TOTAL SOLID DETERMINATION 1.

0 OBJECTIVE

To provide and strengthen knowledge, skill, and 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 : a) Apply knowledge in solid determination b) Analyze the laboratory result and differentiate between suspended solid and dissolve solid. c) Identify problem and use their generic skill to solve problems. d) Develop their ability to work in group. 3.0 THEORY 3.1 Total Suspended Solids (TSS)

Total suspended solids is a water quality measurement usually abbreviated TSS. It is listed as a conventional pollutant in the U.S. Clean Water Act. This parameter was at one time called non-filterable residue (NFR), a term that refers to the identical measurement: the dry-weight of particles trapped by a filter, typically of a specified pore size. However, the term "non-filterable" suffered from an odd (for science) condition of usage: in some circles (Oceanography, for example) "filterable" meant the material retained on a filter, so non-filterable would be the water and particulates that passed through the filter. In other disciplines (Chemistry and Microbiology for examples) and dictionary definitions, "filterable" means just the opposite: the material passed by a filter, usually called "Total dissolved solids" or TDS. Thus in chemistry the non-filterable solids are the retained material called the residue. TSS of a water sample is determined by pouring a carefully measured volume of water (typically one litre; but less if the particulate density is high, or as much as two or

TOTAL SOLID DETERMINATION three litres for very clean water) through a pre-weighed filter of a specified pore size, then weighing the filter again after drying to remove all water. Filters for TSS measurements are typically composed of glass fibres.[1] The gain in weight is a dry weight measure of the particulates present in the water sample expressed in units derived or calculated from the volume of water filtered (typically milligrams per litre or mg/l). Recognise that if the water contains an appreciable amount of dissolved substances (as certainly would be the case when measuring TSS in seawater), these will add to the weight of the filter as it is dried. Therefore it is necessary to "wash" the filter and sample with deionized water after filtering the sample and before drying the filter. Failure to add this step is a fairly common mistake made by inexperienced laboratory technicians working with sea water samples, and will completely invalidate the results as the weight of salts left on the filter during drying can easily exceed that of the suspended particulate matter. Although turbidity purports to measure approximately the same water quality property as TSS, the latter is more useful because it provides an actual weight of the particulate material present in the sample. In water quality monitoring situations, a series of more labor intensive TSS measurements will be paired with relatively quick and easy turbidity measurements to develop a site-specific correlation. Once satisfactorily established, the correlation can be used to estimate TSS from more frequently made turbidity measurements, saving time and effort. Because turbidity readings are somewhat dependent on particle size, shape, and color, this approach requires calculating a correlation equation for each location. Further, situations or conditions that tend to suspend larger particles through water motion (e.g., increase in a stream current or wave action) can produce higher values of TSS not necessarily accompanied by a corresponding increase in turbidity. This is because particles above a certain size (essentially anything larger than silt) are not measured by a bench turbidity meter (they settle out before the reading is taken), but contribute substantially to the TSS value.

TOTAL SOLID DETERMINATION 3.2 Total Dissolved Solids (TDS)

Total Dissolved Solids (often abbreviated TDS) is a measure of the combined content of all inorganic and organic substances contained in a liquid in: molecular, ionized or micro-granular (colloidal sol) suspended form. Generally the operational definition is that the solids must be small enough to survive filtration through a sieve the size of two micrometer. Total dissolved solids are normally discussed only for freshwater systems, as salinity comprises some of the ions constituting the definition of TDS. The principal application of TDS is in the study of water quality for streams, rivers andlakes, although TDS is not generally considered a primary pollutant (e.g. it is not deemed to be associated with health effects) it is used as an indication of aesthetic characteristics of drinking water and as an aggregate indicator of the presence of a broad array of chemical contaminants. Primary sources for TDS in receiving waters are agricultural and residential runoff, leaching of soil contamination and point source water pollutiondischarge from industrial or sewage treatment plants. The most common chemical constituents are calcium, phosphates, nitrates, sodium, potassiumand chloride, which are found in nutrient runoff, general stormwater runoff and runoff from snowy climates where road de-icing salts are applied. The chemicals may be cations, anions, molecules or agglomerations on the order of one thousand or fewer molecules, so long as a soluble micro-granule is formed. More exotic and harmful elements of TDS are pesticides arising from surface runoff. Certain naturally occurring total dissolved solids arise from the weathering and dissolution of rocks and soils. The United States has established a secondary water quality standard of 500 mg/l to provide for palatability of drinking water. Total dissolved solids are differentiated from total suspended solids (TSS), in that the latter cannot pass through a sieve of two micrometers and yet are indefinitely suspended in solution. The term "settleable solids" refers to material of any size that will not remain suspended or dissolved in a holding tank not subject to motion, and excludes both TDS and TSS.[1] Settleable solids may include larger particulate matter or insoluble molecules.

TOTAL SOLID DETERMINATION 3.3 Total Dissolved Solids (TDS) Total Dissolved Solids (often abbreviated TDS) is a measure of the combined content of all inorganic and organic substances contained in a liquid in: molecular, ionized or micro-granular (colloidal sol) suspended form. Generally the operational definition is that the solids must be small enough to survive filtration through a sieve the size of two micrometer. Total dissolved solids are normally discussed only for freshwater systems, as salinity comprises some of the ions constituting the definition of TDS. The principal application of TDS is in the study of water quality for streams, rivers andlakes, although TDS is not generally considered a primary pollutant (e.g. it is not deemed to be associated with health effects) it is used as an indication of aesthetic characteristics of drinking water and as an aggregate indicator of the presence of a broad array of chemical contaminants. Primary sources for TDS in receiving waters are agricultural and residential runoff, leaching of soil contamination and point source water pollutiondischarge from industrial or sewage treatment plants. The most common chemical constituents are calcium, phosphates, nitrates, sodium, potassiumand chloride, which are found in nutrient runoff, general stormwater runoff and runoff from snowy climates where road de-icing salts are applied. The chemicals may be cations, anions, molecules or agglomerations on the order of one thousand or fewer molecules, so long as a soluble micro-granule is formed. More exotic and harmful elements of TDS are pesticides arising from surface runoff. Certain naturally occurring total dissolved solids arise from the weathering and dissolution of rocks and soils. The United States has established a secondary water quality standard of 500 mg/l to provide for palatability of drinking water.

TOTAL SOLID DETERMINATION Total dissolved solids are differentiated from total suspended solids (TSS), in that the latter cannot pass through a sieve of two micrometers and yet are indefinitely suspended in solution. The term "settleable solids" refers to material of any size that will not remain suspended or dissolved in a holding tank not subject to motion, and excludes both TDS and TSS.[1] Settleable solids may include larger particulate matter or insoluble molecules.

* By convention, nominal filter pore size is 0.45 m ** Total solids determined by evaporation (103-105 C) of whole sample, without
o

filtration (Total) Volatile solids = f + h Fixed or Non-volatile total solids = g + i

TOTAL SOLID DETERMINATION 4.0 DIAGRAM Imhoff cone Microwave (at 103 c105c) Total solids (TS)

Settleable solids

Samples

Microwave (at 103 c- 105c)

Fibre glass filter ( < 2.0 m)

Microwave (at 180 c- 2c)

Suspended solids (ss)

Dissolved solids (DS)

Muffle furnace ( at 500 c -50 c)

Muffle furnace ( at 500 c -50 c)

Volatile suspended solids (VSS)

Fixed suspended solids (FSS)

Volatile dissolved solids (VDS)

Fixed dissolved solids (FDS)

Total Volatile solids (TVS) = VSS + VDS

Total Fixed solids (TFS) = FSS + FDS

Total solids (TS)

TOTAL SOLID DETERMINATION 5.0 EQUIPMENTS AND MATERIALS 1. Sets of evaporating dishes: dishes of 100 ml capacity made of porcelain, platinum or high silica glass and apparatus.

2. Muffle furnace for operating at 500 0C + 50 0C

TOTAL SOLID DETERMINATION 3. Desicator

4. Vacuum pump

5. 10 ml pipette

TOTAL SOLID DETERMINATION 6. Oven operating at the temperature 180 0C

7. Analytical balance

TOTAL SOLID DETERMINATION 6.0 PROCEDURE

A. Total Solid Test i. ii. iii. iv. v. vi. vii. viii. Weight of empty evaporation dish is taken. The sample is poured into the dish The sample on evaporating dish is weighted The sample is placed in the incubator for drying process at 180C for 30 minutes. After 30 minutes the sample to removed from incubator and place in the desicator to cool up for 10 minutes. The sample is weight. The sample is put in the furnace for drying process at 300C After 15 minutes, sample size is removed, the sample place in the desicator again for 10 minutes and after that the weight is taken.

B. Total Solid Suspended Solid Test i. Put the filter pad in defecator. The purpose is to drying or inquiring, cooling, desiccating and weighing until the weight of the filter pad change less then 4% or 0.5 mg from the pervious weight. ii. iii. After remove from the desiccators, each filter is weighed and the weight is logged on the beach sheet in the appropriated section. Use tweeters to put the filter pad at the top of the vacuum(stream both).

10

TOTAL SOLID DETERMINATION iv. v. vi. vii. viii. ix. Put the filter pad at the aluminum pad. Weight the filter pad and the aluminum pad Put the sample at the steel tray. Leave the filter pad for a while Weight again the filter pad and aluminum pad again. Put the filter pad and aluminum in the furnace for 15 minute. Remove the filter pad and aluminum and weight again to record data.

C. Total Dissolved Solid Test. i. ii. iii. iv. get the weight. v. at 300C. vi. Remove the sample water and the evaporating dishes from furnace. Put it in the dictator for 10 minutes to balance the temperature and weight. Put the sample water and evaporating dishes in the furnace for 15 minutes Measure the volume of the sample water. Use 5ml for each sample water in the evaporation dishes. Weight the sample water record. Put the sample water and evaporating dished in the oven for 30 minutes at 180C and cool the sample water. Remove from desiccators, each sample water and the evaporating dishes is

11

TOTAL SOLID DETERMINATION

7.0

RESULT AND CALCULATION

TOTAL SOLID Sample A 1 2 3 Volume of sample (ml) Weight of evaporating dish (g) Weight of evaporating dish + sample Weight of sample (g) = (3 2) Weight of evaporating dish + sample after drying process at 103oC - 105oC Weight of solid (g) = (5 2) Weight of evaporating dish ( g ) + solid after drying process at 103c105c Weight of volatile solid ( g ) Total Solid (TS) (mg/L) = [(5 2)g x 1000] / 5 mL Percentage of solid in sample (%) = (6 / 4 ) x 100 5 46.3968 52.5100

6.1132

48.1830

1.7862

7 8 9

46.3924 1.7906 357.24

10

29.2187 358.12 x 103 29.29

11 Total volatile solid ( VS ) ( mg/L ) 12 Percentage of volatile solid ( % )

12

TOTAL SOLID DETERMINATION

TOTAL SUSPENDED SOLID

13

TOTAL SOLID DETERMINATION

1 2 3 4 5 6 7 8

Volume of Sample (ml) Weight of filter paper (g) Weight of filter paper + solid after drying at 103oC - 105oC or at 180oC Weight of solid (g) Weight of filter + solid after drying at 500oC 50oC (g) Weight of volatile solid (g) Total Suspended Solid (SS) (mg/L) Percentage of Volatile Suspended Solid (VSS) %

Sample A 5 0.0930 11.8649 11.7719 0.0866 2.3560 2.3544 235.6

14

TOTAL SOLID DETERMINATION

TOTAL DISSOLVED SOLID

15

TOTAL SOLID DETERMINATION

1 2

Volume of sample (ml) Weight of evaporating dish (g) Weight of evaporating dish + sample (g) Weight of sample (g) = (3 2) Weight of evaporating dish + o sample after drying at 180 C (g) Weight of Solid (g) = (5 2) Total Dissolve Solid (mg/L) = [(5 2) x 1000] / 5 (TDS)

Sample A 5 47.1346

52.3292

5.1946

47.1516

0.0170

3.400

Weight of evaporating dish + solid after drying at 500oC 50oC (g) Weight of dissolved solid (g) = (8 2) Total dissolved Solid (SS) (mg/L) Percentage of Volatile dissolved Solid (VSS) % = (10 / 7) x 100

47.1348

0.0002

10 = [(8 2) x 1000] / 100

0.002

11

0.0588

16

TOTAL SOLID DETERMINATION

CALCULATION FOR TOTAL SOLID 1) weight of sample Sample A : = (3) (2) = 52.5100 46.3968 = 6.1132 g

2) Weight of dissolved solid Sample A : = (5) (2)

17

TOTAL SOLID DETERMINATION = 48.1830 46.3968 = 1.7862 g 3) Weight of volatile solid Sample A : = (5) (7) = 48.1830 46.3924 = 1.7906 g

4) Total solid Sample A : = = = = (6) 103 103 Volume of sample Weight of solid x 103 103 Volume of sample (1.7862 x 103 x 103 ) / 5 ml 357.24 mg/L

5) Percentage of solid in sample Sample A : = [(6) / weight of sample ] x 100% = [ (1.7862) / 6.1132] x 100% = 29.22 %

6) Total volatile solid Sample A : = [ (8) / volume of sample] x 103 x 103 = [ (1.7906) / 5 ] x 103 x 103 = 358.12 x 103 mg/L

7) Percentage of volatile solid Sample A : = [(8) / weight of sample] x 100% = [(1.7906) / 6.1132 ] x 100 % = 29.29 %

CALCULATION FOR TOTAL SUSPENDED SOLID 1) Weight of Filter Paper Sample A : Evaporating Dish + Filter Paper = 18.3669 g Evaporating Dish = 18.2739 g So, weight of filter paper = 18.3669 18.2739= 0.0930 g

18

TOTAL SOLID DETERMINATION 2) Weight of filter paper + solid after drying at 103oC - 105oC or at 180oC Sample A: Weight of Evaporating Dish = 18.2739 g Weight of Evaporating Dish + Filter Paper + Solid after drying = 30.1388 g So, Weight of filter paper + solid after drying at at 180oC = 30.1388 18.2739 = 11.8649g 3) Weight of Solid Sample A: Weight of Evaporating Dish = 18.2739 g Weight of Evaporating Dish + Filter Paper + Solid = 30.1388 g Weight of Filter Paper = 0.0930 g So, Weight of Solid = 30.1388 18.2739 0.0930 = 11.7719 g 4) Weight of filter + solid after drying at 500oC 50oC (g) Sample A: Weight of Evaporating Dish = 18.2739 g Weight of Evaporating Dish + Filter Paper + Solid after drying = 18.3605 g So, Weight of filter + solid after drying at 500oC 50oC (g) = 18.3605 18.2739 = 0.0866 g 5) Weight of volatile solid (g) [(Weight of residue + dish or filter before ignition) (Weight of residue + dish or filter after ignition)] x 1000 / 20 Sample A: Weight of residue + dish or filter before ignition Weight of residue + dish or filter after ignition So, Weight of volatile solid = 11.8649 0.0866 = 11.8649 g = 0.0866 g = 0.01178mg x 1000 / 5 = 2.3560 g

6) Total Suspended Solid (SS)

19

TOTAL SOLID DETERMINATION [(Weight of filter + dried residue) (Weight filter)] x 1000 / 5 Sample A: Weight of filter + dried residue = 11.8649 g Weight filter = 0.0930 g So, Total Suspended Solid = 11.8649 0.0930 = 11.7719g x 1000 /5 = 2.3544 mg/L 7) Percentage of Volatile Suspended Solid (VSS) % Sample A: Weight of volatile solid x 100 = 2.356 x 100 = 235.6

CALCULATION FOR TOTAL DISSOLVED SOLID 1) weight of sample Sample A : = (3) (2) = 52.3292 47.1346 = 5.1946 g

2) Weight of dissolved solid

20

TOTAL SOLID DETERMINATION Sample A : = (5) (2) = 47.1516 47.1346 = 0.017 g

3) Total dissolved solid Sample A : = = = = (6) 103 103 Volume of sample Weight of solid x 103 103 Volume of sample (0.017 x 103 x 103 ) / 5 ml 3.4000 mg/L

4) Weight of dissolved solid Sample A : = [(8) (2)] = 47.1348 47.1346 = 0.0002 g

5) Total dissolved solid Sample A : = [ ( 8 2 ) x 1000 } / 100 = [ 0.0002 x 1000 ] / 100 = 0.002 mg/L

6) Percentage of volatile dissolved solid Sample A : = [ (10) / (7) ] x 100% = [ (0.002) / (3.4)] x 100% = 0.0588 %

8.0

DISCUSSION

1. Distinguish between suspended solid and dissolve solid.

Total suspended solids are retained on a filter and weighed while total dissolved solids are solids dissolved in the solution that passes through the filter.

21

TOTAL SOLID DETERMINATION A suspended solid refers to small solid particles which remain in suspension in water as a colloid or due to the motion of the water. It is used as one indicator of water quality. The dissolved is a very small pieces of organic and inorganic material contained in water. Excessive amounts make water unfit to drink or limit its use in industrial processes.

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

The possible causes of high levels of total suspended solids in could be:

a) Domestic Wastewater has low TSS(around 400mg/L) because this domestic wastewater is discharged from our household usages: we are not using more solid from our house.

b) Industrial Wastewater- has high TSS(around few 1000mg/L) because, the clean water is used for various purposes in various industries. Not all industry discharge wastewater with high TSS but some industries like tannery industries, food industry discharge wastewater weight high TSS. Here the causes of high TSS are animal hair, preservatives and coloring agent.

22

TOTAL SOLID DETERMINATION 3. The suspended solid for a wastewater sample was 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 1050C = 1.5538 g

Total Suspended Solid (TSS), mg/L =____(A B) x 106_____ Volume of Sample (mL)

Where : A : Residue on glass fibre filter after drying at 105oC (g) B : Tare mass of glass fibre filter (g) 175 mg/L = (1. 5538- 1. 5413) x 106 Volume of sample (mL) Volume of sample (mL) = (1.5538- 1. 5413) x 106 175 mg/L = 71.4286 mL

23

TOTAL SOLID DETERMINATION

9.0

CONCLUSION

From the experiment, we able to charaterise a water sample with respect to its solid content. Total solid in water are due to suspended matter and dissolved matter. These are determined separately and then added together. The suspended solids are found by filtering the water through a fine filter. The material retained on the filter is weighed. This gives the dissolved matter. Total solids includes both total suspended solids and total dissolved solids. The average value of total solid (TS) is 357.24 mg/L, total suspended solid (TSS) is 2.3544 mg/L, total dissolved solid (TDS) is 3.4 mg/L. Interim National River Water Quality Standard for Malaysia(INWQS) can also be used to determine the quality of water in stream. It is based on parameter measured then, compared the data with the INQWS. Total dissolved solids are includes all solids present in a water sample filtered . It determined by evaporating a known volume of the filtrate sample in a 180 oC oven. Total suspended solids is includes all solids present in a sample that remain on filter. Determined by filtering a known volume of sample and placing the filter and filter container in a 180 oC oven to evaporate the water. Fixed solids is solids that remain after firing a sample in a 300 oC muffle furnace. It can be performed on total, dissolved, or suspended samples to determine total fixed solids, fixed dissolved solids, or fixed suspended solids. Volatile solids is solids that removed by firing a sample in a 300 oC

24

TOTAL SOLID DETERMINATION muffle furnace. It can be performed on total, dissolved, or suspended samples to

determine total volatile solids, volatile dissolved solids, or volatile suspended solids. The result that we have obtained do not have proper standard, it is because we had to use a temperature of 300 oC for muffle furnace. From this experiment, we can identify that temperature plays an important role to obtain accurate results.

10.0

REFERENCES

Metcalf & Eddy (2003) Wastewater Engineering, Treatment and Reuse, 4th ed. McGraw-Hill, New York.

Mackenzie L. Davis & David A. Cornwell (2008) Introduction to Environmental Engineering, 4th ed. McGraw-Hill, New York.

Hans Hermann Rump (1999). Laboratary Manual for the examination of Water, Wastewater and Soil. 3rd ed.Wiley-Vch, Weinheim.

General Information on Solids. 15th January 2011 retrieved from http://bcn.boulder.co.us/basin/data/NEW/info/TSS.html

Total dissolved solids. 16th January 2011 retrieved from http://en.wikipedia.org/wiki/Total_dissolved_solids

Standard Methods Committee, 1997 http://www.norweco.com/html/lab/test_methods/2540dfp.htm

25

TOTAL SOLID DETERMINATION

26