ESE2401 E1 Lab Report

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1 Abstract In this experiment, several water quality parameters of three water samples (A, B and C) were examined.

Table 1: Parameters investigated in the different parts of experiment

Part 1 Total Solids (TS) Total Volatile Solids (TVS) Total Fixed Solids (TFS)

Total Suspended Solids (TSS) Volatile Suspended Solids (VSS) Fixed Suspended Solids (FSS)

Part 2 Turbidity Conductivity pH

Part 3 Chloride

From the results obtained, it was deduced that A could be drain water, B could be pond water while C could be wastewater. 2 Aims & Theories of Experiment This experiment aims to deduce the possible sources of water samples A, B and C by investigating the solid contents, chemical and physical properties, and the chloride content of the three water samples. 2.1 Part 1: Solid Contents Parameters In this part of the experiment, TS, TVS, TFS, TSS, VSS, FSS of the water samples were determined using gravimetric analysis. The following experimental procedure was carried out to determine the amount of TS, TVS and TFS of the water samples.
103oC 30 min 500oC 20 min

Total solids left after Total fixed solids left evaporation to dryness W3 W2 Figure 1: Schematic diagram illustrating the procedure used to determine TS, TVS and TFS in the water samples. W1 represents the mass of the empty crucible while W2 and W3 represent the measured mass of solid residual. Crucible containing 25 mL of sample

Empty crucible W1

The following experimental procedure was carried out to determine the amount of TSS, VSS and FSS of the water samples.

1. 2.

Filtration Dry at 103oC for 1h

500oC 20 min

Fixed suspended Suspended solids on solids on filter disk filter disk W3 W2 Figure 2: Schematic diagram illustrating the procedure used to determine TSS, VSS and FSS. W2 and W3 represent the measured mass of solid residual. 25 mL of sample Filter apparatus with glass fibre disk

In the above procedures, a heating temperature higher than 100oC (e.g. 103oC) was used to completely drive off the water content of the samples because the samples, which contained impurities, would have boiling points higher than that of pure water i.e. 100oC. The samples were further heated at 500oC to ensure all organics (volatile solids) present were combusted, thereby allowing us to obtain total fixed solids.

2.2 Part 2: Chemical and Physical Parameters This part of the experiment was carried out to study turbidity, conductivity and pH of the three water samples. Turbidity, conductivity and pH measurements were made using a turbidimeter, conductivity meter and pH meter. 2.3 Part 3: Determination of Chloride Content Using Mohr Method To determine the concentration of Cl- present in the water samples, the water samples are titrated against AgNO3(aq) with potassium chromate as the indicator. AgNO3(aq) + Cl-(aq) AgCl(s) + NO3-(aq) The above equation shows that 1 mole of AgNO3 reacts with 1 mole of Cl-, hence the number of moles of AgNO3 is equivalent to number of moles of Cl- present in the water sample. 3 Experimental Results 3.1 Part 1A: Determination of TS, TVS and TFS From the equations
TS W2 W3 W3 W1 W2 W1 , TVS , TFS Volume of sample Volume of sample Volume of sample

where W1: mass of empty crucible W2: mass of crucible with sample after evaporation to dryness at 103oC for 30 min W3: mass of crucible with sample after heating in furnace at 500oC for 20 min, the following table of values of TS, TVS and TFS is obtained:
Table 2: Tabulated values of TS, TVS and TFS of the water samples

Water Sample A B C

Volume of sample / mL 25 25 25

W1 / g 36.3573 33.3934 35.9834

W2 / g 36.3604 33.3992 36.0052

W3 / g 36.3590 33.0052 36.0007

TS / mg L1

TVS / mg L1

TFS / mg L1

124.0 232.0 872.0

56.0 80.0 180.0

68.0 152.0 692.0

3.2

Part 1B: Determination of TSS, VSS, FSS and TDS


Trial I W2 / g 29.7232 30.6936 31.2715 Trial II W2 / g 29.8419 30.3722 35.3878

Table 3: Tabulated values of W1, W2 and W3 of the water samples Water sample A B C Volume of sample / mL 500 300 50 W1 / g 29.7217 30.6870 31.2664 W3 / g 29.7231 30.6922 31.2684 W1 / g 29.8404 30.3675 35.3824 W3 / g 29.8418 30.3708 35.3846

From the equations


TS = TSS + TDS, TSS

W2 W3 W2 W1 W3 W1 , VSS , FSS Volume of sample Volume of sample Volume of sample

where W1: mass of fibre disk and container W2: mass of fibre disk, container and sample, after evaporation to dryness at 103oC for 30 min W3: mass of fibre disk, container and sample, after heating in furnace at 500oC for 20 minutes, the following table of values of TSS, VSS and FSS and TDS is obtained.
Table 4: Tabulated values of TSS, VSS, FSS and TDS of the water samples Sample Volume of <W1> / g <W2> / g <W3> / g TSS / mg VSS / FSS / TDS/

sample / mL A B C 500 300 50 29.78105 30.52725 33.32440 29.78255 30.53290 33.32965 29.78245 30.53150 33.32650

L-1 3.00 18.80 105.00

mg L-1 0.20 4.70 63.00

mg L-1 2.80 14.20 42.00

mg L-1 121.0 231.2 767.0

3.3

Part 2: Chemical & Physical Parameters of the Water Samples


pH 7.39 8.23 5.59

Table 5: Tabulated values of Turbidity, conductivity and pH of the water samples Water sample Turbidity / NTU Conductivity / mS cm-1 A 1.29 1.352 B 3.41 2.085 C 16.7 6.711

3.4 Part 3: Determination of Chloride Content using Mohr Method Standard solution used: NNaCl = 0.0141eq/L
A Titration 1 Initial burette reading/cm3 Final burette reading/cm3 Volume of AgNO3 used/cm3 <Volume of AgNO3 used>/cm3 0.60 3.90 Titration 2 3.90 7.20 Titration 1 23.00 26.15 B Titration 2 26.15 29.25 Titration 1 25.00 27.60 C* Titration 2 27.60 30.10 Standard Titration 1 1.20 22.00 Blank Titration 1 22.00 23.00

3.30

3.30

3.15

3.10

2.60

2.50

20.80

1.00

M1=3.30

M1=3.13

M1=2.55

20.80

M2=1.00

*Sample C is diluted by a factor of 10. NAgNO3 =


Volume of NaCl used (in mL) N NaCl 20 mL 0.0141eqL-1 = = 0.013558 eq/L Volume of AgNO 3 used (in mL) 20.80 mL

Trace chloride content is found to be present in the blank sample (100 mL of deionised water). Chloride content could have contaminated the bottle of deionised water from which the blank sample was taken when the bottle of deionised water was used extensively to rinse the experimental apparatus and to dilute the water samples to 100 mL. To determine the actual [Cl-] of the water samples, this trace [Cl-] must be taken into account. Hence the equation used to calculate the [Cl-] of each water sample is:
[Cl - ] (in mg/L) dilution factor (M1 M 2 ) 35.45 1000 N AgNO3 Volume of sample (in mL)

Example: For water sample C, [Cl-] = 10


(2.55 1.00) 35.45 1000 0.013558 74.5 mg/L 100
A 11.1 B 10.2 C 74.5

Table 6: Tabulated values of [Cl-] of the water samples

Water Sample [Cl-]/mgL-1

Analysis and Discussion

Table 7: Measurements of various water quality parameters of the water samples Water Sample Water sample with A TS / mgL-1 TVS / mgL-1 TFS / mgL-1 TSS / mgL-1 TDS / mgL-1 VSS / mgL-1 FSS / mgL-1 Conductivity / mS cm-1 pH Turbidity / NTU [Cl-] / mgL-1 Possible source 124.0 56.0 68.0 3.00 121.00 0.20 2.80 1.352 7.39 (neutral) 1.29 11.05 Open drain B 232.0 80.0 152.0 18.80 231.20 4.70 14.20 2.085 8.23 (alkaline) 3.41 10.21 Pond C 872.0 180.0 692.0 105.00 767.00 63.00 42.00 6.711 5.59 (acidic) 16.70 74.50 Sewage Highest value C C C C C C C C B C C Lowest value A A A A A A A A C A B

Water sample A could be taken from an open drain in the residential areas because it the lowest amount of TS (124.0 mg/L) and it is generally clear (turbidity of 1.29 NTU). The solids present could be due to the soil and solid particles deposited by surface runoff. It also has a pH value of 7.39 which is close to the pH of tap water (pH=7.6) [1]. The amount of chloride content in water sample A is moderately low and it may have originated from some of the household chemicals e.g. bleach. Water sample B could be taken from a pond. The water sample is slightly alkaline (pH=8.23) and this can be explained by the possibility of the pond being situated near an alkaline fertilizer source. The water sample is generally clear (turbidity of 3.41 NTU) and algae and suspended silt particles can account for the moderate TVS (80.0 mg/L) and TFS (152.0 mg/L) present in it. It has the lowest chloride concentration (10.21 mg/L) which probably originated from chlorinated pesticides. Water sample C could be wastewater because it contains a high amount of solids (TS = 872.0 mg/L) and is murky (high turbidity value of 16.70 NTU). Its pH level is moderately low (pH 5.59) while its [Cl-] is high (74.50 mg/L) and this could be a result of acidic wastewater discharge from homes (human excretion) or industries (muriatic acid). From the results, it is observed that there is a direct relationship between turbidity and the gravimetric results. Water sample A has the highest TSS (105.00 mg/L) and turbidity values (16.70 NTU) while water sample C has the lowest TSS (3.00 mg/L) and turbidity values (1.29 NTU). A higher TSS value corresponds to a higher turbidity because having more suspended solids in the sample would result in more light being scattered in the turbidimeter. A higher NTU value will thus be reflected on the turbidimeter. It is also observed that conductivity and TFS share a direct relationship. Water sample A, which has the highest TFS value, has the highest conductivity value while water sample C, which has the lowest TFS value, has the lowest conductivity value. A high TFS value corresponds to larger conductivity because TDS makes up a large portion of TFS (the dissolved solids in the water sample crystalise instead of combust to become part of the TFS measured when the sample is heated). Since the dissolution of solids may result in the formation of ions which help to carry electric current, a larger TFS value will correspond to larger conductivity.

Precautions

The precautions that were taken to ensure the accuracy of results are as follows: 1) The experimental procedure for the measurement of TSS/ VSS/FSS/TDS was repeated twice and the average results were taken to ensure more accurate results. 2) The burette was rinsed with AgNO3 while the pipette was rinsed with the water sample to be tested before the titration process. This was done to prevent dilution of the reagents. 3) The glass fibre disks were weighed one at a time because they absorb atmospheric moisture very quickly and this would result in erroneous values of W1. 4) The samples in the sample tubes were well-mixed and the surface of the sample tubes and the reference standard tube were wiped clean with lens tissue before they were placed into the turbidimeter. This was done because residues on the surface of the tubes would add on to the intensity of scattered light, resulting in higher NTU value. 5) For thick samples, it might be difficult to remove the air bubbles that form in the sample tubes during the pipetting process. Hence, the pipettin process was carried out slowly and at an angle to minimize the formation of air bubbles. 6) The pH probes were calibrated with standard buffer solutions before they were used to test the water samples.

Possible Sources of Errors and Improvements

The possible sources of errors and improvements are as follows: 1) 30 minutes of drying at 103oC during the gravimetric analysis may not be sufficiently long to completely dry the sample. This would cause the recorded TS value to be higher than the actual TS value. This error could be avoided by extending the drying duration to 1h. 2) The percentage error in the results obtained would be large since the volume of sample used in many parts of the experiment is a small value of 25 mL. This error can be minimized by raising the volume of samples used, and repeating the experiment several times to obtain average results. 3) The fibre disk is still able to absorb moisture from the atmosphere and our fingers despite it being weighed one at a time. This will result in higher W1 values and lower-than-actual TSS values. This error can be minimized by wearing gloves and conducting the weighing process in a controlled environment with lower humidity (e.g. air-conditioned room). 4) Measuring the chloride content in the water samples using the Mohr method leaves out the chlorine present in organic substances that do not dissociate within a short period of time. Persistent substances such as Polychlorinated Biphenyls (PCBs) which may be present in the water samples take a long time to degrade and form Cl-. This error can be overcome by conducting in tandem tests that determine the presence of such persistent chlorinated substances.

Conclusion

This report has discussed the tests that can be conducted to assess selected water quality parameters. Through these tests, it was possible to deduce the sources which the given water samples were taken from. Water samples A, B and C is believed to be taken from an open drain, pond and sewage system respectively.

References

[1] Public Utilities Board (PUB). (n.d.). Water Treatment. http://www.pub.gov.sg/general/pages/watertreatment.aspx (accessed February 26, 2013)

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