Mastersizer 3000e

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Operational Qualification
File Name: OQMS3K03 Operational Qualification for the Mastersizer 3000.docx Issue: 3
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Date: 1 August 2013 Page: 2 of 20
0. Document survey
0.1. Revision Comments
Issue Detail of change Date
Issue 1.0 First Release 23 December 2011
References to default SOPs removed.
Analysis settings applied to the 100nm latex measurement adjusted to reduce the
Issue 2.0 number of false failures observed during system qualification in-field. 15 February 2012
Added the Hydro 2000SM to the list of dispersion units which can be used, along
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with the plastic version of the DIF2021 unit.
References to OQ converted to PV where relevant.
Issue 3.0 As per document approvals
Document updated to reflect Release v2.20 of the software
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0.2. List of subsidiary documents
Note: For Malvern Instruments internal reference only. Note: “N” or” nn” denotes the latest issue number to
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be found on the Malvern Instruments Electronic documents database.
Ref Document Revision

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[1] IQ specification for the Mastersizer 3000 IQMS3Knn (Issue 3.0 or higher)
[2] OQ Specification for Hydro MV OQMV3Knn (Issue 1.0 or higher)
[3] OQ Specification for Hydro LV OQLV3Knn (Issue 1.0 or higher)
[4] OQ Specification for Hydro EV OQEV3Knn (Issue 4.0 or higher)
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[5] OQ Specification for Aero S OQAS3Knn (Issue 5.0 or higher)

[6] OQ Specification for Hydro SM OQSM3Knn (Issue 3.0 or higher)
The procedure requires the use of batch specification files. The latest specification is available on the
Malvern Extranet, if required.
In addition, the performance of a full system OQ on a Mastersizer 3000 unit will usually require an additional
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OQ procedure to be performed for each sample dispersion unit. Such tests are not covered by this
document, and can be found in references [2] to [6] above.
0.3. External References

Ref Document Revision
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[7] Mastersizer 3000 Software PSS0223-nn (version 2.20 or higher)

[8] Mastersizer 3000 Basic Guide MAN0475-nn (version 2.1 or higher)
[9] Mastersizer 3000 User Manual MAN0474-nn (version 2.1 or higher)
[10] Mastersizer 3000 Hydro Wet Dispersion Units Manual MAN0479-nn (version 2.2 or higher)
Note: Installation, Site Requirements and Health and Safety instructions for the Mastersizer 3000 Optical
Bench are included in MAN0475.
This page has been reviewed, Engineer (Initials) Date (dd month yyyy)
understood and the instructions
have been followed.
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Contents
0. Document survey....................................................................................................................................... 2
0.1. Revision Comments ........................................................................................................................... 2
0.2. List of subsidiary documents .............................................................................................................. 2
0.3. External References ........................................................................................................................... 2
1. Scope ........................................................................................................................................................ 4
2. General ...................................................................................................................................................... 4
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3. Equipment Required .................................................................................................................................. 5
4. Prepared Water ......................................................................................................................................... 6
5. Performance Verification ........................................................................................................................... 6
5.1. Preparation for the Test ..................................................................................................................... 7
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5.2. Performance Verification measurement ............................................................................................. 9
6. Result Checking and Documentation ...................................................................................................... 11
6.1. Create the certificate ........................................................................................................................ 11
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6.2. Check the certificate ......................................................................................................................... 11
6.3. Failures and Exceptions ................................................................................................................... 13
6.4. Malvern Customer Support Only: ..................................................................................................... 13
7. Customer Acceptance ............................................................................................................................. 14
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7.1. Product details.................................................................................................................................. 14
7.2. Result Summary and approval ......................................................................................................... 14
7.3. Remedial Actions taken to achieve an Ultimate Pass...................................................................... 15
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7.4. Additional Observations and Comments .......................................................................................... 15

8. Obtaining Batch Specifications................................................................................................................ 17
8.1. Downloading batch specifications .................................................................................................... 17
8.2. PV SOP Settings .............................................................................................................................. 17
9. Frequently asked Questions.................................................................................................................... 19
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have been followed.
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1. Scope
This Operational Qualification (OQ) covers the Mastersizer 3000 (MAZ3000) product only, using production
issue software v2.20 or higher. (For all previous versions of software, please use OQMS3K02). It is provided
for use by Customer Service as a verification of the instrument’s optical performance. It covers the
verification of the optical unit only. It does not challenge the sample dispersion system(s). When Malvern
Customer Support personnel are requested to perform the OQ, they should complete this procedure, initial
each page as the test progresses, and leave the original of this document with the certificate and result
evidence with the Customer. A copy of the sign-off page and the OQ certificate should be made for retention
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by Malvern Customer Support.
Note: If this procedure is being followed as part of a Performance Verification (PV) which is not associated
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with an OQ, this document is to be used for reference only and the tick boxes and signature sign-offs do not
need to be completed.
End of Section:
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Next Section: 2.
2. General
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This Operational Qualification procedure uses standard samples of microspheres in order to perform a
check of the instrument’s optical fidelity. The materials are identified as:
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0.1 µm Polystyrene DVB Microspheres : Catalogue Number 3100

1 µm Polystyrene DVB Microspheres : Catalogue Number 4009
9 µm Polystyrene DVB microspheres : Catalogue Number 2009
(Note: A letter after the catalogue number, if present, refers to the quantity of material in the bottle)
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The DVB refers to Divinylbenzene, which identifies the exact form of polystyrene compound used in the
particles. The samples have been chosen carefully to provide highly reproducible results. Because of the
wide size range of the Mastersizer 3000 product, measurements of several different sizes are required to
ensure that the entire dynamic range of the detectors of the Mastersizer 3000 has been exercised. Note that
the specified sizes have been carefully selected with this requirement in mind – this OQ does not support
the use of other sizes, even from the same supplier.
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Thermo Scientific manufactures each product in batches identified by a Manufacture Batch code that has
the form 2009-002, for example, identifying batch 002 of the nominal 9µm latex. Each manufactured batch
has some differences in particle size from the target size and these are characterised prior to the batch use.
Batches that have been characterised are identified in the OQ certificate issued with this procedure. Results
obtained by the use of material batches other than those identified here cannot be used to obtain a formal
OQ since a successful OQ procedure depends first and foremost on valid pass/fail criteria having been
established.
Each manufactured batch of latex is packaged into lots for sale. To trace individual packaging lots, a Lot No.
is indicated on each bottle. Thus full traceability of any sample is established by use of the Manufacture
Batch No. and the Packaging Lot No. The materials can be obtained from Malvern or direct from Thermo
Scientific by reference to the catalogue numbers detailed above. The material has been developed by
Thermo Scientific independently of Malvern and is on general sale as a particle size standard.
Each material is characterised by Thermo Scientific using optical microscopy in order to determine a mean
size. This mean size is subject to a tolerance that is based on the statistical uncertainty of the microscope
have been followed.
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measurements. For example, batch 2009-003 has a declared size of 9.0µm +/- 0.3µm. The spread of sizes
around the mean is also given as the Coefficient of Variation of the microscope measurements. A larger
coefficient of variation indicates a more polydisperse material. Given that a wider size range requires many
more microscope measurements to verify to the same statistical accuracy, it is normal for more polydisperse
materials to have a larger uncertainty than highly monodisperse materials.
The uncertainty on the mean size is not derived from any property of the material, but is a function of the
limitation of the microscopy technique used to certify the size. The material is in fact highly reproducible
within a batch and it is possible for Malvern, using laser diffraction, to determine a more precise mean size
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for the material. This is referred to in the verification certificate as the target size. This target result is highly
reproducible. For example, typical repeat measurements by the same careful operator on the same
instrument should easily yield a relative standard deviation on repeated DV50 measurements of <0.3%. This
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level of repeatability allows single measurement verifications of instruments to the 2% level specified.
The typical instrument-to-instrument variation of all these samples experienced in Malvern’s production test
facility is dependent on the examples tested, but is generally <0.5% RSD on the DV50. Malvern maintains
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records of the results of applying the OQ procedure on every instrument at completion of manufacture.
These results are regularly reviewed as part of production quality control.
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This Operational Qualification document serves many purposes. It firstly defines to the production tester a
critical subset of the criteria for a successful product build. As part of the installation procedure, it allows an
engineer to confirm that shipment has not disturbed the instrument. It enables an ex-factory performance
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capability to be established and regularly verified on the user’s premises. For the user, it enables the
instrument to be regularly monitored as part of an in-house verification protocol.
End of Section: 2.0

Next Section: 3.
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3. Equipment Required
In order to perform the measurement, the tester will require:
3.1.1. The current version of this OQ procedure, and its companion documents.
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3.1.2. One of the following sample dispersion units:
• MAZ3200/MAZ3210: Hydro MV automated sample dispersion unit.

• DIF2021: Small volume sample dispersion unit (plastic or metal versions)
• Hydro 2000SM Small volume sample dispersion unit
The DIF2021 and the Hydro 2000SM units can be used provided they are correctly configured with
a Mastersizer 3000 measurement cell.
3.1.3. A wet measurement cell (MAZ2010 or MAZ2020)
3.1.4. At least one bottle of latex samples 3100, 4009 and 2009 with the appropriate lot numbers (see
Section 5.1, below)
have been followed.
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Note: latex samples should be within their shelf life (one year) and should be stored at between 5 ° C
and 10 ° C when not in use.
3.1.5. At least 1 litre of water, prepared as described in Section 4.
3.1.6. Alcohol for cleaning (if required in Section 5.1.3).
3.1.7. An SOP for the latex samples being measured. For this procedure, the following versions are
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required:
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PVOP3K01.msop: 9µm and 1µm latex measurement SOP.
• PVOP3K100nm01.msop: 0.1µm latex SOP.
If these versions are not available, they can be created using the settings detailed in Section 8.2.
N NEnd of Section: 3.1.7
Next Section: 4.
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4. Prepared Water
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The dispersion of the sample requires no additives or ultrasound dispersion provided that prepared water is
used. This water should have been degassed, de-ionised and ideally filtered down to < 0.1 µm. Proper
preparation for the measurement must therefore include carrying a source of prepared water sufficient for
the measurements as well as cell cleaning. Testers should be aware that de-ionised water must be carried
in sealed containers to remain de-ionised and even then should be thought of as having a “shelf life” of only
one week. Ideally, a new batch should be prepared the day before a test is needed. Note that water at a
similar temperature to the room will become thermally stable within the sample unit faster.
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If the sample is dispersed in the prepared water, it is usually stable over a long period, typically many hours,
without any handling other than normal stirring and circulation. In tap water, the sample may flocculate,
either immediately or slowly depending on the source of the water. For this reason, tap water must not be
used.
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End of Section: 4.0

Next Section: 5.
5. Performance Verification
The functional testing of the product consists of a number of particle-in-liquid measurements using standard
samples. The following procedure describes in detail the steps required to make a correct PV. The recipient
of the test data should witness the PV being performed at whatever level of supervision is deemed
necessary according to prevailing quality system requirements. The recipient must sign acceptance of the
test for it to be considered as a valid PV measurement.
Malvern provide SOPs configured with the correct settings for performing the PV. However, the Mastersizer
3000 system allows any SOP to be run as a PV SOP. This provides the flexibility of customising an SOP for
consistent company-wide use whilst retaining the essential aspects required for adherence to the PV
procedure. When running an SOP as a PV SOP the software displays a special documentation page that
have been followed.
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enforces entry of digitally-signed latex batch pass/fail criteria and operator, instrument and individual latex
bottle information. Measurement records produced using a PV SOP are internally tagged so they can
subsequently be used to form part of the measurement set that contribute to the PV Certificate.
5.1. Preparation for the Test
5.1.1. Verify that the Latex batch specification files for the sample materials available for the
measurement are available by choosing Tools – PV Series Files to view the latex
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batch specifications that are present on the system.
For example, a displayed batch specification filename such as ‘LTX2009 004 to 010 -
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9um Nom.moqs’ would need be present for a 9µm latex labelled as ‘Batch 005’. Files
labelled ‘LTX4009’ relate to the 1µm latex, whereas those labelled ‘LTX3100’ relate to
the 0.1µm latex
N N If the relevant batch details are not present, refer to Section 8 ‘Obtaining Batch
Specifications’.
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5.1.2. Initial Installation only:
The unit to be tested must be powered up and left to thermally equilibrate for at least
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30 mins before the PV testing commences. If the unit is particularly cold, after
storage in a cold warehouse for example, then an additional 1 to 2 hours warm-up
time should be allowed for the system to arrive at an operating temperature.
Record the equilibration time here:

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5.1.3. The cell should be cleaned prior to the test. Use detergent & hot water to flush the
system until there are no detectable oil or organic residues. After cleaning with
detergents, flush the entire system thoroughly with tap-water to remove residues.
A requirement for as many as ten rinses should be anticipated. Finally, flush with
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pure water and drain. Split the cell and wipe the inner window faces with lens tissue
soaked in alcohol.
Record the number of rinses here:
5.1.4. The cell should be fitted following instructions in the operating manual. Verify that all
connections have been made.
5.1.5. Fill the Hydro unit with tap water and pump/stir it around the cell. Visually inspect for
leaks and bubbles on the cell windows.
have been followed.
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5.1.6. Drain the unit, refill it with the prepared water and repeat the process. Finally, fill the
unit with prepared water ready for the measurement.
5.1.7. Create a measurement file to hold the PV measurements. If all PV measurements are
to be held in one file, locate and open this file.
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5.1.8. Check that the Mastersizer 3000 SOP for the optical bench is available:
PVOP3Kxx.msop: 9µm and 1µm latex measurement SOP.
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PVOP3K100nmxx.msop: 0.1µm latex SOP.
where ‘xx’ is the version number of the SOP.

N N If the specified version of the SOP requested in Section 3.1.7 is not present,
download it from the Malvern Instruments website or amend the latest available
version using the information in Section 8.2.
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An SOP needs to be run for each latex size. Select the SOP to run as a PV SOP by
clicking on the arrow of the Run SOP button and choose Run PV SOP.
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Choose the SOP to run and click OK. The special PV documentation page will be
displayed.
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Using the drop-down listbox, select the PV batch specification for the latex that is to
be used for the PV.
If the relevant batch specification files are not present, refer to Section 8 ‘Obtaining
Batch Specifications’. If you have downloaded a new specification file, then use the
have been followed.
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‘Add from File…’ option. If file access to uncontrolled media such as memory sticks is
not permitted at the site, choose the ‘Add manually...’ option.
Having selected the appropriate batch, complete the SOP documentation fields. The
Tester’s name, unique Test Reference and packaging lot number (from the latex
bottle) are mandatory fields.
Click OK to start the measurement process using the settings defined in the SOP.
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5.1.9. Valid Latex Batch Specification loaded and appropriate SOP selected.
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This will correctly configure the software for the PV measurement.
5.1.10.
N N When prompted, enter the Tester’s name and a Test Reference that identifies the
test uniquely. This same Test Reference must be used as the reference on any PV
certificate based on the results obtained. As a minimum, the name of the Tester, the,
sample Manufacture Batch No. and the Packaging Lot No of the latex used should
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be included in the details recorded using the fields provided. Most other information
will be encoded automatically in the result file created. Add any further information
that may be relevant to the test result in the Notes field.
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Note: the software will automatically specify a Test Reference based on the date of
the test and the name of the user carrying out the PV. This can be edited if required.
5.2. Performance Verification measurement

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The following steps need to be performed for each sample in turn. The samples can be measured in any
order since they are independent of each other. However, the 0.1µm latex measurement is the most difficult
to perform and thus it is advisable to start with the highest sizes and work down. In this way, the easier large
measurements will be performed first and the tester will become familiar with the procedure before the more
sensitive measurements are attempted.
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5.2.1. Latex Measurement Procedure
5.2.2. Drain the dispersant from the cell and refill with prepared water. Leave the
pump/stirrer running at a speed of between 1500rpm and 1600rpm in order to
circulate the water. Check for bubbles by inspecting the cell and, where relevant, the
pipes. If bubbles are seen or suspected, stop the pump/stirrer and allow the cavity to
empty of trapped air. If further bubbles occur, check the fit of the cell windows and
tubing, where relevant. Ultrasonic can be used to help to degas the water. No
bubbles should be seen in the cell or liquid during circulation.
have been followed.
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5.2.3. Perform an automatic alignment according to the procedures in the manual. Inspect
the align display on completion. Look for signs of bursts of scattering in the inner
detector segments. If they occur, the system is seeing occasional large particles.
Check again for bubbles and also verify that the water has been filtered and that the
cell has been properly flushed. Only proceed once a stable signal is obtained
indicating normal alignment.
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5.2.4. In preparation for the sample measurement, inspect the sample bottle and verify that
it is suitable for use. Prepare the bottle for measurement by first agitating the
contents by inverting the bottle at least 30 times. Avoid vigorous shaking as this will
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cause the material to froth. The measurement steps need to be made quickly from
the time that a background is recorded through to the sample being measured.
Continue to invert the bottle regularly during the entire period until the sample has
N N been added to the tank of the sample dispersion unit. This procedure is important and
will ensure that the material stays adequately suspended and that a representative
sample is delivered when required. Once the alignment display is stable, measure the
background according to the procedures in the user manual. The expected
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background value is less than 100, and should be less than 150 after use. If the
background is >150, consider whether the windows should be changed and the
procedure repeated.
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5.2.5. As soon as the background measurement has been completed, enter the inspect
mode using the procedures in the user manual. Add the sample to the sample
dispersion unit drop-by-drop, using the sample bottle to dispense the drops. At the
same time, watch the obscuration display. After each sample addition, wait for a few
seconds to allow the sample to disperse and circulate before judging the obscuration
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reading. Keep inverting the sample bottle during these waits in order to maintain
suspension. The obscuration ranges required to obtain a pass are as follows:
Size Recommended obscuration Drop range

range
0.1 µm 0.8 to 1.2% 6-9 drops
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1 µm 4 to 5% 1-3 drops
9 µm 4 to 5% 40-80 drops
5.2.6. As soon as the desired obscuration is reached, perform the sample measurement
using the procedures in the user manual. Note that the measurement should be
performed 10-20s after the obscuration has been achieved. On completion of a
satisfactory sample measurement, close the Measurement Manager window.
5.2.7. Save the file as a record of the measurement.
Note: Figures higher than those specified will fail the PV criteria and inspection of the fit data will be
necessary. The fit errors should typically be well spread out amongst the points so that the overall residual
is an accumulation of small errors. When a large fit error appears to be generated by odd points fitting badly,
have been followed.
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then the error will need investigation. Start with a re-measurement, ensuring that the instrument is warmed
up and that the sample measurement is taken shortly after the background measurement. Small localised
fitting errors may be caused by small alignment changes between the two measurements caused by the
instrument warm-up. If the problem persists then more detailed instrument checking will be required by
qualified Malvern Customer Support staff. Please note that having the data file available will help to pinpoint
the source of the trouble. See also Section 6.3 “Failures and Exceptions”.
End of Section: 5.2.7
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Next Section: 6.
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6. Result Checking and Documentation
6.1. Create the certificate
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The result obtained needs to be checked against the expected values for the sample. Select either:
(a) three measurements of each latex size (i.e. nine measurements in total)
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or
(b) three averaged measurements of each latex size (i.e. three measurements in total)
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Right click and select ‘Generate PV Certificate’:

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6.2. Check the certificate

The software will compare the result with the target values from the batch specification selected above and
produce a candidate certificate which includes:
(a) A header section with details of the tester, the instrument and the date.
(b) For each size the target specification and measurement result together with a pass or fail
based on the average the three result statistics for each size.
(c) An overall pass/fail result.
(d) A signature section.
An example certificate is shown in figure 1 below.
have been followed.
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6.2.1. Verify that the certificate is correct.
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Figure 1 - Example of a PASS certificate.
have been followed.
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6.3. Failures and Exceptions

In the event of a failure, the tester is required to note the fact of the failure in the space provided in Section
7.3 of the Customer Acceptance Section of this document.
In the event that an error in the performance of the measurement is suspected as the cause of the failure,
the probable source of the error and the corrective action taken is to be recorded. The unit must then be re-
tested. In the event that a re-measurement fails, the fact of the fresh failure is to be recorded together with
subsequent corrective measures undertaken. The User’s representative must countersign against each
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iteration of the process to indicate the user understands and accepts the procedure.
Each single corrective action undertaken should be followed by a test in order to isolate the cause of the
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problem. Once a pass is achieved, a second confirmatory measurement must be undertaken before the
system can be passed. Section 7.4 ‘Additional Observations and Comments’ may be used to record
additional tests and acceptances if necessary. In the event that on-site intervention is not successful, it will
be necessary to repeat the PV procedure for the offending unit on subsequent re-installation.
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6.4. Malvern Customer Support Only:
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6.4.1. To create a Certificate, it should be printed onto Malvern Headed paper or onto
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Headed paper from a Malvern-appointed distributor (Click on ‘Header and Footer’

to toggle the Malvern logo and footer off if printing on headed paper). Sign and date
the Certificate to verify the authenticity of the measurement and make a copy for
Malvern records. Add to the Certificate the printed Analysis Report and Fit Report
for the measurement as this will provide the Result Evidence of the measurement.
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6.4.2. Obtain the signature of the Recipient to confirm acceptance of the Certificate and
Result Evidence as a true record of the measurement.
End of Section: 6.4.2

Next Section: 7.
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have been followed.
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7. Customer Acceptance
The installing engineer has now finished the installation and commissioning of the product. The Installing
Engineer and the User’s Representative should now sign in the spaces provided below where indicated and
all the printouts should be attached to this document.
7.1. Product details
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Mastersizer 3000
Model Number: Serial Number:
(MAZ3000)
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7.2. Result Summary and approval
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The minimum requirement for a successful product OQ is that the tests described in Section 5 of this
procedure must pass. Record here details of the type of pass achieved. In the event that neither type of
pass was achieved, a failure must be recorded.
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Procedure
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Description Test Result (e.g. Outright Pass or Ultimate Pass)

Section
Outright Pass (No remedial actions required)
Tester’s Signature:
Performance
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Verification Ultimate Pass (Remedial actions taken should be recorded in Section 7.3)
Tester’s Signature:
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have been followed.
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7.3. Remedial Actions taken to achieve an Ultimate Pass

In the event that a failure results during initial performance verification, the failure should be recorded here
together with the details of any remedial action taken. Once the remedial action has been taken, this should
be confirmed and, if it is successful, the result should be recorded in the Ultimate Pass box in section 7.2. In
the event that more than one remedial action and retest are required, each remedial action taken must be
recorded below:
Outcome of
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Description of Failure Remedial Action Taken
retest
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7.4. Additional Observations and Comments

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The results recorded in this report were obtained during the tests on the unit specified.
have been followed.
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Field Service Engineer (Malvern) or representative:

Name: Signed:
Title: Date:
(dd month yyyy)
Customer:
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Name: Signed:
Title: Date:
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(dd month yyyy)
Customer
Comments
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End of Section: 7.4

Next Section: 8.
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have been followed.
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8. Obtaining Batch Specifications
8.1. Downloading batch specifications
From the Extranet choose Diffraction – Mastersizer 3000 – IQ/OQ/QAS. In the OQ section choose
Mastersizer 3000 (MAZ3000) and Hydro/Aero Dispersion units – SOPS & MOQS. Click on the link to
download the file. Extract the file you require to your local computer. You can then select this file using the
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‘Add from file...’ button as described in Section 5.1.8.
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Figure 2 - Typical zip file contents
8.2. PV SOP Settings

Note: Some of the settings detailed in the following tables are simply average values commonly used to
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perform a measurement and these may be varied at the tester’s discretion. Other settings are mandatory
and are marked as such. In the event of any conflict between the settings below and the SOP proposed for
use, the information given in this document should be considered to be correct since it is subject to strict
change control procedures.
Reference Page Only

No Engineer Action Required
No Sign-off Necessary
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Table 1: SOP settings for Latex performance verification measurement.

Sample Particle Type: Spherical
(Mandatory)
Material: Material name: Polystyrene Latex
Refractive index: 1.59
Absorption index: 0.00
Different blue-light properties: enabled

Refractive index (blue-light): 1.6
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Absorption index (blue-light): 0
Dispersant: Refractive index: 1.33
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Sample: Instructions Instructions before measurement:
Ensure background is clean and stable.

N N Instructions following measurement:
Clean 3 times with pure water

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Measurement: Duration Background measurement duration (seconds): 5
(Mandatory) Sample measurement duration (seconds): 3
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Use the durations I specify: Enabled

Background measurement duration: 5
Sample measurement duration: 3
Measurement: Sequence Number of measurements: 10

(Mandatory) Delay between measurement (s): 0
Pre-measurement delay (s): 0
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Measurement: Obscuration lower limit (%): 0.1

Obscuration Obscuration higher limit (%): 10
(Mandatory) Auto start measurement, when obscuration is in range: disabled
Enable filtering: disabled
Data Processing Analysis Model: Verification latex

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(Mandatory) Advanced…:
Single Mode: enabled
Number of inner detectors to kill: 0 (1µm / 9µm) or 20 ( 0.1µm)
Remove blue light from analysis: disabled
User Sizes: Use default sizes
End of Section: 8.2

Next Section: 9.
Reference Page Only

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9. Frequently asked Questions
9.1: How do you explain the fact that you only use a 100nm, a 1µm and a 9µm latex for an
instrument which you claim to be capable of measuring from 0.01 to 3500µm?
The OQ simply has to prove that the detector array and the optics are set up correctly in the optical bench. To do this,
we only need the 100nm, the 1 µm and the 9 µm latices which scatter to all the detectors in the array and allow us to
determine that they are responding correctly. Because the instrument is based on first principles of physics, if the
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detectors and the optics are set up correctly, there is no need to measure other samples.
If other sizes need to be measured to prove that the instrument is suitable for the purpose for which it was purchased,
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this is part of the PQ rather than the OQ and this is the responsibility of the user. Although many suppliers of HPLCs and
other standard analytical systems sometimes offer PQs for their systems, this is only possible because their applications
are relatively standardised within the industry and so they are able to offer a limited series of tests which suit most
users. Owing to the diversity of applications for the Mastersizer 3000 in the pharmaceutical industry, there is no such
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convenient set of standard tests available and so the PQ must remain the user’s responsibility.
9.2: How do you determine and maintain the pass/fail criteria for your latices?
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Please refer to Section 2 of this specification.
9.3: Can we inspect your Validation protocols for the PV Certificate Generator?
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There is no need as the calculations can readily be checked by eye. The certificate shows the target values and the
measured values from which the pass/fail decision is made. Confirmation that the measured value is within the target
limits can be checked by inspection.
If you wish to check the target values on the certificate correspond to those in the batch specification file, then open the
EF
.moqs file with a text editor such as ‘Notepad’. The file is a digitally signed xml file. For example, here are the lines
pertaining to the 9um (Nominal) Dv50 target and % tolerance values:
<ExpectedDv50>9.016</ExpectedDv50>
<Dv50Specification>2.5</Dv50Specification>
9.4: Why does your OQ procedure not specify that the original Certificates for the latices
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used are attached to the Certificate or the Specification as part of the procedure?
This is not normally done since each bottle of latex is used to perform a number of OQs and in-field verifications and
only one original Certificate is provided with it. If an original certificate is required, the only way that this requirement
could be accommodated would be for you to arrange the purchase of the bottles of latex in advance of the Engineer’s
visit. This would add an additional cost to the procedure which most of our customers would find unacceptable.
9.5: How can I be certain that the batch specification file has not been edited or become
corrupted? Similarly, how do I know whether manually entered specifications have been
erroneously or deliberately mis-entered?
All the data associated with the specifications is digitally signed to provide a secure check-code. The check code is
used whether the information is loaded from file or manually. Tampering with either the data or the check code is
detected by the software and the data cannot be used.
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9.6: Why do you apply a data kill to the 0.1µm latex? Does this not reduce the ability of the
OQ to detect instrument failures?
The MS3000 OQ requires the measurement of a range of latex standards, in order to verify that the entire detector array
is working correctly. By choosing different latex sizes, different sets of detectors can be tested. The 0.1µm OQ latex
specifically tests the large angle and back-scatter detectors, for both red and blue light detection. The intensity of light
scattered light to the low angle detectors by this latex is negligible, and as a result the 0.1µm material does not provide a
good test for these detectors.
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The small size of the 0.1µm latex means that the scattering intensity observed for this sample is comparatively weak. As
a result, problems with the thermal stability of the dispersant or the presence of bubbles or other contaminants may yield
scattering at small angles which is of a higher intensity than that seen for the latex. Given that the quality of the water
used in the OQ measurements can vary from installation to installation, Malvern have decided to apply a detector 'kill' to
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the inner detectors, removing them from the data set prior to calculation of the particle size of the 0.1µm latex. This
enables a robust test of the performance of the large angle and back-scatter detectors to be carried out, without the risk
of a failure against the test specifications caused by any scattering observed at small angles. The performance of the
small angle detectors that are excluded in the 0.1µm test (detectors 1-20) is then tested using the 9µm latex standard.
N N
End of Section: 9.6
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End of Document
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[5] OQ Specification for Aero S OQAS3Knn (Issue 5.0 or higher)

0.3. External References

[7] Mastersizer 3000 Software PSS0223-nn (version 2.20 or higher)

7.4. Additional Observations and Comments .......................................................................................... 15

0.1 µm Polystyrene DVB Microspheres : Catalogue Number 3100

End of Section: 2.0

3.1.2. One of the following sample dispersion units:

• MAZ3200/MAZ3210: Hydro MV automated sample dispersion unit.

3.1.3. A wet measurement cell (MAZ2010 or MAZ2020)

3.1.5. At least 1 litre of water, prepared as described in Section 4.

3.1.6. Alcohol for cleaning (if required in Section 5.1.3).

End of Section: 4.0

5.1. Preparation for the Test

Record the equilibration time here:

Record the number of rinses here:

PVOP3Kxx.msop: 9µm and 1µm latex measurement SOP.

where ‘xx’ is the version number of the SOP.

5.2. Performance Verification measurement

5.2.1. Latex Measurement Procedure

Size Recommended obscuration Drop range

5.2.7. Save the file as a record of the measurement.

End of Section: 5.2.7

Right click and select ‘Generate PV Certificate’:

6.2. Check the certificate

An example certificate is shown in figure 1 below.

6.2.1. Verify that the certificate is correct.

Figure 1 - Example of a PASS certificate.

6.3. Failures and Exceptions

Headed paper from a Malvern-appointed distributor (Click on ‘Header and Footer’

End of Section: 6.4.2

7.1. Product details

Description Test Result (e.g. Outright Pass or Ultimate Pass)

7.3. Remedial Actions taken to achieve an Ultimate Pass

7.4. Additional Observations and Comments

Field Service Engineer (Malvern) or representative:

End of Section: 7.4

8. Obtaining Batch Specifications

8.1. Downloading batch specifications

Figure 2 - Typical zip file contents

8.2. PV SOP Settings

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Table 1: SOP settings for Latex performance verification measurement.

Different blue-light properties: enabled

Dispersant: Refractive index: 1.33

Ensure background is clean and stable.

Clean 3 times with pure water

Use the durations I specify: Enabled

Measurement: Sequence Number of measurements: 10

Measurement: Obscuration lower limit (%): 0.1

Data Processing Analysis Model: Verification latex

End of Section: 8.2

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9. Frequently asked Questions

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