INTRODUCTION

Solids suspended in water may consist of inorganic and organic particles or of immiscible

liquids. Inorganic solids such as clay, silt, and other soil constituents are common in surface

water. Organic material such as plant fibers and biological solids (algal cells, bacteria, etc.) are

also common constituents of surface waters. These materials are often natural contaminants

resulting from the erosive action of water flowing over surfaces. Because of the filtering capacity

of the soil, suspended material is seldom a constituent of groundwater.

Other suspended material may result from human use of the water. Domestic wastewater

usually contains large quantities of suspended solids that are mostly organic in nature. Industrial

wastewater may result in a wide variety of suspended impurities of either organic or inorganic

nature. Immiscible liquids such as oils and greases are often constituents of wastewater.

Suspended solids, where such material is likely to be organic and/or biological in nature,

are an important parameter of wastewater. The suspended solids parameter is used to measure

the quality of wastewater influent, to monitor several treatment processes, and to measure the

quality of the effluent. Environmental Protection Agency (EPA) has set a maximum suspended

solids standard of 30 mg/L for most treated wastewater discharges.

A well-mixed measured sample is filtered through a weighed standard glass-fiber filter

and the residue retained on the filter is dried to a constant weight at 103°C to 105°C. The

increase in weight of the filter represents the total suspended solids. If the suspended material

clogs the filter and prolongs filtration, it may be necessary to increase the diameter of the filter or

decrease the sample volume.

OBJECTIVE

To provide and strengthen knowledge, skill, and understanding in solid determination and enable

to relate theories taught to the practices in laboratory

THEORY

Solids refer to matter suspended or dissolved in water or waste water. Solids may affect water or

effluent quality adversely in a number of ways. Waters with high dissolved solids generally are

of inferior palatability and may induce a favorable physiological reaction in the transient

consumer. Solids analyses are important in the control of biological and physical wastewater

treatment process and for assessing compliance with regulatory agency wastewater effluent

limitations. Generally, ‘total solids’ is the term applied to the material residue left in the dishes

after evaporation of a sample at 103°C to 105°C. Total solids include ‘total suspended solids’,

and ‘total dissolved solids’. Total suspended solid is the portion of total solids retained by filter,

and total dissolved solids is the portion of solids that passes through a filter of 2.0 μm (or

smaller) nominal pore size under specified conditions. ‘Fixed solids’ is refer to the temperature

(500°C ± 50°C for 15 minutes). The weight loss on ignition is called ‘volatile solids’.

Determination of fixed and volatile solids does not distinguish precisely between inorganic and

organic matter because it includes losses due to decomposition or volatilization of some mineral

salts. ‘settleable solids’ is the term applied to the material setting of of suspension within a

defined period. It may include floating material, depending on the technique.

DIAGRAM

Settle able solids

Inhofe cone

Microwave (at 103 c⁰ -

105 c⁰ )

Total solids (TS)

Microwave (at 180 c⁰ - 2 c⁰ )

Muffle furnace ( at 500 ⁰c -50⁰ c)

Fiber 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

Volatile suspended solids (VSS)

EQUIPMENTS AND MATERIALS

Sets of evaporating dishes: dishes of 100 ml capacity made of porcelain, platinum or high silica glass and apparatus.

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

Steam bathDesicator

Dyring oven

Analytical balance

Magnetic stirrerGraduated cylinder

Wid-bore pipet

Low-form beaker

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 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 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 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 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.

RESULT AND CALCULATION

1. TOTAL SOLID

Sample A Sample B

1 Volume of sample (ml) 5 10

2 Weight of evaporating dish (g) 21.39 20.2

3 Weight of evaporating dish + sample 27.56 30.2

4Weight of sample (g)= (3 – 2)

6.1710

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

22.8621.9

6Weight of solid (g)= (5 – 2)

1.471.7

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

21.32 20.2

8Weight of volatile solid ( g )(5 – 7)

1.54 1.7

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

294.0340.0

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

23.817

11 Total volatile solid ( VS ) ( mg/L ) 308 x 103 170 x 103

12 Percentage of volatile solid ( % ) 25 17

2. TOTAL SUSPENDED SOLIDSample A Sample B

1 Volume of Sample (ml) 5 102 Weight of filter paper (g) 0.0922 0.0922

3Weight of filter paper + solid after

drying at 103oC - 105oC or at 180oC21.40

22.81

4 Weight of solid (g) 27.83 26.69

5Weight of filter + solid after drying

at 500oC 50oC (g)21.39

22.80

6 Weight of volatile solid (g) 0.01 0.017 Total Suspended Solid (SS) (mg/L)

8Percentage of Volatile Suspended

Solid (VSS) %

3. TOTAL DISSOLVED SOLID

CALCULATION FOR TOTAL SOLID

1) weight of sample

Sample ASample B

1 Volume of sample (ml) 5 10

2 Weight of evaporating dish (g) 22.65 21.2

3Weight of evaporating dish + sample (g) 27.21 23.5

4Weight of sample (g)= (3 – 2) 4.56 2.3

5Weight of evaporating dish + sample after drying at 180oC (g) 22.76 22.23

6Weight of Solid (g)= (5 – 2) 0.11 0.03

7Total Dissolve Solid (TDS) (mg/L)= [(5 – 2) x 1000] / 5

4.552 3

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

22.70 21.23

9Weight of dissolved solid (g)= (8 – 2) 0.05 0.03

10Total dissolved Solid (SS) (mg/L)= [(8 – 2) x 1000] / 100 0.5 0.3

11

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

2.27 1

Sample A : = (3) – (2)= 27.56– 21.39= 6.17g

2) Weight of dissolved solid

Sample A : = (5) – (2)= 22.86 – 21.39= 1.47g

3) Weight of volatile solid

Sample A : = (5) – (7)= 22.86 – 21.32= 1.54 g

4) Total solid

Sample A : = (6) × 103 × 103 Volume of sample

= Weight of solid x 10 3 ×10 3 Volume of sample = (1.47x 103 x 103 ) / 5 ml = 294.0 mg/L

5) Percentage of solid in sample

Sample A : = [(6) / weight of sample ] x 100% = [ (1.47) / 6.17] x 100% = 23.8%

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%= [(1.54) / 6.17] x 100 %= 25 %

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

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 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

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.

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

\

CONCLUSION

From the experiment, we able to characterize 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 include 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 are 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.