Index .................................................................................................................61
ii
1. INTRODUCTION
Thank you for choosing the AQUALAB® 4 Series Water Activity Meter from METER Group.
AQUALAB is the most accurate and most reliable instrument available for measuring water
activity (aw ).
The AQUALAB 4 Series includes four models:
• AQUALAB 4TE uses a chilled-mirror dew point sensor and thermoelectric (Peltier)
components to maintain a user-selectable internal temperature.
• AQUALAB 4TEV uses both a chilled-mirror dew point sensor and a capacitance sensor for
measuring nonvolatile and volatile substances, respectively. Either sensor is selected using
the instrument menu system.
• AQUALAB 4TE DUO uses a chilled-mirror dew point sensor and programmed models
obtained from isotherm data to give the user both water activity and moisture content
simultaneously in 5 min or less.
• AQUALAB 4TEV DUO uses both a chilled-mirror dew point sensor or capacitance sensor
as well as programmed models obtained from isotherm data to give the user both water
activity and moisture content simultaneously for samples containing both nonvolatile and
volatilesubstances.
This manual includes instructions for setting up, verifying the calibration, preparing samples,
taking readings, and maintaining AQUALAB instruments.
Verify all instrument contents shipped and appear in good condition:
• AQUALAB Water Activity Meter
• Calibration certificate
• Power cord
• USB A to USB B cable
• 50 disposable sample cups
• AQUALAB Cleaning Kit
• Two vials each of the following verification solutions:
0.760 aw 6.00 mol/kg NaCl
0.500 aw 8.57 mol/kg LiCl
0.250 aw 13.41 mol/kg LiCl
1
OPERATION
2. OPERATION
Please read all instructions before operating the AQUALAB to ensure it performs to its
full potential.
Please observe the following considerations carefully.
• Only allow personnel qualified by METER to carry out service work on the electrical
components.
• Never remove the cover of the instrument. There are no parts inside the housing that can be
serviced or replaced by the user.
WARNING: There is a risk of damaging the instrument or of causing serious injury if live components are touched.
• Only operate this instrument with a main power voltage specified (100 to 240 V AC).
• Plug the instrument into a grounded outlet or power strip.
• Only use the fuse type and rating specified for this instrument (Section3.1).
If the instrument is used in a manner not specified by the manufacturer, the protection
provided by the equipment may be impaired.
PRECAUTIONS
METER sensors are built to the highest standards, but misuse, improper protection,
or improper installation may damage the sensor and possibly void the manufacturer’s
warranty. Before integrating AQUALAB into a system, follow the recommended installation
instructions and arrange proper protections to safeguard the instrument from damage.
2.1 INSTALLATION
Follow the steps listed in Tab le 1 to set up the AQUALAB.
Table 1 Installation
Select Clean, Level Location
Select a location where the temperature remains fairly stable to avoid
temperature changes that can affect accuracy (away from air conditioner and
Preparation
heater vents, open windows, etc.).
Observe clean practices to prevent contamination of the sample chamber.
Maintain a level surface to reduce the chance of spilling sample material and
contaminating the sample chamber.
2
AQUALAB
Table 1 Installation (continued)
Plug In Instrument
Plug the power cord into the back of the AQUALAB unit and into an outlet.
Only use the supplied power cord or one rated for AQUALAB 4 and certied for
the country of use. The cord must be a minimum of 18 AWG and have a rating
Installation
for 10 A or greater.
WARNING: An incorrect main power voltage can damage the instrument.
Turn the Unit ON.
Allow the AQUALAB a 15-min warm-up period to ensure accurate readings.
2.2 SAMPLE PREPARATION
Proper sample preparation is important to keep the AQUALAB clean and achieve repeatable
results. Carefully prepare and load samples to lengthen time between cleanings and help
avoid downtime. Be consistent in sample preparation methods (e.g., crush, grind, slice the
sample) to obtain reproducible results.
More specific considerations regarding sample composition and sample temperature are
discussed in Section2.2.1 and Section2.2.2, respectively.
Follow the steps listed below to prepare samples:
1. Make sure the sample to be measured is homogeneous.
Multicomponent samples (e.g., mufns with raisins) or samples that have outside
coatings (like deep-fried, breaded foods) can be measured, but they need to have
representative portions in the cup and may take longer than other sample types
toequilibrate.
2. Place the sample in a disposable sample cup.
a. Completely cover the bottom of the cup, if possible, to provide enough sample to get
an accurate reading.
The AQUALAB is able to accurately measure a sample that does not (or cannot) cover
the bottom of the cup. For example, raisins only need to be placed in the cup and do
not need to be attened to cover the bottom.
A larger sample surface area increases instrument efciency by providing more
stable infrared sample temperatures. It also speeds up the reading by shortening the
time needed to reach vapor equilibrium.
b. Do not fill the sample cup more than half full.
Overlled cups can contaminate the chamber and do not make the readings faster or
more accurate.
3. Wipe any excess sample material from the rim and outside of the sample cup with a
clean KIMWIPES® tissue.
3
OPERATION
Material left on the rim or the outside of the cup can contaminate the chamber and be
transferred to subsequent samples.
4. If a sample cannot be measured immediately, put the disposable sample cup lid on the
cup to restrict water transfer.
For longer term storage of no more than 4 h, seal the lid by placing tape or Paralm®
laboratory lm completely around the cup to lid junction.
2.2.1 SAMPLE COMPOSITION
The nature of some samples results in longer reading times. These materials may need
additional preparation to ensure accurate readings. Contact Customer Support for
questions on sample composition.
Use the following steps to determine if further sample preparation is necessary:
1. Take several readings of the sample to see if the readings (aw and time) stabilize
(Section2.3).
2. If the readings take less than 6 min to stabilize, the sample can be handled normally.
If the readings take longer than 6 min, remove the sample and take a reading of a
verication standard (Section4.1.1).
3. If the verication standard takes less than 6 min to test, the sample itself is causing the
long read time. Refer to the following sections for pertinent sampling considerations.
If the verication standard also takes longer than 6 min to test, the chamber may
be dirty and will need to be cleaned (Section4.2). Retest the sample after cleaning
thechamber.
2.2.1.1. COATED AND DRIED SAMPLES
Samples with high sugar or fat coatings often require multiple readings, because it
equilibrates very slowly with the sample chamber.
Crush or slice the sample before sampling to reduce the time needed to take a water
activity reading for coated or dried samples. This increases the surface area of the sample,
thus decreasing reading times. However, modifying some samples may alter their water
activityreadings.
For example, a candy may have a soft chocolate center and a hard outer coating. The water
activity reading for the center and the outer coating are different, so one would need to
evaluate which part of the sample needed to be measured before crushing it. When the
candy is crushed, the water activity represents the average water activity of the entire
sample; whereas leaving the candy whole gives a reading for the coating, which may act as a
barrier to the center.
To reduce test time when testing whole samples, see Section3.2.4.2 to set Low-Emitting
mode.
4
AQUALAB
2.2.1.2. LOW WATER-EMITTING SAMPLES
Some extremely dry, dehydrated, highly viscous, water-in-oil emulsions (e.g., butter), high
fat, or glassy compositions may require multiple readings because of their slow wateremitting properties. This is because the slow emission of water decreases the change in
water activity sufficiently that the instrument determines the test to be complete, even
though changes in water activity are still occurring.
The most effective way to test these types of samples is to run them in the AQUALAB using
Continuous or Custom mode and wait for the water activity readings to stabilize.
For faster reading, it is important to have the relative humidity of the chamber at or below
the water activity of these types of samples. This causes the sample to release water to the
vapor phase and equilibrate with the chamber. If the relative humidity of the headspace is
greater than the water activity of the sample, the sample will require a long period of time to
reach equilibrium.
To reduce test time when testing low water-emitting samples, see Section3.2.4.2 to set
Low-Emitting mode.
2.2.1.3. VOLATILE SAMPLES
Samples with certain volatiles in high enough concentrations may give inaccurate water
activity values in the AQUALAB 4TE and AQUALAB 4TE DUO models. Volatiles condense on
the mirror during the reading process but do not evaporate from the mirror as water does.
As a result, the reading on samples with volatiles may not be accurate. The concentration
of volatiles that causes interference is variable and matrix dependent.
The AQUALAB 4TEV measures volatiles such as propylene glycol and ethanol. The AQUALAB
4TEV contains both a chilled-mirror dew point and a capacitance sensor. The capacitance
sensor has a lower accuracy of ±0.015 aw than the dew point sensor, which has an accuracy
of ±0.003 aw.
To determine if volatiles are a problem, compare dew point readings to capacitance readings.
If the dew point readings are >0.018 aw higher than the capacitance readings, volatiles are
likely a problem and the AQUALAB 4TEV, AQUALAB 4TEV DUO, or AQUALAB TDL will need to be
used for the sample.
After measuring volatiles with the capacitance sensor, clean the chamber (Section4.2),
place charcoal in the chamber, and seal for a minimum of 5 min before switching to the dew
point sensor.
2.2.1.4. LOW WATER ACTIVITY
A sample’s water activity value may be below the cooling capacity of the AQUALAB. The
AQUALAB will display an error message indicating the lowest reading it attained on that
particular sample. The AQUALAB may also give the error message even if the sample is not
below 0.03 aw. Section4.5 provides possible solutions to the error message.
5
OPERATION
If a sample has a water activity of <0.03 aw, a < symbol in the Measurement tab indicates the
sample is too dry to be accurately measured by the AQUALAB (Figure1).
Figure1 Low water activity reading
If the measured aw appears lower than the known sample water activity, the instrument
sensors may have been contaminated and need to be cleaned or serviced (Section4.2).
2.2.2 SAMPLE TEMPERATURE
The ambient temperature of the AQUALAB should be between 15 and 50 °C. The AQUALAB
4TE and AQUALAB 4TEV have internal temperature control capabilities that enable them to
read samples at temperatures different from the ambient temperature, but no higher than
50 °C and no lower than 15 °C.
Samples that are more than 4 °C colder or warmer than the instrument chamber
temperature need to equilibrate to instrument temperature before taking a reading, ideally
within 1 or 2 °C of the chamber temperature. Rapid changes in temperature over short
periods of time causes the water activity readings to rise or fall until the temperature
stabilizes. Proceed with normal measurements when the temperature stabilizes within an
optimal 1 or 2 °C of the chamber temperature.
High water activity samples that are warmer than the chamber temperature can cause
condensation inside the measuring chamber, which adversely affects subsequent readings.
A warning message appears if the sample temperature is more than 4 °C above chamber
temperature (Figure2).
Figure2 Sample is too hot! message
6
AQUALAB
If this error message appears,
1. Remove the sample from the instrument.
2. Place a lid on the cup.
3. Allow the sample to cool to within 4 °C of the instrument before measuring.
To check the differences in temperature between the sample and the chamber prior to
beginning a reading, set the sample in the chamber, close the lid without latching it, and
press the RIGHT or LEFT button. Figure3 provides an example of this screen.
Figure3 Temperature difference between sample and sample chamber
2.3 TAKING A READING
The AQUALAB provides readings in 5 min or less. Readings are reliable, providing ±0.003 aw
accuracy.
CAUTIONS
• Never leave a sample in the AQUALAB after a reading has been taken. The sample may spill
and contaminate the instrument chamber if the instrument is accidentally moved or jolted.
• Never move the instrument after a sample has been loaded. Movement may cause the
sample material to spill and contaminate the sample chamber.
• Do not measure a sample that has a temperature greater than ±4 °C than the AQUALAB
chamber (Section2.2.2). Remove the sample until it is at room temperature.
NOTE: After measuring volatiles with the capacitance sensor, clean the chamber (Section4.2), place charcoal in the
chamber, and seal for a minimum of 5 min before switching to the dew point sensor.
Perform the following steps to take a reading.
1. Ensure the AQUALAB is plugged in and turned on.
The splash screen will appear, followed by the main Measurement tab (Section3.2.4.1).
2. For AQUALAB DUO instruments (Section2.5), use the UP and DOWN buttons to scroll
through all available product models that may be used (Figure4).
The moisture content value adjusts based on the selected model.
7
OPERATION
Figure4 Measurement screen for AQUALAB DUO Milk Powder product model
3. Verify cleanliness (Section4.2), calibration (Section4.1), and sample preparation
(Section2.2).
NOTE: The device fan can blow powdery substances; always verify the cleanliness of the sample chamber before
reading a new sample.
4. Move the chamber lever to the OPEN position and lift the chamber lid.
5. Check the top lip and outside surfaces of the sample cup to ensure they are free from
sample residue and conrm the sample cup is not overlled.
NOTE: Overfilling the sample cup may contaminate the chamber sensors.
The sample cup lid must be removed for correct functionality.
6. Place the prepared sample cup in the chamber.
7. Close the chamber lid.
8. Move the lever to the READ position to seal the sample chamber. The reading will
automatically start.
In 1 to 2 min, the rst measurement will display on the screen (this is an intermediate
reading). The instrument crosses the dew threshold numerous times to ensure
equilibrium and the accuracy of readings. Length of read times may vary depending
on temperature differences between the chamber and the sample as well as on other
properties of the sample (Section2.2). The default AQUALAB reading cycle continues
until the rates of change of three consecutive intermediate readings are <0.0005 aw of
each other.
When the instrument has nished its read cycle, results will display. The SAVE icon
replaces the spinning measurement icon, and, if enabled, a series of beeps sounds. The
results will include the water activity, read time, temperature, and, for AQUALAB DUO
instruments (Section2.5), moisture content for the selected product model (Figure5).
NOTE: Autosave only saves the moisture content value of the model selected at the end of the reading. Overwrite
the autosave by selecting the correct model using the UP and DOWN buttons and selecting SAVE.
8
AQUALAB
Figure5 Completed test results with both water activity and moisture content
9. Autosave (default setting) retains the data without any annotation (Section3.2.4.2).
To add an annotation, select SAVE, add desired letters, and select SAVE again (Figure6).
Figure6 Keyboard screen to annotate data results
2.4 VIEWING DATA
To view prior test results, use the following steps:
1. Press MENU to navigate to the Data tab (Figure7).
Figure7 Data tab
2. Select ENTER.
3. Scroll through the list of saved tests using UP and DOWN (to move one item at a time) or
RIGHT and LEFT (to move a page at a time).
9
OPERATION
Figure8 List of saved tests
4. Select ENTER.
The detailed test results screen will appear (Figure9). Tests can also be scrolled through
using the arrow buttons on this detailed screen.
Figure9 Detailed test results screen
5. Select OK to return to the list of tests.
6. Select CANCEL to return to the Data tab.
2.5 USING MOISTURE CONTENT (AQUALAB DUO ONLY)
The relationship between water activity and moisture content is called the moisture
sorption isotherm, and it is complex and unique to each product type.
AQUALAB DUO models generate water activity values and moisture content. The DUO models
use preloaded product-specific isotherm models to calculate moisture content and present
it on the screen with the water activity (Figure10). The AQUALAB 4TE and AQUALAB 4TEV can
be upgraded to an AQUALAB 4TE DUO and AQUALAB 4TEV DUO, respectively.
10
AQUALAB
Figure10 AQUALAB DUO display with water activity and moisture content readings
2.5.1 OBTAINING PRODUCT ISOTHERM MODELS
The isotherm relationship for each product is unique, and each product isotherm model
must be determined experimentally prior to testing moisture content with the AQUALAB
DUO.
There are several strategies that can be used to generate models. Please contact Customer
Support for information on model development.
2.5.2 LOADING AND ORGANIZING PRODUCT ISOTHERM MODELS
A product model must be loaded onto the AQUALAB DUO before it can calculate
moisture content. Models can be loaded onto the instrument by METER or by using
the AquaLink4 software (Section3.3.1). As many as 100 models can be stored on the
instrument.
The AquaLink 4 software uses a model loading tool to add and remove product models from
the AQUALAB DUO, allowing the user to control and organize product models.
The following steps explain how to load new models:
1. Download AquaLink 4 software from software.metergroup.com onto a computer.
2. Save the model les onto the same computer.
3. Open AquaLink software.
4. Connect the AQUALAB to the computer using the USB cord (or an RS-232 cord).
5. Turn the AQUALAB on.
6. In the AquaLink window, select the appropriate COM port from the dropdown menu.
7. Click Connect.
When the instrument is connected, the button will change to Disconnect.
8. Click Models.
11
OPERATION
The Model Manager window will show all current models (Figure11). If no models have
been loaded, the window will be empty.
Figure11 AquaLink 4 model loading tool
9. Click Import.
10. Navigate to the model saved on the computer and select.
Each model will need to be imported individually. The models should now show up in the
Model Manager window.
11. Click in the Sync box next to each model name that will be uploaded to the AQUALAB.
12. Click Apply.
13. After a few seconds, use UP and DOWN on the AQUALAB instrument to test if the
instrument can scroll through the new models (visible at the top of the Measurement
tab). The display screen should also have a placeholder for moisture content
measurements.
14. In the AquaLink window, click Disconnect.
15. Close the AquaLink program.
16. Unplug the AQUALAB from the computer.
2.5.3 MEASURING MOISTURE CONTENT
With product models loaded onto the instrument, the AQUALAB DUO can generate moisture
content and water activity simultaneously while taking a reading.
1. Press MENU to navigate to the Configuration tab (Figure12).
12
AQUALAB
Figure12 Changing moisture content model on the Conguration tab
2. Select %Moisture.
A list of available models appears, organized by name (Figure13).
Figure13 Product models for moisture content
3. Select the model for the product to be analyzed.
If the listed models do not apply, select None. No moisture content will appear on the
Measurement tab.
4. Select SAVE.
5. Navigate to the Measurement tab.
6. Take a reading (Section2.3).
The moisture content measurement (%MC) will appear below the water activity measurement
(Figure14) in the test results.
13
OPERATION
Figure14 AQUALAB DUO display with water activity and moisture content readings
2.5.4 MOISTURE CONTENT MODEL OFFSET
The AQUALAB DUO calculates moisture content values based on water activity readings
by utilizing models stored within the instrument. Because moisture content results vary
between reference methods, it is important to ensure that the model in the instrument
correlates well with the values obtained from the selected reference method (e.g., Karl
Fischer titration or oven loss on drying). Moisture content differences among various
methods are usually linear and can be easily corrected with a linear offset. Therefore, if
moisture contents calculated with the AQUALAB DUO instrument are not agreeing with the
reference method, the problem can likely be addressed by adjusting a linear offset.
Reference methods can differ between laboratories, so check for a linear offset upon receipt
of a new isotherm model from METER. In addition, the linear offset should be adjusted if
moisture contents calculated by the AQUALAB DUO instrument are consistently higher or
lower for a product than reference method values over several samples.
The following steps describe how to adjust for linear offset or how to create a new model
based off an old model:
1. Ensure the instrument is verified (Section4.1).
2. Collect three subsamples of the product for analysis.
3. Place one subsample into a sample cup (Section2.2).
4. Cover sample cup with a lid to limit exposure to ambient conditions.
5. Use the reference method to determine the average moisture content of the other
twosubsamples.
6. On the AQUALAB, press MENU to navigate to the Conguration tab.
7. Select Calibration.
8. Select %Moisture from the list of calibration types (Figure15).
NOTE: If %Moisture is not an option, the instrument may not be an AQUALAB DUO. Contact Customer Support.
14
AQUALAB
Figure15 Select %Moisture on the Calibration tab
The %Moisture Calibration screen will appear (Figure16).
Figure16 %Moisture Calibration screen
9. If creating an existing model, select New.
If editing an existing model, select Edit.
10. Scroll through the reference models for the desired product (Figure17).
11. Select ENTER.
12. Select Start (Figure18).
Figure17 Moisture content model list
15
OPERATION
Figure18 Start test
13. Place a sample in the sample chamber when prompted (Figure19).
Figure19 Prompt to place sample in chamber
14. Remove the lid from the sample cup prepared in step3 and place into the chamber.
15. Close and latch the lid.
16. Select OK to begin a reading.
Once the reading is complete, the measured water activity as well as the moisture
content based on the target model will display on the screen.
17. Adjust the moisture content value using UP and DOWN until it matches the average
moisture content value obtained from the reference method in step5 (Figure20).
Figure20 Adjust the moisture content value to match the reference method
18. Select SAVE.
16
AQUALAB
19. If editing an existing model, the model will update but automatically retain the
samename.
If creating a new model, enter a new name on the Annotation screen.
Select CANCEL to return to the Conguration tab and cancel the moisture content
adjustment.
20. Air out the chamber for at least 1 h.
21. Measure the sample again in normal sampling mode. The AQUALAB DUO should now
read the corrected moisture content value provided in step17.
If moisture content readings are still inconsistent with the reference method, contact
Customer Support.
2.5.5 RESTORE MOISTURE CONTENT DEFAULT SETTINGS
To restore the original model settings, use the following steps:
1. Press MENU to navigate to the Configuration tab.
2. Select Calibration.
3. Select %Moisture from the list of calibration types (Figure21).
NOTE: If %Moisture is not an option, the instrument may not be an AQUALAB DUO. Contact Customer Support.
4. Select Edit (Figure22).
Figure21 List of calibration types
Figure22 Select Edit
17
5. Select the desired model (Figure23).
Figure23 Moisture content model list
6. Select Defaults (Figure24).
OPERATION
Figure24 Default options
A conrmation dialog will appear (Figure25).
Figure25 Conrmation dialog to reset calibration to defaults
7. To restore the original model settings, select OK.
To cancel and return to the Calibration tab, select CANCEL.
A screen will conrm the restoration of factory calibration (Figure26).
18
AQUALAB
Figure26 Conrmation dialog that AQUALAB was reset to factory calibration
8. Select OK to return to the Conguration tab.
2.5.6 DELETING MODELS
If a model is no longer needed, it can be deleted directly from the AQUALAB. Models are not
user-specific, so if a model is deleted from the instrument, all users will lose access to it.
NOTE: Deleted models cannot be recovered from AQUALAB. Use AquaLink 4 to back up models.
1. Press MENU to navigate to the Configuration tab.
2. Select Calibration.
3. Select %Moisture from the list of calibration types (Figure27).
NOTE: If %Moisture is not an option, the instrument may not be an AQUALAB DUO. Contact Customer Support.
5. Select the desired model from the list (Figure28).
Select CANCEL to return to the %Moisture Calibration screen.
19
OPERATION
Figure28 Moisture content model list
A conrmation screen will appear indicating the model to be deleted (Figure29).
Figure29 Conrmation dialog to delete model
6. Select OK to delete the model.
Select CANCEL to return to the previous screen.
20
AQUALAB
3. SYSTEM
This section describes the specifications, components, and theory of the AQUALAB
instrument.
3.1 SPECIFICATIONS
MEASUREMENT SPECIFICATIONS
Water Activity
Range
Resolution
Accuracy±0.003 (4TE dew point)
Repeatability
Moisture Content (DUO only)
Accuracy0.1%–0.5% to moisture content reference
Repeatability0.02%
Temperature
Range15-50 °C
Resolution0.01 °C
Accuracy±0.2 °C
0.030–1.000 a
0.0001 a
±0.015 (4TEV capacitance)
0.001 a
w
w
w
Read Time
~5 min
PHYSICAL SPECIFICATIONS
Case Dimensions
Length26.7 cm (10.5 in)
Width17.8 cm (7.0 in)
Height12.7 cm (5.0 in)
Case Material
POLYLAC PA-765 (ABS) with re retardant
Sample Cup Capacity
14 mL (0.47 oz)
21
Weight
3.1 kg (6.8 lb)
Display
64 × 128 graphical
Operating Temperature
Minimum4 °C
TypicalNA
Maximum50 °C
Operating Environment
0%–90% noncondensing
Data Communications
USB A and RS-232 serial
9,600–115,000 baud
Power
110–220 VAC
50/60 Hz
SYSTEM
COMPLIANCE
Manufactured under ISO 9001:2015
EM ISO/IEC 17050:2010 (CE Mark)
3.2 COMPONENTS
The AQUALAB uses the chilled-mirror dew point technique to measure the water activity of
a sample. In an instrument that uses the dew point technique, the sample is equilibrated
with the headspace of a sealed chamber that contains a mirror and a means of detecting
condensation on the mirror. At equilibrium, the relative humidity of the air in the chamber is
the same as the water activity of the sample.
The AQUALAB DUO models make it possible to determine both moisture content and water
activity with one machine. For information about upgrading an AQUALAB 4TE or 4TEV to a
DUO, contact Customer Support.
The AQUALAB main components include the display screen and sample chamber (Figure30).
22
Display
AQUALAB
Lever
Buttons
Figure30 AQUALAB exterior
Sample chamber
3.2.1 CORDS AND CABLES
The AQUALAB is shipped with a power cord and a USB cable.
The power cord plugs into the back of the instrument and must be plugged into a grounded
outlet or power strip.
WARNING: Only use the supplied power cord or one rated for AQUALAB 4 and certified for the country of use. The cord
must be a minimum of 18 AWG and have a rating for 10 A or greater.
The USB cable has one USB A connector to connect to a computer and one USB B connector
to connect to the AQUALAB. The data from the AQUALAB can be saved to the computer with
this connection (Section3.3.1).
The AQUALAB may also be connected to a computer using a RS-232 serial cable (not
included).
3.2.2 SAMPLE CHAMBER
Externally, the sample chamber lever has two positions: OPEN (handle moved to the right)
and READ (handle moved to the left).
Internally, there are two blocks within the sample chamber: an upper lid block and a
lower sample block (Figure31). The blocks are temperature controlled and regulate the
temperature of the sample and sample chamber.
The mirror temperature is precisely controlled by a thermoelectric (Peltier) cooler. Detection
of the exact point condensation first appears on the mirror is observed with a photoelectric
cell. A beam of light is directed onto the mirror and reflected into a photo detector cell. The
photo detector senses the change in reflectance when condensation occurs on the mirror. A
23
SYSTEM
thermocouple attached to the mirror then records the temperature at which condensation
occurs. The AQUALAB then signals with beeps and displays the final water activity and
temperature.
The AQUALAB uses an internal fan to circulate the air within the sample chamber to
reduce equilibrium time. Since the AQUALAB measures both dew point and sample surface
temperatures simultaneously, it eliminates the need for complete thermal equilibrium,
thereby reducing measurement times to <5 min for most samples.
Additionally, the AQUALAB 4TEV uses a capacitance humidity sensor to measure the water
activity of a sample. The sensor is suspended in the headspace of the chamber and uses
a special polymer material sandwiched between two microporous electrodes to sense
humidity changes. The sensor measures a specific capacitance, which is translated by
the software and displayed as water activity on the instrument screen. At equilibrium, the
relative humidity of the air in the chamber is the same as the water activity of the sample.
Lever
Latch
Thermopile
Capacitance sensor
filter (TEV only)
Mirror
O-ring
Fan
Top block
Photoelectric (optical)
sensor
Sample block
Figure31 Sample chamber interior
3.2.3 BUTTONS
The power switch is located on the lower left corner of the AQUALAB back panel. After
being turned on, the AQUALAB should warm up for 15 minutes before operation to ensure
accuratereadings.
24
AQUALAB
There are four arrow buttons: LEFT, RIGHT, UP, and DOWN (Figure32). These buttons allow
for navigation through the various screens on the AQUALAB. The three round buttons
have variable uses, depending on what icon is represented above them on the display
(Section3.2.4).
Figure32 AQUALAB buttons under the display screen
3.2.4 DISPLAY SCREEN
The display screen (Figure33) has three tabs: Measurement, Configuration, and Data.
Measurement tab
Sensor
Reading time elapsed
Figure33 Display screen
Configuration tab
Reading results
25
Data tabCurrent time
Button icons
SYSTEM
The button icons on the display change to show the available actions for the screen (Table 2).
Table 2 AQUALAB button icons
IconNameAction
ENTERAccepts the current action
CANCELEnds the current action
MENUSwitches between the Measurement, Conguration, and Data tabs
SAVESaves a setting or a reading
OKAccepts the input from the user
AUDIO OFFSilences beeping
AUDIO ONEnables beeping
3.2.4.1. MEASUREMENT TAB
The Measurement tab (Figure34) is the main screen and must be visible to start a reading.
Measurement results are displayed on this screen.
Figure34 Measurement tab
Using the RIGHT or LEFT buttons changes the display to a temperature equilibration screen
(Figure35). This screen shows the temperature difference between the sample and the lid.
26
AQUALAB
Figure35 Temperature difference between sample and lid
On AQUALAB DUO models, using the UP or DOWN buttons changes the results according to
the models loaded onto the instrument.
The main screen shows the water activity in the middle of the screen and above the sample
temperature. The measurement read time is shown at the bottom left of the screen. The
AQUALAB 4TEV model will display either DEW or CAP indicating whether the dew point or
capacitance sensor is being used.
3.2.4.2. CONFIGURATION TAB
The Configuration tab provides a menu of configuration options (Figure36). Use UP and
DOWN to move the selection through the various configuration options or LEFT and RIGHT
to page through the options. Use ENTER to select the highlighted option.
Figure36 Conguration tab screens
27
SYSTEM
• Calibration. Select to start the calibration process (Section4.1) for water activity or
moisture content (Figure37). Resetting factory defaults is described in Section4.1.4.
Figure37 Calibration option
• Temperature. Select to set the AQUALAB to the desired temperature using UP and DOWN.
When finished, select SAVE (Figure38).
The AQUALAB 4TE models may be set between 15 and 50 °C in 0.1 °C intervals. The default
temperature is 25 °C.
Figure38 Temperature option
• Temp Eq. Select to set the acceptable temperature difference between the sample block
and the sample before starting a water activity measurement (Figure39).
The range is 0.1 to 4.0 °C. A setting of 4.0 °C begins the measurement when the sample is
<4.0 °C above or below the block temperature. A setting of 0.1 °C begins the measurement
when the sample is <0.1 °C above or below the block temperature.
28
AQUALAB
Figure39 Temp Eq screen
• Sensor (AQUALAB 4TEV only). Select to choose a capacitance sensor or chilled-mirror dew
point sensor for sampling volatiles or nonvolatiles, respectively. The AQUALAB 4TE model
only has a dew point option.
• Mode. Select to choose between Single, Continuous, Custom, or Low-Emitting mode
(Figure40). The current mode settings appear at the top of the screen with the number of
tests appearing first, followed by the stability value (∆ aw ).
Figure40 Custom mode options
Single mode reads the sample once. Continuous mode reads the sample until the chamber lid is opened or the test is
stopped by selecting CANCEL.
The AQUALAB reads the sample, displays results, and begins another read cycle without
further action from the user. The machine signals the completion of each reading with a
beep. A timer on the screen tracks the cumulative read time.
All readings taken during Continuous mode are saved on the instrument memory if the
autosave feature is turned on (default). If the AQUALAB is connected to a computer using
AquaLink 4 (Section3.3.1), all readings can be downloaded to the AquaLink 4 software.
Custom mode reads a sample multiple times until a set level of stability is achieved. For
example, the instrument could be set to read the sample until two consecutive tests are
within ±0.001 aw of each other.
Use RIGHT and LEFT to change between the Readings or ∆ aw settings.
Use UP and DOWN to change to select the number of readings (2 to 9).
29
SYSTEM
Use UP and DOWN to select the ∆ aw value (any number from 0.0005 to 0.0200)
(Figure41).
Figure41 Custom mode screen
Select SAVE to update and exit. Select CANCEL to exit without updating. The Mode
screen reappears with the updated custom settings at the top of the screen).
If autosave is turned on (default), all test readings will save to the instrument memory,
but only the final reading will remain on the Measurement screen. If the AQUALAB is
connected to a computer using AquaLink 4 (Section3.3.1), AquaLink 4 downloads all
readings taken during a Custom mode test.
Low-Emitting mode gives the option of speeding up test time by adjusting the
equilibrium trigger value (Figure42).
Figure42 Low-Emitting mode screen
AQUALAB determines vapor equilibrium at the end of a test by comparing sequential
water activity values, looking for a trigger value difference <0.0005 aw. This value can be
adjusted to any value between 0.0003 and 0.0030 aw. Increasing the trigger value causes
a subsequent reduction in instrument accuracy and precision but results in a shorter
test time. This mode is for samples that are slow to equilibrate, such as vegetable
oils, high-fat samples, and high-viscosity samples. In these types of cases, the loss
in performance may be acceptable in order to speed up the analysis time. Use a high
trigger value only after careful consideration of the impact on test results.
• Date. Select to set the date in the instrument. Use RIGHT and LEFT to change between
the month, day, and year categories and UP and DOWN to change the individual values
(Figure43).
30
AQUALAB
The date is recorded with each water activity reading.
Figure43 Date option
• Time. Select to set the time in the instrument. Use RIGHT and LEFT to change between the
hour and minute categories and UP and DOWN to change the individual values (Figure44).
The hour setting automatically changes between AM and PM.
The time is recorded with each water activity reading.
Figure44 Time option
• Regional Formatting. Select to configure how the AQUALAB displays information. Choose
the temperature scale (Celsius or Fahrenheit), the date display (mm/dd/yy or dd/mm/yy), the
hour format (12h or 24h), and the language (Figure45).
Figure45 Regional Formatting option
• Admin Settings. Select to create an administrator password as well as create, edit, and
delete additional users (Figure46).
31
SYSTEM
Figure46 Admin Settings option
The Admin Settings allow the administrator to grant or block access to some or all the
configuration options.
NOTE: Once the administrator is set up, the password cannot be recovered. The AQUALAB must be sent back to
METER to be reset.
Administrators can add, edit, or delete users from the User Setup screen. The keyboard
allows for lowercase, uppercase, and accented letters (Figure47).
Figure47 Keyboard screen
NOTE: User setup is not required for instrument operation. It is for users requiring 21 CFR Part11 compliance or who
want to save specific settings.
Once the administrator and users are set up, an Access option will appear on individual
user screens (Figure48).
Figure48 Access option on a user screen
32
AQUALAB
To lock out users from accessing certain settings, enter the Access function and use UP and
DOWN to find the desired option. Selecting the option will toggle it ON or OFF: calibration,
temperature, temperature equilibration, sensor selection, mode, date/time, region,
password, autosave, number of beeps, and delete (Figure49). These options can also be all
locked or unlocked at the same time.
Figure49 Access settings rst screen
• Autosave. Select to turn Autosave on or off. Autosave stores water activity readings within
the instrument automatically for every water activity reading in the internal memory. The
AQUALAB can store up to 8,000 records before the memory is full.
Any individual reading may be saved manually right after completing the test and before
beginning the next test, regardless of the Autosave setting.
NOTE: If a reading is autosaved, it is not possible to give it an annotation later.
• Beeps. Select to change the number of notification beeps for a finished test (four,
continuous, or no beeps). The audible notification can also be turned off.
• Diagnostics. Select to view information regarding pertinent sensors.
For the chilled-mirror dew point sensor, the Diagnostics option provides lid, base, sample
and mirror temperatures, optical voltage, and the user offset. Figure50 shows typical
values for the sensors. Lid, base, and sample temperatures may fluctuate but should
not change more than 0.03 ºC. Typical ranges for the lid, base, and sample temperatures
is between 24.5 and 25.5 °C. The optical sensor has a typical range between 300 and
2,900mV. If values are outside these ranges, refer to Section4.5.
Figure50 Chilled-mirror dew point sensor Diagnostics screen
33
SYSTEM
For the capacitance sensor (TEV models only), Diagnostics provides lid, base, and sample
temperatures, relative humidity, and the capacitive sensor user offset (Figure51). If any of
the temperature values are outside the ranges specified in the previous paragraph, refer to
Section4.5.
Figure51 Capacitance sensor Diagnostics screen
• %Moisture (DUO only). Select to view all isotherm models on the instrument (Section2.5).
• About. Select to view instrument information including the serial number and firmware
code version of the instrument (Figure52).
Figure52 About screen
3.2.4.3. DATA TAB
Data can be viewed or deleted from the Data tab (Figure53).
Figure53 Data tab
34
AQUALAB
• View. Select to view stored measurements with the most recent measurements at the
top of the table (Figure54). Use UP and DOWN to move through the stored data. Use LEFT
and RIGHT to page quickly through the data. Refer to Section3.3 for information about
downloading these readings to a computer.
Figure54 View data
Select a highlighted reading to view detailed information (Figure55).
Figure55 Data sample detail screen
The screen displays the name of the reading (if annotated), the water activity of the sample,
the temperature of the sample, the test time, the user who ran the test (if set up), the
reading date, the sensor used, the time the reading was taken, and the sequence number of
the stored reading. Use UP and DOWN to scroll through readings.
• Delete. Select this option to delete all data currently stored in the instrument. Readings
cannot be deleted individually. If the information has not been backed up with AquaLink 4, a
reminder will appear (Figure56).
NOTE: Deleted data cannot be recovered.
35
SYSTEM
Figure56 Delete option backup reminder dialog
3.3 COMPUTER INTERFACE
The AQUALAB can connect to a computer using USB (included) or RS-232 to send
water activity data for further analysis and storage. The interface is run through the
AquaLink4 software or a terminal communication program.
NOTE: Install the USB driver before connecting the USB cable to the computer by downloading from software.
metergroup.com.
3.3.1 AQUALINK 4 SOFTWARE
AquaLink 4 is available for use with the AQUALAB. AquaLink 4 is a Microsoft® Windows®based program designed for data collection and customized report generation for all
AQUALAB models. AquaLink 4 logs water activity, temperature, and time and date of
measurement along with other information (Figure57). AquaLink 4 also has sample
identification and comment fields to help annotate the data the AQUALAB is gathering.
The AquaLink 4 software can also download data (including moisture content) from the
instrument, present the data in table form, filter the data, and print reports. Refer to
AquaLink 4 software help files for further instructions.
Figure57 AquaLink 4 main screen
36
AQUALAB
3.3.2 USING A TERMINAL PROGRAM
There are several terminal program options. METER has its own terminal program
(DecaTerm) that can be downloaded from software.metergroup.com. Two other options
are TeraTerm, a free program that can be found on the internet, and Hyperterminal, the
standard program with Microsoft Windows prior to Windows 7 software.
To integrate a terminal program with AQUALAB, use the following steps:
1. Power on the AQUALAB.
2. Connect the USB interface cable to the computer.
3. Follow the instructions for the program with the following settings:
c. Choose correct COM Port
d. Set or verify COM Properties
e. Bits per second (Baud rate): 9600
Data: 8 bit
Parity: none
Stop: 1 bit
Flow control: none
Upon successful completion of a water activity reading, the data in the terminal program
displays measurement time (in minutes), sample temperature, and water activity. Table
3 shows an example data return.
Table 3 Terminal data
Measurement
Time
3.124.30.862
Temperature
(ºC)
a
w
3.4 THEORY
Water is a major component of foods, pharmaceuticals, and cosmetics and influences the
product texture, appearance, flavor, and shelf life. Quantifying these attributes require
two basic types of water analysis: moisture content and water activity (aw ).
3.4.1 MOISTURE CONTENT
Moisture content implies a quantitative analysis to determine the total amount of water
present in a sample. There are two primary methods for determining moisture content:
loss on drying and Karl Fisher titration. Secondary methods, such as near infrared
(NIR) and nuclear magnetic resonance (NMR), may also be used. Moisture content
determination is essential in meeting product nutritional labeling regulations, specifying
recipes, and monitoring processes.
37
SYSTEM
However, moisture content alone is not a reliable indicator for predicting microbial responses
and chemical reactions in materials. The limitations of moisture content measurement are
attributed to differences in the intensity that water associates with other components.
3.4.2 WATER ACTIVITY
Water activity (aw ) is a measurement of the energy status of the water in a system. The
value indicates how tightly water is bound, structurally or chemically, within a substance.
The lower a sample’s water activity, the more tightly bound that water is within the sample.
The concept of water activity is of particular importance in determining product quality
and safety. It predicts safety and stability with respect to microbial growth, chemical and
biochemical reaction rates, and physical properties.
Water activity is a measure of the energy status of the water in a system and is a far better
indicator of product stability than moisture content. Figure58 shows how the relative
activity of microorganisms, lipids, and enzymes relate to water activity. While other factors,
such as nutrient availability and temperature, can affect the relationships, water activity is
the best single measure of how water affects these processes.
Figure58 Water activity diagram adapted from Labuza (1976)
Researchers measure the water activity of a system by equilibrating the liquid phase water
in the sample with the vapor phase water in the headspace and measuring the relative
humidity of the headspace. In the AQUALAB, a sample in a sample cup is sealed inside the
sample chamber, which contains a fan, a dew point sensor, and an infrared thermometer.
The fan speeds equilibrium and controls the boundary layer conductance of the dew
point sensor. The dew point sensor measures the dew point temperature of the air in the
chamber, and the infrared thermometer measures the sample temperature. From these
measurements, the relative humidity of the headspace is computed as the ratio of the dew
point temperature saturation vapor pressure to the saturation vapor pressure at the sample
38
AQUALAB
temperature. When the water activity of the sample and the relative humidity of the air
are in equilibrium, the measurement of the headspace humidity gives the water activity of
the sample. Water activity is the relative humidity of air in equilibrium with a sample in a
sealedchamber.
In addition to equilibrium between the liquid phase water and the vapor phase, the internal
equilibrium of the sample is important. If a system is not at internal equilibrium, one might
measure a steady vapor pressure (over the period of measurement) which is not the true
water activity of the system. An example of this might be a baked good or a multicomponent
food. Initially out of the oven, a baked good is not at internal equilibrium; the outer surface is
at a lower water activity than the center of the baked good. One must wait a period of time in
order for the water to migrate and the system to come to internal equilibrium It is important
to keep in mind that by this definition, water activity is an equilibrium measurement.
The water activity of a sample is influenced by factors that affect the binding of water. These
factors include temperature, osmotic, matric, and pressure effects. Typically, water activity
is measured at atmospheric pressure, so only the osmotic, temperature, and matric effects
areimportant.
3.4.2.1. TEMPERATURE EFFECTS
Temperature plays a critical role in water activity determination. Most critical is the
measurement of the difference between sample and dew point temperature. For water
activity measurements to be accurate to 0.001, temperature difference measurements
need to be accurate to 0.017 °C. The AQUALAB infrared thermometer measures the
difference in temperature between the sample surface and the sample block. The
thermometer is carefully calibrated to minimize temperature errors; however, achieving
0.017 °C accuracy is difficult when temperature differences are large. Most accurate
measurements are obtained when the sample is near sample chamber temperature.
Another effect of temperature on water activity occurs when samples are near saturation.
A sample that is close to 1.0 aw and is warmer than the sensor block will cause water to
condense within the chamber. This causes errors in the measurement and in subsequent
measurements until the condensation disappears. For example, a sample at 0.75 aw only
needs to be 4 °C above the sample chamber temperature to cause condensation to form.
The AQUALAB warns the user if a sample temperature is more than 4 °C above the chamber
temperature, but for high water activity samples, the operator needs to be aware that
condensation can occur if a sample is warmer than the sample block.
There are several advantages in having a temperature-controlled water activity meter. A few
major reasons are detailed here.
1. Research purposes.
Researchers can use temperature control to study the effects of temperature on the
water activity of a sample, make a comparison of the water activity of different samples
independent of temperature, and conduct accelerated shelf-life studies or other
water activity studies where temperature control is critical. There are many shelf-life,
packaging, and isotherm studies in which temperature control would be very benecial.
39
SYSTEM
2. Compliance with government or internal regulations for specic products.
Though the water activity of most products varies by less than ±0.02 per degree Celsius,
some regulations require measurement at a specic temperature. The most common
specication is 25 °C, though 20 °C is sometimes indicated.
3. Minimization of extreme ambient temperature uctuations.
If the environmental and AQUALAB temperatures uctuate by as much as ±5 °C daily,
water activity readings may vary by ±0.01 aw. Temperature control eliminates variations
caused by changes in ambient conditions.
The AQUALAB models have thermoelectric components installed to allow the instrument
to maintain a set chamber temperature. Customers can set the temperature using the
Configuration tab of any of the AQUALAB models.
3.4.2.2. OSMOTIC EFFECTS
Osmotic effects are well known from biology and physical chemistry. Water is diluted
when a solute is added. If this diluted water is separated from pure water by a
semipermeable membrane, water tends to move from the pure water side through the
membrane to the side with the added solute. If sufficient pressure is applied to the
solute-water mixture to just stop the flow, this pressure is a measure of the osmotic
potential of the solution. Addition of 1 mol of an ideal solute to 1 kg of water produces an
osmotic pressure of 22.4 atm. This lowers the water activity of the solution from 1.0 to
0.98 aw. For a given amount of solute, increasing the moisture content of the systems
dilutes the solute, decreasing the osmotic pressure, and increasing the water activity.
Since microbial cells are high concentrations of solute surrounded by semipermeable
membranes, the osmotic effect on the free energy of the water is important for
determining microbial water relations and therefore microbe activity.
3.4.2.3. MATRIX EFFECTS
The sample matrix affects water activity by physically binding water within its structure
through adhesive and cohesive forces that hold water in pores and capillaries and to
particle surfaces. If cellulose or protein were added to water, the energy status of the
water would be reduced. Work would need to be done to extract the water from this
matrix. This reduction in energy status of the water is not osmotic, because the cellulose
or protein concentrations are far too low to produce any significant dilution of water.
The reduction in energy is the result of direct physical binding of water to the cellulose
or protein matrix by hydrogen bonding and van der Waals forces. At higher water activity
levels, capillary forces and surface tension can also play a role.
3.4.3 CHILLED-MIRROR DEW POINT LIMITATIONS
The limitation of the AQUALAB 4TE is its ability to accurately measure samples with high
concentrations (typically >1%) of certain volatile compounds such as ethanol or propylene
glycol, which can condense on the surface of the chilled mirror. The extent of the effect
40
AQUALAB
is determined by how readily the material volatilizes, which is both concentration and
matrix dependent. Therefore, even if a sample contains materials that could volatilize, it
may still be possible to make accurate readings using the chilled-mirror dew point sensor.
The AQUALAB TDL provides a solution for products containing volatile materials. The TDL
uses a tunable diode laser which shines light of a controlled wavelength, specific to water
vapor, at a detector that receives light from the laser. The vapor pressure of the headspace
of the instrument in equilibrium is determined by the loss of signal strength from the laser
caused by the presence of water vapor in the headspace. For more information, contact
Customer Support.
3.4.4 WATER POTENTIAL
Water activity is closely related to a thermodynamic property called the water potential,
or chemical potential ( µ) of water, which is the change in Gibbs free energy (∆G ) when
water concentration changes. Equilibrium occurs in a system when µ is the same
everywhere in the system. Equilibrium between the liquid and the vapor phases implies
that µ is the same in both phases. This means the measured water potential of the vapor
phase can be used to determine the water potential of the liquid phase. Gradients in µ
are driving forces for moisture movement. In an isothermal system, water tends to move
from regions of high water potential (high aw ) to regions of low water potential (low aw ).
Moisture content is not a driving force for water movement and, therefore, cannot be
used to predict the direction of water movement, except in homogeneous materials.
3.4.5 SORPTION ISOTHERMS
Changes in moisture content affect both the osmotic and matric binding of water in a
product. Thus, a relationship exists between the water activity and moisture content.
This relationship is called the sorption isotherm and is unique for each product. Besides
being unique to each product, the isotherm changes depending on whether it was
obtained by drying or wetting the sample. Typically, large safety margins are built into
moisture content specifications to allow for these uncertainties.
While the sorption isotherm is often used to infer water activity from moisture content,
one could easily go the other direction and infer moisture content from water activity.
This is particularly attractive because water activity can be measured much more quickly
than moisture content. This method gives particularly good precision in the center of the
isotherm. In order to infer moisture content from water activity, an isotherm for the particular
product is needed. METER sells an isotherm generator called the AQUALAB Vapor Sorption
Analyzer (VSA) or METER can run the isotherm for a fee. Visit metergroup.com/food/services/
water-activity-and-isotherm-testing for more information.
For example, if using the AQUALAB to monitor the moisture content of dried potato flakes,
measure the water activity and moisture content of potato flakes dried to varying degrees
using the standard drying process for those flakes. That data is used to construct an
41
SYSTEM
isotherm and infer the moisture content using the measured water activity of samples and
that isotherm. The DUO upgrade to AQUALAB 4TE and TDL enables users to the determine
moisture content and water activity simultaneously.
42
AQUALAB
4. SERVICE
This section contains calibration and verification information, cleaning and maintenance
guidelines, troubleshooting steps, and customer support information.
4.1 VERIFICATION AND CALIBRATION
It is important to verify the AQUALAB water activity calibration against known standards to
guarantee optimal performance and accuracy. METER recommends verification daily, once
per shift, or before each use.
METER also recommends annual factory calibration to maintain optimal performance.
4.1.1 WATER ACTIVITY VERIFICATION
The AQUALAB uses the chilled-mirror dew point technique to determine water activity.
Because this is a primary measurement of relative humidity, no calibration is necessary;
however, METER recommends periodic verification. The components used by the
instrument to measure water activity are subject to contamination, which may affect
AQUALAB performance. Therefore, frequent verification assures that the AQUALAB is
performing correctly. In addition, providing a linear offset can be used to overcome any
additional instrument drift.
4.1.1.1. VERIFICATION STANDARDS
Verification standards are specially prepared, unsaturated salt solutions having a
specific molality and water activity value that are accurately measurable. The verification
standards that were sent with the initial shipment are very accurate and readily available
from METER. Using verification standards to verify accuracy can greatly reduce preparation
errors. Performance Verification Standards come in seven water activity levels: 1.000,
0.984, 0.920, 0.760, 0.500, 0.250, and 0.150 aw (Table 4). The standards are produced under a
strict quality assurance regime. Please contact Customer Support.
Table 4 Verication standards
Verification Standard at 25 °C
17.18 mol/kg LiCl0.150 ±0.0050.150 ±0.015
13.41 mol/kg LiCl0.250 ±0.0030.250 ±0.015
8.57 mol/kg LiCl0.500 ±0.0030.500 ±0.015
6.00 mol/kg NaCl0.760 ±0.0030.760 ±0.015
2.33 mol/kg NaCl0.920 ±0.0030.920 ±0.015
0.50 mol/kg KCl0.984 ±0.0030.984 ±0.015
Steam Distilled Water1.000 ±0.0031.000 ±0.015
NOTE: Safety Data Sheet (SDS) for these standards are available at sds.metergroup.com.
Dew Point a
43
w
Capcitive a
w
SERVICE
To use a verification standard, remove the twist top and pour the contents into an AQUALAB
sample cup. Information about the standard value and molality can be found printed on
the outside of the plastic vial. If for some reason METER verification standards are not
available,contact Customer Support for instructionson how to create a verification standard
salt solution.
In TEV models, the capacitance sensor can exhibit hysteresis. When a high water activity
standard or sample is measured, this may influence future readings. After measuring a high
water activity sample, allow 1 h for the sensor to dry. Additionally, desiccant or activated
carbon can be used to accelerate the drying process.
NOTE: To avoid inaccurate water activity readings, verification standards should be used once immediately after
opening. Do not store standards in sample cups for repeated use.
4.1.1.2. VERIFICATION OF CALIBRATION
Verification of the calibration should be performed regularly to ensure the AQUALAB is
operating within specification. METER recommends verification be run once per shift or
prior to operation. The procedure for verification involves reading a sample of known water
activity. METER recommends using a standard close to that of the sample being measured.
If operating in volatiles mode using the capacitance sensor or measuring a broad range of
water activity values, METER recommends bracket the sample range. Capacitance sensors
can show significantly more drift when compared to a chilled mirror and can exhibit some
nonlinear behavior. Verifications should not be performed with only water standards.
Checking the water activity of a standard solution checks for the possibility of unit
contamination or shifts in the linear offset from other causes.
The following steps explain how to verify for linear offset of the AQUALAB (Figure59).
1. If measuring samples over a wide range of water activity values, select two standards
that best bracket the region. If measuring a relatively narrow region, select a sample that
most closely matches the sample range being measured.
For example, if testing for water activity readings ranging between 0.621 and 0.713, use
the 8.57 mol/kg LiCl (0.50 aw ) standard for the rst verication and the 6.00 mol/kg,
NaCl (0.76 aw ) for the second verication.
NOTE: The AQUALAB needs to warm up for approximately 15 min to make accurate readings.
2. Empty a vial of the lower water activity verication standard into a sample cup.
3. Place it in the AQUALAB testing chamber. Make sure that the standard is as close to the
instrument temperature as possible. See Section2.2.2 for detailed instructions.
NOTE: Make sure the rim and outside of the sample cup are clean.
4. Carefully close the lid and move the lever to the READ position.
5. Take two readings.
44
AQUALAB
The water activity readings should be within ±0.003 aw of the given value for the dew
point or ±0.015 for capacitance when testing the verication standard. The standards
will read at 25 °C. If other temperatures are required, refer to Table 5.
Table 5 Temperature correction of verication standards
Temperature
(°C)
151.0000.9840.9230.7610.4920.2380.140
201.0000.9840.9220.7600.4960.2450.145
251.0000.9840.9200.7600.5000.2500.150
301.0000.9840.9200.7600.5040.2550.155
351.0000.9840.9200.7600.5080.2610.160
401.0000.9840.9210.7600.5120.2660.165
501.0000.9840.8940.7400.5170.2750.172
NOTE The AQUALAB measures these verification standards to ±0.003 aw with the dew point sensor and ±0.015 aw with
the capacitance sensor.
Water
0.50 mol/kg
KCL
2.33 mol/kg
NaCl
6.00 mol/kg
NaCl
8.57 mol/kg
LiCl
13.41 mol/kg
LiCl
17.18 mol/kg
LiCl
6. The readings may lead to one of three outcomes.
a. If the AQUALAB reads within ±0.003 aw of the rst verication standard for dew point
and ±0.015 for capacitance, take two readings of the second verication standard.
The second water activity reading for the second verication standard should be
within ±0.003 aw for the dew point and ±0.015 for the capacitance sensors.
b. If either verification standard is not correct, it is probably due to contamination of the
sensor chamber. Clean and air out the chamber (Section4.2) and repeat verification
from step2.
c. If readings are consistently outside the water activity of the first verification standard
by more than ±0.003 aw for dew point and ±0.015 for capacitance, a linear offset
can be applied. Adjust the reading to match the correct verification standard value
(Section4.1.2).
45
SERVICE
Measure verification standard
Repeat process
Clean sample
chamber
Reread first
standard
Go to offset
procedure
Figure59 Verication standard owchart. A check indicates AQUALAB veried the standard within
specication; a cross indicates AQUALAB did not verify the standard within specications.
Read second
standard
Go to sampling
procedure
Clean sample
chamber
4.1.2 LINEAR OFFSET
After verification and cleaning, the instrument an offset may be necessary.
1. Navigate to the Configuration tab.
For the AQUALAB 4TEV, the currently selected sensor for the instrument will be the one
offset. Make sure to select the correct sensor before beginning the offset.
2. Select Calibration.
NOTE: The DUO model shows both water activity and moisture content on this screen. Select Water Activity.
3. Select Start (Figure60).
Figure60 Start dew point calibration
To return to the prior tab, select CANCEL.
4. A prompt will appear to insert a fresh standard and seal the chamber (Figure61).
NOTE: The same verification standard can be used to verify and adjust the linear offset. If using the same
verification standard, do not open the sample chamber between verification and offset.
46
AQUALAB
Figure61 Calibration instruction dialog
5. Empty the whole vial of water activity standard into a sample cup.
METER recommends using the 6.00 NaCl (0.76 aw ). Do not adjust for the offset using
steam distilled water.
6. Ensure the rim and outside of the cup are clean.
7. Place the sample cup in the sample chamber.
8. Carefully close the lid and move the lever to the READ position.
9. Select OK to begin testing.
NOTE: To interrupt the offset procedure, return the lever to the OPEN position or select CANCEL to return to the
previous screen.
After the AQUALAB has nished measuring the verication standard, it displays a
Change the offset screen (Figure62).
Figure62 Change the offset screen
10. Use UP and DOWN to adjust the water activity reading to its proper value for the
particular verication standard.
11. Select SAVE to store this new value.
To cancel and return to the main menu, select CANCEL to make no changes.
12. Restart the verication procedure in Section4.1.1.
If incorrect verication standard readings persist after cleaning the chamber and
adjusting for linear offset, contact Customer Support for further instructions.
47
SERVICE
4.1.3 MULTIPOINT CALIBRATION (TEV ONLY)
The capacitance sensor used for measuring the water activity of materials with volatiles
(AQUALAB 4TEV models only) is a secondary method for measuring water activity and
may require a slope change to the calibration in addition to a linear offset. This is the case
when the offset in capacitance mode is different at high water activities than low water
activities.
The 0.25, 0.50, 0.76, and 0.92 aw unsaturated salt standards are needed to proceed with
multipoint calibration.
1. Navigate to the Configuration tab.
For the AQUALAB 4TEV, make sure to select the capacitance sensor before beginning the
multipoint calibration.
2. Select Calibration from the Conguration tab (Figure63).
Figure63 Capacitance sensor calibration screen
3. Highlight Type and select ENTER to toggle to Multipoint.
4. Select Start.
Prompts will instruct the user to insert a fresh standard and seal the chamber
(Figure64).
Figure64 Prompt to insert fresh standard
5. Empty the whole vial of 0.25 aw standard solution into a sample cup.
6. Ensure the rim and outside of the cup are clean.
48
AQUALAB
7. Place the sample cup in the AQUALAB sample chamber.
8. Carefully close the lid and move the lever to the READ position.
9. Select OK to begin testing.
After AQUALAB has nished measuring the verication standard, a new screen appears
requesting that a 0.50 aw standard be placed in the chamber.
10. Repeat steps5 through 9 using 0.50, 0.76, and 0.92 aw standards.
NOTE: To end the multipoint calibration program, select CANCEL to return to the previous screen.
When measurements are complete on all four standards, the Verication Complete
screen appears showing the testing results for each standard (Figure65).
Figure65 Verication Complete screen with results
11. Select OK to continue or CANCEL to cancel the entire process.
NOTE: Select the audio icon to turn beeping on and off.
12. To make adjustments to the calibration, select OK.
Select CANCEL to cancel without adjusting the calibration (Figure66).
Figure66 Prompt to adjust calibration
13. To save the new calibration changes, select SAVE.
To cancel the multipoint calibration without saving the new changes, select CANCEL
(Figure67).
49
SERVICE
Figure67 Calibration Complete screen
Once the multipoint calibration is saved, a conrmation screen will appear (Figure68).
Figure68 Calibration saved conrmation
14. Select OK to continue.
15. If the calibration is canceled at any point, a Calibration Canceled conrmation will
appear. Select OK to continue (Figure69).
Figure69 Calibration canceled conrmation
16. Let the sample chamber air out for at least 1 h.
17. Measure a 0.25 or 0.50 aw verication standard in the Measurement tab (with
capacitance sensor type).
18. Verify the AQUALAB reads within ±0.015 aw at a given temperature.
50
AQUALAB
19. Measure a 0.76 aw verication standard according to the verication procedure detailed
in Section4.1.1.
If both verication readings are within ±0.015 aw , the instrument is ready to begin
testing.
If incorrect verication standard readings persist, contact Customer Support.
4.1.4 RESTORE FACTORY DEFAULTS
To restore original calibration settings, do the following:
1. Navigate to the Configuration tab using MENU.
NOTE: For TEV models, ensure the correct sensor is selected.
2. Select Calibration.
If using a DUO model, also select Water Activity.
3. Select Defaults to access the Restore Factory Defaults routine (Figure70).
Figure70 Calibration screen with Defaults selected
A conrmation dialog will appear (Figure71).
Figure71 Conrmation dialog to reset defaults
4. Select OK.
Select CANCEL to return to the Calibration menu.
The instrument will conrm the factory calibration has been restored (Figure72).
51
SERVICE
Figure72 Conrmation that factory calibration was reset
5. Select OK.
4.2 CLEANING
Keeping the AQUALAB clean is vital to maintaining the accuracy of the instrument. Dust and
sampling debris can contaminate the sampling chamber, so regular cleaning is essential.
To clean the AQUALAB, carefully follow these instructions and refer to the labeled
diagram in Figure73. A video is also available at metergroup.com/meter_knowledgebase/
aqualab-4te-certification.
Lever
Latch
Thermopile
Capacitance sensor
filter (TEV only)
Photoelectric (optical)
sensor
Mirror
O-ring
Fan
Top block
Sample block
Figure73 AQUALAB sample chamber diagram
The purpose of the cleaning procedure is to remove grease, dirt, and other soluble
substances that can absorb or release water during verification, calibration, or sample
testing. The mirror must be perfectly clean for a smooth and even dew formation. If there are
52
AQUALAB
any contaminants (e.g., fingerprints) on the mirror, the dew forms unevenly and can affect
the accuracy of the reading.
The instrument should be cleaned if visual inspection indicates the chamber is dirty or as
part of the verification process (Section4.1).
4.2.1 CLEANING KIT
The AQUALAB comes with an AQUALAB Cleaning Kit that contains enough cleaning supplies
to clean the instrument for about 1 year. The following supplies are included:
• Spatula (a thin plastic rod)
• Deionized water for cleaning
• Cleaning Solution
• KIMWIPES® tissues
• Activated charcoal for removing volatile compounds from the chamber between readings
NOTE: Wash hands with soap and water, and wear clean gloves before starting the cleaning procedure. This prevents
oils from contaminating the cleaning materials, the sample chamber, and the sensors.
4.2.2 AQUALAB 4TEV SPECIAL CONSIDERATIONS
When cleaning an AQUALAB 4TEV, do not to get cleaning solution on the capacitance sensor
filter (Figure73). Repeated exposure of cleaning materials or contaminants to the filter
may cause inaccurate readings. If the filter appears to be contaminated, it may need to
bereplaced.
To replace the capacitance sensor filter, use the following steps:
1. Use a tweezer or small knife blade to pry up the edge of the filter, being careful not to
disturb the sensor beneath.
2. Discard the soiled lter.
3. With clean and gloved hands, gently press a new lter into place.
4.2.3 CLEANING PROCEDURE
The procedure to clean AQUALAB involves washing, rinsing, and drying each area.
NOTE: Isopropyl alcohol can be substituted for the Cleaning Solution.
1. Turn the AQUALAB power OFF.
2. Open the chamber cover to expose the sample chamber and sensors.
3. Clean the sample chamber. The sample chamber consists of all surfaces inside the red
O-ring when the lid is closed.
NOTE: Be extremely careful not to damage the fan blades when cleaning the chamber.
a. Remove any debris that may have collected within or around the sample chamber.
53
SERVICE
b. Wrap a new tissue around the end of the spatula and moisten it with cleaning
solution.
NOTE: Do not dip used tissue into the cleaning solution as the cleaning solution will become contaminated.
c. Clean upper chamber, O-ring, and all surfaces of the sample block within the red
O-ring. Replace the tissue if it becomes too dirty during this process.
d. Clean lower block with a fresh KIMWIPES tissue. Clean the entire block surface.
e. Repeat steps b through d using a new tissue moistened with deionized water.
f. Repeat steps b through d using a new, dry KIMWIPES tissue to remove any moisture
remaining from the cleaning.
NOTE: Do not reuse tissues.
4. Clean the mirror.
a. Wrap a new KIMWIPES tissue around the end of the spatula and moisten it with
cleaning solution.
b. Gently swipe the moistened tissue across the mirror once. A single swipe is usually
sufficient to remove contaminants.
c. Repeat stepsa and b using a new tissue moistened with deionized water.
d. Repeat stepsa and b using a new, dry KIMWIPES tissue to remove any moisture
remaining from the cleaning.
e. Visually inspect the mirror for cleanliness. Clean again if necessary.
5. Clean the thermopile and optical sensor.
a. Wrap a new KIMWIPES tissue around the end of the spatula and moisten it with
cleaning solution.
b. Swipe the moistened tissue across thermopile and optical sensor. A single swipe
across the sensor is usually sufficient to remove contaminants.
c. Repeat stepsa and b using a new tissue moistened with deionized water.
d. Repeat stepsa and b using a new, dry KIMWIPES tissue to remove any moisture
remaining from the cleaning.
e. Visually inspect the thermopile and optical sensor for cleanliness. Clean again, if
necessary.
6. Visually inspect the sample chamber and sensors for contaminants, including moisture.
If necessary, repeat the cleaning process using new KIMWIPES tissues.
7. Let stand for 5 min to ensure the sample chamber is dry.
8. After cleaning the AQUALAB, check the instrument performance and correct for any
linear offset that may have occurred during the cleaning process.
a. Run a sample of the activated charcoal pellets from the AQUALAB Cleaning Kit.
54
AQUALAB
This cleans the air inside the chamber, helping it come back to a stable sampling
environment.
b. Verify the linear offset against known verification standards as described in
Section4.1.2.
c. If a linear offset has occurred, adjust for linear offset.
If the instrument is still not reading samples correctly, contact Customer Support.
4.3 MAINTENANCE PACKAGES
METER offers maintenance and calibration packages to ensure AQUALAB is functioning to its
highest standard (Table 6).
Table 6 Maintenace package options
PackagePreventative MaintenanceBasic Calibration Service
As-found inspection
Replace old/damaged parts
Instrument cleaning
Factory calibration
Extended 1-year warranty
Loaner instrument
AvailableAvailable
IncludedSeparate charge per part
IncludedIncluded
IncludedIncluded
IncludedNot included
AvailableAvailable
Replacement parts can also be ordered from METER. Contact Customer Support.
4.4 REPAIR
METER repairs manufacturer defects and instruments within the 1-year warranty at no
charge. Repairs outside of the warranty window are charged based on cost of parts, labor,
and shipping. An extra fee may be charged for rush work. Contact Customer Support for an
estimated repair cost.
METER has loaner instruments available for a fee while the AQUALAB is being serviced.
All AQUALAB units returning to METER for servicing must be accompanied with a Return
Merchandise Authorization (RMA) number. Prior to shipping the instrument, contact
Customer Support to obtain an RMA number.
The following steps will help to ensure the safe shipping and processing of the AQUALAB:
1. Ship the AQUALAB in its original cardboard box with suspension packaging. If this is not
possible, use a box with at least 4 in of space between the instrument and each wall of
the box.
2. Place the AQUALAB in a plastic bag to avoid disguring marks from the packaging.
55
SERVICE
3. Do not ship the power cord, serial cable, or any other accessories.
4. If the original packaging is not available, pack the box moderately tight with packing
material (e.g., StyrofoamTM peanuts or bubble wrap), ensuring the instrument is
suspended in the packing material.
5. On the RMA form, please verify the ship to and bill to information, contact name, and
problem description. If anything is incorrect, please contact Customer Support.
6. Tape the box in both directions for added support.
7. Include the RMA number in the attention line on the shipping label.
A Certificate of Calibration will be issued upon completion of the work.
4.5 TROUBLESHOOTING
Tab le 7 lists common problems and their solutions. If the problem is not listed or these
solutions do not solve the issue, contact Customer Support.
Table 7 Troubleshooting the AQUALAB
ProblemPossible Solutions
Ensure power cord is securely attached to the back of the
instrument and plugged into the power outlet.
A power surge may have caused a fuse to blow. To change the fuses:
• Unplug the power cord.
• Locate the panel where the power cord plugs in. The fuse box is
on the right side of that panel. Press the release tab and pull the
fuse-holder out.
AQUALAB does not turn on
• Pull the broken fuse out and replace with a 1.25-A, 250-V fuse.
CAUTION: Do not use any other kind of fuse to avoid risk of damaging the
instrument or voiding the warranty.
• Replace the fuse holder and push it into the fuse well until the
release tab snaps in place.
• Connect the power cord and turn the instrument on.
If the fuse blows again, a failed component may be causing the
problem. Contact Customer Support to make arrangements for
repairs.
56
AQUALAB
Table 6 Troubleshooting the AQUALAB (continued)
ProblemPossible Solutions
The sample chamber may be dirty. Refer to Section4.2 for
directions on cleaning the sample chamber.
The temperature difference between the sample and the block
chamber may be too great. Allow the sample to equilibrate to
instrument temperature. Refer to Section2.2.2.
Some products absorb or desorb moisture very slowly, causing
Readings are slow or
inconsistent
Water activity readings on
verification standards are
too high or too low and a
linear offset adjustment
cannot be made any higher
or lower
Remove sample. Sample is
too hot! error message
Displayed aw is below
instrument detection limits
Dew point sensor failure
error message
Crystal Failure. See
Manual for options.
error message
Verification is not correct
Contaminated mirror.
error message
measurements to take longer than usual, and nothing can be done
to speed up the process. Refer to Section2.2.1.
The sample may contain volatiles. Refer to Section2.2.1.3 for
suggestions on reducing difculties with measuring samples with
volatile compounds.
A fan blade in the block chamber may be broken or bent. If salt
standards take a long time to read and the sample chamber is
clean, a broken chamber fan blade is the probable cause. Contact
Customer Support for details on replacement.
The thermopile, which measures sample temperature, may have
become contaminated. Refer to Section4.2 for directions on
cleaning.
The chamber mirror may be dirty. Refer to Section4.2 for directions
on cleaning.
The sample temperature is too high for the instrument to
equilibrate within a reasonable amount of time. Ensure samples are
at the same temperature as the instrument (Section2.2.2).
The sample is too dry for the instrument to read accurately. If a
sample has a water activity that is less than the detection limits of
the instrument, this message appears. There is not enough sample
moisture to condense on the mirror and provide a reading.
The mirror may be dirty. Clean the mirror and chamber (Section4.2)
and measure the sample again.
The cooler is damaged and needs to be serviced by METER. Refer to
Section4.4 for detailed instructions.
The crystal that runs the rmware is having trouble starting. Cycle
the power. If this message continues to appear, the instrument
needs to be serviced by METER (Section4.4).
Clean the sample chamber and mirror. Refer to Section4.2 for
detailed cleaning instructions.
If verication is still not correct, verify and adjust for linear offset
(Section4.1.2).
Clean the chamber mirror (Section4.2) and run the sample again.
If this message continues to appear, contact Customer Support for
further options.
57
SERVICE
Table 6 Troubleshooting the AQUALAB (continued)
ProblemPossible Solutions
Firmware is corrupted. See
Manual for options.
error message
Ran test with wrong model
Moisture content displayed
is not correct
(AQUALAB DUO)
Moisture content does
not show up on the
Measurement tab
(AQUALAB DUO)
Message on the
Measurement tab displays
no moisture content reading
(AQUALAB DUO)
The rmware on the instrument is corrupted and needs to be
reloaded. To download new rmware to the AQUALAB 4 models, the
instrument must be serviced by METER (Section4.4).
On the measurement screen, toggle to the correct model using the
UP and DOWN button (Section2.5). The moisture content value
updates to correspond with the model selected. Use SAVE to save
the updated moisture value.
If the correct model is not available, the model may not be loaded
on the instrument.
To determine which models are loaded on the instrument, cycle to
the Conguration tab, select Moisture and the loaded models will
be listed.
If the correct model is not available, load the appropriate model
using AquaLink 4 software (Section2.5.2). The AQUALAB DUO can
hold a total of 100 models at any one time.
The model selected may not be correct for the product being tested.
Toggle through the available models to nd a more appropriate
model.
If the model is correct but not giving correct moisture content
values, it may be necessary to offset the model. See Section2.5.4
for detailed instructions.
If the model is correct and an offset does not work, it may be
necessary to generate a new model for the product or update an
existing model. For information about updating or generating a
model, contact Customer Support.
Moisture content has not been activated.
Toggle to the Conguration tab, select %Moisture, and select the
appropriate model.
If no models appear in the %Moisture screen, reload models using
AquaLink 4.
If %Moisture is not an active selection, the DUO feature may not be
active. Contact Customer Support to learn how to upgrade to a DUO.
When a moisture content reading is not shown, the water activity or
temperature for that reading is beyond the scope of the moisture
sorption isotherm. This can happen under the following two
conditions:
• The isotherm equation calculates a moisture content that is less
than 0% or greater than 100% with the given water activity.
• The control temperature is signicantly different than the iso-
therm temperature. Make sure that the sample water activity and
the instrument controlling temperature are within the scope of
the selected moisture sorption isotherm model.
58
AQUALAB
Table 6 Troubleshooting the AQUALAB (continued)
ProblemPossible Solutions
If, after cleaning the instrument and following troubleshooting
guidelines, there is still a measurement error, navigate to the
Diagnostics screen.
Sensors are reading outside
of the typical range
The lid, base, and sample temperatures should be between 24.5
and 25.5 °C. If the mirror temperature is at lid temperature, the
cooler has failed and must be replaced. If the mirror is below lid
temperature or appears to be random, the thermocouple wire is
broken and must be repaired.
A typical optical range is between 300 and 2,900 mV. If the sensor is
reading outside of this range, contact Customer Support.
4.6 CUSTOMER SUPPORT
Customer service representatives are available for questions, problems, or feedback
Monday through Friday, 7 am–5 pm Pacific time.
If contacting METER by email, please include the following information:
Name
Address
Phone
NOTE: For AQUALAB sensors purchased through a distributor, please contact the distributor directly forassistance.
Email address
Instrument serial number
Description of the problem
4.7 TERMS AND CONDITIONS
By using METER instruments and documentation, you agree to abide by the METER
Group, Inc. USA Terms and Conditions. Please refer to metergroup.com/terms-conditions
fordetails.
59
REFERENCE
REFERENCE
Labuza TP, Acott K, Tatini SR, Lee RY, Flink J, and McCall W. 1976. Water activity determination: A
collaborative study of different methods. J. Food Sci. 41:910–917.