Standard Operating Procedure (SOP) and Protocol for Calibration of Laboratory Glassware (Class A) like- Volumetric flask, Pipette calibration, Burette calibration used in Quality Control Laboratory for analysis purpose.
Glassware Calibration Procedure
1.0 Purpose:
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- The purpose of this SOP is to describe the procedure for calibration of laboratory glassware.
2.0 Scope:
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- This SOP is applicable for calibration of laboratory glassware used in Quality Control Laboratory.
3.0 References:
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- IP-2020; 2.1.6. Volumetric Glassware
- IP-2020; 2.1.6. Volumetric Glassware
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- Manufacturer COA
4.0 Responsibilities:
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Analyst:
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- To prepare the SOP.
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- To receive and calibrate the glassware as per procedure.
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QC Head or designee:
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- To check the SOP.
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- Impart training to all concerned persons before implementations of SOP.
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- To ensure proper maintenance of respective documents.
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Quality Assurance:
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- To check the SOP.
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- To ensure that implementation of system is as per SOP.
5.0 Procedure for Glassware Calibration:
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- General Procedure:
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- Review the manufactures certificates and put a review stamp on it.
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- To select the glassware (volumetric flask, pipette, burette) for calibration from fresh consignment or as and when required according to √ n+1 method.
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- If the calibration of the above is not within the limit, the consignments shall be returned to party.
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- Numbering of glassware shall be marked as follows :
QC/CAL/Z/YY/XXX
where,
QC = Quality Control
CAL = Calibration
Z = F (Volumetric Flask), P (Pipette), B (Burette)
YY = Last two digit of year (eg;12, for year 2012)
XXX = serial number of glassware
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- Assign calibration ID No to each glassware which to be calibrated, accordingly.
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Precautions during Glassware Calibration:
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- Handle glassware carefully.
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- Use clean and dry glassware for calibration.
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- Pipette/burette should be dried in vertical position and touched against wall of receiving vessel to drain the tips.
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- Use PPE’s such as nose mask, gloves etc. as per requirement during the handling of glassware.
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- Calculation:
%RSD = 100/Xm x [Ʃ(Xi-Xm)²/n-1]½
Xm = Mean value
Xi = Individual value
n = Number of analysis
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Calibration Protocol & Procedure for Volumetric Flask (Glassware):
| Glassware Name | Template Issuance No. | ||
| Make | ID No. | ||
| Nominal Volume | Calibration date |
Calibration Requirement:-
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- Balance Code No.______________ Valid upto _________
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- Digital Thermometer Code No.______________ Valid upto _________
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- Distilled water
Procedure for Volumetric Flask Calibration:-
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- Place the required amount of distilled water in beaker.
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- Allow the temperature of water to equilibrate to room temperature (250C ± 20C).
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- Weigh the dry empty flask on calibrated balance and note down the weight (W1).
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- Record the observed temperature of water before pouring in volumetric flask (T1).
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- Fill the flask to nominal volume with distilled water (25±2°C).
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- Weigh it again and note down the weight (W2).
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- After weighing again record the temperature (T2), the variation in temperature (ΔT) shall not be more than ± 0.50C from the initial temperature of water.
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- Calculate the weight difference (ΔW) between empty flask (W1) and flask with water (W2)
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- Convert weight difference in terms of ml by calculating the wt/ml of water.
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- Calculate the error in ml and percentage.
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- Repeat the above step in triplicate.
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- Calculate the observed volume and relative standard deviation. RSD shall be with in 1.0%.
Calculations:-
Weight difference(gm), ΔW = W2 – W1
Observed Volume (ml), VObserve = ΔW/ D
Volume Difference(ml),ΔV = VNominal – VObserve
ΔV
Relative Error (%) = —————— X 100
VNominal
where,
W1 = Weight of empty flask VNominal = Nominal Volume
W2 = Weight of flask filled with water VObserve = Observe Volume
D = Density of water at 25 0C (0.997 g/ml)
Observations:-
| Sr.
No. |
Water Temp.
(OC) |
Temp.Diff
ΔT(OC) |
Flask Weight
(gm) |
Weight Diff.
ΔW (gm) |
Observe Vol.(ml) | Vol. Diff. ΔV (ml) | Relative Error (%) | ||
| Before Weight (T1) | After
Weight (T2) |
T2 – T1
|
Empty
W1 |
Filled
W2 |
W2 – W1 | VObserve
= ΔW/D
|
VNominal – VObserve | ΔV/VNominal x 100 | |
| Mean | |||||||||
| Limit: NMT 1% |
%RSD |
||||||||
Acceptance Criteria:
| Nominal Volume(ml) | 5 | 10 | 20 | 25 | 50 | 100 | 200 | 250 | 500 | 1000 |
| Class A Tolerance (± ml) | 0.02 | 0.02 | 0.04 | 0.03 | 0.04 | 0.06 | 0.15 | 0.1 | 0.15 | 0.2 |
| Relative Error (± %) | 0.4 | 0.2 | 0.2 | 0.12 | 0.08 | 0.06 | 0.08 | 0.04 | 0.03 | 0.02 |
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Calibration Protocol & Procedure for Pipette (Glassware):
| Glassware Name | Template Issuance No. | ||
| Make | ID No. | ||
| Nominal Volume | Calibration date |
Calibration Requirements:-
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- Balance Code No.______________ Valid upto _________
-
- Digital Thermometer Code No.______________ Valid upto _________
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- Distilled water
Procedures for Pipette Calibration:-
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- Place the require amount of distilled water in beaker.
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- Allow the temperature of water to equilibrate to room temperature (250C ± 20C)
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- Weigh the dry empty beaker on calibrated balance and note down the weight (W1).
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- Record the observed temperature of water before pouring in pipette (T1).
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- Fill the pipette to nominal volume with distilled water (25±2°C).
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- Transfer the filled volume to beaker, weigh it again and note down the weight (W2).
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- After weighing, again record the temperature (T2), the variation in temperature (ΔT) shall not be more than ± 0.50C from the initial temperature of water.
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- Calculate the weight difference (ΔW).
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- Convert weight difference in terms of ml by calculating the wt/ml of water.
-
- Calculate the error in ml and percentage.
-
- Repeat the above step in triplicate.
-
- Calculate the observed volume and RSD shall be within1.0%
Calculations :-
Weight difference(gm), ΔW = W2 – W1 where,
Observed Volume (ml), VObserve = ΔW/ D VNominal = Nominal Volume
Volume Difference(ml),ΔV = VNominal – VObserve VObserve = Observe Volume
ΔV W1 = Weight of empty beaker
Relative Error (%) = ——– X 100 W2 = Weight of beaker filled with water
VNominal D = Density of water at 25 0C (0.997 g/ml)
Observations:-
| Sr.
No. |
Water Temp.
(OC) |
Temp.Diff
ΔT(OC) |
Beaker Weight
(gm) |
Weight Diff.
ΔW (gm) |
Observe Vol.(ml) | Vol. Diff. ΔV (ml) | Relative Error (%) | ||
| Before Weight (T1) | After
Weight (T2) |
T2 – T1
|
Empty
W1 |
Filled
W2 |
W2 – W1 | VObserve
= ΔW/D
|
VNominal – VObserve | ΔV/VNominal x 100 | |
| Mean | |||||||||
| Limit: NMT 1% | % RSD | ||||||||
Acceptance Criteria:
| Nominal Volume (ml) | 1 | 2 | 5 | 10 | 20 | 25 | 50 | 100 |
| Class A One Mark Pipettes | ||||||||
| Tolerance (± ml) | 0.01 | 0.01 | 0.02 | 0.02 | 0.03 | 0.03 | 0.04 | 0.06 |
| Relative Error (± %) | 1 | 0.5 | 0.4 | 0.2 | 0.15 | 0.12 | 0.08 | 0.06 |
| Class A Graduated Pipettes | ||||||||
| Subdivision (ml) | 0.01 | 0.02 | 0.05 | 0.1 | — | 0.2 | — | — |
| Tolerance (± ml) | 0.006 | 0.01 | 0.03 | 0.05 | — | 0.1 | — | — |
| Relative Error (± %) | 0.6 | 0.5 | 0.6 | 0.5 | — | 0.4 | — | — |
| Nominal Volume (ml) | 3 | 4 | 6 | 9 | 15 | — | — | — |
| Class A One Mark Pipettes | ||||||||
| Tolerance (± ml) | 0.01 | ±0.01 | 0.01 | 0.02 | 0.03 | — | — | — |
| Relative Error (± %) | 0.3 | 0.3 | 0.2 | ±0.2 | 0.2 | — | — | — |
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Calibration Protocol & Procedure for Burette (Glassware):
| Glassware Name | Template Issuance No. | ||
| Make | ID No. | ||
| Nominal Volume | Calibration date |
Calibration Requirements:-
-
- Balance Code No.______________ Valid upto _________
-
- Digital Thermometer Code No.______________ Valid upto _________
-
- Distilled water
Procedures for Burette Calibration :-
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- Place the require amount of distilled water in beaker. Allow the temperature of water to equilibrate to room temperature (250C ± 20C)
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- Take the weight of empty beaker (W1).
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- Record the observed temperature of water before pouring in pipette (T1).
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- Fill the burette to nominal volume with distilled water (25±2°C).
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- Transfer the volume to beaker, weigh it again and note down the weight (W2).
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- After weighing, again record the temperature (T2), the variation in temperature (ΔT) shall not be more than ± 0.50C from the initial temperature of water.
-
- Calculate the weight difference (ΔW).
-
- Convert weight difference in terms of ml by calculating the wt/ml of water.
-
- Calculate the error in ml and percentage.
-
- Repeat the above step in triplicate.
-
- Calculate the observed volume and relative standard deviation.
-
- RSD shall be with in 1.0%.
Calculations:-
Weight difference(gm), ΔW = W2 – W1 where,
Observed Volume (ml), VObserve = ΔW/ D VNominal = Nominal Volume
Volume Difference(ml),ΔV = VNominal – VObserve VObserve = Observe Volume
ΔV W1 = Weight of empty beaker
Relative Error (%) = ——– X 100 W2 = Weight of beaker filled with water
VNominal D = Density of water at 25 0C (0.997 g/ml)
Observations :-
| Sr.
No. |
Water Temp.
(OC) |
Temp.Diff
ΔT(OC) |
Beaker Weight
(gm) |
Weight Diff.
ΔW (gm) |
Observe Vol.(ml) | Vol. Diff. ΔV (ml) | Relative Error (%) | ||
| Before Weight (T1) | After
Weight (T2) |
T2 – T1
|
Empty
W1 |
Filled
W2 |
W2 – W1 | VObserve
= ΔW/D
|
VNominal – VObserve | ΔV/VNominal x 100 | |
| Mean | |||||||||
| Limit: NMT 1% | %RSD | ||||||||
Acceptance Criteria:
| Nominal Capacity (ml) | 10 (micro) | 25 | 50 | 100 |
| Subdivision (ml) | 0.05 | 0.05 | 0.1 | 0.1 |
| Class A Tolerance (± ml) | 0.01 | 0.03 | 0.05 | 0.1 |
| Relative Error (± %) | 0.1 | 0.12 | 0.1 | 0.1 |
Attachment : Volumetric flask calibration log book
|
Sr. No |
Receiving date | Date of calibration | Nominal volume | Calibration ID | Calibrated By |
Checked By |
Attachment : Pipette calibration log book
|
Sr. No |
Receiving date | Date of calibration | Nominal volume | Calibration ID | Calibrated By |
Checked By |
Attachment : Burette calibration log book
|
Sr. No |
Receiving date | Date of calibration | Nominal volume | Calibration ID | Calibrated By |
Checked By |
Attachment : Template issuance log book
|
Sr. No |
Date of issuance | Protocol issuance No | Glassware/
Volume |
Glassware code No | Glassware calibration ID No | Issued By | Received By |
Remark |
