ASTM D7077-04

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Designation: D7077 – 04
Standard Test Method for
Evaluation of Drop Size by weight of Solutions and
Suspensions
This standard is issued under the fixed designation D7077; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2.1.5 Drop size—The weight of a single drop of product
dispensed from a package designed to deliver product through
1.1 This standard test method uses a simulated in-use study
a controlling orifice.
to measure the drop size by weight and to determine the
2.1.6 Unsolicited drops—An amount of product that comes
number of drops per container for solutions and suspensions
from the container without the user squeezing the container.
contained in a package system designed to deliver product
2.1.7 Variable—Different plugs, closures, bottles, or formu-
drop-wise through a controlled size orifice by squeezing or
lations.
compressing the package.
2.1.8 Volcanoing—Spewingforthoftheproductuponinitial
1.2 This standard does not purport to address all of the
opening of the container/closure system.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3. Summary of Test Method
priate safety and health practices and to determine the
3.1 Drop size tends to be highly subjective given all the
applicability of regulatory limitations prior to use.
potential variables, however, it is an essential element in
2. Terminology describing the dosage delivered from a specific package. This
test method is structured to mimic patient use of an solution or
2.1 Definitions:
suspension that is delivered through a controlling orifice to
2.1.1 Average drop size per dosing interval—The average
determine an average drop size for the product. The average
weight of a drop of product dispensed from a given package
number of drops per container will then be calculated from the
within a given dosing interval.
data collected.
2.1.2 Average drop size per package—The average weight
of a drop of product dispensed from a given package consid-
4. Significance and Use
ering all dispensed doses.
4.1 This test method may be used to measure the drop size
2.1.3 Controlling orifice—A dispensing plug which fits
and the number of drops per container for solutions and
snuggly enough in the mating bottle to form a seal, thereby
suspensions in a specific package system.
forcing all fluid exiting the package to travel through the plug.
2.1.4 Dosing interval—The time period between product
5. Apparatus
dosings. Testing may be performed “as per label directions,”
5.1 For drop size testing solutions and suspensions, the
which means testing is performed at time intervals defined by
following equipment is required:
label directions (for example, once daily).Alternatively, testing
5.1.1 Analytical balance—accurate to 6 0.0001 gram.
may be performed “continuously,” meaning that a shorter time
period between dosing intervals is used in order to expedite
6. Reagents and Materials
testing.
6.1 Bottles, plugs, and closures that are representative of the
desired package system under investigation.
6.2 It is strongly recommended that actual product be used
This test method is under the jurisdiction of ASTM Committee D10 on
for this test. However, it is recognized that in some instances
Packaging and is the direct responsibility of Subcommittee 10.32 on Consumer,
actual product may not be available. In this case a fluid that has
Pharmaceutical, and Medical Packaging.
similar viscosity and dispensing characteristics as the product
Current edition approved Oct. 1, 2004. Published October 2004. DOI: 10.1520/
D7077-04. under investigation should be used.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D7077 – 04
7. Hazards 12.8 Record the Sample Number and the weight of the drop
to the nearest 0.1 mg.
7.1 Any remaining test product should be disposed of in a
12.9 If the product requires more than one drop per dose,
responsible manner.
tare the balance and repeat steps 12.7 and 12.8, according to
7.2 The disposal requirements of the available MSDS for
the number of drops required per dosing interval, recording the
the product, or key ingredients of the product, or both should
weight of each drop dispensed.
be observed in disposal.
NOTE 2—Drops should be dispensed from the test samples in compli-
8. Sampling, Test Specimens, and Test Units
ance with the dosing regimen defined for the product. As an example, if
the labeling indicates one drop in the affected eye, and we assume both
8.1 Ten test samples are recommended for testing. A test
eyes are affected, then two drops would be individually weighed and
sample is defined as a complete unit consisting of the bottle,
measured and then the closure returned to the closed position and the
plug, and closure intended for use; and the package should be
bottle returned to the upright position. This action comprises one dose for
filled with the appropriate fluid. The fill level should be
this product.
consistent with the level intended for market. Unless otherwise
12.10 Replace the closure and store the test sample in an
specified, samples are to be unopened and unused at the
upright position until the next dosing interval.
beginning of the test.
12.11 Repeat steps 12.1-12.10 for each of the remaining test
8.2 The test samples should be labeled with the product
samples. Calculate the average drop size dispensed from each
label and adhesive intended for marketing. The label will add
package per each dosing interval. Record any unusual occur-
stiffness, or a more durable gripping surface, or both; therefore,
rences, e.g., multiple drops, unsolicited drops, bubbling, foam-
it could potentially impact the “squeezability” of the finished
ing, and so forth.
package.
12.12 Continue testing until the data indicate no significant
8.2.1 Number all test samples sequentially.
trends in the average drop size per dosing interval per package,
8.2.2 Prepare each test sample by removing all tamper-
or until product is exhausted, whichever occurs first. A
evident features, (i.e., shrink bands, tamper-evident ring).
minimum of forty drops is recommended to evaluate the data
for significant trends in drop size.
9. Preparation of Apparatus
12.13 Dosing Intervals—The interval or period of time
9.1 Ensure the balance weigh pan is clean and free from
allowed between product dosings for a given package may be
debris.
either “as per label directions,” or “co
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