9 QUALITY SYSTEM MANUAL CORPORATE QUALITY aan Guideline # 019/02R3 ‘Supersedes : 019/02R2 Page | of 13 Title: Guideline for the Calibration of the Analytical Balance. GUIDELINE PREPARATION HISTORY SHEET EVENT | _iDATE DISCUSSION IN THE CQ GROUP. 04/12/2009 RELEASE FOR CONSULTATION 05/12/2009 DEADLINE FOR COMMENTS. 12/12/2009 DISCUSSION IN THE CQ GROUP. 18/12/2009 ADOPTION BY CQ. — 2612.) 2009 DATE FOR COMING INTO OPERATION Lofot[2alo NEXT REVIEW DATE 10 Jot jaa9 QUALITY SYSTEM MANUAL SUN CORPORATE QUALITY Guideline # 019/02R3 | Supersedes 2019/02R2 Page 2 of 13 | Title: Guideline for the Calibration of the Analytical Balance. 1 Title Guideline for the Calibration of the Analytical Balanee. 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 eheeks and inspections shall be mi ‘The purpose of this guideline is to deseribe 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 ean be established. Scope This guideline is applicable for the Calibration of the Mettler Analytical Balance, Microbalance and other analytical weighing balances. 4 References & Attachments Al References 4.1.1 United States Pharmacopoeia <41> Weights and Balances <1251> Weighing on analytical balance 412 21CFR 211.68 4.2 Attachments 421 Attchment—1 Format for Performance Check Log of Analytical balance 422 — Attachment-2 — Format for Measurement Uncertainty Check Log 423 Attachment—3 Format for Performance check log of Microbalanee, 424 Attachment~4 — Format for Auto performance check log of Microbalance. 4. Attachment—5 — Format for Measurement uncertainty check of Microbalance: Responsibilities Location Quality Head 5.1.1 To ensure this guideline is implemented at the location.9 QUALITY SYSTEM MANUAL SUN CORPORATE QUALITY at Guideline # 019/02R3 Supersedes : 019/02R2 Page 3 of 13 Title: Guideline for the Calibration of the Analytical Balance. 6 Procedure The operating range of the balance shall be established based on manufacturer's manual, It should be displayed on the balance prominently, The calibration shall cover the entire working range of the balance. 61 CALIBRATION PROCEDURE OF THE METTLER ANALYTICAL BALANCE ( CAPACITY : 20 MG - 200 GM) he ealibration shall consist of the following parameters. © Internal calibration Measurement uncertainty check Performance cheek and Drifi" check. Before calibration the balance shall be in exactly horizontal position, If any unevenness is observed in its location, it shall be corrected by tuming two leveling feet until the level bubble is in the center of the indicator. 61d Calibration frequency: + Internal calibration: It shall be performed on every working day, after any maintenance, after power failure and afer the relocation of the balance, . Measurement uncertainty check: 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. sror3, and itis also one of the easiest to reduce or eliminate. Balance drift ean be present withou 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 Drift is one of the most commor . ‘A balance door is open . Temperatures of the balance and the material ta be weighed are not the same: ° ‘The sample is losing or gaining welghe . . ‘The balance has been recently moved but has net heen allowed to equilibrate to its surrounding or lisy not been recalibrate, ° ‘Air currents are present in the laboratory . Femperatures 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 itis primarily due to overloading or to the accidental dropping of an abject onto the pan.)SUN CORPORATE QUALITY Guideline # 19/02R3 Supersedes : 019/022 | Page 4 of 13 Title: Guideline for the Calibration of the Analytical Balance. © Drift check: It shall be performed on every working day, after any maintenance and after the relocation of the balance 6.12 Calibration procedure: 6.1.2.1 Internal calibration It shall be performed as per the manufacturer's instructions, 6.1.2.2 Drift check Follow the manufacture’s operating instructions Place the weight" in the center of the pan to eliminate corner- weighing differences. In the calculation of the drift the aceuracy 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 40.2 mg. E.g.. with a 100 gm weight, if the mean value of the readin 99.9984g. the tolerance would be from 99.9982 to 99.9986 g. were All the 10 measurements of 100 gm weight shall meet the performance check criteria of the mass value ie, 0.1% of actual mass value, 6.123 Performance check Afier the Auto calibration put 20 mg, 500 mg, 1 g, and 200. gm wei individually. ‘The measurement shall be within the 0.1% of actual mass value of the individual weight as given in the performance check log. Note: Mg weight performance check shall be done on the mg scale of the balance and ym weight performance check shall be done on the gm seale of the balance. A weigitt 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 muss value of the weigh shall be used. The weights used for calibration shall be calibrated against standard weights traceable to NIST The tolerance doesn't correspond to the valve of 0.1% for weighing material accurately. Rather. the tolerance is purposelully tiubt to revea! possible drift or calibration errors9 QUALITY SYSTEM MANUAL SUN CORPORATE QUALITY na Guideline 4 019/02R3 Supersedes : 019/02R2 Page 5 of 13 Title: Guideline for the Calibration of the Analytical Balance 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 my on this type of balance should not be used for the quantitative estimation 6.1.2.4 Measurement uncertainty check ‘The meesurement uncertainty shall be 100 am weight arried owt by using 500 mg and Put the external weight of 300 mg on the pan and note the 10 measurements in the measurement uncertaimy check log (Attachment no. 02) Calculate the measurement of uncertainty as follows, Measurement uncertainty Standard deviation x 3 Actual weight of Standard weight Measurement of uncertainty shall be Not More Than 0.001." Carryout the same procedure for 100 gm weight. 6.2 CALIBRATION OF MICROBALANCE: ( CAPACITY 1 MG TO 20 MG) The calibration shall consist of the following parameters. Intemal calibration © Measurement uncertainty cheek © Performance check and © Drift cheek Before calibration make sure that the level bubble is in the center of the indicator. 6.21 Calibration frequency: Internal calibration: It shall be performed on every working day, after any maintenance, after power failure and after the relocation ef the balance Measurement of uncertainty: {t shall be performed monthly, after any maintenance and after the relocation of the balance. Fora number 0.001 to be significant at 0.001, the uncertainty ofthe final digit is + 0.0008, ie) the actual figuce has @ 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, wren substances are wo be “accurately hed” fon apsay, the weighing is to be performed with a weighing device whose measurement uncertainty (random plus systematic error) doesn’t exceed 0,1% of the read9 QUALITY SYSTEM MANUAL, SUN CORPORATE QUALITY Guideline # 019/02R3 Supersedes : 019/02R2 Page 6 of 13 Title: Guideline for the Calibration of the Analytical Balance. 622 6222 62.23 6224 Always use a check w Performance check: It shall be performed on every working day, after any maintenance, aller power failure and alter the relocation of the balance Drift cheek: It shall be performed on every working day maintenance and afier the relocation of the balance after any Calibration procedure: Internal calibration Ic shall be performed as per the manufacturer's instructions Drift check For the calculation of the deift 10 mg weight*shall be used Note dowa 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 2 mg. The 10 my weight shall meet the performance check criteria of the mass Value i.e, 0.1% of actual mass value, Eg. For all the 10 measurements of 10 mg weight, variation in the weighings cannot exceed 0.01 mg Performnee check Afier the Auto calibration put 1 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 (Attachment no. 04) ven in the performance check | 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 fallows. Measurem nt uncertainty = Standard deviation _x_3 Actual weight of Standard weight ight appropriate for tne particular balance, E.. 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 ct check weight9 SUN UALITY SYSTEM MANUAL CORPORATE QUALITY Guideline # 019/02R3 Supersedes : 019/02R2 Page 7 of 13 Title: Guideline for the Calibration of the Analytical Balance, 623 Measurement of uncertainty shall be Not More Than 0.001. CALIBRATION OF TOP PAN BALANCE Calibration frequency: It shall be performed daily, after any maintenance, after the relocation and afier 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 chat 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 cheek of the balanceS SUN QUALITY SYSTEM MANUAL, CORPORATE QUALITY | Guideline # 019/02R3 Supersedes : 019/02R2 Page 8 of 13 | Title: Guideline for the Calibrati ion of the Analytical Balance GUIDELINE [HISTORY GUIDELINE | EFFECTIVE | SUPERSEDES | SUPERSEDES | REASON FOR REVISION NO. DATE DATE oreaRT | ~ 36/04/2005 | 00019702 2002 Balance calibration procedure _ updated as per USP-28.2005. | + O19/02R2 10/10/2007, 019/02R1 26/04/2005 Editorial change in the Purpose, Change in reference, Reduction in weight check in performance qualification of Mettler analytical balance ond - Mierobalance 019/02R3 toler |2o10 019/02R2. 10/10/2007 | Reference updated as per Current USP | On page 4 note added for | weights to be calibrated against standard wt traceable to NIST Prepared by Poongm Sikerwg we (oe Date: 18}}] ©F Reviewed by: Rahul songire ei Date: 2.6 | 12/2004 Appioved by: Vipul Doshi puree ee ae |ite4QUALITY SYSTEM MANUAL CORPORATE Supersedes : None Attachment No. - 01 - Performance C nee Instrument: Analytical balance Code Ni 3 Make : Mettler Model : Left side of the log book Date | Level Daifi': 100.0 (zm) ‘Auto Actual mass v ‘Actual mass value \dicator calibration | 200.0000 (em) 1.00000 (am) : check Limit + 0.2 mg of Mean value 200 gm. imit (199.8000 | 1 ( 0,999 => gm to 200.20000 gm to 1.00100 um) em) Mean: Variation => Maximum em. and Minimum : ny ihe log book F weight eight box No. & | Done by Checked Remark by ‘Attach print out jue 20.00 (me) v ‘Actual mass value $00.00 (mg): | Actual m: Timi (49950 mg t[limiz( 1998 mgt 20.02 500.50 _mg) mg) —_ Attach print out of weight ated considering theoretical mass value. In same way limits should be calculated considering actual mass value of theO2R1 Supersedes : None rement Uncertainty Check Log. Instrument Code No. Make Model Date | Weight used Dbserved Weight Done by Remark 500 mg 100.0000 g of weight Standard de’ Actual weightQUALITY SYSTEM MANUAL CORPORATE QUALITY srsedes : None 902R1 ne Ci al Balance Attachment-(3; Performance Cheeks Log of Mierobalance Instrument: Make Date Ting img 20mg Doneby [+ Checked Remark b Std. Wt. Cal No. => Limit ] Bubble should [~~ 4 +01% OFS = beinCenter | Sid. Weight Weight (0.9990 mg | (9.9900 mg wo to 10.0100 mg | to 20.0200 mg } ) ed considering actual mass value of the dering theoretical mass value, In same way Note: Limits are calculated c1QUALITY SYST CORPORATE QUALITY [ss persedes : None Attachment-4: Auto Performance Cheek Log of Microbalance Instrument: Make 3 Cheek level indicator (Bubble should be in center) : (Paste Performance check printout here) Calibrated by = Date: Checked by Date:5 SUN 1 # O1902RL e Cal Attachment-(5: Measurement Uneertainity Chee! Instrument: Code No: Make: Model: Sd Wi | Sid Wi Observation of | Weight Remark Cal. No. Uncertainty box no. Less than or equal to 0.001 10me | neertainty = Standard dey Actual weight of Standard weight Measurement