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

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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.

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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.

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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.

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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 μ 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 + i

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TOTAL SOLID DETERMINATION

4.0 DIAGRAM

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Settleable solids

Imhoff cone

Microwave (at 103 c⁰ -

105 c⁰ )

Total solids (TS)

Microwave (at 180 c⁰ - 2 c⁰ )

Muffle furnace ( at 500 ⁰c -50⁰ c)

Fibre glass filter

( < 2.0 µm)

Microwave (at 103 c⁰ - 105 c⁰ )

Muffle furnace ( at 500 ⁰c -50⁰ c)

Samples

Dissolved solids (DS)Suspended

solids (ss)

Fixed dissolved solids (FDS)

Volatile dissolved solids (VDS)

Total Fixed solids (TFS) = FSS + FDS

Total solids (TS)

Total Volatile solids (TVS) = VSS + VDS

Fixed suspended solids (FSS)

Volatile suspended solids (VSS)

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

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TOTAL SOLID DETERMINATION

3. Desicator

4. Vacuum pump

5. 10 ml pipette

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TOTAL SOLID DETERMINATION

6. Oven operating at the temperature 180 0C

7. Analytical balance

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TOTAL SOLID DETERMINATION

6.0 PROCEDURE

A. 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 180’C for

30 minutes.

v. After 30 minutes the sample to removed 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 300’C

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 then 4% or 0.5 mg from the pervious 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).

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TOTAL SOLID DETERMINATION

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

180’C 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 300’C.

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.

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TOTAL SOLID DETERMINATION

7.0 RESULT AND CALCULATION

TOTAL SOLID

Sample A

1 Volume of sample (ml) 5

2 Weight of evaporating dish (g) 46.3968

3 Weight of evaporating dish + sample 52.5100

4Weight of sample (g)= (3 – 2)

6.1132

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

48.1830

6Weight of solid (g)= (5 – 2)

1.7862

7Weight of evaporating dish ( g ) + solid after drying process at 103ºc-105ºc

46.3924

8 Weight 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

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

12 Percentage of volatile solid ( % ) 29.29

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TOTAL SOLID DETERMINATION

TOTAL SUSPENDED SOLID

Sample A1 Volume of Sample (ml) 52 Weight of filter paper (g) 0.0930

3Weight of filter paper + solid after

drying at 103oC - 105oC or at 180oC11.8649

4 Weight of solid (g) 11.7719

5Weight of filter + solid after drying

at 500oC 50oC (g)0.0866

6 Weight of volatile solid (g) 2.35607 Total Suspended Solid (SS) (mg/L) 2.3544

8Percentage of Volatile Suspended

Solid (VSS) %235.6

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TOTAL SOLID DETERMINATION

TOTAL DISSOLVED SOLID

Sample A1 Volume of sample (ml) 5

2 Weight 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

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Percentage of Volatile dissolved Solid (VSS) %= (10 / 7) x 100

0.0588

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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)= 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 10 3 ×10 3 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 %

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TOTAL SOLID DETERMINATION

CALCULATION FOR TOTAL SUSPENDED SOLID

1) Weight of Filter Paper

Sample A :

Evaporating Dish + Filter Paper = 18.3669 gEvaporating Dish = 18.2739 gSo, weight of filter paper = 18.3669 – 18.2739= 0.0930 g

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

Sample 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 gWeight of Filter Paper = 0.0930 gSo, 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 gWeight of Evaporating Dish + Filter Paper + Solid after drying = 18.3605 gSo, 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

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TOTAL SOLID DETERMINATION

Sample A:Weight of residue + dish or filter before ignition = 11.8649 gWeight of residue + dish or filter after ignition = 0.0866 gSo, Weight of volatile solid = 11.8649 – 0.0866 = 0.01178mg x 1000 / 5

= 2.3560 g

6) 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 gSo, 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

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TOTAL SOLID DETERMINATION

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

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 10 3 ×10 3 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 %

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TOTAL SOLID DETERMINATION

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.

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.

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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 = 1.5413gResidue on glass fibre filter after drying at 1050C = 1.5538 g

Total Suspended Solid (TSS), mg/L =____(A – B) x 10 6 _____ 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 10 6 Volume of sample (mL)

Volume of sample (mL) = (1.5538- 1. 5413) x 10 6 175 mg/L

= 71.4286 mL

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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

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.

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TOTAL SOLID DETERMINATION

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

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