14.0 EXPERIMENT ON DETERMINATION OF TOTAL SOLIDS IN WATER

Sl. No. Contents

Preamble

14.1 Aim

14.2 Introduction

14.2.1 Environmental Significance

14.3 Principle

14.4 Materials Required

14.4.1 Apparatus Required

14.5 Sample Handling and Preservation

14.5.1 Precautions

14.6 Procedure

14.7 Calculation

14.7.1 Table

14.7.2 Data Sheet

14.8 Interpretation of Results

14.9 Inference

14.10 Evaluation

14.0 EXPERIMENT ON DETERMINATION OF TOTAL SOLIDS IN

WATER PREAMBLE:

“How to determine total solids in Water and Wastewater”.

Test procedure is in accordance to IS: 3025 (Part 15) - Reaffirmed 2003. In addition to our Indian Standard, we also discuss in brief regarding the procedure stated in

(1) APHA Standard Methods for the Examination of Water and Wastewater - 20th Edition. Method 2540 B.

(2) Methods for Chemical Analysis of Water and Wastes, EPA-600/4-79-020, USEPA, Method 160.3.

14.1 AIM

To determine the total solids in the given water sample. Test procedure is in accordance to IS: 3025 (Part 15) - Reaffirmed 2003.

14.2 INTRODUCTION

The term “solids” is generally used when referring to any material suspended or dissolved in water or wastewater that can be physically isolated either through filtration or through evaporation.

Solids can be classified as either filterable or non filterable. Filterable solids may either be settleable or non settleable. Solids can also be classified as organic or inorganic.

Total Solids is the term applied to the material residue left in the vessel after evaporation of a sample and its subsequent drying in an oven at a defined temperature.

Measurement of Solids can be made in different water samples (industrial, domestic and drinking water) and it is defined as residue upon evaporation of free water.

Thus, Total solids are nothing but summation of total dissolved solids and total suspended solids.

14.2.1 ENVIRONMENTAL SIGNIFICANCE

Total solids measurements can be useful as an indicator of the effects of runoff from construction, agricultural practices, logging activities, sewage treatment plant discharges, and other sources.

Total solids also affect water clarity. Higher solids decrease the passage of light through water, thereby slowing more rapidly and hold more heat; this, in turn, might adversely photosynthesis by aquatic plants. Water will heat up affect aquatic life that has adapted to a lower temperature regime.

As with turbidity, concentrations often increase sharply during rainfall, especially in developed watersheds. They can also rise sharply during dry weather if earth-disturbing activities are occurring in or near the stream without erosion control practices in place.

Regular monitoring of total solids can help detect trends that might indicate increasing erosion in developing watersheds.

Total solids are related closely to stream flow and velocity and should be correlated with these factors. Any change in total solids over time should be measured at the same site at the same flow.

In the case of water: Water with total solids generally is of inferior palatability and may induce an unfavorable physiological reaction. It may be esthetically unsatisfactory for purposes such as bathing.

Total solids will be higher in highly mineralized waters, which result in unsuitability for many industrial applications.

It indicates effectiveness of sedimentation process and it affects effectiveness of disinfection process in killing microorganisms.

It is used to assess the suitability of potential supply of water for various uses. In the case of water softening, amount of total solids determine the type of softening procedure.

Corrosion control is frequently accomplished by the production of stabilized waters through pH adjustment. The pH stabilization depends to some extent upon the total solids present as well as alkalinity and temperature.

In the case of waste water:

Solids analyses are important in the control of biological and physical wastewater treatment processes and for assessing compliance with regulatory agency wastewater effluent limitations

Although the waste water or sewage normally contains 99.9 percent of water and only 0.1 percent of solids, but it is the solids that have the nuisance value.

The amount of solids in wastewater is frequently used to describe the strength of the water. The more solids present in a particular wastewater, the stronger that wastewater will be. The environmental impacts of solids in all forms have detrimental effects on quality since they cause putrefaction problems.

If the solids in wastewater are mostly organic, the impact on a treatment plant is greater than if the solids are mostly inorganic.

14.3 PRINCIPLE

The sample is evaporated in a weighed dish on a steam bath and is dried to a constant mass in an oven either at 103-105°C or 179-181°C.

Total solids/residue is calculated from increase in mass.

14.4 MATERIALS REQUIRED

14.4.1 APPARATUS REQUIRED

1. Crucible 2. Oven 3. Desiccators 4. Analytical Balance 5. Dish Tongs 6. Magnetic Stirrer 7. Wash Bottle

14.5 SAMPLE HANDLING AND PRESERVATION

Preservation of sample is not practical. Because biological activity will continue after a sample has been taken, changes may occur during handling and storage.

Both the characteristics and the amount of solids may change. To reduce this change in samples taken for solids determinations, keep all samples at 40 C.

Do not allow samples to freeze.

Analysis should begin as soon as possible.

14.5.1 PRECAUTIONS

The following precautions should be observed while performing the experiment:

• Water or Wastewater samples which contain high concentrations of calcium, chloride, magnesium or sulphate can rapidly absorb moisture from the air.

Such samples may need to be dried for a longer period of time, cooled under proper desiccation and weighed rapidly in order to achieve a reasonable constant weight.

We should be aware prolonged drying may result in loss of constituents, particularly nitrates and chlorides.

• Non-representative particulates such as leaves, sticks, fish and lumps of fecal matter should be excluded from the sample if it is determined that their inclusion is not desired in the final result.

• Floating oil and grease, if present, should be included in the sample and dispersed by a blender device before sub-sampling.

• Volume of sample should be adjusted to have residue left after drying as 100 to 200mg. It is mainly to prevent large amount of residue in entrapping water during evaporation.

• Highly mineralized water containing significant concentration of calcium, magnesium, chloride, and/or sulphate may be hygroscopic. Hence prolonged drying, desiccation and rapid weighing.

• We should be aware prolonged drying may result in loss of constituents, particularly nitrates and chlorides.

• Volume of sample should be adjusted to have residue left after drying as 100 to 200mg. It is mainly to prevent large amount of residue in entrapping water during evaporation.

14.6 PROCEDURE

• To measure total solids, take a clean porcelain dish which has been washed and dried in a hot air oven at 105°C for one hour.

Now weigh the empty evaporating dish in analytical balance. Let’s denote the weight measured as (W1).

• Now we should have to decide what should be the volume of sample to be taken for analysis.

• Volume may be estimated either from values of specific conductance or general thumb rule.

• In general, select a sample volume that will yield residue between 2.5 and 200 mg after drying.

• Using pipette transfer 75mL of unfiltered sample in the porcelain dish.

• Switch on the oven and allowed to reach 105°C. Check and regulate oven and furnace temperatures frequently to maintain the desired temperature range.

• Place it in the hot air oven and care should be taken to prevent splattering of sample during evaporation or boiling.

• Dry the sample to get constant mass. Drying for long duration usually 1 to 2 hours is done to eliminate necessity of checking for constant mass.

• Cool the container in a desiccator. Desiccators are designed to provide an environment of standard dryness. This is maintained by the desiccant found inside. Don't leave the lid off for prolonged periods or the desiccant will soon be exhausted.

• Keep desiccator cover greased with the appropriate type of lubricant in order to seal the desiccator and prevent moisture from entering the desiccator as the test glassware cools.

• We should weigh the dish as soon as it has cooled to avoid absorption of moisture due to its hygroscopic nature.

• Samples need to be measured accurately, weighed carefully, and dried and cooled completely.

• Note the weight with residue as (W2). 14.7 CALCULATION Initial weight of the Crucible (W1) = ……….. g Final weight of the Crucible + sample (W2) = ……….. g Weight of residue (W) = W2 - W1 g

Amount of total solids present in the sample = v

w1000*1000

W = weight of total residue in (mg). (Therefore multiply W with 1000)

V = Volume of the sample (mL)(To convert mL to L)

=…………..mg/L

The readings are required to be tabulated. 14.7.1 TABLE

Description Weight (g)

14.7.2 DATA SHEET

DETERMINATION OF TOTAL SOLIDS

DATA SHEET

Date Tested : August 30, 2010

Tested By : CEM Class, Group A

Project Name : CEM, NITTTR Lab

Sample Number : BH1

Sample Location : Perungudi (Lat 12’ 57’’ 31.74 & Long 80’ 14’’ 8.82)

Sample Description : Surface water

Specimen Calculation:

W1 = 35. 4323 g W2 = 35. 4739 g V = 75. 0 mL

Weight of residue (g) W = W2 - W1

= 35. 4739 - 35. 4323 = 0. 0416 g

Weight of residue in mg (To convert W (g) to W (mg), multiply W (g) with 1000) W (mg) = 0.0416 x 1000 = 41.6mg

Multiply the weight of the dry solids (in mg) by 1,000 mL/L to convert the sample size from mL to L.

Description

Total Solids (mg/L) V = Volume of the sample (mL) (To convert mL to L, multiply by 1000)

=41.6 mg/75 mL = 0.555 mg/mL = 0.555 mg/mL x 1,000 mL/L = 555 mg/L

Weight (g)

Initial Weight of the Crucible (g) W1 35. 4323

Final Weight of the Crucible + sample (g) W2 35. 4739

Weight of residue(g) W 0. 0416

Volume of the Sample (mL) V 75. 0

Total Solids (mg/L) TS 555.0

14.8 Interpretation of Results

In the given sample, a total solid is equivalent to 555.0 mg/L. 14.9 Inference

Total solids are nothing but summation of Total Dissolved Solids and Total Suspended Solids. Regular monitoring of total solids can help detect trends that might indicate increasing erosion in developing watersheds. Total solids also affect water clarity. Total Solids may indicate the presence of agricultural activities, dredging, or mining upstream from your sample site. 14.10 Evaluation

1. After Evaporation, the evaporating dishes needs to be .

a) weighed immediately b) kept in air for cooling to room temperature c) cooled to room temperature in a dessicator d) cooled to a temperature less that 25ºC

2. Total Solids are referred to materials left after evaporation.

a) True b) False

3. A sample was stored @ 4 ºC for 4 days. During the analysis, the temperature of the sample should be

a) maintained at 4 ºC b) brought to room temperature c) below room temperature d) brought above room temperature by adding boiled distilled water

4. The determination of total solids in wastewater gives an idea about

a) the foulness of the sewage b) pH of the sewage c) temperature of the sewage d) colour of the sewage

5. The evaporating dishes needs to be cleaned and dried at _______ to remove the existing organic content.

a) 100° C b) 250° C c) 450° C d) 550° C

6. Sewage contains about 99% of _____.

a) water b) solids c) clay d) microbes

7. Interference in the determination of total solids is due to ______.

a) Oil and Greese b) Large water sample c) Dissolved salts d) Suspended salts

8. For analysis of total solids the sample used should be

a) homogenous sample b) supernatant of the sample c) settled sample d) clear sample

9. The sewage contain

a) suspended and dissolved solids. b) no solids c) only dissolved solids d) only suspended solids

10. The major dissolved substances in natural water are comprised of

a) iron, manganese, silica and nitrate b) calcium, magnesium, sodium, bicarbonate, sulfate and chloride c) all anions d) all cations

KEY TO ITEMS:

1) c

2) True

3) b

4) a

5) d

6) a

7) a

8) a

9) a

10) b