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MILESTONE

H E L P I N G
C H E M I S T S

DMA-80

Operator Manual
MA213
Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Thank you for selecting our DMA-80 system.


We are sure that you will be completely satisfied with the performance of this
new unit entering your laboratory. We invite you to read carefully this user
manual and to keep it in reach for convenient and fast consulting. The person
who will be using this unit should have received an appropriate training from
a Milestone trained technician. For any possible clarification or any request
for assistance please contact either our Representative in your country:

or Milestone at the following address:


Milestone Srl
Via Fatebenefratelli, 1/5
24010 Sorisole (BG) Italy
Tel +39 035 573857
Fax +39 035 575498
Website www.milestonesrl.com
E-mail analytical@milestonesrl.com

Publication date (gg/mm/aaaa) 24/09/2021

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

1 SAFETY RULES ...................................................... 6


1.1 General Information .............................................................. 6
1.2 Safety rules for start-up ........................................................ 6
1.3 Safety rules in operations ..................................................... 6
1.4 Safety in service operations .................................................. 7
1.5 No manipulation on the unit allowed ..................................... 7
1.6 Parts replacement ................................................................ 7
1.7 Customer support ................................................................. 7
1.8 Other hints ............................................................................ 7
1.8.1 Safety of operation............................................................................... 7
1.9 Cleaning instructions ............................................................ 8
1.10 Maintenance instructions ...................................................... 8
1.10.1 Fuses................................................................................................. 8

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

3 DMA-80 EVO GENERAL INFORMATION............. 34


3.1 Technical data .................................................................... 34
3.2 DMA-80 EVO front view...................................................... 36
3.3 DMA-80 EVO back view ..................................................... 37
3.4 DMA-80 EVO internal view ................................................. 37

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

4 DMA-80 EVO MILESTONE CONNECT ................. 39


5 SOFTWARE........................................................... 43
5.1 Login................................................................................... 43
5.2 Operation according to FDA-21 CFR Part 11...................... 43
5.3 Login according to CFR 11 ................................................. 44
5.4 Methods release by signature ............................................. 44
5.5 Data file storage and signature ........................................... 44
5.6 Data safety of measurement file in CFR Part 11 ................. 45
5.7 Documentation - erroneous login - ...................................... 45
5.8 Password expiration ........................................................... 45
5.9 Program end/Logout ........................................................... 45
5.10 General Operations Tips..................................................... 46
5.10.1 Popup menu .................................................................................... 46
5.10.2 File opening, closing, saving and deleting ........................................ 46
5.10.3 Main page DMA-80 EVO Software................................................... 49
5.10.4 Print ................................................................................................. 51
5.10.5 Automatic printout in PDF ................................................................ 53
5.10.6 Import CSV files ............................................................................... 53
5.10.7 How to import a CSV file .................................................................. 53
5.10.8 Importing CSV formatted data into Excel ......................................... 55
5.11 Method page....................................................................... 57
5.11.1 Methods-Parameters ....................................................................... 58
5.11.2 Create a new method....................................................................... 60
5.11.3 Methods management ..................................................................... 63
5.12 Calibration page ................................................................. 64
5.12.1 Calibration- Parameters ................................................................... 64
5.12.2 Create a new calibration .................................................................. 69
5.12.3 How to prepare aqueous standard solutions .................................... 76
5.12.4 Reference page ............................................................................... 77
5.13 Measure page..................................................................... 81
5.13.1 Measurement- Parameters .............................................................. 81
5.13.2 Create a new measurement ............................................................. 91
5.14 System page....................................................................... 93
5.14.1 System- Parameters ........................................................................ 94
5.15 Settings .............................................................................. 96
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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

5.15.1 Settings-Access ............................................................................... 96


5.15.2 Settings-Settings............................................................................ 101
5.16 Service ............................................................................. 120
5.16.1 Service-Autosampler...................................................................... 121
5.16.2 Service-Detector ............................................................................ 124
5.16.3 Service-Test .................................................................................. 126

6 MAINTENANCE ................................................... 128


6.1 Consumables replacement ............................................... 128
6.2 Water discharge from the outlet connection ...................... 137
6.3 Sample boat cleaning ....................................................... 138

7 SOFTWARE MESSAGE AND INQUIRIES .......... 139


7.1 Status message ................................................................ 139
7.2 Analytical error messages ................................................ 139
7.3 Technical error messages ................................................ 142

8 TIPS & TECHNIQUES ......................................... 144


8.1 GENERAL RULES ........................................................... 144
8.2 CALIBRATION.................................................................. 144
8.2.1 How to make a standard liquid solution. ........................................... 144
8.2.2 How to store a liquid standard solution ............................................ 145
8.2.3 How to store standard reference materials....................................... 145
8.3 BLANKS ........................................................................... 145
8.3.1 How to get good blanks ................................................................... 145
8.3.2 Cleaning methods ............................................................................ 146
8.3.3 Tips for a good cleaning................................................................... 146
8.4 QUALITY CONTROL ........................................................ 147
8.4.1 How to set up a QC program ........................................................... 147
8.4.2 Acceptance Criteria for QC Samples ............................................... 147
8.5 SAMPLE PROCESSING .................................................. 148
8.5.1 Recommendations for preservation of samples ............................... 148
8.5.2 How to clean the DMA-80 boats ...................................................... 148
8.5.3 How to work at ultratrace levels ....................................................... 149
8.5.4 How to work at standard levels (ppb/ppm) ....................................... 151
8.5.5 How to increase the reproducibility .................................................. 153

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

8.6 HOW TO WORK WITH UNKNOWN SAMPLES ............... 153


8.6.1 How to work with non-homogeneous samples ................................. 153
8.6.2 How to increase the recovery of difficult samples............................. 154
8.6.3 How to work with difficult matrices ................................................... 154
8.6.4 How to work with liquid samples in auto-sampler mode, in order to
avoid evaporation. ....................................................................................... 155
8.7 CONDITIONING PROCEDURE FOR NEW CATALYST
TUBE 156
8.7.1 Introduction ...................................................................................... 156

9 21CFR-11 DMA SOFTWARE .............................. 157


9.1 Activation of the 21CFR part 11 ........................................ 157
9.2 Overview of user profiles and access levels ..................... 158
9.3 Declaration of compliance “DMA software” with FDA-21CFR
part 11 ......................................................................................... 161

10 SAFETY DATA SHEET ....................................... 167

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

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.

Information = indicates important information/recommendations for the user.

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.

1.2 Safety rules for start-up


 First start-up of the system must exclusively be carried out by authorized and trained service
engineers appointed by Milestone.

1.3 Safety rules in operations


 The DMA-80 EVO device is intended exclusively to measure the mercury content in the
samples. Any different use or any other use is to be considered as improper. The manufacturer
liability will not cover any resulting damages. The risk is exclusively borne by the operator/user.
 The unit must only be operated within the power limits set forth by the technical specifications.
 The unit must be operated exclusively by specially trained people.
 All electrical parts must always be protected from wet and humidity.
 The unit must be kept clean.
 Note all the safety instructions indicated in this manual, that can be treated as accident
prevention regulations, and the general accepted rules to work with devices.

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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.

1.4 Safety in service operations


 In case of failure or damage of the unit, the intervention of an authorized and trained service
operator must be requested. The unit shall not be used until successful repair is completed.
In case of leakages or defective unit, disconnect immediately the power supply. Inside the unit
there are components with a lethal high voltage (above 1000V).
 Service can only be carried out by authorized and trained service engineers of the company
MLS-Milestone.
 Do not operate the unit if a minimum doubt exists about its trouble-free operation and good
functioning.
 Works on the electrical and electronic components of the system must be carried out exclusively
by specialized electrical/electronic engineers.
 Before every repair – service – installation always make sure that the unit is disconnected from
the power supply line and cannot involuntarily be switched on.

1.5 No manipulation on the unit allowed


 Constructive changes/modifications of the unit and its accessories are forbidden.

1.6 Parts replacement


 In order to ensure the correct functioning of the unit and in the same time the user safety, please
employ only Milestone original spare parts.

1.7 Customer support


 The documents received with the shipment should include also the warranty and the service
report.
 Once performed the installation, please send us the warranty sheet completely filled-in by fax
or e-mail.
 When service call is necessary, please send the completely filled-in service report, with
precise error description.
Before any reparation, (meeting with service), the unit must be cleaned. In case the pollution
endangers the health of our collaborator or restricts the correct functioning of the unit, Milestone
reserves the right to invoice additional costs for the cleaning. Please specify also the used
chemicals in the service report.
 For any additional info, feel free to contact Milestone representative in your country or the
following address: analytical@milestonesrl.com

1.8 Other hints


1.8.1 Safety of operation
 The unit shall not be installed in an explosive, corrosive or conductive atmosphere (dust,
vapours, gas).
 The system must be operated with the original power supply cable supplied together with the
unit.

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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.

1.9 Cleaning instructions


 Before any maintenance on the unit and before cleaning it, disconnect the power supply cable.
 Keep the air inlet and outlet openings always free from pollution.
 You can clean the surfaces of the unit with a wet cloth, warm water and a mild household
cleaning detergent, and then wipe dry. Never use solvents.

1.10 Maintenance instructions


 The user shall simply carry out the maintenance instructions described in this user manual.
For all other operations on the unit, a special trained service engineer should be consulted.
 Before opening the device, disconnect it from power and oxygen supply.
 When opening the cover or removing some components, some live parts remain exposed,
while the unit is connected to the power supply.
 Maintenance works on the unit, while it is under tension, shall not be carried out. If such
activities are unavoidable, they must be carried out by a specialist who is familiar with the
hazards involved.
 Any kind of damages to the protective ground inside or outside the unit can endanger the
operator.

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

The following fuses shall be replaced only by service:

Heating coil: 1 x 16 A fuse, 250 V (on motherboard)

Electronics: 1 x 2 A fuse, 250 V (on motherboard)

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

2 INSTALLATION
2.1 Unpacking and checking list

When unpacking, verify that all parts received


correspond to the packing list.

Carefully cut the tie down straps, as shown in the


next picture. Cut through the packing tape and
open the carton from the top.

Remove the smaller boxes located in the upper


part of the main box and set them aside. They
contain accessories, which will be needed during
the installation of the DMA-80 EVO. Lift the main
box up off of the pallet to expose and facilitate
removal of the DMA-80 EVO.

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Check the information paper which contain some


advices to follow before starting the unit

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.

2.1.1 DMA-80 EVO STANDARD EQUIPMENT


- Option 1

Terminal 660

Usb stick

Pen

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Pen holder

RJ45 cable

- Option 2

Pc software package

Software and drivers installed on CD-ROM and


USB stick

Gateway

USB cable

RJ45 cable

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

- Additional parts included in both options

Power cord

Gas carrier tube

Autosampler plate

Mercury trap

Quartz boats pack

Blue accessories box

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

2.2 CATALYST AND AMALGAMATOR INSTALLATION


Before working with DMA- components,wear:
-Mask anti dust FPP3;
-Disposables gloves
-Protection for the shoes.

For safety reason the catalyst and amalgamator are packed separately to the DMA-80 unit so they need
to be installed as first step.

Attention = HOT components

Put the machine on the working table and with


the help of key, open the housing cover.

Release the remaining pressure from the gas


connector on the back side of the unit

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Pull back the horizontal pneumatic actuator in


order to free the catalyst flange.

Loosen the red screw on the spectrophotometer


plate and move far the spectrophotometer arm.

Loosen the two red screws on the slide rails.

It is not necessary to remove completely the


screws

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Pull out the catalyst oven block.

Open the catalyst flange with an hexagonal


screw (you can use the one included in the blue
accessories case).

Take the catalyst marked with label with red line


from the blue accessories case.
This catalyst was used during the QC protocol in
our factory, so we suggest to install it as first.

Wait to connect the amalgamator.


The new catalyst needs to be drained

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Check this catalyst tube has the o-ring at 5 mm


from the catalyst inlet and the silicon joint on the
tip.
Otherwise, take them from the blue accessories
case.

Install the tube, paying attention that it meet


difficulties or friction during the entrance.

Once the new tube has been installed, close the


flange, and push in the catalyst oven block.

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Tightening the red screws.

Check the proper alignment of the horizontal


pneumatic actuator with the catalyst flange.
In case of bad alignment, adjust the two screws
of the cylinder by turning a bit them. The cylinder
will move a bit right or left.

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Connect the gas carrier. See chapter 2.4

Switch on the machine (see chapter 2.3 on how


to set the voltage and connect the controller)

Wait about 20 minutes before to connect the


amalgamator.

During this time you should see the condensate


(bubble of water) gets out from the catalyst tube.

The catalyst is draining.

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

FLOW

After 20 minutes, take the amalgamator marked


with the label with red line from the blue
accessories case.
Connect the amalgamator in the right position.
The amalgamator tube has a little groove on the
glass to indicate the direction of the flow.
The amalgamator must be installed with the
groove close to the cuvette in order to avoid that
FLOW
the material inside moves out during the flow
passage.

Connect the cuvette.

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Place the red cover taking it from the blue


accessories case

Perform the catalyst initialization procedure to


prepare the catalyst tube to the analysis. See
chapter 8.7

2.3 DMA-80 EVO SETUP

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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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

2.3.1 Voltage setting

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.

2.3.1.1 Fuses replacement

- The below procedure has to be made for DMA-80 EVO units before SN 20032968

The voltage selector is included in the fuse holder


Press the two tabs on the sides of the fuse holder of
the plug and take it out

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

The spare fuses are in a bag in the blue accessories


case of the unit.
Select the proper voltage by turning the holding part
of one fuse.

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

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

Press the two tabs on the sides of the fuse holder of


the plug and take it out

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

The spare fuses are in a bag in the blue accessories


case of the unit.

Install the fuse holder into the plug and press it until
the tabs engage

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

2.3.1.2 Change of connections on the voltage transformer (only for DMA-80 EVO units from SN
20032968)

Open the lid of the unit in order to access to the


transformer.

In case of DMA-80 EVO unit you can remove


completely the chassis for a better handling.

If necessary, pull the catalyst oven forward.

Change the wiring of the primary connection of the


transformer.
- for 220-240 VAC: connect the white wire to the
230V terminal
- for 110-120 VAC: connect the white wire to the
115V terminal

Push the oven back and cover the unit

Connect the power cord to the unit, turn on the


machine and check the function.
220-240 VAC 110-120 VAC

2.3.1.3 Indication of set voltage

- The below procedure has to be made for DMA-80 EVO units before SN 20032968

Mark the set voltage somewhere close to the


power socket or on the main label of the
instrument.

- The below procedure has to be made for DMA-80 EVO units from SN 20032968

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Inside the fuse bag, the labels to indicate the


voltage set, are present.
Put the label which indicates the voltage set on
the existing one, next to the power socket

2.3.2 DMA connection with Terminal 660

Place the Terminal beside the DMA-80 EVO unit,


as shown below. A bench space of approximately
150 cm by 70 cm is required with approximately 15
cm of space on all side to ensure movement of air.

Plug-in the serial cable into Terminal (DEVICE


PORT).

Plug-in the end of serial cable into DMA-80 EVO


unit.
Both connections are fine

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Introduce the USB key into the reader port located.

The USB-key must be introduced with


label facing the user.

Plug the power cord into DMA-80 EVO unit.

Do not pass the power cord over


sharp edges.
The unit must be connected to a
grounded, single phase line with 220-
230 VAC output. Provided with the
unit is a grounded power cord with a
Shuko plug. It is important that the
ground pin on the receptacle be
attached to the neutral/common at the
breaker box.

2.3.3 DMA 80 EVO connection with PC

Minimum PC configuration required for DMA-80


EVO

CPU: Pentium III 800


RAM: 256 MB
Space on the disc: 20 MB
No. 1 USB port
No. 1 CD reader
Operative system: all version of Windows from
XP to 10

Printer: all compatible printers with Windows.

Plug the RJ45 cable into DMA-80 EVO unit.

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Plug the other end of the serial cable into the RJ45
interface port of the Gateway.

Plug the USB cable (B) into the Gateway port.

Plug the end of USB cable (A) into the PC USB


port.

When connecting the DMA-80 EVO to the USB of


the PC (via Gateway) for the first time, the
following announcement might be shown: FOUND
NEW HARDWARE.

If the following message appears, then you have to


install the driver.
Driver installation may be different according to the
Windows update version. If you see the Welcome
page, no connection to Windows Update is
required. Then click on “Proceed”.

NOTE: Windows 10 should automatically install the


driver without requesting any user action. If this
does not happen, install the driver you can find in
the folder CDM v2.08.30 WHQL Certified.

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

1. Insert the CD or the USB into the CD-


drive.
2. Select “Install software from a list or “other
source”.
3. Confirm with “Proceed”.

4. Select “Find other drivers (floppy, CD)”.


5. Confirm with “Proceed”.
The drivers have now been installed.
Depending on the Windows version: if you have to
enter the listing of the drivers files, go through the
CD to the (CD-Drive):/CDM 2.08.30 WHQL
Certified.

6. Insert the CD or USB into the CD-drive.


7. Go to the CD-List/USB and copy the
application file: DmaOnPc.exe on a
folder/list of your choice on your hard
disk.(usually we recommend to copy the
software directly on desktop)
This action is necessary to keep further
steps saved avoiding repeating them again
once turned off and on the program.

8. Start the DmaOnPc.exe file on your hard


disk.
The starting menu of the software will be shown.
9. Open un the left upper corner the menu

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

10. Digit the serial number and the licence key


printed on the USB Gateway. Confirm with
OK.
11. After login by service code enter into Panel
Administr./ Access/Panel Control and
check the serial number and the valid
licence key.
12. Change the language of the software if you
want.
13. Confirm clicking on “save icon”.

Copy the contents of the CD-Rom DMA-80 EVO


under the C:\Documents

DMA-80 EVO folder contains the


original calibration, methods, and
data files.

Plug the power cord into DMA-80 EVO unit.

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Do not pass the power cord over


sharp edges.
The unit must be connected to a
grounded, single phase line with
220-240 VAC or 110-120 VAC
output. Provided with the unit is a
grounded power cord with a
Shuko plug. It is important that the
ground pin on the receptacle be
attached to the neutral/common at
the breaker box.

2.3.4 DMA safety switch


The DMA-80 EVO units are equipped with a safety switch that cuts the power when the lid is opened, to
avoid that the users may come into contact with electric live parts.

So, when operating the lid must be closed otherwise the heating element will be not supplied and an error
message will appear

2.4 Gas connection


The Oxygen or Air required for DMA-80 EVO working must be at “research” grade (O2 /Air purity >
99,95%) and must have a flow rate of approximately 160ml/minute (6-8 l/h) and an inlet pressure of 4 bar
(60 psig).

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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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Note: the connections are different if you use air or O2. The outlet connection must be suitable
to connect 6x4 Rilsan tube.

2.4.1 Oxygen tank

Connect the DMA-80 EVO unit to the O2 source


thanks to 6x4 Rilsan blue tube you can find in the
accessories box.

To avoid damages to the pressure regulator


diaphragm, open the tank valve and adjust the
pressure on the oxygen tank/air source from 0 to
4 bar.

Once the unti is switched ON the DMA-80 EVO


internal pressure is set to 3,1 bar.

2.4.2 Milestone Air compressor


Please refers to Milestone Air compressor User Manual

Take the air compressor from its box and place


it on the floor

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Provide a suitable space to


position the device and place it
on the floor. The unit requires
approx. 15 cm on each side to
allow adequate airflow.

Check that you have appropriate power supply


and that the main voltage corresponds with the
one shown on the plate fixed to the compressor.

Make sure that the outlet is closed by turning


the pressure regulator fully anti-clockwise,

then connect one end of the proper air tubing Ø


6/4 without male connector, present in the
accessories box of the DMA-80 unit.

Connect the other end with male connector to


the inlet of the DMA-80 unit.

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Before plugging the electrical cable into the


main supply, make sure that the ON/OFF switch
is turned to the ‘0’ (OFF) position.

Connect the air compressor to the main supply.

Switch on the main supply and turn the ON/OFF


switch to the ‘I’ (ON) position to start the motor
of the compressor.

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Set the outlet pressure about 4 bar (maximum 5


bar) with the pressure regulator by lifting the
knob and turning it clockwise to increase
pressure and anti-clockwise to decrease
pressure. Lock the regulator knob in place by
pushing down until it clicks.

Do not set an outlet pressure


over the tolerance limit (5 bar) of
the DMA-80 EVO unit because
this could cause failure of the
machine

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3 DMA-80 EVO GENERAL INFORMATION


3.1 Technical data
Operating principle
Sample thermal decomposition, amalgamation, atomic absorption with dual beam option

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 analysis time


 5 minutes: dual cell, tri cell with or without double beam option
 8-9 minutes: wide range

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

Maximum capability of sample boats


Solid and liquid: 1.5 g/ml. (sample weight/volume has to be in according with the application note)

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.

Specifications are subject to change without notice.

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3.2 DMA-80 EVO front view


An overview of the front side of the DMA-80 EVO is shown in the picture

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

LIGHT COLOUR MEANING

WHITE: The software is on Measurement pages and the unit is in standby


mode ready for the analysis

GREEN (flashing): The run (in case of measurement in single mode) or


sequence of runs (in case of automatic mode) has finished.

YELLOW (flashing): The software is on Measurement page and the unit is


in stand by mode waiting that some parameters have reached their working
values.

RED (flashing): The software is on Settings pages or the analysis has been
interrupted.

RED: The unit is running

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3.3 DMA-80 EVO back view


An overview of the back side of the DMA-80 EVO is shown in the picture

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

3.4 DMA-80 EVO internal view


Opening the housing of the DMA-80 EVO the overview of the internal of the DMA-80 EVO is shown in the
picture.
If you open the housing when the machine is on, the power supply is cut off thanks to a
protection switch that opens the circuit

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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4 DMA-80 EVO Milestone Connect


Milestone Connect is a website (www.milestoneconnect.com) where you can find information about your
own unit, application notes, scientific paper, user manuals, tips and techniques and everything else you
may need to improve the operations with your system.

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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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.

5.2 Operation according to FDA-21 CFR Part 11


When using T660 or T1660, the CFR-Part 11 can be activated by the Service by the setting „ USB key
and Password”. If you want to save a measurement file, there is the possibility of the signature, once
confirmed the file name.

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5.3 Login according to CFR 11


In CFR Part 11, the user logs in with a signed USB key and his password. The signature is displayed on
the screen. If there is no USB, the symbol flashes. If a USB without signature is used, the name of the
user is missing. Without a properly signed USB and a valid password, it’s not possible to work with the
unit.

5.4 Methods release by signature


In order to be in compliance with CFR Part 11, each method must be signed by the administrator before
the execution. It’s possible to use only signed method for the measurement. This also applies to the
Administrators. If a method of the sample tables is not signed, an appropriate message is displayed.

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.

5.5 Data file storage and signature


Measurement data files and methods can be signed. The signature of the methods can be carried out
only by the Administrator, since the user cannot store any method. Therefore the access to the signature
is denied to the user.
Data files, however, can be electronically signed by the user.
All the users with a signed USB key and a personal password can sign the measurement data files. It is
documented who processed the samples, in addition it can be signed by the same or another person. The
function is linked to the active storage of the run. It’s possible to store also without signature.
When signing, the function can be registered, i.e. „auditor“. Then press on the „pen“ symbol. The login is
displayed. Once introduced the right USB key, the right password can be entered.

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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.

5.6 Data safety of measurement file in CFR Part 11


Cancellation or overwriting on the USB key or B-server of measurement data file is not possible from the
program. If the data is deleted externally (also on a PC) from the media, this is not due to our
responsibility.
This does not apply to other files, such as calibration and methods. Methods can be i.e. deleted from the
administrator.

5.7 Documentation - erroneous login -


After three failed login attempts, this is documented in the trail.

5.8 Password expiration


On demand, the service can set a deadline for password expiration in the setup under Access/Users.

5.9 Program end/Logout


After storing the relevant data, the unit can be easily switched off. By switching off the unit, also the
terminal is switched off. When you switch on again the unit, a new login is necessary. If a user concludes

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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.

5.10 General Operations Tips


The following indications will help you navigating the software.

5.10.1 Popup menu


By pressing the arrow icon in the upper left corner, the popup menu is opened with the available functions
of the current page. The functions are different: files opening, saving, printing, importing CSV files, going
to settings and logout.

5.10.2 File opening, closing, saving and deleting


By the corresponding icons: “load“, “save“ and “print” in popup menu, you can load, save and print the
files.
According to the page, there are some tips to respect (indicated in the next chapters).
Remember:
 Measurement files are saved under Data Folder (.d80)
 Calibration files are saved under Calibration Folder (.c80)
 Method files are saved under Method Folder (.m80)

- FILE ORDERING: Files can be ordered according to the date or name.


In this way, it would be easier to find a file.

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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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5.10.2.1 USB storage on terminal 660

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.

5.10.2.2 Storage on the LAN connection

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

5.10.3 Main page DMA-80 EVO Software


After the login, the software operations pages will appear. There are different windows, all on the same
level. More details about the single pages are described in the next chapters.
You can move through the windows and select the different icons by touching the touch-screen or by the
mouse click.

Popup menu described in chapter 5.10.1

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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Direct link to Connect website only available with DMAonPC software

Some icons (generally used) are available in several menu points and they can be selected
from there.

5.10.3.1 Generally used icons

Here below a list of the most used icons.


Input field: Editable fields are marked with a triangle in the right corner. They
open at the moment of activation both by selection or input field.
Active tabs and pressed icons: Pressed tabs and icons are held with lighter
background and darker word/symbol (colors inverted). Grayed icons or tabs are
not available for the user or the type of unit.
Input or selection confirmation: The tick in the up right corner is used for
confirmation or acceptance of the input.
Quit a page: The arrow is generally located on the top left side and it is used to
quit the operations like storage, loading, keypad field.
It is also used to return to measurement page from the settings page. Pressing
this icon after changing some setting, it will be automatically saved.
If an input keypad field is open and you press the back arrow, then the
procedure is immediately quitted without saving.
Create a new file: Pressing it, the page is “cleaned”. It creates a new and empty
file. (Calibration and Measure pages). The file is deleted from the temporary
memory (but not from the external memory)
Delete a line: the selected line is deleted after confirmation (Calibration and
Measure pages)

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.

START: The unit is ready for measurement with no run ongoing.


After pressing, a new measurement is started, if a new sample has been
introduced.

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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.

INITIALIZATION: When this icon appears in place of START button, then


initialization of the system is required.

INITIALIZATION ON GOING: The external ring shows the progress of the


initialization.

5.10.3.2 Number and text input by touch-screen

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.

By tapping the print function, a preview will be opened.

Print function in
Measure page

Print icon in Settings


By pressing once again the print button, the selected file will be printed if a
printer is connected directly with terminal or PC.
PRINTER NOT AVAILABLE: If no printer is detected, the print icon is displayed
in brighter colour on the preview page.
By a double click of the icon, a list of printers compatible with your software
version will be displayed.
PDF FUNCTION: possibility to create a copy of the file in PDF format. By
pressing this icon the saving field will appear.

The administrator can specify in the setup under setting/files


(5.17.4) whether parallel to the measurement saving you want to
automatically save the PDF files.
PAGES TO BE PRINTED: Select a specific page to be printed. The selected
page will be shown in the preview. Other pages will not be printed.

The only specific page is printed if the MULTIPLE PRINTING function is disabled

MULTIPLE PRINTING: If selected, it allows to print all page regardless of you


selected in preview

LANDSCAPE FORMAT: If available, the page can be printed in landscape


format.
GRAPH PRINTING: Available only for Measure page. Only the name and graph
of the measurement will be printed. No other values.

GROUP PRINTING: groups of measurements previously selected in the


measure page can be printed

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5.10.5 Automatic printout in PDF

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.

5.10.6 Import CSV files


From DMA software rev. 03-C, 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
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.

CSV import layout

- 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.

5.10.7 How to import a CSV file

Open the CSV file you find on the USB key of


your terminal or PC software, on your PC.

Fill the available fields with the desired


information.

Save the file with the same format of the original


file .CSV
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In the software, be sure the function “CSV import”


in Settings/Data Files, is activated.

Only the “Service” access has the permission to


activate this function.

In the Measurement page of the DMA software,


open the drop down menu and click on “Import”
box.

Connect to terminal the USB where you saved the


CSV file previously filled, select and load it.

In the Measurement page, your file will appear.

Now , it is possible to save the file as a normal


data (.d80 format) and start the measurements.

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5.10.8 Importing CSV formatted data into Excel


Sometimes, it can happen that the original CSV file provided by Milestone meets some errors or it is
distorted when it is opened with Excel.
The below procedure allows to adjust the file in the correct format.

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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5.11 Method page


A user cannot create, modify, or remove methods. This right is reserved only to the
administrator.

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.

Initialization method: to be used for catalyst


tube conditioning or reactivation. (300mg of wheat
flour + 0,05ml of distilled water for boat)
It can be also used for safe cleaning of whole
instrument and all its components. (0,3ml of
distilled water for boat)

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Standard method: to be used for most of liquid


and solid samples

Clean procedure: to be used for cleaning boats

Boat holder cleaning: to be used after organic


samples if there is carry over effects by
accumulation of sample residues on the ceramic
plug of the boat holder (no boats)

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

Drying and decomposition parameters can be entered or modified also


graphically by selecting the position that must be entered new or modified. The
position will appear with purple background. Change the Temperature and the
Time by pulling the arrows into the desired position.
Time t can be entered in 10 seconds increments, and Temperature T in 10°C
increments.

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.

Purge time P: It is the time elapsing between the end of drying/decomposition


phase and the start of the Hg measurement (amalgamator heating). Purging
time is set and saved for each method (standard setting is 60 seconds).
During and after the decomposition, all pyrolysis gases are transported with the
oxygen flow from the catalyst to the amalgamator. Hg is trapped in the
amalgamator and all the other gases are flushed out from the system before Hg
is measured in the cuvette. Only in this way a matrix-free measurement can be
carried out.

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Amalgamator time H: It is the time required by the amalgamator heater to


completely release the Hg collected in the amalgamator tube. (Standard setting:
12 seconds)

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

As we see later, it is possible to set a different method for different measurement


lines. So even the amount unit can be different in the same list of
measurements.

5.11.2 Create a new method


A new method is opened based on a basic method.

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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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5.11.3 Methods management


The method to be used for the measurements can be selected directly in Method page, loading it, in case
you need to run a list of samples with the same method.

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

5.12 Calibration 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.

5.12.1 Calibration- Parameters

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

Selected point: when a point is selected, it will be in involved in the tracking of


the curve. If not, it will be shown but not involved in the tracking of the curve.

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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 )

Ng values: Values in “ng” of the calibration points

Abs values: Values of the absorbance (height of the peak) of the calibration
points

Deviation values from the calibration curve:


∆A: is the deviation of the absolute absorbance
∆A%: is the percentage deviation of the measured values
∆Hg[ng]: is the deviation in amount of mercury
∆Hg[%]:is the percentage deviation of amount of mercury

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.

Additional calibration points information: by clicking on any point of the


calibration point list, additional columns will be shown.
- remarks: you can add your comments for each calibration point
- Date: here it is reported date and time of each calibration point

Calibration curve: a line is drawn connecting the calibration points.


The x-Axis shows the Hg value, the y-Axis the absorbance (A). The resulting
formula and the coefficient of calibration determination are displayed.

Calibration points in the graph:


- blue colour: the point is selected from the list of calibration points and the curve
consider it in its track and calculation

- 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

Approximation method: the approximation method is calculated starting from


the mistakes (deviation) of the measurement values included in the calculation.
Closer to 1 the value is, better the calibration curve will be adapted to the
measured values. To be noted that the measurement values are not necessarily
correct. If a curve is analyzed with the function S-curve, the approximation
method is better, although the measurement results are not corrected by a
square analysis.

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- Undefined: use to deactivate a cell in case it is not necessary for analysis


purposes, or when there are not enough points or the distance between them is
not enough to draw linear or square
- Linear: usually it is recommended until ca.1ng (initial part of the curve). The
curves are leveled, especially in the upper range.
Linear Regression: minimum two points required

X ext  X blanc   0  X conc


- Square: default choice. This is optimal in case of full release of the working
range of a cuvette (adjustable by the administrator in the setup).
Square curve calculation: minimum three points required

X ext  X blanc   0  X conc   1   X conc 


2

- S-Curve: recommended only for particularly high number of calibration points.


Strong outliers should be deactivated.
S-Curve: minimum four points required

X ext  X blanc   0  X conc   1   X conc    2   X conc 


2 3

Actions to get Linear or Square function available:


a. reduce the absorbance limit of cell close to the last calibration point.
b. add further points in order to go close the limit of absorbance set.

Calibration cells: An individual calibration curve is provided for each of the


sequential cells. The first optional cell (cell 0) has an high sensitivity and
therefore is used to detect the Hg content in ultra-trace range (normally up to 3
ng (factory setting)), the second cell (cell 1) is used for the measurement of low
and medium Hg content (up to ca. 20 ng), the third one (cell 2) for the
measurement of high Hg content (up to 1500 ng)
In according with the instrument configuration, the available cells can be:
-two, in case of Dualcell system

- three, in case of Tricell system

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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5.12.2 Create a new calibration


Before using the Direct Mercury Analyzer for the first time, the instrument must be calibrated using
prepared Standard solutions of Hg or Standard Reference Materials (SRM or CRM). The instrument does
not have to be re-calibrated every time, but the calibration curve should be checked every morning prior
to analyse unknown samples. The instrument has to be recalibrated only if the calibration check results in
10% higher or 10% lower than expected recoveries.
The instrument has to be also recalibrated when any of the major components are replaced. For example,
calibration must be performed when the catalyst and/or the amalgamator are replaced, or when the
oxygen tank or gas regulator is changed.

The calibration may be performed using two different approaches:


A: Performing calibration using few standard solutions via different volumes: it is the standard method
also used in our QC. We suggest a sample volume of up to 0.3ml. Thus, four to five standards are
required to cover the full range of DMA work, with a volume from 0,02 ml up to 0,3 ml.
B: Perform calibration using the same volume but different standard solutions: it is the method we
suggest for low concentrations (less than 1 ng). If you need to calibrate this range, it is important to use
the same volume for each point (usually 0.3ml), so you need a standard for each point.
Of course, the risk of error in standard preparation is higher so you must pay high attention in the dilution
steps. But when working in linear regression at low concentrations, you do not need many points.

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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6. Go to Measure page and create a blank sheet

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)

The Automatic BV function should be disabled during the calibration procedure.


This because if no approx. method has been selected in calibration graph before the
Automatic BV run, the result of the Automatic BV run has not any reference curve to
be calculated.
The Automatic BV is not a calibration point, so the software sees it like a "normal
measurement", trying to calculate , based on the absorbance value, the absolute value

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)

Cell 0 Cell 1 Cell 2

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.

The maximum number of calibration points in a calibration curve allowed by the


software is 99

5.12.3 How to prepare aqueous standard solutions


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. 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.

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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

5.12.4 Reference page

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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5.12.4.1 Reference- Parameters

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

Reference table: list of reference samples reported automatically from the


Measure page once analyzed.

Number of reference sample: The reference samples are put in order of


execution

Date: execution date and time of reference sample

Ng values: Values in “ng” (absolute value of Hg) of the reference sample

Cal-Factor: value calculated by the “theoretical value” divided by “measured


value” of reference sample

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

Remarks: here operator comments are entered

σ: If more reference samples are selected, here the standard deviation is


calculated
m: here the average of Cal- Factor values is calculated. If only one reference
sample is selected, then here the value is reported. If no reference samples are
selected, the “m” value for Cal- Factor will be automatically set to “1.0000”

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

5.12.4.2 Reference measurements

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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1. Open a measuring file.

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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5.13 Measure page


After the login, the software skips directly into the page Measure/Sample. The last measuring file of the
current user is opened, if available.

Here it is possible to run unknown samples, insert the points for the calibration curve, run reference
samples and a lot of other actions.

5.13.1 Measurement- Parameters


Different sub-sections with different options and functions are available in Measure page:
Sample/Links/Signal and Result.
Some filed are not available in some sub-sections, therefore if you want to get them be sure that you are
in the right page.

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 Signal allows to view all parameters of the signals.

- 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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Samplename (available in all sub-sections): Field to enter the name of the


sample or the measurement line

Amount (available in sub-section “Sample” and “Results”): Field to enter the


weight of sample. It must be always different than zero when you run normal
measurements otherwise the software does not allow to start.
The unit of amount is set on the basis of unit chosen in your analysis method.

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

If balance is connected (to be configured in Settings page), whenever a record is


added, the balance screen will automatically open to allow entering the sample
weight. The symbol will slightly change, depending on the type of balance
connected.
- Standard balance

- Option GMU
Request to tare

Request to sample weighing

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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.

Direct download of weighing: in most of balance models, the


weight is constantly updated on the terminal. In the sample table,
touch the “Weight” icon to download the value into the active cell.
For other balances: touching the print button of the balance (see
appropriate manual of the balance) the weight is transferred on
the terminal and into the active cell.
Automatic taring: In most balance models the balance can be
tared directly from the termina

Stop: the balance screen is closed without loading the weight.

Automatic multiple measurement (n) (only available in sub-section “Sample”):


Here multiple measurements can be activated. The basic requirement is that a
new row is added and you work under automatic mode. In this last line (and only
there), the desired number can be input in the column “n”.

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.

Additional points to be noted:


- Only in the first line marked by “M” the calibration factor is displayed.
This applies also to all measurements.

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- If the line “M” of a group is assigned, automatically also each single


measurement of this group is assigned.
- During normal operations, it’s possible to create as many lines, until
there is still place on the turntable plate (thus max. 40).

State (available in sub-section “Sample”, “Links” and “Results”): Enter in the


menu to define the type of measurement.
- Normal measurement : it refers to a normal run of a sample with unknow Hg
concentration. To start, it is necessary to insert the amount of the sample and
choose a calibration curve and analysis method to which the measurement can
refer.
Otherwise the measurement can not start.

- Calibration: (a C is shown to the right of the status box ): It refers to a


calibration point measurement which will be entered in the calibration graph
indicated in the calibration file reported in the link page under Calibration
column.
It is also necessary to insert the amount of the sample, the Hg concentration
under column ug/Kg and choose the analysis method you want to use.

- Reference: (a R is shown to the right of the status box): It refers to the


reference measurement sample to check the correction factor of the curve.

- Blind value: (a B is shown to the right of the status box): It refers to an


instrument blank since no positions of the plate are considered. The steps can
be set in Settings page of the software (Settings/Blind values).
For automatic blank value measurements, use the method BV-Method.

In case no BV-Method is saved, the method saved in the setup under


setting/blank values will be used. If a file under the name BV-Method is stored,
this is marked by a blue flag and remains always in the method selection. The
administrator can therefore adapt the cleaning and blank value method
according to his need.
The “BV-Method” can be edited by the user and the default parameters can be
modified and overwritten.
This is also performed with automatic blank value measurements, when the
weight in the sample table is “0.0000”. The sample boat is not introduced in this
case..
If the sample is defined as blank value B in the status menu, the “BV-Method” is
automatically recalled under the methods.

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- Concentrate: a curly brace is shown to indicate the accumulation of samples


measured.
Only a defined maximum volume can be loaded into the sample boat. So, with
the Concentrate function, a large weighing (within the limits) can be distributed
and measured in several sample boats. When a red cross is displayed, it means
that the sample can be removed from the series.
The divided samples are sequentially processed and the accumulated Hg is
burnt and measured only with the last sub-sample. The result is thus determined
over the total originally weighted quantity and the collected Hg value.
Example:
1.Weigh all samples in sequence.
2.Mark the record which contains a sub-sample (sample 1.1).
3.Activate the Button. The sample under the one marked will be connected with
a brace- parenthesis to the marked sample (here sample 1.2).
4.Now select the connected sample (here sample 1.2) and activate the function.
The next sample (here sample 1.3) will also be connected to the first two
samples. Following groups with partial samples can be introduced in the same
way.

The State display also indicates the current status:

Sample has not been weighed yet or the amount has not been
confirmed yet

Sample weighed or amount confirmed

Sample in stand-by (automatic sample mode processing) up for


measurement

Sample was removed during the processing run. Sample is removed


from list once the measurement(s) are completed.

Measurement sample ongoing

Measurement interrupted or invalid

Sample measured succesfully

At the end of measurement, a new option is available if you click on State field:

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- Reprocess: It is possible to re-process a sample after the analysis using a


different calibration.
First we need to activate the feature in the Settings page (please, contact your
local distributor to activate this feature).

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.

The software will recalculate the concentration according to the selected


calibration curve.

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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Settings/Analysis, the absorbance is calculated like height of the peak of signal


or area.

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.

ng (only available in sub-section “Result”): Absolute quantity of Hg in the sample


(calculated from active calibration).

Hg concentration (only available in sub-section “Result”): Concentration of Hg


in the sample (calculated from Hg quantity and sample weight).
Different unit are available, but the results will be calculated and shown
considering the unit of sample amount.

Cal-Factor (only available in sub-section “Result”) : here is reported the value


calculated by the “theoretical value” divided by “measured value” of reference
sample. See chapter 5.12.4

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.

Group (only available in sub-section “Result”): The measurement lines can be


ordered in 8 different groups for statistic calculation

Statistics: (only available in sub-section “Result”):here some calculations of the


selected measurement lines are reported
m: here the Hg concentration average value is calculated.
n

 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

Remarks (only available in sub-section “Sample”): here it is possible to write


comments related to the measurement line

Reference Cal.file and Method (only available in sub-section “Links”): By clicking


the corresponding field, the calibration files and methods recently used will be
displayed, so that the desired file can be selected.

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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.

Temperature and signal profile (only available in sub-section “Signal”): Selecting


this icon it is possible to evaluate the trend of all temperature and signal of the
measurement. It is also possible on live, during the running of a sample.

— T1: Ashing oven temperature


— T2: Catalyst temperature
— T3: Cuvette temperature
— Hg: Detector signal(s)
— Absorbance[A]: Absorbance signal
Temperature and signal profile (only available in sub-section “Signal”):
Deselecting this icon it is possible to evaluate the absorbance signal.

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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.

ZOOM-IN AND ZOOM-OUT


Touch the magnification icon to zoom-in on the height of the peak used for
evaluation.
Additional possibility: 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.
By the magnifying glass, the graph is maximum displayed.

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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Analysis time (only available in sub-section “Signal”): After the start, an


estimation of the total time is displayed.
- Total time: in case of automatic measurement of several samples, it is the total
time of all samples.
- Sample Time: indicates the run-off time of the total measurement.

Measurements under simple mode (available in sub-sections “Sample”,


“Links”, “Result”): Each sample is measured individually, and it has to be
manually started.
If Simple Mode is activated and a sample is added, the number over the
selected record will be taken, alternatively the sample can be selected (from pos.
1 to 40), as in this operating mode each sample can be measured individually..
After measurement, the next position of the sample plate, if available, is driven
into load position.

Measurement under automatic mode (available in sub-sections “Sample”,


“Links”, “Result”): 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.
If Automatic Sample Processing is activated and a sample is added, the upper
number increases; the next not occupied number is used, since in this mode the
samples are automatically successively processed. Each position may be
occupied only once. If a position is doubly occupied, no measurement can be
started, and the following error message is displayed:

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.

5.13.2 Create a new measurement


A new measurement can be created by an empty page and new file or it can be added to a list of samples
already measured.
Here it is reported the basic procedure to create a new measurement line:
1. Add a new measurement line

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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)

4. Choose the type (State) of measurement desired.

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5. Go to “Link” page and choose the Calibration file and method to use like reference.

6. Save the file and press Start

5.14 System page


In this page it is possible to check the status of the system in real time. Also it is possible to start the
blank value programs.

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5.14.1 System- Parameters

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.

The spectrometer is calibrated every measurement short before heating of the


amalgamator. In addition, the shutter for measuring the 0% intensity is closed for
short time. After opening of the shutter, the 100% intensity is measured.

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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Amalgamator furnace: the temperature of the amalgamator is not displayed


because no sensor is present. The heating is supplied by the electronic mother
board following proper steps of dedicated times and powers.
Purpose of the amalgamator coil is to keep the amalgamator tube at the stand-
by temperature of 170°C/150°C and then to quickly heat it up to 850°C. The first
temperature is necessary to avoid water condensation and retain of organic
residues in the amalgamator tube; the higher temperature is necessary to
release at the same time the mercury previously “trapped” in the amalgamator.

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.

BV function: pressing this icon, the corresponding furnace will be heated.


- BV furnace 3 Amalgamator: used to clean the amalgamator. The cleaning is
automatically registered in the sample list and documented.
- BV furnace 1 Combustion: used to start a blank value measurement. The purity
of the system is tested, without using any boat. The cleaning is automatically
registered in the sample list and documented.
The used method is “BV-Method”. Any method can be identified by this name.
The best would be to define the standard method as “BV-Method”. Alternatively,
it will be used a setup method.

Autosampler: here, the position of pneumatic cylinders and autosampler plate


is shown. Pressing these different icons, it is possible to move the cylinders and
the autosampler plate.

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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Language: Different languages are available for the software

Beep: enables or disables the sound of software

Touch calibration: in case of terminal, this function allows to make the calibration
of touch screen

Brightness: adjust the brightness of the screen (for terminal only)

Date/Time: possibility to adjust Date and Time

Software information

Floppy: saves all settings changes

Printer: print all settings

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

Users: list of users name

New user: a new user can be added

User settings: here it is possible to change the parameter of the selected user

User deleting: the user selected can be eliminated.

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:

Insert the IP address dedicated for your T660

Insert the Subnet mask of your network

Insert the standard gateway of your network

Insert the DNS server of your network

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

Press APPLY to confirm all the setting.

The terminal will automatically restart

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SERVER Terminal 660

5.15.1.4 Trail

For more details see chapter 5.15.2.5

All: here all actions on the software are reported

System: here all settings changes are reported

Access: here all Login and Logout to software are reported

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Errors: here all software error messages are reported

Application: here all operations on measurement files are reported

Time: date and time of the action are reported

Changes: short description of the action is reported

Filter: field to fast find a key word

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)

Signal filtering: Eliminates the interferences on the peak shape

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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5.15.2.3 Blind values

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.

5.15.2.5 Data files

Save of data after one measurement: if activated, the data is saved everytime
after one measurement

Directory Recycled: With this option it is possible to activate a waste basket.


When deleting a file – if not already available – a folder named “Recycled” is
created on the Flash Card. The file will be stored there before the final
cancellation.

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.

1) How to import a CSV file

Open the CSV file you find on the


USB key of your terminal or PC
software, on your PC.

Fill the available fields with the


desired information.
Save the file with the same format of
the original file .CSV

In the software, be sure the function


“CSV import” in Settings/Data Files, is
activated.
Only the “Service” access has the
permission to activate this function.

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In the Measurement page of the DMA


software, open the drop down menu
and click on “Import” box.

Connect to terminal the USB where


you saved the CSV file previously
filled, select and load it.

In the Measurement page, your file


will appear.
Now, it is possible to save the file as
a normal data (.d80 format) and start
the measurements.

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2) Importing a CSV formatted data into Excell


Sometimes, it can be happen that the original CSV file provided by Milestone
meets some errors or it is formatted wrong when it is opened with Excel.
The below procedure allows to adjust the file in the correct format.
1. Download and save the CSV Milestone file to 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 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.

Support of LIMS: Select this option, if an external LIMS system is connected to


the unit. You can use different options for saving excel files.

Configuration of trail: here it is possible to set different levels of trail. This is


possible only with Service login:
- Standard: the software saves a trace of all setting changes and device errors in
the history trail tables.
- Standard + Applications: the software saves a trace of all setting/applications
(calibration, method and measurements) changes and device errors in the
history trail tables.
- Standard + Application + Confirmation: the software saves a trace of settings
and application (calibrations, methods and measurements) changes and error
devices in the history trail table asking you everytime with a message the reason
of that action
Default path: here you can choose the saving path of history trail

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5.15.2.6 Signaling

Signal error: if enabled, a sound is emitted by the controller after an error


message

Signal termination: if enabled, a sound is emitted by the controller after the


analysis is completed

Sound volume and duration: you can choose the volume and time of the sound

5.15.2.7 Maintenance

Exchange of amalgamator: A software message will inform the user that it is


time to replace the amalgamator when the currently cycles have reached the set
limit (5000).
The limit value should be decided on basis of application since the lifetime of
amalgamator strictly depends by it.

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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.

Turning back, the heating elements will start to work again.

5.15.2.8 Equipment

Additional sample disk: It is possible to add an addition disc to the instrument


once the first one is completed. If activated, this function allows to prepare a list
of 80 sample (40+40) and add the additional plate when all sample of the first
plate have been measured. The software will inform the user when it is the time
to change the plate.

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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.

P/N TER6477. The picture is purely indicative

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PIN CONNECTIONS

RJ45 connector PINS 9 pins RS232 male connector PINS

2, orange wire 2

6, green wire 3

5, white blue wire 5

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.

5.15.2.9.1 Sartorius balance mod. BCE224i-1S configuration

- DMA software parameters (bold parameters are proper for BCE224i-1S model)

Manufacturer of balance: It is possible to select among: Sartorius, Precisa, Kern


and Others (options available starting from DMA-80 software rev. 02-E) in
according with model of balance connected

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

Baudrate: Number of distinct symbol changes (signalling events) made to the


transmission medium per second (you can choose among: 300, 600, 1200,
2400, 4800, 9600, 19200)

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)

Unit of weight: it is possible to choose different unit of weight

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- BCE224i-1S parameters (Highlighted parameters are proper for the communication with DMA software)

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Note: the settings must be the same on balance and 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

Sample numbering: If a sequence of measurements contains a number like


unique or last letter, then, it is possible to create a list of consecutive number or
keep the same number for all measurements.
- Always: if you add measurements lines from one measurement with last or
unique letter in the sample name, the sample names will have the consecutive
numbers.

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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.

Standard weight/Standard volume: A standard weight or volume is used


automatically like default for new samples.

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.

If not, then proceed with the next steps:

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

It must be stable at around 50mV ± 10mV.

- the Gain is the signal of the detector when the lamp is ON

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.

The corrected signal is:


%detector Hg / %reference * 100%
Where:
- % detector is the % of light on the measuring detector (back to smaller cell). Blue line
- % reference is the % of light on the reference detector (double beam detector). Viole line
- Corrected signal is the signal used for final peak detection in order to have a more stable baseline.
Yellow line

Example of baseline correction with variation of the % light

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.

Before working with DMA- components,wear:


-Mask anti dust FPP3;
-Disposables gloves
-Protection for the shoes.

6.1 Consumables replacement

Attention = HOT components

Switch off the machine and open the housing


cover.

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Close the oxygen tank or switch off the Air


compressor. In this last case, discharge the
pressure from the device)

Disconnect the gas carrier tube from the back


side of the machine and release the remaining
pressure from the connector.

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Pull back the horizontal pneumatic actuator in


order to free the catalyst flange.

Remove the amalgamator red cover

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Loosen the red screw on the spectrophotometer


plate and disconnect the amalgamator tube from
the spout of the cuvette, by moving far the
spectrophotometer arm.

Loosen the two red screws on the slide rails.

It is not necessary to remove completely the


screws

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Pull out the catalyst oven block.

Open the catalyst flange with an hexagonal


screw.

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Remove the catalyst and amalgamator.

You should remove the two parts separately


because the two silicon joints on the amalgamator
tube will not allow the amalgamator to pass
through the coil.

In come case it is necessary to cut the coil


between amalgamator and catalyst tube.

Install a new catalyst tube with a new o-ring


placed 5mm from the catalyst inlet, and a new
silicon joint placed on the tip.

Wait to connect the amalgamator.

The new catalyst needs to be drained

Once the new tube has been installed, close the


flange, and push in the catalyst oven block.

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Tightening the red screws.

Check the proper alignment of the horizontal


pneumatic actuator with the catalyst flange.
In case of bad alignment, adjust the two screws of
the cylinder by turning a bit them. The cylinder will
move a bit right or left.

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Connect the gas carrier and open the oxygen


tank/ switch off the compressor

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Switch on the machine and wait about 20 minutes


before to connect the amalgamator.

During this time you should see the condensate


(bubble of water) gets out from the catalyst tube.

The catalyst is draining.

FLOW

After 20 minutes, connect the amalgamator in the


right position.
The amalgamator tube has a little groove on the
glass to indicate the direction of the flow.
The amalgamator must be installed with the
groove close to the cuvette in order to avoid that
the material inside moves out during the flow
FLOW
passage.

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Connect the cuvette.

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

6.2 Water discharge from the outlet connection


On the outlet block of the DMA unit where the mercury trap is connected it is possible to have
accumulation of water.
It is generated by the condensation of the samples especially the ones with high water content.
It is recommended to keep the block free from water in order to avoid its passage through the outlet tube
and mercury trap.
Daily or weekly, according to the use of the instrument open the PP adapter lid and with the help of a
towel, clean block.

It is recommended to replace the mercury trap after 1 year from the installation

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6.3 Sample boat cleaning

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.

Nickel boats 0,5ml sold Quartz boats 1,5ml


in pack of 40 pcs sold in pack of 10 pcs

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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7 SOFTWARE MESSAGE AND INQUIRIES


7.1 Status message
In the System page of the software there is the status line of the unit current status.

ERROR MESSAGE EXPLANATION


DMA_NO_ERROR The is in standby mode and it is ready for measurements

DMA_MEASURE_IN Measurement is under process


_PROGRESS

DMA_ERROR The system detected a malfunctioning and the measurement can not start

7.2 Analytical error messages


Here a list of main error messages which might occur during measurements
ERROR MESSAGE EXPLANATION/SOLUTION
Add a calibration for such samples not yet
measured under measurement/link.

Insert sample amount for one or more samples in


the measurement list.

Add a method under measurement/link.

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CFR Part 11 is activated and one of the methods


is not signed. Please replace such method with a
new signed one.

Sample boats can be measured only once. The


software prevents possible double occupancy. If
needed, the position can be changed after the
start by the sample marked with the hourglass.

Add a valid calibration under measurement/link. At


least one cuvette must be analysed.
Alternative: measure calibration points.

When starting a measurement for calibration or


quality control (reference), the reference value
must be introduced.
In case of blank value, input the value 0.

A maximum of 99 points can be considered for the


calibration. Please create a new calibration or
delete old points.
Deactivation is not enough.

The heating coils are not properly heating or the


temperature is out of standard working range.
There could be problems in the heating element
but also temporary interruption of communication
or the lid of the unit has been opened and the
230V circuit cut.

Setting of the peak monitoring have noted a too


early or too late growth. This can occur i.e. in case
of leak.

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The pneumatic actuator are not in their starting


position. From system page you can move them

With automatic storage, after the creation of a


new sample list, this must be saved.

The detector signal has not reached its starting


value before peak detection. This could be caused
by excessive sample reaction, contamination of
the cuvette or electrical problem of
spectrophotometer components.
In case of excessive reaction of the sample, try to
reduce the amount and use a longer and gentler
analysis method.
- Normal sample reaction

- Excessive sample reaction

The detector voltage is not able to return to its


starting value

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7.3 Technical error messages


ERROR MESSAGE EXPLANATION/SOLUTION
There is not enough gas pressure to pneumatic
section and actuators

Check eventual obstructions and start the unit.


Check the pneumatic arm position.
In case you cannot find any obstruction, please
contact the service.

Catalyst should be replaced because it reached


the limit of cycles

Please test the connection to the network, for


example whether the LAN cable is plug in
correctly.

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8 Tips & techniques


8.1 GENERAL RULES
Before starting to work with the unit, it is necessary to eliminate any contamination coming from
environmental dust or from the samples.
Before each use, a cleaning procedure is always recommended for the metal boats - in the DMA-80 or in
a muffle - and for laboratory tools such as spatula, balance plate, tweezers, etc.
It is particularly important to follow these recommendations when working at low concentrations of Hg.

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.

8.2.2 How to store a liquid standard solution


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.
Do not leave the solution bottles open on the bench and at the end store them into a fridge at 5-10°C

8.2.3 How to store standard reference materials


Standard reference material must be stored in its original tightly sealed bottle away from sunlight, humidity,
and intense sources of radiation. Before each use, the standard should be thoroughly mixed by rotating the
bottle before sampling.
If the determined value of the QC solution differs from the specs of known value, the standard could be
discarded. The value may differ if the catalyst is exhausted.

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.

Indicatively, the instrumental blank is considered good if the absorbance value is


- < or = to 0,0030 in cell 1 for most of applications
- < or = to 0,0015 in cell 0 when working at low Hg levels (ultratrace)

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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8.3.2 Cleaning methods


Different cleaning methods are recommended in according with the purpose. The below method are
saved on the USB stick of the control terminal or PC software package.

Boat Holder cleaning: to be used after organic samples if there is


carry over effects by accumulation of sample residues on the
ceramic plug of the boat holder (run this method without boats on
autosampler plate)

Clean procedure: to be used for cleaning boats (the boats should


be empty without any residue of previous sample inside. If present,
remove it with a spatula)

Clean water: to be used for safe cleaning of whole instrument and


all its components. (0,3ml of distilled water for boat)

Initialization: to be used for catalyst tube conditioning or


reactivation. But even in case of very high contamination of system.
(300mg of flour + 0,05ml of distilled water for boat)

Blind Value (BV): to be used for fast cleaning of the instrument,


directly from “State” column of measure page. (run this method
without boats on autosampler plate)

8.3.3 Tips for a good cleaning


- Boats can also be cleaned in muffle oven (900°C for 10’ for quartz boats, 600°C for 10’ for metal boats)
- Before sample measurement is better to use first Clean water method and then Clean procedure
method just for checking the value of instrumental blank
- If we just want to clean the device between samples, use Clean water method if the samples have
medium or high Hg concentration. Clean procedure method could be enough for samples with low Hg
concentration.
- The use of HCL 2% v/v for cleaning should be limited to cases with carry over effects or whenever the
required instrumental blank value is not achieved with the other methods or in case of acidified samples

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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boat holder. Then run Boat holder cleaning


method. Repeat the test if necessary.
Contamination of sample boats Clean the boats as explained in the dedicated
chapter of this manual. If the contamination grade
is very high and it can not be removed, then replace
the boats.
Measurement of critical or unknow samples with Clean catalyst and amalgamator tube using Clean
very high Hg content or generating big black fumes water or Initialization method. Several runs could
be necessary.
If the blanks are still high, then replace catalyst and
amalgamator.
If after that the contamination is still present, then
it could have involved the cuvette: In this case
contact Milestone technician for a cleaning of the
cells.
Contamination from environment or gas carrier Move the machine in another room or eliminate the
cause of contamination (if possible).
Change gas bottle or in case of air compressor
check the filters.

8.4 QUALITY CONTROL


8.4.1 How to set up a QC program

The QC program is prepared and overseen by the Laboratory Manager, the QC Chemist, and the Scientific
Advisor.

QC protocol Procedure Frequency


The stability of the instrument calibration
is checked during the run by analysis of
Control Standards Checked every 10 samples
the control standards.

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.

8.4.2 Acceptance Criteria for QC Samples

For more details refer to EPA method 7473.

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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).

8.5 SAMPLE PROCESSING


8.5.1 Recommendations for preservation of samples
Full preservation of samples—domestic sewage, industrial wastes, natural waters, etc.—is a practical
impossibility. Regardless of the nature of the sample, complete stability for every constituent can never be
achieved. At best, preservation techniques can only retard the chemical and biological changes that
inevitably continue after the sample is removed from the parent source.

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.

8.5.2 How to clean the DMA-80 boats


Nickel: for solid samples , reusable approx 1000 times. Nickel boats can be cleaned:
- using the DMA-80 with the Clean Procedure method
- using a Muffle at 600°C per 10minutes.

NOTE: Only Hot temperature in order to clean out the Hg!

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.

8.5.3 How to work at ultratrace levels


The purpose of this SOP is calibration from 0 to 1 ng, to work at 0.1 ppb. In order to achieve such low
level, the instrument and the operator need to use some additional care. The SOP report some specific
tips to achieve the desired results.
1. INITIAL INSTRUMENT SETUP:
Prior to start any test, the system must be stable and clean. At these levels it’s important to use only
quartz boats, both for the calibration and samples. While for standard applications, the blanks absorbance
is below 0.0030 in Cell 1, this is not enough for ultra-trace analysis.
- The ABS value of instrumental blanks must be lower than 0.0015 in Cell 0. The instrumental Blank
means run empty boat with our standard method without any sample or standard.
- The first level for ultra-trace calibration is done using the sample boat with 0.5 mL of water and 4% of
HCl.
2. HOW DO WE GET A GOOD BLANK FOR ULTRA-TRACE ANALYSIS?
Below are reported the main parameters that can impact the blanks value
- Dedicated quartz boats. Old boats or boats used for higher Hg range are not suitable for these analyses
and its calibration.
- Good carrier gas. The gas could also impact the blanks.
- Check the parts. Replacement of one or more components or old components could impact blank
values. Fork, catalyst, amalgamator, etc… must be conditioned, if new or replaced, whenever the
required Instrumental blank value (0.0015) is not achieved.
Before starting the calibration or the analysis, we advise you to perform at least 3 tests with clean boats
plus 0.3 ml of water. The method you need to use for these runs is the "Water Cleaning Method" (750°C
for 3 minutes).

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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2. CALIBRATION FOR ULTRATRACE LEVEL 0,1 ppb


Below is reported the procedure to calibrate the system a ultratrace level. Calibration has to begin with a
blank and at least one point lower than 0,1 ppb.
In order to maintain a good linearity of the calibration, we reduce the working range of the cell 0 to 1 ng.
The ultra-trace calibration has to be prepared as follow:
- Prepare fresh standard solutions according to the customer working range. It is recommended to only
use daily prepared standards in glass flask, perfectly cleaned. We suggest using a Standard Stock
solution with a concentration lower than 1000 ppm, such as 10 ppm, to avoid a lot of dilutions.
- Standards have to be stabilized with HCl (2% v/v), in order to avoid mercury evaporation. Use ultrapure
grade HCl.
- Always use 0.3 mL of standard. The use of 0.3 mL instead of 0.1 mL volume to enhance the data
reproducibility
- The first calibration point has to be a real blank with the same volume (0.3 mL) and matrix (water with
2% v/v of HCl) used for all the other points of the calibration. The ABS value of the first calibration point
must be less than 0,0040 in cell 0.
- Perform at least two replicates for each standard
- Calibrate up to 1 ng and then activate the Ultra-trace function

3. PRACTICAL EXAMPLE OF ULTRATRACE CALIBRATION


Below is reported an example of ultra-trace calibration. The target of this calibration is to provide a curve
suitable to analyze samples with a mercury level from 0.1 ppb.
In this specific example we have made 4 standards from 0.0125 ng up to 0.5 ng, each of them in triplicate
in order to show the reproducibility and the stability of the system at that range. We use 0.3 ml both for
standards and QC test. Once the last point of the calibration is done. Activate the Ultra-trace function.
These are the results we got:

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8.5.4 How to work at standard levels (ppb/ppm)


The aim of this SOP is to provide practical guides to use the DMA-80 evo in our standard working range.
DMA 80 evo is capable to operate both at trace and high levels but in order to achieve such low levels,
the instrument and the operator need to use some additional care.
1. INITIAL INSTRUMENT SETUP
Our standard calibration allows to work at values above 0.1 ng. Nevertheless, to begin the calibration
and work at low levels, the system must be stable and clean. It’s important to have a good calibration and
quality check in the real working range required (for example 1 ng to 100 ng). First of all, it is suggested to
analyze samples with homogeneous mercury content. For example, when the system is clean, it is
advisable to run all the water and low concentration samples and then the samples with a high
concentration of mercury. After that, start the cleaning procedure overnight to get a clean instrument for
the next day, if it is required to work again at low concentrations.
As the blank values lead to non-optimal reproducibility and accuracy at low level, see below how to
achieve good blank values.

2. HOW DO WE GET A GOOD BLANK FOR ROUTINE ANALYSIS?

- 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.

The calibration has to be prepared using the following guidelines:


- Prepare fresh standard solutions according to the working range. For new calibration it is safer to
prepare always new standards.
- Standards have to be stabilized with HCl (2% v/v), in order to avoid mercury evaporation.
- The first calibration point has to be a real blank with the same amount and matrix (water with 2%
v/v of HCl) used for all the other points of the calibration.
- Perform two replicates for each standard
- We suggest a 100 ul of standard for each concentration, especially for low mercury levels. For
higher levels the volume could be reduced.
The calibration has a long lifetime, anyway it is suggested to test it routinely with an external standard
(liquid or solid) in two or more points, based on the working range.

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4. PRACTICAL EXAMPLE OF A CALIBRATION AT LOW RANGE (0.1 ng)


This example shows how to properly calibrate the DMA-80 evo at low range, similar approach could be
used to calibrate the system at higher levels, see dedicated chapter in this manual.
The example of calibration has been designed to quantify 0.1 ng, for a working range from 0,1 ng to 1,5
ng.
- Prepare the blank and the standards as explained above.
- System must be clean
- The calibration to quantify 0,1 ng requires a calibration point lower than 0,1 ng, for example 0.05 ng.
- Never force to 0 the calibration (BV correction: OFF) in cell 0, but use a real blank as described in the
calibration paragraph. In Cell 1 and 2 calibration can be forced to zero.
- To maximize the performance of the system and its linearity at low range, the max ABS value has to be
set to a slightly higher absorbance of the 1.5 ng point (last point of this calibration in cell 0). In this specific
example, the “Absorbance limit of cell 0” was set to 0.1500, as the highest calibration point in cell 0 (1.5
ng) was 0.1400 ABS.

Below is reported the obtained calibration:

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8.5.5 How to increase the reproducibility


After calibration, the reproducibility of the unit should be lower than <1.5% for 5 measurements with
0.1 ml of a solution of 100 ppb ug/Kg (10ng).

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.

8.6 HOW TO WORK WITH UNKNOWN SAMPLES


Unknown samples can contain high concentrations of Hg, so in order to avoid contamination of the catalyst
we suggest developing the application with a minimum quantity of sample (<5 mg) and then increasing
according the result.
Note: 1500 ng is our highest absolute value of mercury detectable.
For solid samples with concentrations of Hg higher than our range, it is possible to do a premix from 1:1 to
1:200 with inert material, such as previously decontaminated alumina.
For liquid samples with high Hg concentration, it is possible to do a dilution using the same matrix.

8.6.1 How to work with non-homogeneous samples


Non-homogeneous samples can result in poor reproducibility of the results. It is possible to increase the
performance with a sample preparation procedure.
The problem is due to non-homogeneous distribution of Hg in the matrix, or to different sizes of the same
sample—especially for inorganic samples such as soil, sediment, ore, rocks, plastic, etc.
To solve the first problem, mixing well should suffice. For the second problem, you need to reduce the
sample’s particle size to a powder form, normally below 100 um.
Pre-concentration steps may work as an alternative solution.

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8.6.2 How to increase the recovery of difficult samples


It is possible with the DMA-80 unit to increase the recovery from difficult inorganic sample matrices, such
as metal oxide, by increasing its decomposition temperature and time.

Matrix Sample Program Recovery


1.Max START Temp. 200°C, Drying/Ashing 2
60%
100 mg (size min up to 650°C, 2 min at 650°C
ZnO
100 um) 2. Max START Temp. 200°C, Drying/Ashing
100.5%
200°C, 3 min up to 750°C, 2 min at 750°C
1.Max START Temp. 200°C, Drying/Ashing 2
50 %
100 mg (size min up to 650°C, 2 min at 650°C
MnO
100 um) 2. Max START Temp. 200°C, Drying/Ashing
99.9 %
200°C, 3 min up to 750°C, 2 min at 750°C

8.6.3 How to work with difficult matrices


Difficult matrices such as petrochemical products, samples containing solvent, or large amounts (> 100 mg)
of organic sample (blood , food, feed, agricultural sample, etc.) can explode without warning, and
consequently reduce the sensitivity of the system.
For serious problems, and when it is difficult to determine whether the catalyst or amalgamator is the source
of reduced sensitivity, we recommend replacing both of them.

Dedicated programs must be used for difficult matrices.

Matrix Sample Program Tips and tricks


Low reactivity
Petrochemical 20-50 mg
products and
samples Reduce the drying
containing High reactivity temperature and
solvent 10-20 mg extend
the time if strong
Max START Temp. 200°C, exothermic reaction
persists
High reactivity Drying/Ashing
50 mg 1min at 200°C, Use pre-concentration
Food, feed, 3 min up to 800°C, step to increase
Agriculture 1 min at 8000°C signal of low Hg amount
Low reactivity
100 mg (i.e.
fresh vegetable)

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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8.7 CONDITIONING PROCEDURE FOR NEW CATALYST TUBE


8.7.1 Introduction
The following procedure is to be performed after replacing a new catalyst/amalgamator. It is always
enclosed in all catalyst tube package.

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.

DMA80 analysis method (Initialization)1


Reagent/sample Sample
Step
type amount

1°-2° B/V amalgamator -

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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9 21CFR-11 DMA SOFTWARE


The U.S. FDA Code of Federal Regulations (CFR) Title 21 part 11 (Electronic records: electronic
signatures) defines the criteria under which electronic records and electronic signatures are considered
trustworthy, reliable and equivalent to paper records. The DMA software is fully compliance with this
regulation.
Thought the settings of the software it is possible to select the “CFR login mode” in order to switch on all
the functions requires by the the 21 CFR-11 regulations.

9.1 Activation of the 21CFR part 11


The login mode in accordance with 21 CFR-11 can be done in two different ways.

Create new user profiles with different access privileges.


Each profile have a specific password to login. Method and
measurements file needs to be signed before saving and
CFR Password using.
The password should have at least 5 characters with a
maximum of 8. Only numbers are allowed

Create new user profiles with different access privileges.


Each profile have a specific password with a signed USB
key, both necessary for the login. (Available only in case of
CFR Signature + password terminal)
The password should have at least 5 characters with a
maximum of 8. Only numbers are allowed

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.

9.2 Overview of user profiles and access levels


From the User window, you can create a new login name. there are three different types of users with
different levels of accessibility (privileges) that can be created.

Login type General description Access level

- Method files: can not modify any parameter


- Calibration files: can modify, create, save, load and
User delete calibration curves Low
- Measurement files: can modify as well as create,
save and load measurement files

Can create User and Manager profiles.


- Method files: can modify parameters, create, save,
load and delete method files
Manager - Calibration files: can modify, create, save, load and Medium
delete calibration curves
- Measurement files: can modify as well as create,
save and load measurement files

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Can create User, Manager and Administrator profiles.


- Method files: can modify parameters, create, save,
load and delete method files
- Calibration files: he can modify, create, save, load
Administrator High
and delete calibration curves
- Measurement files: can modify as well as create,
save and load measurement files
It has also access to some setting of the unit

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

Login type General description Access level

This access is only for the Milestone Service


Engineer.
Service It gives access to the most of settings, temperature High
limits, sensor calibrations and other features of the
unit

This access is for Milestone Producer for software


Supervisor High
optimizations and developments

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9.3 Declaration of compliance “DMA software” with FDA-21CFR part


11
The below table reports: the reference code of the regulation, the description of the regulation and how
Milestone instruments with DMA software comply or, when this is requested, how it supports the
organization of the user to fulfilling to.

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.

The organization of the user must produce procedures for


defining the retention period and for the secure back up of
the data copies during that time.
The physical access to the system and to the area where
11.10 Limiting system access to
this is installed must be regulated and it is under the
(d) authorized individuals.
responsibility of the organization of the user.
Use of secure, computer- A Process Report (Trail) records all the relevant events
generated, time-stamped audit including:
11.10 trails to independently record the - software accesses
(e) date and time of operator entries - settings modification
and actions that create, modify, - cycles execution
or delete electronic records. - users management

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Record changes shall not - errors


obscure previously recorded
information. Such audit trail For each recorded event the following information are
documentation shall be retained stored:
for a period at least as long as - date and time
that required for the subject - user name and access level
electronic records and shall be - details of the action
available for agency review and - both previous and new value (in case of data
copying. modification)

The Trail file cannot be modified or imported on DMA


software. It can be exported, saved and printed on
readable format file.

The organization of the user must produce procedures for:


defining the retention period (which as to be at least
longer as the data records), the backup of the Trail during
that time, managing the copy of the Trail file in order to
avoid deletion or alteration of the same, linking the
account name to the related person, managing the
eventual change of local time mode (solar-legal).
Use of operational system The DMA software does not allow to start a run if each
checks to enforce permitted critical parameter has not been properly entered or if all
sequencing of steps and events, the operations (e.g. file saving) have not been confirmed
as appropriate from the related detection device.
11.10 (f)
For critical editable parameters the software does not
allow to enter data out of the defined range.
The software does not allow the modification of the control
parameters during the execution of a program.
Use of authority checks to The access to the system is divided in 5 levels
ensure that only authorized - Supervisor
individuals can use the system, - Service
electronically sign a record, - Administrator
access the operation or - Manager
computer system input or output - User
device, alter a record, or perform The Supervisor and Service levels are reserved to
the operation at hand. Milestone organization personnel.

The access to the software can be further secured by the


use of individual and electronically signed USB sticks
(only for terminal, not PC software package).
11.10
At total, it is possible to create up to 16 login accounts
(g)
with Administrator, Manager and User rights.
The software does not allow to set simultaneously two
accounts with the same name and it is possible to define
an expiration time for the passwords.
It is not possible to use the same password immediately
after the expiration of the previous.
Password must have a minimum length of 5 digits and
must be modified at the first access of a new account.

After 3 consecutive failed unsuccessful attempts from the


same account, this is blocked. The release of a blocked
account can only be authorized from the following login
from a superior level or automatically after 24 hours.
11.10 Use of device (e.g., terminal) The mercury analyser with terminal and dedicated DMA
(h) checks to determine, as software are a “Closed System”. The input of data on the

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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.

There is not any other external data source except this


means
Determination that persons who The organization of the user must define adequate
develop, maintain, or use training procedures for all persons involved in using and
electronic record/electronic maintaining the DMA software but also the generated data
signature systems have the records and trail.
11.10 (i)
education, training, and
experience to perform their Milestone personnel involved with software developments
assigned tasks. and support are trained and qualified to perform their
tasks.
The establishment of, and The organization of the user must guarantee that the
adherence to, written policies persons are responsible for all actions that have been
that hold individuals accountable implemented with their electronic signatures to prevent
and responsible for actions any abuse. This also includes procedures for linking the
11.10 (j) initiated under their electronic account name to the related person.
signatures, in order to deter
record and signature falsification While on standby mode, the software automatically
logouts if for 10 consecutive minutes any interaction from
the user has been noted.
(k) Use of appropriate controls (1) The organization of the user must guarantee that the
over systems documentation documentation received with the system (e.g. user
including: manual) is properly distributed, made accessible and
(1) Adequate controls over the used.
distribution of, access to, and (2) The organization of the user must maintain audit
use of documentation for system minutes of the changes in the documentation for the
11.10
operation and maintenance. system. Milestone will produce and make available in
(k)
(2) Revision and change control each case the updated documentation of the system also
procedures to maintain an audit through Milestone Connect website.
trail that documents time-
sequenced development and
modification of systems
documentation.
Controls for Open system The mercury analyzer with terminal and dedicated DMA
11.30
software are a “Closed System”.
Signed electronic records shall
contain information associated (1) While signing a method or a calibration or a run on
with the signing that clearly DMA software, the name of the signer can be entered
indicates all of the following: manually or automatically if this is used as account name.
(1) The printed name of the
11.50 signer; (2) Actual date and time are automatically recorded.
(a) (2) The date and time when the
signature was executed; and (3) The account level is automatically recorded while other
(3) The meaning (such as signing meaning information can be entered in to the free
review, approval, responsibility, editable “Function” field while signing.
or authorship) associated with
the signature.
The items identified in The above electronic signature information is permanent
paragraphs (a)(1), (a)(2), and and unalterable part of the data record and therefore
11.50
(a)(3) of this section shall be undergoes the same controls as the data records
(b)
subject to the same controls as themselves, including printing or saving on the final report.
for electronic records and shall

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be included as part of any


human readable form of the
electronic record (such as
electronic display or printout).
Electronic signatures and The electronic signature is permanent and unalterable
handwritten signatures executed part of the data record and cannot be separated from this.
to electronic records shall be
linked to their respective
electronic records to ensure that
11.70
the signatures cannot be
excised, copied, or otherwise
transferred to falsify an
electronic record by ordinary
means.
(a) Each electronic signature (a) Each user must identify himself by his own account
shall be unique to one individual name and password.
and shall not be reused by, or The DMA software does not allow the repeated use of the
reassigned to, anyone else. same account name for different users but the
(b) Before an organization organization of the user must implement procedures so
establishes, assigns, certifies, or that an existing access authorization cannot be reused by
otherwise sanctions an or reassigned to anyone else.
individual's electronic signature, The access to the software can be further secured by the
or any element of such use of individual account.
electronic signature, the
organization shall verify the (b)The organization of the user must implement
11.100
identity of the individual. procedures so that an existing access authorization is
(c) Persons using electronic clearly linked to a person and cannot be reused by or
signatures shall, prior to or at reassigned to anyone else.
the time of such use, certify to At the first access to the DMA software of a new account,
the agency that the electronic the default password has to be modified from the person
signatures in their system, used to who that account name has been assigned.
on or after August 20, 1997, are
intended to be the legally (c)The organization of the user is responsible for certifying
binding equivalent of traditional that the electronic signatures are intended to be handled
handwritten signatures. as the legal equivalent of traditional handwritten
signatures.
a) Electronic signatures that are a)(1) The unique combination of username and password
not based upon biometrics shall: achieves the function of two identification components.
The access can be further secured by the use of individual
(1) Employ at least two distinct and electronically signed USB sticks.
identification components such
as an identification code and While on standby mode, the software automatically
password. logouts if for 10 consecutive minutes any interaction from
(i) When an individual executes the user has been noted.
a series of signings during a
single, continuous period of a)(2) The organization of the user is responsible for
controlled system access, the implementing procedures to ensure that electronic
11.200
first signing shall be executed signatures are exclusively used by the owner of the
using all electronic signature account.
components; subsequent The system prevents the repeated use of the same
signings shall be executed using account name for different users.
at least one electronic signature The access to the software can be further secured by the
component that is only use of individual account password.
executable by, and designed to
be used only by, the individual. a)(3) The organization of the user is responsible for
(ii) When an individual executes implementing procedures to ensure that any attempt to
one or more signings not use the electronic signature of someone other than the
performed during a single,

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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.

(b) Electronic signatures based


upon biometrics shall be
designed to ensure that they
cannot be used by anyone other
than their genuine owners.
Persons who use electronic (a) The system prevents the repeated use of the same
signatures based upon use of account name for different users.
identification codes in Each user must identify himself by his own account name
combination with passwords and password.
shall employ controls to ensure The access to the software can be further secured by the
their security and integrity. Such use of individual and electronically signed USB sticks.
controls shall include:
(a) Maintaining the uniqueness (b) DMA software does not allow to set simultaneously
of each combined identification two accounts with the same name and it is possible to
code and password, such that define an expiration time for the passwords.
no two individuals have the It is not possible to reuse an identical password
same combination of immediately after the expiration of the same.
identification code and Passwords must have a minimum length of 5 digits and
password. must be changed at the first access of a new account.
(b) Ensuring that identification
code and password issuances (c) The organization of the user is responsible for
are periodically checked, implementing procedures for the management of accounts
recalled, or revised (e.g., to and password also in case a person left the company or
11.300
cover such events as password changes his working position. Those procedures must
aging). ensure security and integrity of the system also in case of
(c) Following loss management lost, stolen, missing, compromised hardware or software
procedures to electronically access supports.
deauthorize lost, stolen, missing, The DMA software allows Service and Administrator
or otherwise potentially accounts to the delete other existing accounts.
compromised tokens, cards, and
other devices that bear or (d) After 3 consecutive failed unsuccessful attempts from
generate identification code or the same account, this is blocked. The release of a
password information, and to blocked account can only be authorized with a
issue temporary or permanent subsequent login from a superior level account or
replacements using suitable, automatically after 24 hours.
rigorous controls. The organization of the user must guarantee that
(d) Use of transaction unsuccessful access attempts causing locking of an
safeguards to prevent account or anyhow reported on the Trail file are monitored
unauthorized use of passwords and notified to the management.
and/or identification codes, and
to detect and report in an

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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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10 SAFETY DATA SHEET


Amalgamator for DMA-80 EVO
Revision nr. 001

Useful information, in case of Revision date: 2021-09-23

external tube break

1. Identification of the substance/preparation and of the company/undertaking


Trade name: Amalgamator complete with two connections (p/n DMA8134)

Application of the substance/the preparation: for laboratory and R&D purposes

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)

The information mentioned below must be intended, in case of break of the external tube.

2. Handling and storage


· Precaution for safe handling: Avoid contact with skin and eyes. Avoid formation of dust and aerosols.
Provide appropriate exhaust ventilation at places where dust is formed..
· Conditions for safe storage: Store in cool place. Keep container tightly closed in a dry and well-
ventilated place.

3. Ecological information
· Toxicity: n. a.
· Information about elimination (persistence and degradability): n. a.
· Bioaccumulative potential: n. a.
· Mobility in soil: n. a.

4. Accidental release measures


· Personal precautions: Wear respiratory protection. Avoid dust formation. Avoid breathing vapours,
mist or gas. Ensure adequate ventilation. Evacuate personnel to safe areas. Avoid breathing dust.
· Environmental protection: Prevent further leakage or spillage if safe to do so. Do not let product enter
drains. Discharge into the environment must be avoided.

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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.

5. Exposure controls/personal protection


· Personal protective equipment:
Respiratory protection: Where risk assessment shows air-purifying respirators are appropriate use a
full-face particle respirator type N99 (US) or type P2 (EN 143) respirator cartridges as a backup to
engineering
controls. If the respirator is the sole means of protection, use a full-face supplied air respirator. Use
respirators and components tested and approved under appropriate government standards such as
NIOSH (US) or CEN (EU).
Hand protection: Handle with gloves. Gloves must be inspected prior to use. Use proper glove removal
technique (without touching glove's outer surface) 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.
Body protection: Complete suit protecting against chemicals, The type of protective equipment must
be selected according to the concentration and amount of the dangerous substance in the specific
workplace.
Eye protection: Face shield and safety glasses Use equipment for eye protection tested and approved
under appropriate government standards such as NIOSH (US) or EN 166(EU).

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Catalyst for DMA-80 EVO


Revision nr. 001

Useful information, in case of Revision date: 2021-09-23

external quartz tube break

1. Identification of the substance/preparation and of the company/undertaking


Trade name: Quartz catalyst tube complete (p/n DMA8333)
Catalyst tube (p/n DMA8133)

Application of the substance/the preparation: for laboratory and R&D purposes

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)

The information mentioned below must be intended, in case of break of the external quartz tube.

2. Handling and storage


· Precaution for safe handling: Avoid contact with skin and eyes. Avoid formation of dust and aerosols.
Provide appropriate exhaust ventilation at places where dust is formed..
· Conditions for safe storage: Store in cool place. Keep container tightly closed in a dry and well-
ventilated place.

3. Ecological information
· Toxicity: n. a.
· Information about elimination (persistence and degradability): n. a.
· Bioaccumulative potential: n. a.
· Mobility in soil: n. a.

4. Accidental release measures


· Personal precautions: Wear respiratory protection. Avoid dust formation. Avoid breathing vapours,
mist or gas. Ensure adequate ventilation. Evacuate personnel to safe areas. Avoid breathing dust.
· Environmental protection: Prevent further leakage or spillage if safe to do so. Do not let product enter
drains. Discharge into the environment must be avoided.
. 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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5. Exposure controls/personal protection


· Personal protective equipment:
Respiratory protection: Where risk assessment shows air-purifying respirators are appropriate use a
full-face particle respirator type N99 (US) or type P2 (EN 143) respirator cartridges as a backup to
engineering
controls. If the respirator is the sole means of protection, use a full-face supplied air respirator. Use
respirators and components tested and approved under appropriate government standards such as
NIOSH (US) or CEN (EU).
Hand protection: Handle with gloves. Gloves must be inspected prior to use. Use proper glove removal
technique (without touching glove's outer surface) 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.
Body protection: Complete suit protecting against chemicals, The type of protective equipment must
be selected according to the concentration and amount of the dangerous substance in the specific
workplace.
Eye protection: Face shield and safety glasses Use equipment for eye protection tested and approved
under appropriate government standards such as NIOSH (US) or EN 166(EU).

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MSDS issue: May, 2012


Sample Additive A Revision nr. 001
Revision date: 2012-05-09
Material Safety Data Sheet Printing date: 2012-05-09

1. Identification of the substance/preparation and of the company/undertaking


Molecular formula: Silicon Dioxide

Trade name: Sample Additive A (p/n DMA80-SFA)

Article number: MSDS004-001


Application of the substance/the preparation: for laboratory and R&D purposes

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

Classification of the substance or mixture:

According to regulation (EC) No. 1272/2008


Skin irritation (Category 2)
Eye irritation (Category 2)
Specific target organ toxicity –single exposure (Category 3)

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.

GHS label elements, including precautionary statements

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.

6. Accidental release measures


· Personal precautions: Avoid dust formation.
· Environmental protection: Do not let product enter drains.
. Methods and materials for containment and cleaning up: Sweep up and shovel. Keep in suitable,
closed containers for disposal.

7. Handling and storage


· Precaution for safe handling: Provide appropriate exhaust ventilation at places where dust is formed.
Normal measures for preventive fire protection.
· Conditions for safe storage: Store in cool place. Keep container tightly closed in a dry and well-
ventilated place. Hygroscopic.

8. Exposure controls/personal protection


· Personal protective equipment:
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).
Hand protection: For prolonged or repeated contact, use protective gloves.
Eye protection: Safety glasses with side-shields conforming to EN166.
Hygiene measures: General industrial hygiene practice.

9. Physical and chemical properties

Appearance
Form Powder
Molecular weight: 60.08 g/mol
pH-value (g/l) n. a.

Safety Data

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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Melting point (Melting range) n. a.


Boiling point (Boiling range) n. a.
Flash point Not applicable
Ignition temperature n. a.

Explosions limits
Lower n. a.
Higher n. a.
Water solubility n. a.

10. Stability and reactivity


· Chemical stability: stable under recommended storage conditions.
. Conditions to avoid: Avoid moisture.
. Materials to avoid: strong acids, hydrogen fluoride, strong bases, strong oxidizing agents
· Dangerous decomposition products: Hazardous decomposition products formed under fired
conditions: silicon oxides.

11. Toxicological information


Acute toxicity:
LD/LC50 values relevant for classification:
Oral LD50 n. a.
Dermal LD50 n. a.
Inhalative LC50 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.

. Potential health effects


Inhalation: May be harmful, if inhaled. Causes respiratory tract irritation.
Ingestion: May be harmful, if swallowed.
Skin: May be harmful, if absorbed through skin. Causes skin irritation.
Eyes: Causes eye irritation.

. 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.

12. 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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· PBT and vPvB assessment: n. a.


· Other adverse effects: n. a.

13. Disposal considerations


· Product:
Observe all federal, state, and local environmental regulations.
· Contaminated packaging:
Dispose of as unused product.

14. Transport information


· Land transport ADR/RID (cross-border): not dangerous

· Maritime transport IMDG: not dangerous

· Air transport ICAO-TI and IATA-DGR: not dangerous

15. Regulatory information


· Labelling according to EU guidelines:
The product has been classified and marked in according to the requirements of Regulation (EC) No.
1907/2006.

· Code letter and hazard designation of product:

Xi Irritant

. Text of H-code(s) and R-phrase(s) mentioned in Section 3

Eye Irrit. Eye irritation


H315 Causes skin irritation
H319 Causes serious eye irritation

Skin Irrit. Skin irritation


STOT SE Specific target organ toxicity-single exposure
Xi Irritant

16. Other information


WARRANTY
The above information is believed to be correct but does not purport to be all inclusive and shall be used
only as a guide. The information in this document is based on the present state of our knowledge and is
applicable to the product with regard to appropriate safety precautions. It does not represent any
guarantee of the properties of the product. Milestone Srl, shall not be held liable for any damage resulting
from handling or from contact with the above product.
· Department issuing MSDS: Q.A / Normative
· Contact:
Phone: 00 39 035 575837
email: application@milestonesrl.com

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MSDS issue: May, 2012


Sample Additive B Revision nr. 001
Revision date: 2012-05-10
Material Safety Data Sheet Printing date: 2012-05-10

1. Identification of the substance/preparation and of the company/undertaking


Molecular formula: Aluminum Oxide

Trade name: Sample Additive B (p/n DMA80-SFB)

Article number: MSDS005-001


Application of the substance/the preparation: for laboratory and R&D purposes

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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6. Accidental release measures


· Personal precautions: Avoid dust formation. Avoid breathing vapours, mist or gas.
. Environmental protection: No special environment precautions required.
. Methods and materials for containment and cleaning up: Sweep up and shovel. Keep in suitable,
closed containers for disposal.
· Reference to other sections: See Section 13 for disposal information

7. Handling and storage


· Precaution for safe handling: Provide appropriate exhaust ventilation at places where dust is formed.
· Conditions for safe storage, including any incompatibilities: Store in cool place. Keep container
tightly closed in a dry and well-ventilated place. Strongly hygroscopic.
. Specific end uses: n. a.

8. Exposure controls/personal protection


· Control parameters: components with workplace control parameters

·Exposure controls
Appropriate engineering controls: general industrial hygiene practice

. Personal protective equipment:


Eye/face protection: Use equipment for eye protection tested and approved under appropriate
government standards such as NIOSH (US) or EN 166 (EU).

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).

9. Physical and chemical properties

Appearance
Form Solid
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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

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.

Vapour pressure 1 hPa at 2158°C


Relative vapour density 4 g/cm3
Vapour Density n. a.
Solubility in/ Miscibility with n. a.
water
Partition coefficient: n. a.
n-octanol/water
Autoignition temperature n. a.
Decomposition temperature n. a.
Viscosity n. a.
Explosive properties n. a.
Oxidizing properties n. a.

10. Stability and reactivity


· Reactivity: n. a
· Chemical stability: n. a.
. Dangerous reactions: n. a.
. Conditions to avoid: Exposure to moisture.
. Incompatible materials: Strong acids, strong bases, chlorine trifluoride, ethylene oxide, halogenated
hydrocarbon, oxygen.
. Dangerous decomposition products: n. a.

11. Toxicological information


Acute toxicity:
LD/LC50 values relevant for classification:
Oral LD50 n. a.
Dermal LD50 n. a.
Inhalative LC50 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.
This product is or contains a component that is not classified as to its carcinogenicity based on its IARC,
ACGIH, NTP or EPA classification.

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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. Specific target organ toxicity – single exposure (Global Harmonized System): n. a.


. Specific target organ toxicity – repeated exposure (Global Harmonized System): n. a.
. Aspiration hazard: n. a.

. Potential health effects


Inhalation: May be harmful, if inhaled. May cause respiratory tract irritation.
Ingestion: May be harmful, if swallowed.
Skin: May be harmful, if absorbed through skin. May cause skin irritation.
Eyes: May cause eyes irritation

. Signs and Symptoms of Exposure: Cough, chest pain, difficulty in breathing, gastrointestinal
disturbance.
. Additional Information: RTECS: BD1200000

12. Ecological information


· Toxicity: n. a.
· Information about elimination (persistence and degradability): n. a.
· Bioaccumulative potential: n. a.
· Mobility in soil: n. a.
· PBT and vPvB assessment: n. a.
· Other adverse effects: n. a.

13. Disposal considerations


Waste treatment method
· Product:
Offer surplus and non-recyclable solutions to a licensed disposal company.
· Contaminated packaging:
Dispose of as unused product.

14. Transport information


· Land transport ADR/RID (cross-border): not dangerous
· Maritime transport IMDG: not dangerous
· Air transport ICAO-TI and IATA-DGR: not dangerous

15. Regulatory information


· Labelling according to EU guidelines:
The product has been classified and marked in according to the requirements of Regulation (EC) No.
1907/2006.
Safety, health and environmental regulations/legislation specific for the substance or mixture
N. a.
Chemical Safety assessment
N. a.

16. Other information


WARRANTY
The above information is believed to be correct but does not purport to be all inclusive and shall be used
only as a guide. The information in this document is based on the present state of our knowledge and is
applicable to the product with regard to appropriate safety precautions. It does not represent any
guarantee of the properties of the product. Milestone Srl, shall not be held liable for any damage resulting
from handling or from contact with the above product.
· Department issuing MSDS: Q.A / Normative
· Contact:
Phone: 00 39 035 575837
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email: application@milestonesrl.com

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MSDS issue: May, 2012


Hg Trap Revision nr. 002
Revision date: 2014-03-17
Material Safety Data Sheet Printing date: 2021-09-23

1. Identification of the substance/preparation and of the company/undertaking


Product identifier: Adsorbent

Trade name: Hg Trap (p/n 70194)

Article number: MSDS006-001


Application of the substance/the preparation: for laboratory and R&D purposes

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
. 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.

6. Accidental release measures


· Personal precautions: Avoid dust formation. In case of dust released into the air, use a respiratory
protection.
. Environmental protection: Prevent product from entering into sewers, surface water, groundwater
and confined areas.
. Methods and materials for containment and cleaning up: Dry and dispose according to law. Collect
with mechanical tools the spilled materials and then rinse with water. Ensure adequate ventilation of the
place affected by the spill. The disposal of contaminated material shall be done in accordance with the
provisions of section 13.
· Reference to other sections: See Section 13 for disposal information

7. Handling and storage


· Precaution for safe handling: Store in a closed labelled container in a dry area.
· Conditions for safe storage, including any incompatibilities: Normal condition of storage without
any particular incompatibility.
. Specific end uses: n. a.

8. Exposure controls/personal protection


· Control parameters: n. a.

. Personal protective equipment:


Respiratory protection: Required in case of dust.
Eye/face protection: Not required.
Hand protection: Not required
Skin protection: Wash hands after product handling

9. Physical and chemical properties

Appearance
Form Solid pieces
Colour Black
Odour odourless
pH-value (g/l) n. a.

Boiling point (Boiling range) n. a.


Flash point n. a.
Flash (solids and gases) n. a.
Vapour pressure 1 hPa at 2158°C
Solubility in water (at 20°C) Insoluble in water
Partition coefficient: n. a.
n-octanol/water
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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

10. Stability and reactivity


· Reactivity: There are no particular risks of reaction with other substances in normal conditions of use
and storage.
· Chemical stability: The product is stable under normal conditions of use and storage.
. Dangerous reactions: Under conditions of normal use and storage, hazardous reactions are not
predictable.
. Conditions to avoid: None in particular. Follow the usual precautions against chemicals.
. Incompatible materials: Alkali metals, light metals in power form, fluorine, hydrazine and derivatives,
hydroxylamine, hydrogen compounds non-metallic, hot hydrogen, hydrides, silicon compounds, hot
anhydrides. .
. Dangerous decomposition products: When heated or in the event of fire, it can release gases and
vapours potentially harmful to health.

11. Toxicological information


Quantitative data on toxicity are not available. The morphology of the product doesn’t have
hazardous properties, if the product is employed with the proper attention.

12. Ecological information


· Toxicity: n. a.
· Information about elimination (persistence and degradability): n. a.
· Bioaccumulative potential: n. a.
· Mobility in soil: n. a.
· PBT and vPvB assessment: n. a.
· Other adverse effects: n. a.

13. Disposal considerations


Reuse, if possible. The residues of this product are considered as non hazardous special waste. The
disposal is regulated by specific laws and regulation in each country.
· Contaminated packaging: should be handled the same way as dangerous substances, and sent for
recovery or disposal in compliance with national waste management.

14. Transport information


· Land transport ADR/RID (cross-border): not dangerous
· Maritime transport IMDG: not dangerous
· Air transport ICAO-TI and IATA-DGR: not dangerous

15. Regulatory information


· Labelling according to EU guidelines:
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The product has been classified and marked in according to the requirements of Regulation (EC) No.
1907/2006.

16. Other information


WARRANTY
The above information is believed to be correct but does not purport to be all inclusive and shall be used
only as a guide. The information in this document is based on the present state of our knowledge and is
applicable to the product with regard to appropriate safety precautions. It does not represent any
guarantee of the properties of the product. Milestone Srl, shall not be held liable for any damage resulting
from handling or from contact with the above product.
· Department issuing MSDS: Q.A / Normative
· Contact:
Phone: 00 39 035 575837
email: application@milestonesrl.com

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AdsoQUICK

Material Safety Data Sheet

1. Designation of Material/Manufacturer and Company name


Information of the product

Trade name: adsoQUICK

Recommended Use/Application: various

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

Emergency call: Tel. 07561/9818-19 or 07561/9818-0

2. Composition/Data of the components


Chemical characterization
CAS-Nr.: 7440-44-0, designation: Carbon EG-Nr. 231-153-3

Hazardous/Dangerous Ingredients
None of the ingredients classified in RL 67/548/EWG

Additional references: none

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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Milestone Srl MA213-003 – DMA-80 EVO – User Manual

Drink water.

Notes for the physician: None

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5. Fire Prevention and Fighting

Suitable fire extinguishers:


Water jet,/nebulized water, foam, sand, CO2

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.

Special protections during fire:


No special requirement, provided there is sufficient ventilation, in case of insufficient ventilation
put on the oxygen mask.

6. Measures in case of unintentional spillage:


Avoid formation of dust, but in case of dust use protection mask or P1 filtering half mask.

Environmental protection:
No special measures are required.

Cleaning/collecting procedure:
Remove/wipe mechanically.

Additional warning: slip (and fall) hazard.

7. Handling and storage

Handling
Recommendations for safe handling:
In case of dust provide good ventilation/exhaust of the working room/site.

Prevention/protection against fire and explosion:


Keep away all ignition sources. In case of dust formations beware UEG (see point 9).

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.

Other storage conditions:


None
Store Class: void

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8. Exposure limits and personal protective equipment


Measures for limiting and monitoring exposure:
In case of dust, provide good ventilation of the working environment.

Additional requisites for organization of technical plants


No further data see point 7

Components with limit values to be controlled


CAS-Nr. Designation of the material value unit
7440-44-0 Carbon (alveolar fraction) AGW 3 mg/m3
(general dust limit value according to TRGS 900)

Additional requirements: none

Personal protection equipments

General protection and hygiene measures: none

Respiratory protection:
In case of dust use protection, for example P1 half filtering masks.

Hand protection: Not necessary

Eye protection: in case of dust fall.

Body protection: none

9. Physical and chemical properties

Form: solid
Colour: grey/black
Smell: odourless

Characteristics/ Safety-connected Parameters:


Size Value/Range Unit Method
Softening point: not applicable
Boiling point/ Boiling range not applicable
Fusion point/ Fusion range: not applicable
Inflammability: not applicable
Ignition point: not applicable
Ignition temperature: > 300 °C
Self inflammability: none 01)
Fire promotion properties: none
Danger of explosion: none 01)
Explosion limits: UEG > 50 g/cm³
OEG: not applicable

Note:
01)
with appropriate handling and storage

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9. Physical and chemical properties (continuation)


Size Value/Range Unit Method
Steam pressure: not applicable at 20 °C
Density: at 20 °C > 1,9 – 2,3 g/cm3
Solubility in water at 20 °C: insoluble
pH-Value: not applicable
Distribution coefficient: not applicable
n-Octanol/Water
Viscosity not applicable
Other data: none

Note:
01)
with appropriate handling and storage

10. Stability and Reactivity:


Conditions to be avoided:
None

Materials to be avoided:
None

Dangerous decomposition products:


None when properly used

Others: None

11. Toxicology Data


According to our experience and on the basis of the available information, in case of proper use
and appropriate handling, the product does not cause any unhealthy side-effect.

12. Environmental impact data


Can be mechanically separated in purification plants. Do not disperse to the grounds, into water
or drain pipes.

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.

Contaminated Packing material:


According to the local official regulations.

14. Transport regulations


No hazardous material according to national and international transport regulations.

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15. Data on legal requirements


Marking according to EEC guidelines
Identification letter and designation of danger:
No marking obligation

Dangerous component (s) for labelling:


None

National regulations
Notes on restrictions of use:
None

Regulations in case of accidents:


No

Water endangerment class:


Not dangerous for water (Self-classification).

Other regulations and restrictions:


None

16. Other Information:


None
The supplied data are based on today’s state of our knowledge. They describe our products
regarding safety requirements; however they do not represent any specific warranty of the
product properties or of a specific performance/application, and do not constitute any legal
contractual obligation.

Data sheet issued by: MLS GmbH


Person in charge: Mr Kopp Tel. 07561/9818-19

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

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