1.

OBJECTIVE

To provide and strenghten knowledge, skill, understanding in solid determination and enable
to relate theories taught to the practices in laboratory.
2.0

LEARNING OUTCOME

At the end of this course students are able to:

(1)

Apply knowledge in solid determination

(2)

Analyze the laboratory result and differentiate between suspended solid and
dissolve solid

(3)

Identify problems and use their generic skill to solve problems

Develop their ability to work in group

3.0

THEORY
Solids refer to matter suspended or dissolved in water or waste water. 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 a favorable physiological reaction
in the transient consumer. Solids analyses are important in the control of biological and
physical wastewater treatment process and for assessing compliance with regulatory agency
wastewater effluent limitations.
Generally, total solids is the term applied to the material residue left in the dishes
after evaporation of a sample at 103C to 105C. Total solids include total suspended solids,
and total dissolved solids. Total suspended solids is the portion of total solids retained by
filter, and total dissolved solids is the portion of solids that passes through a filter of 2.0 m
(or smaller) nominal pore size under specified conditions. Fixed solids is refer to the residue
of total, suspended, or dissolved solids after heating to dryness for a specified time at a
specified temperature (500C 50 C for 15 minutes).
The weight loss on ignition is called volatile solids. Determination of fixed and
volatile solids does not distinguish precisely between inorganic and organic matter because it
includes losses due to decomposition or volatilization of some mineral salts. 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.

Settleable solids

Imhoff cone

Samples

Total solids

Microwave (at(TS)
103C - 105C)

Filter paper

Fibre glass filter (

2.0m)

Microwave (at
103C - 105C)

Microwave (at
180C 2C)

Suspended solids (SS)

Dissolved solids (DS)

Muffle furnace (at

500C 50C)

Volatile suspended
solids (VSS)

Dissolved Solid

Muffle furnace (at

500C 50C)

Fixed suspended solids

(FSS)

Volatile dissolved
solids (VDS)

Total volatile solids TVS

= VSS + VDS

Fixed dissolved solids

(FDS)

Total fixed solids

TFS = FSS + FDS

Total solids (TS)

DIAGRAM 1.0

4.0 EQUIPMENTS AND MATERIAL

i.

Evaporating dishes: Dishes of 100mL capacity made of porcelain, platinum or

high-silica glass.

ii.

Muffle furnace for operating at 500C 50C

iii.

Steam bath

iv.

Desicator

v.

Drying oven

vi.

Analytical balance

vii.

Magnetic stirre

5.0

viii.

Graduated cylinder

ix.

Wid-bore pipet

x.

Low-form beaker

PROCEDURES
There are three procedures to determine the Total Solid (TS) where

At the first procedure is by complete the Total Suspended Solid (TTS),

Second is determine the Total Dissolved Solids (TDS)
And lastly determine the Total Volatile Solids (TVS).

To determine the total suspended solids, the glass fiber filter disc were prepared
and then the filter disc inserted onto the base and the funnel was clamped. The discs
were washed with three successive 20ml distilled water while vacuum is applied. All
traces of water were removed by continuing to apply vacuum after water had passed
through. Funnel from base was removed and filter was placed in the dish and dried in
an oven at 103c - 108c for 45 minute. The dish removed from the oven and then
desiccated and the weights were got. 10mL sample volume were selected that will
yield not more than 200mg of total suspended solids. The filter was placed on the base
and clamped on funnel and applied the vacuum. The filters with small volume water
were wet to seal filter against the base.

The samples vigorously were shake and quantitatively transfer required volume
(mL) of sample to the filter using a large orifices, volumetric pipette. All trace of
water was removed by continuing to apply volume after samples had passed through.
The Pipette and funnel rinsed onto the filter with small volume of distilled water. All
traces of water were removed by continuing to apply vacuum after samples had
passed through. The disc was removed carefully from the base. At least one hour dried
at 103c - 108c and then cooled in a desiccator and weighed.
The second procedures were to determine the total dissolved solids where at
the first step were by prepared the evaporating dish. Ignite cleaned evaporating dish at
500C + 50C for one hour in muffle furnace and then stored in desiccator until
needed. Immediately weigh before used. Samples volume were choose to yield
between 2.5 and 200 mg dried residue. More than 10 minutes are required to complete
filtration.
The samples stirred with magnetic stirrer and a measures volume filled onto
glass-fibre filter by using pipette with applied vacuum. Three successive 10 mL of
distilled water washed, allowed complete drainage between washings, and continued
suction for about three minutes after filtration complete.
Total filtrate (with washing) were transferred to a weighed evaporating dish
and evaporated to dryness on a drying oven. Evaporated samples were dried for at
least 1 h in an oven at 180C + 2C, and then cooled in a desiccator to balance
temperature, and weighed. Drying cycle of drying, cooling, desiccating, and weighing
until a constant weigh is obtained was repeated. (The filtrate from the total suspended
solids determination may be used for determination of total dissolved solids.
Lastly is by determine the total volatile solids where if the volatile solids are to
be measured, the residue from method A and B is ignited at 500C + 50C for 15
minutes in a muffle furnace and then cooled in desiccator to balance temperature and
weigh. Cycle of drying or igniting, cooling, desiccating, and weighing until a constant
weight change less than 4 % of the previous weighing or 0.5 mg, whichever is less
were repeated and then stored in desiccator until needed.

6.0

RESULT AND CALCULATION

6.1 Unfiltered Sample

(a)

Data For Total Solid Test

1
2
3
4
5

Volume of sample (ml)

Weight of evaporating dish (g)
Weight of evaporating dish + sample
Weight of sample (g)
Weight of evaporating dish +sample after drying process at 103C -

Sample
5
48.9166
52.9388
4.0222
48.8888

105C
Weight of solid (g)

0.0278

6.2 Filtered Sample

(b) Data For Total Suspended Solid (Ss)

1
2

Volume of sample (ml)

Weight of filter paper (g)

Sample
5
0.0912

3
4
5
6
7
8

Weight of filter paper + solid after drying at 180C

Weight of solid (g)
Weight of filter + solid after drying at 500C 50C
Weight of volatile solid (g)
Total suspended solid (SS)(mg/L)
Percentage of solid volatile suspended solid (VSS) %

Total Suspended Solid/L

= ( (Weight of filter + dried residue) - Weight filter) x 1000
------------------------------------------------------------------Sample Volume
= (0.0876 0.0912) X 1000
-------------------------------(5 1000)
= 720

0.0876
0.0036
0.0951
0.0039
720
108.33%

(C) Data for Total Dissolve Solid (TDS)

No

Data

Sample

Volume of sample (ml)

Weight of evaporating dish (g)
Weight of evaporating dish + sample (g)
Weight of sample (g)
Weight of evaporating dish + sample after drying at

5
34.1020
39.2944
5.1924
34.213

180oC (g)
Weight of Solid (g)
Total Dissolve Solid (TDS) (mg/L)
Weight of evaporating dish + solid after drying at

0.111
22200
34.0792

500oC 50oC (g)

Weight of dissolved solid (g)
Total dissolved Solid (SS) (mg/L)
Percentage of Volatile dissolved Solid (VSS) %

0.1338
79.92
120.54

.
1
2
3
4
5
6
7
8
9
10
11

Total Dissolve Solid

Weight of sample
= (Weight of evaporating dish + sample) (Weight of evaporating dish)
= 39.2944 34.1020
= 5.1924g

Weight of solid
= (Weight of evaporating dish + sample after drying at 180oC) (Weight of evaporating dish)
= 34.213 34.1020
= 0.111g
Total Dissolve Solid
= (Weight of solid) x 1000 x 1000
volume of sample
= 0.111x 1000 x 1000
5
= 22200 mg/L
Weight of dissolved solid
= (Weight of evaporating dish + sample after drying at 180oC) (Weight of evaporating dish
+ solid after drying at 500oC 50oC)
= 34.213 34.0792
= 0.1338g
Total Dissolved Solid
= (Weight of solid) x 1000 x 1000
volume of sample
= 0.0003996 x 1000 x 1000
5
= 79.92 mg/L
Percentage of Volatile Dissolved Solid
= (Weight of dissolved solid) x 100
weight of solid
= 0.1338 x 100
0.111
= 120.54%

7.0

DISCUSSION AND CONCLUSION

7.1 DISCUSSION
1. Distinguish between suspended solid and dissolve solid.

SUSPENDED SOLID
DISSOLVE SOLID
The smaller the particle size, the
Generally the operational definition
greater the surface area per unit

is that the solids must be small

mass of particle, and so the greater

enough to survive filtration through

the pollutant load that is likely to be

a sieve the size of two micrometer

carried.

Solid in water that can be trapped

The total amount of all inorganic

by a filter. Include a wide variety of

and organic substance including

material such as silt, decaying plant

minerals, salt, metals, cat ions or

and animal matter, industrial wastes

anions that are dispersed within a

and sewage.
Include solid that either float on

volume of water.
Include colloidal solids that not

water or suspended in water.

large or heavy enough to settle

readily,

It also include small settle able

nor

small

enough

to

dissolve in the water.

Dissolve substance are undesirable

solids that will not remain afloat, it

in water because it can impart

will slowly separate from the water

aesthetically displeasing color, taste

(settle out) if the water is left

and odor.

relatively undisturbed.
Important as a pollutant

and

Generally considered not a primary

pathogens. Carried on the surface of

pollutant, but it is rather used as an

particles. The greater the pollutant

indication

load that is likely to be carried.

characteristics of drinking water.

of

aesthetic

2. Suggest some possible causes of high levels of total suspended solids.

The possible causes of the high levels of total suspended solids in wastewater could
be divided by 2, the first is depends mainly on the usage/purpose of fresh water and
the second is depends on where the wastewater comes from and what purpose it was
used for. Besides, the range of the flow rate can cause of high levels of total

suspended solid. In that case, Fast running water can carry more particles and largersized sediment. Heavy rains can pick up sand, silt, clay, and organic particles from the
land and carry it to surface water.
3. The suspended solids for a wastewater sample were found to be 175mg/L. If the
following test results were obtained, what size sample was used in the analysis?

Tare mass of glass fibre filter = 1.5413g

Residue on glass fibre filter after drying at 105C = 1.5538g

Mg total suspended solids/L =

( AB ) x 1000
Sample volume , ml

( 1553.81541.3 ) x 1000
Sample volume , mL

175 mg/L =

Sample volume, ml =

( 1553.81541.3 ) X 1000
175
12500
175

= 71.4 ml

7.2

CONCLUSION
From the result on Total Dissolve Solid (TDS) and Volatile Dissolve Solid (VDS) that

we got, weight of sample for sample A and sample B are 5.1924g and 3.69g. Meanwhile, the
dissolved solid for sample A and sample B are only 0.1338g and 0.063g. Total Dissolve Solid

(TDS) for this experiment are 79.92 mg/L for sample A and 1476 mg/L for sample B. From
calculation, the percentage of solid in sample is 120.54% for sample A and 0.813% for
sample B. So, we can conclude that these two samples are serious on pollution and their
water quality is in bad condition because the percentage of solid sample are too high.
For experiment on Total Suspended Solid (TSS) and Volatile Suspended Solid (VSS),
weight of suspended solid for sample A and sample B are 720 mg/L and 400mg/L. On the
other hand for sample A, 108.33% from TDS is Volatile Suspended Solid (VSS) or organic
material. And for sample B, there is 0.042% from TDS is VSS.
Supposedly, the Total Solid (TS) that we should get for this experiment is the total
summation of TDS and TSS. So, if we compare these two results we can conclude that there
are some errors occurred while doing this experiment. So, from the result base on the data in
this experiment, we can conclude that the standard deviation for both samples is small. It
maybe cause by some reason like maybe have an error occur during we take the data
especially the weight value measurement and maybe the sample are not enough heating in the
oven, that why the value of experimental more than theoretical.