REPORT

ON

INDUSTRIAL TRAINING
AT

ASHWIN FINE CHEMICALS &

PHARMACEUTICALS

IN THE YEAR 2014

Submitted by-

MR. MAKRAND ASHOK TORASKAR

Seat No: 968
MSc II, Semester IX

Five Year Integrated Course in Bioanalytical

Sciences

Ramnarain Ruia College

INDUSTRIAL TRAINING REPORT

ASHWIN FINE CHEMICALS AND PHARMACEUTICALS

RAMNARAIN RUIA COLLEGE

DEPARTMENT OF BIOANALYTICAL
SCIENCES
THIS IS TO CERTIFY THAT
Ms. /Mr. _____________________________________ OF THE
M.Sc.

II

CLASS

HAS

SATISFACTORILY

COMPLETED

THE

INDUSTRIAL TRAINING OF _____________________ WEEKS AT

__________________________________________________
BETWEEN__________________________________________
TOWARDS THE PARTIAL FULFILMENT OF THE M.Sc. DEGREE IN
BIOANALYTICAL SCIENCES, UNIVERSITY OF MUMBAI.

COURSE COORDINATOR

HEAD OF DEPARTMENT

DATE OF CERTIFICATION: _________

COLLEGE SEAL

INDEX

SR. No.

TITLE

PAGE NO.

1.

Acknowledgement

2.

Learning Objective

3.

Company Profile

4.

Instrumentation Observed

5.

Analysis Observed

5.1

Ayurvedic Products : Alcoholic

11

5.2

Ayurvedic Products : Non-Alcoholic

20

5.3

Raw Materials

26

5.4

External Products

32

5.5

Repacking

43

6.

Chemical Assays & Tests

53

7.

Work Done

56

8.

Learning Outcome

59

References

60

ACKNOWLEDGEMENT

It has been a privilege to be a part of Ashwin Fine Chemicals & Pharmaceuticals as student
trainee. My sincere appreciation goes to the management of Ashwin Fine Chemicals &
Pharmaceuticals for their support throughout the training period.
I would like to thank Dr. Suhas Pednekar (Principal, Ramnarain Ruia College) for always
supporting us in all our endeavours.
I would like to thank Mrs Dhanashree Kulkarni (Course coordinator Bioanalytical
Sciences, Ramnarain Ruia College) for her love, support, guidance and for providing me with
this wonderful opportunity.
I would like to thank Mr. Sachin Palekar, as its the synergy of all that he had taught that
made this training meaningful.
I sincerely thank Mr. Keshav Karania (Managing Director, Ashwin Fine Chemicals &
Pharmaceuticals) for approving this proposal of training.
I thank all the QC chemists (Mrs. Pallavi Gawas & Ms. Satyavati Pawar) for giving me the
actual practical training and in depth knowledge.
My sincere thanks to each one of them for sharing their experiences, knowledge and making
my training worthwhile.

LEARNING OBJECTIVES

The main aim behind the Industrial Training program was to experience and understand
the applications of principles of Bioanalytical Sciences into Industrial organizations and their
related environments.

To acquire knowledge, hands-on experience and the necessary skills required in the

analytical and application science that harbours the world of testing laboratories and
analytical services.

As a student my learning objective was to, work and learn the different types of
analysis done and the analytical tools used for that in this organization. To acquire skills
in safety practices carried out in this organization & also may have the chance to develop
skills include: operating an analytical instrument, handling a variety of situations
simultaneously, organizing or analyzing data, records, improving teamwork, writing, and
speaking abilities & also to discover the job opportunities available in this field.

ABOUT ASHWIN FINE CHEMICALS & PHARMACEUTICALS

Ashwin Fine Chemicals & Pharmaceuticals is based at Thane, (MAHARASHTRA) and

has been involved in Manufacturing & Exporting of various Ayurvedic & Allopathic
products. Their range comprises of Cough Syrup, Pain Relief Oil, Rose Water, Mustard Oil
and many more. One can get all the varieties of Ayurvedic Essential Oils and Natural Herbal
Oil at ASHWIN. We have been issued with GMP Certification (Schedule M & Schedule T)
by Food & Drug Administration, Maharashtra which makes us one of the most trusted Cough
Syrup Exporters and Suppliers from India.
Currently the company is serving to the various international markets, but having a vision to
serve the whole world. We value our customers. Serving for the more than three decades we
experienced customer expectations, and serving them according to their wants. We excel in
the field of Ayurvedic, and Allopathic formulations.
Ashwin Fine Chemicals & Pharmaceuticals is dealing in the Manufacturing and Exporting of
Ayurvedic & Allopathic formulations since 1977. Its more than three decades that they are in
the field and continually satisfying the customers. Mr. Keshav Karania, the CEO of the
company, has started the company with the vision to serving mild & pure cure to the world.
Only due to his dedication towards the vision, they are holding a position among the top five
companies in the same sector, across the world. They supply Pharmaceutical Oil (especially
Herbal Hair Oil) which is further used by different pharmaceutical firms in production
process of various medicines. They are known as one of the pure Almond Oil Manufacturers
all over India.

Milestone
They are serving best Ayurvedic & Allopathic solutions to the society; they have received a
Certificate for our Quality Products from FDA, Maharashtra.

Infrastructure
They are having a huge plant for our process, which is well equipped with high-tech &
productive machineries. Due to these high productive machineries they are able to meet
demand in the market place.

Specialization
They are highly specialized in manufacturing of the Ayurvedic & Allopathic formulations.
Our specialization lies in the fact that they use only premium raw material for products
manufacturing.
3

Clientele
Due to these dedicated efforts towards quality management, they have been able to establish a
whopping list of satisfied clients. Currently, they are serving clients from USA, UK,
Mauritius, Reunion Islands, Various African countries, Australia, South African markets
including Indian market.

NAME OF CEO

MR. KESHAV KARANIA

ESTABLISHMENT YEAR

1977

PRIMARY BUSINESS TYPE

MANUFACTURER & EXPORTER

NUMBER OF EMPLOYEES

60

MARKETS COVERED

USA, UK, Mauritius, Reunion Islands,

Various African countries, Australia &
South Africa

PRODUCT PORTFOLIO
Manufacturer & Exporter of Ayurvedic & Allopathic medicines, formulations, natural
essential oils and other product.
ALLOPATHIC MEDICINES:
Benzyl Benzoate IP
Merbromin Solution Nf Xii Mercurochrome
(Solution 2% W/V)
Tannic Acid Glycerin
Borax Glycerin
Turpentine Liniment
Hydrogen Peroxide Solution IP/USP/BP
Compound Benzoin Tincture IP
Iodine Tincture USP
Aromatic Spirit Of Ammonia BP
Ichthamol Glycerin BPC
Povidone Iodine Solution IP (5%/10% W/V)

Gentian Violet Solution

Surgiclin Clinical Spirit (Isopropyl Rubbing
Alcohol USP)
Acriflavine Solution
Calamine Lotion IP
Cresol With Soap Solution IP
Chloroform Spirit BP
Mandls Paint BPC68
Sodium Hypochlorite Solution USP
Turpentine Liniment BP93
Lindane Lotion USP
Glycerin Oral Solution USP

NATURAL ESSENTIAL OILS/ AROMATIC OILS:

Neem Oil
Camphor Oil
Mustard Oil
Ajowen Oil

Clove Oil
Eugenol
Eucalyptus Oil
Cotton Seed Oil

Citronella Oil
Cassia Oil
Caraway Oil
Cumin Seed Oil

Lemon Oil
Lemon grass Oil
Nutmeg Oil
Olive Oil
4

AYURVEDIC PRODUCTS / HERBAL PRODUCTS:

Rose Water
Maha Narayan Tel
Adulsa Syrup
Gulkand
Ashwins Pain Balm
Kumari Asav-1
Kumari Asav-3
Balant Kadha-1
Cegarwood Oil
Palmarosa Oil
Basil Oil
Lavender Oil
Chamomile Oil
Geranium Oil

Balant Kadha-2
Balant Kadha-3
Balkadu
Castor Oil
Erandel Tel
Glycerin with Rose Water
Wheat germ Oil
Creosote
Rosemary Oil
Coriander Oil
Vetiver Oil
Tilseed (Sesame) Oil
Linseed Oil
Sandalwood Oil

REPACKING PRODUCTS:

Acetyl Salicylic Acid IP

Acriflavin BP, Acacia I
Boric Acid IP/BP
Castor Oil IP/BP
Cetrimide IP
Iodoform Nf/BP
Light Magnesium Carbonate IP
Magnesium Sulphate IP
Methyl Salicylate IP
Turpentine Liniment IP
66Petroleum Jelly White IP(White Soft
Paraffin)
Zinc Oxide IP
Benzyl Benzoate IP
Emulsifying Wax IP
Olive Oil BP
Ichthamol IP 66
Sodium Benzoate IP
Light Liquid Paraffin IP

Ammonium Bicarbonate IP
Ammonium Carbonate IP
Calcium Carbonate IP
Calamine IP
Cinnamon Oil IP
Glycerin IP / BP / USP
Kaolin Light IP, Kaolin Nf
Liquid Paraffin IP
Potassium Permanganate IP
Potassium Chloride IP
Petroleum Jelly Yellow IP (Yellow Soft
Paraffin)
Salicylic Acid IP
Sodium Bicarbonate IP
Turpentine Oil IP 66 / BP
Talc IP
Phenol IP
Acetone IP
Magnesium Sulphate BP

QUALITY CONTROL & SAMPLING PROCEDURE

Quality Control is that part of GMP, which is concerned with sampling, specification and
testing, and with the organization, documentation and release procedures, which ensure that
the necessary and relevant tests are, in fact, carried out, and that materials are not released for
use, nor products released for sale or supply, until their quality has been judged to be
satisfactory.
It involved the examination of a raw material, process product, for certain minimum levels of
quality. The goal of a quality control team was to identify products that do not meet a
companys specified standards of quality. If a problem was identified, the job of a quality
control team or professional may involve stopping production temporarily.
Quality control department is backbone of the industry. It not only gives assurance of
required quality in given product through various analytical techniques but also faces audits
conducted by customers, so a strong quality control department indicates higher quality in its
product.
Sampling procedures depends on the nature of the raw material, in process or finished
product lots, conveying and sampling equipment. Prior knowledge of the product data and
sampling resources allows the assignment of the appropriate sampling procedures. The use of
recognized international sampling methods ensures a standardized administrative and
technical approach and facilitates the interpretation of results of analysis related to lots.
Colour code system:Red label: Raw material is rejected
Yellow label: Raw Material under test
Green label: Raw material is approved
Sampling is done in a well defined area in order to avoid difficulties in the executing of
procedures, reduce the risk of contamination and cross contamination, enable the proper
execution of laboratory analysis and include all necessary safety and health precautions to the
sampler and environment.
For the execution of the sampling procedures proper tools and materials are available.
Personnel responsible for the sampling activities are trained on the applicable procedures. All
tools and auxiliary materials are inert, and in a clean condition before and after their use.
Rule of sampling - when there are more than 5 containers of raw material, the number of
container sampled is determined by following formula

Where, N=number of containers.

6

Quantity of sample to be sampled There are number of factor which determine the amount
of sample to be sampled. They are amount required for analysis, cost of material.
Samplings of solid Solid samples are sampled by using bigger size spatula or sampling
cork.
Sampling of Liquid-Liquid samples is sampled by using sampling rod.
Before going for sampling analyst sees GRN slip given by warehouse to see what to be
sampled & accordingly labels of Under Test, labels of sampled by should be prepared. The
sampling form is filled during sampling. Once the sampling is done analyst sticks under test
label to all the containers. Once sample is analyzed and approved then approved label is put
on. If sample is analyzed and fails to pass all the tests given in its SOP of analysis then the
rejected label is put on the container.

INSTRUMENTS OBSERVED

1. KARL FISHER TITRATOR

Karl Fischer titration is a classic titration method in analytical chemistry that uses
colorimetric or volumetric titration to determine trace amounts of water in a sample. It was
invented in 1935 by the German chemist Karl Fischer.

Colorimetric titration
The main compartment of the titration cell contains the anode solution plus the analyte. The
anode solution consists of an alcohol (ROH), a base (RN), SO2 and I2. A typical alcohol that
may be used is methanol or diethylene glycol monoethyl ether, and a common base is
imidazole.
The titration cell also consists of a smaller compartment with a cathode immersed in the
anode solution of the main compartment. The two compartments are separated by an ionpermeable membrane.
The Pt anode generates I2 when current is provided through the electric circuit. The net
reaction as shown below is oxidation of SO2 by I2. One mole of I2 is consumed for each mole
of H2O. In other words, 2 moles of electrons are consumed per mole of water.
CH3OH + SO2 + RN [RNH] SO3CH3
H2O + I2 + [RNH] SO3CH3 + 2RN [RNH] SO4CH3 + 2 [RNH] I
(RN = Base)
The end point is detected most commonly by a bipotentiometric method. A second pair of Pt
electrodes is immersed in the anode solution. The detector circuit maintains a constant current
between the two detector electrodes during titration. Prior to the equivalence point, the
solution contains I but little I2. At the equivalence point, excess I2 appears and an abrupt
voltage drop marks the end point. The amount of current needed to generate I2 and reach the
end point can then be used to calculate the amount of water in the original sample.

Volumetric titration
The volumetric titration is based on the same principles as the coulometric titration except
that the anode solution above now is used as the titrant solution. The titrant consists of an
alcohol (ROH), base (B), SO2 and a known concentration of I2.
One mole of I2 is consumed for each mole of H 2O. The titration reaction proceeds as above
and the end point may be detected by a bipotentiometric method as described above.
8

Advantage of analysis
The popularity of the Karl Fischer titration is due to several practical advantages that it holds
over other methods of moisture determination, including:
1
High accuracy and precision
2
3
4
5
6
7
8
9

Selectivity for water

Small sample quantities required
Easy sample preparation
Short analysis duration
Nearly unlimited measuring range (1ppm to 100%)
Suitability for analyzing:
Solids

Liquids
10
Gases
11
Independence of presence of other volatile compounds

12

Suitability for automation

In contrast, loss on drying will detect the loss of any volatile substance.
The major disadvantage is that the water has to be accessible and easily brought into
methanol solution. Many common substances, especially foods such as chocolate, release
water slowly and with difficulty, and require additional efforts to reliably bring the total water
content into contact with the Karl Fischer reagents.

2. pH METER

A pH meter is a handheld device that tests water for its level of acidity versus base
or alkalinity. If water is equally acidic and alkaline, it registers as neutral on a pH
meter. The pH meter utilizes a standard pH scale for
measuring these aspects of
water quality. The level of concentration of positive hydrogen ions in the water
determines the result. The acidic side of the pH scale runs from 0 to 6.9, with 7.0
being neutral. Because 7.0 is neutral, 6.8 is considered only slightly acidic. Similarly,
7.2 is only slightly alkaline, with the base scale running to 10.0 or higher. Generally
speaking, acidic water is soft while alkaline
or base water is hard.
9

PRINCIPLE:
A pH meter measures essentially the electro-chemical potential
between a known
liquid inside the glass electrode (membrane) and an unknown liquid outside. Because
the thin glass bulb allows mainly the agile and small hydrogen ions to interact with
the glass, the glass electrode measures the electro-chemical potential of hydrogen ions
or the potential of hydrogen. To complete the electrical circuit, also a reference
electrode is needed. Note that the instrument does not measure a current but only an electrical
voltage, yet a small leakage of ions from the reference electrode is needed, forming a
conducting bridge to the glass electrode. A pH meter must thus not be used in moving liquids
of low conductivity (thus measuring inside small containers is preferable).
The calomel reference electrode consists of a glass tube with a potassium chloride (KCl)
electrolyte which is in intimate contact with a mercuric chloride element at the end of a KCL
element. It is a fragile construction, joined by a liquid junction tip made up of porous ceramic
or similar material. This kind of electrode is not easily poisoned by heavy metals and
sodium.
The glass electrode consists of a sturdy glass tube with a thin glass bulb welded to
it. Inside is a known solution of potassium chloride (KCl) buffered at a pH of 7.0. A
silver electrode with a silver chloride tip makes contact with the inside solution. To minimise
electronic interference, the probe is shielded by a foil shield, often found inside the glass
electrode.

Calibration of pH METER:
For normal use calibration should be performed at the
reason for this is that the glass electrode does not give
longer period of time.

beginning of each day. The

a reproducible e.m.f. Over a

PROCEDURE:
1
2
3

Switch on pH METER.
Allow the pH METER to attend temperature around 21C.
The glass electrode is rinsed with distilled water and wiped with clean tissue
paper.

4
Use standard solution of buffer 4.00, 7.00, 9.20 respectively.
Immersed the glass electrode in standard buffer solution with intermittent
washing with distilled water.
1
Keep the record of reading into the log book of pH METER
Note :- Glass electrode tip must be kept wet at all times.

10

AYURVEDIC PRODUCTS: ALCOHOLIC

1.
2.
3.
4.

BALANT KADHA NO. 1

BALANT KADHA NO. 2
BALANT KADHA NO. 3
BALKADU

INFORMATION ON BALANT KADHA

Basically, Balant Kadha, as names suggest are for Post Delivery care of our body, as it has
undergone lot of changes in past 9 months & we have to bring it to normal in natural &
systematic way. This Balant Kadha nos. suggests that when they should be taken based on
their actions.
Balant Kadha No-1 should be taken in the first ten days as it has specific action to control
vata which has been increased as a result of excess space in uterus after delivery. Hence
controlling vata as well as to clean & purify uterus are the main functions.
Balant Kadha No-2 generally should be taken between 10th -20th day which helps in
restoration of uterus and providing strength to the uterus as well as entire body. Decreasing
vata is obviously is done by this kadha also.
Balant Kadha No-3 from 20th day to 60th day, aims more on generalized body then specific
part of the body like regularizing motions, increasing appetite & proper Digestion, Lactation
& providing various supplements like iron, calcium etc.

TESTING OF KADHAS (INHOUSE METHOD/ PROTOCOL)

All the kadhas are tested in Ashwin fine chemicals are performed with reference to the Ayu
Sara Sangraha; there are 3 types of tests conducted
1
2
3

pH
Specific gravity
Alcohol content.

11

BALANT KADHA NO.1

Product Description & Composition (as on package)
Composition: Each 10 ml contains.
CONTENTS
Salaparni

AMOUNT OF
MATERIAL
PRESENT
418.910 gms

Prsniparmi

418.910 gms

Brhati

418.910 gms

Kantakari

418.910 gms

Goksura

418.910 gms

Bilva

418.910 gms

Agnimantha

418.910 gms

Syonka

418.910 gms

Ghambari

418.910 gms

Patala

418.910 gms

Guda

3.273 gms

Dhataki

3.2727 mg

Asava base

3.2727 mg

Balant Kadha No.1 contains decocation of dashmool which are well known herbs for
overcoming post pregnancy weakness.
1
It helps to relieve weakness due to excessive bleeding & increases lactation.
2
Regular intake of this helps to increase appetite.
3
It helps to relieve constipation, cough and gives & Strength. Its an excellent
tonic for the first 10 days after delivery.
4
Balant Kadha No.2 is to be taken next.

12

RESULT
1 OF ANALYSIS FOR BALANT KADHA NO.1
SPECIFIC GRAVITY at RT:
Weight of Bottle: 21.7148 gms
Weight of Bottle + Water: 46.4664 gms
Weight of Water: 24.7516 gms
Weight of Bottle + Sample: 46.4184 gms
Weight of Sample: 24.7036 gms
Weight of Sample = 24.7036 gms = 0.9981 (limit 0.9930 to 1.0300)
Weight of Water 24.7516 gms

ALCOHOL CONTENT at
25 C Weight of pycnometer =
41.5140 gms
Weight of pycnometer + water = 65.2659 gms
Weight of water = 23.7519 gms
Weight of pycnometer + sample = 65.2126 gms
Weight of sample: 23.6986 gms.
Weight of sample = 23.6986 = 0.9976
Weight of water 23.7519
Using alcohol content reading chart at 25 C
I.e. 1.60 x 4 = 6.40 % (limit NMT 12.0 % W/V)
(By comparing above specific gravity value using Alcohol content chart)

pH: 4.51

(limit : 3- 5)

13

BALANT KADHA NO.2

Product Description & Composition (as on package)
Composition: Each 10 ml contains.
CONTENTS
AMOUNT OF
MATERIAL PRESENT
Devadaru
204 mg
Vaca

204 mg

Kustha

204 mg

Pippali

204 mg

Sunthi

204 mg

Katphala

204 mg

Musta

204 mg

Kiratatikla

204 mg

Katuka

204 mg

Dhanyaka

204 mg

Goksura

204 mg

Dhanvayasa

204 mg

Brhati

204 mg

Ativisa

204 mg

Guduci

204 mg

Kartkatasmgi

204 mg

Krsna Jiraka

204 mg

Dhatak

204 mg

Asav Base

3.2727 mg

1
2
3

This is to be taken from the eleventh day after delivery.

It is an excellent tonic for post delivery.
It helps to relieve complications that occur after delivery like Constipation,
Weakness etc.
4
It helps to give all types of nutrition to infants through mothers milk. This
Kadha should be taken regularly for 10 days.
5
Is taken regularly for 10 days.
6
Balant Kadha No.3 is to be taken next.

14

RESULT
1 OF ANALYSIS FOR BALANT KADHA NO.2
SPECIFIC GRAVITY at RT:
Weight of Bottle = 21.7167 gms
Weight of Bottle + Water = 46.4538 gms
Weight of Water = 24.7371 gms
Weight of Bottle + Sample = 47.0694 gms
Weight of Sample = 25.3527 gms
Weight of Sample = 24.3527 gms = 1.0249 (limit 0.9930 to 1.0300)
Weight of Water
24.7371 gms

ALCOHOL CONTENT at
25 C Weight of pycnometer =
41.5140 gms
Weight of pycnometer + water = 65.2659 gms
Weight of water = 23.7519 gms
Weight of pycnometer + sample = 65.2168 gms
Weight of sample = 23.7028 gms.
Weight of sample = 23.7028 = 0.9979
Weight of water
23.7519

Using alcohol content reading chart at 25 C I.e.

1.40 x 4 = 5.60 % (limit NMT 12.0 % W/V)
(By comparing above specific gravity value using Alcohol content chart)

pH: 4.56

(limit : 3- 5)

15

BALANT KADHA NO.3

Product Description & Composition (as on package)
Composition: Each 10 ml contains.
CONTE AMOU
NTS
NT OF
MATERIAL
PRESENT
Sunthi
255.696 mg
VIdanga
255.696 mg
Pippalimula
255.696 mg
Guduci
255.696 mg
Dhanvayasaka
255.696 mg
Devadaru
255.696 mg
Kantakari
255.696 mg
Musta
255.696 mg
Erandmula
255.696 mg
Bhringaraja
255.696 mg
Punarnava
255.696 mg
Dhataki
255.696 mg
Asava base
Q.S

1
2

st

This is to be started Kadha from 21 day from delivery.

Regular intake of Kadha No.3 helps to tone up the blood circulation and
formation of new blood cells.
3
It helps to maintain Vitality, Energy & Strength of the body.
4
It also helps to relieve complications that occur due to worms.
5
It is an excellent tonic for both mother and infant.

16

RESULT
1 OF ANALYSIS FOR BALANT KADHA NO.1
SPECIFIC GRAVITY at RT:
Weight of Bottle: 21.7148 gms
Weight of Bottle + Water: 46.4664 gms
Weight of Water: 24.7516 gms
Weight of Bottle + Sample: 46.4447 gms
Weight of Sample: 24.7299 gms
Weight of Sample = 24.7299 gms = 0.9991 (limit 0.9930 to 1.0300)
Weight of Water 24.7516 gms

ALCOHOL CONTENT at
25 C Weight of pycnometer =
41.5140 gms
Weight of pycnometer + water = 65.2659 gms
Weight of water = 23.7519 gms
Weight of pycnometer + sample = 65.2037 gms
Weight of sample: 23.6897 gms.
Weight of sample = 23.6897 = 0.9974
Weight of water 23.7519
Using alcohol content reading chart at 25 C
I.e. 1.74 x 4 = 6.96 % (limit NMT 12.0 % W/V)
(By comparing above specific gravity value using Alcohol content chart)

pH: 3.6

(limit : 3- 5)

17

BALKADU KADHA
Product Description & Composition (as on package)

CONTENT
Adulsa
Brahmi
Jeshtmadh
Vavding
Lakadi revachini
Gulabkali
Nishottar
Kakadshingi
Bakana nimb
Indrajav
Raktachandan
Ativish
Manjishta
Murusheng
Kutki
Akkalkadha
Kapashipala
Shivanmool
Chiknamool
Pittapapada
Lodhra
Maiphal
Chitrak
Kirmani ova

Composition each 5 ml contains

AMOUNT
OF CONTENT
MATERIAL
PRESENT
57.00 mg
Kale miri
66.45 mg
Shuddha Kuchala
5.95 mg
Sagargota magaj
49.60 mg
Kapila
3.55 mg
Dhaitiphool
3.55 mg
Arjunsal
3.55 mg
Kudasal
4.20 mg
Unhali
3.00 mg
Dalimb
3.55 mg
Survari harda
3.00 mg
Balharda
3.55 mg
Avalkathi
1.50 mg
Behada
1.50 mg
Kath
1.50 mg
Kala boal
1.50 mg
Vanshlochan
1.50 mg
Samudrafen
0.75 mg
Takankhar
0.75 mg
Draksha
0.75 mg
Mohaphool
0.75 mg
Nagarmotha
1.206 mg
Vekhand
3.00 mg
Upalsari
2.40 mg
Chavak

AMOUNT
MATERIAL
PRESENT
1.50 mg
1.50 mg
1.50 mg
5.95 mg
24.35 mg
3.00 mg
2.40 mg
0.75 mg
1.50 mg
7.10 mg
4.75 mg
2.40 mg
7.10 mg
1.50 mg
1.00 mg
1.50 mg
1.50 mg
3.00 mg
125.60 mg
24.35 mg
4.75 mg
3.00 mg
3.00 mg
3.00 mg

OF

A time-tested Ayurvedic Health restorative for

infants. Tones up metabolism. Protects infants
from digestive complaints like flatulence, colic
diarrhoea, vomiting etc.
Direction of Use
Dose: 5 to 10 drops according to age, thrice a
day with a little warm water. Self generated
Alcohol not more than 9.5 % v/v.

18

RESULT
1 OF ANALYSIS FOR BALKADU
SPECIFIC GRAVITY at RT:
Weight of Bottle = 21.7148 gms
Weight of Bottle + Water = 46.4664 gms
Weight of Water = 24.7516 gms
Weight of Bottle + Sample = 46.5968 gms
Weight of Sample: 24.8820 gms
Weight of Sample = 24.8820 gms = 1.0053 (limit 0.9930 to 1.0300)
Weight of Water
24.7516 gms

ALCOHOL CONTENT at
25 C Weight of pycnometer =
41.5140 gms
Weight of pycnometer + water = 65.2659 gms
Weight of water = 23.7519 gms
Weight of pycnometer + sample = 65.2209 gms
Weight of sample: 23.7069 gms.
Weight of sample = 23.7069 = 0.9981
Weight of water
23.7519
Using alcohol content reading chart at 25 C.
I.e. 1.27 x 4 = 5.08 % (limit NMT 12.0 % W/V)
(By comparing above specific gravity value using Alcohol content chart)

pH: 4.33

(limit : 3- 5)

19

AYURVEDIC PRODUCT: NON ALCOHOLIC

1.
2.
3.
4.

MAHANARAYAN TAILA
NARAYAN TAILA
ERANDEL TEL
KALONJI TEL

TAILA
Taila are preparations in which taila is boiled with prescribed kasayas (Decoction) & kalkas
of drugs according to the formula this process ensure absorption of the active therapeutic
properties of the ingredient used.
General method of preparation:
There are generally three essential for preparation of sneha(gharta or taila)
Drava (a liquid which may be one more as kasaya, svarasa, dugdha, mastu .etc)
Kalka (a fine paste of the drugs)
Sneha, Dravyas (taila, murcchita taila etc.)
Generally unless otherwise mentioned in the text if kalka is the one part by weight Sneha,
should be four parts and Drava- Dravya should be sixteen parts exceptions are,
1

Where the
no weight
Drava of
is the
prescribed
fourth
sneha. four part of water is added to one part of sneha, the kalka is the one

Where Drava-Dravya is kwatha kalka should be one sixth of sneha

Where
Drava
Dravya
swarasa,
ksira, takra, dadhi the kalka should be one-eighth of the sneha and
four times
water
is addedisfor
good Paka.

Where
the number Dravyas is four or less than four, each dravya has to be taken four times the weight
of sneha.

Where the Drava Dravyas are five or more, each dravya will be equal in weight to
the sneha.

If in a preparation, no kalka dravya is prescribed, then the drugs of the kasaya may be used as
kalka.
The kalka are the dravya are mixed together, sneha is added to the boiled and mild fire and
stirred well continuously so that the kalka is not allowed to adhere to the vessel. Sometimes
the Drava- Dravyas are direct to be added one after another as the process of boiling is
continued till the Drava-Dravyas added earlier has evaporated.
When all the Drava-Dravaya has evaporated the moisture in the kalka will also begin to
evaporate at this stage, it has to be stirred more often and the carefully to ensure that the
kalka does not stick to the bottom of the vessel. The kalka is taken out of the ladle and tested
from time to now the condition and stage of the Paka.
20

1
There
are threeMrdu
stagespaka
of Paka.
2

Madhyam Paka
Khara Paka

In mrudu paka, kalka is waxy and when rolled between fingers rolls like lac without sticking.
In Madhyam Paka, kalka is harder and when put in fire burns without any cracking noise a
further degree of heating lead to khara Paka. Any further heating will lead to dagdha paka and
the sneha becomes unfit for use when the taila attains the correct paka stage froth comes out.
In the sneha group savkara, if mentioned is added in fine powder form to the final product
when cool.
Where the Parka is to be done with kwacha, svarasa, dugdha & mamsarasa, etc. the Paka is to
be done
with the dravas separately in the above order. The period of paka with various
1 should
Dravyas
be below.
Kvatha,
aranata, takra, etc 5 days
2

Svarasa etc 3days

Dugdha etc 2 days

Mamsarasa etc 1day.

CHRACTERISTICS of Taila:
Taila will generally have the color, odor, & tastes of drugs used & have the consistency of the
oil. When considerable quantity of milk is used in the preparation; the oil becomes thick due
to Ghrita & in cold season may condense further.

PRESERVATION:
Taila are preserved in the glass, polythene or aluminium containers. Preparations for internal
use help their potency for about sixteen months.

METHOD OF USE:
Tailas are generally used for abhyanga, some of them are also used externally & in ayurvedic
texts various types of anupanas are described for this purpose. When no such anupana is
mentioned it should be taken with warm water or warm milk

21

MAHANARAYAN TAILA
Contents of Mahanarayan Taila:
It contains the following ingredients Bilva, Asvagandh, Brhati, Svadamstra(goksura),
Syonaka, Vatyaleka, Paribhadra, Ksudra(rakta punarnava), Alibala, Agnimatha, Savarni,
Patali, Water for decoction, Taila (tila), Aja dugdha / go dugdha, Satavari rasa, Rasna,
Asvagandha,Misi(misery), Daru (devdaru), Kushtha, Salaparni, Prsniparni, Mudgaparni,
Masaparni, Agav, Ksura(nagaksura), Sindhutha (saindhara lavana), Mamsi (jatamasi),
Haridra, Davaharidra, Saileya, Chandana(rakta chandana), Puskara,Ela(sukmaila), Asra
(manjishta), YastiTagara, Abdu (musta), Patra(tejapatra), Bhringa(twak), Jivaka, Rashaka,
Meda, Mahameda, Kakoli, Kijira kakaoli, Riddhi, Vruddhi, Arbu, Vaca, Palasa, Sthauneya,
Vrsuraka, Corcka, Karpura, Kasmira(kumkum), Mrgandja(mrgamda).

DOSAGE:
6 gms used externally for nasya, abhyanga & anuvasana

ANUPANA: Milk and warm water.

IMPORTANT THERAPUETIC USE:

Ardita, badhiratva, pangutva, gatra kampa, manya stambha, hanu stambha, ekanga,
vadhayatva, siroruja, jivha stambha, dantasula, unmade, kubja. snayu bhagna, asthi bhagna.

22

RESULT
1 OF ANALYSIS FOR MAHANARAYAN TAILA
SPECIFIC GRAVITY:
Weight of Pycnometer = 41.5140 gms
Weight of Pycnometer + Water = 65.2659 gms
Weight of water = 23.7579 gms
Weight of Pycnometer + sample = 63.3388gms
Weight of Sample = 21.8248 gms
Weight of Sample x 0.99602
Weight of Water
21.8248 x 0.99602 = 0.9152 (limit =0.9050 to 0.9180)
23.7579

ACID VALUE:
Sample taken: 2.0056 gms
Burette Reading: 1.57 ml

1.57 x 5.61 x 0.1054 = 4.63 (limit = NMT 8.0)

0.1 x 2.0056

SAPONIFICATION VALUE :
Sample taken: 2.0610 gms
Blank Burette reading: 21.3 ml
Test Burette reading: 7.5 ml
Difference between readings: 13.8 ml.
13.8 x 28.05 x 0.5243 = 189.99 (limit =185 to 200)
0.5 x 2.0610

23

NARAYAN TAILA
Contents of Narayan taila:
CONTENTS
Bilva
Agnimantha
Syonaka
Patala
Prasarani
Asvagandha
Brhati
Katakori
Bala
Alibala
Svadamsta(goksura)
Water for decoction
Taila
Satapuspa
Devadaru
Mamsi(jatamansi)
Saileyeka
Naca
Chandana(rakta
chandana)
Tagara
Kushta
Ela( Suchamaila)
Salparni
Prsniparni
Mudgaparni
Masaparni
Rasna
Turagagandha
Saindharava
Punarana
Satavarasa
Go dughdha

AMOUNT
USED
480 mg
480 mg
480 mg
480 mg
480 mg
480 mg
480 mg
480 mg
480 mg
480 mg
480 mg
49.152 l
3.072 Kg
96 mg
96 mg
96 mg
96 mg
96 mg
96 mg
96 mg
96 mg
96 mg
96 mg
96 mg
96 mg
96 mg
96 mg
96 mg
96 mg
96 mg
3.072 l
2.288 l

DOSAGE: 6 gms used externally for abhaynaga, nasya & anuvasana also.
IMPORTANT THERAPUETIC USAGE: Vata roga , pangu, sirogata vata, manyastambha,
hanustambha, danta roga, galagraha, ekaanga sosa, kumpa, ksinendriya, ksina sukara,
badhivya, lailajihavata, medalpata anda suta, antra vrddhi
24

RESULT OF ANALYSIS FOR NARAYAN TAILA

SPECIFIC GRAVITY:
Weight of Pycnometer = 34.4247 gms
Weight of Pycnometer + Water = 59.6733 gms
Weight of water = 25.2536 gms
Weight of Pycnometer + sample = 57.6271gms
Weight of Sample = 23.2024 gms
Weight of Sample x 0.99602
Weight of Water
23.2024 x 0.99602 = 0.9151 (limit =0.9050 to 0.9180)
25.2536

ACID VALUE:
Sample taken: 2.0077 gms
Burette Reading: 1.45 ml

1.45 x 5.61 x 0.1034 = 4.19 (limit = NMT 6.0)

0.1 x 2.0077

SAPONIFICATION VALUE
Sample taken: 2.0518 gms
Blank Burette reading: - 21.6 ml
Test Burette reading: 8.2 ml
Difference between readings: 13.4 ml.
13.4 x 28.05 x 0.5132 = 188.02 (limit =185 to 200)
0.5 x 2.0518

25

RAW MATERIALS
IODINE USP
9.

SAMPLING
1
2

Quantity of Sample required for Testing: 1 x 10 g

Sampling Procedure: From each container separate samples are taken and
mixed and representative sample is taken from the mixed sample.
3
Container for Test Samples: Clean, Dry, Plain Glass Bottles
4
Reference Samples: 1 x 10 g
5
Storage: Preserve Iodine in a well closed container.

35.

REFRENCE BOOK OF STANDARDS: U.S Pharmacopoeia 36

61.

TESTING METHOD

Iodine is tested as per USP 36 .The given sample should comply with the given standards.
Iodine contains NLT 99.8 % and NMT 100.5 % of I.

STANDARDS
Description: Greyish violet brittle plates or small crystals with a metallic sheen; odour,
irritant. It volatalises slowly at room temperature.
Solubility: Soluble in chloroform, in ethanol (95%); slightly soluble in glycerin; very slightly
soluble in water. very soluble in concentrated solution of iodides.
Identification: (A) Solution (1 in 1000) in chloroform and in carbon disulfide has a violet
colour.
(B) To a saturated solution add starch-potassium iodide TS: a blue colour is produced. When
the mixture is boiled, the colour vanished but reappears as the mixture cools, unless it has
been subjected to prolonged boiling.
Non-volatile residue: Place 5.0 g in a tared porcelain dish, heat on a stem bath until the
iodine has been driven off, and dry at 105
0
for 1 hour: not more than 0.05 % of residue remains.
Chloride or bromide: Triturate 250 mg of finely powdered Iodine with 10 ml of water, and
filter the solution. Add drop wise, sulphurous acid (free from chloride), previously diluted
with several volumes of water, until the iodine colour just disappears. Add 5 ml of 6 N
ammonium hydroxide, followed by 5 ml of silver nitrate TS in small portions. Filter, and
26

acidify the filtrate with nitric acid: the resulting liquid is not more turbid than a control made
with the same quantities of the same reagents to which 0.10 ml of 0.020 N hydrochloric acid
has been added, the sulphurous acid being omitted (0.028 % as chloride).
Assay: Place about 500 mg of powdered Iodine in a tared, glass-stoppered flask, insert the
stopper, weigh accurately, and add 1 g of potassium iodide dissolved in 5 ml of water. Dilute
with water to about 50 ml, add 1 ml of 3 N hydrochloric acid, and titrated with 0.1 N sodium
thiosulfate VS, adding 3 ml of starch TS as the end-point is approached. Each ml of 0.1 N
sodium thiosulfate is equivalent to 12.69 mg of I.
RESULT
1 OF ANALYSIS FOR IODINE USP
Identification Test: A & B passes IP
2

Assay:

Sample: 0.5244
Reading: 40.8

1= 40.8 x 0.01269 x 0.1015 x 100

0.1 x 0.5244
2= 100.21 % (Limit between 99.8 % to 100.5 %)

27

ISOPROPYL ALCOHOL IP
9.

SAMPLING
1
2

Quantity of Sample required for Testing: 2 X 200 ml

Sampling Procedure: From each container separate samples are taken with
liquid sampler.
3
Container for Test Samples: Clean, Dry, Amber Glass Bottles.
4
Reference Samples: 1 x 200 ML
5
Storage: Store in well closed containers

35.

REFRENCE BOOK OF STANDARDS: Indian Pharmacopoeia

61.

TESTING METHOD

Isopropyl Alcohol is tested as per IP2014 .The given sample should comply with the given
standards as per IP2014. \

STANDARDS
Description: Clear, colourless liquid; odour characteristic and spirituous; flammable.
Identification: (A) Mix 1 ml of a 10%, v/v solution with 2 ml of mercuric sulphate solution
and heat just to boiling; a white or yellowish white precipitate is produced.
(B) Gently heat 1 ml with 4 ml of dilute potassium dichromate solution and 1 ml of sulphuric
acid; acetone, recognisable by its odour, is evolved.
Acidity or Alkalinity: Gently boil 25 ml for 5 minutes with 25 ml carbon dioxide-free water
and cool, taking precautions to exclude carbon dioxide. Not more than 0.06 ml of 0.1M
sodium hydroxide is required to make the resulting solution alkaline to phenolphthalein
solution.
Distillation range: Not less than 95.0% v/v distills between 81
0
0
and 83
0

Refractive Index: Between 1.377 and 1.378, determined at 20 .

0

Weight per ml: Between 0.782 g and 0.786 g, determined at 20 .

Aldehydes and ketones: Mix in a cylinder 25 ml with 25 ml of water and 50 ml of
hydroxylamine solution, allow to stand for 5 minutes and titrate with 0.1M sodium hydroxide
until the colour is the same as that of a mixture of 50 ml of hydroxylamine solution and 50 ml
of water contained in a similar cylinder, each being viewed down the vertical axis of the
cylinder .Not more than 2.0 ml of 0.1M sodium hydroxide is required.
28

Benzene and related substances: Carry out the method for gas chromatography, Appendix
4.2, using the following solutions. Solution (1) Test Sol: is the substance being examined.
Reference Solution (a) is a 0.1%v/v solution of 2-butanol reagent in the substance being
examined. Ref Solution (b) 0.1 % v/v solution of 2 - butanol & 1 - propanol in substance
being examined. Ref Solution (c) is a 0.00020% v/v of benzene in the substance being
examined. The chromatographic procedure may be carried out using (a) a glass column (1.8x
2mm) packed with acid-washed diatomaceous support (80 to 100mesh) coated with 15% w/v
of polyethylene glycol 400 and maintained at 50% with an injection port temperature of 150,
(b) nitrogen as the carrier gas with a flow rate of 30ml per minute and (c) a flame ionization
detector at a temperature of 200. Inject separately 2 microlitre of each of solutions (1) and
(a). The chromatogram obtained with solution (1) shows no peak with retention time similar
to the peak due to 2-butanol (retention time similar to the peak due to 2-butanol (retention
time relative to isopropyl alcohol, about 1.5) obtained with solution (a). Inject 2 microlitre of
solution (b) and adjust the sensitivity of the system so that the height of the peaks due to 2butanol and 1-propanol in the chromatogram obtained with solution (b) are not less than 50%
of the full scale of the recorder. The test is not valid unless the resolution between the peaks
due to 2-butanol and 1-propanol in the chromatogram obtained with solution(b) is at least
1.2.Inject 2 microlitre of each of solution(a) and (c) alternatively. The area of any peak due to
benzene in the chromatogram obtained with solution (1) is not greater than the difference
between the area pf the peak due to benzene in the chromatogram obtained with solution(c)
and that of the peak due to benzene in the chromatogram obtained with solution (1).In the
chromatogram obtained with solution (a) the sum of areas of any peaks other than the
principal peak and the peaks due to 2-butanol is not greater than 3 times the area of the peak
due to 2-butanol (0.3%)
Non-volatile matter: Not more than 0.002 % w/v, determined by evaporating 100 ml on a
0
water-bath and drying the residue at 105 .
Water-insoluble matter: Mix 1 volume with 19 volumes of water; no opalescence is
produced.
Water: Not more than 0.50% w/w, determined on 5 g.

RESULT OF ANALYSIS
FOR(Limit
ISOPROPYL
ALCOHOL IP
Acidity: 0.05ml
NMT 0.06)
2

Weight per ml: At 20o C

Weight of pycnometer: 41.5140 gms

Weight of pycnometer + water: 65.2921 gms
Weight of water: 23.7781 gms
Weight of pycnometer + sample: 60.2385 gms
Weight of sample: 18.7245 gms
18.7245 x 0.99718 = 0.99718 (limits 0.817 to 0.827)
23.7781
2
9

SODIUM IODIDE USP

9.

SAMPLING

1
2

Quantity of Sample required for Testing: 2 x 10 g.

Sampling Procedure: From each container separate samples are taken and mixed and
representative sample is taken from the mixed sample.
3
Container for Test Samples: Polyethylene bags.
4
Reference Samples: 1 x 10 g
5
Storage: Preserve Sodium Iodide in a well-closed container.

35.

REFRENCE BOOK OF STANDARDS: U.S Pharmacopoeia 36

61.

TESTING METHOD

Sodium Iodide is tested as per USP 36 .The given sample should comply with the given
standards as per USP 36.
Sodium Iodide contains not less than 99.0 percent and not more than 101.5 percent of NaI,
calculated on anhydrous basis.

STANDARDS
Description: A white crystalline powder, odourless, taste saline, bitter. Deliquescent in moist
air.
Solubility: Very soluble in water and also soluble in alcohol.
Identification: A solution (1 in 20) responds to the tests for Sodium (191) and for Iodide
(191).
Alkalinity: Dissolve 1.0 g in 10 ml of water, and add 0.15 ml of 0.10 N sulphuric acid and 1
drop of phenolphthalein TS to the sample solution: no red colour is produced.
Water: Method I (921): not more than 2.0 %.
IMPURITIES
Iodate solution: Dilute 1 ml of potassium iodate solution (1 in 2500) with water to 100 ml.
Standard solution: Dissolve 100 mg of sodium Iodide in ammonia- and carbon dioxide-free
water and add 1 ml of Iodate solution to obtain 10 ml solution. Transfer to a colourcomparison tube.
30

Sample solution: Dissolve 1.1 g in sufficient ammonia- and carbon dioxide-free water to
obtain 10 ml of solution. Transfer to a colour-comparison tube.
Analysis: To each comparison tube add 1 ml of starch TS and 0.25 ml of 1.0 N sulphuric acid,
and mix.
Acceptance criteria: Any colour produced in the sample solution does not exceed that in the
Standard solution (NMT 4 ppm).
Thiosulfate and barium:
Sample solution: Dissolve 0.5 g in 10 ml of ammonia-and carbon dioxide-free water.
Analysis: Add 2 drops of 2N sulphuric acid to the Sample solution.
Acceptance criteria: No turbidity develops within 1 min.
Potassium:
Sample solution: Dissolve 1 g in 2 ml of water.
Acceptance criteria: The sample solution yields no precipitate with 1 ml of sodium bitartrate
TS.
Heavy metals: (231) Dissolve 2.0 g in 25 ml of water: the limit is NMT 10 ppm.
Assay: Weigh accurately about 500 mg of sodium Iodide, and dissolve in about 10 ml of
water. Add 35 ml of hydrochloric acid, and titrate with 0.05 M potassium iodate VS until the
dark brown solution that is produced becomes plane brown. Add 1 ml of amaranth TS, and
continue the titration slowly until the red colour just changes to yellow. Each ml of 0.05 M
potassium iodate is equivalent to 14.99 mg of NaI.
Acceptance criteria: 99.0 % to 101.5 % on the anhydrous basis.
RESULT
1 OF ANALYSIS FOR SODIUM IODIDE USP
Identification Test: A & B passes IP
2

Assay: Sample: 0.503, Reading: 33.5

2= 33.5 x 0.01499 x 0.0499 x 100 = 99.63 % (Limit between 99% to 101.5%)

0.5 x 0.503

3
1

EXTERNAL PRODUCTS
GENTIAN VIOLET SOLUTION (1 % W/V)
9.

SAMPLING
1

Quantity of Sample required for Testing: 1 x 50 ml

2
3

Sampling Procedure: Random Sampling. (Final Packing)

Control Samples: 2 x 100 ml (As per Packing)

II.

COMPOSITION

85

Crystal Violet IP
1.0 %
Purified Water q.s

61.

TESTING METHOD

Gentian Violet Solution (1%w/v) is tested as per in-house specifications, as follows:

STANDARDS FOR BULK ANALYSIS

Gentian Violet Solution contains NLT 90.0% and NMT 110% of Crystal Violet.
Description: A violet coloured liquid.
Solubility: Slightly soluble in water, soluble in chloroform, in alcohol and in glycerin;
practically insoluble in solvent ether
Identification: (A) Sprinkle about 1 mg on 1 ml of sulphuric acid; it dissolves giving an
orange brownish-red colour. On diluting cautiously with water, the colour at first changes to
brown, then to green and finally to blue.
(B) To 10 ml of a 0.2 %w/v solution add about 0.25 ml of hydrochloric acid. Add drop by
drop tannic acid solution; a deep blue precipitate is produced.
Assay: Take 5 ml of sample in a 500 ml volumetric flask and dilute to 500 ml with water.
From this solution take 5 ml in a volumetric flask and dilute to 250 ml with water. Shake
well. Take this sample and measure the Absorbance at 585 nm. E1 = 2250.
From the Absorbance calculate the concentration of the sample.

3
2

RESULT OF ANALYSIS FOR GENTIAN VIOLET SOLUTION (1 % W/V)

ASSAY:
Dilute 5 ml of sample to 500 ml. From this dilute 5 ml to 250 ml. Measure the Absorbance at
585 nm. Et = 2250
Reading: 0.451
A = e. c. t
1= 0.451 x 500 x 250
2250 x 5 x 5
2= 1.0022 x 100
1.0
=

100.22 % (Limit between 90.0 % to 110 %)

33

HYDROGEN PEROXIDE SOLUTION IP

9.

SAMPLING
1
2
3

35.

Quantity of Sample required for Testing: 1 X 100 ml

Sampling Procedure: Random Sampling. (Final Packing)
Control Samples : 2 x 100 ML (As per Packing)

COMPOSITION

Hydrogen Peroxide Solution (20 Vol) contains between 5.0 % w/v to 7.0 % w/v of H2O2

61.

TESTING METHOD

Hydrogen Peroxide Solution IP is tested as per IP 2014

STANDARDS FOR BULK ANALYSIS

Hydrogen Peroxide Solution (20 Vol) contains not less than 5.0 %w/v and not more than 7.0
% w/v of H2O2, corresponding to about 20 times its volume of available oxygen.
Description: Clear, colourless liquid; odourless.
Identification: (A) To 1 ml add 0.2 ml of 1 M sulphuric acid and 0.25 ml of 0.02 M
potassium permanganate; the solution becomes colourless with evolution of gas.

34

(B) Shake 0.05 ml with 2 ml of 1 M sulphuric acid, 2 ml of ether and 0.05 ml of potassium
chromate solution; the ether layer becomes blue.
Acidity or Alkalinity: To 10 ml add 20 ml of water and add 0.25 ml of methyl red solution.
Not less than 0.20 ml and not more than 1.0 ml of 0.1M sodium hydroxide is required to
change the colour of the solution.
Organic Stabilisers: Shake 20 ml with successive quantities of 10, 5 and 5 ml of chloroform.
o
Evaporate the combined chloroform extracts at a temperature not exceeding 25 at pressure of
2kPa and dry in a desiccator. The residue weighs not more than 10 mg.
Non-volatile matter: Place 10 ml in an evaporating dish and allow it to stand until
o
effervescence ceases. Evaporate the solution on a water bath and dry the residue at 105 ; the
residue weighs not more than 20 mg.
Assay: To 1ml add 20ml of 1M sulphuric acid and titrate with 0.02M KMnO4. Each ml of
0.02 M KMnO4 is equivalent to 0.001701 g of H2O2 or 0.56 ml of oxygen.
RESULT OF ANALYSIS FOR HYDROGEN PEROXIDE SOLUTION IP
ACIDITY: 0.8 mL (limit NMT 1.0 ml)
ASSAY: 6.74 % (limit 5.0 % to 7.0 %)

CALCULATION:
ASSAY: BURETTE READING 36.0 ml
Burette reading X 0.001701 X actual molarity x 100
Molarity of KMnO4 x amount of sample

= 36.0 x 0.001701 x 0.022 x 100 = 6.73 % (limit 5 to 7 %)

0.02 x 1.0
Standardization of KMnO4
= 0.1034 x 0.02 = 0.022 M
14.9 x 0.006303

3
5

IODINE TINCTURE SOLUTION USP

9.

SAMPLING
1
2
3

35.

Quantity of Sample required for Testing: 1 X 100 ml

Sampling Procedure: Random Sampling. (Final Packing)
Control Samples: 2 x 100 ml (As per Packing)

COMPOSITION

Iodine: 20g
Sodium Iodide: 24g
Absolute Alcohol: 500 ml
Purified Water: Sufficient to produce 1000 ml

61.

TESTING METHOD

Iodine Tincture is tested as per USP 36 which is as follows:

STANDARDS FOR BULK ANALYSIS

Description: Deep brown liquid, odour characteristic of iodine & alcohol.
Identification: (A) Add 1 drop to a mixture of 1 ml of starch TS and 9 ml of water: a deep
blue colour is produced.
(B) Evaporate a few ml on a steam bath to dryness: the residue responds to the flame test of
sodium (191) and to the tests for Iodide (191).
Alcohol Content (611): Between 44.0 % and 50.0 % of C2H5OH
Assay for Iodine: Pipette 10 ml of Iodine Tincture solution into a glass - stoppered, 500 ml
flask, add 10 ml of water, and titrate with 0.1 N potassium arsenate VS, adding 3 ml of starch
TS as the end-point is approached. Each ml of 0.1 N potassium arsenate is equivalent to
12.69 mg of I. (Between 1.8 g to 2.2 g of I)
Assay for Sodium Iodide: To the titrated solution obtained in the Assay for iodine add 25 ml
of hydrochloric acid, cool to room temperature, add 5 ml of chloroform, and titrate with 0.05
M potassium iodate VS until the purple colour of iodine disappears from the chloroform. Add
the last portion of the iodate solution drop wise, while shaking the mixture vigorously and
continuously. Allow the mixture to stand for 5 minutes. If the chloroform develops a purple
36

colour, titrate the mixture further with the iodate solution. The difference between the number
of ml of 0.05 M potassium iodate used and the number of ml of 0.1N potassium arsenate
used, multiplied by 14.99, represents the number of mg of NaI in the volume of Iodine
Tincture taken.(Between 2.1 g to 2.6 g of NaI.)
RESULT OF ANALYSIS FOR IODINE TINCTURE SOLUTION USP
1. Assay for Iodine:
Test Reading: 16.0 ml
Normality of 0.1 N Potassium Arsenate: 0.1035 N
16.0 x0.01269 x 0.1035 x 100 = 2.10 (Limits between 1.8 g to 2.2 g of I)
0.1 x 10
2. Assay for Sodium Iodide:
(28.7 - 14.2) x 14.99 x 0.0570 = 2.47 (Limits between 2.1 g to 2.6 g of
NaI) 100 x 0.05
Standardization of 0.1 N I2 (By Arsenous Trioxide)
(153.01) (0.1) = 0.1101
(4.946) (28.1)
Standardization of 0.1 N Potassium Arsenate
N1 V1 = N2V2
N1 x 10 = 0.1101 4.7 = 0.1034
5.0
3. ALCOHOL CONTENT:
0

Specific Gravity (At 25 )

Weight of pycnometer
Weight of pycnometer + water
Weight of water
Weight of pycnometer + sample :
Weight of sample

:
:
:
:

41.5140 g
65.2659 g
23.7519 g
64.5535 g
23.0445 g

23.0445 = 0.9702
23.7519
I.e., 23.6 2 = 47.2 % v/v of alcohol. (Limits Between 44.0 to 50.0 % of C2H5OH)
37

SURGICAL SPIRIT BP
9.

SAMPLING
1Quantity of Sample required for Testing: 1 X 50 ml.
2Sampling Procedure: Random Sampling.
3Control Samples : 2 x 100 ml (As per Packing)

II.COMPOSITION

61.

Methyl Salicylate

: 0.5 %

Diethyl Phthalate

: 2.0 %

Castor Oil

: 2.5 %

Industrial Methylated Spirit

: q.s.

TESTING METHOD

Surgical Spirit is tested as per BP 2013

STANDARDS FOR BULK ANALYSIS

Surgical Spirit contains not less than 0.45 % and not more than 0.55 % of Methyl Salicylate
& not less than 1.80 % and not more than 2.20 % of Diethyl Phthalate by volume, the
remainder consisting of Industrial Methylated Spirit.
Description: Clear, odour characteristic, flammable liquid.
Identification:
(1) To 1 ml add 0.5 ml of 0.4 M iron (III) chloride hexahydrate. A Violet colour produced.
(2) To 1 ml add 50 mg of resorcinol and 1 ml of sulphuric acid, heat for 1 min, cool, pour
into water and make alkaline with 5 M sodium hydroxide. A distinct green fluorescence
is produced which disappears when the solution is made acidic and reappears when it is
made alkaline.
Weight per ml: Between 0.817 and 0.827 at 20

38

Assay:
For Methyl salicylate: Dilute 5 ml to 100 ml with absolute ethanol, further dilute 10 ml of
the this solution to 100 ml with absolute ethanol and measure the absorbance of the resulting
solution at the maximum at 306 nm, Appendix II B. Calculate the content of C 8H8O3 taking
335 as the value of the absorbance of a 1 % v/v solution of methyl salicylate at the maximum
at 306 nm using a 1 cm cell.
For Diethyl Phthalate: Further dilute 10ml of the final solution prepared in the Assay for
methyl salicylate to 50 ml with absolute ethanol and measure the absorbance of the resulting
solution at 227 nm, Appendix IIB. Subtract from the observed absorbance the absorbance due
to the methyl salicylate present, as the determined above, taking 432 as the value of the
absorbance of a 1 % v/v solution of methyl salicylate using a 1cm cell. For the purposes of
calculation take 419 as the value of the absorbance of a 1 % v/v solution of diethyl phthalate
at 227 nm using a 1 cm cell.
RESULT OF ANALYSIS FOR SURGICAL SPIRIT BP

1. Weight per ml: - At 20o C

Weight of pycnometer

41.8140 g

Weight of pycnometer + water

65.2921 g

Weight of water

23.7781 g

Weight of pycnometer + sample :

Weight of sample

19.6017 x 0.99718 =
23.7781

61.1157 g
:

0.8220

19.6017 g

(limits 0.817 to 0.827)

2. Assay
1) For Methyl Salicylate
Absorbance at 306 nm: 0.911
0.911 x 100 x 100 = 0.54 (Limits 0.45 to 0.55 % v/v)
335 x 5 x 10

3
9

ALCOHOL CONTENT:
0

Specific Gravity (At 20 ) Weight of pycnometer Weight

of pycnometer + water Weight of water

1:

41.514 g

2:

65.2921 g

3:

23.7781 g

4:

64.6632 g

5:

23.1492 g

Weight of pycnometer + sample Weight of sample

23.1492 = 0.9735
23.7781

I.e., 21.724 = 86.88

%v/v of alcohol.

40

SURGICLIN CLINICAL SPIRIT USP

9.

SAMPLING
1
2
3

35.

Quantity of Sample required for Testing: 1 X 200 ml

Sampling Procedure: Random Sampling.
Control Samples: 2 x 400 ml or 4 x 100 ml (As per Packing)

COMPOSITION
Isopropyl Alcohol 70.0 %
Purified Water q.s

61.

TESTING METHOD

Surgiclin Clinical Spirit (Isopropyl Rubbing Alcohol 70% USP) is tested as per USP 36

41

STANDARDS FOR BULK ANALYSIS

Surgiclin Clinical Spirit contains not less than 68.0 % and not more than 72.0 % of isopropyl
alcohol, by volume, the remainder consisting of water.
Description: Clear, colourless, liquid.
Specific Gravity: Between 0.872 and 0.883 at 20

Acidity: Transfer 50 ml to a suitable flask and add 75 ml of carbon dioxide free water. Titrate
potentiometrically to a pH of 8.5; not more than 1.0 ml of 0.020 N sodium hydroxide is
required for neutralization.
Non-volatile residue: Evaporate 50 ml to dryness in a tared porcelain dish on a steam bath
o
and dry at 105 for 1 hour. The weight of the residue does not exceed 5 mg (0.01%)
Assay: Transfer 50 ml of Isopropyl Rubbing Alcohol to a 250 ml distilling flask and add 100
ml of water. Arrange the flask for distillation, distill and collect 95 ml of distillate in a 100 ml
volumetric flask. Dilute to volume with water, mix and determine the specific gravity of the
o
distillate at 25 (841). The specific gravity is between 0.955 and 0.950, corresponding to
between 68.0% and 72.0% of isopropyl alcohol in the specimen taken.

RESULT OF ANALYSIS FOR SURGICLIN CLINICAL SPIRIT USP

1:

1. Specific Gravity: - At 20o C

Weight of pycnometer Weight of pycnometer + water
Weight of water
Weight of pycnometer + sample Weight of sample

1:

41.5140 g

2:

65.2921 g

3:

23.7781 g

1:

62.3491 g

20
.8
35
1
g

23.778
20.8351 = 0.8762

(limits 0.872 to 0.883)

42

REPACKING PRODUCTS
EUCALYPTUS OIL IP
9.

SAMPLING

1
2

Quantity of Sample required for Testing : 2 X 100 ml

Sampling Procedure: From each container separate samples are taken with liquid
sampler.
3
Container for Test Samples: Clean, Dry, Plain PET Bottles.
4
Reference Samples: 2 x 100 ml
5
Storage: Store in well filled, tightly-closed containers in a cool place

35.

REFERENCE BOOK OF STANDARDS: Indian Pharmacopoeia

61.

TESTING METHOD

Eucalyptus Oil is tested as per IP2014. The given sample should comply with the given
standards as per IP2014.

STANDARDS
Eucalyptus Oil is the essential oil obtained by steam distillation & rectification from the fresh
leaves or the fresh terminal branches of various species of eucalyptus like Eucalyptus
globulus (Fam. Myetaceae)
Eucalyptus oil contains not less than 60 % and not more than 80 % of 1, 8-cineole, and not
less than 10 % and not more than 22 % of -pinene.
Description: A colourless or pale yellow liquid; free from sediment, suspended matter, odour
aromatic and camphoraceous; taste pungent followed by a sensation of cold.
Identification
(A) Determine by gas chromatography (2.4.13)
Test solution: A 2.0 % w/v solution of the oil under examination in ethanol (95 %)
Reference solution: A 2.0 % w/v solution of eucalyptus oil RS in ethanol (95 %)
Use chromatographic system describe in the Assay.
The peak in the chromatogram obtain with the test solution corresponds to the peak in the
chromatogram obtained with the reference solution.
4
3

(B) Flash point (2.4.44).52 to 56 .

Tests:
Relative Density: 0.905 to 0.925. (2.4.29)
o

Optical Rotation: Between + 2 and +10 (2.4.22)

Refractive Index: Between 1.457 and 1.470, (2.4.27)
Weight per ml: Between 0.897 and 0.924 g, (2.4.29)
Assay:
Determination by gas chromatography (2.4.13).
Test solution. A 2.0 % w/v solution of the oil under examination in ethanol (95 %)
Reference solution (a). A 2.0 % w/v solution of 1, 8-cineol RS in ethanol (95 %)
Reference solution (b). A 2.0 % w/v solution of -pinene RS in ethanol (95 %)
Chromatographic system:
1
2
3

A capillary column 30m x 0.25 mm, coated with methyl 5 % phenylposiloxane,

Temperature:
0

Column.50 for 1 minute, increase from 50 to 220 at a rate of 10 per minute and
maintain at this temperature for 13 minutes
0
0
4
Inlet port at 250 and detector at 280 ,
5
Detection by flame ionization detector,
6
Flow rate 1 ml per minute sing nitrogen as carrier gas,
7
Injection volume: 1.0l.
8
Split ratio: 1: 25.
Inject reference solution (a), (b) and the test solution.
Calculate the content of 1, 8-cineole, and -pinene contents in the oil using area
normalization procedure.

44

RESULT OF ANALYSIS FOR EUCALYPTUS OIL IP

0

1. Relative Density : At 25 C
Weight of pycnometer

41.5140 g

Weight of pycnometer + water

65.2659 g

Weight of water

23.7519 g

Weight of pycnometer + sample

62.9191 g

Weight of sample

21.4051 g

21.4051 = 0.9012 (Limits 0.905 to 0.925 g)

23.7519
0

2. Weight Per ml : At 25 C
Weight of pycnometer

41.5140 g

Weight of pycnometer + water

65.2659 g

Weight of water

23.7519 g

Weight of pycnometer + sample

62.9197 g

Weight of sample

21.4057 g

21.4057 x 0.9012 = 0.8976 (Limits 0.897 to 0.924 g)

23.7519

45

GLYCERIN IP
9.

SAMPLING

1
2

Quantity of Sample required for Testing: 1 X 120 gms

Sampling Procedure: From each container separate samples are taken with liquid
sampler.
3
Container for Test Samples: Clean, Dry, Plain PET Bottles.
4
Reference Samples: 1 x 120 gms
5
Storage: Store in well closed containers

35.

REFRENCE BOOK OF STANDARDS: Indian Pharmacopoeia

61.

TESTING METHOD

Glycerin is tested as per IP2014. The given sample should comply with the given standards
as per IP2014.

STANDARDS
Glycerin contains not less than 98.0 per cent and not more than 101.0 per cent of C 3H8O3,
calculated with reference to the anhydrous substance.
Description: Clear, colourless syrupy liquid, odourless, very hygroscopic.
Solubility: Miscible with water and with ethanol (95 %); slightly soluble in acetone;
practically insoluble in ether and in fixed oils and volatile oils.
Identification:
Test A may be omitted if tests B, C and D are carried out. Tests B and C may be omitted if
tests A and D are carried out.
(A)To 5 ml add 1 ml of water and mix carefully. The infra-red absorption spectrum of the
resulting solution, is concordant with the reference spectrum of glycerin (85%) or with the
spectrum obtained from glycerin (85%) RS.
(B)Mix 1 ml with 0.5 ml of nitric acid and superimpose 0.5 ml of potassium dichromate
solution; a blue ring develops at the interface of the two liquids.
Allow standing for 10 minutes; the blue colour does not diffuse into the lower layer.
(C)Heat 1 ml with 2 g of potassium hydrogen sulphate in an evaporating dish. Irritant
vapours are evolved which blacked filter paper moistened with alkaline potassium mercuryiodide solution.
4
6

(D)Refractive Index, between 1.470 and 1.475, determined at 20 C

Appearance of solution: Dissolved 50 g of the substance in sufficient carbon dioxide free
water to produce 100ml (Solution A). Solution A is clear, .Dilute 10 ml of solution A to 25 ml
with water. The solution is colourless.
Acidity or Alkalinity: To 50 ml of a 50.0 % w/v solution in carbon dioxide free water add
0.5 ml of phenolphthalein solution. The solution is colourless and not more than 0.2 ml of 0.1
M sodium hydroxide is required to produce a pink colour. Reserve the final solution for the
test for Ester.
Heavy Metals : Not more than 5 PPM, determined by Method A on a solution of 4.0 g in 2
ml of 0.1 M hydrochloric acid and sufficient water to produce 25 ml
Iron: 10 g complies with the limit test for iron, (4 ppm)
Chloride: 20 ml of solution A complies with the limit test for chlorides, (25 ppm)
Sulphate: 10 ml of Solution A complies with limit test for sulphates, (30 ppm)
Aldehydes & Reducing substances: To 7.5 ml of solution A in a glass stoppered flask add
7.5 ml of water and 1 ml of decolorized pararosaniline solution, close the flask and allow to
stand for 1 hour. Any colour produced is not more intense than that obtained in a standard
prepared at the same time and in the same manner but using 7.5 ml of formaldehyde standard
solution (5 ppm CH2O) in place of solution A. The test is not valid unless the standard
solution is pink.

RESULT OF ANALYSIS FOR GLYCERIN IP

Assay:
Sample: 0.1007 gm
Blank Reading: 14.5 ml
Test Reading : 21.9 ml
Difference

: 7.4 ml

7.4 x 0.00921 x 0.1463 x 100 = 99.01 % (Limit 98.0 % to 101 %)

0.1 x 0.100

47

LIQUID PARAFFIN IP
9.

SAMPLING

1
2

Quantity of Sample required for Testing: 2 X 100 ml

Sampling Procedure: From each container separate samples are taken with liquid
sampler.
3
Container for Test Samples: Clean, Dry, Plain PET Bottles.
4
Reference Samples: 1 x 100 ml
5
Storage: Store in well closed light-resistant containers.

35.

REFERENCE BOOK OF STANDARDS: Indian Pharmacopoeia

61.

TESTING METHOD

Liquid Paraffin IP is tested as per IP2014. The given sample should comply with the given
standards as per IP2014.

STANDARDS
Light Liquid Paraffin is a purified mixture of liquid saturated hydrocarbons obtained from
petroleum to which not more than 10 ppm of tocopherol or of butylated hydroxytoluene may
be added. It may contain a suitable stabilizer.

48

Description: Transparent, colourless, oily liquid, free from fluorescence by daylight;

odourless or almost odourless.
Acidity or Alkalinity: To 10 g add 20 ml of boiling water, heat in a water-bath for 5 minutes,
shake vigorously for 1 minute, cool, allow it to separate and filter the aqueous layer.
To 10 ml of the filtrate add 0.1 ml of phenolphthalein solution. The solution is colourless and
not more than 0.1 ml of 0.1 M sodium hydroxide is required to change the colour of the
solution to pink
Weight per ml: Between 0.860 and 0.904 g (G.A.M 2)
o

Dynamic viscosity: Between 110 and 230 mPas, determined at 20 + 1 by Method B.

Light absorption: Absorbance in the range 240 to 280 nm of a 2.0 % w/v solution in 2, 2, 4trimethylpentane, not more than 0.1 (G.A.M - 2)
Readily carbonisable substances: Place 5 ml in a dry heat- resistant glass stoppered testtube (125mmx 18 mm) previously rinsed with chromic acid solution, then with water and
dried. Add 5 ml of nitrogen free sulphuric acid (containing 94.5 % to 95.5 %w/w of H2SO4),
insert the stopper and shake as vigoursly as possible in the longitudinal direction of the tube
for 5 seconds. Loosen the stopper, immediately place the tube in a bath of boiling water,
supporting it so as to prevent contact of the tube with the bottom or side of the bath and heat
for 10 minutes. At the end of the second, fourth, sixth and eighth minutes, remove the tube
from the bath and shake as vigorously as possible in the longitudinal direction of the tube for
5 seconds. At the end of 10 minutes from the time the tube was placed in the bath remove the
tube and allowed to stand for 10 minutes. The lower acid layer is not more intensely coloured
than a mixture of 3 ml of FCS, 1.5 ml of CCS and 0.5 ml of CSS, Appendix 6.2, overlaid with
5 ml of liquid paraffin. If the sulphuric acid remains dispersed in the molten paraffin, the
colour of the emulsion is not darker than that of the standard mixture when shaken vigoursly.
o

Solid Paraffin: Place a suitable quantity, previously dried by heating at 100 for 2 hours and
cooled in a dessicator over sulphuric acid, in a glass cylindrical vessel having an internal
diameter of approximately 25 mm. Close the vessel and immerse in a mixture of ice and
water; after 4 hours the liquid is sufficiently clear that a black line, 0.5 mm in width, held
vertically behind the vessel is easily seen.
Sulphur Compounds: Mix 4 ml with 2 ml of ethanol (95 %), and 2 drops of a clear,
o
saturated solution of lead monoxide in sodium hydroxide solution and heat at 70 for 10
minutes with frequent shaking; the mixture remains colourless.

4
9

RESULT OF ANALYSIS FOR LIQUID PARAFFIN IP

0

5:

1. Weight Per ml : At 25 C
Weight of pycnometer
Weight of pycnometer +

1:

41.5140
g

2:

65.2659
g

3:

23.7519
g

4:

62.0821
g

water Weight of water

Weight of pycnometer +
sample Weight of sample
NMT
0.1)
2.0397

20.5681 x
0.99602 =
0.8625 (Limits
0.860 to 0.904
g)
Dyna
23.7519
mic
Viscos
2. Light
ity:
Absorption:

t = 12
Absorbance
Reading at 260 min 18
sec
nm:
i.e. 738
0.023 x 2.0 = sec.
0.022 (Limits

2
0
.
5
6
8
1
g

p
Kpt
=
0.91=
0.326 x 0.8609 x
98 738
20
3 x2=
207.12
mpas
0.8 (Limits 110.0 to 230
62 mpas)
5
1=
0.8
6
0
9
2
=

50

METHYL SALICYLATE IP
9.

SAMPLING

1
2

Quantity of Sample required for Testing: 1 X 100 gms

Sampling Procedure: From each container separate samples are taken with liquid
sampler.
3
Container for Test Samples: Clean, Dry, Plain Glass Bottles.
4
Reference Samples: 2 x 100 gms
5
Storage: Store in well-closed , light resistant containers

35.

REFERENCE BOOK OF STANDARDS: Indian Pharmacopoeia

61.

TESTING METHOD

Methyl Salicylate is tested as per IP2014.The given sample should comply with the given
standards as per IP2014.

STANDARDS
Methyl Salicylate contains not less than 99.0 per cent w/w and not more than 100.5 per cent
w/w of C8H8O3.
Description: Colourless or slightly yellow liquid, odour, strong, persistent, characteristic and
aromatic.
Solubility: Miscible with chloroform and with ethanol (95 %) and with fixed and volatile oils
very slightly soluble in water.
Identification: (A) To 10 ml of a standard aqueous solution add 0.05 ml of ferric chloride
test solution: a violet colour develops.
(B)Heat 0.25 ml with 2 ml of 2M sodium hydroxide on a water-bath for 5 minutes and add 3
ml of 1M sulphuric acid. Filter and wash the precipitate with water. The melting range of the
0
0
0
precipitate, after drying at 105 for 1hour, is between 156 and 161
Acidity: Dissolve 5 g in 50 ml of ethanol (95 %), previously neutralised to a blue colour with
bromocresol green solution by the addition of 0.1M sodium
Hydroxide. Not more than 0.4 ml of 0.1M sodium hydroxide is required to restore the blue
colour.
Appearance of solution: To 2 ml add 10 ml of ethanol (95%). The resulting solution is clear
and not more intensely coloured than reference solution YS7.
51

Refractive Index: Between 1.534 and 1.538.

Weight per ml: Between 1.175 g and 1.185 g.
Assay: Weigh accurately about 0.5 g, dissolve in 25 ml of ethanol (95%), add 0.05 ml of
phenol red solution and neutralise with 0.1M sodium hydroxide. Add 50.0 ml of 0.1M sodium
hydroxide and heat under a reflux condenser on a water-bath for 30 minutes. Cool and titrate
with 0.1M hydrochloric acid. Perform a blank determination and make any necessary
correction. Each ml of 0.1M sodium hydroxide is equivalent to 0.01522 g of C8H8O3.
RESULT OF ANALYSIS FOR METHYL SALICYLATE IP
0

3:

1. Weight Per ml : At 25 C
Weight of Pycnometer Weight of pycnometer + water
Weight of water
Weight of pycnometer + sample Weight of sample

28.1276 x 0.99602 = 1.1795

(Limits 1.175 to 1.185 g)
23.7519
2. Assay :

Sample Taken

: 0.5701 g

Blank Reading

: 52.0 ml

Test Reading

: 15.4 ml

Difference

: 36.6 ml

M
N
o
r
m
a
l

1:

41.5140 g

2:

65.2659 g

2:

23.7519 g

1:

69.6416 g

28
.1
27
6
g

0.1 x 0.5101

2
H

0
.

2=
100.3 % w/w of C8H8O3
(Limits 99 % to 100.5 % w/w of
C8H8O3)
52

CHEMICAL ASSAYS AND TESTS

WEIGHT PER ML
The weight per millilitre (weight per ml) of a liquid is the weight in g of 1 ml of
liquid when weighed in air at 20C, unless otherwise specified in the monograph.

The weight per millilitre is determined by dividing the weight in air, expressed in g,
of the quantity of liquid that fills a pycnometer at the specified temperature by the
capacity, expressed in ml, of the pycnometer at the same temperature. The capacity
of the pycnometer is ascertained from the
weight in air, expressed in g, of the
quantity of water required to fill the pycnometer at that temperature. The weight of a litre of
water at specified temperatures when weighed against brass weights in air of
density 0.0012 g per ml
is given in the following table. Ordinary deviations in the
density of air from the above value, here taken as the mean, do not affect the result
of a determination in the significant
figures prescribed for Pharmacopoeial substances.

Pycometer
Temperature (C )

Weight of a litre of water (mg)

20

997.18

25

996.02

30

994.62

53

LOSS ON IGNITION

Muffle Furnace
The Loss on Ignition test is a method to measure the loss in mass when the sample is ignited
under the condition specified in each monograph. This method is usually applied to inorganic
drugs which lose a part of the components or impurities during ignition.

PROCEDURE:
1 Heat a silica or platinum crucible to redness for 10 minutes, allow to cool in a
Desiccator and weigh.
2 Transfer to the crucible 1g of substance under examination and weigh the crucible and
the content accurately.
3 Ignite gently at first until the substance is thoroughly charred.

Cool moisten the residue with 1ml of concentrated H2SO4 heat gently until the
white fumes are no longer evolved and ignite at 800C 25C until all black
particles have disappeared.

Conduct the ignition in a place protected from the air current.

drops of H2SO4 and heat.

Allow the crucible to cool, add few

1 Ignite as before, allow cooling and weighing.

DETERMINATION OF SAPONIFICATION VALUE

The saponification value is the number which expresses in milligrams, the amount of
potassium hydroxide necessary to neutralize the free acids and to saponify the esters present
in 1 gm of substance.
It is measure of the average molecular wt. (chain length) of all the fatty acids presents. As
most of the mass of a fat or trimester is in the 3 fatty acids. It allows the comparison of
average fatty acid chain length. The long chain fatty acid found in fats have low
saponification value because they have a relatively fewer number of carboxylic functional
groups per unit mass of the fat as compared to short chain fatty acids
54

Saponification value gives an indication of nature of fatty acids in the fat since longer carbon
chain; the lesser is the amount of acid liberated per gram of fat hydrolyzed. When fat or oil is
heated with an alcoholic solution of KOH, free fatty acids & glycerol are liberated. The
refluxing with glycerol esters yields glycerol & K-salt of fatty acids. Subsequently the test
sample as well as control is titrated against HCL to determine the amount of KOH used in the
saponification process.
Procedure:
1) Introduce about 2 gm of the substance to be examined accurately weighed into a 200
ml flask of borosilicated glass fitted with a reflux condenser.
2) Add 25 ml of 0.5 N alcoholic potassium hydroxide, accurately measured.
3) Boil under reflux on a water bath for 30 minutes, frequently rotating the content.
4) Add 1 ml of phenolphthalein solution & immediately titrate with 0.5 N HCL.
5) Note the volume in ml of titrant (a)
Blank: Carry out a blank test under the same condition, omitting the substance. Note the
volume in ml of titrant (b)

Calculation:
Saponification value = (b-a) x 28.05
W
Where, W = weight in gm of the substance

55

Total Viable Count

The viable count is one method of determining the density of a microbial population. It gives
a quantitative idea about the presence of microorganisms such as bacteria, yeast and mold in a
sample. Serial dilutions of suspension of bacteria are plated onto a suitable solid medium.
Dilution procedure influences overall counting process. The suspension is spread over the
surface of growth medium. The plates are incubated so that colonies are formed.
Multiplication of a bacterium on solid media results in the formation of a macroscopic colony
visible to naked eye. To be specific, the count actually represents the number of colony
forming units (CFU) per g (or per ml) of the sample.
Materials and Methods
Glassware:
1
2
3

Petri plates 36
Test tubes 12
Pipettes (1ml) 12

Media:
1
2
3

MacConkey's Agar
Nutrient Agar
Sabouraud's Agar

Samples:
1
2
3

Formulation 1 (Presumptive: Kadha)

Formulation 2 (Semi-solid)
Formulation 3 (Presumptive: Rose Water)

Miscellaneous:
1
2
3

Spreader
Disinfectants
Incubator

Standard Plate Count Method

1

The standard plate count is usually done by diluting the original sample, plotting
aliquots of the dilutions onto an appropriate culture medium, and then incubating the
plates under proper conditions so that colonies are formed.
2
After incubation, the colonies are counted and from knowledge of dilution used, the
original number of viable cells can be calculated. The total viable cells are usually
reported as colony forming units (CFUs).
3
This method of plate count is relatively easy to perform and is much more sensitive
then turbidimetric measurements. A measure disadvantage is that, the time necessary for
dilutions, plotting and incubations as well as the time needed for media preparations.
5
6

Observations & Results:

1. Formulation 1 (Presumptive: Kadha)
Incubation Time: 48 hrs (since no growth was observed on incubation for 24 hrs)
Dilutions
MacConkey's
Agar
Nutrient Agar
Sabouraud's
Agar

1:10
No growth

1:20
No growth

1:50
No growth

1:100
No growth

No growth
4

No growth
2

No growth
2

No growth
0

Sabourauds Agar
Dilutions
CFU/ml

1:10
300

1:20
200

1:50
-

1:100
-

2. Formulation 2 (Semi-solid)
Incubation Time: 24 hrs
Dilutions
MacConkey's
Agar
Nutrient Agar
Sabouraud's
Agar

1:10
No growth

1:20
No growth

1:50
No growth

1:100
No growth

7
No growth

4
No growth

2
No growth

0
No growth

Nutrient Agar
Dilutions
CFU/ml

1:10
900

1:20
600

1:50
500

1:100
-

57

3. Formulation 3 (Presumptive: Rose Water)

Incubation Time: 24 hrs
Dilutions
MacConkey's
Agar
Nutrient Agar
Sabouraud's
Agar

1:10
No growth

1:20
No growth

1:50
No growth

1:100
No growth

72
No growth

3
No growth

0
No growth

0
No growth

Nutrient Agar
Dilutions
CFU/ml

1:10
7200

1:20
600

1:50
-

1:100
-

Interpretations:
Total viable count for the provided 3 formulations were efficiently done using Spread Plate
technique
1

In
Formulation
1 growth
wasrespectively.
observed on Sabourauds agar plate in dilutions 1:10 and 1:20 & the CFU/ml
calculated
was 300
and 200

In
Formulation
2 growth
on Nutrient agar plate in dilutions 1:10, 1:20 and 1:50 & the
CFU/ml
calculated
was 900,was
600observed
and 500 respectively.
In Formulation 3 growth was observed on Nutrient agar plate in dilutions 1:10 and 1:20 & the CFU/ml
calculated was 7200 and 600 respectively.

Since growth was observed in Nutrient agar plate and Sabourauds agar plate, it is of fungal
and yeast contamination.

Conclusion:
Total Viable count is an effective and widely used technique for assessing the microbial
count. All the three formulations showed growth due to microbial contamination which
further indicates that the formulations are of inferior quality.

58

Learning Outcomes
1
2

The
training
which Iand
underwent
atapproach.
Ashwin
Fine
& gained
Pharmaceuticals
helped
me
develop
a sincere
practical
TheChemicals
experience
wasBioanalytical
thoroughly
enriching
fruitful
which
helped
me understand
the application
of
Sciences
inand
industry.
IAyurvedic
had an opportunity
to perform
assays and to develop and grasp data interpretation skills for
products such
as Tailas Chemical
and Kadhas

Working
in aofQA/QC
also helped me to understand various norms and regulations related to
applications
QA/QCdepartment
in such an industry.

Training offered me a chance to work in Ashwin fine Chemicals and thus I could learn
various aspects related to Standardization of Ayurvedic formulations & helped me in
enhancing my techniques literature survey/referencing, planning of the experiments, its
execution and efforts to meet the dead line.

Thus to conclude, I would like to say that this experience has been positive in every way and
will definitely help me in the future.

59

References

Ayurvedic Formulary of India. Part II. First English Edition. Published By- The
Controller of Publication, Civil Line, Delhi 110054.

Ayurvedic Formulary of India. Part I. Second Revised Indian Edition. Published ByThe Controller of Publication, Civil Line, Delhi 110054.

Pharmacopoeia Of India, Volume II, Third Edition

Chemical Tests & Assays

60