Loaner Service .........................................74
14. Further Reading ....................... 75
Water Activity eory & Measurement ...75
Food Quality and Safety ..........................78
Water Activity and Microbiology .............80
Water Activity in Foods ...........................83
Appendix A .....................................93
Preparing Salt Solution ............................93
Appendix B .....................................95
Temperature Correction ..........................95
Appendix C .....................................96
AquaLab Calibration Standards ..............96
Declaration of Conformity ........... 101
Certificate of Traceability .............102
iii
iv
AquaLab
1. Introduction
1. In t r o d u c t I o n
Welcome to Decagon’s AquaLab Series 4TE, 4TEV, and DUO, the
industry standard for measuring water activity (aw). AquaLab is the
quickest, most accurate, and most reliable instrument available for
measuring water activity. Whether you are researching or working
on the production line, AquaLab will suit your needs. It is easy to
use and provides accurate and timely results.
About this Manual
Included in this manual are instructions for setting up your AquaLab,
verifying the calibration of the instrument, preparing samples, and
maintaining and caring for your instrument. Please read these instructions before operating AquaLab to ensure that the instrument
performs to its full potential.
Customer Support
If you ever need assistance with your AquaLab, or if you just have
questions or feedback, there are several ways to contact us:
NOTE: If you purchased your AquaLab through a distributor, please
contact them for assistance.
E-mail
support@decagon.com
Please include your name, contact information, instrument serial
number(s), and a description of your problem or question.
sales@decagon.com
Please include your name, address, phone number, the items you
wish to order and a purchase order number. Credit card numbers
should always be called in.
1
AquaLab
1. Introduction
Phone
1-800-755-2751 (USA and Canada Only)
1-509-332-2756 International
Our Customer Support and Sales Representatives are available
Monday thru Friday.
Fax
1-509-332-5158
Warranty
AquaLab has a 30-day satisfaction guarantee and a three-year warranty on parts and labor. Your warranty is automatically validated
upon receipt of the instrument. We will contact you within the first
90 days of your purchase to see how the AquaLab is working for
you.
Seller’s Liability
Seller warrants new equipment of its own manufacture against defective workmanship and materials for a period of three years from
date of receipt of equipment (the results of ordinary wear and tear,
neglect, misuse, accident and excessive deterioration due to corrosion from any cause are not to be considered a defect); but Seller’s
liability for defective parts shall in no event exceed the furnishing
of replacement parts Freight On Board the factory where originally
manufactured. Material and equipment covered hereby which is
not manufactured by Seller shall be covered only by the warranty
of its manufacturer. Seller shall not be liable to Buyer for loss, dam-
2
AquaLab
1. Introduction
age or injuries to persons (including death), or to property or things
of whatsoever kind (including, but not without limitation, loss of
anticipated profits), occasioned by or arising out of the installation,
operation, use, misuse, nonuse, repair, or replacement of said material and equipment, or out of the use of any method or process
for which the same may be employed. e use of this equipment
constitutes Buyer’s acceptance of the terms set forth in this warranty.
ere are no understandings, representations, or warranties of any
kind, express, implied, statutory or otherwise (including, but without limitation, the implied warranties of merchantability and fitness
for a particular purpose), not expressly set forth herein.
3
AquaLab
2. About AquaLab
2. About AquaLab
AquaLab is the fastest and most accurate instrument for measuring
water activity, giving readings in five minutes or less. Its readings
are reliable, providing ±0.003 aw accuracy. e instrument is easy
to clean and checking calibration is simple.
AquaLab Model and Options
Series 4TE: User-selectable internal temperature control model,
uses thermoelectric (Peltier) components to maintain internal temperature.
Series 4TEV: Uses both a chilled-mirror dewpoint sensor and a capacitance sensor for measuring non-volatile and volatile substances,
respectively. Either sensor is easily selected using the instrument’s
menu system.
Series 4TE DUO: Uses chilled-mirror dewpoint and programmed
models obtained from isotherm data to give the user both water activity and moisture content simultaneously in five minutes or less.
AquaLab 4 Instrument Specifications
Water Activity Range: 0.050 to 1.000 a
Water Activity Accuracy: ±0.003 (4TE Dew Point Mode)
Water Activity Accuracy: ±0.015 (4TEV Capacitance Mode)
Water Activity Resolution: 0.0001
Read Time1: ≤5 min.
Sample Temperature Range: 15 to 50° C
Sample Temperature Accuracy: ±0.2° C
4
w
AquaLab
2. About AquaLab
Sample Temperature Resolution: 0.01° C
Sample Dish Capacity: 15ml Full
Operating Environment: 5 to 50° C 20 to 80% Humidity
Case Dimensions: 26.7 x 17.8 x 12.7cm
Weight: 3.1 Kg
Case Material: Lustran 433 (ABS) with fire retardant
Display: 64 x 128 Graphical
Data Communications: RS232A Serial, 9600 to 115200 baud
Power: 110 to 220 VAC, 50/60Hz
Warranty: 3 year parts and labor
1
On samples with no significant impedance to vapor loss
AquaLab 4 DUO Specifications
Moisture Content Repeatability: 0.02%
Accuracy to Moisture Content Ref.: 0.1% to 0.5%
AquaLab and Water Activity
Water activity (aw) is a measurement of the energy status of the water
in a system. It indicates how tightly water is “bound”, structurally
or chemically, within a substance. Water activity is the relative humidity of air in equilibrium with a sample in a sealed measurement
chamber. e concept of water activity is of particular importance
in determining product quality and safety. Water activity influences
color, odor, flavor, texture and shelf-life of many products. It predicts safety and stability with respect to microbial growth, chemical
and biochemical reaction rates, and physical properties. For a more
detailed description of water activity as it pertains to products,
please refer to Chapter 3 of this manual, titled “ Water Activity
eory”.
5
AquaLab
2. About AquaLab
How AquaLab Works
AquaLab uses the chilled-mirror dewpoint technique to measure the
water activity of a sample. In an instrument that uses the dewpoint
technique, the sample is equilibrated with the head-space 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. In
the AquaLab, the mirror temperature is precisely controlled by a
thermoelectric (Peltier) cooler. Detection of the exact point at which
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. e photo detector senses the change
in reflectance when condensation occurs on the mirror. A thermocouple attached to the mirror then records the temperature at which
condensation occurs. AquaLab then signals you by beeping and displays the final water activity and temperature.
In addition to the technique described above, AquaLab uses an internal fan that circulates the air within the sample chamber to reduce
equilibrium time. Since both dewpoint and sample surface temperatures are simultaneously measured, the need for complete thermal
equilibrium is eliminated, which reduces measurement times to less
than five minutes.
AquaLab and Temperature
Samples not read at room temperature during the read cycle will
equilibrate with the AquaLab’s temperature before the water activity
is displayed. Large temperature differences will cause longer reading
times, since a complete and accurate reading will not be made until
the sample and the instrument are within 2°C of each other.
6
AquaLab
2. About AquaLab
ere are several advantages in having a temperature-controlled water activity meter. A few major reasons are:
1. Research purposes. Temperature control can be used 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. ere are
many shelf-life, packaging, and isotherm studies in which temperature control would be very beneficial.
2. To comply with government or internal regulations for specific
products. ough the water activity of most products varies by less
than ± 0.002 per °C, some regulations require measurement at a specific temperature. e most common specification is 25°C, though
20°C is sometimes indicated.
3. To minimize extreme ambient temperature fluctuations. If the
environmental and AquaLab temperatures fluctuate by as much as ±
5°C daily, water activity readings will vary by ± 0.01 aw. Temperature
control eliminates variations due to changes in ambient conditions.
Series 4TE/4TEV/4TE-DUO
e AquaLab Series 4TE models have thermoelectric components
installed to allow the instrument to maintain a set chamber temperature. e temperature is set using the configuration menu of any
of the Series 4 models.
7
AquaLab
2. About AquaLab
Chilled Mirror Dewpoint Limitations
AquaLab’s limitation is its ability to accurately measure samples with
high concentrations (typically >1%) of certain volatiles such as ethanol or propylene glycol, which can condense on the surface of the
chilled mirror. e extent of the effect is determined by how readily
the material volatilizes, which is both concentration- and matrixdependent. erefore, even if your sample contains materials that
could volatilize, it may still be possible to make accurate readings
using the chilled mirror dewpoint sensor.
AquaLab Series 4TEV which incorporates both a chilled mirror sensor and a capacitance sensor for measuring volatile substances is
Decagon’s solution for products containing volatile materials. If you
are unsure if you need the TEV model, please call and discuss your
product with a Decagon Representative. Refer to Chapter 8’s section
titled ”Volatile Samples” or call Decagon for more details.
8
AquaLab
3. Water Activity eory
3. Water Activity eory
Water is a major component of foods, pharmaceuticals, and cosmetics. Water influences the texture, appearance, taste and spoilage of these
products. ere are two basic types of water analysis: moisture content
and water activity.
Moisture Content
e meaning of the term moisture content is familiar to most people.
It implies a quantitative analysis to determine the total amount of
water present in a sample. Primary methods for determining moisture content are loss on drying and Karlf Fisher titration, but secondary methods such as infrared and NMR are also used. Moisture
content determination is essential in meeting product nutritional
labeling regulations, specifying recipes and monitoring processes.
However, moisture content alone is not a reliable indicator for predicting microbial responses and chemical reactions in materials.
e limitations of moisture content measurement are attributed to
differences in the intensity with which water associates with other
components.
Water Activity
Water activity is a measure of the energy status of the water in a
system, and thus is a far better indicator of perishability than water
content. Figure 1 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.
9
AquaLab
3. Water Activity eory
Fig. 1: Water Activity Diagram—adapted from Labuza
Water activity of a system is measured by equilibrating the liquid
phase water in the sample with the vapor phase water in the headspace and measuring the relative humidity of the head-space. In
the AquaLab, a sample is placed in a sample cup which is sealed
inside a sample chamber. Inside the sample chamber is a fan, a dew
point sensor, a temperature sensor, and an infrared thermometer.
e dewpoint sensor measures the dewpoint temperature of the air
in the chamber, and the infrared thermometer measures the sample
temperature. From these measurements, the relative humidity of
the head-space is computed as the ratio of dewpoint temperature
saturation vapor pressure to saturation vapor pressure at the sample
temperature. When the water activity of the sample and the relative humidity of the air are in equilibrium, the measurement of the
head-space humidity gives the water activity of the sample. e purpose of the fan is to speed equilibrium and to control the boundary
layer conductance of the dewpoint sensor.
10
AquaLab
3. Water Activity eory
In addition to equilibrium between the liquid phase water in the
sample 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 multi-component 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
remember the restriction of the definition of water activity to equilibrium.
Temperature Effects
Temperature plays a critical role in water activity determination.
Most critical is the measurement of the difference between sample
and dewpoint temperature. If this temperature difference were in error by 1°C, an error of up to 0.06 aw could result. In order for water
activity measurements to be accurate to 0.001, temperature difference measurements need to be accurate to 0.017°C. AquaLab’s infrared thermometer measures the difference in temperature between
the sample and the block. It is carefully calibrated to minimize temperature errors, but achieving 0.017°C accuracy is difficult when
temperature differences are large. Best accuracy is therefore obtained
when the sample is near 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 only
slightly warmer than the sensor block will condense water within the
block. is will cause errors in the measurement, and in subsequent
measurements until the condensation disappears. A sample at 0.75 aw
needs to be approximately 4°C above the chamber temperature to
11
AquaLab
3. Water Activity eory
cause condensation. e AquaLab warns the user if a sample 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 that is warmer than the block is put in the AquaLab.
Water Potential
Some additional information may be useful for understanding what
water activity is and why it is such a useful measure of moisture
status in products. 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 () is the same in both phases. It
is this fact that allows us to measure the water potential of the vapor
phase and use that to determine the water potential of the liquid
phase. Gradients in (µ) are driving forces for moisture movement.
us, in an isothermal system, water tends to move from regions of
high water potential (high aw) to regions of low water potential (low
aw). Water content is not a driving force for water movement, and
therefore can not be used to predict the direction of water movement, except in homogeneous materials.
Factors In Determining Water Potential
e water potential of the water in a system is influenced by factors
that effect the binding of water. ey include osmotic, matric, and
pressure effects. Typically water activity is measured at atmospheric
pressure, so only the osmotic and matric effects are important.
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
12
AquaLab
3. Water Activity eory
separated from pure water by a semi-permeable 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 one mole of an
ideal solute to a kilogram of water produces an osmotic pressure of
22.4 atm. is lowers the water activity of the solution from 1.0 to
0.98 aw. For a given amount of solute, increasing the water 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 semi-permeable membranes,
the osmotic effect on the free energy of the water is important for
determining microbial water relations and therefore their activity.
Matric Effects
e 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. is
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. e reduction in energy is the result of direct physical
binding of water to the cellulose or protein matrix by hydrogen bonding
and van der Waal forces. At higher water activity levels, capillary forces
and surface tension can also play a role.
Sorption Isotherms
Relating Water Activity to Water Content
Changes in water content affect both the osmotic and matric binding of water in a product. us a relationship exists between the
water activity and water content of a product. is relationship is
13
AquaLab
3. Water Activity eory
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. ese factors need to be kept in mind if one tries to use water content to infer
the stability or safety of a product. Typically, large safety margins are
built into water content specifications to allow for these uncertainties.
While the sorption isotherm is often used to infer water activity from
water content, one could easily go the other direction and use the
water activity to infer the water content. is is particularly attractive because water activity is much more quickly measured than water content. is method gives particularly good precision in the
center of the isotherm. In order to infer water content from water
activity, one needs an isotherm for the particular product. Decagon
sells an Isotherm Generator called the AquaSorp IG or you can also
have Decagon run the isotherm for a fee.
For example, if one were using the AquaLab to monitor the water
content of dried potato flakes, one would measure the water activity
and water content of potato flakes dried to varying degrees using the
standard drying process for those flakes. An isotherm would be constructed using those data, and the water content would be inferred
using the measured water activity of samples and that isotherm. We
have an upgrade available to Series 4TE users that would allow you
to determine moisture content and water activity simultaneously.
is instrument is called the Series 4TE DUO.
e importance of the concept of water activity of foods, pharmaceuticals, and cosmetics cannot be over emphasized. Water activity is
a measure of the energy status of the water in a system. More importantly, the usefulness of water activity in relation to microbial growth,
chemical reactivity, and stability over water content has been shown.
14
AquaLab
4. Getting Started
4. Getting Started
Components of your AquaLab
Your AquaLab should have been shipped with the following items:
AquaLab water activity meter•
Calibration Certificate•
Power cord•
RS-232 interface cable•
100 disposable sample cups•
Operator’s Manual•
Quick Start guide•
Cleaning Kit•
3 vials each of the following verification solutions:•
1.000 a
0.760 a
0.500 aw 8.57 molal LiCl
0.250 aw 13.41 molal LiCl
Distilled Water
w
6.0 molal NaCl
w
Choosing a Location
To ensure that your AquaLab operates correctly and consistently,
place it on a level surface. is reduces the chance that sample material will spill and contaminate the sample chamber. Also select a
location where the temperature remains fairly stable to avoid temperature changes that can affect accuracy. is location should be
well away from air conditioner and heater vents, open windows, etc.
Place the AquaLab in a location where cleanliness can be maintained
to prevent contamination of the sample chamber.
15
AquaLab
4. Getting Started
Preparing AquaLab for Operation
After finding a good location for your AquaLab, plug the power cord
into the back of the unit. e ON/OFF switch is located on the
lower left corner of the AquaLab’s back panel. When the AquaLab
is turned on, you should see a model name/number screen and then
the main screen as shown below.
e main screen shows the water activity (aw) in the middle of the
screen and the sample temperature right below. On the Series 4TEV
model you will also see either DEW or CAP indicating whether you
are using the dewpoint or capacitance sensor respectively.
NOTE: In order to provide the most accurate readings, your AquaLab
should be allowed a 15 minute warm-up period.
16
AquaLab
4. Getting Started
If users have been setup on the instrument, the following screen will
appear instead of the main screen. (See Chapter 5 for more information on administrative settings and user setup).
Select the appropriate user and login to begin.
17
AquaLab
5. Menus
5. Menus
At the top of the display screen there are three tabs: Measurement,
Configuration, and Data. ese tabs indicate the three menus you
can access. To change between the tabs press the right most button
below the document icon.
e enter icon is the read or enter button. Once the latch is set to the
read position, the document icon will switch to an “X” icon, which
allows the user to stop the current reading. During a reading, pressing enter again will restart the reading.
Measurement Tab
e measurement tab, as seen above, is the main screen which displays each time you turn on your AquaLab. If this screen doesn’t
appear, refer to Chapter 12 for troubleshooting instructions. As
mentioned earlier, the water activity and sample temperature are
displayed on the screen.
18
AquaLab
5. Menus
Pushing the right or left arrow keys will change the display to a
temperature equilibration screen shown below. is screen shows the
temperature difference between the sample temperature and the block
temperature.
Configuration Tab
When at the configuration screen, pressing the up and down arrow
keys moves the cursor through the various configuration options
Press the left and right arrows to page through the options. e
enter button will allow you to change the highlighted setting.
19
AquaLab
5. Menus
Calibration:
Pressing the Enter button when Calibration is highlighted starts the
verification process. For more details on the verification procedure
refer to Chapter 7. You may also reset the calibration to the factory defaults by highlighting the Defaults option and pressing Enter.
is will reset all options to the way they were when the instrument
arrived at your location.
Temperature:
e default temperature is 25°C. Press the enter button to change
the temperature setting. e AquaLab Series 4TE models may be set
between 15 and 50°C by 0.1°C intervals. Using the up and down
arrows, set the AquaLab to your desired temperature and press the
save button.
20
AquaLab
5. Menus
Temp Eq:
e Temperature Equilibration option allows you to set the level of
temperature equilibration desired before the water activity measurement begins. e range is 0.5 to 4.0°C. A setting of 4.0°C begins
the measurement immediately (assuming the sample is not >4.0°C
above or below the block temperature). A setting of 0.5 °C will
cause the instrument to wait until the sample temperature is within
<0.5°C of the block temperature before starting the water activity
measurement.
Sensor:
In the AquaLab Series 4TEV model only, this option indicates the
selected sensor type, either dewpoint or capacitance (e Series 4TE
models will always be Dewpoint). Pressing Enter when the Sensor
option is highlighted allows you to change between a chilled mirror
dewpoint or capacitance sensor for sampling with or without volatiles, respectively.
21
AquaLab
5. Menus
Mode:
Users may choose between single, continuous, or custom mode by
pushing the save button.
Single Mode
Single mode reads the sample once, after which the instrument notifies you that it is finished and the water activity and temperature are
displayed on the screen.
Continuous Mode
Continuous mode reads your sample until you open the chamber
lid or stop the test using the stop button. AquaLab reads the sample,
displays the water activity and temperature, then begins another read
cycle without further input from the user. Between samples, the machine will signal you with beeps. is mode eliminates the possibility
of moisture exchange with the environment outside the chamber in
between readings. A time on the bottom left of the screen tracks the
cumulative read time. All readings taken during continuous mode
are saved on the instrument’s memory if the autosave feature is selected (see Auto Save below). If AquaLab is connected to a computer
using AquaLink RG (See Chapter 11), all readings taken during continuous mode will be downloaded to the AquaLink RG software.
Custom Mode
Custom mode allows a sample to be read multiple times until
a desired level of stability is achieved. e user determines how
many consecutive tests they want to be within a given water activity stability setting. For instance, the customer can choose to
have 4 consecutive tests be within +/- 0.001aw. e instrument
will continue to run tests until it records 4 tests that are within +/-
0.001aw and then will stop and report the value of the final test. If
autosave is turned on, all test readings will be saved to the instruments memory, but only the final reading will appear on the main
22
AquaLab
5. Menus
measurement screen. If AquaLab is connected to a computer using
AquaLink RG (See Chapter 11), all readings taken during a custom mode test will be downloaded to the AquaLink RG software.
On the mode screen, at the top of the page, will appear the current
mode settings with the number of tests appearing first, followed by the
stability value (∆aw). Pressing enter with the custom mode highlighted will allow the number of tests and stability settings to be changed.
To change the number of readings, use the right/left arrow buttons to highlight the number under Readings, and then use the
up and down buttons to change to any value between 2 and 9.
To change the stability setting, use the right/left arrow buttons to
23
AquaLab
5. Menus
highlight the number under ∆aw, and then use the up and down buttons to change to any value between 0.0005 and 0.0030. To save the
settings and finish, press the save button (to exit without updating,
press the cancel button). e mode screen will now appear with the
updated custom settings appearing at the top of the screen. Press the
save button to return to the configuration screen and begin using the
custom mode (To exit without updating, press the cancel button).
Date:
AquaLab Series 4 models now have an internal calendar and clock.
e time and date are recorded with each water activity reading.
Pressing Enter when the Date option is highlighted allows you to set
the date in the instrument. Press the left and right arrows to change
between the month, day and year. Press the up or down arrows to
change any of the individual values.
Time:
Pressing Enter when the Time option is highlighted allows you to
set the current local time. Press the up or down arrows to change
any of the individual values. Press the left or right buttons to change
between hour and minutes. e hour setting automatically changes
between AM and PM.
24
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