This document discusses methods for determining various properties of powders including heavy metals, fineness, density, and moisture content. It describes common techniques like atomic absorption spectrophotometry and x-ray fluorescence for measuring heavy metals in powders. Methods are provided for assessing the fineness of powders based on their particle size distribution using sieves. Density determination techniques including displacement type densitometers and solvent displacement are outlined. Finally, thermal, loss on drying, and Karl Fischer titration methods for measuring moisture in powders are summarized along with references.

1. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 1
A Seminar as a part of curricular requirement
for I year M. Pharm II semester
Presented by
M.MALARVANNAN. (20L81S0704).
M.PHARM
Department of Pharmaceutical Analysis
DETERMINATION OF HEAVY METALS
FINENESS OF PWDER,
DENSITY AND MOISTURE

2. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 2
S.NO CONTENT
1 Heavy metals
2 Heavy metal determination
3 Powder
4 Determination of fineness of powder
5 Density
6 Density determination methods
7 Determination of moisture content
8 Reference
Content Table

3. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 3
• Heavy metals are generally defined as metals with relatively high
density (5 g/cm3), atomic weights, or atomic numbers.
• Heavy metals are toxic to human health. it is are largely found in
nature as minerals and ore.
Heavy metals
Lead- 10 PPM Cadmium- 0.3 PPM
Arsenic- 3 PPM Mercury- 1 PPM

4. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 4
Methods for measurement of trace metals
• Most common method of collecting particulate matter is through
filters.
• Identification and concentration of individual trace metals like lead,
cadmium, arsenic, mercury and chromium is determined by
• 1: Atomic absorption spectrophotometer
• 2: X-ray fluorescence
Determination of heavy metals

5. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 5
1. Atomic absorption spectrophotometry is a destructive method
and requires at least 1 to 2 ml of solution.
2. X-ray fluorescence is a non-destructive method and works
independent of the chemical state of the sample.
Cont…

6. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 6
• Powders are mixtures of dry finely divided drugs and or chemicals
that may be indented for internal or external use.
• Example: face powder, baby powder, dusting powder etc…
Powders

7. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 7
For course and moderate coarse powder:
• Place 25 to 100g of the powder being examined upon the appropriate
sieve having a close fitting pan and cover.
• Shake the sieve in a rotatory horizontal direction and vertically by
tapping on a hard surface for not more then 20mins or until shifting is
practically complete.
• Weigh accurately the amount reaming on the sieve and the receiving
pan.
Calculation:
Material retained on the specified sieve, percent by mass = 100×𝑀1/ 𝑀
M-total wt of sample taken M1-sample retained in the individual sieve
Determination of fineness
of Powders

8. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 8
For fine and very fine powder:
• Proceed as described under Coarse and moderately coarse powders
except that
• (a) The test sample should not exceed 25 g.
• (b) The sieve is to be shaken for not less than 30 minutes or until sifting
is practically complete.
• (c) The particles passing through a sieve of nominal mesh aperture of
45 mm are determined by suitable microscopic examination.
Cont….

9. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 9
For micro fine and superfine powders:
• Proceed as described under Fine and very fine powders except that the
particles passing through a sieve of nominal mesh aperture of 45 µm (for
fine powders.) or those less than 10 mm in size are determined by
suitable microscopic examination.
• With oily and other powders which tend to clog the openings, carefully
brush the screen at intervals during sifting. Break up any lump that may
form.
Cont….

10. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 10
• A material's density is defined as its mass per unit volume. It is, essentially, a
measurement of how tightly matter is crammed together.
• The principle of density was discovered by the Greek scientist Archimedes.
• To calculate the density of an object, take the mass ( m ) and divide by the
volume ( v ). This will give you the density in g/cm 3
Density

11. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 11
For powders and granules:
Bulk density
True density
Density determination

12. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 12
Displacement type Densitometer:
Mainly it consist of float and chain. The test liquid will flow through the
transparent chamber from bottom to top. When the float movement depends
upon the density of sample and the floating positions a function of the density.
Cont…

13. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 13
Solvent displacement method:
• Select the solvent in which powder is insoluble. The Pycnometer or sp.
gravity bottle were used.
• Wt. of pycnometer: w1
• Wt. of pycnometer + sample: w2
• Sample wt.: w3= w2-w1
• Wt. of pycnometer + sample + solvent: w4
• Wt. of liquid displaced by sample: w5 = w4-w2
• Thus, true density = w3/ w5
Cont…

14. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 14
“condensed or diffused liquid, especially water which is present in
the sample is called moisture”
Determination of moisture content:
• Thermal method
• LOD method
• Chemical method
• Karl fischer method (KF-titration).
Moisture

15. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 15
Loss on drying method:
Cont…

16. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 16
Karl fischer titration method:
• The titrimetric determination of water is based upon the quantitative
reaction of water with an a solution of excess sulfur dioxide and known
iodine concentration (mg H2O/mL KFR) in a suitable medium (methanol) in
the presence of a base (buffering agent) that reacts with hydrogen ions.
Cont…
• The water content is determined by measuring
the amount of iodine consumed as a result of
reaction with water in a sample.

17. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 17
1. The International Pharmacopoeia - Eighth Edition, 2018 1.12 Powder
fineness and sieves.
2. Indian Standard SKIN POWDER — SPECIFICATION BEAUREA OF INDIAN
STANDARDS.
3. https://www.slideshare.net/SrinivasaRao110/density-and-viscocity, 2017.
4. https://www.slideshare.net/ragavarsha/moisture-determination-
techniques , 2017.
5. Determination of essential and toxic trace elements in ten herbal medicines
using energy-dispersive XRF analysis. X-Ray Spectrometry, 40(1), 31–36.
6. https://www.slideshare.net/NimraIqbal/heavy-metals-43930266
Reference: