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EN2703: Laboratory 2C
Laboratory Manual
For
Solids Analysis
Session 2004/2005
Solids (Residue) Analysis
1. OBJECTIVES
2. THEORY
Dried at 103 C
Filtrate Dissolved Solids
Wastewater Filtration (TDS)
Sample Volatile Suspended
Dried at 103 C Burnt at 500 C Solids (VSS)
Non-Filtrate Suspended Solids
(TSS)
Fixed Suspended
Solids (FSS)
Volatile Solids (VS)
Sludge Dried at 103 C Burnt at 500 C
Sample Total Solids
(TS)
Fixed Solids (FS)
The total solids (TS) contents of sludges are used in the design and process control of
wastewater treatment facilities. Total dissolved solids (TDS) are used to evaluate the
suitability of water for both domestic supplies and industrial purposes. The total
suspended solids (TSS), including the volatile fraction (VSS), are commonly monitored
to evaluate the degree of pollution in natural waters and serves as a key process
control parameter for wastewater treatment operation.
3. MEASUREMENT
The total solids concentration of a sample can be found directly by weighing the
sample before and after drying at 103oC. However, the remaining forms, TDS, TSS,
FSS (Fixed fraction), and VSS require filtration of the sample. For liquid samples, all
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these solids levels are reported in mg/L. VSS is occasionally reported as a percentage
of TSS, rather than as mg/L.
Sewage sludges are often too thick to allow direct filtration to take place. In these
instances, centrifugation can be applied before direct filtration. Sometimes, only the
total solids, total fixed solids and total volatile solids concentrations need to be
determined to replace the corresponding TSS, FSS and VSS, respectively. Sludge
solids are reported as either mg/L, g/L or more commonly in percentage solids as dry
weight (1% dry solids is approximately 10,000 mg/L). Sludges can also be reported as
percent moisture. Total volatile solids for sludges are usually reported as a percentage
of total solids.
Because of general inaccuracies with the test, analysis for solids is often performed in
triplicate. Large and floating particles or submerged agglomerates of non-
homogeneous materials should be excluded from the sample. Visible floating oil and
grease should be dispersed with a blender before withdrawing the sample for analysis.
4. EXPERIMENT
Five wastewater samples and five sludge samples are to be analyzed in this laboratory
session for their TSS and VSS, and for their TS and VS, respectively. Each batch of
students is to carry out solids tests on one wastewater and one sludge sample. The
allocation of samples to each batch of students is given below:
(i) Prepare three evaporating dishes for each sample by cleaning and ignition
at 500oC for 1 hour in a muffle furnace.
(ii) Cool, desiccate, weigh, and store dish in a desiccator until ready for use.
(iii) Transfer sample to the prepared dish and weigh (weight of wet sample plus
dish) and evaporate to dryness on a steam bath or in a drying oven.
Choose a sample volume that will yield a residue of between 2.5 mg and
200 mg. If necessary, add successive sample portions to the same dish.
When evaporating in a drying oven, lower the temperature to approximately
98oC to prevent splattering.
(iv) Dry the evaporated sample for at least 1 hour at 103 to 105oC.
(v) Cool dish in the desiccator and weigh (weight of dry solids).
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(vi) Repeat cycle of drying at 103 to 105oC, cooling, desiccating, and weighing
until a constant weight is obtained, or until weight less than 4% of previous
weight.
(vii) Calculate:
4.2 Volatile and Fixed Solids (volatile and fixed residues, burned at 500oC )
(i) After completing the total solids analysis, ignite the sample and dish for 20
minutes at 500oC in a muffle furnace. (perform analysis in triplicate.)
(ii) When cooling dish in the desiccator, open the top cover for about 2 min to
let off the hot gas. Close desiccator to complete cooling.
(iii) Weigh the cooled dish.
(iv) Calculate:
(i) Place the pre-treated glass-fibre filters on filtration manifold with distilled
water.
(ii) Select sample size that will yield between 10 and 200 mg residue. Keep
sample mixed.
(iii) Filter sample to dryness. If pipetting small volumes (use a sawed-off pipette)
and pipette into approximately 10 mL of distilled water to ensure sample is
well distributed over filter. Do not use 10 mL of distilled water if saving the
filtrate for analysis of total dissolved solids.
(iv) Transfer filter back to its original planchet with forceps and dry filter plus
planchet for 1 hour at 103oC.
(v) Cool in desiccator and weigh (dry weight of solids plus filter and planchet).
(vi) Calculate:
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where:A = dry weight of solids plus filter and planchet, mg, and
B = weight of filter plus planchet, mg.
4.4 Volatile and Fixed Suspended Solids (volatile and fixed non-filterable
residue, burned at 500oC)
(i) After determination of TSS, ignite filter plus planchet at 500oC for 20
minutes.
(ii) Cool in desiccator and weigh (weight of burned solids plus filter and
planchet).
(iii) Calculate:
where:A = weight of solids plus filter and planchet before burning, mg,
B = weight of solids plus filter and planchet after burning, mg, and
C = weight of filter plus planchet, mg.
5. REPORT
Enter the results into the separate handout which you have been given, and answer
the question. Hand in the completed results sheet and the discussion/answer sheet to
the supervisor before leaving the laboratory.
6. DISCUSSION
(i) Calculate the solids removal efficiencies of the primary treatment process
based on raw sewage (input) and on primary effluent (output). Comment on
the results obtained.
(ii) Calculate the solids removal efficiencies of the primary treatment process
based on combined water (input) and on primary effluent (output). Comment
on the results obtained.
(iii) Compute the VSS/TSS ratios of the various wastewater samples. Comment
on the results with regard to the aerobic and anaerobic treatment processes.
Cinput - Coutput
Note : Assess the efficiency as { } 100%.
Cinput
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Table 1 Test results of solids analysis.
Sample
TSS % VSS %
Removal Removal