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Guideline # 00019/02R1 Supersedes : None Page 1 of 13

Title: Guideline for the Calibration of the Analytical Balance.

GUIDELINE PREPARATION HISTORY SHEET

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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Guideline # 00019/02R1 Supersedes : None Page 2 of 13

Title: Guideline for the Calibration of the Analytical Balance.

1 Title Guideline for the Calibration of the Analytical Balance.

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.

4 References & Attachments

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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Guideline # 00019/02R1 Supersedes : None Page 3 of 13

Title: Guideline for the Calibration of the Analytical Balance.

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.

CALIBRATION PROCEDURE OF THE METTLER ANALYTICAL


BALANCE ( CAPACITY : 20 MG - 200 GM)

The calibration shall consist of the following parameters.


7 Internal calibration
8 Measurement uncertainty check
9 Performance check and
10 Drift check.
Before calibration the balance shall be in exactly horizontal position. If any
unevenness is observed in its location, it shall be corrected by turning two
leveling feet until the level bubble is in the center of the indicator.

10.2.1 Calibration frequency:


11 Internal calibration: It shall be performed on every working day, after any
maintenance, after power failure and after the relocation of the balance.

12 Measurement uncertainty check: It shall be performed monthly, after any


maintenance and after the relocation of the balance.

13 Performance check: It shall be performed on every working day, after any


maintenance, after power failure and after the relocation of the balance.

14 Drift check: It shall be performed on every working day, after any


maintenance and after the relocation 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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Guideline # 00019/02R1 Supersedes : None Page 4 of 13

Title: Guideline for the Calibration of the Analytical Balance.

14.2.1 Calibration procedure:


14.2.1.1 Internal calibration
It shall be performed as per the manufacturers instructions.
14.2.1.2 Drift check
Follow the manufactures operating instructions.
Place the weight in the center of the pan to eliminate corner- weighing
differences.

In the calculation of the drift the accuracy is not important but the only
factor of interest is whether the drift has occurred.

For the calculation of the drift 100 gm weight shall be used.

Note down the 10 measurements of the 100 gm weight in the performance


check log. ( Attachment no. 01)

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.

All the 10 measurements of 100 gm weight shall meet the performance


check criteria of the mass value i.e. 0.1% of actual mass value.

14.2.1.3 Performance check


After the Auto calibration put 200 g, 100 g, 50 g, 5 g, 500 mg, 100 mg and
20 mg weights individually. The measurement shall be within the 0.1% of
actual mass value of the individual weight as given in the performance
check log.
If the least count of the analytical balance is 0.1 mg then the performance
check should be done by using the weights of 100 mg and more. The
weights weighed below 100 mg on this type of balance should not be used
for the quantitative estimation.
14.2.1.4 Measurement uncertainty check
The measurement uncertainty shall be carried out by using 500 mg and 100
gm weight.

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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Guideline # 00019/02R1 Supersedes : None Page 5 of 13

Title: Guideline for the Calibration of the Analytical Balance.

Calculate the measurement of uncertainty as follows.

Measurement uncertainty =

Measurement of uncertainty shall be Not More Than 0.001.


Carryout the same procedure for 100 gm weight.
14.3 CALIBRATION OF MICROBALANCE: ( CAPACITY 1 MG TO 20 MG)
The calibration shall consist of the following parameters.
15 Internal calibration
16 Measurement uncertainty check
17 Performance check and
18 Drift check.
Before calibration make sure that the level bubble is in the center of the
indicator.

18.2.1 Calibration frequency:


Internal calibration: It shall be performed on every working day, after any
maintenance, after power failure and after the relocation of the balance.

Measurement of uncertainty: It shall be performed monthly, after any


maintenance and after the relocation of the balance.

Performance check: It shall be performed on every working day, after any


maintenance, after power failure and after the relocation of the balance.

Drift check: It shall be performed on every working day, after any


maintenance and after the relocation of the balance.

18.2.2 Calibration procedure:


18.2.2.1 Internal calibration
It shall be performed as per the manufacturers instructions.
18.2.2.2 Drift check
For the calculation of the drift 10 mg weight shall be used.

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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Guideline # 00019/02R1 Supersedes : None Page 6 of 13

Title: Guideline for the Calibration of the Analytical Balance.

Note down the 10 measurements of the 10 mg weight in the performance


check log. ( Attachment no. 03)

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.

18.2.2.3 Performnce check


After the Auto calibration put 1 mg, 2 mg, 5 mg, 10 mg and 20 mg weights
individually. The measurement shall be within the 0.1% of actual mass
value of the individual weight as given in the performance check log.
( Attachment no. 04)

18.2.2.4 Measurement uncertainty check


The measurement of uncertainty shall be carried out by using 10 mg weight.

Put the external weight of 10 mg on the pan and note the 10 measurements.
(Attachment no. 05)

Calculate the measurement of uncertainty as follows.

Measurement uncertainty =

Measurement of uncertainty shall be Not More Than 0.001.


18.2.3 CALIBRATION OF TOP PAN BALANCE
Calibration frequency: It shall be performed daily, after any maintenance,
after the relocation and after the power failure of the balance.

Each manufacturer supplies the maximum loading condition of the balance.


The calibration of the balance shall be designed in such a way that the
performance check weights cover the entire loading range of the balance.
Lower and higher load limits shall be checked for the performance check.
Before calibration make sure that the level bubble is in the center of the
indicator and if internal calibration facility is available in the balance then it
shall also be performed daily before performance check of the balance.
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Guideline # 00019/02R1 Supersedes : None Page 7 of 13

Title: Guideline for the Calibration of the Analytical Balance.


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Guideline # 00019/02R1 Supersedes : None Page 8 of 13

Title: Guideline for the Calibration of the Analytical Balance.

Attachment No. - 01 - Performance Check Log of Analytical balance


Instrument : Analytical balance Code No. :
Make : Mettler Model :
Left side of the log book
Date Level Drift : 100.0 (gm) Auto Actual Actual mass Actual mass value
indicator calibration mass value 50.0000 (gm) :
check value 100.0000
200.0000 (gm) :
(gm) :
Limit Bubble should 0.2 mg of Mean value 200 gm Limit: ( Limit: Limit: ( gm to
be in Center gm to ( gm to gm )
gm ) gm )
Mean:

Variation Maximum : gm , and


Minimum : gm
Right side of the log book
Attach print out of weight
Actual mass value Actual mass value Actual mass value Actual mass Weight box No. Done Checked Remark
5.0000 (gm) : 0.5000 (gm) : 0.1000 (gm) : value 0.0200 & Valid up to by by
(gm) :
Limit: ( gm to Limit: ( gm to Limit: ( gm to Limit: ( gm to
gm ) gm ) gm ) gm )

Attach print out of weight


Attachemt-2
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Guideline # 00019/02R1 Supersedes : None Page 9 of 13

Title: Guideline for the Calibration of the Analytical Balance.

Attachment No. 02 - Measurement Uncertainty Check Log

Instrument : Analytical balance Code No. :


Make : Mettler Model :

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

Attach the print out of weight.

Calculation
Measurement uncertainty =
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Guideline # 00019/02R1 Supersedes : None Page 10 of 13

Title: Guideline for the Calibration of the Analytical Balance.

Attachment-3: Performance Check Log of Microbalance

Instrument:_____________________ Code No :______________

Make :_____________________ Model :_______________

Date Level 1 mg 2 mg 5 mg 10 mg 20 mg Weight Done by Checked Remark


indicator box no. by
check and
Std. Wt. Cal No. valid
upto
Limit Bubble + 0.1% of + 0.1% of + 0.1% of + 0.1% of + 0.1% of
should be in Std. Weight Std. Weight Std. Weight Std. Weight Std. Weight
Center ( to ) ( to ) ( to ) ( to ) ( to )
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Guideline # 00019/02R1 Supersedes : None Page 11 of 13

Title: Guideline for the Calibration of the Analytical Balance.

Attachment-4: Auto Performance Check Log of Microbalance

Instrument:_____________________ Code No :______________


Make :_____________________ Model :_______________
Check level indicator (Bubble should be in center) : ____________________________________________

(Paste Performance check chart here)

Calibrated by : _______________ Date : ____________________


Checked by : _______________ Date : ____________________
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Title: Guideline for the Calibration of the Analytical Balance.

Attachment-5: Measurement Uncertainity Check of Microbalance

Instrument:_____________________ Code No :______________

Make :_____________________ Model :_______________

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 # 00019/02R1 Supersedes : None Page 13 of 13

Title: Guideline for the Calibration of the Analytical Balance.

GUIDELINE HISTORY

GUIDELINE EFFECTIVE SUPERSEDES SUPERSEDES REASON FOR REVISION


NO. DATE DATE
00019/02 2002 None NA Balance calibration procedure
updated as per USP-28, 2005.

Prepared by: Rahul Songire. Reviewed by: Bhavesh Shah Approved by:

Date: Date: Date:

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