1) Explain common laboratory apparatus used in quantitative analysis. Define molality, ppm and ppb.

a) Common laboratory apparatus used in quantitative analysis are:

1) Beaker: Also known as a boiling flask, the Florence flask has a round bottom and a long neck. It is
used to hold liquids and can be easily swirled and heated. It can also easily be capped by rubber or glass
stoppers. Once again, safety dictates that this flask never be heated when capped. Pressure build-up and
explosions can and do occur.

2) Test tube: A test tube is a glass tube with one end open and the other end closed. The closed end is
rounded. Test tubes are used to hold small samples. They are primarily used for qualitative assessment
and comparison. A common place to see these is the biochemistry lab. When a large number of samples
need to be tested and compared, test tubes are used to make this easier. They are also easily capped
with a rubber or glass stopper.They are generally held in a test tube rack specifically designed for the
purpose. If the test tubes become unsafe to touch with bare hands (whether due to heat or another
reason), test-tube tongs can be used to move them.

3) Watch glass: A watch glass is just a round piece of glass that is slightly concave/convex (think of a
lens). It can hold a small amount of liquid or solid. They can be used for evaporation purposes and also
can function as a lid for a beaker.

4) Conical flask: Also known as a conical flask, the Erlenmeyer flask was named after its inventor in
1861. It has a narrow neck and expands toward its base. This allows easy mixing and swirling of the flask
without too much risk of spilling. The narrow opening also allows for the use of a rubber or glass stopper.
It can easily be clamped to a ring stand (discussed below) as well as heated or shaken mechanically

5) Lab funnel: A lab funnel is just like any other funnel except that it was designed to be used in a
laboratory setting. They can be made of plastic or glass and can have either a short stem or a long stem,
depending on what they are needed for. There are several sizes that can be chosen from based on the
amount of liquid that needs to go through them quickly.

6) Graduated cylinders (Measuring cylinders): This is a primary measuring tool for the volume of a
liquid. There are several markings up and down the length of the container with specific increments.
Graduated cylinders come in many sizes. The smaller they are in diameter, the more specific the volume
measurements will be. When reading the volume from a graduated cylinder, you will notice that the liquid
seems to have an indentation. The liquid around the edges will be higher than the liquid in the center,
sloping down like the sides of a trampoline when someone is standing in the middle. This is called the
meniscus. Line the lowest point of the meniscus up with the nearest marking, keeping the cylinder level
to properly read the volume.

7) Volumetric flask: A volumetric flask is a round flask with a long neck and flat bottom. It is used to
measure an exact volume of liquid. There is a small line on the neck that indicates how far to fill the
bottle (use the bottom of the meniscus). They come with special caps that will not let anything in or out.
8) Droppers: These are small glass tubes with narrow tips on one end and a rubber bulb on the other.
They suck up liquid that can then be squeezed out in small drops. These can be used to add an indicator
to a solution about to be titrated.

9) Pipettes: There are a large variety of pipettes designed to accomplish specific goals. However, they
are all for measuring an exact volume of liquid and placing it into another container.

10) Burettes: To determine how much liquid is added, write down how much is initially in the burette.
Then when you're finished adding, write down how much is left. Subtract the final amount from the initial
amount and you have the volume of liquid added. Again, remember to measure from the bottom of the
meniscus.

11)Crucible: A crucible is a small clay cup made of a material that can withstand extreme temperatures.
They are used for heating substances and come with lids.

12) A funnel: A lab funnel is just like any other funnel except that it was designed to be used in a
laboratory setting. They can be made of plastic or glass and can have either a short stem or a long stem,
depending on what they are needed for. There are several sizes that can be chosen from based on the
amount of liquid that needs to go through them quickly.

Spatulas and scoopulas are for scooping solid chemicals. They are typically used to scoop a chemical out
of its original container onto a weigh boat so that it can be weighed on a balance.

Tongs and forceps are for grabbing things that should not be touched by hand. Some tongs are specially
made to hold beakers, others to hold test tubes, and so on. There are also general tongs.

Always make sure everything is clamped to the stand tightly. When clamping glass, be careful not to
shatter the glass. Only tighten until snug. When using a ring on the stand, there are usually other pieces
necessary to accomplish the goal. Wire mesh is laid across the ring to distribute evenly heat and support
the beaker. A clay triangle with an open center is used to suspend crucibles. Make sure everything is
balanced! Do not let the whole setup tip over.

Molality: Molality is defined as the “total moles of a solute contained in a kilogram of a solvent.” Molality
is also known as molal concentration. It is a measure of solute concentration in a solution .

Formula:

m= mol / kg,

m = molality, mol=moles of solute kg = kilograms

PPM: This is an abbreviation for "parts per million" and it also can be expressed as milligrams per liter
(mg/L). This measurement is the mass of a chemical or contaminate per unit volume of wate r.
Whereas, 1 ppm is equal to 0.0001 percent. To convert the ppm value to percentage, divide the ppm
value by 10,000.

PPM is the US standard unit of measurement in water chemistry. It tells us the density of a given
substance dissolved in water. Examples include free chlorine, calcium hardness, and total alkalinity. 1
PPM means that substance is one-millionth of the total amount of water.

PPB: Parts per billion (ppb) is a term that expresses the number of units (parts) of a given substance
that exist as a portion of a greater substance comprised of one billion parts. “Parts-per” notations such as
ppb are referred to as “volume in volume” measurements.

One part per billion equates to one particle existing within a substance comprised of 999,999,999 other
particles. This measurement can be expressed as 1ppb, which is equal to 1 x 10− 9 or 0.000 0001% of the
total substance.

2) Explain the determination of dissolved salts, Dissolved oxygen and COD.

a) 1) Determination of Dissolved salts: 1) TDS can be determined by two methods:

1. Gravimetric analysis: This method is a laboratory method and is time taking but results are
accurate. Here, water sample is prepared by filtering water by 1.5 micron filter so as to separate
suspended soilds from the water.

Procedure-Step1- Take an empty beaker and note down its weight, say- 20 g.

Step2- Put water sample in the beaker and take weight again, say-220 g which, means weight of

water=220 g – 20 g=200 g.

Step3- Heat the beaker to evaporate water and once all the water is evaporated take the weight of

beaker along with the residue, say-21 g which means weight of residue is= 21g – 20 g=1 g.

Weight of residue= 1 g= 1000 mg

Weight of water=200 g

Volume of water=200/1(density of water= 1 g/cc)

=200 cc=200 mL=0.2 litres

TDS=1000 mg/0.2 Litres= 5000 mg/L=5000 ppm

2) Total Suspended solids are determined by Gravimetric Analysis in laboratory. Since water contains

both dissolved as well as suspended solids, hence for the determination it is essential to separate the two

solids.First, water sample is filtered using 1.5 micron filter and the residual contents over filter contains
suspended solids. This filter is kept inside oven at 104°C and taken out after an hour. The dried weight of

filter along with dried residue is taken. After subtracting the weight of filter in this weight , the suspended

solids weight is found out and by dividing the weight of suspended solids by volume of water, the Total

Suspended Solids value in ppm or mg/L can arrived at.

2) Determination of Dissolved oxygen:

1: The Winkler Method
When a manganese peroxide solution and a sodium hydroxide solution are combined with sample water,
a precipitate of manganese hydroxide (II) is formed. This manganese hydroxide (II) precipitate interacts
with dissolved oxygen in the water and is oxidized in proportion to the quantity of DO, leaving a brown
precipitate.
If DO is missing: 

If it reacts with DO:

 
If you dissolve this brown precipitate in an acid containing iodine ions (I-), iodine (I 2) will be liberated in
proportion to the amount of DO. The amount of liberated iodine is then determined by titration with
sodium thiosulfate.

Modified Winkler’s Method Using Sodium Azide

The goal of this approach is to increase the accuracy of DO measurement using Winkler's method. The
I2 that remains after the titration with sodium thiosulfate in the last procedure of Winkler's technique, is
titrated with a starch solution again in this approach.
2: Miller's technique is another titration method

Diaphragm Electrode Technique

Dissolved oxygen levels are commonly measured using the diaphragm electrode technique. This
technique uses electrodes to measure the amount of oxygen passing through a highly oxygen permeable
diaphragm. The galvanic electrode method and the polarographic method are two ways for determining
dissolved oxygen levels using electrodes.

Sensors for Pulsed Polarographic Dissolved Oxygen

When detecting dissolved oxygen, pulsing polarographic dissolved oxygen sensors eliminate the need to
mix the sample. A steady-state polarographic DO sensor is similar to a rapid-pulse DO sensor in that both
use a gold cathode and a silver anode. Both steady-state and rapid-pulse sensors detect dissolved
oxygen by polarizing the electrodes with a constant voltage.

3) Determination of COD:
The most common test method is the colorimetric analysis after oxidizing the COD with acid and using
indicator compounds, such as hexavalent dichromate. In some instances, however, there are compounds
that will interfere with the colorimetric analysis, and titration is required to determine COD levels .