D-725

Loss on Drying

Section D — Laboratory Operations and Specifications Revision 6 8 pages

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1.0 Purpose

The purpose of this procedure is to define the process used for the determination of volatile
chemical loss during drying under a specified set of conditions.

2.0 Scope

This procedure applies to the determination of loss on drying as a percentage of weight for
powder samples. This procedure follows Loss on Drying USP<731> guidelines. Unless

otherwise noted in a monograph or pharmacopeia, LOD should only be performed on solids

whose melting point is above the temperature used for drying. Other forms of moisture
determination should be used when this is not the case.

3.0 Responsibility

3.1 It is the responsibility of QC and Analytical Chemists to follow this procedure.

3.2 It is the responsibility of QC Laboratory Management to implement this procedure and
to ensure that the procedure is being followed.

3.3. «It is the responsibility of QC Laboratory and/or Analytical Development Management

to keep this procedure current with latest Ion Labs practices.

4.0 Definitions

4.1 LOD — Loss on Drying

4.2 QC - Quality Control

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Loss on Drying

5.0 References

5.1 D-725-F1, Form, LOD Test Record

5.2. D-725-F2, Form, Halogen Moisture Analyzer Test Record

5.1 | USP<731>, Method, Loss on Drying

6.0 Procedure

6.1 Equipment

6.1.1 WWRSymphonyTM Vacuum oven or equivalent

6.1.2 Mettler Toledo Halogen Moisture Analyzer HE73 or equivalent

6.1.3 ’%4HP vacuum pump

6.1.4 Analytical Balance

6.1.5 Temperature probe

6.2 Supplies

6.2.1 30mL 34/12 Kimax Weigh Bottle or equivalent

6.2.2 Watch Glass, 12.5cm diameter

6.2.3 Mettler Toledo SmartCal Sachets

6.2.4 Aluminum Sample Pans

6.3 Testing — Drying Oven

Note: If a monograph is available to give conditions for testing LOD for a material

then the monograph conditions supersede Ion Labs standard conditions.

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Loss on Drying

63.1 Equilibrate the oven to 105°C or appropriate temperature. Use a calibrated
digital thermometer to confirm temperature of oven.

6.3.2 If the melting point of the sample is below 105°C then adjust temperature 5 to
10°C below the melting point.

63.3 Dry a clean watch glass or Weigh Bottle before adding sample.

6.3.4 Weigh a clean and dry watch glass or weigh bottle on the analytical balance.

6.3.5 Print the tare weight of the watch glass or weigh bottle.

6.3.6 Mix the substance to be tested and, if it is in the form of large particles, reduce

the particle size to about 2 mm by crushing before weighing. Apply a 1 to 2 g

test sample to the tared container.

6.3.7 By gentle, sidewise shaking, distribute the test specimen as evenly as practicable

to a depth of about 5 mm generally, and NMT 10 mm in the case of low bulk
density materials.

6.3.8 Print the sample weight.

6.3.9 The weight of the tare and sample is the initial weight.

6.3.10 Place the open container holding sample into a pre-equilibrated oven.

6.3.11 If necessary, apply 20 +/- 4 inches of vacuum and dry for 2 hours. Once

vacuum is applied, ensure oven temperature is at testing conditions.

6.3.12 After allotted time, be sure to cap samples to keep them from drawing moisture

from the air and move the sample to a desiccator to cool for 20 minutes or until

the sample has equilibrated to room temperature. Use caution when moving
samples as they may be hot. Weigh the sample again after cooling. This is the

final weight of container and sample.

6.3.13 Print the final container and sample weight.

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Loss on Drying

6.3.14 The % LOD is determined by the following equation:

initial weight — final weight
%LOD = x 100%
sample weight

6.3.15 Record results on Form D-725-F1 LOD Test Record.

6.4 Cautionary Measures when using a drying oven

6.4.1 Cautionary measures should be taken when drying multiple samples

concurrently.

6.4.2 A recommended maximum of 10 samples should be dried in the oven at the

same time.

6.4.3 Care should be taken when drying samples with higher moisture content with

those containing lower moisture contents and hygroscopic in nature.

6.5 Testing - Halogen Moisture Analyzer

6.5.1 Monthly Check

6.5.1.1 Level Instrument.

6.5.1.2 Place empty sample pan into the sample pan handler. Place sample

pan handler into the draft shield, ensuring the tongue of the sample pan
handler lies exactly in the slot of the draft shield. The pan must lie flat

in the pan holder.

6.5.1.3 Close lid. The instrument will tare automatically.

6.5.1.4 Remove a SmartCal stick from blister pack, open and distribute
contents evenly over the sample pan. Close lid.

6.5.1.5 Press menu and select “CAL”. In “CAL” menu, select “S.CAL”.

6.5.1.6 Set temperature that closely matches the preferred application.

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Loss on Drying

Confirm entry with the backwards arrow button.

6.5.1.7 Compare the test results to the below table and evaluate whether the

result meets the control limits

3} ¥ x ‘A =|f Steeys)h ases teesaaoee Fs $,. g|E RTESSE Je?BSS* ee SSSPh ESAGSSs
‘ a c T S. A i aE 4’ RIZRAIE J SS NS: 5 es x5 sy Re : Measnasaneens ei
2-4.4%
°
5.2 — 6.4%
7.4 — 8.8%
9.9 —11.7%
6.5.1.8 Capture monthly check in instrument logbook/ notebook.
6.5.1.9 If the test falls outside of the above control limits, take the following

measures:

6.5.1.9.1 After instrument has cooled down, repeat the test and

ensure all steps have been carried out correctly.

6.5.1.9.2 If the failure persists, perform a temperature and weight

adjustment and perform an additional SmartCal test.

6.5.1.9.3 If the result continues to fail, reference Troubleshooting

guide in instrument manual.

6.5.2 Performing a simple measurement

6.5.2.1 Let instrument warm up for one hour.

6.5.2.2 Place empty sample pan into the sample pan handler. Place sample
pan handler into the draft shield, ensuring the tongue of the sample pan

handler lies exactly in the slot of the draft shield. The pan must lie flat
in the pan holder.

6.5.2.3 Close lid. The instrument will tare automatically.

6.5.2.4 Open lid and place specimen into sample pan. A minimum of 0.5

grams of sample is required. Ensure the sample is distributed evenly to

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Loss on Drying

obtain good analysis results.

6.5.2.5 Close the heating module lid. The drying and measuring process starts

automatically.

6.5.2.6 Results will automatically print.

6.5.2.7. Capture results on Form D-725-F2 Halogen Moisture Analyzer Test
Record.

7.0 Revision History

| Rev | Date | Description of Changes | CCR # | By |
|-----|----------|------------------------|-------|----|
| 0 | 10/05/10 | New procedure. ~ - l 01/26/12 Updated SOP format - - | - | - |
| 2 | 02/21/13 | Reformatted = ‘ Two forms added, updated instrument and supply information, more | - | - |
| 3 | 08/28/13 | detailed instruction on use of the vacuum oven and electronic moisture analyzer, removed USP <921> references Biennial review: Reformatted SOP. Removed electronic moisture | 13-764 | B. Johns |
| 4 | 01/05/16 | analyzer instructions and form. Added use of temperature probe. Added tolerances. | 16-0023 | N. Zhang |
| 5 | 02/04/19 | peak review: updated responsibilities, fixed typos, clarified | 19-0117 | J. Maipnan |
| 6 | 06/06/22 | Update to reflect current practices. Added additional instruction to CC- incorporate Halogen Moisture analyzer. Updated logo and format. | 22-0159 | J. Sassman |

[SOP

IANLABS LOD Test Record
Form: D-725-F 1 CCR No. CC-22-0159 Revision: 4

(Initial Weight - Final Weight) X 100
Sample Weight

Determination (circle one): Pass Fail
Comments:

Performed By/Date:

Reviewed By/Date:

[SOP

IANLABS Halogen Moisture Analyzer Test Record
Form: D-725-F2 CCR No. CC-22-0159 Revision: 0

Analyzer Result Tape:

Determination (circle one): Pass Fail
Comments:

Performed By/Date:

Reviewed By/Date: