ODOR (2150)/Introduction 2-11

lined in s 2b and 4a for care and handling of sample cells, ties and discrepancies in turbidity measurements make it
degassing, and dealing with condensation. unlikely that results can be duplicated to greater precision
c. Measurement of turbidity: Gently agitate sample. Wait than specified.
until air bubbles disappear and pour sample into cell. When
possible, pour well-mixed sample into cell and immerse it in 6. Reference
an ultrasonic bath for 1 to 2 s or apply vacuum degassing,
causing complete bubble release. Read turbidity directly from 1. U.S. ENVIRONMENTAL PROTECTION AGENCY. 1993. Methods for Deter-
instrument display. mination of Inorganic Substances in Environmental Samples. EPA-
d. Calibration of continuous turbidity monitors: Calibrate con- 600/R/93/100 - Draft. Environmental Monitoring Systems Lab., Cin-
tinuous turbidity monitors for low turbidities by determining tur- cinnati, Ohio.
bidity of the water flowing out of them, using a laboratory-model
nephelometer, or calibrate the instruments according to manufac- 7. Bibliography
turers instructions with formazin primary standard or appropriate
secondary standard. HACH, C.C., R.D. VANOUS & J.M. HEER. 1985. Understanding Turbidity
Measurement. Hach Co., Technical Information Ser., Booklet 11,
5. Interpretation of Results Loveland, Colo.
KATZ, E.L. 1986. The stability of turbidity in raw water and its
Report turbidity readings as follows: relationship to chlorine demand. J. Amer. Water Works Assoc.
78:72.
Report to the MCCOY, W.F. & B.H. OLSON. 1986. Relationship among turbidity,
Turbidity Range Nearest particle counts and bacteriological quality within water distribution
NTU NTU lines. Water Res. 20:1023.
BUCKLIN, K.E., G.A. MCFETERS & A. AMIRTHARAJAH. 1991. Penetration
01.0 0.05
of coliform through municipal drinking water filters. Water Res.
110 0.1
25:1013.
1040 1
HERNANDEZ, E., R.A. BAKER & P.C. CRANDALL. 1991. Model for evalu-
40100 5
ating turbidity in cloudy beverages. J. Food Sci. 56:747.
100400 10
HART, V.S., C.E. JOHNSON & R.D. LETTERMAN. 1992. An analysis of
4001000 50
low-level turbidity measurements. J. Amer. Water Works Assoc.,
1000 100
84(12):40.
LECHEVALLIER, M.W. & W.D. NORTON. 1992. Examining relationship
When comparing water treatment efficiencies, do not esti- between particle counts and Giardia, Cryptosporidium, and turbid-
mate turbidity more closely than specified above. Uncertain- ity. J. Amer. Water Works Assoc. 84(12):54.

2150 ODOR*

2150 A. Introduction

1. Discussion Odor is recognized1 as a quality factor affecting acceptability

of drinking water (and foods prepared with it), tainting of fish
Odor, like taste, depends on contact of a stimulating substance and other aquatic organisms, and esthetics of recreational waters.
with the appropriate human receptor cell. The stimuli are chem- Most organic and some inorganic chemicals contribute taste or
ical in nature and the term chemical senses often is applied to odor. These chemicals may originate from municipal and indus-
odor and taste. Water is a neutral medium, always present on or trial waste discharges, from natural sources such as decomposi-
at the receptors that perceive sensory response. In its pure form, tion of vegetable matter, or from associated microbial activity,
water is odor-free. Man and other animals can avoid many and from disinfectants or their products.
potentially toxic foods and waters because of adverse sensory The potential for impairment of the sensory quality of water
response. These senses often provide the first warning of poten- has increased as a result of expansion in the variety and quantity
tial hazards in the environment. of waste materials, demand for water disposal of captured air
pollutants, and increased reuse of available water supplies by a
growing population. Domestic consumers and process industries
* Approved by Standard Methods Committee, 1997. such as food, beverage, and pharmaceutical manufacturers re-
Joint Task Group: 20th EditionIrwin H. Suffet, (chair), John A. Arrington, quire water essentially free of tastes and odors.
Larry D. Benefield, Larry David Cole, Thomas S. Gittelman, James P. Kizer,
Shundar Lin, Gerald L. Mahon, Morten C. Meilgaard, James R. Nugent.
2-12 PHYSICAL & AGGREGATE PROPERTIES (2000)

Some substances, such as certain inorganic salts, produce taste 3. MALLEVIALLE, J. & I.H. SUFFET. 1987. Identification and Treatment of
without odor and are evaluated by taste testing (Section 2160). Tastes and Odors in Drinking Water. American Water Works Asso-
Many other sensations ascribed to the sense of taste actually are ciation Research Foundation and Lyonnaise des Eaux. AWWARF,
odors, even though the sensation is not noticed until the material Denver, Colo.
4. BRUVOLD, W.H. 1989. A Critical Review of Methods Used for the
is taken into the mouth. Because some odorous materials are
Sensory Evaluation of Water Quality. CRC Crit. Rev. Environ. Con-
detectable when present in only a few nanograms per liter, it is trol. 19(4):291.
usually impractical and often impossible to isolate and identify 5. SUFFET, I., E. KAWCZYNSKI & J. MALLEVIALLE. 1995. Advances in
the odor-producing chemical. The human nose is the practical Taste and Odor Treatment and Control. American Water Works
odor-testing device used in this method. Odor tests are per- Association Research Foundation and Lyonnaise des Eaux,
formed to provide qualitative descriptions and approximate AWWARF, Denver, Colo.
quantitative measurements of odor intensity. The method for 3. Bibliography
intensity measurement presented here is the threshold odor test,
based on a method of limits.2 This procedure, while not univer- MONCRIEFF, R.W. 1946. The Chemical Senses. John Wiley & Sons, New
sally preferred,3 has definite strengths.4 York, N.Y.
Sensory tests are useful as a check on the quality of raw and BAKER, R.A. 1961. Problems of tastes and odors. J. Water Pollut.
finished water and for control of odor through the treatment Control Fed. 33:1099.
process.2,3,5 They can assess the effectiveness of different treat- BAKER, R.A. 1963. Odor effects of aqueous mixtures of organic chem-
ments and provide a means of tracing the source of contamina- icals. J. Water Pollut. Control Fed. 35:728.
tion. ROSEN, A.A., R.T. SKEEL & M.B. ETTINGER. 1963. Relationship of river
Section 6040 provides an analytical procedure for quantifying water odor to specific organic contaminants. J. Water Pollut. Con-
several organic odor-producing compounds including geosmin trol Fed. 35:777.
WRIGHT, R.H. 1964. The Science of Smell. Basic Books, New York,
and methylisoborneol.
N.Y.
AMERINE, M.A., R.M. PANGBORN & E.B. ROESSLER. 1965. Principles of
Sensory Evaluation of Food. Academic Press, New York, N.Y.
2. References ROSEN, A.A. 1970. Report of research committee on tastes and odors.
J. Amer. Water Works Assoc. 62:59.
1. U.S. ENVIRONMENTAL PROTECTION AGENCY. 1973. Proposed Criteria GELDARD, F.A. 1972. The Human Senses. John Wiley & Sons, New
for Water Quality. Vol. 1, Washington, D.C. York, N.Y.
2. AMERICAN SOCIETY FOR TESTING AND MATERIALS COMMITTEE E-18. MEILGAARD, M.C. 1988. Sensory evaluation techniques applied to water
1996. Sensory Testing Methods: Second Edition. E. Chambers & works samples. Water Quality Bull. 13(2/3):39. WHO Collaborat-
M.B. Wolf, eds. American Soc. Testing & Materials, W. Consho- ing Centre on Surface and Groundwater Quality, Burlington, Ont.,
hocken, Pa. Canada.

2150 B. Threshold Odor Test

1. General Discussion b. Application: This threshold method is applicable to sam-

ples ranging from nearly odorless natural waters to industrial
a. Principle: Determine the threshold odor by diluting a sam- wastes with threshold numbers in the thousands. There are no
ple with odor-free water until the least definitely perceptible odor intrinsic difficulties with the highly odorous samples because
is achieved. There is no absolute threshold odor concentration, they are reduced in concentration proportionately before being
because of inherent variation in individual olfactory capability. presented to the test observers.
A given person varies in sensitivity over time. Day-to-day and c. Qualitative descriptions: A fully acceptable system for
within-day differences occur. Furthermore, responses vary as a characterizing odor has not been developed despite efforts over
result of the characteristic, as well as concentration, of odorant. more than a century. Nevertheless, Section 2170 (Flavor Profile
The number of persons selected to measure threshold odor will Analysis) specifies a set of 23 odor reference standards that may
depend on the objective of the tests, economics, and available be used if qualitative descriptions are important. These descrip-
personnel. Larger-sized panels are needed for sensory testing tors can be used with the Threshold Odor Test to standardize
when the results must represent the population as a whole or methods for sensory analysis.
when great precision is desired. Under such circumstances, pan- d. Sampling and storage: Collect samples for odor testing in
els of no fewer than five persons, and preferably ten or more, are glass bottles with glass or TFE-lined closures. Complete tests as
recommended.1 Measurement of threshold levels by one person soon as possible after sample collection. If storage is necessary,
is often a necessity at water treatment plants. Interpretation of the collect at least 500 mL of sample in a bottle filled to the top;
single tester result requires knowledge of the relative acuity of refrigerate, making sure that no extraneous odors can be drawn
that person. Some investigators have used specific odorants, such into the sample as it cools. Do not use plastic containers.
as m-cresol or n-butanol, to calibrate a testers response.2 Others e. Dechlorination: Most tap waters and some wastewaters are
chlorinated. Often it is desirable to determine the odor of the
have used the University of Pennsylvania Smell Identification
chlorinated sample as well as that of the same sample after
Test to assess an individuals ability to identify odors correctly.3
dechlorination. Dechlorinate with thiosulfate in exact stoichio-
ODOR (2150)/Threshold Odor Test 2-13

metric quantity as described under Nitrogen (Ammonia), Section

4500-NH3.
f. Temperature: Threshold odor values vary with temperature.
For most tap waters and raw water sources, a sample temperature
of 60C will permit detection of odors that otherwise might be
missed; 60C is the standard temperature for hot threshold odor
tests. For some purposes because the odor is too fleeting or
there is excessive heat sensationthe hot odor test may not be
applicable; where experience shows that a lower temperature is
needed, use a standard test temperature of 40C. For special
purposes, other temperatures may be used. Report temperature
at which observations are made.

2. Apparatus

To assure reliable threshold measurements, use odor-free

glassware. Clean glassware shortly before use with nonodorous
soap and acid cleaning solution and rinse with odor-free water.
Reserve this glassware exclusively for threshold testing. Do not
use rubber, cork, or plastic stoppers. Do not use narrow-mouth
vessels.
a. Sample bottles, glass-stoppered or with TFE-lined closures.
b. Constant-temperature bath: A water bath or electric hot
plate capable of temperature control of 1C for odor tests at
elevated temperatures. The bath must not contribute any odor to
the odor flasks.
c. Odor flasks: Glass-stoppered, 500-mL (ST 32) erlenmeyer
flasks, to hold sample dilutions during testing.
d. Pipets:
1) Transfer and volumetric pipets or graduated cylinders:
200-, 100-, 50-, and 25-mL.
2) Measuring pipets: 10-mL, graduated in tenths.
e. Thermometer: Zero to 110C, chemical or metal-stem dial
type.

3. Odor-Free Water

a. Sources: Prepare odor-free water by passing distilled,

deionized, or tap water through activated carbon. If product Figure 2150:1. Odor-free-water generator.
water is not odor-free, rebuild or purify the system. In all cases
verify quality of product water daily.
b. Odor-free-water generator (Figure 2150:1):* Make the Check quality of water obtained from the odor-free-water gener-
PVC generator from a 2-ft length of 4-in. PVC pipe approved for ator daily at 40 and 60C before use. The life of the carbon will vary
use for drinking water purposes (e.g., Schedule 80, or National with the condition and amount of water filtered. Subtle odors of
Water Council-approved in U.K.). Thread pipe end to accept biological origin often are found if moist carbon filters stand idle
threaded caps. Have a small threaded nipple in the cap center for between test periods. Detection of odor in the water coming through
water inlet or outlet. To retain the activated carbon, place coarse the carbon indicates that a change of carbon is needed.
glass wool in top and bottom of generator. Regulate water flow
to generator by a needle valve and a pressure regulator to provide 4. Procedure
the minimum pressure for the desired flow. Use activated carbon
of approximately 12 to 40 mesh grain size. a. Precautions: Carefully select by preliminary tests the per-
c. Generator operation: Pass tap or purified water through sons to make taste or odor tests. Although extreme sensitivity is
odor-free-water generator at rate of 100 mL/min. When gener- not required, exclude insensitive persons and concentrate on
ator is started, flush to remove carbon fines and discard product, observers who have a sincere interest in the test. Avoid extra-
or pre-rinse carbon. neous odor stimuli such as those caused by smoking and eating
before the test or those contributed by scented soaps, perfumes,
and shaving lotions. Insure that the tester is free from colds or
* For approximate metric dimensions in centimeters multiply dimensions in allergies that affect odor response. Limit frequency of tests to a
inches by 2.54.
Nuchar WV-G, Westvaco, Covington, VA; Filtrasorb 200, Calgon Carbon number below the fatigue level by frequent rests in an odor-free
Corporation, Pittsburgh, PA; or equivalent. atmosphere. Keep room in which tests are conducted free from
2-14 PHYSICAL & AGGREGATE PROPERTIES (2000)

TABLE 2150:I. THRESHOLD ODOR NUMBERS CORRESPONDING TABLE 2150:II. DILUTIONS FOR VARIOUS ODOR INTENSITIES
TO VARIOUS DILUTIONS
Sample Volume in
Sample Sample Which Odor Is Volumes to Be Diluted
Volume Volume First Noted to 200 mL
Diluted to Diluted to mL mL
200 mL Threshold 200 mL Threshold
mL Odor No. mL Odor No. 200 200, 140, 100, 70, 50
50 50, 35, 25, 17, 12
200 1 12.0 17 12 12, 8.3, 5.7, 4.0, 2.8
140 1.4 8.3 24 2.8 Intermediate dilution
100 2 5.7 35
70 3 4.0 50
50 4 2.8 70
35 6 2.0 100
25 8 1.4 140 1) Place proper volume of odor-free water in the flask first,
17 12 1.0 200
add sample to water (avoiding contact of pipet or sample with lip
or neck of flask), mix by swirling, and proceed as follows:
Determine approximate range of the threshold number by
adding 200 mL, 50 mL, 12 mL, and 2.8 mL sample to separate
distractions, drafts, and odor.2 If necessary, set aside a special 500-mL glass-stoppered erlenmeyer flasks containing odor-free
odor-free room ventilated by air that is filtered through activated water to make a total volume of 200 mL. Use a separate flask
carbon and maintained at a constant comfortable temperature containing only odor-free water as reference for comparison.
and humidity.4 Heat dilutions and reference to desired test temperature.
For precise work use a panel of five or more testers. Do not 2) Shake flask containing odor-free water, remove stopper,
allow persons making odor measurements to prepare samples or and sniff vapors. Test sample containing least amount of odor-
to know dilution concentrations being evaluated. Familiarize bearing water in the same way. If odor can be detected in this
testers with the procedure before they participate in a panel test. dilution, prepare more dilute samples as described in 5) below.
Present most dilute sample first to avoid tiring the senses with If odor cannot be detected in first dilution, repeat above proce-
the concentrated sample. Keep temperature of samples during dure using sample containing next higher concentration of odor-
testing within 1C of the specified temperature. bearing water, and continue this process until odor is detected
Because many raw and waste waters are colored or have clearly.
decided turbidity that may bias results, use opaque or darkly 3) Based on results obtained in the preliminary test, prepare a
colored odor flasks, such as red actinic erlenmeyer flasks. set of dilutions using Table 2150:II as a guide. Prepare the five
b. Characterization: As part of the threshold test or as a dilutions shown on the appropriate line and the three next most
separate test, direct each observer to describe the characteristic concentrated on the next line in Table 2150:II. For example, if
sample odor using odor reference standards (see Section 2170). odor was first noted in the flask containing 50 mL sample in the
Compile the consensus that may appear among testers and that preliminary test, prepare flasks containing 50, 35, 25, 17, 12, 8.3,
affords a clue to the origin of the odorous component. The value 5.7, and 4.0 mL sample, each diluted to 200 mL with odor-free
of the characterization test increases as observers become more water. This array is necessary to challenge the range of sensi-
experienced with a particular category of odor, e.g., earthy, tivities of the entire panel of testers.
musty, chlorine. Insert two or more blanks in the series near the expected
c. Threshold measurement: The threshold odor number, des- threshold, but avoid any repeated pattern. Do not let tester know
ignated by the abbreviation TON, is the greatest dilution of sample which dilutions are odorous and which are blanks. Instruct tester
with odor-free water yielding a definitely perceptible odor. Bring to smell each flask in sequence, beginning with the least con-
total volume of sample and odor-free water to 200 mL in each test. centrated sample, until odor is detected with certainty.
Follow dilutions and record corresponding TON presented in Table 4) Record observations by indicating whether odor is noted in
2150:I. These numbers have been computed thus: each test flask. For example:
mL
A B Sample
TON Diluted to
A
200 mL 12 0 17 25 0 35 50
where:
Response
A mL sample and
B mL odor-free water.
5) If the sample being tested requires more dilution than is
provided by Table 2150:II, prepare an intermediate dilution
consisting of 20 mL sample diluted to 200 L with odor-free
There are numerous methods of arranging and presenting samples for odor water. Use this dilution for the threshold determination. Multiply
determinations. The methods offered here are practical and economical of time TON obtained by 10 to correct for the intermediate dilution. In
and personnel. If extensive tests are planned and statistical analysis of data is
required, become familiar with the more accurate methods that have been used rare cases more than one tenfold intermediate dilution step may
extensively by flavor and allied industries.5 be required.
ODOR (2150)/Threshold Odor Test 2-15

5. Calculation M.B. Wolf, eds. American Soc. Testing & Materials, W. Consho-
hocken, Pa.
The threshold odor number is the dilution ratio at which odor 2. BAKER, R.A. 1962. Critical evaluation of olfactory measurement. J.
is just detectable. In the example above, 4c4), the first detect- Water Pollut. Control Fed. 34:582.
able odor occurred when 25 mL sample was diluted to 200 mL. 3. DOTY, R.L., P. SHAMAN, M.S. DANN & C.P. KIMMELMAN. 1984.
University of Pennsylvania smell identification test: a rapid quanti-
Thus the threshold is 200 divided by 25, or 8. Table 2150:I lists
tative olfactory function test for the clinic. Laryngoscope 94(2):176.
the threshold numbers corresponding to common dilutions. 4. BAKER, R.A. 1963. Odor testing laboratory. J. Water Pollut. Control
The smallest TON that can be observed is 1, as in the case Fed. 35:1396.
where the odor flask contains 200 mL undiluted sample. If no 5. INTERNATIONAL ORGANIZATION FOR STANDARDIZATION. 1985. ISO 6658
odor is detected at this concentration, report No odor observed Sensory AnalysisMethodologyGeneral Guidance. International
instead of a threshold number. (In special applications, fractional Org. for Standardization, Geneva, Switzerland.
threshold numbers have been calculated.6) 6. ROSEN, A.A., J.B. PETER & F.M. MIDDLETON. 1962. Odor thresholds
Anomalous responses sometimes occur; a low concentra- of mixed organic chemicals. J. Water Pollut. Control Fed. 34:7.
tion may be called positive and a higher concentration in the
series may be called negative. In such a case, designate the
threshold as the point after which no further anomalies occur. 8. Bibliography
For instance:
HULBERT, R. & D. FEBEN. 1941. Studies on accuracy of threshold odor
value. J. Amer. Water Works Assoc. 33:1945.
Increasing Concentration 3 SPAULDING, C.H. 1942. Accuracy and application of threshold odor test.
J. Amer. Water Works Assoc. 34:877.
Response THOMAS, H.A., JR. 1943. Calculation of threshold odor. J. Amer. Water
Works Assoc. 35:751.
2
CARTWRIGHT, L.C., C.T. SNELL & P.H. KELLY. 1952. Organoleptic panel
Threshold
testing as a research tool. Anal. Chem. 24:503.
LAUGHLIN, H.F. 1954. Palatable level with the threshold odor test. Taste
where: Odor Control J. 20:No. 8 (Aug.).
SHELLENBERGER, R.D. 1958. Procedures for determining threshold odor
signifies negative response and concentrations in aqueous solutions. Taste Odor Control J. 24:No.
signifies positive response. 5 (May).
LAUGHLIN, H.F. 1962. Influence of temperature in threshold odor eval-
Occasionally a flask contains residual odor or is contaminated uation. Taste Odor Control J. 28:No. 10 (Oct.).
inadvertently. For precise testing repeat entire threshold odor test The threshold odor test. 1963. Taste Odor Control J. 29:Nos. 6, 7, 8
to determine if the last flask marked was actually a (June, July, Aug.).
mislabelled blank of odor-free water or if the previous was SUFFET, I.H. & S. SEGALL. 1971. Detecting taste and odor in drinking
a contaminated sample. water. J. Amer. Water Works Assoc. 63:605.
STAHL, W.H., ed. 1973. Compilation of Odor and Taste Threshold
Use appropriate statistical methods to calculate the most prob-
Values Data. Amer. Soc. Testing & Materials Data Ser. DS 48,
able average threshold from large numbers of panel results. For Philadelphia, Pa.
most purposes, express the threshold of a group as the geometric AMERICAN SOCIETY FOR TESTING AND MATERIALS. 1973. Annual Book of
mean of individual thresholds. ASTM Standards. Part 23, D-1292-65, ASTM, Philadelphia, Pa.
AMERICAN SOCIETY FOR TESTING AND MATERIALS. 1986. Physical Require-
ment Guidelines for Sensory Evaluation Laboratories. STP 913,
6. Interpretation of Results American Soc. Testing & Materials, Philadelphia, Pa.
AMERICAN SOCIETY FOR TESTING AND MATERIALS COMMITTEE E-679. 1990.
A threshold number is not a precise value. In the case of the Standard Practice for Determination of Odor and Taste Thresholds
single observer it represents a judgment at the time of testing. by a Forced-Choice Ascending Concentration Series Method of
Panel results are more meaningful because individual differences Limits. American Soc. Testing & Materials, Philadelphia, Pa.
have less influence on the result. One or two observers can AMERICAN SOCIETY FOR TESTING AND MATERIALS. 1991. E1432 Standard
Practice for Defining and Calculating Individual and Group Sensory
develop useful data if comparison with larger panels has been
Thresholds from Forced Choice Data Sets of Intermediate Size.
made to check their sensitivity. Do not make comparisons of data American Society for Testing and Materials, Philadelphia, Pa.
from time to time or place to place unless all test conditions have BRUVOLD, W.H. 1989. A critical review of methods used for the sensory
been standardized carefully and there is some basis for compar- evaluation of water quality. Crit. Rev. Environ. Control 19:291.
ison of observed intensities. YOUNG, W.F., H. HORTH, R. CRANE, T. OGDEN & M. ARNOTT. 1996. Taste
and odour threshold concentration of potential potable water con-
taminants. Water Res. 30:331.
7. References

1. AMERICAN SOCIETY FOR TESTING AND MATERIALS COMMITTEE E-18.

1996. Sensory Testing Methods: Second Edition. E. Chambers &