Standard Methods for the Examination of Water and Wastewater

2540 SOLIDS#(1)*

2540 A. Introduction
Solids refer to matter suspended or dissolved in water or wastewater. Solids may affect water or
effluent quality adversely in a number of ways. Waters with high dissolved solids generally are of
inferior palatability and may induce an unfavorable physiological reaction in the transient
consumer. For these reasons, a limit of 500 mg dissolved solids/L is desirable for drinking
waters. Highly mineralized waters also are unsuitable for many industrial applications. Waters
high in suspended solids may be esthetically unsatisfactory for such purposes as bathing. Solids
analyses are important in the control of biological and physical wastewater treatment processes
and for assessing compliance with regulatory agency wastewater effluent limitations.

1. Definitions
‘‘Total solids’’ is the term applied to the material residue left in the vessel after evaporation
of a sample and its subsequent drying in an oven at a defined temperature. Total solids includes
‘‘total suspended solids,’’ the portion of total solids retained by a filter, and ‘‘total dissolved
solids,’’ the portion that passes through the filter.
The type of filter holder, the pore size, porosity, area, and thickness of the filter and the
physical nature, particle size, and amount of material deposited on the filter are the principal
factors affecting separation of suspended from dissolved solids. ‘‘Dissolved solids’’ is the
portion of solids that passes through a filter of 2.0 µm (or smaller) nominal pore size under
specified conditions. ‘‘Suspended solids’’ is the portion retained on the filter.
‘‘Fixed solids’’ is the term applied to the residue of total, suspended, or dissolved solids after
heating to dryness for a specified time at a specified temperature. The weight loss on ignition is
called ‘‘volatile solids.’’ Determinations of fixed and volatile solids do not distinguish precisely
between inorganic and organic matter because the loss on ignition is not confined to organic
matter. It includes losses due to decomposition or volatilization of some mineral salts. Better
characterization of organic matter can be made by such tests as total organic carbon (Section
5310), BOD (Section 5210), and COD (Section 5220).
‘‘Settleable solids’’ is the term applied to the material settling out of suspension within a
defined period. It may include floating material, depending on the technique (Section 2540F.3b).

2. Sources of Error and Variability

Sampling, subsampling, and pipeting two-phase or three-phase samples may introduce
serious errors. Make and keep such samples homogeneous during transfer. Use special handling
to insure sample integrity when subsampling. Mix small samples with a magnetic stirrer. If
suspended solids are present, pipet with wide-bore pipets. If part of a sample adheres to the

© Copyright 1999 by American Public Health Association, American Water Works Association, Water Environment Federation
 Standard Methods for the Examination of Water and Wastewater

sample container, consider this in evaluating and reporting results. Some samples dry with the
formation of a crust that prevents water evaporation; special handling is required to deal with
this. Avoid using a magnetic stirrer with samples containing magnetic particles.
The temperature at which the residue is dried has an important bearing on results, because
weight losses due to volatilization of organic matter, mechanically occluded water, water of
crystallization, and gases from heat-induced chemical decomposition, as well as weight gains due
to oxidation, depend on temperature and time of heating. Each sample requires close attention to
desiccation after drying. Minimize opening desiccator because moist air enters. Some samples
may be stronger desiccants than those used in the desiccator and may take on water.
Residues dried at 103 to 105°C may retain not only water of crystallization but also some
mechanically occluded water. Loss of CO2 will result in conversion of bicarbonate to carbonate.
Loss of organic matter by volatilization usually will be very slight. Because removal of occluded
water is marginal at this temperature, attainment of constant weight may be very slow.
Residues dried at 180 ± 2°C will lose almost all mechanically occluded water. Some water of
crystallization may remain, especially if sulfates are present. Organic matter may be lost by
volatilization, but not completely destroyed. Loss of CO2 results from conversion of bicarbonates
to carbonates and carbonates may be decomposed partially to oxides or basic salts. Some
chloride and nitrate salts may be lost. In general, evaporating and drying water samples at 180°C
yields values for dissolved solids closer to those obtained through summation of individually
determined mineral species than the dissolved solids values secured through drying at the lower
temperature.
To rinse filters and filtered solids and to clean labware use Type III water. Special samples
may require a higher quality water; see Section 1080.
Results for residues high in oil or grease may be questionable because of the difficulty of
drying to constant weight in a reasonable time.
To aid in quality assurance, analyze samples in duplicate. Dry samples to constant weight if
possible. This entails multiple drying-cooling-weighing cycles for each determination.
Analyses performed for some special purposes may demand deviation from the stated
procedures to include an unusual constituent with the measured solids. Whenever such variations
of technique are introduced, record and present them with the results.

3. Sample Handling and Preservation

Use resistant-glass or plastic bottles, provided that the material in suspension does not adhere
to container walls. Begin analysis as soon as possible because of the impracticality of preserving
the sample. Refrigerate sample at 4°C up to the time of analysis to minimize microbiological
decomposition of solids. Preferably do not hold samples more than 24 h. In no case hold sample
more than 7 d. Bring samples to room temperature before analysis.

4. Selection of Method

© Copyright 1999 by American Public Health Association, American Water Works Association, Water Environment Federation
 Standard Methods for the Examination of Water and Wastewater

Methods B through F are suitable for the determination of solids in potable, surface, and
saline waters, as well as domestic and industrial wastewaters in the range up to 20 000 mg/L.
Method G is suitable for the determination of solids in sediments, as well as solid and
semisolid materials produced during water and wastewater treatment.

5. Bibliography
THERIAULT, E.J. & H.H. WAGENHALS. 1923. Studies of representative sewage plants. Pub. Health
Bull. No. 132.
U.S. ENVIRONMENTAL PROTECTION AGENCY. 1979. Methods for Chemical Analysis of Water
and Wastes. Publ. 600/4-79-020, rev. Mar. 1983. Environmental Monitoring and Support
Lab., U.S. Environmental Protection Agency, Cincinnati, Ohio.

2540 D. Total Suspended Solids Dried at 103–105°C

1. General Discussion
a. Principle: A well-mixed sample is filtered through a weighed standard glass-fiber filter
and the residue retained on the filter is dried to a constant weight at 103 to 105°C. The increase
in weight of the filter represents the total suspended solids. If the suspended material clogs the
filter and prolongs filtration, it may be necessary to increase the diameter of the filter or decrease
the sample volume. To obtain an estimate of total suspended solids, calculate the difference
between total dissolved solids and total solids.
b. Interferences: See Section 2540A.2 and Section 2540B.1. Exclude large floating particles
or submerged agglomerates of nonhomogeneous materials from the sample if it is determined
that their inclusion is not representative. Because excessive residue on the filter may form a
water-entrapping crust, limit the sample size to that yielding no more than 200 mg residue. For
samples high in dissolved solids thoroughly wash the filter to ensure removal of dissolved
material. Prolonged filtration times resulting from filter clogging may produce high results owing
to increased colloidal materials captured on the clogged filter.

2. Apparatus
Apparatus listed in Section 2540B.2 and Section 2540C.2 is required, except for evaporating
dishes, steam bath, and 180°C drying oven. In addition:
Aluminum weighing dishes.

3. Procedure
a. Preparation of glass-fiber filter disk: If pre-prepared glass fiber filter disks are used,
eliminate this step. Insert disk with wrinkled side up in filtration apparatus. Apply vacuum and
wash disk with three successive 20-mL portions of reagent-grade water. Continue suction to
remove all traces of water, turn vacuum off, and discard washings. Remove filter from filtration

© Copyright 1999 by American Public Health Association, American Water Works Association, Water Environment Federation
 Standard Methods for the Examination of Water and Wastewater

apparatus and transfer to an inert aluminum weighing dish. If a Gooch crucible is used, remove
crucible and filter combination. Dry in an oven at 103 to 105°C for 1 h. If volatile solids are to be
measured, ignite at 550°C for 15 min in a muffle furnace. Cool in desiccator to balance
temperature and weigh. Repeat cycle of drying or igniting, cooling, desiccating, and weighing
until a constant weight is obtained or until weight change is less than 4% of the previous
weighing or 0.5 mg, whichever is less. Store in desiccator until needed.
b. Selection of filter and sample sizes: Choose sample volume to yield between 2.5 and 200
mg dried residue. If volume filtered fails to meet minimum yield, increase sample volume up to 1
L. If complete filtration takes more than 10 min, increase filter diameter or decrease sample
volume.
c. Sample analysis: Assemble filtering apparatus and filter and begin suction. Wet filter with
a small volume of reagent-grade water to seat it. Stir sample with a magnetic stirrer at a speed to
shear larger particles, if practical, to obtain a more uniform (preferably homogeneous) particle
size. Centrifugal force may separate particles by size and density, resulting in poor precision
when point of sample withdrawal is varied. While stirring, pipet a measured volume onto the
seated glass-fiber filter. For homogeneous samples, pipet from the approximate midpoint of
container but not in vortex. Choose a point both middepth and midway between wall and vortex.
Wash filter with three successive 10-mL volumes of reagent-grade water, allowing complete
drainage between washings, and continue suction for about 3 min after filtration is complete.
Samples with high dissolved solids may require additional washings. Carefully remove filter
from filtration apparatus and transfer to an aluminum weighing dish as a support. Alternatively,
remove the crucible and filter combination from the crucible adapter if a Gooch crucible is used.
Dry for at least 1 h at 103 to 105°C in an oven, cool in a desiccator to balance temperature, and
weigh. Repeat the cycle of drying, cooling, desiccating, and weighing until a constant weight is
obtained or until the weight change is less than 4% of the previous weight or 0.5 mg, whichever
is less. Analyze at least 10% of all samples in duplicate. Duplicate determinations should agree
within 5% of their average weight. If volatile solids are to be determined, treat the residue
according to 2540E.

4. Calculation

where:
A = weight of filter + dried residue, mg, and
B = weight of filter, mg.

5. Precision
The standard deviation was 5.2 mg/L (coefficient of variation 33%) at 15 mg/L, 24 mg/L
© Copyright 1999 by American Public Health Association, American Water Works Association, Water Environment Federation
 Standard Methods for the Examination of Water and Wastewater

(10%) at 242 mg/L, and 13 mg/L (0.76%) at 1707 mg/L in studies by two analysts of four sets of
10 determinations each.
Single-laboratory duplicate analyses of 50 samples of water and wastewater were made with
a standard deviation of differences of 2.8 mg/L.

6. Bibliography
DEGEN, J. & F.E. NUSSBERGER. 1956. Notes on the determination of suspended solids. Sewage
Ind. Wastes 28:237.
CHANIN, G., E.H. CHOW, R.B. ALEXANDER & J. POWERS. 1958. Use of glass fiber filter medium in
the suspended solids determination. Sewage Ind. Wastes 30:1062.
NUSBAUM, I. 1958. New method for determination of suspended solids. Sewage Ind. Wastes
30:1066.
SMITH, A.L. & A.E. GREENBERG. 1963. Evaluation of methods for determining suspended solids
in wastewater. J. Water Pollut. Control Fed. 35:940.
WYCKOFF, B.M. 1964. Rapid solids determination using glass fiber filters. Water Sewage Works
111:277.
NATIONAL COUNCIL OF THE PAPER INDUSTRY FOR AIR AND STREAM IMPROVEMENT. 1975. A
Preliminary Review of Analytical Methods for the Determination of Suspended Solids in
Paper Industry Effluents for Compliance with EPA-NPDES Permit Terms. Spec. Rep. No.
75-01. National Council of the Paper Industry for Air & Stream Improvement, New York,
N.Y.
NATIONAL COUNCIL OF THE PAPER INDUSTRY FOR AIR AND STREAM IMPROVEMENT. 1977. A
Study of the Effect of Alternate Procedures on Effluent Suspended Solids Measurement.
Stream Improvement Tech. Bull. No. 291, National Council of the Paper Industry for Air &
Stream Improvement, New York, N.Y.
TREES, C.C. 1978. Analytical analysis of the effect of dissolved solids on suspended solids
determination. J. Water Pollut. Control Fed. 50:2370.

© Copyright 1999 by American Public Health Association, American Water Works Association, Water Environment Federation
 Standard Methods for the Examination of Water and Wastewater

Endnotes
1 (Popup - Footnote)
* APPROVED BY STANDARD METHODS COMMITTEE, 1997.

© Copyright 1999 by American Public Health Association, American Water Works Association, Water Environment Federation