The European method

Comparative Study of Two
Methods for Olfactory
Measurement
Triangle Odor Bag Method
and Dynamic Olfactometry
○ Saeko Amano , Hiroyuki Ueno
Tokyo Metropolitan Research Institute for Environmental
Protection
Outline of this presentation
1. Dilution accuracy between the European
method and the Japanese method using GC
and HPLC
2. Difference of odour threshold between the
European method and the Japanese method
3. Difference among 3 method
the European method, the Japanese method
and European-like Japanese method
Outline of this presentation
1. Dilution accuracy between the
European method and the
Japanese method using GC and
HPLC
2. Difference of odour threshold between the
European method and the Japanese method
3. Difference among 3 method
the European method, the Japanese method
and European-like Japanese method
1. Dilution accuracy between the European method and the Japanese method
Differences between the Japanese
method and the European method
The Japanese
method
The European
method
Dilution
Bag &
Syringe
Flow controller,
Needle valve, etc.
Presentation
Descending
Ascending
random
Step factor
3
2
Sniffing condition
Air in the bag
Air emanated from
port
Panel Selection
5 standard
solutions
n-Butanol
1. Dilution accuracy between the European method and the Japanese method
Sample, Dilution factor
Sample
Hydrogen
Sulfide
Hexanal
Propion
aldehyde
Dilution factor
The European
method
Dilution
No
factor
The Japanese
method
Dilution
factor
4
33
5
65
6
136
100
7
266
8
560
300
9
1032
30
1000
1. Dilution accuracy between the European method and the Japanese method
Analytical method
Make the original gas
Dilute with odor-free air according to
European method or Japanese method
Adsorb gas to cartridge
（SUPELCO DNPH)
Elute with acetnitrile
HPLC－UV
Aldehyde
Trap gas to cold
concentration tube
Heat tube and inject to GC
GC-FPD
Hydrogen Sulfide
1. Dilution accuracy between the European method and the Japanese method
Result of dilution test -1
( Hydrogen Sulfide)
Hydrogen Sulfide is hardly adsorbed
during the test .
Recovery (%)
150
◆ Dynamic
Olfactometer
（The European method)
125
100
■ Triangle Odor
Bag Method
（The Japanese method)
75
50
10
100
1000
Dilution Factor
10000
1. Dilution accuracy between the European method and the Japanese method
Result of dilution test -2
( Hexanal)
The Japanese method have nice recovery when
dilution factor is more than 300.
The European method nearly get good recovery of
each dilution factor.
Recovery (%)
200
◆ Dynamic
Olfactometer
（The European method)
150
100
■ Triangle Odor
Bag Method
（The Japanese method)
50
0
10
100
1000
Dilution Factor
10000
1. Dilution accuracy between the European method and the Japanese method
Result of dilution test -3
( Propion aldehyde)
Recovery (%)
The result is as same as that of hexanal .
150
◆ Dynamic
Olfactometer
（The European method)
100
■ Triangle Odor
Bag Method
（The Japanese method)
50
0
10
100
1000
Dilution Factor
10000
1. Dilution accuracy between the European method and the Japanese method
Conclusion of dilution accuracy test
The difference of dilution accuracy between the European
method and the Japanese method was shown by using
Hydrogen Sulfide, hexanal and propionaldehyde as samples.
Concerning hydrogen sulfide, both method could get almost
100% recovery.
About aldehyde containing hexanal and propionaldehyde,
recovery varied a little widely at the European
method ,however, the European method nearly got good
recovery . On the other hand, the Japanese method didn’t get
good result when their dilution value was lower. But when
dilution factor was more than 300, the Japanese method had
good recovery as to the European method.
Outline of this presentation
1. Dilution accuracy between the European
method and the Japanese method using GC
and HPLC
2. Difference of odour threshold
between the European method and
the Japanese method
3. Difference among 3 method
the European method, the Japanese method
and European-like Japanese method
2.Difference of odour threshold between two method for olfactory measurement
odorant
 n-butanol
 Hexanal
Standard odourants of
the European method
Odour quality
Smell of cutting grass
 Hydrogen Sulfide
Smell of rotten egg
 Trimethylamine
Smell of rotten fish
 Isobutyric acid
smell of stinking socks,
smell of natto
 Ethyl Acetate
Smell of thinner
Standard odourants of
the Japanese methos
2.Difference of odour threshold between two method for olfactory measurement
Olfactory measurement
Measurements by both method for each
odourant were performed in a same day
using same panel members
Number of Measurement : 3~
2.Difference of odour threshold between European method and Japanese method
Result of odour threshold
measurement
Except for isobutyric acid, threshold of the European
method are higher than that of the Japanese method
Dynamic
Olfactmetry
n-butanol
Hexanal
Ethyl Acetate
Hydrogen Sulfide
Trimethyl amine
Isobutyric acid
4.8
3.4
3.1
3.1
3.1
3.6
Triangle odor
bag method
4.1
2.4
2.6
2.5
2.7
4.0
log Threshold (ppｔ)
2.Difference of odour threshold between European method and Japanese method
Result of odour threshold
measurement
Concentrations of threshold measured by the European
method are about 3-9 times higher than that measured
by the Japanese method except for butyric acid.
Dynamic
Olfactmetry
(A)
n-butanol
Hexanal
Ethyl Acetate
Hydrogen Sulfide
Trimethyl amine
Isobutyric acid
75
2.9
1389
1.5
1.7
4
Triangle odor
Proportion
bag method
(A/B)
(B)
14
0.3
384
0.3
0.5
11
5.3
9.0
3.6
4.5
3.2
0.4
Threshold (ppｂ)
2.Difference of odour threshold between two method for olfactory measurement
Standard deviation of odour
threshold
Standard division of each sample is also same between
two method.
Dynamic
Triangle odor
Olfactmetry
bag method
n-butanol
0.1
0.3
Hexanal
Ethyl Acetate
Hydrogen Sulfide
Trimethyl amine
Isobutyric acid
0.2
0.2
0.4
0.2
0.2
0.1
0.2
0.2
0.1
0.1
Standard deviation
2.Difference of odour threshold between two method for olfactory measurement
Summary of odour threshold’s
difference
Olfactory measurement was done using 6
odour substances.
Except for isobutyric acid, concentrations of
threshold measured by the European method
are about 3-9 times higher than that
measured by the Japanese method.
Standard division are also same between two
methods.
Outline of this presentation
1. Dilution accuracy between the European
method and the Japanese method using GC
and HPLC
2. Difference of odour threshold between the
European method and the Japanese method
3. Difference among 3 method
the European method, the Japanese
method and European-like Japanese
method
3. Difference among three methods
Differences between Japanese
method and European method
Dilution
Presentation
The Japanese
method
Bag & Syringe
The European
method
Flow controller,
Needle valve, etc.
Descending
Ascending random
Step factor
3
2
Forced choice
3
2
Sniffing condition
Air in the bag
Air emanated from
port
Panel Selection
5 standard
solutions
n-Butanol
3. Difference among three methods
Condition of experiment
European-like
The European The Japanese
Japanse
method
method
method
Flow
controller,
Dilution
Bag & Syringe Bag & Syringe
Needle valve,
etc.
Ascending
Ascending
Presentation
Descending
random
random
Step factor
2
3
2
Forced choice
2
3
2
Sniffing
condition
Air emanated
Air in the bag Air in the bag
from port
3. Difference among three methods
Condition of experiment
European-like
The European The Japanese
Japanse
method
method
method
Flow
controller,
Dilution
Bag & Syringe Bag & Syringe
Needle valve,
etc.
Ascending
Ascending
Presentation
Descending
random
random
Step factor
2
3
2
Forced choice
2
3
2
Sniffing
condition
Air emanated
Air in the bag Air in the bag
from port
3. Difference among three methods
Samples and Panels
Samples
n-butanol
Source sample of offset printing
(mixture of odour)
Panel members
12 persons
(divide 2 groups and 6 members each)
Measurements
Each measurement was done one time in a
day and repeated four days
3. Difference among three methods
Differences among 3 methods
(offset printing smell)
50
10 x log Odour
concentration
Low ←Sensitivity → High
European-like Japanese method had same log odour conc. as
the European method and lower than the Japanese method.
40
30
20
The1
European
method
The
2
Japanese
method
European-like
3
Japanese method
3. Difference among three methods
Differences among 3 methods
(n-butanol)
0
log Threshold (ppb)
Low ←Sensitivity → High
Sensitivity of European-like Japanese method is
lower than the Japanese method.
1
2
3
The
European
method
1
The
Japanese
method
2
European-like
Japanese method
3
3. Difference among three methods
Results of odour threshold in this year’s
( n-butanol)
0
log Threshold (ppb)
Low ←Sensitivity → High
Sensitivity by Japanese method are higher than that by
European method. This result show same trend as that of
offset printing
1
2
3
4
1
2
3
First time
Second time
◆The European method ■ The Japanese method
3. Difference among three methods
Summary of difference among 3 method
European-like Japanese
method( ascending presentation and two
forced choice mode) was compared with
the European method and the Japanese
method.
Sensitivity of European-like Japanese
method is lower than the Japanese
method
Conclusion(1/2)
Dilution accuracy of hydrogen sulfide and
aldehyde is good on both method when
dilution factor is more than 300.
Concentrations of threshold measured by
the European method are 3-9 times
higher than that measured by the
Japanese method
European-like Japanese method had
same threshold as the European method.
Conclusion(2/2)
These results shows that deference between
Japanese and European methods is mainly
caused by the definition of the threshold, not by
dilution method or materials.
Main reason may be as follows: Answer of
panelist is recognized as “true” when “correct
and certain” is observed in the European
method while the Japanese method recognize
the answer as “true” whenever it is correct.
Future Plan
Study of difference in race.
( We take a test in Poland on and after tomorrow with
your help, and compared with the result in Japanese)
research dilution accuracy of Isobutyric
acid
END
Thank you for your attention
Conclusion
Dilution accuracy of hydrogen sulfide is good on
both method. Concerning hexanal, the
European method is almost well and the
Japanese method as same as that one which is
limited dilution factor to more than 300.
Except for isobutyric acid, concentration s of
threshold measured by the European method
are about 3-9 times higher than that measured
by the Japanese method
European-like Japanese method had same log
odour concentration as the European method in
the case of using off-set printing, but difference
that of using n-butanol.
2.Difference of odour thresold between European method and Japanese method
Result of odour thresold-2 (winter)
Log Threshold (ppｔ)
High ← Sensitivity of panel
→ low
Except for isobutyric acid, thresold of Europian
method are higher than that of Japanese method
7
6
5
4
3
2
1
Isobutyric
Ethyl
hexanal
hexanal
Isobutyric acid
Ethylacetate
Acid
Acetate
◆Dynamic Olfactometer ■ Triangle Odor Bag Method
n-Butanol
n-butanol
2.Difference of odour thresold between European method and Japanese method
Thresold of Europian method are higher than that of
Japanese method. But standard deviation are different.
5
Log Threshold (ppｔ)
High ← Sensitivity of panel
→ low
Result of odour thresold-1 (summer)
4
3
2
n-Butanol
n-butanol
hexanal
hexanal
Hydrogen Trimethyl
sulfide
amine
H ydrogen
Trim ethylam ine
sulfide
◆Dynamic Olfactometer ■ Triangle Odor Bag Method
3. Study of difference among three method
Main Points
におい袋を用いた、オルと同一の希釈倍数、
サンプルの出し方の方法をMethodAとし、オ
ル、におい袋法と比較した。
オフセット印刷臭については、Method Aと折
るファクトメーターは同一の臭気濃度をしめし
た。
ブタノールについてはMethodAのみ高い閾
値を示し、オルファクトとにおいは差がなかっ
た。
2点比較と3点比較
臭袋法４
２倍系列上昇法
臭袋法５
２倍系列上昇法
３点比較
２点比較
2.0
2.0
0.34
0.27
0.29
0.25
3.3
3.3
0.32
0.22
0.26
0.29
n-ブタノール
個人閾値の全平均
(ppbの対数）
標準偏差（個人間）
標準偏差（個人内）
オフセット印刷臭
個人閾値の全平均
（希釈倍数の対数）
標準偏差（個人間）
標準偏差（個人内）
3. Study of difference among three method
Differences among 3 methods
Concering off-set printing, Method A had same log
odour conc. as European method and be different from
Japanese method. But as n-butanol, Log threshold of
method A is high among 3 methods.
European
method
Japanese
method
MethodA
1.6
1.6
2.0
3.2
3.8
3.3
n-butanol
Log Threshold (ppb)
Off-set printing
Log Odour Conc.
Caution!
High ← Sensitivity of panel
→ Low
Low
High
→ High
→ Low
←
←
log threshold (ppb)
log odor coc.
差異の要因の定量的検討
上昇法と下降法（閾値の定義（回答方法）の
違い）
２倍系列と３倍系列
３点比較と２点比較
実験方法
上昇法・下降法等の測定条件を変えて同一臭気を
同一パネルにより両手法によって測定
オルファクトメーターはハードウェア・ソフトウェアの
制約から条件の変更が難しいため、臭袋法の条件
を変更
各条件で1日１回ずつ合計４日間測定

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