TITLE

Gravimetric Analysis

OBJECTIVE

To examine the solids content of water samples.

INTRODUCTION

Particulate matter that found in ground water and surface can cause cloudy
appearance. Due to the high specific surface area, these matter play a major role in
regulating the transport and distribution of chemical compound. Suspended particle in
water also indicate the present of bacterial and non-bacterial pathogens. The size of the
waterborne particle spanning roughly 0.001 m to 100 m. The composition of these
particle can either be organic, inorganic or both. Suspended particle which diameter less
than 1 m cannot settle readily, they are mobile hence can enhance the transportation of
contaminants in surface as well as ground water.

Gravimetric Analysis.

There are a few method that are commonly use to gravimetrically classify solid by size
and its chemical characteristic. Filtration is used to separate suspended particle with
dissolved particle. In this technique, glass fiber are used to obtain the suspended particle as
they pass through the deep mat of fiber. As the average pore size and collection efficiency
of commercial filter are different, so it is important to specify the type of filter used.
 Evaporation separate water from the dissolved and suspended particle. The drying
temperature has an significance effect upon the result. Two drying temperature that
commonly used is 103-105C and 179-181C. For a solution which contain high
concentration of organic matter, lower temperature is used. High temperature may cause
volatilization and decomposition of the organic matter and lead to significant weight loss.

Conductivity.

The conductivity of a solution is a measure of its ability to carry an electric current. It

depend of the temperature, present of ion, concentration, mobility and valence.
Conductivity of a solution can used as a measure of dissolved solid in the solution and the
higher the conductivity, the greater amount of dissolved solid. The conductivity of
deionized water is typically between 0.5 and 3.0 S/cm, and that of portable water range
between 50 and 1500S/cm. Waste water conductivity can be as high as 10000 S/cm.

Unit for conductivity are in current use. While the tradition unit for conductivity is 1
ohm-cm, or mho/cm. In the SI system of units, siemens (S) is the reciprocal of ohm and
conductivity is usually in S/cm. Thus S/cm and mho/cm are equivalent units By using
the conductivity, we can estimate the total dissolved solids of water sample by multiply the
conductivity value by an empirical constant. This empirical constant should be determined
for a particular water sample by comparing the conductivity measurement to a direct
gravimetric analysis.
 EQUIPMENT AND MATERIAL

1. Tap water 1L

2. Student water sample 1L

3. Deionized water 1L

4. Standard solution (100mg/L kaolin + 100mg/L Nacl)

5. Filter paper

6. Volumetric flask

7. Schott bottle

8. Measuring cylinder

9. Beaker

10. Volumetric pipette

11. Pipette pump

12. Evaporating dish

13. Tweezers

14. Conical flask

15. Filter funnel

16. Desiccator

17. Conductivity mter and probe

18. Oven

19. Analytic balance

 PROCEDURE

Conductivity:

1. Conductivity meter is turned on and the conducting probe is placed in the conductivity
standard solution to verify that the meter is responding accurately.

2. 200 ml of sample is obtained and placed in a 250 ml beaker.

3. Probe is placed inside the solution and conductivity is measured. The data is recorded
in S/cm.

4. TDS (in mg/L) is estimated by multiplying the conductivity by a conversion factor of

0.55.

5. Mode for the conductivity meter is changed to pH measurement and the pH of our
sample is recorded.

Total Solid (TS)

1. Balanced is set to zero before use.

2. A glass beaker is weighted to nearest 0.1 mg.

3. 25.0 ml of sample solution is added using a volumetric pipe.

4. The sample then evaporated in an oven at 105C. After that, it is cooled in a desiccator
to room temperature.

5. The balance is set to zero again .Glass beaker is removed and reweighed to the nearest
0.1 mg.

Total Suspended Solid (TSS)

1. Balance is set to zero.

2. The pre-washed and dried filter is transfered from the desiccator to a balance and its
weight is measured to the nearest 0.1 mg.

3. A filter funnel is placed on top of 250 ml flask.

4. 0.250 litre of sample is measured and poured through using a volumetric flask.

5. The sample container is washed with 50 ml of deionized water and poured the solution
onto the filter. After all the solution [passed through the filter, the solution is discarded
in the filter flask.

6. Filter is then removed by tweezers and evaporated to dryness at 105C.

7. After that, the filter paper is cool in the desiccator.

8. The balance is set to zero and filter paper is weighted. The filter paper is remove and
reweighed to the nearest 0.1 mg.
 RESULTS AND CALCULATIONS

Conductivity and pH

Conductivity ( S/cm ) TDS

Water Sample pH
1 2 3 Average (mg/L)
Standard Solution 1451 1391 1425 1422.33 5.2 782.2815
Tap Water 69.7 69.5 69.0 68.73 6.0 37.8015
Drinking Water 66.8 66.7 67.3 66.93 6.0 36.8115
Deionized Water 0.83 0.79 0.80 0.81 6.2 0.4455
Table 1.0 The Conductivity and pH for Different Water Samples

Total Solids (TS)

Standard Drinking
Water Samples Tap Water Deionized Water
Solution Water
Weight of Dish (g) 41.3166 43.0544 48.1428 44.5483
Weight of Dish +
65.2791 67.5035 71.9712 68.8053
Water Sample (g)
Weight of Dish +
41.3256 43.0436 48.1237 44.5062
Residue (g)
Weight of Water
23.9625 24.4491 23.8284 24.2570
Sample (g)
Weight of Residue (g) 0.0090 -0.0108 -0.0191 -0.0421
Total Solids (mg/L) 360 -432 -764 -1684
Percentage of Total
0.0376 -0.0442 -0.0802 -0.1736
Solids (%)
Table 2.0 The Weights of Water Sample, Residue, Total Solids and Percentage of Total
Solids for Different Water Samples.

Total Suspended Solids (TSS)

Standard Drinking
Water Samples Tap Water Deionized Water
Solution Water
Weight of Filter (g) 0.5179 0.5297 0.5264 0.5193
Weight of Filter +
0.5136 0.5180 0.5155 0.5076
Residue (g)
 Weight of Water
249.55 249.55 249.55 249.55
Sample (g)
Weight of Residue (g) -0.0043 -0.0117 -0.0109 -0.0117
Total Suspended
-17.2 -46.8 -43.6 -46.8
Solids (mg/L)
Percentage of Total
-0.00172 -0.00469 -0.00437 -0.00469
Suspended Solids (%)
Table 3.0 The Weights of Water Sample, Residue, Total Suspended Solids and
Percentage of Total Suspended Solids for Different Water Samples.

Sample Calculation

Conductivity and pH

Let's take standard solution from Table 1.0 as the sample calculation.

1451+ 1391+ 1425

Average of conductivity= =1422.33 S /cm
3

TDS=1422.33 0.55=782.2815 mg/L

Total Solids (TS)

Let's take standard solution from Table 2.0 as the sample calculation.

Weight of Water Samp ( Weight of Dish+Water Sample )(Weight of Dish)

Weight of Water Sample=65.279141.3166=23.9625 g

Weight of Residue= (Weight of Dish+ Residue )(Weight of Dish)

Weight of Residue=41.325641.3166=0.0090 g
 Weight of Residue
Total Solids=
Volume of Water Sample

1000mg
0.0090 g
1g
Total Solids= =360 mg/ L
1L
25.0 mL
1000 mL

Weight of Residue
Percentage of Total Solids= 100
Weight of Water Sample

0.0090
Percentage of Total Solids= 100 =0.0376
23.9625

Total Suspended Solids (TSS)

Let density of water = 998.2 g/L at 20 , volume of water = 0.250 L.

Weight of Water Sample=Density of water Volume of water

Weight of Water Sample=998.2 0.250=249.55 g

Weight of Residue= (Weight of Filter + Residue )(Weight of Filter )

Weight of Residue=0.51360.5179=0.0043 g

Weight of Residue
Total Suspended Solids=
Volume of Water Sample
 1000 mg
0.0043 g
1g
Total Suspended Solids= =17.2 mg/ L
0.25 L

Weight of Residue
Percentage of Total Suspended Solids= 100
Weight of Water Sample

0.0043
Percentage of Total Suspended Solids= 100 =0.00172
249.55
 DISCUSSION

Conductivity and pH

Conductivity of water allows measuring ionic constituents of all types of water

including surface waters, process waters in water supply and treatment plants. Pure water
is not a good conductor of electricity. Ordinary distilled water in equilibrium with carbon
dioxide of the air has a conductivity of about 10 x 10 -6 W-1*m-1 (20 dS/m). Because the
electrical current is transported by the ions in solution, the conductivity increases as the
concentration of ions increases. Thus, conductivity increases as water dissolved ionic
species.

Nevertheless, by referring to the Table 1.0, we can conclude that the conductivity is
the highest in the standard water and the least in the deionized water, while, tap water and
drinking water have almost similar conductivity values. This clearly gives us an idea that
the standard water solution contains a high amount of dissolved ionic species, while the
deionized water which has a value nearly 0 indicates that the water contains no ions.

Total dissolved solids (TDS) comprise inorganic salts (principally calcium,

magnesium, potassium, sodium, bicarbonates, chlorides, and sulfates) and some small
amounts of organic matter that are dissolved in water. The total dissolved solids
concentration can be related to the conductivity of the water, but the relationship is not a
constant. The relationship between total dissolved solids and conductivity is a function of
the type and nature of the dissolved cations and anions in the water and possible the nature
of any suspended materials. Nevertheless, based on table 1, we can see that the standard
solution has the highest TDS while the deionized water has the lowest Thats because
conductivity is a factor of TDS and standard solution has the highest conductivity and
deionized water has the lowest conductivity too.

Moving further on to the pH values of the sample, the standard solution has the lowest
pH value at about pH 5. This means that the standard solution is slightly acidic. The
remaining samples are also having pH values which less than 7 which suggests that they
are also slightly acidic. However, drinking water and top water are supposed to be slightly
alkaline while deionized water is supposed to show a reading value of pH 7. This can be
due to several reasons that cause the deviation of the readings. For example, the tip of the
pH sensors did not clean well with the deionized water before dipping into the water
sample. This action might cause contamination of the water sample thus giving wrong
values of pH. The previous group got the pH readings which are about 7 by using the same
pH sensors and water samples.

Total Solid And Total Suspended Solid

Gravimetric analysis is a relatively easy method to test for the quality of water in terms
of solid-containing speaking. By general, the solid content in the drinking water can be
categorised into total solids (TS), total suspended solids (TSS) and total dissolved solids
(TDS) and they are interrelated by the equation:

TS = TSS + TDS

TS, defined by Standard Methods and EPA, is the residue left in a vessel after evaporation
and drying of the sample in a 103-105C oven. TSS is particles that can be retained by
using a glass-fibre filter paper of pore size 45m in a filtration process and is usually made
up of decaying animal or plant matter, sewage and etc. On the other hand, TDS is solid that
is dissolved in the filtrate in the filtration process and is usually made up of inorganic
matter such as calcum, magnesium, carbonates and such. (Relationship Between TS, TSS
and TDS, 2009). In this experiment, the TS and TSS content is being experimented.

Total Solids TS

In this part of the experiment, the weight of the empty dish is measured. Then, the
water sample is poured into the dish and is allowed to evaporate at 105C in an oven for
one day. After the drying process, the weight of the empty dish with the leftover residue is
measured again. At this temperature, the organic would not be decomposed, and at the
same time the water molecules would not be fully evaporated as well. It is expected that
the weight of the dish after the drying would be larger than that empty one because the
solids in the water sample would be leftover in the dish after the water evaporated.

However, by referring to Table 2.0, the weight of the dish after drying is even lower
than the initial one. This cannot be happening because the solids in the water sample, if not
all, then at least a tiny fraction of them will be left in the dish. The only explanation to this
is that the dish is not dry and it might be containing water moisture at the beginning when
its weight is being measured. After the drying all the water molecules have been
evaporated, hence the weight becomes lighter.

Total Suspended Solids TSS

Referring to Table 3.0, similar results are observed in the TSS experiment as well
where the final weight of the filter paper was larger than the initial weight of the filter
paper. It can be argued that the filter papers were not placed in the desiccators when the
experiments are being conducted, therefore water moisture has already been attached onto
them when the initial weight of the filter papers are being measured.

Generally, the results of this experiment can be said to be inaccurate because the
weight of the dish and filter paper after the drying should not be lesser than the initial
weight after all. It can also be argued that not enough deionized water is used to wash the
filter paper after the filtration hence this leads to the inaccurate result. If all the data was
assumed to be correct by ignoring the negative sign, a table of the TS, TSS and TDS can be
obtained as below:

Standard Deionized
Tap Water Drinking Water
Solution Water
TS (mg/L) 360 432 764 1684
TSS (mg/L) 17.2 46.8 43.6 46.8
TDS (mg/L) 342.80 385.20 720.40 1637.20
Table 4.0: TS, TSS And TDS Relationship of All Water Sample.

This result shows that deionized water has the highest content of TDS where in fact,
deionized water being a solution where all the charged organic and inorganic matter are
removed, should not contain this high amount of TDS as there are only virus and bacteria
in the solution. The result is again proven to be irrelevant and not trustworthy. The value of
TDS is important because it is an indication of the quality of the drinking water. Below is
the category of the quality of drinking water.
 TDS (mg/L) Quality
< 300 Excellent
300 - 600 Good
600 - 900 Fair
900 -1200 Poor
> 1200 Unacceptable
Table 5.0: TDS and Relationship with Water Quality.

Precautionary Steps

Besides that, there are few precautions should be taken in the experiment. For the
conductivity test, we should switch on the conductivity meter for at least 30 minutes before
starting the experiment so that the instrument get stabilize. Next, during the experiment,
electrode must always dip in solution and do not expose to air. Other than that, the tip of
conductivity and pH sensors must be rinsed with deionized water before dip into another
type of water sample. For gravimetric analysis, it is important to make sure that weighing
balance set to zero before use. Lastly, we should ensure that the evaporating dish and filter
paper is completely dry before weight to ensure that the outcome of the result will not be
affected.
 CONCLUSION

After examining all 4 different types of sample, we can all agree that the standard
solution has the highest amount of suspended solids and dissolved solids, while the
deionized water contains the least suspended and dissolved solids. The tap water and
drinking water have some amounts of suspended and dissolved solids which are not as
harmful as the amounts they have in the standard solution. Besides that, the water
sample with the highest total solids content is deionized water. Based on the result,
deionized water is not suitable for water-drinking purpose. Drinking water and tap
water are acceptable, while for standard solution, doubts are being held because error
might occur due to the inaccurate result.

REFERENCE

1. Lenntech B.V. (2009) Water Conductivity. Retrieved 15 Feb 2017 from

http://www.lenntech.com/applications/ultrapure/conductivity/water-
conductivity.htm#ixzz4ZC4BEgvm

2. The Complete Guide of Water Chemistry& Treatment. (2009). Relationship Between

TS, TSS and TDS. Retrieved 15 Feb 2017 from http://www.water-
chemistry.in/2009/12/relationship-between-ts-tss-and-tds/

3. Quality, D. (1996). Total Dissolved Solids in Drinking water Background Document

for development of, 2. Retrieved 15 Feb 2017.