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DMA-80
Operator Manual
MA122
Milestone DMA-80 Operator Manual – Revision 01/2010
We are sure that you will be completely satisfied with the performance of this new unit entering your laboratory.
We invite you to read carefully this user manual and to keep it in reach for convenient and fast consulting.
For any possible clarification or any request for assistance please contact either Milestone Srl at the following
address:
Milestone Srl
Via Fatebenefratelli, 1/5
I-24010 Sorisole (BG) Italy
Tel +39 035 573857
Fax +39 035 575498
Website www.milestonesci.com
Email analytical@milestonesrl.com
Caution!
Please read the operator manual before using the instrument!
DMA-80 INDEX 1
Milestone DMA-80 Operator Manual – Revision 01/2010
INDEX
______________________________________________________________________________________________
1 DMA-80 INSTALLATION Page 4
1.1 Unpacking and checking list Page 4
1.2 Options Page 9
1.3 DMA80 Setup Page 11
1.3.1 DMA80 with Terminal 1640/640 Setup Page 11
1.3.2 DMA80 with PC Setup Page 13
2 DMA-80 GENERAL DESCRIPTION Page 19
2.1 Technical data Page 19
2.2 Front view Page 21
2.3 Back side view Page 21
2.4 Inside view Page 22
3 TERMINAL 640/1640 and PC Page 24
3.1 Description Page 23
3.2 Installation Page 23
3.2.1 DMA-80 Page 23
3.2.2 Terminal connections Page 23
3.2.3 Terminal front panel connections Page 23
3.2.4 Terminal back panel connections Page 24
3.2.5 Connection of Terminal to DMA-80 Page 25
3.2.6 First Start Page 25
3.2.7 Printer and memory card Page 26
3.3 General Operation Page 27
3.3.1 Program Start/Login Page 27
3.3.2 Electronic Signature Page 28
3.3.3 End program/Logout Page 29
3.3.4 Desktop Page 29
3.3.5 Control sections Page 29
3.3.6 Operating program: DMA measurements Page 30
3.3.7 Generally used symbols Page 31
3.3.8 Numerical input via screen Page 32
3.3.9 Text input via screen Page 32
3.3.10 Print Page 33
3.4 Methods Page 34
3.4.1 Create new method Page 34
3.4.2 Open/Save/Delete Methods Page 35
3.4.3 Method Print-out Page 35
3.4.4 Method Parameters Page 36
3.5 Calibration Page 39
3.5.1 Create new calibration file Page 39
3.5.2 Open/Save/Delete Calibration file Page 39
3.5.3 Print Calibration file Page 40
3.5.4 Cuvette0/Cuvette1/Cuvette 2 Page 40
3.5.5 Description of Calibration file Page 41
3.6 Measurement Page 43
3.6.1 Tables Page 45
3.6.2 Reference measurements for high quality assurance Page 46
3.6.3 Blind value Page 47
3.6.4 Sample Page 49
3.6.5 Links Page 53
3.6.6 Signal Page 54
3.6.7 Results Page 55
3.7 System Page 57
3.8 Sample measurement Page 59
DMA-80 INDEX
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Milestone DMA-80 Operator Manual – Revision 01/2010
DMA-80 INDEX
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Milestone DMA-80 Operator Manual – Revision 01/2010
1 DMA-80 INSTALLATION
Provide a bench of at least 150 cm length and 70 cm wide and place the DMA-80 on the bench. The unit
requires sufficient clearance (approx. 15 cm) on all sides to allow adequate movement of air.
( WARNING
The weight of the DMA-80 is approximately 56 kg; at least 2 people are needed to remove
the unit from its box and place it on the bench.
1 DMA-80 INSTALLATION 4
Milestone DMA-80 Operator Manual – Revision 01/2010
1 DMA-80 INSTALLATION 5
Milestone DMA-80 Operator Manual – Revision 01/2010
1 DMA-80 INSTALLATION 6
Milestone DMA-80 Operator Manual – Revision 01/2010
1 DMA-80 INSTALLATION 7
Milestone DMA-80 Operator Manual – Revision 01/2010
1 DMA-80 INSTALLATION 8
Milestone DMA-80 Operator Manual – Revision 01/2010
1.2 OPTIONS
1 DMA-80 INSTALLATION 9
Milestone DMA-80 Operator Manual – Revision 01/2010
1 DMA-80 INSTALLATION 10
Milestone DMA-80 Operator Manual – Revision 01/2010
Connect the keyboard and the mouse to the back panel of the
Terminal (supplied only with Terminal 1640).
DMA-80 INSTALLATION 1 11
Milestone DMA-80 Operator Manual – Revision 01/2010
Introduce the memory flash card into the reader port located.
DMA-80 INSTALLATION 1 12
Milestone DMA-80 Operator Manual – Revision 01/2010
Plug the other end of the serial cable into the RJ45 interface
port of the Gateway.
DMA-80 INSTALLATION 1 13
Milestone DMA-80 Operator Manual – Revision 01/2010
Plug the end of USB cable (A) into the PC USB port.
DMA-80 INSTALLATION 1 14
Milestone DMA-80 Operator Manual – Revision 01/2010
DMA-80 INSTALLATION 1 15
Milestone DMA-80 Operator Manual – Revision 01/2010
Check that the main power switch of the unit is OFF; only
after that, connect both power cords to the electrical outlets.
Switch on the DMA-80. The main switch is located on the
front panel of the unit and PC (only for PC version).
DMA-80 INSTALLATION 1 16
Milestone DMA-80 Operator Manual – Revision 01/2010
Depending on the Windows version: if you have to enter the listing of the
drivers files, go through the CD to the (CD-Drive):/CDM 2.04.06 WHQL
Certified.
5 Digit the serial number and the valid licence key. These
data are printed on the Gateway. Confirm with OK.
DMA-80 INSTALLATION 1 17
Milestone DMA-80 Operator Manual – Revision 01/2010
User: 123
Administrator: 123456
Service: contact directly our service@milestonesrl.com
Next picture shows the DMA-80 software.
DMA-80 INSTALLATION 1 18
Milestone DMA-80 Operator Manual – Revision 01/2010
Operating principle
Atomic absorption thermal decomposition.
Light source
Low pressure mercury lamp.
Wavelength
253.65 nm.
Detectors
UV enhanced photodiodes.
Instrument controller
Terminal 640
• Touch-screen industrial grade controller 6.5” screen with 65.000 colors; VGA resolution 640x480 for sharp
process graphic.
• 1 USB port for printer, 2 PS2 ports for mouse and keyboard, 3 RS 232 ports for external devices.
• Methods and runs saved on PC-compatible flash-card or USB pen-drive.
Terminal 1640
• Touch-screen industrial grade controller 12” screen with 65000 colors; VGA resolution 800x600 for sharp
process graphic.
• 1 USB port for printer, 2 PS2 ports for mouse and keyboard, 3 RS 232 ports for external devices.
• Methods and runs saved on PC-compatible flash-card or USB pen-drive.
Personal Computer (minimum requirements)
• CPU Pentium III 800.
• RAM 256 MB.
• 20 MB free space on hard disk.
• 1 USB port, 1 CD-ROM reader, operating system Windows 7, XP or Vista.
Instrument software
Milestone easyCONTROL®
• LIMS compatible.
• compliant to FDA regulations 21 CFR Part 11.
Detection limit
for solids, liquids and gas
0.005 ng (dual-cell).
0.0015 ng (tri-cell).
Typical precision
Less than 1.5%.
Working ranges
Sample treatment
User-adjustable ‘on-the-fly’ in time and temperature.
Calibration
Standard solution of certified reference materials.
Type of sample
Solids, liquids and gas.
Auto-sampler
40-place, with dual-tray option for continuous operation.
Sample boat
Metal or Quartz.
Sample weighing
External analytical balance with automatic weight transfer.
Carrier
Oxigen or Milestone Air Compressor
Power
110-230V/50-60Hz.
Dimensions
Unit: 80 x 42 x 30 (H) cm.
Gas module: 12.5 x 6.5 x 16 (H) cm.
Vacuum pump: 28 x 40 x 17 cm.
Weight
Unit: 56 kg.
Gas module: 0.5 kg; vacuum pump: 15 kg.
3
1
11
On the right side of the DMA-80 the exhaust outlet
(11).
2
DMA-80 Ducon Cuvette
5
DMA-80 Tricell Cuvette (option)
Catalyst oven.
Heating coils
The picture shows how the amalgamator and
the catalyst are connected inside the catalyst
oven module. Notice where the heating coils are
located: 1) covers the amalgamator, 2) is around
the catalyst tube, and 3) covers the end of the
catalyst tube. Oxygen Flow
1 2 3
The screen, i.e. the positioning of the Buttons can be different from the screenshots
represented in this manual, depending on the terminal that has been adopted.
3.2 INSTALLATION
3.2.1 DMA-80
The DMA-80’s Software is already installed in the supplied Terminal. For DMA-80 with PC software (see
chapter 1.2). Software’s updates are carried out by Customer Service.
Be careful that the plug (DMA-80 as well as the terminal) must be unlocked when pulling out,
which means that the “nose” of the plug must be pressed when pulled out.
CONNECTION
D Serial Interfaces.
■ Connection for additional device (Balance) (e.g. COM1)
(See also Configuration)
Used cable: at terminal side RJ45 plug
PIN SIGNAL
2 RxT (In)
5 GND
6 TxD (Out)
Pin 1 is placed on the right side of the terminal.
CONNECTION
I J K L
CONNECTION
J Mains connection
K Flow controller
L O2-connection
Voltage supply to the terminal is switched on and off simultaneously with the DMA.
1 Switch off the DMA-80 unit (place on OFF the ON/OFF switch placed on the front of the unit).
The following Start routine is described in detail in the operating instructions. This
is only a short description.
3 Open the oxygen supply. Incoming pressure of DMA-80 must be 400 kPa (4 bar).
4 Switch on the main switch of the DMA-80 placed on the front panel.
TERMINAL and DMA-80-Software are automatically initialized.
6 Log in with your password.
Starting the software will simultaneously initialize the DMA-80 unit, i.e. all functions are in Standby
operating mode.
⇒ The auto sampler tray is initialized and driven to starting position.
⇒ All heaters are brought to starting temperature.
The Start-Switch in the Software is only active when all heating systems are at operating
temperature. Pre-heating time is approx. 15 to 20 minutes.
We recommend to use PCL3 enhanced (Printer Command Language) printer from HP. The
Software has an “Economy Modus”, for ink saving.
Successfully tested HP-Printer: HP1100, HP1280, HP5150, HP5160, HPD5360, HP5440, HP5650,
HP5652, HP5740, HP5940, HP6160, HP6540, HP6940, HP6980, HPD7160.
Printers are not supplied by Milestone, but must be purchased from a local supplier.
If you can not find locally a supplier , Easydoc software (enclosed in each DMA-80)
can be used to transfer data from terminal to your PC and then print out the report
with your own printer. For more information, see chapter 5.
EEPROM
Internal storage area (32 kB): Data are kept also during interruption of power supply. EEPROM is
reserved for System Protocol and settings.
How to insert Flash Card: The drive for the Flash Card is
located on the back of the Terminal.
Insert the Flash Card with the label in front of you. The
Flash Card must be introduced completely. The cart rises up
from the terminal at the same height of the black ejection
lever.
How to remove Flash Card: Press down the black lever
to release the card and then take it out.
The Flash Card may not be removed during writing of reading, otherwise the formatting
could be damaged and the files lost. Writing and reading are indicated on the screen with a
sand clock.
1 Insert your Flash Card. The user defined on the card will be recognized and requested to
identify.
For all DMA-80 configurations
2 Select your user name on the Login window. Type your user id and confirm with OK. Use the
Touch Screen or mouse; the keyboard is not active at this point.
Login
With the shipment of the unit the following passwords are assigned:
The passwords can be changed in the Administrator Panel.
The electronic signature only on Flash Card (Terminal 640/1640)
f a file is stored in the Measurement Menu, the signature button will appear
(Flash-Card and password must be set in the User Panel) and the file can be
provided with an electronic signature.
1 Press the signature button to sign your file.
After selection of the button you will be requested to enter the kind of
signature.
2 Enter the kind of signature, e.g. for control or release.
3 Press the Ok button and the Login dialogue window will appear Select
your User Name and User Id.
4 Confirm with Ok.
Your document is now provided with User Name, Date/Time and type.
This signature appears also on top of all results print-outs.
3.3.3 END PROGRAM AND LOGOUT
3.3.4 DESKTOP
After Login the start page of the DMA-80 is opened. Gently touch the surfaces to enter the control
program or the software administration panel.
Start-Desktop
BALANCE SET-UP
Here are the communication settings for the balance. These must be
adjusted only when switching over to a new type of balance.
HISTORY TRAIL
All changes in the system are automatically documented, e.g. login,
logout, etc.
GENERAL ADMINISTRATION
This area is dedicated to the basic adjustments/settings and to the user
administration. The basic settings to a major extent are reserved to
Service.
LOGOUT
With Logout you go out of the system. The Login window appears where
the next user can log in with his own password.
DMA-80 MEASUREMENTS
Control of DMA-80.
The actual control program is opened. This is divided into four main
registers that are extensively described in the following chapters.
Software is operated via Touch-Screen. Touching the screen or clicking with mouse the different
switching surfaces or input fields are activated.
Activated input fields are ready for entering data from a keyboard. Double-clicking on the activated
fields will open on the screen a numerical or standard keyboard.
Some symbols are present in each menu (or are generally used). They are described in the
following chapter.
Symbols that are used only in certain menus are described in the respective chapters.
OPEN FILE
Open file button.
SAVE FILE
Save file button. Name must be assigned to the file to be saved.
PRINT FILE
Print file button to print out reports.
GO BACK
The operating program is quitted and will go back to the start screen.
Save any changes before quitting.
BREAK
Input is terminated without saving and the input window is quitted.
DELETE
File is deleted.
START
To start a measuring run. If there is a sand clock on, this means that a
current procedure must first be accomplished (e.g. heating of furnace and
cuvette).
STOP
The current measurement is interrupted and the sample boats are taken
back to the auto sampler tray. The Stop-Button must then be re-set
touching the red-green Stop-Button.
At different steps of the program it is necessary to enter numeric values. Touching twice on the field
or number to be changed, a numeric keyboard appears.
Numeric keyboard
At steps where a designation is needed, touching twice on the touch-screen a standard keyboard
will appear.
Standard keyboard
3.3.10 PRINT
Printer
Touch the icon to pen a preview. Touch again to print out diagrams and/or
data.
Different printing options are available depending from which menu the print is made.
Additional copies of Sample Table (can also be printed from the “Sample”
register).
3.4 METHODS
Methods
NEW METHOD
To create a new method, open an empty method file. The current method will
be deleted from the main memory. Therefore save it before opening a new
method.
OPEN METHODS
To open one of the methods saved on the Flash Card (Terminal 640/1640) or
on PC.
SAVE METHODS
A method can be saved and recalled at any time.
Designate a Name. The ending .m80 will be automatically added.
Touch the Save icon to save the current method and to close the window.
DMA-80 with Terminal: always save methods under A:\Methods
DMA-80 with PC: always save methods under
C:\Documents\DMA80\Methods
DELETE METHODS
Select from the list the methods to cancel. The name will appear in the
Name field.
DMA-80 with Terminal: Touch the icon and – after a request to confirm –
the method will be deleted. A deleted method is definitely cancelled.
DMA-80 with PC: C:\Documents\DMA80\methods , select the method and
delete.
PRINT-OUT METHODS
The diagram can be printed before measurement is started under
Measurement ⇒ Signal .
The sample decomposition takes place at high temperatures (>600°C), to release Hg from the
sample. To prevent sample losses and spraying around of liquids, these should be dried before
decomposition.
For samples with high water content it is recommended to start a first drying Step of 200°C.
Samples containing liquids with boiling point under 100°C require an accordingly lower temperature.
Directly after drying the sample is decomposed at high temperature (burned in the oxygen flow).
A temperature of 650°C worked satisfactorily as decomposition temperature. This high temperature
ensures a complete decomposition and release of mercury. Only at a sufficiently high temperature
the entire Hg is set free and can be measured.
Example Method for wet sample:
Pos t T
1 00:00:30 200
Drying
2 00:03:00 200
3 00:01:00 650
Decomposition
4 00:02:00 650
Max. Start-T
Purge time
Recording Time
Unit of Sample
• Solid samples: g
• Liquid samples: ml
• Gas sample: cm3, dm3 or m3
Diagram Input
When making a new entry in position 1 the first value to be specified is the Time (pull to the
right), then Temperature T (pull upward) can be specified.
Graphic Input
3.5 CALIBRATION
This register administers calibration data. Different calibration files can be opened, created and saved.
Calibration
DMA-80 with Terminal: Touch the icon and – after a request to confirm –
the calibration will be deleted. A deleted method is definitely cancelled.
DMA-80 with PC: C:\Documents\DMA80\Calibration , select the calibration
and delete.
DMA-80: The first and long one is used for measuring low Hg content (up to approx. 20 ng), the
second and short one for measuring high Hg content (up to approx. 1200 ng).
Tricell DMA-80: The first and long one is used for measuring low Hg content (up to approx. 10 ng),
the second medium one (10-20ng), the third and short one for measuring high Hg content (up to
approx. 1200 ng).
Both cuvettes are always used for measurement. If the maximum peek of the first signal is over
0,8 A (standard setting), the maximum of the second signal will be used to calculate the result.
The column ∆E or ∆Hg shows the value by which the measured value deviates from the calibration
curve. Depending on the system setting the error is indicated is unit [ng], Extinction or in %.
The R² is calculated from the deviations of the measured values that have been
3 DMA-80 SOFTWARE 640/1640 and PC 42
Milestone DMA-80 Operator Manual – Revision 1/2010
calculated. The closer to 1 is the value, the better the calibration curve is adapted to
the measured values.
ENTER REMARKS
Click on any value of the table to open the columns for remarks and date. Clicking on the diagram
the fields will close again.
ULTRATRACE RANGE
For cuvette 0 only.
The calibration curve can be adapted to measuring for ultratrace analysis. To the highest
measured value an additional 40% (settable in the system administration) of the highest value is
added. No more values are calculated over this measuring value.
Highest value
CALIBRATION METHODS
It is possible to determine the type of calibration curve. If „undefined“ is
selected, then only the measured points will be shown and not curve.
ε 0 , ε1 , ε 2 Correction factors
Depending on how the calibration points are distributed, the program requires more than the
minimum measuring points necessary for calculation.
3.6 MEASUREMENT
MEASUREMENT
This Menu is divided into four registers.
In the Sample, Links and Signal registers, the designations of the
sample table columns are partly repeated.
Number of measurements
The average final result with the relative standard deviation is shown in the headline of the
multiple measurements. Individual values can be disabled removing the sigma sign.
Average of measurements
Std deviation
3.6.1 TABLES
Pos / Position
If Simple sample processing is activated, and a sample is added, the number over the selected
record will be taken, alternatively the sample can be selected (from pos. 1 to 40), as in this
operating mode each sample can be measured individually.
The measurement of each sample is started manually. After measurement, the next position of the
sample plate, if available, is driven into load position.
If Automatic Sample Processing is activated, and a sample is added, the upper number increases,
i.e. the next not occupied number is used, since in this mode the samples are automatically
successively processed. Each position may be occupied only once.
In a file samples can be processed both in automatic and simple mode.
Liquid samples should be measured in Simple mode, as mercury can evaporate if the sample
remains for long time in the sample boats.
Sample name
The Name is taken over from the selected record and can be changed/modified.
Status
Weight
A weight must always be entered, see also the chapter Enter weight.
Remarks/Comments
The reference measurements however are now fully documented and plotted (graphically) under
Calibration / Reference.
The table of the reference measurements includes: date, Hg in ng, Cal-Factor, used calibration and
remarks.
Average (m) of the reference values with the blue sigma sign.
It is a fast heating program of Furnace 1 and amalgamator, this in order to remove all deposit of
mercury / dust into the unit.
Is possible to define a blind value program, into the Panel administration>Settings>Limits.
In this page it is possible to set: Maximum heating temperature, Maximum heating time and Purge
time of Blind value method.
Here an example of Blind value:
3.6.4 SAMPLE
Add data
Add data
A new line is added to the table. The sample name in the „Name“ column is
taken over by the marked data record. If the name has a number as the
last figure, this will be increased automatically by 1.
Enter weight
If balance is connected, whenever a record is added, the balance screen will automatically
open to allow entering the sample weight.
With all data records a weight must always be entered, since otherwise the measurement
cannot be started.
The sample weight is indicated in gram, milligram or micro gram according to setting (see
chapter Balance Settings).
The sample weight is entered either manually over the keyboard/Touch screen, or taken
directly from an electronic balance through the interface cable.
Downloading of weight
Precisa balances: The weight is constantly updated on the terminal. In the
sample table touch the Weight icon to download the value into the active
cell.
Other balances: touching the print button of the balance (see appropriate
manual of the balance) the weight is transferred on the terminal and into
the active cell.
AUTOMATIC TARING
Touch the T to tare the Precisa balance.
STOP
The balance screen is closed without loading the weight.
DELETE SAMPLE
Select from a list the sample to be deleted.
Touching the Delete icon the selected sample will be deleted after a safety
inquiry. A deleted sample is deleted irrevocably.
SIMPLE MODE
Each sample is measured individually. Each measurement has to be
manually started.
1 Click on the sample to measure and start the measurement.
After measurement the rotating plate is turned to loading position of the
next sample. However it is possible to click on and measure any sample.
AUTOMATIC MODE
Samples are automatically measured in sequence one after the other. After
measurement the rotating plate turns to loading position of the next
sample, and the next measurement starts automatically.
Example
1 Weigh all samples in sequence.
2 Mark the record which contains a sub-sample (test1).
3 Activate the Button. The sample under the one marked will be connected with a brace-
parenthesis to the marked sample (test2).
4 Now select the connected sample (test2) and activate the Concentrate Button. The next sample
(test3) will also be connected to the first two samples.
You can add as many samples as desired. All sub-samples linked with a brace-parenthesis will
be considered.
In a file several sub-samples can be combined to several samples. (See example : Sample 1
includes 3 sub-samples, Sample 2 consists of 2 sub-samples)
Load file
3.6.5 LINKS
Screenshot of Links
In this Register you can select the calibration file (Cal-Date) and Methods to be used for the
process.
3.6.6 SIGNAL
Peek Cell 0
Peek Cell 1
Peek Cell 2
Signal
TOTAL TIME
After Start the Total Time and the Sample Time will be
displayed. Total time - in case of automatic measurement of
several samples - is the total time of all samples.
Sample Time indicates the run-off time of the total
measurement.
With the reduction icon the diagram will return to maximum extinction = 1.
Catalyst Furnace
Temperature (°C)
Amalgamator
Temperature (°C)
Absorbance
Cuvette
Temperature (°C)
Temperature Gradients
3.6.7 RESULTS
Screenshot of Results
Height
It's the maximum height of the evaluated peak.
Extinction = lg (100 % Transmission / X % Transmission)
Hg [ng]
Absolute quanty of Hg in the sample (calculated from active calibration)
c[µg/kg] or c[mg/kg]
Concentration of Hg in the sample (calculated from active calibration and sample weight).
CalFactor
The result is multiplied by the calibration factor (Standard value 1.00). With a
eference measurement, the calibration factor can be adapted to a slightly modified
sensitivity of the system. Thus a calibration can be further used.
Σ
Clicking twice in this field, the sample will be included in the statistics
calculations. The Sigma icon can be removed at any time by clicking
again.
Group
Samples can be ordered into different groups, up to 8 groups can be
provided.
1 Click on the small arrow toopen a selection menu.
2 Select a group number for your samples.
Unit of Measurement
Introduce the correct unit of measurement of concentration in order to
visualize the results.
Statistics
If a sample is identified with Sigma sign, it will be included in the statistics evaluation.
Results are shown in the following field :
m : Average Value
n
∑ Xi
m= i =1
n
Xi: Concentration values
n: number of samples
∑ (Xi − m)
n
2
σ abs = i =1
σ abs
σ rel = * 100%
m
3.7 SYSTEM
System Screenshot
From here you can check the conditions of the system, and follow the current conditions of the
measurement in real time.
After the start of the system all Standby functions are activated:
• The Hg lamp of the spectrometer is switched on
• The catalyst tube is locked by the pneumatic cylinder
• Oxygen flushes the catalyst, as long as there is gas pressure.
Catalyst, amalgamator unit and absorption cells are heated up to Standby temperatures. After
reaching these temperatures the Start button is released.
SPECTROMETER
The light intensity measured by the detector/s at the cuvette is represented as a blue bar.
The spectrometer is calibrated every measurement short before heating of the amalgamator.
In addition the shutter for measuring the 0% intensity is closed for short time. After opening
of the shutters the 100% intensity is measured.
In order to control the function of the shutter and the dark tension
(0 to 0,05V), the shutter can be closed and opened again between the measurements, by
clicking the screen symbol.
HEATERS
HEATING 1: for drying and decomposition of the sample. Here also the oxygenation takes
place.
HEATING 2: Heating of the catalyst zone at constant temperature.
HEATING 3: Heating of the amalgamator: at constant temperature to prevent separation of
condensation water. Heating to high temperature is then used to release very rapidly the
accumulated Hg.
HEATING 4: Heating of the cuvette block at constant temperature, to avoid condensation.
AUTOSAMPLER
Graphic display of the pneumatic cylinders. The white points indicate
opened limit switches, the blue and red closed limit switches.
The cylinders are moved automatically only to take up or put back
the sample boats. Each cylinder however can be controlled
individually. Operating a cylinder symbol (rectangle), the cylinder will
change its position.
If a cylinder may not be moved to a certain point of time, no control
is possible (e.g. cylinder III may not be raised, if the rotation plate
moves).
1 select as load position the appropriate number, in order to position
a certain boat.
During a measurement the position of the measured sample is
indicated on the sample rotating plate.
TIME DISPLAY
After Start both Total Time and Sample Time will be displayed.
Sample Time shows the time already run off of a measuring series or of the current sample in
the following format : hh:mm:ss an.
In Automatic Mode the Total Time is calculated multiplying the number of samples by the
time required for the method :
e.g. 20 x 4 min = 1:20:00
The time to move the boats adds up to the time for data communication; to adjust this
deviation to the total time, after each measurement the time is calculated and the time
indication is corrected.
The coloured bar represents the measurement times (Rinsing time S, Amalgam heating time
H and recording time A). The current status of the measurement is indicated by the blue bar.
1 Switch on the DMA-80 System with Terminal. The DMA-80 System requires approx. 15 minutes of
pre-heating time before measurement can be started.
2 Select under Sample Measurement an existing file or create a new file for the sample, or create a
new Sample Table.
Select the operating mode, either automatic or simple.
It is recommended to run a number of "Blank" values before starting to measure. This will
determine if the system is clean and free from contaminations. Water condensation or dust may
give undefined absorptions in the spectrometer. The impurities are in this way eliminated.
To enable the system to carry on a measurement, it is required to enter a weight different from
0,0000. Any entry other than 0,0000, for example “1.0000” will enable the measurement. The
calculated concentration is not substantial for the blank value. The absolute Hg-detected amount is
indicated in [ng]
A blank run should be performed without any sample boat to test the system, as otherwise it is not
sure if the blank comes from the system or from Hg traces in the boat.
The sample boats should be cleaned in a separate cleaning step.
3.8.3 AUTO-BLANK SETTINGS
In the column CalFactor of "Results" table is entered the calibration factor used for measuring the
Hg-contents (Standard value : 1.00). The calibration curve can be corrected with a calibration
factor lower or higher than 1.
Use a reference sample to check the calibration curve. A new calibration factor is calculated after
sample measurement.
To make a calibration two files are required, one measuring file (same as the one for sample
measurement) and one calibration file. The calibration file must be loaded or opened prior to the
measurement, and must be entered under Measurement/Links.
After measurement of a calibration sample, the data are taken automatically over and are used for
the computation of the calibration curve.
1 Create a new calibration file. If you want to add a new calibration sample from an existing
calibration, enter the desired calibration under Measurement/Links.
2 Change into Measurement Menu and open in the File register an existing file or create a new file
for the data of the calibration sample. Select Simple operating mode.
3 Run a blank measurement to make sure that the system is free from Hg contaminations.
4 Add one data record. Select for this data record the method that you want to use for calibration.
5 Define in the Status column of the "Result" menu the sample as calibration sample. The
"Concentration" c[µg/kg] column, otherwise closed, is ready for input.
6 Enter concentration and weight of the sample, put the calibration sample into the Autosampler
(use only perfectly cleaned boats) and start measurement. After measurement the data will be
automatically taken over in the calibration file. Also with a blank value as calibration point,
concentration (0.0) and weight (>0.0) must be entered, as the Software with check these
inputs.
7 Repeat Points 5 and 6 for additional measurements.
8 After measuring the calibration sample, go back to the calibration menu. Select measuring
data to be used for the calculation of the calibration curve.
9 Enter the kind of computation for each cuvette.
10 Save the new or modified calibration file.
3 DMA-80 SOFTWARE 640/1640 and PC 62
Milestone DMA-80 Operator Manual – Revision 1/2010
HISTORY TRAIL
The menu point of the History Trail is located in the Start page.
In the History Trail all changes in the system are logged with time, date
and person, and saved in the internal memory.
SPACE ALLOCATION
Display of space allocation in the Flash card(only terminal)
PRINT
The History Trail is printed out.
SYSTEM ADMINISTRATION
From here the basic settings of the software can be looked at or modified
according to level of authorization.
User does not have any access to the system administration.
Changes must be stored in the Administration Panel. Otherwise the changes
are automatically saved when quitting the Administration panel.
3.10.1 ACCESS
Panel- Here are carried out the settings for the terminal
Administration (e.g. brightness of the screen).
3.10.2 PANEL-ADMINISTRATION
Access
SUMMER
Used to acrivate or disactivate the acoustic signal when touching the screen
icons/buttons.
CONTROLLER/TERMINAL-VERSION
The Software program is only accessible if the licence number for the Software-Version and
the Serial number of the Terminal are matching. The licence number can only be given by
Service.
SAVE
To secure that setting modifications are maintained also after new start of
the terminal.
User-Administration
LOGIN-MODE
Check-marking „Password only“, one valid password
is sufficient to log in. Otherwise also a personal Flash
Card with signature is required. To modify the Login-
Mode a Flash Card with Service Signature (for
Service only) is necessary.
See also Chapter FDA-21CFR Compliance.
CHANGE PASSWORD
It is possible to change your own password ( or a subordinate password) as
well as access rights. Do not use „0“ as initial of a password, as „0“ will be
ignored.
DELETE USER
The Administrator can delete an User (with user access).
3.10.4 SETTINGS
PRINT
All current settings will be printed out.
Setup 1
Setup 1
Others functions The gray spaces are locked; these functions can be not modified.
Setup 2
Setup 2
Save of data after one The measured values are saved after each measurement.
measurement They will remain in memory without any later saving.
Setup 3
Setup 3
Additional sample disk Function to abilitate only in case is present a second auto-
sampler tray (40 positons).
The first sample disk is running and the second is prepared
externally. After removing the first disk, user is asked how to
proceed.
Additional sample disk Function to abilitate only in case is present a second auto-
sampler tray (40 positons).
The first sample disk is running and the second is prepared
externally. After removing the first disk, user is asked how to
proceed.
Others functions The gray spaces are locked; these functions can be not
modified.
Limits
Limits
3.10.5 CONFIGURATION
Configuration
Definition of interfaces for balance, DMA unit and support for LIMS can be set by Service.
However the user can select the separator, type of file and decimal for LIMS.
Balance Setting
SETTING OF BALANCE
An electronic balance can be connected to the terminal via an interface
cable. Communication settings are made under Balance setting (see also
the user manual of the balance).
No saving is required after modification.
Received Text, With functioning communication with the balance, the text and the
Weight display weight received from the balance are indicated here.
Manufacturer of the <Other>: touching Print on the balance (see also the user manual
balance of the balance) the weight is transferred to the terminal and from
here touching the balance icon it can then be transferred to the
Sample Table.
Precisa: The weight is constantly updated on the terminal. Touching
the Balance icon the value is transferred into the active cell of the
Sample Table.
Interface cable Cable with RJ45 plug at the terminal. For Precisa balances a 1:1
cable can be used.
Plug position
PIN Signal
2 RxT
5 GND
6 TxD
Status Messages
STATUS LINE
In the system main menu there is the status line of the currente status of the unit. .
DMA_NO_ERROR
The system is in Standby-Mode and is ready for sample measurement.
DMA_MEASURE_IN_PROGRESS
Measurement is under process.
DMA_MOVE_IN_PROGRESS
The rotating plate or the pneumatic cylinders are moving.
TREAD STOPPED
This message appears only for very short time after the measuring has
been broken off pushing the Stop button.
Push the red-green Start button and the system is again ready to start.
ERROR MESSAGES
INIT
When an error has been recognized by the software, an error message
appears on the screen. After acknowledgement, the error message will also
appear in the status line.
After repair of the error (by the user if this is possible) the unit must be re-
initialized clicking on Init (The Init button appears over the Start button).
COMMUNICATION ERROR
If the communication between DMA and terminal is disturbed, or the DMA
does not react to an instruction from the terminal, communication error is
indicated.
1 Check if the connecting cable from DMA-80 ⇔ Terminal is correctly
plugged in.
DMA_LIGHT_BARRIER_ERROR
The DMA-System controls at all times the Autosampler
turntable. When the software is started, it will look for and
find the reference position (double hole in tray at position
31).
Taking out the sample tray, it will interfere with the
position light sensor and the software will display the error
message. This means that the position of the turntable is
no more known to the system.
Verify that the turntable is inserted correctly and initialize
the unit with Init.
DMA_CALIBRATION_ERROR
Initialization Error:
During initialization of the autosampler, if the reference
position of the turntable (double hole at pos. 31) is not
found within one complete turn (360°), the calibration error
is displayed.
Make sure that the sample tray is correctly inserted and re-
initialize the equipment clicking on "init" start button.
DMA_PNEUMATIC_ERROR
Pneumatic Error:
The pneumatic actuators did not move after the command
was sent from the terminal.
The reason may be due to a blocked or disconnected
oxygen line (empty bottle or incorrect setting of the
pressure regulator) or the pneumatic actuators are
blocked.
Check the oxygen line and re-initialize the equipment.
DMA_T1_FAILURE
This message indicates that the measured temperature
increase was too low if compared with the required value.
This means that the heating coil for drying/decomposition
is not functioning, or the required value is too high.
Initialize the equipment from the System-Page.
DMA_MOVE_ERROR
Move Error:
No signal was sent to the light barrier within a certain
time, although the sample tray should move.
Make sure that the sample tray is not blocked.
See also Initialization Error.
INCORRECT EXTINCTION
The extinction [A] (height) of the measuring signal of the
2nd cuvette is larger than 0.8. The measured value is
therefore invalid and is not evaluated.
MA_CONTROLLER_ERROR
There is a small CPU/controller board installed inside the DMA-80. When the system is
switched on the board boots and checks the system. This error message indicates that the
CPU/controller board is not working correctly.
Re-start the system or call the local Milestone representative fort service.
DMA_HARDWARE_VERIFY_ERROR
The signal of the light barrier is controlled several times by the controller board before it is
recognized as valid. Thus it is guaranteed that no electrical disturbance falsifies the signal.
The error message means that the signal was not received correctly.
Contact your local Milestone representative for any technical support, application advice and
supplemental operator training.
Before using the Direct Mercury Analyzer for the first time, the instrument must be calibrated using prepared
Standard solutions of Hg or Standard Reference Materials (SRM or CRM). The instrument does not have to be
re-calibrated every time, but the calibration curve must be checked every morning prior to analyze unknown
samples. The instrument has to be recalibrated only if the calibration check results in 10% higher or 10% lower
than expected recoveries.
The instrument has to be also recalibrated when any of the major components are replaced. For example,
calibration must be performed when the catalyst and/or the amalgamator are replaced, or when the oxygen
tank or gas regulator is changed.
The Direct Mercury Analyzer can be calibrated using solid Standard Reference Materials or diluted aqueous
standards. Diluted aqueous standards (or working standards) may be prepared by diluting either 1,000 ppm or
100 ppm Hg standards (stock solutions). Both standards are commercially available. Use the equation below to
dilute the standards.
Working standard (ppm) = Stock solution (ppm) x (Volume of the stock solution (mL)/Total
volume (mL)
Total volume is the volume of the working standard.
For Example:
To prepare 1,000 µg/Kg(1 ppm) working standard, take 100 µl of the 1,000 ppm Stock solution and dilute up
to 100 mL.
To prepare 2,000 µg/Kg(2 ppm) working standard, take 200 µL of the 1,000 ppm Stock solution and dilute
up to 100 mL.
To prepare 5,000 µg/Kg(5 ppm ) working standard, take 500 µL of the 1,000 ppm Stock solution and dilute
up to 100 mL.
To prepare 7,000 µg/Kg(7 ppm) working standard, take 700 µL of the 1,000 ppm Stock solution and dilute
up to 100 mL.
To prepare 10,000 µg/Kg(10 ppm) working standard, take 1,000 µL of the 1,000 ppm Stock solution and
dilute up to 100 mL.
The diluted aqueous standards for low and medium concentration (ppb range) are prepared from the 1 and 5
ppm solution.
To prepare 5 µg/Kg(5 ppb) working standard, take 0.5 mL of the 1 ppm solution and dilute up to 100 mL.
To prepare 10 µg/Kg(10ppb) working standard, take 1 mL of the 1 ppm solution and dilute up to 100 mL.
To prepare 20 µg/Kg(20 ppb) working standard, take 2 mL of the 1 ppm solution and dilute up to 100 mL.
To prepare 30 µg/Kg(30 ppb) working standard, take 3 mL of the 1 ppm solution and dilute up to 100 mL.
To prepare 50 µg/Kg(50 ppb) working standard, take 1 mL of the 5 ppm solution and dilute up to 100 mL.
To prepare 100 µg/Kg(100 ppb) working standard, take 2 mL of the 5 ppm solution and dilute up to 100 mL.
To prepare 200 µg/Kg(200 ppb) working standard, take 4 mL of the 5 ppm solution and dilute up to 100 mL.
To prepare 500 µg/Kg(150 ppb) working standard, take 5 mL of the 10 ppm solution and dilute up to 100 mL.
There are three different working range responses that the instrument may be calibrated on:
To calibrate the instrument for its full range, prepare 5 ppb up to 10 ppm Hg working standards as described
above. Use 0.5 % - 5 % (1 % suggested) dilute hydrochloric for the dilutions.
Make sure the stock standard is not old or contaminated. As soon as the working standards are prepared,
transfer them into brown glass bottles. Aqueous standards with low Hg concentration are very unstable when
stored in plastic or regular clear bottles. Do not expose the Hg standards to the air for any length of time. Mix
the aqueous samples each time prior the analysis. As soon as the sample is pipetted out, close the storage
container. Don’t leave the solution bottles open on the bench and at the end store them into a fridge at 5-10°C.
Now apply the following formula in order to get the correct concentration value of new standard.
Working standard (ppm) = [Stock solution (ppm) x Weight of injection (g)] / Total volume (mL)
As example:
- 1000 mg/Kg (ppm): take 100 µl from 1000 ppm Stock solution and dilute up to 100 ml.
[1000 ppm (stock sol.) x 0.100 g (Weight of injection)] / 100 ml (total volume of flask)= 1ppm
-25 µg/Kg (ppb): take 0.5 µl from 5 ppm (5000 ppb) solution and dilute up to 100 ml
[5 ppm (standard sol.) x 0.500 g (Weight of injection)] / 100 ml (total volume of flask)= 0.025 ppm (25 ppb)
Open the “Methods”, type a new method name, description and assign the working parameters of the
instrument, such as drying and decomposition time and save the new method file.
Drying time varies with the volume of the sample and has to be calculated using the following equation:
Drying time (sec) = Sample Volume (µ µL) × 0.6
Decomposition time is 150 sec
Open the “DMA-80 Measurement ” click the button to obtain a new empty data file, type a new data name,
description and save new data file.
Open the “DMA-80 Calibration”, click the button for provide new empty calibration file, type a new data name,
description and save the new calibration file.
Return to the “DMA-80 Measurement ”, and load the data file saved.
Open “Sample” table of “Data”. Click “magic wand” button to build a new line. Click in the “Sample name” field
and type sample name. Under the “Weight” column, enter the weight in units of gram (or volume in mL) of the
working Hg standard that will be used for calibration (if 100 µL is used, then enter 0.1).
Open “Result” table and clicking the “Calibration” button appears under State “C”. Enter with the concentration
of your working standard solution in units of µg/Kg(ppb) or mg/Kg(ppm). For example, 100 µg/Kg (see Figure
1).
Ignore the “Hg (ng)”, the “Calibration Factor” and the Cal file. Nanograms of mercury will be plotted against
absorbance in the “Calibration” panel (see Figure 3).
When performing a calibration, the instrument first has to be calibrated for 0 ng of mercury. To do it, firstly, run
an analysis of several empty boats (this cleans the system and the boats). Empty boats must be repeatedly
processed until a low, stable absorbance is obtained. Then, follow the calibration procedure that has been
described above, running one of the clean empty boats. In the “Result” table, enter 0.0000 in the “C (µg/Kg)”
column and 0.1 g in the “Weight” column.
The calibration may be performed using two different approaches: Type A or Type B (the most commonly
used).
Calibration type A
Performing calibration using three standard solutions via different volumes
Use the following Table 1 as a guide to calibrate the instrument. Always start with the lowest amount of
mercury. Make sure that the sample boat is at room temperature before introducing the sample into it.
Use the following equation to determine the volumes of various working standards you should use to calibrate
the instrument.
Use variable volumes of the 0.1 ppm (100ppb) , 1 ppm, 10 ppm working Hg standards, and the following
equation, to calibrate the instrument i.e for low range, Hg (ng) = 0.1 ppm x Sample weight (mg). For 0.1
ppm(100 ppb) Hg standard liquid solutions, 10 µL solution contains 1 ng of Hg.
Table 1
Figure 4. Complete cal. of Cell 0 Figure 5. Complete cal. of Cell 1 Figure 6. Complete cal. of Cell 2
(only for DMA-80 Tricell)
After calibration, the user can select different calibration algorithms: linear, s-curve or square.
Clicking on the button of Cell 0 you can force the curve to 0 (when yellow, the function is activated).
Clicking on the button of magnifying lens the ultratrace range is selected (when yellow, the function is
activated); see chapter 3 (ultratrace range) for more details.
Calibration type B
Perform calibration using the same volume but different standards solutions.
To calibrate the instrument use the following Table 2 as a guide. Always start with the lowest amount of
mercury. Make sure that the sample boat is at room temperature prior to introducing the sample into the boat.
Use the following equation to determine the volumes of various working standard to use to calibrate the
instrument:
Use a fixed volume of 100 µL aliquots from various concentrations of standard solutions, and the following
equation, to calibrate the instrument for the low range, i.e., Hg (0.5 ng) = 0.005 ppm (25 µg/Kg) x Sample
weight (100 mg), etc... For standard solutions at room temperature, 100 mg is equivalent to 100 µl.
Table 2.
Figure 7. Complete cal. of Cell 0 Figure 8. Complete cal. of Cell 1 Figure 9. Complete cal. of Cell 2
(only for DMA-80 Tricell)
After calibration, the user can select different calibration algorithms: linear or square etc...
Clicking on the button of Cell 0 you can force the curve to 0 (when yellow, the function is activated).
Clicking on the button of magnifying lens the ultratrace range is selected (when yellow, the function is
activated); see chapter 3 (ultratrace range) for more details.
For measuring a calibration sample, you have to select a new line in the “Results” table of “DMA-80
Measurement\Data” and click the “Calibration” button. All calibration samples are stored in the table on the
Calibration in the software.
Activating the calibration function appears under state “C”, type sample name in the field of “Sample name”.
After editing the “Weight” field of the sample, it is absolutely required to edit the “Concentration” field of the
measured sample in the “Result” table. Without editing the “Concentration” field, the sample will be used as a
calibration sample of 0 ng.
Note: The concentration needs to be entered in units of “µg/kg” (ppb) or mg/Kg (ppm).
The Result field is normally blocked: no entry is allowed when measuring a sample. This field can be edited only
when working with Calibration and Reference sample functions.
You have to enter “0.00” in the Result field only when measuring the “Blank” value as a “Calibration” point. The
software requires an entry in the weight field that differs from “0.0000” to enable the measurement of this
sample, e.g. “1.0000”.
After measuring the calibration sample, the data are written in the “Result” table and into the Calibration table
panel.
If this calibration function is activated, the measured result will be automatically added to the active calibration
table. To add the samples to a new or different calibration curve, firstly, create a new table.
To abort the Calibration function, click again the “Calibration” button. This is possible only before the sample is
processed. After the measurement, the data can not be changed any more by the operator.
(1) Start the software and turn on the “System” of “DMA-80 Measurement” and
allow some time to warm up
(2) Select a pre-stored method in the “Methods” , or create a new method for
your samples.
If you create a sample file first, the actual selected method file is stored
automatically. Therefore, first select the method file!
(3) Create a new sample file for saving the data from your samples. Select
between Auto or Single mode.
Note: It is recommended to measure liquid samples only in Single mode
using metal boat.
(5) Run some “blank” measurements to make sure the system is clean.
If no calibration is selected, the system cannot calculate the result of the
measurement.
(7) Measure your samples. For unknown samples introduce small amount(<5mg)
in order to avoid DMA contamination.
(8) Measure some blank values in between your samples to see if the system is
contaminated or not.
Blank measurement
It is recommended to run a number of “Blank” values before starting to measure unknown samples. The
measurement of the “Blank” determines if the system is clean and has no contamination of Hg inside.
Moreover, water condensation or dust can give an undefined absorption in the spectrometer. This can be
eliminated by running some blank values.
To enable a sample measurement with the software, it is required to enter a weight different than “0,0000” in
the “Result” table of “DMA-80 Measurement\Data”. If the entry in the weight field is “0.0000” the measurement
can not be started. Any entry different than “0,0000” will enable the measurement. e.g. “1.0000”
The measured value in the height field shows the result of the blank run. e.g. 0,0015 abs. This gives the
absolute amount of detected Hg, shown in the field “Hg” e.g. 0,05 ng Hg absolute
The calculated concentration depends on the entry for the weight.
Depending on the concentration of the sample to measure, a higher or lower blank value can be tolerated. A
blank run should be performed without any sample boat to test the system itself.
If the blank run is done with an empty sample boat, it is not possible to determine if the measured signal is
coming from the DMA system or if there is some residue in the sample boat. The sample boats should be
cleaned in a separate cleaning step. With liquid samples, a film may appear on the sample boat which can be
removed with a laboratory spatula. For solid samples, a brush can be used to remove any combustion residue.
It is recommend to clean the sample boats after every run to ensure correct analysis.
Auto-blank measurement
This function allows to automatically start blanks when the Hg amount detected is over a set limit.
More information about settings in chapter 3.8.3.
For the measurement of a Reference sample, select a new line in the “Result” table of DMA-80
Measurement\Data” and click the “Reference” button. A Reference sample is used to check the validity of the
calibration curve. Measuring this sample will calculate a calibration factor for correction of the curve. This factor
is displayed in a separate column of the “Results” of “Data” screen. The standard calibration factor is “1.00”.
Once activated, the Reference function appears under state “R”. After editing the weight of the sample, it is
absolutely required to edit the concentration of the measured sample in the “Result” field. Without editing the
concentration, the sample can not be used as a reference sample for calculating the calibration factor.
The “Result” field is normally locked when measuring a sample. This field need to be edited only for Calibration
and Reference Samples.
After measuring the reference sample, the data are written in the “Results” table and the calibration factor is
calculated by the “theoretical value” divided by “measured value”.
If the values match exactly, the calibration factor is calculated to be “1,00”. According to the deviation between
the two values the factor is higher or lower that 1,00.
Factor 0,97 result from reference sample is 3 % higher than the calibration value
Factor 1,00 result from reference sample is equal to the calibration value
Factor 1,12 result from reference sample is 12 % lower than the calibration value
To abort processing a Reference sample, click again the Reference button. It is possible to do it only before the
sample is processed.
To measure an unknown sample, the maximum volume is limited by the size of the sample boats for the
autosampler.
Using the Concentrate function, a large volume sample can be split into several aliquots and processed in the
system separately. This means the amount of Hg is collected in the system until the end of concentration
function is selected.
To measure a Concentrate, for instance, create: three new lines in the “Results” table of “DMA-80
Measurement\Data”. Weigh the samples normally and type the amount of each one in each “Weight” field of
“Sample” table. Return to “Result” table, select the first sample line and click the “Concentrate” button. The first
two samples will be automatically selected. By clicking on the second sample and then on “Concentration”
button, the first three samples will be selected. For first and second line the setting of the program will change
to Amalgam time = “0” and Recording time = “0”.
The sample is processed (thermally decomposed) in the system and all the Hg is collected on the amalgamator,
without measurement of the Hg in the absorption cell. This procedure is repeated for all the subsequent
samples marked with the Concentrate function. All the collected Hg is measured together with the last sample
of the concentration process.
To abort both functions, click again the corresponding button. This is possible only before the sample is
processed.
4.9 ANALYSIS
To start analysis, first make sure that calibration curve is loaded. Open the “DMA-80 Calibration” and choose
the curve to use.
Under “Program” table (Fig. 20) change working parameters of the instrument for every sample, such as drying,
decomposition and waiting time, if needed. Drying time varies with the volume of the sample or with
percentage of the water in the sample and has to be calculated using the following equation:
Max start temperature: Measurement starts only when temperature T1 (drying- and
decomposition furnace) is under the maximum Start-Temperature. This prevents the sample
boats to be exposed to high temperatures especially when working with flammable sample.
µL) × 0.6. or
Drying time (sec) = Sample Volume (µ
Drying time (sec) = Sample weight (mg) × 0.6 x % H2O.
For dry inorganic samples
Drying time =10 sec
For high organic samples
Drying time =30 sec - 1 min 30 sec
Decomposition temperature = 650°C for most samples (see also applications notes)
After all samples are loaded into the sample tray (in case of automode) and the data entered in the “DMA
Measurement”, open the “Results” table of “DMA-80 Measurement\Data” and press the “Start” button.
As samples are analyzed, the absorbance will appear in “Result” table under “Height” column, absolute amount
of Hg in the sample under “Hg (ng)” column and Hg concentration in the “C(µg/kg)” (Fig. 2).
5.1 SOFTWARE
LIMITED WARRANTY
The manufacturing company MLS GmbH fully guarantee for 90 days from purchase that memory media
and documentation are free from material and labour defects. MLS / MILESTONE shall replace defective
memory media and documentation provided they are.
The aforementioned warranty is limited to being the defect funded. It is limited to the replacement of the
defective memory media or documentation. The replacement of other damages is excluded. This applies
in particular to loss of profit, loss of data, or non-usability of the software as well as indirect damages.
This limitation is valid also in case MLS had particular knowledge of the possibilities of damages. In any
case the responsibility of MLS for damages occurred to the user or to a third person is limited to an
amount which is the minimum paid according to price list for software package.
MLS / MILESTONE hereby expressly exclude all express or tacitly given warranties,
guarantees, or properties in particular all warranties related with usability of the software
for use in the frame of a planned contract. Any contrary conditions are not valid.
MLS / MILESTONE particularly do not take over any special warranty for the "defect-free" software or
documentation and also is not responsible for matching customers standards or special requirements. In
any case all express and tacitly given warranties on the properties of the memory media and
documentation are limited to a validity period of 90 days.
It is excluded any warranty for products, memory media, software or documentation not supplied nor
delivered by MLS / MILESTONE. This is particularly valid for programs of these parties which are intended
for use in connection with MLS-Software or which contain MLS-Programs or Files.
5.1.2 REGISTRATION
Read very carefully the License Agreement. The installation of the Software or issue of safety
copies of the program mean that you accepted the terms of the license agreement.
REGISTRATION
When started for the first time the Software must be
registered before use.
Click on Registration. The easyDOC Registration form will be
opened.
Registration screenshot
Key After sending out the form you will get via e-mail your Key-Number.
Enter this number into the Key field.
OK
As soon as you have filled all fields including the Key-Number, click
on OK. The Software is now ready to operate.
FAX REGISTRATION
You can also register the software via fax. A form will be opened
to be filled in and returned by fax to MLS.
Telefax: 0049-7561-981812
CANCEL
To quit the Menu without saving.
5.2.1 GENERAL
The easyDOC software enables the downloading of all measured values and system parameters as well as
copies of screenshots from the terminal to a Windows-PC. All data can then be saved and filed on the PC,
opened, printed out and exported.
With easyDOC all data files can be displayed both in the form of graphics and tables.
The data files can be saved in Excel, ASCII, PDF and JPG formats.
No manipulations of the original data files are possible.
1 Install the easyDOC software on your PC or Laptop: Start the Setup-file and follow the
instructions for installation.
TERMINAL 1024
1 Connect your PC or Laptop via 0-Modem-cable with the PC-interface of the terminal 1024.
TERMINAL 640/1640
1 With Terminal 640 all data are saved on a flash card. This
Flash card is read with a card reader connected to the PC.
Card types: Flash Cards Type PC-Card or CF-Card (Compact
Flash Card) can be used.
Memory capacity: the Terminal is supplied complete with a Flash
Card with minimum 128MB. All memory capacities can be used.
Since the files are very small, some MB are sufficient.
DOWNLOAD
DOWNLOAD
This operation will download the selected data-files
displayed by the easyDOC-Software from the terminal to the
PC. The data files can then be saved.
Download-screenshot
1 Select under Port the COM-interface of the PC for connection to the terminal.
After successful connection the listing structure of the terminal will be displayed.
2 Select the files to be downloaded to the PC and confirm with OK. The file is shown in the
easyDOC software and the question Save under will appear. The standard path for memory is
indicated in the Set-up settings.
3 Save the file.
5.2.4 SETUP
SETUP
The Setup Menu is started from the upper line of the menu
OK
To save settings.
CANCEL
To quit without saving.
PATH
Path Settings-screen
1 Here are selected the directories for the single file types.
RS232 COMMUNICATION
RS232 Communication-screenshot
5.2.5 BACKUP
BACKUP
With the Backup-Tool it is possible to download and save
simultaneously multiple files on the PC.
Backup-screenshot
1 Select in the right window (under Save to) the directory path under which the files should be
saved.
2 Press the Synchronization button. If in the list there are files that were already downloaded
from the Terminal and are still present in the terminal, they will be displayed in the right
window.
3 Mark in the left window with a check-mark all the files to be downloaded.
4 Press the double arrow (in case only one file has to be downloaded, the single arrow must be
operated), to be able to download the files.
SYNCHRONIZATION
If the Terminal is synchronized with the PC-Directory, it will check which
files can be downloaded.
5.3 EASYDOC
Start-screenshot
OPEN FILES
This opens the Explorer, which can open an existing file.
The path selected in Setup will appear. Select the desired Folder and
File.
MAKE SCREENSHOT
This will generate a copy of the terminal screen.
DOWNLOAD
The selected file will be downloaded from the terminal to the PC and
will be announced in the easyDOC-Software. The file can then be
saved.
PRINT
Pressing the Print button the print preview will appear. The document
can then be printed out.
Print screen
PDF
This will generate a PDF of the current document.
Operating this button will open Explorer.
Indicate a name for the document and select the directory in which it
should be saved.
BACKUP
With the Backup-Tool it is possible to download and save
simultaneously multiple files on the PC.
TYPES OF FILES
System Protocol
Status of the system and modifications of settings.
5.3.3 CALIBRATION
CALIBRATION
System Parameters and diagram of the calibration are
represented.
1 Open or download a file with extension *.c80.
Calibration-screnshot
The heading of the columns may be different, depending on the way it was set in the DMA-
Software. Instead of Peak (Maximum value) the column can be designated as Area (Integral).
ZOOM
GRAPHIC BUTTONS
COPY TO CLIPBOARD
The diagram is saved in the clipboard.
GRAPHIC EXPORT
EXPORT GRAPHIC
Data or diagrams can be exported in different formats.
Register Picture
▪ Bitmap, GIF, JPEG: image formats
Options: specify resolution
▪ Metafile: Format for 32-Bit-Windows-
Systems; Options: Activation of enhanced
with Win95 and over
Size: specify size
Keep aspect ratio: maintain aspect ratio with
scale.
Register Data
▪ Text: Text format
▪ XML: Extensible Markup Language,
Standard for definition of language.
▪ HTML: Hyper Text Markup Language,
Document format for definition of Hypertext
in World Wide Web
▪ Excel: Microsoft Office Excel-Tabele calcu-
lation program
Series: definition of data to be saved together
Include: definition of additional data to be
saved together.
Delimiter: Specify column separation
PRINT GRAPHIC/DIAGRAM
PRINT GRAPHIC
Print window will be opened
The window shows a side view of the easyDOC Report.This contains the
data of the current project.
SAVE AS
5.3.4 SAMPLE
SAMPLE
Data files with extension *.d80 can be opened.
The screen on the left will show the data for Sample, Program
and Results. The right side shows the signal process of the
selected sample.
Sample-screenshot
PRINT SIGNAL
Print window will be opened.
SHOW GRAPHIC
The signal diagram can be faded in or out with the following buttons.
CHANGE SCALE
CHANGE SCALE
The axle scale can be changed to preset values for a better view.
AUTO SCALING
Axles are automatically adjusted to the optimal scale.
SHOW STATISTIC
This will open a window to show statistics. The currently opened file can
now be downloaded with Refresh Resuls..
▪ The file is shown as a table in the upper part of the screen.
▪ In the center of the screen are shown the numerical values of maximum
and minimum, average and absolute or relative standard deviation.
▪ In the lower part of the screen is shown the diagram of the marked
single values and the average. The single values are shown as a curve of
the marked numbers.
Sample-Bildschirm
REFRESH RESULTS
The currently opened file will be transferred to statistics elaboration.
PRINT GRAPHIC
The print window will be opened.
CHANGE UNIT
To switch from [µg/kg] to [mg/kg].
CHANGE SCALE
The axle scale for R Results can be changed to preset values for better
view.
AUTO SCALING
The axles are automatically adjusted to the best scale.
CLOSE STATISTIC
The statistic window will be closed.
5.3.5 PARAMETER
PARAMETER
Here are shown the parameters for calibration and sample
measurement.
Depending on the type of file that is open (Calibration or Sample) the calibration parameters
are shown on the left and the sample parameters on the right.
Parameter-Bildschirm
5.3.6 DISPLAY
DISPLAY
This generates a copy of the Terminal screen.
A dialog is shown for downloading of the screen.
Select an interface port (e.g. COM1) and press OK to
confirm. The downloading will be started.
SAVE SCREENSHOT AS
The file will be saved as image file (*.jpg).
COPY CAPTURE
The file will be saved to the clipboard.
PRINT GRAPHIC
The print window will be opened.
5.3.7 TRAIL
TRAIL
This will collect the protocol of the system (Trail files *.trl). All
changes are noted in the MLS Terminal.
5.3.8 METHOD
METHOD
Methods, i.e. Files with extension *.m80 can be opened.
Method-screenshot
6 DMA-80 MAINTENANCE
During routine maintenance of the DMA-80, both the unit and the labTerminal should
be turned OFF and disconnected from the power supply. The oxygen supply must be
turned OFF at the tank. Change the internal consumables only after the unit has
cooled to room temperature.
Wear body protection during the maintenance!
Gas flow
If the stability test is according to the specs, please proceed making new calibration (see user manual), otherwise
repeat the conditioning procedure again.
If the unit is not used for long time, the procedure for catalyst/amalgamator’s activation is
suggested!
It is suggested that the mercury sample boats be cleaned before starting to work with the samples. To do
this, bake them out collectively in a muffle furnace or use the following program:
Repeat this cleaning procedure until the absorbance is a stable, low number < 0.003
Note: consult the available Application Notes before starting to work with the unit; some samples, such as
crude oil, require a dedicated or specific configuration of the system.
The Tri-cell DMA-80 System with control software fulfils the requirements of a “Closed System“.
11.10 (a) Validation of systems The Owner / Operator of the Tri-cell DMA-80 can
establish a Validation of the Tri-cell DMA-80 software,
if one is desired. On request "Milestone" can provide
detailed documentation on the software development,
test, update, administration and filing.
11.10 (a) Ability to discern invalid or The Tri-cell DMA-80 Software controls the validity of
altered data records. the data on the basis of check sums. Altered records
cannot be opened or used.
11.10 (b) Ability to generate accurate All data records can be viewed, copied and printed
and complete copies of data with the Tri-cell DMA-80 Software and the PC utility
records program “easyWAVE”. With the utility program
"easyVIEW" the data can be exported in any standard
Windows Text format.
11.10 (c) Protection of records to The data records can always be viewed and printed,
enable their accurate and using the same version of Tri-cell DMA-80 Software
ready retrieval that was used for their recording.
Additionally they can be exported with the PC utility
program "easyVIEW" in any standard Windows Text
Format. These files can be viewed with every text
editor.
11.10 (d) Limited system access to The Tri-cell Dma-80 system fulfils the requirements of
authorized persons a "Closed System". Access to the system is divided
into 3 levels
- Supervisor + Service
- Administrator
- User
Access to the appropriate level is only possible by
using a write-protected electronic access card and an
additional password.
Every access level has different rights on the system
and control parameters which cannot be modified.
11.10 (e) Complete and secure A Process Report (History trail) captures all changes
recording of changes on the on the system that have influence on the analytical
system results or data recording.
The Process Report includes date, time, user name
and access level, and the kind of action that was
accomplished.
11.10 (f) Operational System checks The Owner / Operator of the Tri-cell DMA-80 System
to enforce permitted can establish and enforce Standard Operating
sequencing of steps. Procedures (SOP) for permitted sequencing of steps,
within the context of the “closed system” features and
functions of the System as delivered by the
Manufacturer. Calibration Checks, and Blank
Determination, as described in the System
documentation, are the only Operational Performance
checks provided by the Manufacturer.
11.10 (g) Use of authority checks The Tri-cell DMA-80 System fulfils the requirements of
a "Closed System". Access to the system is divided
into 3 levels
- Supervisor + Service
- Administrator
- User
Access to the appropriate level is only possible by
using a write-protected electronic access card and an
additional password.
Every access level has different rights on the system
and control parameters which cannot be modified.
11.10 (h) Use of device checks… In the Tri-cell DMA-80 System, data are generated by
validity of source data a Tri-cell DMA-80 Direct Mercury Analyzer directly
connected to the related control terminal with control
software. The terminal and software are dedicated to
the task. There are no other data sources
communicating with the terminal or software. For this
reason device checks are not necessary.
11.10 (i) Training of the persons All persons with access authorization for Service
according to their assigned and/or Supervisor level receive appropriate Education
access authorization. and Training by the Manufacturer. Education and
training of system operators (Administrator and User
level) is provided by the Manufacturer’s
Representative within the context and at the time of
the initial on-site installation of the system. Education
And Training of additional system operators is the
responsibility of the Owner / Operator of the Tri-cell
DMA-80. On request, supplemental Education and
Training courses can be provided by the
Manufacturer’s Representative.
11.10 (j) Responsibility for the The Owner / Operator of the Tri-cell DMA-80 System
execution of electronic can establish policies that hold individuals accountable
signatures. and responsible for all actions initiated under their
electronic signatures.
11.10 (k)(1) Controls over distribution The Owner/Operator of the Tri-cell DMA-80 System is
and access of the system responsible for establishing and using appropriate
11.10 (k)(2) Controls over System The Owner/Operator of the Tri-cell DMA-80 System
Document Revisions and are responsible for establishing and using appropriate
Change Control Procedures. controls over Tri-cell DMA-80 System Documentation
revisions and Change Control procedures.
11.50 Signature manifestations
11.50 (a)(1) Data records with electronic Together with the Signature; the complete Name /
signature must show the Identification of the person is printed out.
complete, printed names.
11.50 (a)(2) Data records with electronic Together with the signature; the date and time of the
signature must include the execution of the signature are printed out...
date and the time of the
execution of the signature.
11.50 (a)(3) Data records with electronic Together with the signature; the meaning of the
signature must contain the signature is printed out.
meaning of the signature.
11.50 (b) For the electronic signature The electronic signature is part of the Tri-cell DMA-80
the same controls as for data record and therefore undergoes the same
electronic data records must controls as the data records themselves.
be applied.
11.70 Secure linking of the The electronic signature is imbedded as part of the
signature with the data Tri-cell DMA-80 data record and cannot be separated,
record copied or transferred from the data record by ordinary
means.
Subpart C Electronic Signatures
11.100 (a) Unique identification of each The Tricell DMA-80 System prevents the repeated use
Person of the same password for different users.
Each user must identify him using a write-protected
electronic access card and an additional password.
11.100 (b) Verification of the identity of The Owner / Operator of the Tri-cell DMA-80 System
the signature must verify the identity of the individual prior to
assigning a write-protected electronic access card and
password.
11.100 (c) Certification of electronic The Owner / Operator of the Tri-cell DMA-80 System
signatures. is responsible for communicating with the Agency
regarding the use, authenticity, and intended
equivalence of electronic signatures for hand written
signatures.
11.200 (a)(1) Use of two different To access the Tri-cell DMA-80 System and for
components for the executing the electronic signature, unique
identification. identification is required using a write-protected
electronic access card and an additional password.
11.200 Signature components used To gain access to the Tri-cell DMA-80 System, unique
(a)(1)(i) for a series of signings identification must be made by the write-protected
during a continuous access electronic access card and an additional password.
period. During a single continuous period of controlled access,
the presence of the electronic access card installed in
the system, is sufficient for repeatedly executing the
signature. The presence of the electronic access card
is polled for automatically.
11.200 Signature components used To gain access to the Tri-cell DMA-80 System, unique
(a)(1)(ii) during discontinuous access identification must be made by the write-protected
periods. electronic access card and an additional password. If
the electronic access card is removed from the
system, then the access period is terminated. To
regain access to the Tri-cell DMA-80 System, the
unique identification must again be made using the
write-protected electronic access card and the
additional password.
11.200 (a)(2) Signature Components used Each user of the Tri-cell DMA-80 System chooses their
only by the genuine owner own unique password to associate with the write-
protected electronic card assigned to them for their
personal use by the Owner / Operator of the System.
11.200 (a)(3) Attempted misuse of The Owner / Operator of the Tri-cell DMA-80 System
Signature Components. is responsible for administering and executing
electronic signature components in such a way that
the collaboration of two or more individuals is required
in any attempt to misuse the electronic signature
owned by another user.
11.300 (a) Combination of The Tri-cell DMA-80 System prevents the use of the
identification and password same password in association with different electronic
must be unique. cards. Each user of the Tri-cell DMA-80 System must
identify himself to the system using a write-protected
electronic access card and a unique additional
password.
11.300 (b) Periodic checks of the The Owner /Operator of the Tri-cell DMA-80 System
passwords. are responsible for periodic review, maintenance and
11.300 (c) Loss management Access to the Tri-cell DMA-80 System is in 3 levels
procedures - Supervisor + Service
- Administrator
- User
A superior level can, at any time, administer and also
delete the subordinate levels.
11.300 (d) Transaction Safeguards to If more than three (3) consecutive attempts to access
prevent unauthorized use of the system fail due to incorrect combination of
passwords electronic access card and password time, the incident
will be indicated in the Process Report (History trail).
The Owner / Operator of the Tri-cell DMA-80 System
must ensure that the Process Reports are evaluated at
reasonable time intervals.
11.300 (e) Periodic test of the function During each access to the system the functioning of
of the system security the write-protected electronic access card and
checks. associated password are checked.
If damage is present in the electronic access card or
the card reader, access will be denied.
The software with the administration of the password
points cannot be deleted or installed by the user.
For this reason this point cannot be used.
Accident release
measures
Personal precaution no special protection required
Methods for cleaning up mechanical cleaning
Accident release
measures:
Personal precaution Ensure adequate ventilation
Use personal protective clothing
Methods for cleaning up Avoid raising dust
Take up with absorbent material (e.g. sand, kieselguhl,
universal binder)
Pick for disposal in tightly closed container
Storage The material is delivered inside of a catalytic tube.
Store the tube in a cool, dry, well-ventilated place.
Handling Contact to the human body is only possible when the
catalyst tube is broken. Wear goggles, rubber gloves,
protective clothing. Ensure adequate ventilation
Physical and chemical
properties
Appearance Solid, with black – brown colour, odourless
Flash point not applicable
explosion limit not applicable
solubility in water partly soluble, alkaline solution is formed
Ecological Do not discharge product unmonitored into the
considerations environment
Disposal considerations In accordance with regulations for special waste
Must be taken to a special waste disposal site
1 - Product and Company Information Wear self-contained breathing apparatus and protective
clothing
Product Name SAMPLE ADDITIVE A to prevent contact with skin and eyes.
Product Number DMA-80 - SFA
Company Milestone S.r.l. 6 - Accidental Release Measures
Via Fatebenefratelli, 1-5
I-24010 Sorisole (BG) PROCEDURE(S) OF PERSONAL PRECAUTION(S)
Technical Phone # 39-035 573857 Wear respirator, chemical safety goggles, rubber boots,
Fax 39-035 575498 and heavy rubber gloves.
E-mail address application@milestonesrl.com METHODS FOR CLEANING UP
Sweep up, place in a bag and hold for waste disposal.
2 - Hazards Identification Avoid
raising dust. Ventilate area and wash spill site after
SPECIAL INDICATION OF HAZARDS TO HUMANS material pickup is complete.
AND THE ENVIRONMENT
Irritating to eyes and respiratory system. 7 - Handling and Storage
No data available.
DISCLAIMER
For R&D and chemical laboratory use only. Not for drug, household or other uses.