Completion Date: 07-Oct-2019

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 17299-5
First edition
2014-04-15
Textiles — Determination of
deodorant property —
Part 5:
Metal-oxide semiconductor sensor
method
Textiles — Détermination de la propriété de déodorant —
Partie 5: Méthode par capteur à semi-conducteur métal-oxyde
Reference number
ISO 17299-5:2014(E)
©
ISO 2014

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ISO 17299-5:2014(E)

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
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Published in Switzerland
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ISO 17299-5:2014(E)

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents . 2
6 Apparatus and materials. 3
7 Preparation of the odour test gas . 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 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) Specifications of the odour test instrument .14
Annex C (informative) Practical testing results .17
Bibliography .26
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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 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. 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.
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
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 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 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 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 ISO’s 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 deodorant
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 method
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ISO 17299-5:2014(E)

Introduction
This part of ISO 17299 describes a test method 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.
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INTERNATIONAL STANDARD ISO 17299-5:2014(E)
Textiles — Determination of deodorant property —
Part 5:
Metal-oxide 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 body 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 principle
3 Terms and definitions
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 follows:
— 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 the rate of the odour chemical concentration in μl/l against the olfactory
threshold concentration
3
Note 1 to entry: It is expressed in OU/m .
3.3
olfactory threshold concentration
minimum concentration at which human could perceive
Note 1 to entry: Olfactory threshold concentration value of the odour chemical substances used in this part of
ISO 17299 is shown in Table 1.
Note 2 to entry: See Reference [1] in the Bibliography.
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Table 1 — Olfactory threshold concentration
Unpleasant odour Acetic Isovaleric Hydrogen Methyl mer-
Ammonia Nonenal Indole
components acid aicid sulfide captan
Olfactory threshold
1,5 0,006 0,000 078 0,000 08 0,000 41 0,000 07 0,000 3
concentration [μl/l]
3.4
metal-oxide semiconductor sensor
sensor using a metal-oxide semiconductor made of e.g. tin dioxide
Note 1 to entry: The response 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 the 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 vector 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 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 odour
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, reagent of 28 % in concentration of ammonia (NH ) in water.
3
5.2 Acetic acid, reagent of 99,7 % in concentration of acetic acid (CH COOH) in water.
3
5.3 Methyl mercaptan, 100 μl/l in concentration of standard gas by nitrogen dilution.
5.4 Hydrogen sulfide, 100 μl/l in concentration of standard gas by nitrogen dilution.
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5.5 Indole, indole (C H N) reagent.
8 7
5.6 Isovaleric acid, 98,0 % solution.
5.7 Nonenal, 2-nonenal (C H O) reagent (95,0 % solution).
9 16
5.8 Diluent gas, dry air obtained from nitrogen - oxygen mixture cylinder with 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 flow 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 μl.
6.5 Syringe, with a capacity of 200 ml.
6.6 Detector tube, with a concentration measurement range of 50 μl/l to 500 μl/l for ammonia.
6.7 Heat seal, capable of 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 cylinder.
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 plastic 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 Hydrogen sulfide and methyl mercaptan
7.1.3.1 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 at 80 °C for 10 min.
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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
Acetic Isovaleric Hydrogen Methyl mer-
Master gas Ammonia Nonenal Indole
acid acid sulfide captan
Master gas target
1 500 500 50 15 100 100 6
concentration [μl/l]
Diluent gas quantity
2 500 2 500 2 500 2 500 0 0 2 500
[ml]
Ammonia Acetic Isovaleric Hydrogen Methyl mer- Indole rea-
Materials of odour
Nonenal
water acid acid sulfide captan gent
components chemi-
(5.7)
cals
(5.1) (5.2) (5.6) (5.4) (5.3) (5.5)
Quantity of injection
odour component 10 μl 5 μl 2 μl 5 μl 2 500 ml 2 500 ml 0,3 g powder
chemicals
Dilute to
1/10 and
Inspection No action
use detec-
tor tube
7.2 Preparation of the test quasi unpleasant odours
The compositions of the quasi unpleasant odours are shown in Table 3. The compositions give the initial
concentration of odour chemicals for test.
Table 3 — Composition of chemicals in the quasi unpleasant odours
Total
Composition of chemicals for master gas (ml)
(ml)
Unpleasant odour com-
ponents
Acetic Isovaleric Hydrogen Methyl Diluent
Ammonia Nonenal Indole
acid acid sulfide mercaptan gas
Sweat
50 250 500 - - - - 1 700 2 500
odour
Body
Quasi odour
unpleasant (nonenal 50 250 500 830 - - - 870 2 500
odour mixture
odour)
Excrement
50 250 - - 100 200 1 250 650 2 500
odour
Initial concentration of
30 50 10 5 4 8 3
components [μl/l]
7.2.1 Preparation of the quasi sweat 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 plastic bag by using the syringe (6.5) according to Table 3. See Figure 1.
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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 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.
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 hydrogen
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 odour 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 unpleasant 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.
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Table 4 — Odour unit concentration for the component chemicals
Unpleasant odour Isovaleric Hydrogen Methyl mer-
Ammonia Acetic acid Nonenal Indole
components aicid sulfide captan
Olfactory thresh-
old concentration 1,5 0,006 0,000 078 0,000 08 0,000 41 0,000 07 0,000 3
[μl/l] (a)
Initial concentra-
tion of compo- 30 50 10 5 4 8 3
nents [μl/l] (b)
Odour unit concen-
20 8 333 128 205 62 500 9 756 114 286 10 000
tration (b)/(a)
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
Odour unit concentration for selection
Quasi
quasi
unpleasant
Acetic Isovaleric Hydrogen Methyl mer-
unpleasant Ammonia Nonenal Indole
odour
acid acid sulfide captan
odours
Sweat odour 128 205 20 8 333 128 205
Body odour
(non-
128 205 20 8 333 128 205 62 500
enal mixture
odour)
Excrement
114 286 20 8 333 9 756 114 286 10 000
odour
9.3 Creation of calibration curve for quasi unpleasant odours
9.3.1 Preparation of dilution series
9.3.1.1 Clean 3 l of the plastic bags by using diluent gas.
9.3.1.2 Inject the master gas and diluent gas with the amount shown in Table 6 by using the air pump
into the plastic bags.
Table 6 — Mixing recipe for dilution series
Dilution series master gas (ml) diluent gas (ml) Total (ml)
Initial concentration 2 500 0 2 500
1/3 830 1 670
1/10 250 2 250
1/100 25 2 475
9.3.2 Measurement
Obtain the response values for dilution series of all quasi unpleasant odours by using the odour test
instrument.
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ISO 17299-5:2014(E)

9.3.3 Calibration curves
9.3.3.1 Calculate the response vector length by square-root of sum of squares from all response values
for all dilution series.
9.3.3.2 Obtain the calibration curves of quadratic approximation between the calculated vector lengths
and the odour unit concentrations. An example is shown in Annex A.
NOTE Because of a quadratic curve, the differential equation of the calibration equation gives the specific
response vector length value for the minimum odour unit concentration at zero. To validate this test, the obtained
vector length from the test may be larger than the specific vector length value.
10 Deodorant test
10.1 Preparation of test specimen
The dimension or mass of test specimens is shown in Table 7.
Table 7 — Dimension or mass of test specimens
Type Dimension or mass
2 2
Cloth (woven, knitted, non-woven and tape) 100 cm ± 5 cm
Yarn, fibre and feather 1,0 g ± 0,05 g
In case of products consisting of multi-layers, it is recommended to cover the parts not intended for this
test by aluminium foil in order to avoid any unintended effect. The specimen can be folded in half so as
to place the part not intended for test inside.
10.2 Conditioning of the specimen
Condition the specimen as specified in ISO 17299-1.
10.3 Test procedure
10.3.1 Preparation of plastic bags
Prepare six plastic bags (6.1), three plastic bags for the test with specimen and three plastic bags for the
test without specimen and clean the plastic bags by using diluent gas before testing.
10.3.2 Insertion of specimen
Place the test specimen in three plastic bags one by one so as to spread as much as possible.
In case the specimen is curled, smooth the specimen as much as possible.
10.3.3 Removal of air from the plastic bags
Remove any remaining air from the plastic bags with specimen after heat seal by using the inlet of
plastic bags as much as possible. To do so, place the specimen near the inlet to make easy removal of air.
10.3.4 Injection of testing gas
Inject 2 500 ml of the testing gas i.e. the quasi unpleasant odour into the plastic bag with and without
specimen. See Figure 2.
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ISO 17299-5:2014(E)

Figure 2 — After injection of quasi unpleasant odour gas in plastic bags with or without
specimen
10.3.5 Reaction time
Place the testing plastic bags for 2 h after injection of test gas.
10.3.6 Measurement by using the odour test instrument
Measure the test gas after the reaction time of 2 h by using the odour test instrument for both the
test gases with and without specimen. Carry out three measurements for both the test gases with and
without specimen.
11 Calculation of the odour unit concentration
11.1 Calculate the vector lengths for all tests by the square root of sum of squares from the all sensor
response values.
11.2 Average three calculated vector lengths for both test gases with and without specimen
respectively.
11.3 Calculate the odour unit concentration from the calibration curve.
11.4 The odour unit concentration of the test gas without specimen is denoted by B and with specimen
is denoted by A.
12 Calculation of reduction rate
Calculate the reduction rate of quasi unpleasant odour by using the following equation:
()BA−
ORR= ×100
B
where
ORR is the reduction rate of quasi unpleasant odour in percentage;
B is the odour unit concentration of the test gas without specimen;
A is the odour unit concentration of test gas with specimen.
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ISO 17299-5:2014(E)

13 Test report
The following items are at least recorded in the test report:
a) a reference to this part of ISO 17299 (i.e. ISO 17299-5);
b) details of the sample for test;
c) name of quasi unpleasant odour;
d) reduction rate;
e) any deviation from this part of ISO 17299.
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ISO 17299-5:2014(E)

Annex A
(informative)

Example of the test
A.1 General
This is an example of the deodorant test using the quasi sweat odour according to this part of ISO 17299.
A.2 Test sample
— deodorant treatment; sweat odour deodorant chemicals,
— material: polyester,
— structure: plain woven fabric, tropical,
2
— mass: 158 g/m .
A.3 Quasi unpleasant odour
Quasi sweat odour. Prepared as specified in 7.2.1.
A.4 Odour test instrument
The odour test instrument with 10 metal-oxide semiconductor sensors was used.
A.5 Sensor response check
The sensor response check was done for component chemicals at the initial concentration of the quasi
sweat odour individually.
The response of all sensors was confirmed as appropriate as shown in Table A.1.
Table A.1 — Response check for all component chemicals of the quasi sweat odour
Concen- Response
tration Response data of each sensors vector
Odour compo-
[μl/l] length
nent chemicals
CH1 CH2 CH3 CH4 CH5 CH6 CH7 CH8 CH9 CH10
Ammonia 30 0,290 0,802 0,417 0,190 0,368 0,616 0,269 0,386 0,243 0,820 1,551
Acetic acid 50 0,381 0,887 0,793 0,172 0,689 0,806 0,931 0,818 0,423 1,010 2,334
Isovaleric acid 10 0,275 0,470 0,637 0,105 0,551 0,541 0,624 0,533 0,365 0,588 1,569
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A.6 Calibration curves preparation
A.6.1 Odour unit concentration of the quasi sweat odour
The odour unit concentration of quasi sweat odour is determined as in Table 5 as an initial concentration.
So, the odour unit concentrations for the dilution are given in Table A.2. The calculation of the odour unit
concentrations is simple as the initial value multiplied by the dilution rate.
Table A.2 — Odour unit concentration for the quasi sweat odour
Unpleasant odour components Quasi sweat odour
Odour unit concentration Initial 128 205
[μl/l] 1/3 dilution 42 735
1/10 dilution 12 820
1/100 dilution 1 282
A.6.2 Test for the calibration curve
The test to create the calibration curves was carried out according to 9.3.
Table A.3 — Response data for the quasi sweat odour dilution series
Response value from each sensor
Quasi sweat
odour
CH1 CH2 CH3 CH4 CH5 CH6 CH7 CH8 CH9 CH10
Initial 0,385 1,058 0,698 0,235 0,602 0,824 0,830 0,833 0,390 1,115
1/3 dilution 0,277 0,562 0,474 0,144 0,352 0,617 0,520 0,519 0,317 0,647
1/10 dilution 0,229 0,367 0,235 0,126 0,171 0,543 0,277 0,324 0,230 0,424
1/100 dilution 0,207 0,317 0,082 0,122 0,057 0,524 0,151 0,221 0,162 0,351
A.6.3 Creation of the calibration curves
A.6.3.1 Calculation of the response vector length
The calibration curve is to obtain the relationship between response vector length and odour unit
concentration.
The response vector length is calculated from data in Table A.3 using Formula (A.1). The result is shown
in Table A.4 with the odour unit concentration from Table A.2.
22 22 22 22 22
ZC=+()HC12()HC++()HC34()HC++()HC56()HC++()HC78()H +(()CH91+()CH 0 (A.1)
where
Z is the response vector length;
CH1 to CH10 is the response value from each sensor.
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Table A.4 — Calculated vector lengths for the quasi sweat odour
Quasi sweat odour Odour unit concentration Response vector length
Initial 128 205 2,373
1/3 dilution 42 735 1,484
1/10 dilution 12 820 0,998
1/100 dilution 1 282 0,815
A.6.3.2 Calibration curve
The calibration curve (see Figure A.1) is calculated by using proper statistic calculation soft with the
quadratic approximation as follows.
140000
120000
100000
80000
60000
40000
20000
0
0 2,5
0,51 1,52
Response vector length
Figure A.1 — Calibration curve of quasi sweat odour
The calibration Formula (A.2) obtained here is as follows:
2
YX=−30849 18846X (A.2)
where
Y is an odour unit concentration;
X is a response vector length.
The specific response vector length at the minimum of the odour unit concentration is given by the
differential equation as follows:
dY 18 846
=×230 849X−=18 846 0 , then =0,305 (A.3)
dX 61 698
NOTE This value was referred to the test value.
A.7 Deodorant test
The deodorant test was performed according to Clause 10. The ten response values for the test with and
without specimen were obtained and vector lengths were calculated as shown in Table A.5.
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Table A.5 — Result of deodorant test without specimen and response vector length
Response data of each sensors Response
Deodorant
vector
test
CH1 CH2 CH3 CH4 CH5 CH6 CH7 CH8 CH9 CH10
length
Without
0,364 0,923 0,662 0,196 0,563 0,744 0,788 0,756 0,380 0,989 2,156
specimen
With speci-
0,232 0,407 0,277 0,125 0,202 0,534 0,308 0,356 0,236 0,455 1,059
men
The minimum value is 1,
...