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DMA-80
Operator Manual
MA213
Milestone Srl MA213-003 – DMA-80 EVO – User Manual
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Milestone Srl MA213-003 – DMA-80 EVO – User Manual
2 INSTALLATION ....................................................... 9
2.1 Unpacking and checking list ................................................. 9
2.1.1 DMA-80 EVO STANDARD EQUIPMENT........................................... 10
2.2 CATALYST AND AMALGAMATOR INSTALLATION .......... 13
2.3 DMA-80 EVO SETUP ......................................................... 20
2.3.1 Voltage setting ................................................................................... 21
2.3.2 DMA connection with Terminal 660.................................................... 24
2.3.3 DMA 80 EVO connection with PC ...................................................... 25
2.3.4 DMA safety switch ............................................................................. 29
2.4 Gas connection................................................................... 29
2.4.1 Oxygen tank ...................................................................................... 30
2.4.2 Milestone Air compressor .................................................................. 30
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1 SAFETY RULES
1.1 General Information
Please read carefully this operator manual before switching on the system and follow its
prescriptions with the utmost care.
In case the system has been delivered with additional accessories, also carefully read the
instruction manuals of such accessories.
Follow with particular attention the recommended instructions for Service and Maintenance.
This Operator Manual is part of the delivery, hence must be always kept together with the
instrument on its working place.
It is imperative that every person operating this system has read and fully understood this
manual.
The non-observance of the instructions contained herein or improper use may involve
damages/injuries that are not covered by product liability!
The national ruling and international safety norms in working environment shall in any case be
observed under user’s responsibility.
It is also user’s responsibility to keep constantly updated all safety norms ruling in the country
or operation.
All additional safety guidelines of this manual and the safety guidelines on the unit are as well
to be noted.
Attention = means that the non-observance of the warning may cause damages to unit or
properties.
Warning means that the non-observance of the warning may cause injuries, even severe, to
people.
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Milestone Srl MA213-003 – DMA-80 EVO – User Manual
Basic rules of chemistry will always apply. The basic rules of chemistry are valid also for handling
chemicals in this unit. Working with chemicals always takes all those safety measures that are
usually required (e.g. lab coat, protective gloves, protective glasses mask, exhausts hood, etc.)
The user is responsible for the compliance of the above safety instructions with the local
regulations.
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Milestone Srl MA213-003 – DMA-80 EVO – User Manual
The power supply cable must be in perfect conditions and must not show any damage. Do not
bend the cable. Do not place it over hot surfaces or hang it and protect it from oil. Never
connect the cable if you have wet hands.
When you connect the unit, check that the voltage and the frequency of power supplies match
with the value indicated on the label place on the back of DMA-80 EVO.
Never touch parts with live wires. This may cause an electric shock, which can result in serious
injuries or even death.
The exhaust gases may contain high Hg concentrations, depending on the working
conditions. A proper treatment of the gases is necessary.
Should a neon tube or a low pressure lamp break, this could increase the Hg mercury in the
DMA-80 EVO. The area must be properly aired.
1.10.1 Fuses
In case of a fuse replacement, this part must be replaced following the indications described
in this manual. The fuses below are built in the unit:
Power Supply: 2 x 6,3 A fuses, 250 V for a power supply of 230 V
2 x 10 A fuses, 250 V for a power supply of 115 V
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Milestone Srl MA213-003 – DMA-80 EVO – User Manual
2 INSTALLATION
2.1 Unpacking and checking list
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Milestone Srl MA213-003 – DMA-80 EVO – User Manual
Provide a bench of at least 150 cm length and 70 cm wide and place the DMA-80 EVO on the bench. The
unit requires sufficient space (approx. 15 cm) on all sides to allow adequate movement of air.
The weight of the DMA-80 EVO is approximately 56 kg; at least 2 people are
needed to remove the unit from its box and place it on the bench.
Terminal 660
Usb stick
Pen
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Pen holder
RJ45 cable
- Option 2
Pc software package
Gateway
USB cable
RJ45 cable
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Power cord
Autosampler plate
Mercury trap
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For safety reason the catalyst and amalgamator are packed separately to the DMA-80 unit so they need
to be installed as first step.
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FLOW
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The DMA-80 EVO system must be installed in a well ventilated, dust free room, free from acid
vapours or highly corrosive chemical atmosphere. Aggressive vapours can attack the system
through its ventilation openings and cause heavy damage to the electronic boards, plugs, etc.
The optimal placement is in an air-conditioned room with approx. 20 °C (± 3 °C).
Install the amalgamator and catalyst before proceeding with DMA-80 EVO SETUP (see chapter
2.2).
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An incorrect voltage setting of the unit can cause damages on the electrical components.
Always measure the inlet voltage on the power socket before to proceed with the voltage
setting.
The factory voltage setting on the DMA-80 EVO units is 220-240 VAC
The DMA-80 unit can operate with a voltage of 220-240 VAC or 110-120 VAC and indifferently with 50Hz
or 60Hz. The change of voltage needs some modifications.
From DMA-80 EVO SN 20032968, the voltage setting of the device also needs wiring the primary
connections of the transformer.
- The below procedure has to be made for DMA-80 EVO units before SN 20032968
Replace the two fuses from the holder with the ones
suitable for the inlet voltage:
- for 220-240 VAC: 2 x T6,3A
- for 110-120 VAC: 2 x T10A
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Install the fuse holder into the plug and press it until
the tabs engage
- The below procedure has to be made for DMA-80 EVO units from SN 20032968
Replace the two fuses from the holder with the ones
suitable for the inlet voltage:
- for 220-240 VAC: 2 x T6,3A
- for 110-120 VAC: 2 x T10A
Install the fuse holder into the plug and press it until
the tabs engage
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2.3.1.2 Change of connections on the voltage transformer (only for DMA-80 EVO units from SN
20032968)
- The below procedure has to be made for DMA-80 EVO units before SN 20032968
- The below procedure has to be made for DMA-80 EVO units from SN 20032968
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Plug the other end of the serial cable into the RJ45
interface port of the Gateway.
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So, when operating the lid must be closed otherwise the heating element will be not supplied and an error
message will appear
In case of Oxygen, the pressure switch module will not be provided by Milestone.
It must be provided with a pressure indicator and a manometer with scale from 0 to 10bar(for example)
and with division 0,25bar in order to be able to set a pressure of 4 bar. The inlet connection must be
dedicated for O2 or Air tank.
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Note: the connections are different if you use air or O2. The outlet connection must be suitable
to connect 6x4 Rilsan tube.
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Light source
One low pressure mercury lamp.
Wavelength
253.65 nm.
Detectors
UV enhanced photodiodes,
Instrument controller
Terminal 660
Touch-screen industrial grade controller 6.5” screen with 65.000 colors; VGA resolution 640x480
for sharp process graphic.
5 USB port, 1 LAN connection for network, 2 RS 232 ports for external devices, 2 video port.
Methods and runs saved on PC-compatible 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, Vista or 10.
Instrument software
Milestone easyCONTROL®
LIMS compatible.
Compliant to FDA regulations 21 CFR Part 11.
Detection limit
for solids and liquids
0.003 ng (dual-cell)
0.001 ng (dual-cell double beam)
0.0003 ng (tri-cell double beam)
Typical precision
Less than 1.5%: dual cell, tri cell with or without double beam option at 10ng
Less than 5%: wide range at 5000ng
Working ranges
for solids and liquids
Automatic switch-over.
Dual-cell: Low range: 0.03 to 20 ng. High range: 20 to 1500 ng.
Wide Range: 10 ng to 20000 ng
Dual-cell Double beam: Low range: 0.01 to 20 ng. High range: 20 to 1500 ng.
Tri-cell Double beam: Low range: 0.003 to 5 ng. Medium range: 0.01 to 20 ng. High range: 20 to
1500 ng.
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Calibration
Standard solution and certified reference materials.
Type of sample
Solids and liquids
Auto-sampler
40-place, with dual-tray option for continuous operation.
Sample container
Metal or Quartz boats for liquid /solid samples
Sorbent traps for gas samples
Sample weighing
External analytical balance with automatic weight transfer.(option)
Carrier
Oxygen or Milestone Air Compressor (option)
Power
110-230V/50-60Hz.
Dimensions
Unit: 80 x 42 x 30 (H) cm.
Weight
Unit: 56 kg.
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a
f
c
d e
Legend
a. Autosampler section
b. Air grids for cooling
c. Lock for main chassis
d. Main power switch
e. Terminal or personal PC
f. Back light logo
RED (flashing): The software is on Settings pages or the analysis has been
interrupted.
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k
i
m
g
h l
j
Legend:
g. RJ45 port for controller connection
h. Power entry module
i. Instrument identification label
j. Exhaust outlet for Hg trap connection
k. Window for detector regulation
l. Gas carrier connection
m. Flow regulation valve
Attention: do not bypass the switch with the housing open. This causes presence of voltage in
the system
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x x
v
r n
u p
q
w
o
x
t s
Legend:
n. Pneumatic section
o. Autosampler plate
p. Drying/decomposition furnace
q. Catalyst furnace
r. Amalgamator furnace
s. Power supply 24V
t. Hg power supply
u. Hg lamp
v. Cuvette
w. Dual beam option (optional)
x. Cooling fans.
y. Autosampler led
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Milestone Srl MA213-003 – DMA-80 EVO – User Manual
A special link to connect directly to web site is available on DMA-80 EVO PC software in the
Measurement page.
The website is divided into different sections for three different Milestone instrument. Choose the DMA-80
EVO section. Here different function that you can find into the website
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Milestone Srl MA213-003 – DMA-80 EVO – User Manual
CONNECT
This button will automatically connect the browser to the main page of the
terminal, so you can monitor your run.
NEWS
Here you can find news about info and products connected to the unit.
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MY PROFILE
Here you can find personal information, warranty and configuration of your
unit.
CONTACTS
You can ask a support for application issues to Milestone local
representative and to Milestone Application Team.
LIBRARY
Here you can find a lists of scientific papers for different applications.
When you open the website, the browser asks for username and password:
For the first login, please use the information reported in the special card you can find in the Terminal
box.
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ATTENTION : username and password of this area are different from the login credentials for T660
terminal.
After the first login, please fill in the form with your personal info.
Attention:
IP Address is the same as you set in
the T660.
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5 SOFTWARE
5.1 Login
Switching on the DMA-80 EVO unit, also the terminal 660/1660 is turned on and the program is initialized.
If the login mode USB key and Password has been selected (FDA-21CFR part11), the software requires
to introduce your USB key with signature. In case of unit controlled by PC software package, this is not
requested.
There are different levels of access authorization. Select your access in the login window. Type your
name and confirm it by the tick on the top right of the page or by pressing the left large icon. At this point
use the touch screen or the mouse, since the keypad is not active yet.
The factory password for Administrator and User are Administrator 123456
here reported. User 123
The password can be changed in the Control Panel,
if needed.
Once completed the login, the DMA main page is opened. Here the samples can be set up for the direct
mercury determination. If the user has already operated with the unit, the most recent file is available.
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The method signature is carried out during the storage. There the administrator can sign the methods and
release them for the user. The method signature is carried out in the same way as the file data (described
later). Once saved a method with signature, the signed method is marked with the corresponding symbol
in the quick selection.
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After the signature, the file can be saved with the tick up right. The signature is part of the file and now the
document is signed with username, date/time and type of signature. The signature is displayed also on
the top of all results printouts.
The symbol „eraser“ is used to remove a signature. In case of changes to files, the signature is no longer
valid. This occurs for example by a further measurement. If necessary, it must be re-signed.
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Milestone Srl MA213-003 – DMA-80 EVO – User Manual
his work and he wants to logout without switching off the unit, the popup window here below is displayed.
After the logout, the login window is displayed again.
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- FILE OPENING: Files can be opened from the storage memory by the popup menu “Load”.
The software allows to see and open only the files with the extension of the page where you are.
For example, if you are in Calibration page and open the pop up menu for opening the files, then you can
just see and load calibration files in .c80 format. Data and method files will not be seen.
For this reason, files should have been saved in the proper folder in according with their extension
(measurement files in .d80 format will be in the Data folder, calibration files in .c80 format will be in
calibration folder, method files in .m80 format will be in method folder).
Choose the desired file from the list and confirm by the tick up right. The file will be opened.
In case of calibration or method files, you can also find them in the quick selecting panel. Here, only the
most recent or the last 10 created methods and calibrations are available for quick selection.
- FILE SAVING: Files can be saved in the storage memory by the popup menu “Save”.
Input the desired name in the field “Name” and confirm by the tick up right..
Once entered the name, the system will automatically add the appropriate extension (i.e. „.d80“). By the
tick up right, the file is stored, and the window closed.
When any modifications is made to the file, it should be saved. Anyway, if you forget to do it,
when you change the page, a message appears so that you can make the saving if you need.
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During the writing or reading of the USB key, do not remove the USB, otherwise you could lose
the data. The writing or reading procedure is displayed on the screen by an hourglass.
- FILE DELETING: File can be eliminated definitely from the LOAD or SAVE page.
When the window for saving or loading is open, it’s possible to cancel a file by selecting it from the list.
The name of the file is displayed in the field “name”. The software will ask you confirmation with a
message before to proceed.
Files can be also removed from the page where they are currently opened (“cleaning of the page”), but
the elimination is not permanently since they will be stored in the external memory.
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There are several USB ports available on terminal 660 (or 1660). The UBS key can be connected to all
USB ports available on the terminal, but always only one at a time.
In case you want to change the USB key, then, first of all you have to remove the one currently connected
and then, introduce the new one.
The other outputs are used to connect printer, mouse, keypad and barcode reader.
Mobile storage area: The USB memory is used to save methods, sample tables and measurement data.
It is also used as signature to work in accordance with CFR Part 11.
The directory for the USB key in the terminal is A:\ (USB-Stick).
Storage: The terminal is supplied with a USB key. All memory sizes can be used. If the files are very
small, few MB as memory is enough.
In terminal 660 (or 1660) it’s also possible to save files on a shared directory of NFS- or CIFS- server.
The procedure is described in the chapters 5.15.1.3
Here you can manage your methods. It’s possible to create, edit, save and delete
methods. In each method you can set the heating, amalgamator, flushing and
recording time of the measurement programs. Appropriate basic methods are
automatically uploaded upon delivery.
Here you can manage the calibration files. From a calibration file, you can
choose the measurement points for the calibration and the type of regression
curve for each cuvette. You can find also a control chart of the reference sample.
This window and its subpages represent the main user interface. Here you can
set the sample weighing as well as recording and evaluation of the signals and
also the output of the results.
Here the status of the system is monitored (position of pneumatic cylinders and
autosampler, temperatures of heating elements and detector voltages).
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Some icons (generally used) are available in several menu points and they can be selected
from there.
Add a new line: a new line is added in Measure page. There are some options
that you can set when you make a new line. They will be explained in the
chapter 5.13
The sample name, calibration and method are taken over by the marked data
record. If the name has a number as the last figure, this will be increased
automatically by 1.
If no position has been entered yet, no sample name would be registered in this
first line.
Create a new method: pressing it, a new method can be created. Some values
are set as default but you can change them as you like.
Delete the method: Pressing it, the method page is “cleaned”. It creates a new
method with some default values. The file is deleted from the temporary memory
(but not from the external memory)
Switch OFF for function activation: in case the function is not active, the icon
color is blue and it is marked with “0”
Switch ON for function activation: in case the function is active, the icon color is
green and it is marked with “I”
Switch LOCKED:grey color means that the option can not be changed by the
current user.
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START BLINKING: The warming up of the unit has not completed yet since
some temperatures or detector voltages have not reached their starting values,
yet. If you press the icon and the table with measurements is ready, then the run
will begin automatically after the warming up is completed.
STOP: A measurement is ongoing. The external ring shows the progress of the
sample analysis
STOP BLINKING: By pressing this icon, it starts blinking and the run will be
interrupted once completed. This means that the system is stopped, after
completing the ongoing analysis. The icon flashes until the analysis conclusion.
If you want to stop the analysis immediately, press the button once again. Then
the boat will be removed.
A complete stop of the system by double click of the icon during a
measurement can cause damages to the catalyst (i.e. when stopping
the measurement of liquid samples) and release of combustion
fumes.
Several fields need the input of numerical values or words. After double click on the respective field or
numbers that should be modified, a numeric keypad is displayed. Where words can be entered, after
double click the standard keypad will be displayed
PC USB keypad or externally one connected to terminals can be used.
5.10.4 Print
With terminals type 660 and 1660 is possible to connect directly a printer but the number of compatible
models is very limited due to high language protocols that the new printers satisfy.
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Therefore, the PDF function is the best way to take the data from the terminal and then print them from a
common PC.
In case of PC software package , you can use all models of printer compatible with your PC.
PRINT: Print function is available from the popup menu of the Method,
Calibration and Measure pages.
Print icon is available for all pages of Settings menu.
Print function in
Measure page
The only specific page is printed if the MULTIPLE PRINTING function is disabled
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The administrator can specify in the setup under setting/files whether parallel
to the measurement saving you want to automatically save the PDF files. It’s
possible to choose as well, if you want to save the measurement in tables
form (“table”) or each single signal with all data („graphic”). Alternatively both
PDF files can be saved in the background.
Here below a screenshot of the CSV layout where in blue the customizable fields are marked.
- The Amount field must contain at least a number. If this is left empty, then the DMA software will
not read the import file
- Cal file and Method file field can be left empty and filled on the DMA software once the file is
opened. If they are left empty the software automatically will fill them with the method and
calibration opened on the terminal.
Otherwise you can fill them before to import the file, but you have to insert the exact name of
calibration and method file saved on the terminal.
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1. Download and save the CSV Milestone file in your chosen location
2. Start Excel
3. Select 'Data' on the ribbon, and then 'From Text'. (If the menu options are greyed out this could
be because you do not have a workbook open).
4. Browse for the *.csv file you need to import, and click “Import”.
5. In the Text import wizard, ensure the 'Delimited' option is selected. Click Next.
6. In the delimiters section, tick “Semicolon”. The text qualifier box should show the double-quote
symbol. Click Next.
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7. Mark every columns as “General”. The first column only will initially be highlighted. Move the
horizontal cursor as far as it will go to the right; then, holding the shift key down, click the very last
column heading. You should now have every column highlighted. Click the “General” data format.
Click Finish.
8. It may ask you 'Where do you want to put the data?'. It will allow you to click into any cell on the
blank worksheet to determine where the data should go. Click 'OK' to proceed.
9. The data should now appear in the spreadsheet. Where column headings are included these will
appear in the top row. Check that fields have not lost leading zeros where applicable.
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In this page it is possible to create, handle, modify, save, print, delete and load the analysis methods.
The administrator defines the steps of time and temperature and parameters of the method in according
with the type of samples to measure. After the storage, the method is available as well in the quick
selection field.
Factory basic methods are available upon delivery and they are suitable for most of applications.
Reactive or special samples need specific and dedicated methods which are available by contacting
Milestone Application Dept. or by consulting the Application NOTE document supplied with the unit or
downloadable accessing to Milestone Connect portal.
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5.11.1 Methods-Parameters
Quick selecting panel: Here, only the most recent or the last 10 created
methods are available for quick selection.
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Drying and decomposition steps: Here you can choose the best values of
time and temperature of the different drying and decompositions steps of your
analysis method.
This phase happens in the first empty part of the catalyst tube (ashing chamber,
furnace 1) which is surrounded by an heating coil and the temperature is
controlled by a thermocouple installed in the sample boat holder.
Ideal method graph: graphic representation of your analysis method where the
following steps are also shown by a coloured bar:
- Drying/decomposition time: red colour
- Purge time: grey colour
- Amalgamator heating time: purple colour
- Signal recording time: blue colour
Description: here you can enter all information regarding you method
Max. start T: The measurement only starts when the temperature of the ashing
oven (furnace 1) has dropped below the maximum starting temperature. This
would avoid evaporation of the sample (in case of liquid) before closing the
catalyst flange.
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Signal recording time R: Here the spectrometer signal (Hg content of our
sample released by the amalgamator) is noted and later analyzed and calculated
Unit of sample: Different unit are available in according with type of sample to
measure.
The chosen unit will be used as unit for “Amount” field in the Measurement page
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By pressing the white paper icon, the previous method will disappear and a “new method” will be
available.
It is also possible to create a new method starting from an existing method, just changing some
parameters.
The administrator can enter the values of time and temperature, the unit of sample and aall information
concerning the new method.
Milestone recommend to contact Milestone Application Dept. or consult the Application NOTE
document before to create a new method for uncommon samples.
Milestone recommend to use always as value of Purge time, Amalgamator time and signal
recording time the following:
Everytime a new or existing method has been created or modified, it has to be saved.
From the popup menu, select Save, choose a name for the new method and save it in the destination you
prefer (Method folder is the default destination)
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For opening, deleting, and printing method file, refers to chapter 5.10.2 and 5.10.4
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This should be made when you want to create a new list of measurement in Measure page.
Method selected from popup menu Method selected from quick panel (only the last
created /loaded methods are available)
In this way, all measurement lines in Measure page will have the same method you selected in the
Method page.
If you want to use different methods for a list of measurements or you want to add measurements and
change the methods, then you have to do it in Links page.
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The available methods in the popup menu of the Links page are the ones temporarily saved in the quick
panel; therefore be sure that the method you want is available otherwise load it in Method page and then
select it form popup menu of Links page
In this page it is possible to create, modify, save and print the calibration curve of the unit and also
manage the reference samples.
Here all calibration points are automatically reported in the graph from the Measure page and
subsequently connected together by the user.
It is not possible to add or create calibration points from this page. This is only the graphic representation
of the calibration curve (file .c80 format).
The data file of the calibration curve is created in the Measure page where it is possible to insert the
calibration points.
Quick selecting panel: Here, only the most recent or the last 10 created
calibration curves are available for quick selection.
Calibration points: these are the calibration points automatically reported by the
software, from the Measure page, where they have been created
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If selected in grey colour, it means that the point is resulted out of the
absorbance limit of the cell but the the curve considers it in its track and
calculation.
You should uncheck these points.
This normally happens in cell 0 since it has a dedicated detector and/or in cell 1
to an existing calibration, when you change the limit of absorbance of the cell
(Settings/Analysis page. Please see chapter 5.17.1 )
Abs values: Values of the absorbance (height of the peak) of the calibration
points
Example:
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The value A on the curve for 1ng should be 0.0547. If you multiply the measured
value of 0.0437(real value) with 1.252, you get the 0.0547.
Or if you subtract 0.0110 from 0.0547 you get 0.0437.
The value A 0.0437 matches on the curve with the amount of 0.679ng mercury.
If you substract from 1ng 0.321ng, you will get 0.679ng.
Or if you subtract from 1ng 32.1%, you will get 0.679ng.
- grey colour: the point is not selected from the list of calibration points and the
curve does not consider it in its track and calculation
- red colour: the point is new and it has just been added to a calibration file. The
calibration needs to be saved other wise the point will be lost. After confirmation,
the point will become blue colour and the curve consider it in its track and
calculation
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For each sample are always displayed and analyzed all the existing
measurement signals. If the maximum height of the peek of the first signal (i.e.
cuvette 0) exceed the limit of absorbance of the cell (set in Settings/Analysis
page. Please see chapter 5.17.1 ) , then the maximum height of the next signal
will be automatically used to calculate the result.
The Administrator can adjust the limit of absorbance of the cells,
according to his need.
Ultratrace analysis: This function works only for the most sensitive cell.
So, in case of tricell it works for cell 0, in case of dualcell for cell 1.
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The calibration curve can be adjusted accordingly for the measurement values in
ultra-trace range. This function adds a percentage range (40% as default but
Settable in Setting/Analysis.) to the highest measured value. All values
exceeding this range will not be calculated in this cell and they will be analysed
in the next cell without affecting the slope and quality of the curve at lower
ranges.
The function ultra-trace allows a linear track in the most sensitive cell, without
changing the maximum limit of absorbance for this cell.
In particular, in case of tricell unit, an optimized measurement range is reached
by exceeding the linear range of cuvette 0 in cuvette 1.
The advantage to use the Ultratrace function is that the limit of absorbance of
the cells remains untouched. This is important for who needs to use different
calibration curves on the basis of his samples with different Hg concentrations..
In this way, the limit of absorbance of cell does not need to be changed every
time every time.
So, a dedicated ultra-trace calibration curve should be saved and used
whenever required.
BV correction: with this function you can set the absorbance point on y-axis
where the calibration curve meets it.
When the function is activated, the curve is determined by the set value. For the
ultra-trace calibrations, the curve can be forced through the typical blank value,
in order to optimize the accuracy of low range.
In cell 2, the blank value should not be considered. The calibration must be
forced through the zero point and the registration of the correction value is not
necessary in this case.
Zoom: a specific area of the calibration graph can be zoomed by pressing with
finger or mouse curser a point in the graph and then move down or right to
select the interested space.
The magnifying glass icon will scale the image to its original size.
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Here below is reported the standard procedure type A which can be followed to make a standard and
common calibration curve valid for DMA -80 EVO dualcell and tricell configurations.
Anyway, the solutions or samples as well as weighing and ng points can be chosen by the customer
according to his need.
Dedicated calibration procedures for ultrarace and standard working ranges will be better explained in the
Tips & Techniques chapters.
Procedure:
1. First of all, choose the solutions or samples to use for performing the calibration curve in
according with working range.
2. In the main page of the software, go to Method page and choose the method to be used for the
calibration procedure. (you can create a new method or load an existing one). Usually this
method will be the same for all calibration points since the sample used for the calibration should
be the same for all points (you can also select the method for all points in the Measure/link page).
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3. The calibration should start only when the unit is perfectly cleaned. This means that the
acceptable blank should reach a value based on the working range and minimum value to
quantify. So make enough blanks until the desired value is reached. (it should be at least three
times lower than first calibration point) If the unit is perfectly cleaned go to point 4.
3.1. Go to method page and create/load the suitable cleaning method (See chapter: Tips and
Techniques). For cleaning of the instrument, the best way is using “Clean water” method”. It
consists to fill quartz boats with 0.3ml of distilled water.
3.2. Go to Calibration page and load the existing calibration curve: this is necessary to allow the
software to start with measurements. If no calibration curve is loaded, n measurements can start
3.3. Go to Measure Page and add new measurements line. You can create a new measurement file
or add lines to an existing file. (How to create a new measurement file will be better seen in the
next chapters).
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In the links Page you should have the method and calibration files previously selected
3.4. Take a cleaned quartz boat (it should have been cleaned before, following the cleaning methods
described in the Tips and Techniques chapter) and fill it with 0,3ml of distilled water. Save the file
and press START button.
3.5. In according with the final result (absorbance) and working range, you could need to run
additional blanks. You can also check the cleaning of the instrument without using boat and
water. This will give you an indication of the instrument blank but it will not clean the machine
thoroughly: in other words, the instrument blanks should be run after obtained a good results with
clean water method.
4. Go to Calibration page and create a blank sheet where the software will insert the calibration
points from Measure page.
5. Save the calibration: choose a name for the new calibration and save it in the destination you
prefer (Calibration folder is the default destination)
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7. Before to insert the calibration points, choose if you want run them in Single mode or Automatic
mode.
Single mode: Each sample is measured individually. Each measurement has to be manually started
pressing START button. After measurement the rotating plate is turned to loading position of the next
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.
Milestone recommends to work in single mode during the calibration especially using
aqueous solutions to avoid the evaporation of the samples waiting for measurement.
The procedure below is made using Single mode.
8. Insert the first calibration point: The first calibration point has to be a real blank with the same
volume and matrix used for all the other points of the calibration. Perform at least two replicates
for this point in order to get the minimum and stable ABS value.
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8.1. Under Pos column, choose the position of the autosampler plate where the boat with sample will
be placed
8.2. Under SampleName column, give a name to the calibration point
8.3. Under Amount column, put the exact sample amount after checking it with a balance (It is
intended the weight of sample, without boat)
8.4. Under State column, select Calibration
8.5. Under Hg Concentration column, enter the concentration of Hg present in your sample (in case of
first calibration point (real blank), the Hg concentration will be 0 ug/Kg)
The absolute value of Hg [ng] is automatically calculate by the software after entering
Hg concentration and amount of calibration sample. The values in Hg [ng] column do
not have to be changed or entered
9. Take a cleaned quartz boat (it should have been cleaned before, following the cleaning methods
described in the Tips and Techniques chapter) and fill it with the same volume and matrix used
for all the other points of the calibration as explained in point 8.
10. Before to Start with the measurement, verify in Link page that the Calibration and method file are
the ones you selected before and you want us for the calibration.
11. The software will ask to save before to Start with the measurement, so choose a name for the
new measurement file and save it in the destination you prefer (Data folder is the default
destination)
You can use the same name used for the Calibration file since it is the data file of the
calibration curve. There is not conflict by using the same name because the extension
is different (for data file, the extension is .d80)
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12. Press Start and wait the end of measurement. At the end of measurement the software will switch
automatically in calibration page, showing the new calibration point added to the calibration
graph.
13. In calibration page, save the new point otherwise it will be lost changing the page. The calibration
point will become blue color.
14. At this point, it is possible to add further calibration points in according with the working range to
cover.
Go to point 8. and repeat each single step for each new calibration point. You can also already
create the table of all calibration points. Remember that working in Single Mode only the selected
sample will be run after pressing Start.
The quartz boats have not to be hot when injecting samples, especially in case of
aqueous solution. Wait enough time to get them cooled before to inject sample,
otherwise the solution could evaporate
15. When all calibration points have been measured, then you can join them by choosing between
the different functions available in Approximation method.
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The connection of the points can be made even before all calibration points have been
measured. The availability to have the connection functions (linear, square, ..) will
depend by the number of points, position in the graph and distance between them.
It is recommend to joint the point everytime a calibration cell has been covered. For
example, in case of dualcell, join the points in cell 1 after measuring the 20 ng
calibration point (value close to the limit of the cell)
In case you want to keep Automatic BV function enabled during the calibration,
remember to join the previous points on basis of the ng value set for Automatic BV.
(see chapter 5.17.1.2. Blind values)
In the calibration above we used aqueous standard solutions stabilized with ultrapure HCL 2%
v/v.
With different standard solutions we could cover a working range from 0ng to 1000ng:
The columns circled in red are the values that the operator has to enter
The columns circled in green are the values calculated by the software (absolute value of Hg[ng])
on the basis of “Amount” and “Concentration”([ug/Kg]) and generated by the instrument (Height)
These values will be used by the software like reference to trace the calibration curve.
The choice of which cell use for the points is automatically decided by the software on the basis
of the limit of absorbance of the cell set in software settings page.
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It is possible to change the limit of absorbance of the cell to increase or decrease the
range of each cell in according with the customer's needs.
Changing the limit of absorbance of the cell (up to their min. and max allowed by the
software), the [ng] scale will change accordingly.
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
Example:
To prepare 1000 µg/Kg(1 ppm) working standard, take 100 µl of the 1000 ppm Stock solution and dilute
up to 100 mL.
To prepare 2000 µg/Kg(2 ppm) working standard, take 200 µl of the 1000 ppm Stock solution and dilute
up to 100 mL.
To prepare 5000 µg/Kg(5 ppm ) working standard, take 500 µl of the 1000 ppm Stock solution and dilute
up to 100 mL.
To prepare 7000 µg/Kg(7 ppm) working standard, take 700 µl of the 1000 ppm Stock solution and dilute
up to 100 mL.
To prepare 10000 µg/Kg(10 ppm) working standard, take 1000 µl of the 1000 ppm Stock solution and
dilute up to 100 mL.
The diluted aqueous standards for low and medium concentration (ppb range) can be prepared from the
1 and 5 ppm solution.
To prepare 5 µg/Kg(5ppb) working standard, take 0.5 mL of the 1 ppm solution and dilute up to 100 mL.
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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(20ppb) working standard, take 2 mL of the 1 ppm solution and dilute up to 100 mL.
To prepare 30 µg/Kg(30ppb) 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 100µg/Kg(100ppb) working standard, take 2mL of the 5ppm solution and dilute up to 100 mL.
To prepare 200µg/Kg (200ppb) working standard, take 4mL of the 5ppm solution and dilute up to 100mL.
To prepare 500µg/Kg(150ppb) working standard, take 5mL of the 10ppm solution and dilute up to 100
mL.
There are three standard different working range responses that the instrument may be calibrated on:
- The low range is 0- 10 ng Hg
- The medium range is 10-20 ng Hg
- The high range is 20-1000 ng Hg.
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 . Mix the
aqueous samples each time prior to 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
Reference measurements are saved in these page. The file are stored in the disk with the format “.r80”
and the table with information on each measurement can be printed and serves as QC for the unit.
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 “1.0000”.
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Name of file: here is reported the name used to save the reference file
Reference: Reference samples are reported in this graph for monitoring the
trend in the time
Summation: clicking in this field, the line is selected, and the sample will be
included in the statistic calculations. The sum icon can be removed at any time
by clicking on again.
Cal. File: here the calibration curve to the which the reference sample is
calculated is reported
Standard Cal- Factor: Clicking on the arrow, the “m” value calculated after
selecting reference samples will be reported as standard Cal- Factor and
automatically set in the “Cal-Factor” columns when you start a new
measurement line in Measure page
The calibration curve can be corrected with a calibration factor lower or higher than “1.0000”. Measure a
reference sample with known Hg content, in order to keep the calibration under control.
Procedure:
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2. Create the reference measurement(s). (You could carry out a multiple determination, in order to
be sure that the result is correct).
3. Define the sample in the Status column of "Results" table as "Reference" sample. The column
"Concentration" c[µg/kg] (otherwise closed) is ready for input. Without editing the concentration,
the sample can not be used as a reference sample for calculating the calibration factor.
4. Enter concentration and weight of sample, insert the reference sample into the Autosampler (use
only perfectly clean boats) and start the measurement.
5. After measuring the reference sample, the result is automatically compared to the set limit values
and, in case of exceeding of the maximum deviation, the specific actions will be taken. 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. Reference measurements are documented in a
Reference window of the Calibration page
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6. The new Cal- factor can be automatically used for measurements once selected.
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Here it is possible to run unknown samples, insert the points for the calibration curve, run reference
samples and a lot of other actions.
In order to set up a sample, the user can pass through these sections from left to right and new samples
can be added at any time, also during ongoing measurements.
- The section Sample allows to enter comments on samples and to create multiple measurements.
- The section link allows to select the suitable working method and calibration which are introduced in the
quick selection. If only a calibration or method is used, please remove all the others from the quick
selection, in order to avoid confusion or any mistake. In this case it’s no longer necessary to enter this
page.
- The section Results, shows all results, including the possibility of a statistic analysis, calibration factor
and methods with volume indication of dilution factor.
Pos “1” (available in all sub-sections): It is the position of the autosampler plate
where the sample is loaded. The number of position can be changed by the user
(1): it is the sequential number of the measurements which continuously
increases by 1 for each record. It can not be changed.
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You can not change the unit of amount from the Measure page but you can
create methods with different amounts and the select them form “Links” page
- Option GMU
Request to tare
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With all data records a weight must always be entered, since otherwise the
measurement cannot be started.
The sample weight is indicated in “g”, “mg” or “µg” according to settings.
The sample weight is entered either manually by the keyboard/touch screen or
taken directly from an electronic balance through the interface cable.
In this way, it’s possible to add several lines. If in the starting line a sample
amount is entered, this is applied to all measurements. Even method and name
are taken. The first line is kept, since it is used for the results.
At the end of the analysis, in the first line of multiple measurements, the average
result is represented with related standard deviation. Single values can be
deactivated, while the sum sign is removed.
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Sample has not been weighed yet or the amount has not been
confirmed yet
At the end of measurement, a new option is available if you click on State field:
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Selecting “reprocess” in the “State” field, a new window will open and you can
select a different calibration from your calibration folder, change the name of
your measurement and use a different cal factor. Other parameters can not be
changed.
NOTE: the calibration must be opened previously in the calibration page so that
it will be saved in the drop-down menu.
Height (available in sub-section “Signal” and “Results”): In this column the value
of the absorbance is reported. Based on the type of calculation set in
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The value refers to the first signal within the limit of the absorbance of the cell. If
the limit is exceeded, then the next signal in the next cell will be considered.
Dilution (only available in sub-section “Result”): This field is available when you
set a method with “ml” like unit by clicking on cal. factor field.
The final result can be influenced by the dilution factor. The dilution factor can
correct the dilution of an original sample by the digestion.
Example: 1,605 g of a sample has been diluted in 45 ml. Dilution factor: 28,037.
When using the factor, the result is calculated with reference to the original
sample and not to the measured solution.
The input field dilution disappears by clicking another field. The dilution is
displayed under cal factor (here 333,33).
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Summation (only available in sun-section “Result”: clicking in this field, the lines
are selected, and the sample will be included in the statistic calculations. The
sum icon can be removed at any time by clicking on again.
Xi
m i 1
n
σabs: If more reference samples are selected, here the absolute standard
deviation is calculated
n
( Xi m)²
abs
i 1
n 1
σrel: If more reference samples are selected, here the relative standard deviation
is calculated
rel
abs *100%
m
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If you want to recall a different calibration file or method which is not included in
this list, the file must be first opened in the Calibration page and Method page,
so that it can be stored in the quick memory.
If a new line is added, the calibration file and method are taken from the original
selected lines.
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Signal Height (absorbance): The height of the peaks will be displayed at the
top of the peaks. The height of the peak within the limit of absorbance of the first
cell will be shown in the Measure page under column “Height”.
Signal Peak Width at Half-Height: The width at half maximum is independent
on the Hg-value, gas flow and installation of the amalgamator.
Peak Location: The time when the maximum signal has been detected is
displayed under the peak. The time measurement starts with the beginning of
annealing or the recording.
Peek zooming (only available in sub-section “Signal”): with the temperature and
signal profile icon deselected it is possible to zoom the peak.
By dragging from the top left to bottom right of the desired section, this section
will be zoomed. Stay briefly on the end position, it can also be zoomed more
than once.
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Anyway, it’s possible to use the same position several times. This can be
performed by a later change of the sample position, during an ongoing automatic
measurement. The measurement must be started for this purpose. The positions
of the samples on hold marked by the hourglass can now be changed. This
allows for example to clean a boat by repeated annealing.
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2. Choose the position of the autosampler plate where the sample is loaded and insert the name of
sample.
3. Enter the sample amount. (directly from a balance if connected to the terminal or writing the value
in amount field)
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5. Go to “Link” page and choose the Calibration file and method to use like reference.
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Spectrometer: here the detector voltage values of the maximum light intensity
(gain) of the lamp are shown.
The first signal refers to the detector on cell 1 and 2. (dual cell configuration)
The second signal refers to detector on long cell (cell 0, more sensitive)(tri cell
configuration)
The third signal is an option and it refers to the double beam detector installed
directly in front of the lamp.
Lamp: the lamp can be turned off manually for few seconds by clicking on this
icon. This action permits to check the dark signal (offset) with 0% of light.
Cuvette furnace: here is reported the heating element of the cuvette and its
temperature.
The temperature should be stable and constant at 125°C ± 5°C to avoid
condensation inside the cells.
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Catalyst furnace: here it is reported the temperature of the heating coil that
covers the part with material of the catalyst tube.
Purpose of the catalyst oven is to keep the temperature of the tube stable, which
is necessary for its optimal functioning. Inside the catalyst tube, mercury coming
from the sample is converted in metallic mercury and the reaction products
generated during the sample decomposition are neutralized.
Combustion furnace: here it is reported the temperature of the heating coil that
covers the empty part of the catalyst tube.
Purposes of this furnace are moisture removal from solid samples, bulk
evaporation from liquid samples and final decomposition.
Analysis time: Once started a measurement, the total time will be displayed
(Format hh:mm:ss). Independent on the time, in automatic mode, the estimated
time is constantly updated during the sample processing.
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The colored bar represents the measurement run through the different phases.
The blue bar indicates the current status of the ongoing measurement.
Waiting time: when an hourglass is shown on the counter bar, it means that the
temperature of this furnace is over the set value and it is reaching it to allow the
measurement to start.
The corresponding furnace shows the set temperature value (arrow in blue
colour) and the current temperature (arrow in red colour)
System status: This field shows the status of the system. Here different
messages are reported in case of errors in the system.
5.15 Settings
From the measurement pages, it is possible to access to the settings of the instrument clicking on the
Settings field of the popup menu.
Most of settings are only accessible with Service permissions, so here below are reported the settings
available for Administrator use.
5.15.1 Settings-Access
5.15.1.1 Panel
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Touch calibration: in case of terminal, this function allows to make the calibration
of touch screen
Software information
5.15.1.2 Users
In this page you can manage the access authorizations for users. In addition it can be unlocked the
special function according to FDA-21CFR Part 11.
See chapter 9
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Login mode: It is possible to choose different login mode . Only the Service can
change the mode once selected
User settings: here it is possible to change the parameter of the selected user
5.15.1.3 LAN
With the DMA-80 EVO software, it is possible to connect the terminal directly with a shared folder of your
network using a CIFS server.
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The Common Internet File System (CIFS) is the standard way that computer users share files across
corporate intranets and the Internet.
To set the CIFS you have to enter in the Settings/Access/LAN
If your network supports the automatically assigned IP address function for all
client connected to the network, you can select this option and your network will
assign an automatic IP address to your T660.
If your network doesn’t support the automatically assigned IP address you must
set the following settings:
Terminal 660 Insert the address of server and his shared folder where you want to save
directly the file of your T660.
Server ATTENTION:
T660 needs “/” (slash) as separator for the address.
Windows-server save the address using “\” (backslash).
Insert the name and password that networking administrator has assigned to
T660.
Username and password must be set in the server otherwise the server will not
recognize/accept T660
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5.15.1.4 Trail
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Usage: memory of the terminal used by trail. When it is full, you have to get it
free to continue to keep the actions saved.
Save the trail and delete it from the page
5.15.2 Settings-Settings
5.15.2.1 Analysis
Signal analysis: Set the type of software calculation to detect the quantity of
mercury present in the sample. You can choose Integral (area of the peak) or
Maximum (height of the peak)
Absorbance or emission limit of cell: absorbance limit considered from each cell
of the cuvette. The peak is considered and measured only if it is within the limit
of the cell. It the peak exceed then the next peak will be considered in the next
cell.
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5.15.2.2 Observation
Peak- Detection- Distance 1-2: for a proper detection of the peaks, the distance
between peak in cell 1 and peak in cell 2 should be within the range of 13 and 16
seconds.
Check: if activated, the software checks the distance between the peaks during
every measurement. In case of wrong value an error message will be displayed.
Milestone suggests to not activate this function.
Show: If activated, the software shows the value of the distance between T2 and
T1.
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Automatic blank value cycles: here it is possible to set the values for the
automatic cleaning of the system after a measurement with a certain ng value of
mercury. (No positions of the plate will be to set since the sample boat holder will
remain into the catalyst.)
In the example: In case of measurement resulting with Hg value corresponding
to 100 ng or more, the blank cycle starts up automatically to get a lower blank <
1 ng for a maximum of 5 times.
You can also set different ng 0-10000, blank cycles 0-100 and at the end of the
cycle it’s possible to select to “Continue” or “abort” the next run.
NOTE: for deep cleaning of boats and instrument refer to procedures described
on chapter 5.11 and 8.3
Blind value method: here are the values of the blind value used for autoblank
cycle.
The blind value can be also used manually by the user for cleaning the machine.
It can be set in the measurement page.
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5.15.2.4 Reference
Parameters of reference samples: here you can set the limits of the calibration
factor of your reference samples. When it is out of range you can choose if
continue anyhow with next measurements already set or stop the analysis.
Save of data after one measurement: if activated, the data is saved everytime
after one measurement
CSV import: This option can be set with Service login. If activated, it is possible
to import a CSV file from an external source.
The standard model of CSV file compatible with the DMA.80 software is supplied
with the USB key shipped with terminal or PC software package
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The file can be filled with desired information but the name of the column and
other data can not be modified otherwise the DMA software is not able to read
the file.
Here below a screenshot of the CSV layout where in blue the customizable fields
are marked.
- The Amount field must contain at least a number. If this filed is left empty, then
the DMA software will not read the import file.
- Cal file and Method file field can be left empty and filled on the DMA software
once the file is opened. If they are left empty, the software automatically will fill
them with the method and calibration opened on the terminal.
Otherwise you can fill these fields before to import the file, but you have to insert
the exact name of calibration and method file saved on the terminal.
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4. Browse for the *.csv file you need to import and click “import”.
5. In the Test import wizard, ensure the “Delimited” option is selected. Click Next
6. In the delimiters section, tick “Semicolon”. The text qualifier box should show
the double quote symbol. Click Next.
7. Mark every column as “General”. The first column only will initially be
highlighted. Move the horizontal cursor as far as it will go to the right; then,
holding the shift key down, click the very last column heading. You should now
have every column highlighted. Click the “General” data format. Click Finish.
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8. It may ask you 'Where do you want to put the data?'. It will allow you to click
into any cell on the blank worksheet to determine where the data should go.
Click 'OK' to proceed.
9. The data should now appear in the spreadsheet. Where column headings are
included these will appear in the top row. Check that fields have not lost leading
zeros where applicable.
Save PDF files parallel: a copy of the files in PDF format can be saved. You can
choose if save a copy of only the tables or graphics or both.
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5.15.2.6 Signaling
Sound volume and duration: you can choose the volume and time of the sound
5.15.2.7 Maintenance
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Milestone suggest to replace both amalgamator and catalyst at the same time
when one of the two reached the end of lifetime
Exchange of catalyst: A software message will inform the user that it is time to
replace the catalyst tube when the currently cycles have reached the set limit
(5000).
The limit value should be decided on basis of application since the lifetime of
catalyst tube strictly depends by it
Milestone suggest to replace both amalgamator and catalyst at the same time
when one of the two reached the end of lifetime
Switch off all heating elements: This function is useful during the catalyst
replacement: All heating elements stop to work but the unit keeps ON. In this
way the fans cool more quickly the tube.
5.15.2.8 Equipment
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5.15.2.9 Balance
In this page you can connect and configure a balance in order to transfer the sample weight directly to
software. Different models can be compatible with DMA-80 software, anyway Milestone strictly
recommends the Sartorius BCE224i-1S model.
The Sartorius BCE224i-1S balance can be directly connected to control terminal or PC through the proper
connecting cable.
Milestone offers the Sartorius BCE224i-1S balance model through two special kits based on the type of
connection:
a) P/N WAA0220-IT: Sartorius balance mod. BCE224i-1S + interface cable RJ45/RS232 (9pins) for
connection with terminal 660/1660.
The interface cable RJ45/RS232 (9pins) is also sold separately with p/n TER6477 or it can be created by
the user.
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PIN CONNECTIONS
2, orange wire 2
6, green wire 3
b) P/N WAA0220-PC: Sartorius balance mod. BCE224i-1S + interface cable USB A-C for connection
with PC (for DMA controlled by PC software package).
The interface cable USB A-C is a common cable sold in any electronic shop.
- DMA software parameters (bold parameters are proper for BCE224i-1S model)
Balance port: Port (COM) in the terminal where the balance is connected.
In case of DMA on PC software package, select the available port of the PC
where ethe balance is connected
Databits: Number of bits used to represent one character of data (you can
choose between 7 or 8 bit)
Parity: It indicates when a number is even or odd (you can choose among: even,
odd or none)
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- BCE224i-1S parameters (Highlighted parameters are proper for the communication with DMA software)
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5.15.2.10 Others
Switch off gas automatically: you can decide to stop the gas flow if the unit is not
used for some time. If activated, the valve in the system closes the flow passage
after the selected time from the last measurements.
It will be automatically activated, once you restart with the measurements.
This function avoids gas consumption when the unit is not in use. Of course, this
will cause accumulation of moisture inside the instrument (catalyst,
amalgamator, cuvette, so some blanks should be necessary before to restart
with the runs.
Show markers: if activated, the points to calculate the height of the peak and the
baseline are shown in the graph of the signal
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- Not when “n”: if you use the option “Automatic multiple measurement”, then the
software will not increase the number in the sample name of the measurement
sequence.
- Never: the software never increases the number in sample name in a list of
consecutive measurements.
5.16 Service
This section is normally used by Service engineer trained by Milestone, but some functions are also
available for Administrator.
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5.16.1 Service-Autosampler
In this page the Administrator can check and in case calibrate the autosampler plate if the position are not
aligned well with the pneumatic arms.
1) Connect the gas carrier to the DMA-80 EVO unit and place the autosampler plate on the drive
disc verifying that the positions 1 market on the drive disc and autosampler plate fit together.
2) In the software, open the main menu from the top left corner of the screen and go to
Settings/Service/Autosampler
3) Press on “Cylinder II and then Cylinder I icons to move the horizontal arm completely out from the
catalyst oven.
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4) Then, press “Cali” button: the autosampler plate starts to rotate and it stops when the hypothetic
position 1 of the plate is located above the vertical cylinder III.
At the same way, the software indicates the correspondent position of the autosampler plate directly in
front of the operator.
If the autosampler motor is properly calibrated, then the position 1 of the plate is in front of the catalyst
tube entrance and the position 11 is in front of the user.
5) Press the “+” or “-“ (for a faster movement) and “+1”, “-1” (for a slower movement) on the
software for moving the plate clockwise or under clock wise until the position 1 is placed in front
of the catalyst entrance.
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6) Adjust the alignment of the position 1 with the vertical cylinder so that the boat lift plate is
perfectly centered with the slot 1 of the autosampler plate when it lifts.
NOTE: with the boat lift up it is not possible to move the pate left or right.
7) Press “Cali.” Button again for saving of position 1.
Now also other three reference positions (Pos.11, Pos.21, Pos.31) have to be calibrated.
8) Press “Pos.11” icon: the autosampler plate should rotate in order to place the position 11 directly
in front of the catalyst flange.
9) Press the “+” or “-“ (for a faster movement) and “+1”, “-1” (for a slower movement) on the
software for moving the plate clockwise or under clock wise and adjust the alignment of the
position 11 with the vertical cylinder so that the boat lift plate is perfectly centered with the slot 11
of the autosampler plate when it lifts.
10) Then, press the next reference positions “21” and “31” and repeat the above actions. Everytime
you move from one reference position to the other the current position will be saved.
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5.16.2 Service-Detector
In this page the Administrator can check the detectors signals. In according with the spectrophotometer
configuration, it is possible to have two signals represented by two voltage values and two green lines in
the graph.
There are two different values of detector voltages: Offset and Gain
- the Offset is the signal of the detector when the lamp is OFF
Milestone set this value at around to 4,000V but it can change during the time because of heating of the
lamp, humidity inside the cuvette, etc.). The minimum acceptable Gain signal is set to 2V, after that the
software does not permits to run measurements.
It is also possible to have a further detector signal, “Double Beam”, if the configuration so provides. It is
represented with a blue line in the graph
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The double beam function is an option available for DMA-80 EVO units with configuration Dual cell and
Tri cell. A dedicated detector, also called “reference”, is installed directly in front of the lamp and in perfect
line with the smallest cell (cell 0 in case of tri cell, cell 1 in case of dual cell) for the continue monitoring of
its complete intensity.
The double beam function guarantees a better signal to noise ratio, a lower quantification limit and a
superior precision.
It works like follow: The software takes account of the maximum and minimum (lamp off) intensity of the
light detected by the detectors before each analysis
- Maximum intensity of the light =100%
- Minimum intensity (lamp off) = 0%
Therefore:
- Maximum intensity (100%) - Minimum intensity (0%) = 100% of light
The electrical amplification (GAIN value) does not matter at this point, because it is a relative
measurement.
In this page you can also check the stability of detector signal and signal noise.
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5.16.3 Service-Test
In this page you can test the proper working of the heating elements. Milestone suggests letting the
Milestone technician to do this.
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6 MAINTENANCE
Here some simple maintenance actions that the user can do to maintain the instrument in proper working
conditions.
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FLOW
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Perform the catalyst initialization procedure to See “Catalyst conditioning procedure” enclosed in
prepare the catalyst tube to the analysis all new catalyst tubes
It is recommended to replace the catalyst and amalgamator together after around 5000 runs
It is recommended to replace the mercury trap after 1 year from the installation
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Before working with used parts, which might be contaminated you should
wear:
o Mask anti dust FPP3;
o Disposables gloves
o Protection for the shoes.
The samples are weighed and carried out for measurement in special sample boats which can be made
of Nickel or Quartz.
Normally boats in nickel are indicated for solid samples or when you do not need to work at high precision
levels. Quartz boats are indicated for liquids or when you need high precise results free from any
minimum carry over effect.
Their volume does not refer to the maximum volume of sample you can put in the boats but it
refers to the maximum volume that they would be able to contain.
The amount of the sample does not depend by the capacity of the boats you are using but by the
application.
Standard volumes/amount recommended are:
- 0.1 ml for liquid samples (max 0.5ml)
- Up to 100mg for solid sample
- Always check the DMA-80 application note or contact Milestone representative of your
country to know the recommended amount to use before to analyse the sample.
- Always start by using the minimum amount allowed in case of unknown samples or of
unknown origin.
The nickel boats are more subjected to contamination than quartz and the lifetime strictly depends by use
and kind of sample introduced.
In order to avoid contamination from previous analysis it is suggested to clean them before starting to
work with next samples.
So, it is possible to put them in a muffle furnace (900°C for 10’ for quartz boats, 600°C for 10’ for metal
boats) or they can be run without sample in the DMA-80 EVO at 650°C (decomposition) for 180 seconds.
In case of residues of solid sample (ash, powder, etc.) you can remove them with a spatula.
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DMA_ERROR The system detected a malfunctioning and the measurement can not start
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8.2 CALIBRATION
8.2.1 How to make a standard liquid solution.
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
1000 ppm or 100 ppm Hg standards (stock solutions).
Solutions must be stabilized with ultrapure HCL 2% v/v.
Both standards are commercially available. (Stock solutions on market can be stabilized with HNO3 or
HCL).
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
Example:
To prepare 1000 µg/Kg(1 ppm) working standard, take 100 µl of the 1000 ppm Stock solution and dilute
up to 100 mL.
To prepare 2000 µg/Kg(2 ppm) working standard, take 200 µl of the 1000 ppm Stock solution and dilute
up to 100 mL.
To prepare 5000 µg/Kg(5 ppm ) working standard, take 500 µl of the 1000 ppm Stock solution and dilute
up to 100 mL.
To prepare 7000 µg/Kg(7 ppm) working standard, take 700 µl of the 1000 ppm Stock solution and dilute
up to 100 mL.
To prepare 10000 µg/Kg(10 ppm) working standard, take 1000 µl of the 1000 ppm Stock solution and
dilute up to 100 mL.
The diluted aqueous standards for low and medium concentration (ppb range) can be prepared from the
1 and 5 ppm solution.
To prepare 5 µg/Kg(5ppb) 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(20ppb) working standard, take 2 mL of the 1 ppm solution and dilute up to 100 mL.
To prepare 30 µg/Kg(30ppb) 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.
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To prepare 100µg/Kg(100ppb) working standard, take 2mL of the 5ppm solution and dilute up to 100 mL.
To prepare 200µg/Kg (200ppb) working standard, take 4mL of the 5ppm solution and dilute up to 100mL.
To prepare 500µg/Kg(150ppb) working standard, take 5mL of the 10ppm solution and dilute up to 100
mL.
There are three standard different working range responses that the instrument may be calibrated on:
- The low range is 0- 10 ng Hg
- The medium range is 10-20 ng Hg
- The high range is 20-1000 ng Hg.
The working standards solution must be freshly prepared before every calibration.
8.3 BLANKS
8.3.1 How to get good blanks
Good blanks are obtained using dedicated quartz boats, a good carrier gas and good conditions of each
component and environment where the unit is installed: the replacement of one or more components or old
components could impact blank values. Fork, catalyst, amalgamator, etc… must be cleaned and
conditioned, if new, or replaced, whenever the required instrumental blank value is not achieved.
These values are intended for empty boats, running Standard Method without any sample or standard.
Acceptable blank value depends on the minimum value to quantify.
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Here below are reported the most common reasons of high blanks
CAUSE REMEDY
Contamination of sample boat holder by organic With the help of a sand paper remove the film
samples. accumulated on the ceramic head of the sample
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The QC program is prepared and overseen by the Laboratory Manager, the QC Chemist, and the Scientific
Advisor.
Method blanks are analyzed to confirm With each sample batch or one per 20
Blanks
the absence of contamination. samples(5%) for each matrix
Duplicates are analyzed to check With each sample batch or one per 20
Duplicates
method and stability and performance samples(5%) for each matrix
Sample matrix effects are checked by
spiking samples with a known amount of
With each sample batch or one per 20
Matrix Spikes standard and subsequently measuring
samples(5%) for each matrix
the recovery of the analyte in the
sample.
Certified standards are used as control
Standard Reference
samples to check the method For each matrix
Materials
performance in the matrix.
All values shall be documented, maintained, and available for easy reference and inspection.
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ACCEPTANCE LIMITS. Control limits shall be listed on charts for different matrices. Acceptable criteria
should be set through the use of historical analyses. In the absence of historical data this limit should be
set for:
Control standards for checking the stability of the instrument calibration at ±10% of their true value. To do
this use two reference standards with range of interest ( see point 3.5 of EPA Method 7473).
For each batch of samples processed, a method blank must be carried out. A method blank is prepared by
using a volume or weight of reagent water at the volume or weight specified in the preparation method. In
absence of project specifics, if the blank is less than 10% of the lowest sample concentration for each
analyte, then the method blank would be considered acceptable (see point 9.4 of EPA Method 7473).
For each batch of samples processed, a duplicate is carried out to check stability and performance. The
acceptable criteria in absence of historical analysis is set at ±10%.
Matrix Spike/Matrix Spike duplicated at ± 20% of the spiked for precision and ≤ 20 relative percent
difference. After determination of historical data, 20% must still be the limit of maximum deviation for both
percent recovery and relative percent difference to express acceptability (see point 9.3 of EPA Method
7473).
The changes that take place in a sample are either chemical or biological. In the former case, certain
changes occur in the chemical structure of the constituents that are a function of physical conditions. Metal
cations may precipitate as hydroxides or form complexes with other constituents; cations or anions may
change valence states under certain reducing or oxidizing conditions; other constituents may dissolve or
volatilize (Hg) with the passage of time. Metal cations may also adsorb onto surfaces (glass, plastic, quartz,
etc.), such as, iron and lead.
Biological changes taking place in a sample may change the valence of an element or a radical. Soluble
constituents may be converted to organically bound materials in cell structures, or cell lysis may result in
release of cellular material into solution. The well-known nitrogen and phosphorus cycles are examples of
biological influence on sample composition.
Therefore, as a general rule, it is best to analyse the samples as soon as possible after collection. This is
especially true when the analyte concentration is expected to be in the low range.
Quartz: for liquid and semi-liquid samples, reusable approx 2000 times. Quartz boats can be cleaned:
- using the DMA-80 with the Clean Procedure method
- using a Muffle at 900°C per 10 minutes.
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It is also possible to pre-wash them using a ultrasonic water bath with deionized water.
In case the DMA-80 is working with the Milestone Air Compressor flow, it is possible to clean the boats
overnight in order to be completely ready and Hg free tomorrow.
The system is clean, when you’ll have a value of ABS with boat and water lower than 0,0040. It’s
important to have this value to calibrate but also to analyze samples with low mercury content (0,1 ppb).
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- Always use quartz boat for calibration and for low level analysis.
- Clean the boats in muffle (900°C for 10’ for the quartz boats, 600°C for 10’ for the metal boats) or
directly into the instrument with the standard method.
- Perform some BV method before working to ensure the right cleanliness of the instrument. The
acceptance of the BV values strongly depends on the user working range. Typically has to be
lower than 0.0030 ABS in the cell 1.
- If the working range start from 0,1 ng, the following cleaning has to be performed: run clean boats
plus 0.3 ml of water with the Water Cleaning method
- The expected ABS value has to be lower than 0.0040 in cell 0
3. CALIBRATION
DMA-80 evo comes with a factory calibration from 0,1 ng up to 1000 ng. A customized calibration is
suggested to match specific needs and working range.
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If this goal is not achieved with your samples, the cause may be one or more of the following :
Causes Resolution
Solid/liquid sample contaminated Repeat the test with new sample.
Solid sample with non-homogeneous Mix well and increase the sample amount.
distribution of Hg
Solid/liquid sample with low amount of Mix well solid and use pre-concentration step up to
Hg satisfactory results.
Old standard liquid solution/liquid Prepare fresh standard liquid solution.
solution with precipitated due to not
enough acid.
Weight/volume not accurate Check balance calibration / Pipette calibration.
DMA-80 unit is not cleaned after high Cleaning procedure up to blank absorbance < 0.0030
concentration or “over range”
Process parameter too short Increase: waiting (purge) time/ drying time/ decomposition
time.
Leakage of oxygen through the
silicone joint between
cuvette/amalgamator, Repair as shown in the “Maintenance of
amalgamator/catalyst or catalyst/flange The DMA-80” manual.
Oxygen contaminated Use only O2, 99.50% pure for research, or replace supplier.
The catalyst and or/and amalgamator Change catalyst and amalgamator and repeat calibration.
exhaust
Environment contaminated Cleaning procedure up to blank absorbance < 0.0010, if
after this the contamination persists, transfer unit to another
laboratory.
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Food 100 mg
containing oil
Longer drying step allows a pre-combustion of sample before rapid decomposition at high temperature,
reducing the exothermic reaction.
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8.6.4 How to work with liquid samples in auto-sampler mode, in order to avoid
evaporation.
With liquid samples, metal boats can be used only in single mode, to minimize the loss of mercury due to
chemical interaction between the acid matrix and the metal boat.
Milestone offers boats made of quartz, a completely inert material, to solve this problem and ensure good
results.
The following two experiments illustrate the problem, and the effectiveness of this solution.
TEST 1:
Metal boat effect with lost of mercury
6 samples of 105 µg/Kg (10ng) have been prepared and run by auto-sampler mode.
After starting the autosampler, the waiting metal sample boats react chemically with the liquid standard,
and consequently there is a loss of mercury.
TEST 2:
Quartz boats (without lost of mercury).
5 samples of 105 µg/Kg (10ng) have been prepared and run in auto-sampler mode.
All the runs have been successfully done without evaporation, good stability and reproducibility, RSD: 0.85
We recommend using the quartz boats for all liquid samples.
With the quartz boats, is possible to optimize the recovery (<1 ng absolute) of Hg without a pre-
concentration step.
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Note: before to start the procedure, install properly the catalyst tube. Connect the oxygen/air flow, switch
ON the DMA-80 unit and do not install the amalgamator tube at once, but leave the catalyst free for about
20 minutes to prevent condensation and impurities in the amalgam trap and cells.
After, that connect the amalgamator and be sure the DMA80 unit is ready to operate (alignment of
actuators, stability of Oxygen/air flow). For more details see operator manual.
Blank
3°-4°-5° 1g (indicative
(without sample value)
boat)
Common white
6° flour + distilled 300mg+50mg
H2O
Blank
7°-8° 1g (indicative
(without sample value)
boat)
Common white
9° flour + distilled 300mg+50mg
H2O
Blank
10° 1g (indicative
(without sample value)
boat)
(1) The
analysis method “Initialization” is saved on the USB stick supplied with control terminal or PC
software package
- Replicate the procedure up to get the last blank absorbance < 0.0030 in cell 1 or satisfied for your
working range.
-After conditioning a stability test is required. In a quartz sample boats, repeat 5 times: a fresh aqueous
standard of 100ppb, the RSD must be < 3%.
For this evaluation it is not important the recovery but only the DMA stability so the previous calibration
curve can be used.
- If the stability test is in according to the specs, please proceed making new calibration (see operator
manual) otherwise repeat the conditioning procedure until getting satisfactory results.
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You can set a password expiration. At the end of its lifetime, the software will ask to change the old
password with a new one.
Activating this function, the software immediately asks to change the old password with a new one.
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Anyway, with Login mode set on Standard, the software also ask you a password every time you switch
on the machine to access to software.
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Here below a table with more details concerning the privileges according with the login type.
Open and
Choose a Open and Create Open and Create
modify an Create
method file modify an and save a modify an and save a
existing and save a
from the existing new existing new
method file new
quick calibration calibration measurem measurem
from the method file
panel file file ent file ent file
memory
User
Manager
Administra
tor
Create a Change
Create a
Run a new Create a Data and
new Access to Access to
measurem Administra new User Time
Manager the trail Settings
ent tor account parameter
account
account s
User
Manager
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Administra
tor
Reset of
Data files
LAN Change of amalgama Service
settings
network Software absorbanc tor and tests and Balance
and LIMS
configurati updating e limit of catalyst adjustment setup
configurati
on cells counter s
on
cycles
User
Manager
Administra
tor
There are two additional login levels that cannot be modified by the Administrator
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DMA software
Ref. # Description
(rev. 03-D and following)
Persons who use closed systems to create, modify, maintain, or transmit electronic records
shall employ procedures and controls designed to ensure the authenticity, integrity, and,
11.10 when appropriate, the confidentiality of electronic records, and to ensure that the signer
cannot readily repudiate the signed record as not genuine. Such procedures and controls
shall include the following:
Validation of systems to ensure The organization of the user must accomplish a validation
accuracy, reliability, consistent of the DMA software.
intended performance, and the Documents such as, IQ, OQ, PQ, SV protocols are
ability to discern invalid or available. An official Validation package will be available
altered records. soon.
11.10
(a) The DMA software controls the correctness of the data on
the basis of check sums. Invalid records cannot be
opened nor used. Executed cycles are not open files and
cannot be altered while any other modification of
electronic records is registered and fully traceable in the
Trail section.
The ability to generate accurate Records generated by DMA software are automatically
and complete copies of records saved on the memory support (terminal, USB stick or LAN
in both human readable and network folder) according to the type of data and to the
electronic form suitable for software configuration.
inspection, review, and copying All data records can be viewed, copied and printed with
11.10
by the agency. Persons should the DMA software and then exported on standard file
(b)
contact the agency if there are formats like .pdf, .csv, xls.
any questions regarding the
ability of the agency to perform
such review and copying of the
electronic records.
Protection of records to enable The data records can always be viewed and printed, with
their accurate and ready the same software version that was used for their
retrieval throughout the records recording.
retention Additionally, records can be exported as standard file
formats like .pdf, .xls, .csv.
11.10
Automatic records saving features are available on DMA
(c)
software.
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appropriate, the validity of the terminal from the user can be done via touch screen,
source of data input or keyboard or mouse.
operational instruction.
The software recognizes the validity of the entered data
and immediately notifies the user in case of invalidity or
the same.
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continuous period of controlled owner will require the collaboration of two or more
system access, each signing individuals.
shall be executed using all of the This target can be achieved also through DMA software
electronic signature thanks to the obligation of change the password at the first
components. access of a new account and to the periodic expiration
(configurable) of the passwords.
(2) Be used only by their
genuine owners; and
(b) N/A
(3) Be administered and Electronic signatures on the system are not based upon
executed to ensure that biometrics
attempted use of an individual's
electronic signature by anyone
other than its genuine owner
requires collaboration of two or
more individuals.
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immediate and urgent manner (e) The organization of the user is responsible for
any attempts at their implementing procedures for the periodic testing of the
unauthorized use to the system USB memory sticks if these are used for the identification
security unit, and, as of the user (option).
appropriate, to organizational
management.
(e) Initial and periodic testing of
devices, such as tokens or
cards, that bear or generate
identification code or password
information to ensure that they
function properly and have not
been altered in an unauthorized
manner.
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Manufacturer/Supplier:
Milestone S.r.l.
Via Fatebenefratelli, 1/5
I-24010 Sorisole (BG)
Tel.: 0039 035.575837
Fax: 0039 035.575498
The information mentioned below must be intended, in case of break of the external tube.
3. Ecological information
· Toxicity: n. a.
· Information about elimination (persistence and degradability): n. a.
· Bioaccumulative potential: n. a.
· Mobility in soil: n. a.
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. Methods and materials for containment and cleaning up: Pick up and arrange disposal without
creating dust. Sweep up and shovel. Keep in suitable, closed containers for disposal.
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Manufacturer/Supplier:
Milestone S.r.l.
Via Fatebenefratelli, 1/5
I-24010 Sorisole (BG)
Tel.: 0039 035.575837
Fax: 0039 035.575498
The information mentioned below must be intended, in case of break of the external quartz tube.
3. Ecological information
· Toxicity: n. a.
· Information about elimination (persistence and degradability): n. a.
· Bioaccumulative potential: n. a.
· Mobility in soil: n. a.
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Manufacturer/Supplier:
Milestone S.r.l.
Via Fatebenefratelli, 1/5
I-24010 Sorisole (BG)
Tel.: 0039 035.575837
Fax: 0039 035.575498
Further information obtainable from:
email: application@milestonesrl.com
Information in case of emergency:
MILESTONE S.R.L. – tel: 0039 035 573857
From 8:30 to 12:30 and 13:30 to 17:30, from Monday to Friday (Time zone: ITALY/ROME)
2. Hazards identification
Hazard description:
Xi Irritant
The product has to be labelled due to the calculation procedure of the "General Classification
guideline for Substances of the EU", DIR. 67/548/EC, in the latest valid version.
Irritating to eyes and respiratory system.
Warning
H315 Causes skin irritation
H319 Causes serious eye irritation.
H335 May cause respiratory irritation.
Prevention:
P261 Avoid breathing dust/fume/gas/mist/vapours/spray.
Response:
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P305+P351+P338 IF IN EYES: Rinse cautiously with water for several minutes. Remove contact
lenses, if present and easy to do. Continue rinsing.
3. Composition/information on ingredients
Formula: SiO2
Chemical characterization:
Name CAS No. Description EINECS Number: Index number:
Molecular sieve 63231-69-6 - -
4. First-aid measures
· After inhalation: If breathed in, move person into fresh air. If not breathing, give artificial respiration.
· After skin contact: Wash off with soap and plenty of water.
· After eye contact: Flush eyes with water as a precaution.
· After swallowing: Never give anything by mouth to an unconscious person. Rinse mouth with water.
5. Fire-fighting measures
· Suitable extinguishing agents: Use water spray, alcohol-resistant foam, dry chemical or carbon
dioxide.
. Special protective equipment for fire-fighters: Wear self contained breathing apparatus for fire
fighting, if necessary.
Appearance
Form Powder
Molecular weight: 60.08 g/mol
pH-value (g/l) n. a.
Safety Data
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Explosions limits
Lower n. a.
Higher n. a.
Water solubility n. a.
. Skin corrosion/irritation: n. a.
. Serious eye damage/eye irritation: n. a.
. Respiratory or skin sensitization: n. a.
. Germ cell mutagenicity: n. a.
. Carcinogenicity
IARC: No component of this product present at levels greater than or equal to 0.1% is identified as
probable, possible or confirmed human carcinogen by IARC.
. Reproductive toxicity: n. a.
. Specific target organ toxicity – single exposure (Global Harmonized System):
Inhalation – May cause respiratory irritation-
. Specific target organ toxicity – repeated exposure (Global Harmonized System):
No data available
. Aspiration hazard: n. a.
. Signs and Symptoms of Exposure: To the best of our knowledge, the chemical, physical, and
toxicological properties have not been thoroughly investigated.
. Additional Information: RTECS: n. a.
Xi Irritant
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Manufacturer/Supplier:
Milestone S.r.l.
Via Fatebenefratelli, 1/5
I-24010 Sorisole (BG)
Tel.: 0039 035.575837
Fax: 0039 035.575498
email: application@milestonesrl.com
Information in case of emergency:
MILESTONE S.R.L. – tel: 0039 035 573857
From 8:30 to 12:30 and 13:30 to 17:30, from Monday to Friday (Time zone: ITALY/ROME)
2. Hazards identification
Classification of substance or mixture
. According to regulation (EC) No. 1272/2008:
Not a hazardous substance or mixture according to Regulation (EC) No. 1272/2008.
. The product has to be labelled due to the calculation procedure of the "General Classification
guideline for Substances of the EU", DIR. 67/548/EC, in the latest valid version.
This substance is not classified as dangerous, according to Directive 67/548/EC.
. Other hazard:
None
3. Composition/information on ingredients
Synonims: Alumina
Formula: Al2O3
4. First-aid measures
· After inhalation: If breathed in, move person into fresh air. If not breathing, give artificial respiration.
· After skin contact: Wash off with soap and plenty of water.
· After eye contact: Flush eyes with water as a precaution.
· After swallowing: Never give anything by mouth to an unconscious person. Rinse mouth with water.
· Most important symptoms and effects, both acute and delayed: Cough, chest pain, difficult in
breathing, gastrointestinal disturbance..
· Indication of any immediate medical attention and special treatment needed: n. a.
5. Fire-fighting measures
· Suitable extinguishing agents: Use extinguishing measures that are appropriate to local
circumstances and the surrounding environment.
. Special hazards caused by the substance, its products of combustion or resulting gases:
Aluminum Oxide.
· Advice for firefighters: Wear self contained breathing apparatus for fire fighting if necessary.
· Further information: Do not use halocarbon extinguishers. The product itself does not burn.
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·Exposure controls
Appropriate engineering controls: general industrial hygiene practice
Skin protection:
Protective gloves
Handle with gloves. Gloves must be inspected prior to use. Use proper glove removal technique (without
touching glove’s outer face) to avoid skin contact with this product. Dispose of contaminated gloves after
use in accordance with applicable laws and good laboratory practices. Wash and dry hands.
Material of gloves:
The selected protective gloves have to satisfy the specification of EU Directives 89/686/EEC and the
standard EN 374 derived from it.
Immersion protection Splash protection
Material: Nitrile rubber Material: Nitrile rubber
Minimum layer thickness: 0,11 mm Minimum layer thickness: 0,11 mm
If used in solution, or mixed with other substances, and under conditions which differ from EN 374,
contact the supplier of the CE approved gloves. This recommendation is advisory only and must be
evaluated by an Industrial Hygienist familiar with the specific situation of anticipated use by our
customers. It should not be construed as offering an approval for any specific use scenario.
Body protection: Choose body protection in relation to its type, to the concentration and amount of
dangerous substances, and to the specific workplace. The type of protective equipment must be selected
according to the concentration and amount of the dangerous substance at the specific workplace.
Respiratory protection: Respiratory protection is not required. Where protection from nuisance levels
of dusts are desired, use type N95 (US) or type P1 (EN 143) dust masks. Use respirators and
components tested and approved under appropriate government standards such as NIOSH (US) or CEN
(EU).
Appearance
Form Solid
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Odour n. a
Odour Threshold n. a
Molecular weight: 101.96 g/mol
pH-value (g/l) 9.4 – 10.1 at 20°C
Change in condition
Melting point (Melting range) 2040°C – lit.
Boiling point (Boiling range) 2980°C
Flash point n. a.
Ignition temperature n. a.
Flammability (solid, gas) n. a.
Explosions limits
Lower n. a.
Higher n. a.
IARC: No component of this product present at levels greater than or equal to 0.1% is identified as
probable, possible or confirmed human carcinogen by IARC.
. Reproductive toxicity: n. a.
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. Signs and Symptoms of Exposure: Cough, chest pain, difficulty in breathing, gastrointestinal
disturbance.
. Additional Information: RTECS: BD1200000
email: application@milestonesrl.com
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Manufacturer/Supplier:
Milestone S.r.l.
Via Fatebenefratelli, 1/5
I-24010 Sorisole (BG)
Tel.: 0039 035.575837
Fax: 0039 035.575498
email: application@milestonesrl.com
Information in case of emergency:
MILESTONE S.R.L. – tel: 0039 035 573857
From 8:30 to 12:30 and 13:30 to 17:30, from Monday to Friday (Time zone: ITALY/ROME)
2. Hazards identification
Classification of substance or mixture
. The product has to be labelled due to the calculation procedure of the "General Classification
guideline for Substances of the EU", DIR. 67/548/EC, in the latest valid version.
This substance is not classified as dangerous, according to Directive 67/548/EC.
. Other hazard:
None
3. Composition/information on ingredients
. Surface
Surface and inner part in carbon and ceramic.
. Mixture
N. a.
4. First-aid measures
No episodes of damage to personnel operating the product. However, when necessary, follow the below
general measures.
· After inhalation: If breathed in, move person into fresh air. If not breathing, give artificial respiration
and consult a doctor.
· After skin and eye contact: Wash off with soap and plenty of water. If irritation persists, consult a
doctor.
· After swallowing: Never give anything by mouth to an unconscious person. Consult a doctor. Induce
vomit, only if instructed by the doctor.
· Most important symptoms and effects, both acute and delayed: No episodes of damage to health
are attributable to the product.
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· Indication of any immediate medical attention and special treatment needed: Follow doctor’s
advice.
5. Fire-fighting measures
· Suitable extinguishing agents: Tools of Absorbance are the traditional one: carbon dioxide, foam,
dust and water spry.
· Unsuitable extinguishing agents: no one in particular.
. Special hazards caused by the substance, its products of combustion or resulting gases: Avoid
breathing combustion products (carbon oxides, toxic pyrolysis products, etc.)
· Advice for fire-fighters: Cool containers with water to avoid product decomposition and substances
development potentially hazardous to health. Always wear full fire protection. Collect fire-fighting water
that must not be discharged into sewers. Dispose of contaminated water used for Absorbance.
Equipment: peaked helmet, fireproof clothing, gloves, a mask with facemask covering the entire operator
face or a self-protector for large amount of smoke.
Appearance
Form Solid pieces
Colour Black
Odour odourless
pH-value (g/l) n. a.
Viscosity n. a.
Explosive properties n. a.
Oxidizing properties n. a.
Water solubility n. a.
Density (at 20°C) 0.6g/cm3
Speed evaporation n. a.
Melting > 1300°C
Boiling Point n. a.
Temperature of ignition n. a.
Lower Flammable limit n. a.
Upper Flammable limit n. a.
Other information
VOC (Directive 1999/13/CE) 0
VOC (Volatile Carbon) 0
The product has been classified and marked in according to the requirements of Regulation (EC) No.
1907/2006.
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AdsoQUICK
Indication of Manufacturer/Supplier
Manufacturer/Supplier: MLS GmbH
Auenweg 37 / 88299 Leutkirch
Tel.: 07561/9818-0 / Telefax: 07561/9818-12 / Email: applikation@mls-mikrowellen.de
Information contact:
MLS Application laboratory applikation@mls-mikrowellen.de
Hazardous/Dangerous Ingredients
None of the ingredients classified in RL 67/548/EWG
3. Possible Hazard
Special hazard/danger for humans and environment:
None
4. First Aid
General information:
No special measures are required.
Inhalation:
After inhalation of large quantities of dust, take the person out in the open and fresh air.
Skin contact:
Wash with soap and flush thoroughly with much water.
Eye contact:
Flush immediately the eye, keeping the eyelid open, under flowing water for several minutes.
Swallowing:
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Drink water.
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Special dangers of the material or its preparation, related burning products or developing
gases:
Carbon dust can be released at temperature above 300°C into the oxygen-containing
atmosphere. In case of glowing or fire, carbon monoxide and dioxide will be generated.
Environmental protection:
No special measures are required.
Cleaning/collecting procedure:
Remove/wipe mechanically.
Handling
Recommendations for safe handling:
In case of dust provide good ventilation/exhaust of the working room/site.
Storage
Requisites for stock room and containers:
Store the containers always tight sealed. Store dry.
Storage recommendations:
Do not store together with the following materials:
- Medicines, food, feed
- Infectious, radioactive and explosive materials
- Fire hazard materials of the Group according to TRGS 515.
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Respiratory protection:
In case of dust use protection, for example P1 half filtering masks.
Form: solid
Colour: grey/black
Smell: odourless
Note:
01)
with appropriate handling and storage
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Note:
01)
with appropriate handling and storage
Materials to be avoided:
None
Others: None
13. Disposal
Product/ Preparation
The use and handling of the product is possible in the economic cycle provided all
impurities/contaminations are eliminated. Can be disposed of according to local regulations, for
example taken to a suitable combustion plant.
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National regulations
Notes on restrictions of use:
None
189
MILESTONE
Milestone Srl - via Fatebenefratelli 1/5 - 24010 Sorisole (BG) - Italy
Phone +39 035 573857 - Fax +39 035 575498
H E L P I N G
e-mail: analytical@milestonesrl.com - web: www.milestonesrl.com
C H E M I S T S