QA-A-SOP-02 Active Ingredient Flush Test

STANDARD Document ID QA-A-SOP-02
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
3.1 Batching tank/tote

3.2 Overhead line
3.3 Filler machine head
3.4 Powder induction system
3.5 Filter
3.6 Glass sample jar
4. PROCEDURE
4.1 Pre/Post Production Flush:
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.
4.1.1.1 If a customer requires PLZ to follow strict guidance from a cross

contamination grid that the customer supplies, then this must be
referenced at each flush event for allowable levels of contaminants.
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.
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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
The exception to this is any pesticide procedure that includes an internal

standard. In this case, there will be a coinciding method that does not include
an internal standard calculation. This method will be used to run the flush
test.
4.1.6 The flush checks that need to be collected are:
4.1.6.1 Pre-Batch Tank Flush (Not required if a tank is dedicated for that
formula)
4.1.6.2 Pre-Fill Overhead Line Flush.
4.1.6.3 Pre-Fill Filler Flush (Performed separately if possible from the Pre-Fill
Overhead Line Flush).
4.1.6.4 Post-Fill Tank/Overhead Line Flush (Flushed from Tank/Tote and

collected on the Overhead line).
4.1.6.5 Post-Fill Filler Flush (Once the Post-Fill Tank/Overhead Line Flush is
approved).
4.1.7 Samples will be submitted with QA-A-FRM-01 Flush Sample Submission

with a Flush Submission Sticker attached to the Sample jar. See attachment
5.4.

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.
4.1.10 Record each flush check as a separate line item.
4.1.11 Under Lot Number, record the lot of the batch as well as the flush type as
either:
4.1.11.1 PBT (Pre-Batch Tank)
4.1.11.2 PFL (Pre-Fill Line)
4.1.11.3 PFT (Post-Fill Tank/Overhead Line)
4.1.11.4 PFFI (Pre-Fill Filler)
4.1.11.5 PFF2 (Post-Fill Filler)
i.e. PBT = Lot 001 Pre-Batch Tank Flush
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 Filler Hopper In-Process Testing:
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
Attachment 1: Flush Overview
Tank/Line Flush Solvents

Previous Batch Base Water Solvent Pesticide
First Flush Heptane Acetone Acetone
Second Flush SDA SDA Acetone
Third Flush Acetone
Lab Test Moisture Acetone in SDA Residual Active
Attachment 2: Flush Volumes per Equipment/Line

Tank/Line Flush Volumes*
Tanks 5 gal
PAC 5 Lines 75 gal
PAC 5 Fillers 75 gal
PAC 3 Lines 50 gal
PAC 2 Lines 75 gal
PAC 1 Lines 50 gal
*Flush volumes are approximate and may be adjusted as needed.

Attachment 3: SDA in Acetone Chromatogram
Attachment 4: Flush Submission Sticker

6. CALCULATIONS
Flush Moisture Calculation

(Flush SDA Moisture) - (Bulk Head SDA Moisture) = Residual Moisture
7. REFERENCES
7.1 QA-A-FRM-01 Flush Sample Submission
8. REVISION HISTORY
Date Revised By Revision Description of Changes

Luke
4-9-18 1 New document
Pendleton
12-3-18 Brock Evans 3 Added section 3.1 to update flush
procedure to the 3 flush system. Added
attachments to section 5 and 6 to support
update.
11-21-19 Sheila Breckle 4 Revised for new document system. Added
flush submission sticker to attachments
and added Volumes table. Obsoleted
PAC-LAB-SOP-018 Pesticide Flush Test
Procedure. Unable to locate version 2
14 May 2021 David Myers 5 Added customer cross contam-grid
requirements. Updated water and oil
phase flushing to current practice ‘1 part
and 1 part’. Updated volume of flush
needed table (attachment 2) to account for
data trend.

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STANDARD Document ID QA-A-SOP-02

3.1 Batching tank/tote

4.1 Pre/Post Production Flush:

4.1.1.1 If a customer requires PLZ to follow strict guidance from a cross

Uncontrolled when printed Page 1 of 6

The exception to this is any pesticide procedure that includes an internal

4.1.6 The flush checks that need to be collected are:

4.1.6.2 Pre-Fill Overhead Line Flush.

4.1.6.4 Post-Fill Tank/Overhead Line Flush (Flushed from Tank/Tote and

4.1.7 Samples will be submitted with QA-A-FRM-01 Flush Sample Submission

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4.1.10 Record each flush check as a separate line item.

4.1.11.1 PBT (Pre-Batch Tank)

4.1.11.2 PFL (Pre-Fill Line)

4.1.11.3 PFT (Post-Fill Tank/Overhead Line)

4.1.11.4 PFFI (Pre-Fill Filler)

4.1.11.5 PFF2 (Post-Fill Filler)

i.e. PBT = Lot 001 Pre-Batch Tank Flush

4.2 Filler Hopper In-Process Testing:

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Attachment 1: Flush Overview

Tank/Line Flush Solvents

Attachment 2: Flush Volumes per Equipment/Line

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Attachment 3: SDA in Acetone Chromatogram

Attachment 4: Flush Submission Sticker

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Flush Moisture Calculation

7.1 QA-A-FRM-01 Flush Sample Submission

Date Revised By Revision Description of Changes

Uncontrolled when printed Page 6 of 6

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