NANYANG TECHNOLOGICAL UNIVERSITY

School of Civil and Environmental Engineering

EN2703: Laboratory 2C

Laboratory Manual

For

Experiment Lab2C-4 (EN)

Solids Analysis

Location : Environment Laboratory II, N1-B3c-49

Session 2004/2005
 Solids (Residue) Analysis

1. OBJECTIVES

(i) To introduce the definitions, analysis methods, and environmental

significance of various kinds of solids, and
(ii) To determine the solids content of different sewage and sludge samples.

2. THEORY

Environmental engineering is concerned with the solid material in a wide range of

natural waters and wastewaters. The usual definition of solids (referred to as "total
solids") is the matter that remains as residue upon evaporation at 103~105oC. The
organic fraction of solid material is estimated (by weight loss) by burning the sample at
500 50oC to volatilize the organics. The various components of "total solids" can be
simplified as follows:

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)

Figure 1: Solids Analysis

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 measurement of solids is by means of the gravimetric procedure. The various

forms of solids are determined by weighing after the appropriate handling procedures.

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:

Batch Wastewater Sample Sludge Sample

1 Raw waste Primary sludge

2 Combined water Thickened activated sludge
3 Primary effluent Digested sludge
4 Secondary effluent Dewatered sludge
5 Mixed liquor Return sludge
6 Combined water Primary sludge
7 Primary effluent Digested sludge
8 Secondary effluent Return sludge

4.1 Total Solids (Total residue, dried at 103oC)

(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:

Total solids, as % by weight = A C 100 (1)

B C

where:A = weight of dried residue plus dish, mg,

B = weight of wet residue plus dish, mg, and
C = weight of dish, mg.

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:

Volatile solids, as % total solids = A B 100 (2)

A C

Fixed solids, as % total solids = B C 100 (3)

A C
where:A = weight of residue plus dish before burning, mg,
B = weight of residue plus dish after burning, mg, and
C = weight of dish, mg.

4.3 Total Suspended Solids (total non-filtrable residue, dried at 103oC)

(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:

TSS, mg / L = (A B) 1,000 (4)

mL sample

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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:

Volatile Suspended Solids, mg / L = (A B) 1,000 (5)

mL sample

Fixed Suspended Solids, mg / L = (B C) 1,000 (6)

mL sample

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.

Wastewater TSS (mg/L) VSS (mg/L) VSS / TSS ratio

Sample

Result 1 Result 2 Average Result 1 Result 2 Average

Raw Sewage
Combined Water
Primary Effluent
Secondary Effluent
Mixed Liquor
Sludge Sample TS (% Dry Weight ) VS (% TS)

Result 1 Result 2 Average Result 1 Result 2 Average

Primary Sludge
Thickened AS
Digested Sludge
Dewatered Sludge
Return Sludge
 Table 2 % of Removal Efficiency

TSS % VSS %
Removal Removal

Raw Sewage to Primary Raw Sewage to Primary

Effluent Effluent
Combined Water to Primary Combined Water to Primary
Effluent Effluent

Comments on VSS / TSS Ratio

January 14, 2005

Lab2C-4(EN) Solids Analysis.doc