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EVENT DATE
DISCUSSION IN THE CQ GROUP 03/03/2005
RELEASE FOR CONSULTATION 08/03/2005
DEADLINE FOR COMMENTS 08/04/2005
DISCUSSION IN THE CQ GROUP 25/04/2005
ADOPTION BY CQ 25/04/2005
DATE FOR COMING INTO OPERATION 26/04/2005
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2 Purpose 21 CFR 211.68 , Automatic, mechanical and electronic equipment mentions that
the equipments used shall be routinely calibrated, inspected or checked
according to a written programme designed to assure proper performance. Written
records of those calibration checks and inspections shall be maintained.
Weighing is a frequent step in the analytical procedures, and the balance is an
essential piece of laboratory equipment in most analysis as Pharmacopoeial tests
and assays require balances that vary in capacity, sensitivity and reproducibility.
Thus the weighing should not only be very precise and accurate but also should
meet stringent Pharmacopoeial as well as regulatory requirements and weighing is
no longer as simple as it used to be.
The purpose of this guideline is to describe the calibration procedure of the
balances. The detailed calibration procedure of the Mettler analytical balance
and microbalance is explained in this guideline. Based on this thinking the
calibration procedure of other balances can be established.
3 Scope This guideline is applicable for the Calibration of the Mettler Analytical
Balance, Microbalance and other analytical weighing balances.
References
3.1.1 United States Pharmacopoeia 28, 2005.
3.1.2 21 CFR 211.68
Attachments
3.2.1 Attachment Format for Performance Check Log of Analytical balance.
1
3.2.2 Attachment Format for Measurement Uncertainty Check Log.
2
3.2.3 Attachment Format for Performance check log of microbalance.
3
3.2.4 Attachment Format for Auto performance check log of microbalance.
4
3.2.5 Attachment Format for Measurement uncertainity check of
5 microbalance.
5 Responsibilities
Location Quality Head
3.3.1 To ensure this guideline is implemented at the location.
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Procedure
The operating range of the balance shall be established based on manufacturers
manual. It should be displayed on the balance prominently. The calibration shall cover
the entire working range of the balance.
Drift is one of the most common errors, and it is also one of the easiest to reduce or eliminate. Balance drift can be
present without the operators being aware of the problem. Check the sample, the balance, and the laboratory
environment for the following causes of errors, and eliminate them:
A balance door is open.
Temperatures of the balance and the material to be weighed are not the same.
The sample is losing or gaining weight.
The balance has been recently moved but has not been allowed to equilibrate to its surroundings or has
not been recalibrated.
Air currents are present in the laboratory.
Temperatures in the laboratory vary.
The balance is not properly leveled.
Laboratory operations are causing vibration.
Hysteresis of the mechanical parts occurs during weighing. (Note: Hysteresis in the balance is caused
by excessive stretching of the springs, and it is primarily due to overloading or to the accidental dropping of an
object onto the pan.)
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In the calculation of the drift the accuracy is not important but the only
factor of interest is whether the drift has occurred.
Variation in the observed weight from the mean value does not exceeds
0.2 mg.
E.g., with a 100 gm weight, if the mean value of the readings were
99.9984g, the tolerance would be from 99.9982 to 99.9986 g.
Put the external weight of 500 mg on the pan and note the 10 measurements
in the measurement uncertainty check log (Attachment no. 02)
A weight class chosen for calibration is so that the tolerance of the weights used doesnot exceeds 0.1% of the amount
weighed. Weights should be calibrated yearly, preferably against an absolute standard weight. In the measurement
uncertainty, drift and performance check the actual mass value of the weight shall be used.
The tolerance doesnt correspond to the value of 0.1% for weighing material accurately. Rather, the tolerance is
purposefully tight to reveal possible drift or calibration errors.
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Measurement uncertainty =
For a number 0.001 to be significant at 0.001, the uncertainty of the final digit is 0.0005, i.e. the actual figure has a
potential true value of anywhere from 0.0005 to 0.0015. The MU of 0.00149 cited would meet the specification because
it falls within the limits stated and unless otherwise specified, when substances are to be accurately weighed for assay,
the weighing is to be performed with a weighing device whose measurement uncertainty (random plus systematic error)
doesnt exceed 0.1% of the reading.
Always use a check weight appropriate for the particular balance. E.g. a 100 mg check weight might be selected for
a balance that has a load limit of 150 mg. Thus the operator must know the maximum capacity of the balance to select
the correct check weight.
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Variation in the observed weight from the mean value does not exceeds
0.2 mg.
The 10 mg weight shall meet the performance check criteria of the mass
value i.e. 0.1% of actual mass value.
E.g. For all the 10 measurements of 10 mg weight, variation in the
weighings cannot exceed 0.01mg.
Put the external weight of 10 mg on the pan and note the 10 measurements.
(Attachment no. 05)
Measurement uncertainty =
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Date Weight used Weight Box Observed Weight Measurement Done by Checked Remark
No. & Valid uncertainty by
up to Limit: NMT
0.001
500 mg
100.0000 g
Calculation
Measurement uncertainty =
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Date Std. Wt. Std. Wt. Observation Observation of Weight Done Check Remark
Cal. No. Uncertainty box no. by ed by
Less than or equal to and
0.001 valid
upto
10 mg
Calculation
Measurement uncertainty =
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GUIDELINE HISTORY
Prepared by: Rahul Songire. Reviewed by: Bhavesh Shah Approved by: