Lab. 2-Moisture and Determination (Gravimetric Method)

Experiment No.
2
MOISTURE DETERMINATION
(Gravimetric Method)
Culhi, Ralph Aubrey B.

Student
Brent Jericko P. Narciso, RPh.

Instructor
February 15, 2022

Date
OBJECTIVE:
To determine the moisture content of a plant material by gravimetric analysis and to
understand its significance.
MATERIALS:
Dried plant samples (Expt. No. 1), evaporating dish,
Desiccator, oven, digital balance
PROCEDURE:
(For drugs, which do not contain constituents volatile at 105°c)
1. Weigh approximately 5g of the pulverized sample in a *tared evaporating dish. Record the
weight.
2. Dry the drug continuously for 5 hours. Cool in the desiccator and then weigh.
3. Continue heating and weighing at one hour intervals until the difference between two
successive weights does not exceed 0.25% (0.0025g). The loss in weight represents the moisture
present in the dried sample.
4. Determine the percentage moisture content from the weight of the plant sample taken.
5. *Taring of Evaporating Dish: Wash, dry and place the evaporating dish in an oven for 20
minutes. Cool and then weigh. Return in the oven and weigh again. Repeat the heating,
cooling and weighing processes until a difference of not more than 0.2mg (0.00025) between
two (2) successive weights is obtained or until constant weight is obtained.
Formula:
Loss in weight = Weight of the dried plant sample - Constant weight of the drug
𝐿𝑜𝑠𝑠 𝑖𝑛 𝑤𝑒𝑖𝑔ℎ𝑡
% Moisture = 𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑡ℎ𝑒 𝑑𝑟𝑖𝑒𝑑 𝑝𝑙𝑎𝑛𝑡 𝑠𝑎𝑚𝑝𝑙𝑒
x 100
Data and Results: (Tabular Form)
Computations:
Conclusion:
QUESTIONS:
1. Enumerate and explain the significance of moisture determination of drugs.
- The moisture content of a product influences its processibility, shelf life, usability, and
quality. Accurate moisture content determination thus plays a critical role in ensuring
quality in many industries, including food, pharmaceuticals, and chemicals. Furthermore,
the maximum allowable moisture content in certain products may be governed by
legislation. Typically, moisture content is determined using a thermogravimetric
approach, i.e., loss on drying, in which the sample is heated and the weight loss due to
moisture evaporation is recorded.
- Excessive or insufficient moisture content can have a negative impact on a pharmaceutical

product's physical properties, which in turn affect the chemical reactivity and binding
properties that define the product's shelf-life. Furthermore, pharmaceutical products may
contain compounds that are harmful when in contact with the skin or inhaled, and
moisture content is critical to the crystallization, agglomeration, and chemical form of
these compounds during tablet manufacturing. Moisture analysis is thus a standard
quality control procedure in the pharmaceutical industry.
2. What are the USP/NF official methods of moisture determination? Describe the principle, give
their specific uses, advantages and disadvantages.
- The USP provides two methods for determining the moisture content of solids: Titrimetry
/Titration (Karl Fisher titration) and Gravimetric analysis (e.g., thermal gravimetric
analysis).
o Titration Analysis refers to a group of methods of quantitative analysis in which

an analyte is determined basing on its stoichiometric reaction with a reagent of
established concentration introduced to a sample gradually until the analyte is
consumed quantitatively.
❖ Advantages ❖ Disadvantages
- It is generally inexpensive and - It is a destructive method that
requires little in the way of frequently consumes relatively large
equipment. amounts of the substance being
- It does not necessitate a high level of analyzed.
expertise. - It can generate large amounts of
- It is frequently possible to complete it chemical waste, which must be
quickly. disposed of.
- The results are available right away. - It is not very accurate.
o Gravimetric analysis is a quantitative chemical analysis method in which the

constituent sought is converted into a substance of known composition that can be
separated and weighed from the sample.
❖ Advantages - When using a modern analytical
balance, it is accurate and precise.
- Possible sources of error can be easily ❖ Disadvantage
identified because filtrates can be - The main disadvantage is that it takes
tested for completeness of a long time to complete.
precipitation and precipitates can be - When modern instrumental methods
tested for impurities. are available, the chemist frequently
- It is an absolute method that involves prefers them.
direct measurement without the need - Gravimetric analysis is typically
for any kind of calibration. limited to analyzing a single element
- Determination can be done with or a small group of elements at a time.
relatively inexpensive equipment; the - Methods are frequently complicated,
most expensive items are a muffle and a minor hiccup in a procedure can
furnace and, occasionally, platinum often spell disaster for the analysis
crucibles. (colloid formation in precipitation
- Many elements' atomic masses were gravimetry, for example).
determined with six-figure accuracy - Gravimetric analysis is based on mass
using gravimetric analysis. measurement.
3. What is the official monograph limit for moisture content of drugs?

Drugs Moisture Content W/W
Aloes Not More than 10
Digitalis Not More than 5
Starch Not More than 15
4. Explain how the term "constant weight" is used in analytical procedures.

- Weighing is critical in chemical synthesis because it is frequently the only way to
determine how much of a substance will be used or formed in a chemical reaction.
Constant weight means a difference of no more than 0.5 mg or one percent of total weight
less tare weight, whichever is greater, between two consecutive weighings, with no less
than six hours of desiccation time between weightings.
References:
Constant weight definition. Law Insider. (2014). Retrieved February 15, 2022, from
https://www.lawinsider.com/dictionary/constant-weight
Kumar, A. (2011, December 7). Moisture content: A stability problem in pharmaceutical products.
PharmaTutor. Retrieved February 15, 2022, from https://www.pharmatutor.org/articles/moistutre-
content-stability-problem-in-pharmaceutical-
products#:~:text=The%20USP%20offers%20two%20methods,e.g.%2C%20thermal%20gravimetric%20
analysis).
Sponsored by CEM Corporation. (2019, May 14). Moisture Analysis in the pharmaceutical industry.
AZoM.com. Retrieved February 15, 2022, from
https://www.azom.com/article.aspx?ArticleID=18029#:~:text=Excessive%20or%20deficient%20moist
ure%20content,define%20the%20product's%20shelf%2Dlife.&text=Moisture%20analysis%20is%20th
us%20a%20routine%20quality%20check%20in%20the%20pharmaceutical%20industry.

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Experiment No.

Culhi, Ralph Aubrey B.

Brent Jericko P. Narciso, RPh.

February 15, 2022

Data and Results: (Tabular Form)

- Excessive or insufficient moisture content can have a negative impact on a pharmaceutical

o Titration Analysis refers to a group of methods of quantitative analysis in which

o Gravimetric analysis is a quantitative chemical analysis method in which the

3. What is the official monograph limit for moisture content of drugs?

4. Explain how the term "constant weight" is used in analytical procedures.

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