FACULTY OF CHEMICAL AND PROCESS ENGINEERING TECHNOLOGY

PHARMACEUTICAL FORMULATION METHOD

(BTF2153 )
Semester I 2023/2024
Title of Experiment : Tap Density
Date of Experiment :
Lecturer’s Name : En. Razhan Bin Hassan

Group Number: 6

NO NAME NO. ID

1 NUR IZZAIDAH BINTI ZAIRUL FAMI TJ22054

2 WAN ANIS 'AQILAH BINTI WAN KHAIRULAMIN TJ22044

3 NAZHIRATUL FARHANAH BINTI RUSDI TJ22045

4 ZULAIKA BINTI ZAINAL ABIDIN TJ22046

5 MUHAMMAD NAQIUDDIN BIN KHAMISAN TJ22047

6 NURUL AIN NABILA BINTI MOHD JIDI TJ22048

MARKS
TABLE OF CONTENTS

ABSTRACT 2

INTRODUCTION 3

EXPERIMENTAL PROCEDURES 4

RESULT 5- 6

DISCUSSION 7- 8

CONCLUSION 9

REFERENCES 10

APPENDICES 11

1
ABSTRACT

The tapped density is an increased bulk density attained after mechanically tapping a
container containing the powder sample. The tapped density is obtained by mechanically
tapping a graduated measuring cylinder or vessel containing the powder sample. The main
purpose of this experiment is to determine the compressibility index of sago and corn starch.
Tapped density is important to determine the optimum volume in tablet manufacturing by
providing the information about the volume changes that occur after tapping. In this
experiment the sample that has been used is sago seed and corn starch. The experiment starts
by weighing the measuring cylinder without cornstarch or sago seed. The sago seed is
inserted into the measuring cylinder and weighed again. The measuring cylinder is inserted
at the machine and the machine is set up. The START key is pressed and the METHOD key
is pressed to select either USP I or USP II. USP I is used in this experiment. The SET key is
and the weight of the sample is entered and the ENTER key is pressed to set the weight of the
sample. The initial volume of sago seed inserted in the measuring cylinder is determined and
entered in the machine. The ENTER key is pressed to set the initial volume. After all the
setup is complete the START key is pressed to run the test. The cylinder will be tapped 300
times for V1. The volume after tapping is recorded. The tapping continues for 490 times for
V2 and 750 times for V3. The test is continued until constant volume is obtained. If the
difference of the volume between V2 and V3 is less than 2 ml, the V3 value is the final
volume otherwise the test will run again to obtain V4 with 1250 times of tapping. After the
test is finished the STOP key is pressed. The step is repeated for cornstarch and all the results
are recorded. Based on the result obtained for sago seed, the tapped density is 0.7390 g/ml
and the bulk density is 0.6978 g/ml with compressibility index 5.56%. For cornstarch, the
tapped density is 0.5723g/ml and the bulk density is 0.4769 g/ml with compressibility index
16.67%. In summary, tapped density experiment is a crucial step to ensure a good quality of
powder for drug manufacturing.

2
INTRODUCTION

The tapped density is an increased bulk density attained after mechanically tapping a
container containing the powder sample[1]. To determine the tapped density, a graduated
measuring cylinder or vessel holding the powder sample must be mechanically tapped. After
observing the initial powder volume or mass, the measuring cylinder or vessel has been
mechanically tapped and then volume or mass readings are taken until there is little more
observed change in the volume or mass of the powder. Raise the cylinder or vessel and let it
fall at a specific height under its own weight to accomplish the mechanical tapping.

A comparison of the bulk and tapped densities can provide an indication of the
relative importance of the inter-particulate interactions affecting a powder's bulking
properties, as these interactions also interfere with powder flow in a given powder. Such a
comparison, such as the Compressibility Index or the Hausner Ratio, was frequently used as
an indicator of the powder's flowability. The propensity of a powder to be compressed as
previously mentioned was measured by the Hausner Ratio and Compressibility Index. They
were therefore measurements of the powder's settling ability and allow for the evaluation of
the relative significance of interparticulate interactions. In a free-flowing powder, such
interactions are less significant, and the bulk and tapped densities will be closer in value. For
poorer flowing materials, there are frequently greater inter-particulate interactions, and a
greater difference between the bulk and tapped densities will be observed[1]. The Hausner
Ratio and the Compressibility Index both show these differences.

3
MATERIAL & METHODOLOGY
● Material
Corn starch, sago seed,tap density instrument

● Methodology

The sample test was filled into the measuring cylinder

↓
The measuring cylinder and the sago seed (granule) were weighed

↓
The measuring cylinder was inserted and locked in the holder

↓
The test would be started by pressing the start key. The elapsed tap and drops per
minute would be shown on the display

↓
After the programmed tap count 1 was over, the tapped volume V1 was measured
and the start key was pressed to continue the test. This was repeated until tap count
4 to get V4

↓
The STOP key was pressed

↓
The procedure was repeated using another material which is corn starch (powders)

4
DATA PROCESSING AND ANALYSIS
𝑀(𝑔)
BULK DENSITY, 𝑉 (𝑚𝑙)

1. SAGO SEED

62.806 𝑔
90.0 𝑚𝑙
= 0. 6978𝑔/𝑚𝑙

2. CORN STARCH

42.919 𝑔
90 𝑚𝑙
= 0. 4769𝑔/𝑚𝑙

𝑀 (𝑔)
TAPPED DENSITY, 𝑉𝑡 (𝑚𝑙)

1. SAGO SEED

62.806 𝑔
85 𝑚𝑙
= 0. 7390 𝑔/𝑚𝑙

2. CORN STARCH

42.919 𝑔
75
= 0. 5723 𝑔/𝑚𝑙

𝑉0− 𝑉𝑓
COMPRESSIBILITY INDEX, 100 × 𝑉0

1. SAGO SEED

90 − 85
100 × 90
= 5. 56 %

2. CORN STARCH

90 −75
100 × 90
= 16. 67%

𝝆𝑇𝐴𝑃
HAUSNER RATIO, 𝐻𝑅 = 𝝆𝐵𝑈𝐿𝐾
1. SAGO SEED

0.7390
0.6978
= 1. 06

2. CORN STARCH
0.5723
0.4769
= 1. 20

5
RESULT

TYPES SAGO SEED CORN STARCH

INITIAL MASS (𝑀0), 𝑔 62.806 42.919

INITIAL VOLUME (𝑉0), 𝑚𝑙 90 90

VOLUME (𝑉1), 𝑚𝑙 85 75

VOLUME (𝑉2), 𝑚𝑙 83 67

VOLUME (𝑉3), 𝑚𝑙 83 66

VOLUME (𝑉4), 𝑚𝑙 - 66

TAPPED DENSITY, 𝑔/𝑚𝑙 0.7390 0.5723

BULK DENSITY, 𝑔/𝑚𝑙 0.6978 0.4769

COMPRESSIBILITY INDEX, % 5.56 16.67

HAUSNER RATIO 1.06 1.20

Table 1 : Result for tapped density, bulk density, compressibility index and Hausner ratio for
granule (sago seed) and powder (corn starch)

6
DISCUSSION
The results of the experiment revealed that the compressibility index and Hausner
ratio of sago seeds are 5.56% and 1.06, respectively. In contrast, the compressibility index
and Hausner ratio for corn starch are 16.67% and 1.20, respectively. According to the United
States Pharmacopeia (USP), there are specified ranges for flow characteristics based on the
compressibility index and Hausner ratio. In this experiment, the results show that the
compressibility index and Hausner ratio of sago seeds fall within the excellent flow character
range. The USP specifies an excellent range for compressibility index as 1-10%, and for
Hausner ratio, it is 1.00-1.11.On the other hand, for corn starch, both the compressibility
index and Hausner ratio fall within the fair flow character range, which is 16-20% and
1.19-1.25, respectively, according to USP specifications. The results for both the granule and
powder are considered acceptable, marking the success of this experiment.

Compressibility index is the Car’s index that has the ability to decrease the volume
under the pressure. The Carr’s index can be calculated by using this formula:

𝑇𝑎𝑝𝑝𝑒𝑑 𝐷𝑒𝑛𝑠𝑖𝑡𝑦 − 𝐵𝑢𝑙𝑘 𝐷𝑒𝑛𝑠𝑖𝑡𝑦

Carr's index = 𝑇𝑎𝑝𝑝𝑒𝑑 𝐷𝑒𝑛𝑠𝑖𝑡𝑦
× 100

Generally, the Hausner ratio is another measure that is related to compressibility. It is

a ratio of tapped density to bulk density and it is calculate by using formula :

𝑇𝑎𝑝𝑝𝑒𝑑 𝐷𝑒𝑛𝑠𝑖𝑡𝑦
Hausner ratio = 𝐵𝑢𝑙𝑘 𝐷𝑒𝑛𝑠𝑖𝑡𝑦

From both of the formulas that have been shown, it is proven that the powder that
can be packed and its compressibility. The higher compressibility index and Hausner ratio
will produce the poor flowability of formulation and greater powder cohesion. Thus, the
uneven filling process equipment of formulation will occur and many processes such as
powder blend and particle size need to be considered again before moving to another step. If
the compressibility and the Hausner ratio is lower in measurement, the flowability can be
improved to have a good flowability and the formulation can move smoothly while in
processing equipment. This can be concluded that if the Hausner ratio is higher, it means that
the cohesiveness of powder is increased but the flowability is decreased.. This resulted in

7
poor flowability on the product. Last but not least, compressibility index, Hausner ratio and
flow character of the powder are relatable to each other as it gives impact on powder
properties. It depends on each other as it is important in ensuring the consistency and
efficiency in manufacturing products.

Tapped density helps to optimise tablet compression. Generally, compression is about

the ability to reduce the volume of the powder by using mechanical strength. It is relatable
with a tapped density as it can produce the consistency of density and hardness when the
powder shows good compressibility.

Tapped density also helps to determine the powder characteristics in the

pre-formulation studies. Powder characteristics such as bulk density and Carr’s index are
helpful to selecting the suitable process and equipment in order to make the formulation of
medicine. It helps the manufacturer to be alert on how the particles of the formulation react in
certain conditions. Thus, any improvement in the formulation can be made to the better
version and optimising the process in order to get the best quality of products.

Lastly, tapped density is an important parameter in manufacturing pharmaceutical

products. One of the main importance of having tapped density in the pre-formulation studies
is to acknowledge the powder of flowability. Flowability is important for the product to move
smoothly through the machines while in progress. It prevents the uneven amount in the
formulation from occurring. Tapped density generally helps to determine the quantity of
formulation to pack the tablets or capsule efficiently ensuring the consistency in dosage.
Tapped density also can be measured by using the Hausner ratio. If the Hausner ratio is
higher, it means that the cohesiveness of powder is increased but the flowability is decreased..
This resulted in poor flowability on the product and thus, rejecting it.

8
CONCLUSION
In conclusion, the experiment focused on evaluating the tap density, bulk density,
compressibility index, and Hausner ratio of sago seed and corn starch.Flow Characteristics:
Sago seed demonstrated superior flow characteristics compared to corn starch, evident from
its lower compressibility index (5.56%) and Hausner ratio (1.06). These values fall within the
excellent flow character range according to USP standards. Conversely, corn starch exhibited
higher compressibility index (16.67%) and Hausner ratio (1.20), suggesting fair flow
characteristics.Pharmaceutical Significance: Understanding tap density is crucial in
pharmaceutical manufacturing. It directly influences the formulation's flowability, impacting
the efficiency and consistency of manufacturing processes. This knowledge aids in
optimising tablet compression and ensuring dosage consistency.Interpretation of Results: The
experiment's results align with the expected ranges specified by the United States
Pharmacopeia, validating the quality assessment of sago seed and corn starch for their
intended pharmaceutical applications.Relationship Between Properties: Compressibility
index and Hausner ratio serve as indicators of powder flowability and cohesion. Higher
values indicate poor flowability and increased powder cohesion, affecting the manufacturing
process and formulation characteristics.Optimization and Quality Assurance: Tap density
measurements assist in pre-formulation studies, guiding the selection of suitable processes
and equipment. They enable manufacturers to understand powder behaviour under various
conditions, allowing for formulation improvements and process optimization.In essence, tap
density determination plays a pivotal role in ensuring the quality, efficiency, and consistency
of pharmaceutical formulations. The experiment's results and analysis shed light on the
crucial relationship between powder properties and their implications in pharmaceutical
manufacturing processes, highlighting the significance of tap density assessments in the
formulation of high-quality pharmaceutical products.

9
REFERENCES

1. Method II-Measurement in a Volumeter. (n.d.).

https://www.usp.org/sites/default/files/usp/document/harmonization/gen-chapter/bulk
_density.pdf

2. Neveu, A. (2023, June 5). POWDER CHARACTERISATION FOR

PHARMACEUTICALS: BEYOND STANDARDS. ONdrugDelivery.
https://www.ondrugdelivery.com/powder-characterisation-for-pharmaceuticals-beyon
d-standards/

3. Evaluating the powder testing toolkit: Tapped density. (2019, August 28). LinkedIn.

https://www.linkedin.com/pulse/evaluating-powder-testing-toolkit-tapped-density-tim

-freeman (Accessed on 8 December 2023)

10
APPENDICES

11