2-8 PHYSICAL & AGGREGATE PROPERTIES (2000)

tristimulus (ordinate) values, preferably by using the weighted- facturers directions. Express results as prescribed in 2120C.6c
ordinate method.* Calibrate calculation algorithm software for both original and pH-adjusted samples.
against platinum-cobalt standard reference. Alternatively, obtain ADMI weighted-ordinate values for
b. Spectrophotometer cells, 1 cm. color by a published computation method.2
c. Filtering apparatus and filter: See 2120B.2c.
4. Quality Control

3. Procedure See Section 2120B.7.

a. Sample collection: See 2120B.5a. 5. References

b. Sample preparation: Prepare two 100-mL sample portions,
one at the original pH and one at pH 7.0. Filter turbid samples 1. MCLAREN, K. 1970. The Adams-Nickerson colour-difference for-
according to 2120B.5b. mula. J. Soc. Dyers Colorists 86:354.
c. Spectrophotometric measurement: Let spectrophotometer 2. ALLEN, W., W.B. PRESCOTT, R.E. DERBY, C.E. GARLAND, J.M. PERET &
warm up in accordance with the manufacturers instruction. Set M. SALTZMAN. 1973. Determination of color of water and wastewater
instrument to pre-programmed calibration curve for ADMI by means of ADMI color values. Proc. 28th Ind. Waste Conf., Purdue
Univ., Eng. Ext. Ser. No. 142:661.
Weighted Ordinate Method. Zero instrument and take measure-
ments of original and pH-adjusted samples according to manu- 6. Bibliography

HACH COMPANY. 1999. Hach DR/4000 Spectrophotometer Procedures

* Hach DR/4000 Spectrophotometer, Program No. 1660, or equivalent. Manual, 9th ed. Hach Co., Loveland, Colo.

2130 TURBIDITY*

2130 A. Introduction

1. Sources and Significance cause a negative interference. Some commercial instruments

may have the capability of either correcting for a slight color
Clarity of water is important in producing products destined interference or optically blanking out the color effect.
for human consumption and in many manufacturing operations.
Beverage producers, food processors, and potable water treat- 2. Selection of Method
ment plants drawing from a surface water source commonly rely
on fluid-particle separation processes such as sedimentation and Historically, the standard method for determination of turbidity
filtration to increase clarity and insure an acceptable product. has been based on the Jackson candle turbidimeter; however, the
The clarity of a natural body of water is an important determi- lowest turbidity value that can be measured directly on this device
nant of its condition and productivity. is 25 Jackson Turbidity Units (JTU). Because turbidities of water
Turbidity in water is caused by suspended and colloidal treated by conventional fluid-particle separation processes usually
matter such as clay, silt, finely divided organic and inorganic fall within the range of 0 to 1 unit, indirect secondary methods were
matter, and plankton and other microscopic organisms. Tur- developed to estimate turbidity. Electronic nephelometers are the
bidity is an expression of the optical property that causes light preferred instruments for turbidity measurement.
to be scattered and absorbed rather than transmitted with no Most commercial turbidimeters designed for measuring low
change in direction or flux level through the sample. Corre- turbidities give comparatively good indications of the intensity
lation of turbidity with the weight or particle number concen- of light scattered in one particular direction, predominantly at
tration of suspended matter is difficult because the size, shape, right angles to the incident light. Turbidimeters with scattered-
and refractive index of the particles affect the light-scattering light detectors located at 90 to the incident beam are called
properties of the suspension. When present in significant nephelometers. Nephelometers are relatively unaffected by small
concentrations, particles consisting of light-absorbing mate- differences in design parameters and therefore are specified as
rials such as activated carbon cause a negative interference. In the standard instrument for measurement of low turbidities.
low concentrations these particles tend to have a positive Instruments of different make and model may vary in response.
influence because they contribute to turbidity. The presence of However, interinstrument variation may be effectively negligible
dissolved, color-causing substances that absorb light may
Nephelometers that instrument manufacturers claim meet the design specifica-
tions of this method may not give the same reading for a given suspension, even
* Approved by Standard Methods Committee, 2001. when each instrument has been calibrated using the manufacturers manual. This
Joint Task Group: 20th EditionRaymond D. Letterman (chair), John A. Ar- differential performance is especially important when measurements are made for
rington, Alvin Lieberman, Kemon J. Papacosta, Theodore S. Tanaka, Brannon H. regulatory purposes. Consult regulatory authorities when selecting a nephelometer
Wilder. to be used for making measurements that will be reported for regulatory purposes.
TURBIDITY (2130)/Nephelometric Method 2-9

if good measurement techniques are used and the characteristics Its precision, sensitivity, and applicability over a wide
of the particles in the measured suspensions are similar. Poor turbidity range make the nephelometric method preferable to
measurement technique can have a greater effect on measure- visual methods. Report nephelometric measurement results as
ment error than small differences in instrument design. Turbi- nephelometric turbidity units (NTU).
dimeters of nonstandard design, such as forward-scattering de-
vices, may be more sensitive than nephelometers to the presence
of larger particles. While it may not be appropriate to compare 3. Storage of Sample
their output with that of instruments of standard design, they still
Determine turbidity as soon as possible after the sample is
may be useful for process monitoring.
An additional cause of discrepancies in turbidity analysis is taken. Gently agitate all samples before examination to ensure a
the use of suspensions of different types of particulate matter for representative measurement. Sample preservation is not practi-
instrument calibration. Like water samples, prepared suspen- cal; begin analysis promptly. Refrigerate or cool to 4C, to
sions have different optical properties depending on the particle minimize microbiological decomposition of solids, if storage is
size distributions, shapes, and refractive indices. A standard required. For best results, measure turbidity immediately without
reference suspension having reproducible light-scattering prop- altering the original sample conditions such as temperature or
erties is specified for nephelometer calibration. pH.

2130 B. Nephelometric Method

1. General Discussion 3) Angle of light acceptance by detectorCentered at 90 to

the incident light path and not to exceed 30 from 90. The
a. Principle: This method is based on a comparison of the detector and filter system, if used, shall have a spectral peak
intensity of light scattered by the sample under defined conditions response between 400 and 600 nm.
with the intensity of light scattered by a standard reference suspen- b. Sample cells: Use sample cells or tubes of clear, colorless
sion under the same conditions. The higher the intensity of scattered glass or plastic. Keep cells scrupulously clean, both inside and
light, the higher the turbidity. Formazin polymer is used as the out, and discard if scratched or etched. Never handle them where
primary standard reference suspension. The turbidity of a specified the instruments light beam will strike them. Use tubes with
concentration of formazin suspension is defined as 4000 NTU. sufficient extra length, or with a protective case, so that they may
b. Interference: Turbidity can be determined for any water be handled properly. Fill cells with samples and standards that
sample that is free of debris and rapidly settling coarse sediment. have been agitated thoroughly and allow sufficient time for
Dirty glassware and the presence of air bubbles give false results. bubbles to escape.
True color, i.e., water color due to dissolved substances that Clean sample cells by thorough washing with laboratory soap
absorb light, causes measured turbidities to be low. This effect inside and out followed by multiple rinses with distilled or
usually is not significant in treated water. deionized water; let cells air-dry. Handle sample cells only by
2. Apparatus the top to avoid dirt and fingerprints within the light path.
Cells may be coated on the outside with a thin layer of silicone oil
a. Laboratory or process nephelometer consisting of a light to mask minor imperfections and scratches that may contribute to
source for illuminating the sample and one or more photoelectric stray light. Use silicone oil with the same refractive index as glass.
detectors with a readout device to indicate intensity of light scat- Avoid excess oil because it may attract dirt and contaminate the
tered at 90 to the path of incident light. Use an instrument designed sample compartment of the instrument. Using a soft, lint-free cloth,
to minimize stray light reaching the detector in the absence of spread the oil uniformly and wipe off excess. The cell should appear
turbidity and to be free from significant drift after a short warmup to be nearly dry with little or no visible oil.
period. The sensitivity of the instrument should permit detecting Because small differences between sample cells significantly
turbidity differences of 0.02 NTU or less in the lowest range in impact measurement, use either matched pairs of cells or the
waters having a turbidity of less than 1 NTU. Several ranges may be same cell for both standardization and sample measurement.
necessary to obtain both adequate coverage and sufficient sensitivity
for low turbidities. Differences in instrument design will cause
differences in measured values for turbidity even though the same 3. Reagents
suspension is used for calibration. To minimize such differences,
observe the following design criteria: a. Dilution water: High-purity water will cause some light
1) Light sourceTungsten-filament lamp operated at a color scattering, which is detected by nephelometers as turbidity. To
temperature between 2200 and 3000K. obtain low-turbidity water for dilutions, nominal value 0.02
2) Distance traversed by incident light and scattered light NTU, pass laboratory reagent-grade water through a filter with
within the sample tubeTotal not to exceed 10 cm. pore size sufficiently small to remove essentially all particles
2-10 PHYSICAL & AGGREGATE PROPERTIES (2000)

larger than 0.1 m;* the usual membrane filter used for bacte- turbidity of the standard after calibrating the instrument with a
riological examinations is not satisfactory. Rinse collecting flask fresh formazin or microsphere suspension. If there is any doubt
at least twice with filtered water and discard the next 200 mL. about the integrity or turbidity value of any secondary standard,
Some commercial bottled demineralized waters have a low check instrument calibration first with another secondary stan-
turbidity. These may be used when filtration is impractical or a dard and then, if necessary, with user-prepared formazin. Most
good grade of water is not available to filter in the laboratory. secondary standards have been carefully prepared by their man-
Check turbidity of bottled water to make sure it is lower than the ufacturer and should, if properly used, give good agreement with
level that can be achieved in the laboratory. formazin. Prepare formazin primary standard only as a last
b. Stock primary standard formazin suspension: resort. Proper application of secondary standards is specific for
1) Solution IDissolve 1.000 g hydrazine sulfate, each make and model of nephelometer. Not all secondary stan-
(NH2)2H2SO4, in distilled water and dilute to 100 mL in a dards have to be discarded when comparison with a primary
volumetric flask. CAUTION: Hydrazine sulfate is a carcinogen; standard shows that their turbidity value has changed. In some
avoid inhalation, ingestion, and skin contact. Formazin suspen- cases, the secondary standard should be simply relabeled with
sions can contain residual hydrazine sulfate. the new turbidity value. Always follow the manufacturers di-
2) Solution IIDissolve 10.00 g hexamethylenetetramine, rections.
(CH2)6N4, in distilled water and dilute to 100 mL in a volumetric
flask. 4. Procedure
3) In a flask, mix 5.0 mL Solution I and 5.0 mL Solution II.
Let stand for 24 h at 25 3C. This results in a 4000-NTU a. General measurement techniques: Proper measurement tech-
suspension. Transfer stock suspension to an amber glass or other niques are important in minimizing the effects of instrument vari-
UV-light-blocking bottle for storage. Make dilutions from this ables as well as stray light and air bubbles. Regardless of the
stock suspension. The stock suspension is stable for up to 1 year instrument used, the measurement will be more accurate, precise,
when properly stored. and repeatable if close attention is paid to proper measurement
c. Dilute turbidity suspensions: Dilute 4000 NTU primary techniques.
standard suspension with high-quality dilution water. Prepare Measure turbidity immediately to prevent temperature
immediately before use and discard after use. changes and particle flocculation and sedimentation from chang-
d. Secondary standards: Secondary standards are standards ing sample characteristics. If flocculation is apparent, break up
that the manufacturer (or an independent testing organization) aggregates by agitation. Avoid dilution whenever possible. Par-
has certified will give instrument calibration results equiva- ticles suspended in the original sample may dissolve or other-
lent (within certain limits) to the results obtained when the wise change characteristics when the temperature changes or
instrument is calibrated with the primary standard, i.e., user- when the sample is diluted.
prepared formazin. Various secondary standards are available Remove air or other entrained gases in the sample before
including: commercial stock suspensions of 4000 NTU measurement. Preferably degas even if no bubbles are visible.
formazin, commercial suspensions of microspheres of sty- Degas by applying a partial vacuum, adding a nonfoaming-type
rene-divinylbenzene copolymer, and items supplied by in- surfactant, using an ultrasonic bath, or applying heat. In some
strument manufacturers, such as sealed sample cells filled cases, two or more of these techniques may be combined for
with latex suspension or with metal oxide particles in a more effective bubble removal. For example, it may be neces-
polymer gel. The U.S. Environmental Protection Agency1 sary to combine addition of a surfactant with use of an ultrasonic
designates user-prepared formazin, commercial stock forma- bath for some severe conditions. Any of these techniques, if
zin suspensions, and commercial styrene-divinylbenzene sus- misapplied, can alter sample turbidity; use with care. If degas-
pensions as primary standards, and reserves the term sec- sing cannot be applied, bubble formation will be minimized if
ondary standard for the sealed standards mentioned above. the samples are maintained at the temperature and pressure of the
Secondary standards made with suspensions of microspheres water before sampling.
of styrene-divinylbenzene copolymer typically are as stable as Do not remove air bubbles by letting sample stand for a period of
concentrated formazin and are much more stable than diluted time because during standing, turbidity-causing particulates may
formazin. These suspensions can be instrument-specific; there- settle and sample temperature may change. Both of these conditions
fore, use only suspensions formulated for the type of nephelom- alter sample turbidity, resulting in a nonrepresentative measure-
eter being used. Secondary standards provided by the instrument ment.
manufacturer (sometimes called permanent standards) may be Condensation may occur on the outside surface of a sample
necessary to standardize some instruments before each reading cell when a cold sample is being measured in a warm, humid
and in other instruments only as a calibration check to determine environment. This interferes with turbidity measurement. Re-
when calibration with the primary standard is necessary. move all moisture from the outside of the sample cell before
All secondary standards, even so-called permanent stan- placing the cell in the instrument. If fogging recurs, let sample
dards, change with time. Replace them when their age exceeds warm slightly by letting it stand at room temperature or by
the shelf life. Deterioration can be detected by measuring the partially immersing it in a warm water bath for a short time.
Make sure samples are again well mixed.
b. Nephelometer calibration: Follow the manufacturers op-
erating instructions. Run at least one standard in each instrument
* Nuclepore Corp., 7035 Commerce Circle, Pleasanton, CA, or equivalent.
AMCO-AEPA-1 Standard, Advanced Polymer Systems, 3696 Haven Ave., range to be used. Make certain the nephelometer gives stable
Redwood City, CA, or equivalent. readings in all sensitivity ranges used. Follow techniques out-
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.