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Environmental Pollutants Analytical Method

Solid Substance

Name : Shinta Sagita Aritonang


NRP : 0321164000007
Lab. Assistant : Teuku Fazhamy Rafiandra
Lecturer : Welly Herumurti, ST, M.Sc

DEPARTMENT OF ENVIRONMENTAL ENGINEERING


FACULTY OF CIVIL ENGINEERING ENVIRONMENTAL AND EARTH
INSTITUT TEKNOLOGI SEPULUH NOPEMBER SURABAYA
2017
PURPOSE
The purpose of this experiment is to determine the amount of solid substance that dissolved in
water
PRINCIPAL
Solids analysis use gravimetric method which use precipitation process. Water filtration use
vacuum pump, residual burning use funace at 550C, drying use oven at 105C, and temperature stabilize
with desicator and weighing use analytical balance. Settleable solid use gravitation to precipitate lindi
sludge which put in imhoffcone funnel for observating the lindi sludge precipitation time.
LITERATURE REVIEW
Total solids in a liquid sample consist of total dissolved solids and total suspended solids. Total
dissolved solids are materials in the water that will pass through a filter with a 2.0-m or smaller nominal
average pore size. The material retained by the filter is the total suspended solids. The amount and nature
of dissolved and suspended matter occurring in liquid materials vary greatly. In potable waters, most of
the matter is in dissolved form and consists mainly of inorganic salts, small amounts of organic matter,
and dissolved gases. The total dissolved-solids content of potable waters usually ranges from 20 to 1000
mg/L, and, as a rule, hardness increases with total dissolved solids. Unlike the measurement of total solids
where sample drying is conducted at 103 to 105C, total dissolved solids analysis for water supplies is
conducted at 180C. The reason for the higher temperature used in the latter is to remove all mechanically
occluded water. Here, organic material is generally very low in concentration, so losses due to the higher
drying temperature will be negligible. In all other liquid materials, the amounts of suspended colloidal
and larger matter increase with the degree of pollution. Sludges represent an extreme case in which most
of the solid matter is suspended, and the dissolved fraction is of minor importance. Determination of the
amounts of dissolved and suspended matter is accomplished by making tests upon filtered and unfiltered
portions of samples. The term settleable solids is applied to solids in suspension that will settle, under
quiescent conditions, because of the influence of gravity. Only the coarser suspended solids with a
specific gravity sufficiently greater than that of water will settle. Sludges are accumulations of settleable
solids. Their measurement is important in practice to determine the need for sedimentation units and the
physical behavior of waste streams entering natural bodies of water. The settleable-solids determination is
used extensively in the analysis of industrial wastes to determine the need for and design of primary
settling tanks in plants employing biological treatment processes. The test is also widely used in waste-
treatment-plant operation to determine the efficiency of sedimentation units. The suspended and volatile-
suspended-solids determinations are used to evaluate the strength of domestic and industial wastes.
(Sawyer, 2003)
Total Dissolved Solids (TDS). High concentrations of TDS may affect taste adversely and
deteriorate plumbing and appliances. The EPA recommends that water containing more than 500 mg/l of
dissolved solids not be used if other less mineralized supplies are available. However, water containing
more than 500 mg/l of TDS is not dangerous to drink. Exclusive of most treated public water supplies, the
Missouri River, a few freshwater lakes and scattered wells, very few water supplies in North Dakota
contain less than the recommended 500mg/L concentration of total dissolved solids. Many households in
the state use drinking water supplies with concentrations up to 2,000 mg/l and greater. Treatment for
household use is reverse osmosis. (Scherer, 2015)
The expression, total dissolved solids (TDS), refers to the total amount of all inorganic and
organic substances including minerals, salts, metals, cations or anions that are dispersed within a
volume of water. By definition, the solids must be small enough to be filtered through a sieve measuring
2 micrometers. TDS concentrations are used to evaluate the quality of freshwater systems. TDS
concentrations are equal to the sum of positively charged ions (cations) and negatively charged ions
(anions) in the water. Sources for TDS include agricultural run-off, urban run-off, industrial wastewater,
sewage, and natural sources such as leaves, silt, plankton, and rocks. Piping or plumbing may also release
metals into the water. (Rashmi, 2015).
Water has the ability to dissolve a wide range of inorganic and some organic minerals or salts such
as potassium, calcium, sodium, bicarbonates, chlorides, magnesium, sulfates etc. These minerals
produced un-wanted taste and diluted color in appearance of water. There is no agreement have been
developed on negative or positive effects of water that exceeds the WHO standard limit of 1,000 ppm.
Total dissolved solids (TDS) in drinking water is originates many ways from sewage to urban industrial
wastewater etc. Therefore, TDS test is considered a sign to determine the general quality of the water.
Figure 5 clears that in Islamic colony these values were ranges from 290-595 ppm. In Satellite town TDS
range is 406-694 ppm and in Shahdrah these values range from 401-429 ppm. Hence, these ranges were
acceptable and concentration of TDS is not harmful. (Mohsin,2013)
Total suspended solids are the portion of solids that usually remains on the filter paper. TSS will
also increase the temperature and reduce photosynthesis. Fine particles may also clog and abrade fish and
insect gills and tissue and interfere with egg and larval development. The wastewater with high TDS
value can cause salinity problem if discharged to irrigation water. It may also add a laxative effect to the
water or cause the water to have an unpleasant mineral taste. Moreover, it can impart undesirable color to
the wastewater too. (K., Ghayas, 2015).

SCHEME :
1.1 Total Solid Analysis
Petri dish

Burn Petri dish in furnace at 550C for an hour. Then oven it for 15
minutes and then put it in desiccators. Weigh it using analytical
25 ml balance.
sample Pour 25 ml sample into Petri dish. Oven it for 24 hours and then
put it in desiccators for 15 minutes. Weigh it using analytical
balance. Calculate the total solids.

Result
1.2 Total Organic and Inorganic Solid Analysis
Petri dish and residue of total solid analysis

Burn it in furnace for an hour then oven it for 15 minutes


and then put it in desiccators for 15 minutes. Calculate
the total organic and inorganic solid.
Result
2.1. Total Suspended Solid Analysis
Petri dish

Burn in furnace for an hour.

Petri dish and Filter paper


Oven its for 15 minutes then put its on desiccators for 15 minutes.
Weigh its using analytical balance.
Filter Paper, and 25
ml sample
Put filter paper on vacuum pump then pour solution through it.

Filter paper contain residue and


petri dish
Put filter paper on petri dish. Then oven its for an hour. Cool it
down in desiccators for 15 minutes and weigh it using analytical
balance
Result

2.2 Total Organic and Inorganic Suspended Solid Analysis

Petri dish + residu after oven


Burn in furnace for an hour.

Petri dish and filter after furnace


Oven its for 15 minutes, and then put it in desiccators for 15 minutes.
Weigh its using analytical balance and calculate the total organic and
inorganic suspended solid.
Result

OBSERVATION RESULT
Total Solid
Nu Treatment Observation Result Photo
mbe
r
1 Take the petri dish from Petri dish was in room temperature.
desiccators, it has been in furnace Petri dish weight : 29,0503 gr
and oven before. Weigh it using
analytical balance.

Fig.1 Petri dish in


desiccators
2 Pour 25 ml sample into Petri dish. The sample : turbit, the color brown-
Oven it for 24 hours. yellowish, in room temperature, odorless.

Temperature of oven is 1050C

Fig.2 Pour sample in


petri dish

Fig.3 Petridish + sample


in oven
3 Put it in desiccators for 15 minutes. After oven, there was no water in the
Weigh it using analytical balance. petridish, just yellow cycle in the petri dish (
Calculate the total solids. yellow ashes )
After desiccators the temperature decrease
and became in room temperature.
Weight after oven : 29,0866 gr
Fig.4 Petridish + sample in
desiccators

Fig.5 Petridish + sample


weighted
4 Burn the sample + petridish (step2) The temperature of furnace is 550oC.
in furnace for an hour. After furnace it looked like there was no
sample in the petri dish because all was
burned.

Fig.6 Petri dish +


sample ignated
5 Oven it for 15 minutes. The temperature of oven is 1050C

Fig.7 Petri dish +


sample in oven
6 Put it in desiccators for 15 minutes. The temperature decrease after desiccator and
Calculate the total organic and became room temperature.
inorganic solid. Weight after furnace : 29,0802 g

Fig.8 Petridish + sample in


desiccators.

Total Suspended Solid


Nu Treatment Observation Result Photo
mbe
r
2 Take the petri dish and filter paper Weight of :
from desiccators, it has been in Petri dish : 20,7541 gr
furnace and oven before (filter Filter paper : 0,1659 g
paper only from oven ). Weigh it
using analytical balance
Fig.9 Petri dish +filter
paper in desiccators

Fig.10 Petri dish


+filter paper weighted
3 Put filter paper on vacuum pump The sample : turbit, the color brown-
then pour 25mL sample through it. yellowish, in room temperature, odorless.
After filtered, there were some yellow thin
ashes residue on the filter paper.

Fig.11 Sample filtered


in vacuum pump Fig.11 Sample filtered in
vacuum pump
4 Put filter paper on petri dish. Then Oven is 105oC.
oven its for an hour. After oven, the filter paper become dry and
the temperature high.

Fig.12 Petri dish + sample


in oven
5 Cool it down in desiccators for 15 After desiccators, the sample had same
minutes and weigh it using temperature as room temperature.
analytical balance. Weight after oven : 20,9206 gr

Fig.13
Petridish + sample after
ovenin desiccators.

Fig.14
Petridish + sample after
oven weighted
6 Burn the sample + petridish (step5) Furnace is 550oC.
in furnace for an hour. After furnace the filter paper become grey
ashes. The temperature was high.

Fig.15 Petri dish +


sample ignated
7 Oven it for 15 minutes. Oven is 105oC.
The sample was still hot, but the temperature
was not as high as after burned in furnace

Fig.16 Petri dish +


sample in oven
8 Put it in desiccators for 15 minutes. After desiccators, the sample had same
Calculate the total organic and temperature as room temperature.
inorganic solid. Weight after furnace : 20, 7536 gr

Fig.17 Petri dish +


sample in
desiccators

DICUSSION
The third experiment of Environmental Pollutants Analytical Method was held
on Friday, Novenber, 3 2017 at 08.00 WIB until around 12.00 WIB in Water
Treatnment Laboratory of Environmental Engineering Department, ITS Surabaya. The
experiment consists of two parts. First was Total Solod Analysis and second Total
Suspended Solid Analysis. In this experiment we must prepare the sample. Sample of
this experiment was taken in long storage of ITS, the location is behind the Composting Fig.18 Location
of sampling
House, Jl. Arif Rachman Hakim (shown by the picture beside) using manual method.
The sample was taken using bucket that tied with rope then throw into the water. The sample is clear,
odorless, at room temperature, and aqueous. The equipments that we used for this experiment were
Porselain cups, furnace, oven, desiccators, pin set, analytical balance, a measuring cylinder, filter paper,
vacuum pump.
1. Total Solids
Total solids in a liquid sample consist of total dissolved solids and total suspended solids. Total
dissolved solids are materials in the water that will pass through a filter with a 2.0-m or smaller nominal
average pore size. The material retained by the filter is the total suspended solids. The amount and nature
of dissolved and suspended matter occurring in liquid materials vary greatly. In potable waters, most of
the matter is in dissolved form and consists mainly of inorganic salts, small amounts of organic matter,
and dissolved gases. The total dissolved-solids content of potable waters usually ranges from 20 t/o 1000
mg/L, and, as a rule, hardness increases with total dissolved solids. Unlike the measurement of total solids
where sample drying is conducted at 103 to 105C, total dissolved solids analysis for water supplies is
conducted at 180C (Sawyer, 2003). The purpose of this analysis is to know the amount of total solids in
the water sample. First thing to do was took and prepared the materials and equipments which are needed.
take pocelain from decicator the porcelain has been furnace and oven first this step was to sterilize the
petri dish. Weigh it with analytical balace. Petri dish weight was 29,0503 gr. Then pour 25 ml sample into
the porselain cup that already weighed, note the sample volume. 25 ml water sample is clear-yellowish, a
little bit odorous, at room temperature, aqueous, and there is a little bit of dirt. Store it in the 105oC oven
for 24 hours to remove water content. After stored in oven for 24 hours, the sample was dry, yellow
ashes, and had high temperature(105C). Here, organic material is generally very low in concentration, so
losses due to the higher drying temperature will be negligible (Sawyer, 2003). Then cooled it down in
desicator for 15 minutes to stabilize the temperature. Weigh with analytical balance. Petri dish+sample
weight was 29,0866 gr. Then calculate the total solid :
TS = (29,0866gr - 29,0503gr) x 106 : 25 = 1452 mg/L.
To find total fix solids, the dish contain sample was burned in furnace 550C for an 1 hours to remove all
the organic matter. After that stored in the 105oC oven for 15 minutes to stabilized the temperature after
burned in furnace. Cooled it down in the desicator for 15 minutes to stabilize the temperature become
room temperature. Finally weighed it again using analytical balance.
Petridish+sample weight after furnaced was 29,0802 gr.
TVS= (mg Petridish+sample before ignate - mg Petridish+sample after ignate) x 106 : 25
= (29,0866gr - 29,0802gr) x 106 : 25 = 256 mg/L.
TFS = (mg Petridish+sample after ignate - mg Petridish) x 106 : 25
=(29,0802gr - 29,0503gr) x 106 : 25 = 1196 mg/L.

2. Total Suspended Solids


Total suspended solids are the portion of solids that usually remains on the filter paper. TSS will
also increase the temperature and reduce photosynthesis. Fine particles may also clog and abrade fish and
insect gills and tissue and interfere with egg and larval development (K., Ghayas, 2015). The purpose of
this analysis is to know the amount of total of suspended solids in the water sample. First thing to do was
took and prepared the materials and equipments which are needed.. Then, take porselain cups and filter
paper from desiccators that has been in oven and furnace ( filter paper only from oven ). After desiccators,
the sample had same temperature as room temperature. Filter paper is white and has 2.5m pore diameter,
it should be 1.2m or less. Weigh the porselain cup and filter paper with analytical balance. Petri dish
weight was 20,7541 gr. The filter paper weight was 0,1659 gr. Put the filter papers that has been weighed
into the filter vacuum. Pour 25 ml Sample into the filter, note the sample volume. Filter the sample to get
the suspended solid. 25 ml water sample is clear-yellowish, a little bit odorous, at room temperature,
aqueous, and there is a little bit of dirt. After filtered, there were some grey thin ashes residue on the filter
paper. Place the filter paper into the petridish and store it into 105oC oven for 1 hour. Cool it in the
desiccators for 15 minutes. Weigh with analytical balance. Petri dish + filter paper + residue weight was
20,9206 gr. The residue retained on the sieve is dried until it reaches a constant weight at a temperature of
103C to 105C. The weight increase of the filter represents total suspended solids (TSS). If suspended
solids inhibit the filter and prolong the filtration, the pore diameter of the filter needs to be enlarged or
reduces the sample test volume. To obtain a TSS estimate, we calculated the difference between total
dissolved solids and total solids.
TSS = (mg Petridish+residu after oven - mg Petridish+filter paper before oven) x 106 : 25
= (20,9206 gr (20,7541 gr + 0,1659 gr. )) x 106 : 25 = 24 mg/L.
To find total fix solids, the dish contain sample was burned in furnace 550C for an hour minutes. After
that stored in the 105oC oven for 15 minutes to stabilized the temperature after burned in furnace. Cooled
it down in the desicator for 15 minutes because desiccators can stabilize the temperature to become room
temperature. Finally weighed it again using analytical balance. Petridish+sample weight after furnaced
was 20,7536 gr.

TVSS = (20,9206 - 20,7536 ) x 106 : 25 = 6680 mg/L


TFSS = (20,7536 20,7541 ) x 106 : 25 = -20 mg/L
TDS = TS TSS
= 1452 mg/L -24 mg/L = 1428 mg/L
TVDS = TVS TVSS
= 256 mg/L - 6680 mg/L = -6424 mg/L
TFDS = TFS TFSS
= 1196 mg/L - -20mg/L = 1216 mg/L.

The minus velue in calculation happened may caused by the petridish was not steril, so when we weight
the petri dish, the organic matter was weighted too and was also burned in furnace.
Checking the precision value of TS base on analysis and formula :
TS = 1452 mg/L.
TS = TSS + TFS = 24 + 1196 = 1220 mg/L
The difference between TS analysis and formula is 232 mg/L.
The expression, total dissolved solids (TDS), refers to the total amount of all inorganic and
organic substances including minerals, salts, metals, cations or anions that are dispersed within a
volume of water. By definition, the solids must be small enough to be filtered through a sieve measuring
2 micrometers. TDS concentrations are used to evaluate the quality of freshwater systems. TDS
concentrations are equal to the sum of positively charged ions (cations) and negatively charged ions
(anions) in the water. Sources for TDS include agricultural run-off, urban run-off, industrial wastewater,
sewage, and natural sources such as leaves, silt, plankton, and rocks. Piping or plumbing may also release
metals into the water. (Rashmi, 2015)
TSS is closely related to turbidity because turbidity in water is due to suspended substances present
in the water. Suspended substances present in water consist of various substances, such as fine sand, clay
and natural mud which are inorganic materials or can also be organic materials floating in water. Organic
substances that are suspended substances consist of various types of compounds such as cellulose, fats,
proteins that float in water or can also be microorganisms such as bacteria, algae, etc., but because the
suspended substances present in the water consist of various kinds of substances of different shapes and
weights are different then turbidity is not always proportional to the level of suspended substances.
Base on PERMENKES RI 2010 for Total Dissolved Solid is 500 mg / L. So it can be concluded the water
from long storage is not feasible for consumption.
CONCLUSION

By this experiment, we can determine the amount of solid substance that dissolved in water.
TS = (29,0866gr - 29,0503gr) x 106 : 25 = 1452 mg/L.
TVS = (mg Petridish+sample before ignate - mg Petridish+sample after ignate) x 106 : 25
= (29,0866gr - 29,0802gr) x 106 : 25 = 256 mg/L.
TFS = (mg Petridish - mg Petridish+sample after ignate) x 106 : 25
=(29,0802gr - 29,0503gr) x 106 : 25 = 1196 mg/L.
TSS = (mg Petridish+residu after oven - mg Petridish+filter paper before oven) x 106 : 25
= (20,9206 gr (20,7541 gr + 0,1659 gr. )) x 106 : 25 = 24 mg/L.
TVSS = (20,9206 - 20,7536 ) x 106 : 25 = 6680 mg/L
TFSS = (20,7536 20,7541 ) x 106 : 25 = -20 mg/L
TDS = TS TSS
= 1452 mg/L -24 mg/L = 1428 mg/L
TVDS = TVS TVSS
= 256 mg/L - 6680 mg/L = - 6424 mg/L
TFDS = TFS TFSS
= 1196 mg/L 20 mg/L
REFERENCES

K., Ghayas, Ayaz K., Arshad A., Naveed A., M. Jawad A., H. Shahab, H. Umaira S. 2015. The Study on
Textile Mill Effluent. 1(3):90-94.
Mohsin, M., Samira Safdar, Faryal Asghar, Farrukh Jamal. 2013. Assessment of Drinking Water Quality
and its Impact on Residents Health in Bahawalpur City. 3(15).
Rashmi. 2015. An Examination of Total Solid Percentage Comparison between Oven, Mojonnier. SSRG
International Journal of Humanities and Social Science (SSRG-IJHSS).
Sawyer, Clair N., and Pervy L. Mc. Carty. 2003. Chemistry For Environmental Engineering And Science.
New York: Mc. Graw Hill Book Company. Pp: 649, 651, 657.
Scherer, Tom. 2015. Drinking Water Quality: Testing and Interpreting Your Results. North Dakota State:
NDSU Extension Servipce.
QUESTION AND ANSWER
1. What can be known by an existance of organic solid?

By an existance of organic solid that can be used as the basic of :

Fastening the water treatment plant Secondary precipitation


system, so that can prevent the Sludge treatment plant for waste water
effectivelessness treatment
Activated sludge system Sludge composition inside the river
Primary precipitation water
2. What must be prevented in the solid organic and inorganic analysis? Explain why!

The temperature that too high or too low Loosen the crystal water by burning
Left sample water process
Organic substances that ravelled by heat The porselain cup that not sterile.
Moisture content
By the existance of those disturbances affect the analysis by reducing or adding extra organic
substances.

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