PRACTICAL - 02
Aim - To determine particle size particle size distribution of a powder by using
microscopic method
Theory:
Powder is a collection of particle of different sizes. For powder analysis size of
individual particle and how many particle having same size exists in the same sample is
very important. The powder particle generally expressed in number or weight.
There are various methods used to determine particle size and size distribution these
are:
Sieving method
Sedimentation method
Volume method
Optical microscopy method
The microscopy is used direct to determine particle size distribution ,these method used
to determine particle size having 0.2 to 100 [Link] determining particle size of
powder sample required in the form of suspension, emulsion, and diluted powders is
mounted on slide and size range is measured by using eyepiece micrometer by using
this method depth can not be estimated only diameter is obtained is a disadvantage of
this method.
The particle size, and size distribution is represented by number and weight distribution
size frequency normal distribution, log normal distribution and cumulative distribution
Advantages of microscopic method:-
1. Particles can be view easily
2. This method is simple and accurate within certain limit of the particle size
3. This technique may give detection of agglomerated particles
Ditadvantages of microscopiemethode:-
1 This method is only measure length and width of the particles depth of the particle
cannot be measure.
2 This is a time consuming method it required to count more than 500 particles for
accuracy
3 Presence of moisture causes problem such as, aggreation
4 This method is not suitable for extremely small size particles
Requirement:-
Chemicals Any powder sample OR Diluted suspension
Apparatus Microscope, Eyepiece micrometer scale Standard stage micrometer scale,
Glass slide, Cover slip etc
Procedure:-
1 Clean all the apparatus and glasswares like slides ,stage micrometer scale eyepiece of
microscope and light reflecting mirror
2. Light is adjust for maximum intensity and mount the standard stage micrometer on
stage
3. For calibration fit eyepiece scale in eyepiece microscope
4. Calibrate eyepiece scale using standard stage micrometer scale as described under
calculation
5. And find one division of eyepiece scale with respect to micrometer unit.
6 Prepare a dilute suspension of given powder sample in distilled water, place a drop of
the suspension on the glass slide and cover with coverslip.
7. Observe the particles under the microscope with calibrated eyepiece micrometer.
8. Place the slide on stage microscope and rotate it for better resolution.
Observations:-
Standardization of eyepiece micrometer:-
One division of standard stage micrometer is = 0.01 mm =10u
Sr Division of eye Division of stage One division of eyepiece
no. piece micrometer micrometer micrometer u = Sm/Em ˟ 10
1
2
3
4
Calibration of eye piece scale:-
The calibration of eyepiece scale, standard stage micrometer is used and place in
eyepiece of microscope, eyepiece scale is glass slide on which linear scale is there
having length 1.0mm. the 1 mm is divided into 100 equal parts.
One division of standard stage micrometer =10mm OR 0.01 mm
The linear scale having 10mm length engraved on glass disc at centre and divided into
100 equal parts each part is equal to 0.1 mm
Observation table:-
Sr no. Size Mean of Numbers % % nd Nd2 Nd3
range in size d of particles frequancy
micron (micron) particles
(n)
1 0-0.5 0.25
2 0.5-1.0 0.75
3 1.0-1.5 1.25
4 1.5-2.0 1.75
5 2.0-2.5 2.25
Ʃn= Ʃnd= Ʃnd2= Ʃnd3=
Calculate statistical diameter defined as...
1. Arithmetic mean diameter is denoted by(d/n) and calculated by the equation d/n=
Ʃnd2/Ʃn
2. Surface length mean diameter is denoted by dsl dsl= Ʃnd2/Ʃnd
3, Volume surface mean diameter is denoted by dvs dvs = Ʃnd3/Ʃn2
4. Surface number mean diameter is denoted by dsn dsn = (Ʃnd2/Ʃn)1/3
5. Volume number mean diameter is denoted by dvn dvn = (Ʃnd3/Ʃn)1/3
plot the graph of % frequency VS particle size d % frequency particle size
Precautions:-
1. Calibrate the eyepiece micrometer with stage micrometer
2. Used dilute suspension to avoid aggregates
3, 10X and 45X objective is used for observation
4. Avoid entrapment of air bubble if coverslip is used
Results:- The statistical parameters are –
Arithmetic mean diameter (d/n)=.................... um
Volume surface mean diameter(dvs) =............... um
Surface length mean diameter(dsl) =................., um
Surface number mean diameter(dsn) = ................... um
Volume number mean diameter(dvn) =......................... um