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* Approved by Standard Methods Committee, 1997.
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 2540A.2 and 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.
Apparatus listed in Sections 2450B.2 and 2540C.2 is required, except for evaporating dishes, steam bath, and 180°C drying oven. In addition:
Aluminum weighing dishes.
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 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.
mg total suspended solids/L =
sample volume, mL
A = weight of filter + dried residue, mg, and
B = weight of filter, mg.
The standard deviation was 5.2 mg/L (coefficient of variation 33%) at 15 mg/L, 24 mg/L (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.
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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.
©Standard Methods for the Examination of Water and Wastewater. 20th Ed. American Public Health Association, American Water Works Association, Water Environment Federation.