TOTAL SOLID DETERMINATION

1.0OBJECTIVETo provide and strengthen knowledge, skill, and understanding in solid determination and enable to relate theories taught to the practices in laboratory.

2.0LEARNING OUTCOMEAt 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

3.1Total Suspended Solids (TSS)Total suspended solidsis awater qualitymeasurement usually abbreviatedTSS. It is listed as aconventional pollutantin 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 afilter, 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 (ChemistryandMicrobiologyfor examples) and dictionary definitions, "filterable" means just the opposite: the material passed by a filter, usually called "Total dissolved solids" orTDS. Thus in chemistry the non-filterable solids are the retained material called theresidue.TSS of a water sample is determined by pouring a carefully measured volume of water (typically one liter; but less if the particulate density is high, or as much as two or three liters 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 ofglass fibers.[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 liter or mg/l).

Recognize that if the water contains an appreciable amount of dissolved substances (as certainly would be the case when measuring TSS inseawater), these will add to the weight of the filter as it is dried. Therefore it is necessary to "wash" the filter and sample withdeionized waterafter 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.

Althoughturbiditypurports 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 streamcurrentor 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.

3.2Total Dissolved Solids (TDS)Total Dissolved Solids(often abbreviatedTDS) is a measure of the combined content of allinorganicandorganicsubstances 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 ofwater qualityforstreams,riversand lakes, 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 ofdrinking waterand as an aggregate indicator of the presence of a broad array of chemical contaminants.

Primary sources for TDS in receiving waters areagriculturaland residential runoff, leaching ofsoil contaminationandpoint sourcepollution discharge from industrial orsewage treatmentplants. The most common chemical constituents arecalcium,phosphates,nitrates,sodium,potassiumandchloride, which are found innutrientrunoff, generalstorm waterrunoff and runoff from snowy climates where roadde-icingsalts are applied. The chemicals may beactions,anions,moleculesor agglomerations on the order of one thousand or fewer molecules, so long as a soluble micro-granuleis formed. More exotic and harmful elements of TDS arepesticidesarising fromsurface runoff. Certain naturally occurring total dissolved solids arise from the weathering and dissolution of rocks and soils. TheUnited Stateshas established a secondary water quality standard of 500mg/l to provide for palatability of drinking water.

Total dissolved solids are differentiated fromtotal suspended solids(TSS), in that the latter cannot pass through a sieve of two micrometers and yet are indefinitely suspended in solution. The term "settle able 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]Settle able solids may include larger particulate matter or insoluble molecules.3.3Total Dissolved Solids (TDS)Total Dissolved Solids(often abbreviatedTDS) is a measure of the combined content of allinorganicandorganicsubstances 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 ofwater qualityforstreams,riversand lakes, 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 ofdrinking waterand as an aggregate indicator of the presence of a broad array of chemical contaminants.

Primary sources for TDS in receiving waters areagriculturaland residential runoff, leaching ofsoil contaminationandpoint sourcepollution discharge from industrial orsewage treatmentplants. The most common chemical constituents arecalcium,phosphates,nitrates,sodium,potassiumandchloride, which are found innutrientrunoff, generalstorm waterrunoff and runoff from snowy climates where roadde-icingsalts are applied. The chemicals may beactions,anions,moleculesor agglomerations on the order of one thousand or fewer molecules, so long as a soluble micro-granuleis formed. More exotic and harmful elements of TDS arepesticidesarising fromsurface runoff. Certain naturally occurring total dissolved solids arise from the weathering and dissolution of rocks and soils. TheUnited Stateshas established a secondary water quality standard of 500mg/l to provide for palatability of drinking water.Total dissolved solids are differentiated fromtotal suspended solids(TSS), in that the latter cannot pass through a sieve of two micrometers and yet are indefinitely suspended in solution. The term "settle able 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]Settle able solids may include larger particulate matter or insoluble molecules.

* By convention, nominal filter pore size is 0.45 m

** Total solids determined by evaporation (103-105oC) of whole sample, without filtration

(Total) Volatile solids = f + h

Fixed or Non-volatile total solids = g + i4.0DIAGRAM

5.0EQUIPMENTS 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

3. Desicator

4. Vacuum pump

5. Wid-bore pipette

6. Oven operating at the temperature 180 0C

7. Analytical balance

6.0PROCEDUREA. Total Solid Test

i. Weight of empty evaporation dish is taken.

ii. The sample is poured into the dish

iii. The sample on evaporating dish is weighted

iv. The sample is placed in the incubator for drying process at 180C for 30 minutes.

v. After 30 minutes the sample to remove from incubator and place in the desicator to cool up for 10 minutes.

vi. The sample is weight.

vii. The sample is put in the furnace for drying process at 300C

viii. 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 than 4% or 0.5 mg from the previous weight.

ii. After remove from the desiccators, each filter is weighed and the weight is logged on the beach sheet in the appropriated section.

iii. Use tweeters to put the filter pad at the top of the vacuum (stream both).

iv. Put the filter pad at the aluminum pad.

v. Weight the filter pad and the aluminum pad

vi. Put the sample at the steel tray. Leave the filter pad for a while

vii. Weight again the filter pad and aluminum pad again.

viii. Put the filter pad and aluminum in the furnace for 15 minute.

ix. Remove the filter pad and aluminum and weight again to record data.

C. Total Dissolved Solid Test.

i. Measure the volume of the sample water. Use 5ml for each sample water in the evaporation dishes.

ii. Weight the sample water record.

iii. Put the sample water and evaporating dished in the oven for 30 minutes at 180C and cool the sample water.

iv. Remove from desiccators, each sample water and the evaporating dishes is get the weight.

v. Put the sample water and evaporating dishes in the furnace for 15 minutes 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.

7.0 RESULT AND CALCULATIONTOTAL SOLID

Sample ASample B

1Volume of sample (ml)

510

2Weight of evaporating dish (g)

21.3920.2

3Weight of evaporating dish + sample

27.5630.2

4Weight of sample (g)= (3 2)

6.1710

5Weight of evaporating dish + sample after drying process at 103oC - 105oC

43.8640.9

6Weight of solid (g)= (5 2)

22.4720.7

7Weight of evaporating dish ( g ) + solid after drying process at 103c-105c46.3924

8Weight of volatile solid ( g )1.7906

9Total Solid (TS) (mg/L)= [(5 2)g x 1000] / 5 mL

357.24

10Percentage of solid in sample (%)= (6 / 4 ) x 100

29.2187

11Total volatile solid ( VS ) ( mg/L )358.12 x 103

12Percentage of volatile solid ( % )29.29

TOTAL SUSPENDED SOLID

Sample ASample B

1Volume of Sample (ml)510

2Weight of filter paper (g)0.09220.0922

3Weight of filter paper + solid after drying at 103oC - 105oC or at 180oC21.4022.81

4Weight of solid (g)27.8326.69

5Weight of filter + solid after drying at 500oC ( 50oC (g)21.3922.80

6Weight of volatile solid (g)

7Total Suspended Solid (SS) (mg/L)

8Percentage of Volatile Suspended Solid (VSS) %

TOTAL DISSOLVED SOLID

Sample A

1Volume of sample (ml)5

2Weight of evaporating dish (g)

47.1346

3Weight of evaporating dish + sample (g)

52.3292

4Weight of sample (g)

= (3 2)

5.1946

5Weight of evaporating dish + sample after drying at 180oC (g)

47.1516

6Weight of Solid (g)

= (5 2)

0.0170

7Total Dissolve Solid (TDS) (mg/L)

= [(5 2) x 1000] / 5

3.400

8Weight of evaporating dish + solid after drying at 500oC ( 50oC (g)

47.1348

9Weight of dissolved solid (g)

= (8 2)

0.0002

10Total dissolved Solid (SS) (mg/L)

= [(8 2) x 1000] / 100

0.002

11Percentage of Volatile dissolved Solid (VSS) %

= (10 / 7) x 100

0.0588

CALCULATION FOR TOTAL SOLID

1) weight of sampleSample A := (3) (2)

= 52.5100 46.3968

= 6.1132 g

2) Weight of dissolved solid

Sample A := (5) (2)

= 48.1830 46.3968

= 1.7862 g

3) Weight of volatile solidSample A := (5) (7)

= 48.1830 46.3924

= 1.7906 g

4) Total solidSample 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/L7) Percentage of volatile solidSample A := [(8) / weight of sample] x 100%

= [(1.7906) / 6.1132 ] x 100 %

= 29.29 %CALCULATION FOR TOTAL SUSPENDED SOLID1) 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

2) Weight of filter paper + solid after drying at 103oC - 105oC or at 180oCSample A:

Weight of Evaporating Dish

= 18.2739 gWeight of Evaporating Dish + Filter Paper + Solid after drying = 30.1388 gSo, 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 gWeight 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 = 11.8649 gWeight of residue + dish or filter after ignition= 0.0866 g

So, Weight of volatile solid = 11.8649 0.0866= 0.01178mg x 1000 / 5

= 2.3560 g6) Total Suspended Solid (SS)[(Weight of filter + dried residue) (Weight filter)] x 1000 / 5

Sample A:

Weight of filter + dried residue = 11.8649 gWeight 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 = 235.6CALCULATION FOR TOTAL DISSOLVED SOLID

1) weight of sample

Sample A := (3) (2)

= 52.3292 47.1346

= 5.1946 g

2) Weight of dissolved solid

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/L4) Weight of dissolved solidSample 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 DISCUSSION1. 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.

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.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

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 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.10.0REFERENCES

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.htmMicrowave (at 180 c- 2c)

Microwave (at 103 c- 105c)

Muffle furnace ( at 500 c -50 c)

Muffle furnace ( at 500 c -50 c)

Total solids (TS)

Microwave (at 103 c- 105c)

Total Fixed solids (TFS) = FSS + FDS

Total Volatile solids (TVS) = VSS + VDS

Volatile dissolved solids (VDS)

Fixed dissolved solids (FDS)

Volatile suspended solids (VSS)

Fixed suspended solids (FSS)

Suspended solids (ss)

Total solids (TS)

Dissolved solids (DS)

Fiber glass filter ( < 2.0 m)

Settle able solids

Inhofe cone

Samples

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