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QA-A-SOP-02 Active Ingredient Flush Test
QA-A-SOP-02 Active Ingredient Flush Test
OPERATING Revision 5
PROCEDURE Issue Date 20 May 2021
Dept. / Sub-Dept. Quality / Analytical Lab Issued By Sheila Breckle
Title Active Ingredient Flush Test
Reviewed By David Myers Date Reviewed 14 May 2021
Approved By William Drennen Date Approved 20 May 2021
1. PURPOSE
This procedure describes how to flush and test equipment used before and after
batching materials containing an active ingredient.
2. RESPONSIBILITIES
Lab Personnel are responsible for following this procedure when testing the tank /
filler flushes before and after batching products containing an active ingredient.
Production personnel are responsible for following this procedure when performing
tank / filler flushes before and after batching products containing an active
ingredient.
3. EQUIPMENT
4. PROCEDURE
4.1.1 If the customer requires pesticide flushes, every pesticide made for that
customer is required to pass a flush test prior to batching and after filling.
4.1.2 The flush test needed is decided by using the previous product run through
the tank, line, or filler. For solvent-based products, a solvent flush is
performed, for water-based products, a water flush is performed, and for
pesticide products, a pesticide flush is performed. These flushes are
summed up in Attachment 5.1 with volumes in Attachment 5.2.
4.1.3 Solvent flushes consist of flushing 1 part acetone, followed by 1 part SDA.
The SDA is then run by GC using the "SDA in Acetone" Procedure, to test for
residual acetone. To pass, the acetone found must be below 1000ppm. This
is shown in Attachment 5.3
4.1.4 Water flushes consist of flushing 1 part heptane, followed by 1 part SDA. The
SDA is then run using a Karl Fischer to test moisture. This moisture is then
compared to the moisture from a bulkhead SDA sample using the calculation
in 6.1. To pass, the residual moisture calculated must be below 1000ppm.
4.1.5 The pesticide flushes consist of acetone flushes. When testing this flush, the
active method of the previous pesticide is run to ensure that the pesticide
has been flushed from the system. To pass, the residual pesticide must be
below 500ppm or 0.5g/L
4.1.6.1 Pre-Batch Tank Flush (Not required if a tank is dedicated for that
formula)
4.1.6.3 Pre-Fill Filler Flush (Performed separately if possible from the Pre-Fill
Overhead Line Flush).
4.1.6.5 Post-Fill Filler Flush (Once the Post-Fill Tank/Overhead Line Flush is
approved).
4.1.8 Complete the Top portion of the form and sticker then submit to the
Analytical Chemist when complete.
4.1.9 All flush results will be recorded in the Lab database under the active
formula's number.
4.1.11 Under Lot Number, record the lot of the batch as well as the flush type as
either:
4.1.12 Enter the volume of the solvent used to flush under Amount. If a flush check
fails, the next flush check Amount should be a running total of the previous
flush volume plus the new flush volume.
4.1.13 Enter the solvent used under Mixer/Line, i.e. Methanol or Acetone
4.1.14 Only the Flush Check test column needs to entered and only needs to be
documented as Pass (1) or Fail (O). N/A the other test columns.
4.2.1 If required by the customer, if pesticides are ran back to back, at the start of
the run, a sample must be taken from a filler hopper each time it empties and
refills for the first 5 cycles. For the exact timing of sampling, see the Quality
Manager/Supervisor.
4.2.2 Test the Filler In-Process sample for the previous run's active ingredient, not
the current active.
4.2.3 The Filler Hopper In-Process sample should be free of any actives from the
previous run. If it is not free of the previous actives, contact the Quality
Manager/Supervisor immediately.
4.2.4 Enter the testing under the active formula's number under the flush check.
Under Lot Number, record the lot of the batch as well as FHT (Fill Hopper
Testing) and finally the replicate of the test. For example, if it were the
second Fill Hopper Test for batch 001, it would be 001 FHT 2.
5. ATTACHMENTS
6. CALCULATIONS
7. REFERENCES
8. REVISION HISTORY