You are on page 1of 132

MILESTONE

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

DMA-80

Operator Manual
MA122
Milestone DMA-80 Operator Manual – Revision 01/2010

MILESTONE DMA-80 USER MANUAL


Thank you for choosing our DMA-80 direct mercury analyzer and welcome to the ever-growing world of Milestone
users.

We are sure that you will be completely satisfied with the performance of this new unit entering your laboratory.

We invite you to read carefully this user manual and to keep it in reach for convenient and fast consulting.

For any possible clarification or any request for assistance please contact either Milestone Srl at the following
address:

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

Or Milestone distributor in your country at:

Caution!
Please read the operator manual before using the instrument!

SYMBOLS USED IN THIS MANUAL

An instruction accompanied by this symbol provides a cautionary statement: WARNING.


Failure to follow the instruction may endanger the user or cause damage to the instrument.

Please read carefully this instruction.

DMA-80 INDEX 1
Milestone DMA-80 Operator Manual – Revision 01/2010

INDEX
______________________________________________________________________________________________
1 DMA-80 INSTALLATION Page 4
1.1 Unpacking and checking list Page 4
1.2 Options Page 9
1.3 DMA80 Setup Page 11
1.3.1 DMA80 with Terminal 1640/640 Setup Page 11
1.3.2 DMA80 with PC Setup Page 13
2 DMA-80 GENERAL DESCRIPTION Page 19
2.1 Technical data Page 19
2.2 Front view Page 21
2.3 Back side view Page 21
2.4 Inside view Page 22
3 TERMINAL 640/1640 and PC Page 24
3.1 Description Page 23
3.2 Installation Page 23
3.2.1 DMA-80 Page 23
3.2.2 Terminal connections Page 23
3.2.3 Terminal front panel connections Page 23
3.2.4 Terminal back panel connections Page 24
3.2.5 Connection of Terminal to DMA-80 Page 25
3.2.6 First Start Page 25
3.2.7 Printer and memory card Page 26
3.3 General Operation Page 27
3.3.1 Program Start/Login Page 27
3.3.2 Electronic Signature Page 28
3.3.3 End program/Logout Page 29
3.3.4 Desktop Page 29
3.3.5 Control sections Page 29
3.3.6 Operating program: DMA measurements Page 30
3.3.7 Generally used symbols Page 31
3.3.8 Numerical input via screen Page 32
3.3.9 Text input via screen Page 32
3.3.10 Print Page 33
3.4 Methods Page 34
3.4.1 Create new method Page 34
3.4.2 Open/Save/Delete Methods Page 35
3.4.3 Method Print-out Page 35
3.4.4 Method Parameters Page 36
3.5 Calibration Page 39
3.5.1 Create new calibration file Page 39
3.5.2 Open/Save/Delete Calibration file Page 39
3.5.3 Print Calibration file Page 40
3.5.4 Cuvette0/Cuvette1/Cuvette 2 Page 40
3.5.5 Description of Calibration file Page 41
3.6 Measurement Page 43
3.6.1 Tables Page 45
3.6.2 Reference measurements for high quality assurance Page 46
3.6.3 Blind value Page 47
3.6.4 Sample Page 49
3.6.5 Links Page 53
3.6.6 Signal Page 54
3.6.7 Results Page 55
3.7 System Page 57
3.8 Sample measurement Page 59

DMA-80 INDEX
2
Milestone DMA-80 Operator Manual – Revision 01/2010

3.8.1 Measurement of samples Page 59


3.8.2 Blank Measurement Page 60
3.8.3 Auto Blank Settings Page 60
3.8.4 Reference Sample Measurement Page 61
3.8.5 Calibration Sample Measurement Page 61
3.9 History Trail Page 62
3.10 System Administration Page 62
3.10.1 Access Page 63
3.10.2 Panel Administration Page 63
3.10.3 User Administration Page 63
3.10.4 Settings Page 65
3.10.5 Configuration Page 69
3.11 Balance Setting Page 70
3.12 Messages and inquiries Page 71
3.12.1 Technical Support Page 73
4 OPERATING WITH THE UNIT Page 75
4.1 Calibrations standards Page 75
4.2 How to prepare aqueous Hg standard Page 76
4.3 Calibration process using aqueous Hg standards Page 77
4.4 Calibration sample measurement Page 80
4.5 Running samples Page 81
4.6 Blank measurement / Auto-blank measurements Page 82
4.7 Reference sample measurement Page 82
4.8 Concentration sample measurement Page 83
4.9 Analysis Page 83
5 EASYDOC SOFTWARE 3.3 FOR DMA-80 Page 85
5.1 Software Page 85
5.1.1 License agreement Page 85
5.1.2 Registration Page 86
5.2 Downloading of data files Page 88
5.2.1 General Page 88
5.2.2 Connection Terminal-PC Page 88
5.2.3 Start downloading Page 88
5.2.4 Setup Page 89
5.2.5 Backup Page 91
5.3 EasyDOC Page 92
5.3.1 End program/Exit Page 92
5.3.2 Main buttons Page 92
5.3.3 Calibration Page 95
5.3.4 Sample Page 99
5.3.5 Parameter Page 103
5.3.6 Display Page 103
5.3.7 Trail Page 104
5.3.8 Method Page 104
6 DMA-80 MAINTENANCE Page 105
6.1 How to remove the catalyst and the amalgamator Page 105
6.2 How to install the catalyst and the amalgamator Page 112
6.3 How to do the ordinary maintenance to the pneumatic actuators Page 117
6.4 How to properly align the actuators Page 119
7 APPENDIX OF 21 CFR SECTION PART 11 Page 122
7.1 Explanation for agreement with CFR 21 part 11 Page 122
8 DMA-80 EC SAFETY DATA Page 127
8.1 Amalgamator Page 127
8.2 Catalyst Page 128
8.3 Sample Additive A Page 129

DMA-80 INDEX
3
Milestone DMA-80 Operator Manual – Revision 01/2010

1 DMA-80 INSTALLATION

1.1 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. Lift the main box up off of the
pallet to expose and facilitate removal of
the DMA-80.

Provide a bench of at least 150 cm length and 70 cm wide and place the DMA-80 on the bench. The unit
requires sufficient clearance (approx. 15 cm) on all sides to allow adequate movement of air.

( WARNING
The weight of the DMA-80 is approximately 56 kg; at least 2 people are needed to remove
the unit from its box and place it on the bench.

Open the boxes containing the accessories of the DMA-80, as below:

1 DMA-80 INSTALLATION 4
Milestone DMA-80 Operator Manual – Revision 01/2010

Terminal 640 Terminal 1640 PC software package (without PC)

PN TER6463 Flash memory card of 128


MB (only for T640 and T1640).

PN 933920 power cord for the DMA80 230V


10A.

P/N TER6459 RJ 45 cable.

1 DMA-80 INSTALLATION 5
Milestone DMA-80 Operator Manual – Revision 01/2010

USB cable A-B with Gateway (only for PC


configuration).

P/N DMA 8143 - Turntable for auto-sampler


with 40 positions.

The next five items are routine


consumables and recommended spares.
P/N DMA 8142 – DMA-80 sample boats (set
of 40 pieces).

P/N DMA 8134 - amalgamator with 2


Silicon joints,
included p/n DMA 8322 – Silicon joints (Set
of 5 pieces)

P/N DMA 8333 – Complete Catalyst Set,


including a Silicon joint and
O-rings set: TFM O-ring ∅ 23X0.3mm,
Silicon O-ring ∅ 22x3 mm.

Additional Spares: P/N DMA 8323 -


Ceramic insulation discs (Set of 5 pieces),
are to be ordered separately.

1 DMA-80 INSTALLATION 6
Milestone DMA-80 Operator Manual – Revision 01/2010

P/N DMA8357 - O-rings set for cuvette.

P/N DMA 8314 - maintenance grease for


pneumatic actuator.

P/N DMA 8327 - set of fuses 230V (includes 2 X


6.3 AT main power, 2 X 2 AT Transformer, and
1 x 16 AT main board).

P/N DMA 8328 - set of fuses 115V (includes 2 X


10 AT main power, 2 x 2 AT Transformer, and 1
x 16 AT main board).

P/N DMA 8318 – Chassis key.

P/N 60009 - tool kit (includes 4 mm hex


driver, 3 mm hex driver).

1 DMA-80 INSTALLATION 7
Milestone DMA-80 Operator Manual – Revision 01/2010

P/N DMA8385 - external flow meter (for


service purpose).

P/N 536132 - connector for oxygen supply.

Adapter plate with tubing connector for


exhaust.

Stand for sample boats PN DMA0464.

EasyDOC Software Package for DMA- 80


P/N LT00010.
USB-Pen for data transfer on PC

1 DMA-80 INSTALLATION 8
Milestone DMA-80 Operator Manual – Revision 01/2010

The next set of pictures shows the parts


installed in the unit that are not routine
consumables, but may eventually wear out.

P/N DMA-8058 - heating coil for


amalgamator (mercury release).

P/N SO0376D- heating coil for


drying/ashing.

P/N DMA 8344 - sample boat carrier


including P/N OR0024CH o-ring ∅
20x3mm.

Mercury trap P/N 70200 .

1.2 OPTIONS

P/N DMA00640 sample tray complete.

1 DMA-80 INSTALLATION 9
Milestone DMA-80 Operator Manual – Revision 01/2010

Quartz boats P/N 8347 (1500 ul, set of 10


pieces), indicated for aqueous samples, i.e.
waste water, standards etc.

Sample Additive A P/N SFA (Absorbing


material for DMA-80 applications), i.e.
petrochemical, chemical, vegetal oil, etc.

DMA-80 Air Compressor, P/N DMA-80AC:


lower running cost compared to oxygen
tanks.

DMA-80 upgrading kit for direct mercury


determination at trace level in gases, P/N
DMA-80GK

Sorbent trap for DMA-80 to measure the


mass concentration of mercury in gases,
P/N DMA00718

1 DMA-80 INSTALLATION 10
Milestone DMA-80 Operator Manual – Revision 01/2010

1.3 DMA-80 SETUP


During the DMA-80 setup both the unit and the Terminal 640/1640 or PC should not
be connected to the main power supply.
The DMA-80 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 proceed with DMA-80 SETUP (see
chapter 6.2).

1.3.1 DMA-80 with Terminal 1640/640 setup

Place the Terminal beside the DMA-80 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.

Connect the keyboard and the mouse to the back panel of the
Terminal (supplied only with Terminal 1640).

Plug-in the serial cable into Terminal (device).

DMA-80 INSTALLATION 1 11
Milestone DMA-80 Operator Manual – Revision 01/2010

Plug-in the end of serial cable into DMA-80 unit.

Introduce the memory flash card into the reader port located.

The flash card must be introduced with label


facing the user.

Flash card properly introduced.

Plug the power cord into DMA-80 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.

DMA-80 INSTALLATION 1 12
Milestone DMA-80 Operator Manual – Revision 01/2010

1.3.2 DMA-80 with PC setup

Minimum PC configuration required for DMA-80

CPU: Pentium III 800


RAM: 256 MB
Space on the disc: 20 MB
No. 1 USB port
No. 1 CD reader
Operative system: Windows XP or Vista

Printer: all compatible printers with


Windows XP and Vista

Plug the RJ45 cable into DMA-80 unit.

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.

DMA-80 INSTALLATION 1 13
Milestone DMA-80 Operator Manual – Revision 01/2010

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

Plug the power cord into DMA-80 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.

DMA-80 set up for all configurations

Attach the 6x4mm oxygen supply connector on to the supply


tube and tighten the compression fitting.

Insert the oxygen supply connector into the quick connect


located on the back of the DMA-80.

DMA-80 INSTALLATION 1 14
Milestone DMA-80 Operator Manual – Revision 01/2010

Correct connection is shown below.

The adapter plate for the exhaust outlet is already installed on


the back panel of the DMA-80.

Connect the exhaust tube (tube not supplied) to the adapter


plate with connection.

Exhaust tube correctly installed into the exhaust outlet.

DMA-80 INSTALLATION 1 15
Milestone DMA-80 Operator Manual – Revision 01/2010

Connect the exhaust tube to the mercury trap PN 70200


(optional).

The other end of the exhaust tube is normally directed to a


fume hood.

Check that the main power switch of the unit is OFF; only
after that, connect both power cords to the electrical outlets.
Switch on the DMA-80. The main switch is located on the
front panel of the unit and PC (only for PC version).

After a switch off wait 30 sec. before


switching on again.

Only for DMA-80 PC

When connecting the DMA-80 to the USB of the PC (via


Gateway) for the first time, the following announcement will
be shown: FOUND NEW HARDWARE.

Now you have to install the driver. Driver installation may be


different according to the Windows update version. If you see
welcome page, no connection to Windows Update is required.
Then click on “Proceed”.

1 Insert the CD into the CD-drive.

2 Select “Install software from a list or “other source”.

3 Confirm with “Proceed”.

DMA-80 INSTALLATION 1 16
Milestone DMA-80 Operator Manual – Revision 01/2010

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 2.04.06 WHQL
Certified.

1 Insert the CD into the CD-drive.

2 Go to the CD-List, copy the application file:


DmaOnPc.exe and add this file to a folder/list of your choice
on your hard disk.

3 Start the DmaOnPc.exe file on your hard disk.

The starting menu of the software will be shown.

4 Open un the left upper corner the menu

5 Digit the serial number and the valid licence key. These
data are printed on the Gateway. Confirm with OK.

After login by service code enter into Panel Administr./


Access/Panel Control (see chapter 3.10.2) and digit the
serial number and the valid licence key. Confirm clicking
on “save icon”.

6 Switch on the DMA unit.

With switched on DMA unit, the software

⇒ unit communication is established.

7 Copy the contents of the CD-Rom DMA-80 under the


C:\Documents

DMA-80 folder contains the original


calibration, methods, and data files.

DMA-80 INSTALLATION 1 17
Milestone DMA-80 Operator Manual – Revision 01/2010

For all DMA-80 configurations


When the DMA-80 software is completed, select your name
and enter your password.

User: 123
Administrator: 123456
Service: contact directly our service@milestonesrl.com
Next picture shows the DMA-80 software.

Now open the oxygen flow.

To avoid damage of the regulator


diaphragm, open the tank valve only when
the DMA-80 unit and Terminal are
communicating, then make adjustments to
the pressure from 0 to 4 bar (60 psig).

After approx. 15 minutes the message “START” of the


software will indicate that the DMA-80 is ready to work.
The mercury sample boats should be cleaned before starting
to work with the samples. To do this operation, bake them
out collectively in a muffle furnace or use the program here
on the right side.
Repeat this cleaning procedure until the absorbance has a
stable, low number <0.003

Notes: Consult the available Application Notes before starting


to work with the unit; some samples, such as crude oil,
require a dedicated or specific configuration of the system. If
the unit has not been used for a long time, it is suggested to
carry out the activation procedure (see chapter 6).

Now you are ready to work!

DMA-80 INSTALLATION 1 18
Milestone DMA-80 Operator Manual – Revision 01/2010

2 DMA-80 GENERAL DESCRIPTION


2.1 TECHNICAL DATA

Operating principle
Atomic absorption thermal decomposition.

Light source
Low pressure mercury lamp.

Wavelength
253.65 nm.

Detectors
UV enhanced photodiodes.

Instrument controller
Terminal 640
• Touch-screen industrial grade controller 6.5” screen with 65.000 colors; VGA resolution 640x480 for sharp
process graphic.
• 1 USB port for printer, 2 PS2 ports for mouse and keyboard, 3 RS 232 ports for external devices.
• Methods and runs saved on PC-compatible flash-card or USB pen-drive.
Terminal 1640
• Touch-screen industrial grade controller 12” screen with 65000 colors; VGA resolution 800x600 for sharp
process graphic.
• 1 USB port for printer, 2 PS2 ports for mouse and keyboard, 3 RS 232 ports for external devices.
• Methods and runs saved on PC-compatible flash-card or USB pen-drive.
Personal Computer (minimum requirements)
• CPU Pentium III 800.
• RAM 256 MB.
• 20 MB free space on hard disk.
• 1 USB port, 1 CD-ROM reader, operating system Windows 7, XP or Vista.

Instrument software
Milestone easyCONTROL®
• LIMS compatible.
• compliant to FDA regulations 21 CFR Part 11.

Detection limit
for solids, liquids and gas
0.005 ng (dual-cell).
0.0015 ng (tri-cell).

Typical analysis time


Solid and liquid: 5 minutes.
Gas: 3 minutes.

Typical precision
Less than 1.5%.

Working ranges

for solids and liquids


Automatic switch-over.
• Dual-cell: Low range: 0 to 20 ng.
High range: 20 to 1200 ng.
• Tri-cell: Low range: 0 to 10 ng.

2 DMA-80 GENERAL DESCRIPTION 19


Milestone DMA-80 Operator Manual – Revision 01/2010

• Medium range: 10 to 20 ng.


• High range: 20 to 1200 ng.
for gas (1L sample volume)
• Dual-cell: low range 0.05 to 20 µg/m3; high range 20 to 1200 µg/m3
• Tri-cell: low range 0.015 to 10 µg/m3; medium range: 10 to 20 µg/m3; high range 20 to 1200 µg/m3

Sample treatment
User-adjustable ‘on-the-fly’ in time and temperature.

Calibration
Standard solution of certified reference materials.

Type of sample
Solids, liquids and gas.

Maximum sample size/volume


Solid and liquid: 1.5 g/ml.
Gas: 0.05-100 l.

Auto-sampler
40-place, with dual-tray option for continuous operation.

Sample boat
Metal or Quartz.

Sample weighing
External analytical balance with automatic weight transfer.

Carrier
Oxigen or Milestone Air Compressor

Power
110-230V/50-60Hz.

Dimensions
Unit: 80 x 42 x 30 (H) cm.
Gas module: 12.5 x 6.5 x 16 (H) cm.
Vacuum pump: 28 x 40 x 17 cm.

Weight
Unit: 56 kg.
Gas module: 0.5 kg; vacuum pump: 15 kg.

Specifications are subject to change without notice.

2 DMA-80 GENERAL DESCRIPTION 20


Milestone DMA-80 Operator Manual – Revision 01/2010

2.2 FRONT VIEW

The picture below shows the front view of the


DMA-80. You can notice the main power switch
(1), the autosampler (2) and the chassis housing
4
2
lock (3). On the Terminal, the flash card (4).

3
1

2.3 BACK SIDE VIEW

An overview of the backside of the DMA-80 is


shown in the picture: on the left side there is the 2
RJ45 port (1) that connects the DMA-80 with the
Terminal, the power cord connection (2), the inlet 4
3
and the gas flow regulation valve (3 and 4). 7
On the back side of the Terminal there are the USB
6 1
interface (5) for printer or memory stick, the PC 5
port (6) i.e. LIMS , PC card (7).

On the front view of the Terminal, Keyboard and


mouse port (8), RJ 45 port (9), COM 1, 2 and 3 8 9 10
port (10) for additional device i.e. balance.

11
On the right side of the DMA-80 the exhaust outlet
(11).

2 DMA-80 GENERAL DESCRIPTION 21


Milestone DMA-80 Operator Manual – Revision 01/2010

2.4 INSIDE VIEW

The picture shows the inside view of the hardware


of the DMA-80.

2
DMA-80 Ducon Cuvette

1. Ducon cuvette (two cells) 1


2. Detector
3. Hg lamp

5
DMA-80 Tricell Cuvette (option)

4. Tricon cuvette (three cells)


4
5. n. 2 Detectors
6. Hg lamp
6

Infrared temperature sensor on the left controls


temperature of the amalgamator.

2 DMA-80 GENERAL DESCRIPTION 22


Milestone DMA-80 Operator Manual – Revision 01/2010

ATC thermocouple on the right controls the


drying/decomposition temperature.

Catalyst oven.

Heating coils
The picture shows how the amalgamator and
the catalyst are connected inside the catalyst
oven module. Notice where the heating coils are
located: 1) covers the amalgamator, 2) is around
the catalyst tube, and 3) covers the end of the
catalyst tube. Oxygen Flow

1 2 3

External flow meter for oxygen flow check. During


regular operation is not connected (service
purpose).

Vertical pneumatic actuator.

Horizontal pneumatic actuator.

2 DMA-80 GENERAL DESCRIPTION 23


Milestone DMA-80 Operator Manual – Revision 1/2010

3. TERMINAL 640/1640 and PC software


3.1 DESCRIPTION
TERMINAL 640/TERMINAL 1640 has a high resolution colour monitor with Touch Screen Function, provided
with switching surfaces to create, run and save DMA-80 programs.

TERMINAL 640 TERMINAL 1640 DMA80 PC software


The terminal is operated either by touching the switching surfaces of the screen (Touch Screen) or using
mouse and keyboard.
The DMA-80 Software is firmly installed in the main memory of the terminal.
Creation of methods on the Terminal is supported by graphic as well as numeric input mode.

The screen, i.e. the positioning of the Buttons can be different from the screenshots
represented in this manual, depending on the terminal that has been adopted.

3.2 INSTALLATION

3.2.1 DMA-80

The DMA-80’s Software is already installed in the supplied Terminal. For DMA-80 with PC software (see
chapter 1.2). Software’s updates are carried out by Customer Service.

3.2.2 CONNECTIONS TO TERMINAL

Be careful that the plug (DMA-80 as well as the terminal) must be unlocked when pulling out,
which means that the “nose” of the plug must be pressed when pulled out.

3.2.3 TERMINAL FRONT PANEL CONNECTIONS

3 DMA-80 SOFTWARE 640/1640 and PC 24


Milestone DMA-80 Operator Manual – Revision 1/2010

Terminal front panel connections

CONNECTION

A PS/2-Interface for mouse.


Mouse is not included in the supply of Terminal 640.

B PS/2- Interface for keyboard.


Keyboard is not included in the supply of Terminal 640.

C RJ45- Interface for device.


Connection for power supply of the Terminal 640.

D Serial Interfaces.
■ Connection for additional device (Balance) (e.g. COM1)
(See also Configuration)
Used cable: at terminal side RJ45 plug

PIN SIGNAL

2 RxT (In)
5 GND
6 TxD (Out)
Pin 1 is placed on the right side of the terminal.

■ DMA-80 Connection for Communication (e.g. COM3)


(connection to interface H of DMA)

3.2.4 TERMINAL BACK PANEL CONNECTIONS

Terminal Back Panel Connection

CONNECTION

E USB-Interface (for USB1.1 or USB2.0) for Printer

3 DMA-80 SOFTWARE 640/1640 and PC 25


Milestone DMA-80 Operator Manual – Revision 1/2010

for connection of a printer or memory stick.


See also chapter Printer and Memory cards

F PC Connection for LIMS connection

G PC-Card drive for Flash Card (included in the supply).


See also chapter FlashCard.

3.2.5 CONNECTIONS OF TERMINAL TO DMA-80

I J K L

Connection Terminal to DMA-80

CONNECTION

H RJ45- Terminal port

I RJ45- (not used)

J Mains connection

K Flow controller

L O2-connection

Voltage supply to the terminal is switched on and off simultaneously with the DMA.

3.2.6 FIRST START OF THE UNIT

1 Switch off the DMA-80 unit (place on OFF the ON/OFF switch placed on the front of the unit).

Never switch on or off the Terminal with switched on DMA-80

2 Connect the Device-connection C of the Terminal with connection H of DMA-80.


3 DMA-80 SOFTWARE 640/1640 and PC 26
Milestone DMA-80 Operator Manual – Revision 1/2010

The following Start routine is described in detail in the operating instructions. This
is only a short description.

3 Open the oxygen supply. Incoming pressure of DMA-80 must be 400 kPa (4 bar).
4 Switch on the main switch of the DMA-80 placed on the front panel.
TERMINAL and DMA-80-Software are automatically initialized.
6 Log in with your password.
Starting the software will simultaneously initialize the DMA-80 unit, i.e. all functions are in Standby
operating mode.
⇒ The auto sampler tray is initialized and driven to starting position.
⇒ All heaters are brought to starting temperature.

The Start-Switch in the Software is only active when all heating systems are at operating
temperature. Pre-heating time is approx. 15 to 20 minutes.

3.2.7 PRINTER AND MEMORY CARD

Printer for Terminal ( for PC, see chapter 1.2.2)

We recommend to use PCL3 enhanced (Printer Command Language) printer from HP. The
Software has an “Economy Modus”, for ink saving.
Successfully tested HP-Printer: HP1100, HP1280, HP5150, HP5160, HPD5360, HP5440, HP5650,
HP5652, HP5740, HP5940, HP6160, HP6540, HP6940, HP6980, HPD7160.
Printers are not supplied by Milestone, but must be purchased from a local supplier.
If you can not find locally a supplier , Easydoc software (enclosed in each DMA-80)
can be used to transfer data from terminal to your PC and then print out the report
with your own printer. For more information, see chapter 5.

EEPROM

Internal storage area (32 kB): Data are kept also during interruption of power supply. EEPROM is
reserved for System Protocol and settings.

Flash Card (only for Terminal 640/1640)

Mobile Storage area: Flash Card is used to store methods,


samples, and runs. It is used also for signature in the
Terminal the Flash Card uses the A:\ path.
Type of card: Flash Cards Type PC-Card or CF-Card
(Compact Flash Card) can be used. The PC-Card can be
directly inserted in the Terminal, for the CF-Card an
adapter is required.

3 DMA-80 SOFTWARE 640/1640 and PC 27


Milestone DMA-80 Operator Manual – Revision 1/2010

Storage capacity: The Terminal is delivered with a Flash


Card with min. 128MB. All memory sizes can be used. Since
the files are very small, some MB are sufficient.

How to insert Flash Card: The drive for the Flash Card is
located on the back of the Terminal.
Insert the Flash Card with the label in front of you. The
Flash Card must be introduced completely. The cart rises up
from the terminal at the same height of the black ejection
lever.
How to remove Flash Card: Press down the black lever
to release the card and then take it out.

The Flash Card may not be removed during writing of reading, otherwise the formatting
could be damaged and the files lost. Writing and reading are indicated on the screen with a
sand clock.

3.3 GENERAL OPERATION

3.3.1 PROGRAM START/LOGIN

Only for Terminal


Switching on the DMA-80 unit also the TERMINAL 640/1640 shall be initialized.
If in Login-Mode Flash Card and Password is selected user is requested by the Software to insert
his personal Flash Card (with signature).
There are different levels of access authorizations to operate that are described in the following
program description.

Request to insert Flash Card

1 Insert your Flash Card. The user defined on the card will be recognized and requested to
identify.
For all DMA-80 configurations
2 Select your user name on the Login window. Type your user id and confirm with OK. Use the
Touch Screen or mouse; the keyboard is not active at this point.

3 DMA-80 SOFTWARE 640/1640 and PC 28


Milestone DMA-80 Operator Manual – Revision 1/2010

3.3.2 ELETRONIC SIGNATURE

Login

With the shipment of the unit the following passwords are assigned:
The passwords can be changed in the Administrator Panel.
The electronic signature only on Flash Card (Terminal 640/1640)

f a file is stored in the Measurement Menu, the signature button will appear
(Flash-Card and password must be set in the User Panel) and the file can be
provided with an electronic signature.
1 Press the signature button to sign your file.
After selection of the button you will be requested to enter the kind of
signature.
2 Enter the kind of signature, e.g. for control or release.
3 Press the Ok button and the Login dialogue window will appear Select
your User Name and User Id.
4 Confirm with Ok.

3 DMA-80 SOFTWARE 640/1640 and PC 29


Milestone DMA-80 Operator Manual – Revision 1/2010

Your document is now provided with User Name, Date/Time and type.
This signature appears also on top of all results print-outs.
3.3.3 END PROGRAM AND LOGOUT

Touching the Logout switching surface the Login-window will be opened.


Now you can switch off the system or another person can log in.
Switching off the DMA-80 also the Terminal\PC will be disconnected.

3.3.4 DESKTOP

After Login the start page of the DMA-80 is opened. Gently touch the surfaces to enter the control
program or the software administration panel.

Start-Desktop

3.3.5 CONTROL SECTIONS

BALANCE SET-UP
Here are the communication settings for the balance. These must be
adjusted only when switching over to a new type of balance.

HISTORY TRAIL
All changes in the system are automatically documented, e.g. login,
logout, etc.

GENERAL ADMINISTRATION
This area is dedicated to the basic adjustments/settings and to the user
administration. The basic settings to a major extent are reserved to
Service.

3 DMA-80 SOFTWARE 640/1640 and PC 30


Milestone DMA-80 Operator Manual – Revision 1/2010

LOGOUT
With Logout you go out of the system. The Login window appears where
the next user can log in with his own password.

3.3.6 OPERATING PROGRAM: DMA-80 MEASUREMENTS

DMA-80 MEASUREMENTS
Control of DMA-80.
The actual control program is opened. This is divided into four main
registers that are extensively described in the following chapters.

Methods Purpose is to administer methods. Methods can be created, modified


and deleted, Methods specify the temperatures, the drying time,
the heating intervals, decomposition and rinsing time of the
measuring program.

Calibration Purpose is to administer the calibration files. From a calibration file


you can select the used measuring points and specify the regression
curves for each cuvette.

Measurements Here is specified the program for Hg analysis.

The calibration to be used is pre-selected in DMA-80


calibration.

The extinction process can be monitored in real time. Previously


measured data can be recalled and displayed at any time.
Results and statistics (over selected data) are calculated and can be
printed out.

System Here the system is supervised (Auto sampler, heating elements,


spectrometer).

Software is operated via Touch-Screen. Touching the screen or clicking with mouse the different
switching surfaces or input fields are activated.
Activated input fields are ready for entering data from a keyboard. Double-clicking on the activated
fields will open on the screen a numerical or standard keyboard.

Some symbols are present in each menu (or are generally used). They are described in the
following chapter.

3 DMA-80 SOFTWARE 640/1640 and PC 31


Milestone DMA-80 Operator Manual – Revision 1/2010

Symbols that are used only in certain menus are described in the respective chapters.

3.3.7 GENERALLY USED SYMBOLS

CREATE NEW FILE


This provides a new, empty file. The current file will be deleted, so save any
changes.

OPEN FILE
Open file button.

SAVE FILE
Save file button. Name must be assigned to the file to be saved.

PRINT FILE
Print file button to print out reports.

GO BACK
The operating program is quitted and will go back to the start screen.
Save any changes before quitting.

BREAK
Input is terminated without saving and the input window is quitted.

DELETE
File is deleted.

START
To start a measuring run. If there is a sand clock on, this means that a
current procedure must first be accomplished (e.g. heating of furnace and
cuvette).

STOP
The current measurement is interrupted and the sample boats are taken
back to the auto sampler tray. The Stop-Button must then be re-set
touching the red-green Stop-Button.

3 DMA-80 SOFTWARE 640/1640 and PC 32


Milestone DMA-80 Operator Manual – Revision 1/2010

3.3.8 NUMERIC INPUT VIA TOUCH-SCREEN

At different steps of the program it is necessary to enter numeric values. Touching twice on the field
or number to be changed, a numeric keyboard appears.

Numeric keyboard

3.3.9 TEXT INPUT TOUCH-SCREEN

At steps where a designation is needed, touching twice on the touch-screen a standard keyboard
will appear.

Standard keyboard

3 DMA-80 SOFTWARE 640/1640 and PC 33


Milestone DMA-80 Operator Manual – Revision 1/2010

3.3.10 PRINT

Printer
Touch the icon to pen a preview. Touch again to print out diagrams and/or
data.

If no printer is recognized, the icon will show faded.

Different printing options are available depending from which menu the print is made.

PAGE SELECTION FOR PRINTING


After selection the pages are pink.
Print-out of page 1 with diagram, method parameters, system data and
microwave program.

Additional copies of Sample Table (can also be printed from the “Sample”
register).

File is printed in landscape format.

To print the diagram of the actually selected data.

To print all diagrams of the current Sample Table.

If the document has several pages, you can go through it back


and forwards.

If the single samples of a table have been divided into different


groups, it is possible to print the data of a specific group.
See chapter of Results.

3 DMA-80 SOFTWARE 640/1640 and PC 34


Milestone DMA-80 Operator Manual – Revision 1/2010

3.4 METHODS

Methods

Here methods can be created, stored, changed, deleted and loaded.


To create a new method its Program steps must be defined, as well as the related parameters
(temperature, heating ramp, decomposition time, amalgam heating time, purge time of the
process.
This method, which normally remains unchanged, will be used to run standard programs in the
DMA-80 system.

It is possible to create as many methods as


desired. Only the last methods used can be called
directly under the Current Method menu-list.
All Methods can be opened touching the Open
Button.

3.4.1 CREATE NEW METHOD

NEW METHOD
To create a new method, open an empty method file. The current method will
be deleted from the main memory. Therefore save it before opening a new
method.

3.4.2 OPEN/SAVE/DELETE METHODS

3 DMA-80 SOFTWARE 640/1640 and PC 35


Milestone DMA-80 Operator Manual – Revision 1/2010

OPEN METHODS
To open one of the methods saved on the Flash Card (Terminal 640/1640) or
on PC.

Select the method from the list.


DMA-80 with Terminal: the name of the method
will appear the Name field. Touch the Open icon
and the selected method will be loaded in the
working memory, and then the window will be
closed.
DMA-80 with PC: touch the Open icon and
selected method through
C:\Documents\DMA80\Methods, the method will
be loaded in the working memory, and then the
window will be closed.

SAVE METHODS
A method can be saved and recalled at any time.
Designate a Name. The ending .m80 will be automatically added.
Touch the Save icon to save the current method and to close the window.
DMA-80 with Terminal: always save methods under A:\Methods
DMA-80 with PC: always save methods under
C:\Documents\DMA80\Methods

DELETE METHODS
Select from the list the methods to cancel. The name will appear in the
Name field.
DMA-80 with Terminal: Touch the icon and – after a request to confirm –
the method will be deleted. A deleted method is definitely cancelled.
DMA-80 with PC: C:\Documents\DMA80\methods , select the method and
delete.

3.4.3 PRINT-OUT METHODS

PRINT-OUT METHODS
The diagram can be printed before measurement is started under
Measurement ⇒ Signal .

3 DMA-80 SOFTWARE 640/1640 and PC 36


Milestone DMA-80 Operator Manual – Revision 1/2010

3.4.4 METHOD PARAMETERS

Ramp Control for Drying and Decomposition

The sample decomposition takes place at high temperatures (>600°C), to release Hg from the
sample. To prevent sample losses and spraying around of liquids, these should be dried before
decomposition.
For samples with high water content it is recommended to start a first drying Step of 200°C.
Samples containing liquids with boiling point under 100°C require an accordingly lower temperature.
Directly after drying the sample is decomposed at high temperature (burned in the oxygen flow).
A temperature of 650°C worked satisfactorily as decomposition temperature. This high temperature
ensures a complete decomposition and release of mercury. Only at a sufficiently high temperature
the entire Hg is set free and can be measured.
Example Method for wet sample:

Example of ramp control

Pos t T

1 00:00:30 200
Drying

2 00:03:00 200

3 00:01:00 650
Decomposition
4 00:02:00 650

3 DMA-80 SOFTWARE 640/1640 and PC 37


Milestone DMA-80 Operator Manual – Revision 1/2010

For solid samples the drying steps can be omitted.

Max. Start-T

Measurement starts only when temperature T1 (drying- und


decomposition furnace) is under the maximum Start-
Temperature. This prevents that sample boats are exposed
to high temperatures.

Purge time

Purge time is the time elapsing between the end of


drying/decomposition and the start of the Hg measurement.
Standard setting of purge time is 60 seconds.
During and after decomposition all pyrolysis gases are
transported with the oxygen flow by the catalyst to the
amalgamator. Hg is trapped in the amalgamator and all the
other gases are flushed out of the system before Hg is
measured in the cuvette.

Amalgam Heater Time

Amalgamator time is the time required by the


amalgam heater to completely release the Hg
collected in the absorption cell.
Standard setting: 12 seconds. In the Concentrate
measuring mode only the last of a series of samples
is heated.

Recording Time

In the recording time is noted and evaluated the


measuring signal of the spectrometer.
Standard setting : 30 seconds. In the Concentrate
measuring mode only the signal of the last of a
series of samples is recorded.

3 DMA-80 SOFTWARE 640/1640 and PC 38


Milestone DMA-80 Operator Manual – Revision 1/2010

Unit of Sample

Introduce the correct unit of measurement of your


sample.

• Solid samples: g
• Liquid samples: ml
• Gas sample: cm3, dm3 or m3

After unit modification save the method.

Diagram Input

The Parameters can be entered or modified also graphically.


1 Select the position that must be entered new or modified.
The Position will appear with yellow background.
2 Change the Temperature T and the Time 1 pulling the arrows in the desired direction.

When making a new entry in position 1 the first value to be specified is the Time (pull to the
right), then Temperature T (pull upward) can be specified.

Time t can be entered in 10 seconds increments, and Temperature T in 10°C increments.

Graphic Input

3 DMA-80 SOFTWARE 640/1640 and PC 39


Milestone DMA-80 Operator Manual – Revision 1/2010

3.5 CALIBRATION

This register administers calibration data. Different calibration files can be opened, created and saved.

Calibration curve for Ultratrace analysis

3.5.1 CREATE NEW CALIBRATION FILE

OPEN NEW CALIBRATION FILE


Open a new empty file touching this icon. The currently opened calibration
file will be cancelled from the memory. Therefore save the current file
before opening a new one.

3.5.2 OPEN/SAVE/DELETE CALIBRATION FILES

OPEN CALIBRATION FILE


Touch the Open icon will open the window to open a calibration file stored
on the Flash Card or from your PC C:\Documents\DMA80\Calibration. Select
the desired Sample Table from the list. The name of the file will appear in
the Name field.
Touch Open to download the file into the working memory and close the
window.

3 DMA-80 SOFTWARE 640/1640 and PC 40


Milestone DMA-80 Operator Manual – Revision 1/2010

Calibration

SAVE CALIBRATION FILE


Designate a Name. The ending .m80 will be automatically added.
Touch the Save icon to save the current Table and to close the window.
DMA-80 with Terminal: always save calibration files under A:\Calibration.
DMA80 with PC: always save calibration files under
C:\Documents\DMA80\Calibration.

DELETE CALIBRATION FILE


Select from the list the files to cancel. The name will appear in the Name
field.

DMA-80 with Terminal: Touch the icon and – after a request to confirm –
the calibration will be deleted. A deleted method is definitely cancelled.
DMA-80 with PC: C:\Documents\DMA80\Calibration , select the calibration
and delete.

3.5.3 PRINT CALIBRATION FILE

PRINT CALIBRATION FILE


Touch the Print icon to open a preview of the Print-Report. Touch again to
print the calibration file.

3.5.4 CUVETTE 0/CUVETTE 1/ CUVETTE 2

An individual calibration curve is provided for each of the sequential cuvettes.

DMA-80: The first and long one is used for measuring low Hg content (up to approx. 20 ng), the
second and short one for measuring high Hg content (up to approx. 1200 ng).

3 DMA-80 SOFTWARE 640/1640 and PC 41


Milestone DMA-80 Operator Manual – Revision 1/2010

Tricell DMA-80: The first and long one is used for measuring low Hg content (up to approx. 10 ng),
the second medium one (10-20ng), the third and short one for measuring high Hg content (up to
approx. 1200 ng).
Both cuvettes are always used for measurement. If the maximum peek of the first signal is over
0,8 A (standard setting), the maximum of the second signal will be used to calculate the result.

3.5.5 DESCRIPTION OF CALIBRATION FILE

 The x-Axis shows the Hg value, the y-Axis the decomposition.


 Calibration points are included in the Table by check marking the calculation of the
calibration curve. A repeated click cancels the selection, the checkmark disappears and the value
is not considered in the calculation.

Measuring points are included in the calculation. Blue Cross


Marked blue in the Table.
Measuring points are included in the calculation, but new Red Cross
calibrated and not confirmed by the user (e.g. saving).
Measuring points are not included in the calculation. No Grey Cross
marking in the Table.

Unselected values are not


taken for computation

Selected values are


taken for computation

Calibration Table and Curve

The column ∆E or ∆Hg shows the value by which the measured value deviates from the calibration
curve. Depending on the system setting the error is indicated is unit [ng], Extinction or in %.

The R² is calculated from the deviations of the measured values that have been
3 DMA-80 SOFTWARE 640/1640 and PC 42
Milestone DMA-80 Operator Manual – Revision 1/2010

calculated. The closer to 1 is the value, the better the calibration curve is adapted to
the measured values.

ENTER REMARKS
Click on any value of the table to open the columns for remarks and date. Clicking on the diagram
the fields will close again.

ULTRATRACE RANGE
For cuvette 0 only.
The calibration curve can be adapted to measuring for ultratrace analysis. To the highest
measured value an additional 40% (settable in the system administration) of the highest value is
added. No more values are calculated over this measuring value.

Highest value

40% of the highest value

ZERO POINT SETTING


Here it is specified whether the calibration curve is to be placed across the
zero point. The curve is placed across the zero point using the yellow
button. Normally it makes sense to put the calibration curve across the
zero point. An exception is represented by the Ultratrace analysis.

CALIBRATION METHODS
It is possible to determine the type of calibration curve. If „undefined“ is
selected, then only the measured points will be shown and not curve.

Linear: minimum two points are required

3 DMA-80 SOFTWARE 640/1640 and PC 43


Milestone DMA-80 Operator Manual – Revision 1/2010

X ext − X blanc = ε 0 ∗ X conc

Square : minimum three points are required

X ext − X blanc = ε 0 ∗ X conc + ε 1 ∗ ( X conc )


2

S-Curve (non linear) : minimum four points are required

X ext − X blanc = ε 0 ∗ X conc + ε 1 ∗ ( X conc ) + ε 2 ∗ ( X conc )


2 3

X ext Measured value in extinction units (or areas)

X blanc Blank value in extinction units (or areas)

X conc Concentration value

ε 0 , ε1 , ε 2 Correction factors

Depending on how the calibration points are distributed, the program requires more than the
minimum measuring points necessary for calculation.

3.6 MEASUREMENT

MEASUREMENT
This Menu is divided into four registers.
In the Sample, Links and Signal registers, the designations of the
sample table columns are partly repeated.

Conditions valid for all registers :


Greyfield
Grey Field
■ only white fields can be worked on.
■ grey fields cannot be worked on as the sample was
already measured. It is possible however to add remarks and
make statistics.
Yellow Field White Field
■ yellow fields are marked and ready for input. Yellow field White field

3 DMA-80 SOFTWARE 640/1640 and PC 44


Milestone DMA-80 Operator Manual – Revision 1/2010

AUTOMATIC MULTIPLE MEASUREMENTS


Under Measurement \ Sample window there is a small additional column n (= number). From
here it is possible to activate multiple measurements.
Select the number of measurements into the “n” column.

Number of measurements

In this way the corresponding number of lines is automatically added.

The average final result with the relative standard deviation is shown in the headline of the
multiple measurements. Individual values can be disabled removing the sigma sign.

Average of measurements
Std deviation

3 DMA-80 SOFTWARE 640/1640 and PC 45


Milestone DMA-80 Operator Manual – Revision 1/2010

3.6.1 TABLES

Table in Sample Menu:

Table in Links Menu:

Table in Signal Menu:

Table in Results Menu:

Pos / Position

Consists of two numbers: a e.g. 1


b e.g. (1)

If Simple sample processing is activated, and a sample is added, the number over the selected
record will be taken, alternatively the sample can be selected (from pos. 1 to 40), as in this
operating mode each sample can be measured individually.
The measurement of each sample is started manually. After measurement, the next position of the
sample plate, if available, is driven into load position.
If Automatic Sample Processing is activated, and a sample is added, the upper number increases,
i.e. the next not occupied number is used, since in this mode the samples are automatically
successively processed. Each position may be occupied only once.
In a file samples can be processed both in automatic and simple mode.

Liquid samples should be measured in Simple mode, as mercury can evaporate if the sample
remains for long time in the sample boats.

The lower number increases by 1 for each record.

Sample name

The Name is taken over from the selected record and can be changed/modified.

3 DMA-80 SOFTWARE 640/1640 and PC 46


Milestone DMA-80 Operator Manual – Revision 1/2010

Status

Enter the Status menu to define the type of file.


1. Normal
2. Calibration file (a C is shown to the right of the
status box )
3. Reference file (a R is shown to the right of the
status box)
4. Blind value (a B is shown to the right of the status
box)

The Status box indicates the current Status

Sample measured Measurement interrupted or


invalid
(e.g.: calibration file is
indicated by C)

Sample weighed Sample not weighed

Measuring sample Sample in stand-by


(automatic sample processing)

Weight

A weight must always be entered, see also the chapter Enter weight.

Remarks/Comments

It is possible to enter comments on the corresponding samples.

3.6.2 REFERENCE MEASUREMENTS FOR HIGH QUALITY ASSURANCE

The reference measurements however are now fully documented and plotted (graphically) under
Calibration / Reference.

3 DMA-80 SOFTWARE 640/1640 and PC 47


Milestone DMA-80 Operator Manual – Revision 1/2010

The table of the reference measurements includes: date, Hg in ng, Cal-Factor, used calibration and
remarks.
Average (m) of the reference values with the blue sigma sign.

The average of calibration factor values:


“Standard” can be selected clicking on right
button and automatically introduce as Cal-
Factor in all new measurements.

3.6.3 BLIND VALUE

Average between Cal-Factor values

It is a fast heating program of Furnace 1 and amalgamator, this in order to remove all deposit of
mercury / dust into the unit.
Is possible to define a blind value program, into the Panel administration>Settings>Limits.

3 DMA-80 SOFTWARE 640/1640 and PC 48


Milestone DMA-80 Operator Manual – Revision 1/2010

In this page it is possible to set: Maximum heating temperature, Maximum heating time and Purge
time of Blind value method.
Here an example of Blind value:

3 DMA-80 SOFTWARE 640/1640 and PC 49


Milestone DMA-80 Operator Manual – Revision 1/2010

3.6.4 SAMPLE

Screenshot of Sample Measurement

Add data

Add data
A new line is added to the table. The sample name in the „Name“ column is
taken over by the marked data record. If the name has a number as the
last figure, this will be increased automatically by 1.

If no position has been entered yet, no sample name would be registered in


this first line.
If a balance is connected, the balance screen will open simultaneously, to
be able to enter the weight of the sample.

3 DMA-80 SOFTWARE 640/1640 and PC 50


Milestone DMA-80 Operator Manual – Revision 1/2010

Enter weight

If balance is connected, whenever a record is added, the balance screen will automatically
open to allow entering the sample weight.

With all data records a weight must always be entered, since otherwise the measurement
cannot be started.
The sample weight is indicated in gram, milligram or micro gram according to setting (see
chapter Balance Settings).
The sample weight is entered either manually over the keyboard/Touch screen, or taken
directly from an electronic balance through the interface cable.

Downloading of weight
Precisa balances: The weight is constantly updated on the terminal. In the
sample table touch the Weight icon to download the value into the active
cell.
Other balances: touching the print button of the balance (see appropriate
manual of the balance) the weight is transferred on the terminal and into
the active cell.

AUTOMATIC TARING
Touch the T to tare the Precisa balance.

STOP
The balance screen is closed without loading the weight.

DELETE SAMPLE
Select from a list the sample to be deleted.
Touching the Delete icon the selected sample will be deleted after a safety
inquiry. A deleted sample is deleted irrevocably.

3 DMA-80 SOFTWARE 640/1640 and PC 51


Milestone DMA-80 Operator Manual – Revision 1/2010

Open new record

OPEN NEW RECORD


Touching this icon will open a new empty file. The file currently opened will
be deleted from the memory. Therefore always save before opening a new
file.

Processing of samples in simple or automatic mode

SIMPLE MODE
Each sample is measured individually. Each measurement has to be
manually started.
1 Click on the sample to measure and start the measurement.
After measurement the rotating plate is turned to loading position of the
next sample. However it is possible to click on and measure any sample.

AUTOMATIC MODE
Samples are automatically measured in sequence one after the other. After
measurement the rotating plate turns to loading position of the next
sample, and the next measurement starts automatically.

Concentrate over Several Samples

CONCENTRATE OVER SEVERAL SAMPLES


Only a defined maximum volume can be loaded into the sample boat.
With the Concentrate function a large sample can be distributed and
measured in several sample boats.
The divided samples are thermally decomposed and the total Hg of all sub-
samples is collected successively in the Amalgamator. The accumulated Hg
is only burnt and measured with the last sub-sample. The result is thus
determined over the total originally weighted-in quantity and the collected
Hg value. Active Button

Example
1 Weigh all samples in sequence.
2 Mark the record which contains a sub-sample (test1).
3 Activate the Button. The sample under the one marked will be connected with a brace-
parenthesis to the marked sample (test2).
4 Now select the connected sample (test2) and activate the Concentrate Button. The next sample
(test3) will also be connected to the first two samples.

3 DMA-80 SOFTWARE 640/1640 and PC 52


Milestone DMA-80 Operator Manual – Revision 1/2010

You can add as many samples as desired. All sub-samples linked with a brace-parenthesis will
be considered.
In a file several sub-samples can be combined to several samples. (See example : Sample 1
includes 3 sub-samples, Sample 2 consists of 2 sub-samples)

During this operation the Hg is not burnt.


Adding data into the sample table, the program of the selected record will be
taken over. Therefore be careful, when adding data (via the related button) to
the sample table, that no data within the "concentrate" data are marked, as
otherwise the Hg will not be burnt also for the added sample.

Print Sample Table

PRINT SAMPLE TABLE


Touching the Print icon will open a preview of the Print-Report. Second
touch will print-out the report. .

Open/Save Sample Table

OPEN SAMPLE TABLE


Touching the icon will open a window to the sample tables stored in the
Flash Card or from your PC C:\Documents\DMA80\Data. Select from the
list. The name of the file will be shown in the Name field.
Opening the selected file to load it into the working memory and the
window will close.

Load file

3 DMA-80 SOFTWARE 640/1640 and PC 53


Milestone DMA-80 Operator Manual – Revision 1/2010

SAVE SAMPLE TABLE


Enter name into the Name field. The ending .d80 will be added
automatically. Touch the Save icon to save the current table and close the
window.
DMA80 with Terminal: always save sample table under A:\Data.
DMA80 with PC: always save save sample files under
C:\Documents\DMA80\Data.

3.6.5 LINKS

Screenshot of Links

In this Register you can select the calibration file (Cal-Date) and Methods to be used for the
process.

3 DMA-80 SOFTWARE 640/1640 and PC 54


Milestone DMA-80 Operator Manual – Revision 1/2010

3.6.6 SIGNAL

Peek Cell 0

Peek Cell 1

Peek Cell 2

Signal

On the left of the screen there is a listing of the samples.


If one sample is check-marked, its curve is shown in the graphic on the right.
Each measurement is shown in real time and can be observed during process run.
During a current measurement you can also look at earlier runs.

TOTAL TIME
After Start the Total Time and the Sample Time will be
displayed. Total time - in case of automatic measurement of
several samples - is the total time of all samples.
Sample Time indicates the run-off time of the total
measurement.

ZOOM- IN AND ZOOM-OUT


Touch the magnification icon to zoom-in on the height of the peak used for
evaluation.

With the reduction icon the diagram will return to maximum extinction = 1.

3 DMA-80 SOFTWARE 640/1640 and PC 55


Milestone DMA-80 Operator Manual – Revision 1/2010

TEMPERATURE CURVE GRADIENTS


Touch the Temperature button (yellow background) to display the
temperature gradients of the selected sample.
Touch again the button to return to the curve.

Voltage of lamps (V) Drying/Decomposition Furnace


Temperature (°C)

Catalyst Furnace
Temperature (°C)

Amalgamator
Temperature (°C)
Absorbance

Cuvette
Temperature (°C)

Temperature Gradients

3.6.7 RESULTS

Screenshot of Results

Height
It's the maximum height of the evaluated peak.
Extinction = lg (100 % Transmission / X % Transmission)

3 DMA-80 SOFTWARE 640/1640 and PC 56


Milestone DMA-80 Operator Manual – Revision 1/2010

or area of the peak.

Hg [ng]
Absolute quanty of Hg in the sample (calculated from active calibration)

c[µg/kg] or c[mg/kg]
Concentration of Hg in the sample (calculated from active calibration and sample weight).

CalFactor
The result is multiplied by the calibration factor (Standard value 1.00). With a
eference measurement, the calibration factor can be adapted to a slightly modified
sensitivity of the system. Thus a calibration can be further used.

Σ
Clicking twice in this field, the sample will be included in the statistics
calculations. The Sigma icon can be removed at any time by clicking
again.

Group
Samples can be ordered into different groups, up to 8 groups can be
provided.
1 Click on the small arrow toopen a selection menu.
2 Select a group number for your samples.

In case the group assignment has to be cancelled, mark


the sample with X .

Unit of Measurement
Introduce the correct unit of measurement of concentration in order to
visualize the results.

Statistics

If a sample is identified with Sigma sign, it will be included in the statistics evaluation.
Results are shown in the following field :

m : Average Value
n

∑ Xi
m= i =1

n
Xi: Concentration values
n: number of samples

3 DMA-80 SOFTWARE 640/1640 and PC 57


Milestone DMA-80 Operator Manual – Revision 1/2010

σ abs : absolute Standard Deviation

∑ (Xi − m)
n
2

σ abs = i =1

σ rel : relative Standard Deviation

σ abs
σ rel = * 100%
m

3.7 SYSTEM

System Screenshot

From here you can check the conditions of the system, and follow the current conditions of the
measurement in real time.
After the start of the system all Standby functions are activated:
• The Hg lamp of the spectrometer is switched on
• The catalyst tube is locked by the pneumatic cylinder
• Oxygen flushes the catalyst, as long as there is gas pressure.
Catalyst, amalgamator unit and absorption cells are heated up to Standby temperatures. After
reaching these temperatures the Start button is released.

3 DMA-80 SOFTWARE 640/1640 and PC 58


Milestone DMA-80 Operator Manual – Revision 1/2010

STATUS OF THE UNIT


This shows the current status of the unit.
See also the Chapter of Messages

SPECTROMETER
The light intensity measured by the detector/s at the cuvette is represented as a blue bar.
The spectrometer is calibrated every measurement short before heating of the amalgamator.
In addition the shutter for measuring the 0% intensity is closed for short time. After opening
of the shutters the 100% intensity is measured.
In order to control the function of the shutter and the dark tension
(0 to 0,05V), the shutter can be closed and opened again between the measurements, by
clicking the screen symbol.

DMA-80: Spectrometer or Tricell DMA-80: Spectrometer

HEATERS
HEATING 1: for drying and decomposition of the sample. Here also the oxygenation takes
place.
HEATING 2: Heating of the catalyst zone at constant temperature.
HEATING 3: Heating of the amalgamator: at constant temperature to prevent separation of
condensation water. Heating to high temperature is then used to release very rapidly the
accumulated Hg.
HEATING 4: Heating of the cuvette block at constant temperature, to avoid condensation.

Activate the BV icons, to start the amalgamator or catalyst - heating program.


This is used to rapidly attain no blanks, even after large Hg quantity
measurements.

3 DMA-80 SOFTWARE 640/1640 and PC 59


Milestone DMA-80 Operator Manual – Revision 1/2010

AUTOSAMPLER
Graphic display of the pneumatic cylinders. The white points indicate
opened limit switches, the blue and red closed limit switches.
The cylinders are moved automatically only to take up or put back
the sample boats. Each cylinder however can be controlled
individually. Operating a cylinder symbol (rectangle), the cylinder will
change its position.
If a cylinder may not be moved to a certain point of time, no control
is possible (e.g. cylinder III may not be raised, if the rotation plate
moves).
1 select as load position the appropriate number, in order to position
a certain boat.
During a measurement the position of the measured sample is
indicated on the sample rotating plate.

TIME DISPLAY

After Start both Total Time and Sample Time will be displayed.
Sample Time shows the time already run off of a measuring series or of the current sample in
the following format : hh:mm:ss an.
In Automatic Mode the Total Time is calculated multiplying the number of samples by the
time required for the method :
e.g. 20 x 4 min = 1:20:00
The time to move the boats adds up to the time for data communication; to adjust this
deviation to the total time, after each measurement the time is calculated and the time
indication is corrected.
The coloured bar represents the measurement times (Rinsing time S, Amalgam heating time
H and recording time A). The current status of the measurement is indicated by the blue bar.

3.8 SAMPLE MEASUREMENTS

3.8.1 MEASUREMENT OF SAMPLES

Here after, there is a short description of how to measure samples.

1 Switch on the DMA-80 System with Terminal. The DMA-80 System requires approx. 15 minutes of
pre-heating time before measurement can be started.

3 DMA-80 SOFTWARE 640/1640 and PC 60


Milestone DMA-80 Operator Manual – Revision 1/2010

2 Select under Sample Measurement an existing file or create a new file for the sample, or create a
new Sample Table.
Select the operating mode, either automatic or simple.

For unknown liquid always operate in simple mode.

3 Select the right calibration under Measurement/Links.


4 Select the method under Measurement/Links.
5 Carry on an blank measurement to make sure that the system is free from Hg contaminations.
6 Check calibration of the system measuring a reference sample. At the end also the signal curve
can be tested in the Measurement/Signal menu.
7 Add the data necessary for the measurement. Be careful that measurement can be started only
when weight is indicated for all data records.
8 Enter the sample weight, put the sample in the Autosampler (use only cleaned samples) and
start measurement.
9 If the samples show heavily different Hg values, it is recommended to carry out blank
measurements after samples with high values.

3.8.2 BLANK MEASUREMENT

It is recommended to run a number of "Blank" values before starting to measure. This will
determine if the system is clean and free from contaminations. Water condensation or dust may
give undefined absorptions in the spectrometer. The impurities are in this way eliminated.

To enable the system to carry on a measurement, it is required to enter a weight different from
0,0000. Any entry other than 0,0000, for example “1.0000” will enable the measurement. The
calculated concentration is not substantial for the blank value. The absolute Hg-detected amount is
indicated in [ng]
A blank run should be performed without any sample boat to test the system, as otherwise it is not
sure if the blank comes from the system or from Hg traces in the boat.
The sample boats should be cleaned in a separate cleaning step.
3.8.3 AUTO-BLANK SETTINGS

This function allows to run blanks in automatic


mode when the Hg amount of sample is over the
setting limit (i.e 100ng).
For setting-up this function select Panel
Administration\Settings\Setup2.
Into “Automatic blank values cycles” there are
default parameters and may be modified according
user needs.

3 DMA-80 SOFTWARE 640/1640 and PC 61


Milestone DMA-80 Operator Manual – Revision 1/2010

3.8.4 REFERENCE SAMPLE MEASUREMENT

In the column CalFactor of "Results" table is entered the calibration factor used for measuring the
Hg-contents (Standard value : 1.00). The calibration curve can be corrected with a calibration
factor lower or higher than 1.
Use a reference sample to check the calibration curve. A new calibration factor is calculated after
sample measurement.

1 Open a measuring file.


2 Make a blank run to make sure that the system is free from Hg contaminations.
3 Go to the Measurement/Links menu and add a data record. Select for this record the method
and calibration that you want to use for the reference run.
4 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.
5 Enter concentration and weight of sample, insert the reference sample into the Autosampler
(use only perfectly clean boats) and start the measurement.
6 After measuring the reference sample, the calibration factor is calculated and displayed in the
related column CalFactor.
In the System Administration are set limit values for the calibration factor and the consequences in
case limits are exceeded.

3.8.5 CALIBRATION SAMPLE MEASUREMENT

To make a calibration two files are required, one measuring file (same as the one for sample
measurement) and one calibration file. The calibration file must be loaded or opened prior to the
measurement, and must be entered under Measurement/Links.
After measurement of a calibration sample, the data are taken automatically over and are used for
the computation of the calibration curve.
1 Create a new calibration file. If you want to add a new calibration sample from an existing
calibration, enter the desired calibration under Measurement/Links.
2 Change into Measurement Menu and open in the File register an existing file or create a new file
for the data of the calibration sample. Select Simple operating mode.
3 Run a blank measurement to make sure that the system is free from Hg contaminations.
4 Add one data record. Select for this data record the method that you want to use for calibration.
5 Define in the Status column of the "Result" menu the sample as calibration sample. The
"Concentration" c[µg/kg] column, otherwise closed, is ready for input.
6 Enter concentration and weight of the sample, put the calibration sample into the Autosampler
(use only perfectly cleaned boats) and start measurement. After measurement the data will be
automatically taken over in the calibration file. Also with a blank value as calibration point,
concentration (0.0) and weight (>0.0) must be entered, as the Software with check these
inputs.
7 Repeat Points 5 and 6 for additional measurements.
8 After measuring the calibration sample, go back to the calibration menu. Select measuring
data to be used for the calculation of the calibration curve.
9 Enter the kind of computation for each cuvette.
10 Save the new or modified calibration file.
3 DMA-80 SOFTWARE 640/1640 and PC 62
Milestone DMA-80 Operator Manual – Revision 1/2010

3.9 HISTORY TRAIL

HISTORY TRAIL
The menu point of the History Trail is located in the Start page.
In the History Trail all changes in the system are logged with time, date
and person, and saved in the internal memory.

SPACE ALLOCATION
Display of space allocation in the Flash card(only terminal)

PRINT
The History Trail is printed out.

SAVE ON FLASH CARD


The system log can also be stored on a Flash Card ( A:\ :\ *.m80) or on a
PC (C:\Documents\*.m80)

CUT HISTORY TRAIL (ADMINISTRATOR ONLY)


With this icon up to the last 100 entries can be cancelled.

DELETE HISTORY TRAIL


With this icon all enties are cancelled.

3.10 SYSTEM ADMINISTRATION

SYSTEM ADMINISTRATION
From here the basic settings of the software can be looked at or modified
according to level of authorization.
User does not have any access to the system administration.
Changes must be stored in the Administration Panel. Otherwise the changes
are automatically saved when quitting the Administration panel.

Register of System Administration

Access To make settings for the terminal and to administer users.

Settings Here are specified the system settings.

Configuration Here are specified the interfaces.

3 DMA-80 SOFTWARE 640/1640 and PC 63


Milestone DMA-80 Operator Manual – Revision 1/2010

3.10.1 ACCESS

The Access Register consists of three pages :

Panel- Here are carried out the settings for the terminal
Administration (e.g. brightness of the screen).

User- Used to administer the access authorizations by users.


Administration

Software This page is used for Software-Update (only for Service).

3.10.2 PANEL-ADMINISTRATION

Access

CHOICE OF THE LANGUAGE


Used to define language between English and German.

SUMMER
Used to acrivate or disactivate the acoustic signal when touching the screen
icons/buttons.

DATE AND TIME


The change of time from Summer to Winter is not automatic.

BRIGHTNESS OF LCD (SCREEN)


Used to adjust brightness of the screen to the
environmental conditions.

SERIAL NUMBER, SOFTWARE-VERSION, LICENCE-NUMBER AND

3 DMA-80 SOFTWARE 640/1640 and PC 64


Milestone DMA-80 Operator Manual – Revision 1/2010

CONTROLLER/TERMINAL-VERSION
The Software program is only accessible if the licence number for the Software-Version and
the Serial number of the Terminal are matching. The licence number can only be given by
Service.

SAVE
To secure that setting modifications are maintained also after new start of
the terminal.

3.10.3 USER ADMINISTRATION

To administer the access authorizations for users.

User-Administration

LOGIN-MODE
Check-marking „Password only“, one valid password
is sufficient to log in. Otherwise also a personal Flash
Card with signature is required. To modify the Login-
Mode a Flash Card with Service Signature (for
Service only) is necessary.
See also Chapter FDA-21CFR Compliance.

AUTHORIZE NEW USER


The Administrator can authorize additional users (with user access). A
dualogue window will open to enter User Name, Password and Access
rights.

3 DMA-80 SOFTWARE 640/1640 and PC 65


Milestone DMA-80 Operator Manual – Revision 1/2010

CHANGE PASSWORD
It is possible to change your own password ( or a subordinate password) as
well as access rights. Do not use „0“ as initial of a password, as „0“ will be
ignored.

DELETE USER
The Administrator can delete an User (with user access).

FLASH CARD SIGNATURE


The Flash Card can be provided with a signature (Signature = User Name
of the active user). Cards can be provided with signatures under own name
or subordinate name.

3.10.4 SETTINGS

PRINT
All current settings will be printed out.

If no printer is found or recognized, the icon will show faded.

Setup 1

Setup 1

3 DMA-80 SOFTWARE 640/1640 and PC 66


Milestone DMA-80 Operator Manual – Revision 1/2010

Signal analysis Maximum: Hg-content is calculated based on the peak-height


(Maximum extinction).
Integral: Hg-content is calculated based on the peak-surface
(Integral of the extinction).

Be careful when switching from one calculation mode


to the other. Values already measured will be switched
as well from height to surface or viceversa. However
the results (Hg and c) will not be recalculated.
After switching calculation mode it is necessary to
recalculate a new calibration curve before measuring
any new sample.
It is recommended to measure always in one modality
only.

Others functions The gray spaces are locked; these functions can be not modified.

Setup 2

Setup 2

Save of data after one The measured values are saved after each measurement.
measurement They will remain in memory without any later saving.

Signal of errors Errors recognized by the software are announced by an


acoustic signal.

Signal termination The end of a measurement is announced acoustically.

3 DMA-80 SOFTWARE 640/1640 and PC 67


Milestone DMA-80 Operator Manual – Revision 2/2010

Setup 3

Setup 3

Parameters of reference CalFactor (min): Minimum value of calibration factor


samples
CalFactor (max): Maximum value of calibration factor
When out of range: If the signal is out of range the
instrument: stop the working analysis, ask with a request
message if you prefear to continue or stop, continue the
analysis without any alarm.

Additional sample disk Function to abilitate only in case is present a second auto-
sampler tray (40 positons).
The first sample disk is running and the second is prepared
externally. After removing the first disk, user is asked how to
proceed.

3 DMA-80 SOFTWARE 640/1640 and PC 68


Milestone DMA-80 Operator Manual – Revision 1/2010

Additional sample disk Function to abilitate only in case is present a second auto-
sampler tray (40 positons).
The first sample disk is running and the second is prepared
externally. After removing the first disk, user is asked how to
proceed.

Exchange of Maximum number of cycles (analysis) for amalgamator


amalgamator replacement. When this value is reached, an error message
will apperar informing that you need to replace the
amalgamator.
Note: after amalgamator replacement edit new “maximun
number of cycles”.

Exchange of catalyst Maximum number of cycles (analysis) for catalyst


replacement. When this value is reached, an error message
will apperar informing that you need to replace the catalyst
tube.
Note: after catalyst replacement, edit new “maximun number
of cycles”.

Directory recycled When deleting a file, a folder named “Recycled” is created on


the Flash Card. The file will be stored in there, until it is finally
deleted.

Others functions The gray spaces are locked; these functions can be not
modified.

3 DMA-80 SOFTWARE 640/1640 and PC 69


Milestone DMA-80 Operator Manual – Revision 1/2010

Limits

Limits

3.10.5 CONFIGURATION

Configuration

Definition of interfaces for balance, DMA unit and support for LIMS can be set by Service.
However the user can select the separator, type of file and decimal for LIMS.

3 DMA-80 SOFTWARE 640/1640 and PC 70


Milestone DMA-80 Operator Manual – Revision 1/2010

3.11 BALANCE SETTINGS

Balance Setting

SETTING OF BALANCE
An electronic balance can be connected to the terminal via an interface
cable. Communication settings are made under Balance setting (see also
the user manual of the balance).
No saving is required after modification.

Received Text, With functioning communication with the balance, the text and the
Weight display weight received from the balance are indicated here.

Manufacturer of the <Other>: touching Print on the balance (see also the user manual
balance of the balance) the weight is transferred to the terminal and from
here touching the balance icon it can then be transferred to the
Sample Table.
Precisa: The weight is constantly updated on the terminal. Touching
the Balance icon the value is transferred into the active cell of the
Sample Table.

Baudrate, Data bits Communication settings of the balance.


and Parity

Measuring Unit The selected format is used in the weighing-in table.

Interface COM-Port for the balance is defined in the page Configuration/Unit.


Connect the balance to the appropriate COM-Port. Connections are
located in front of the terminal.

3 DMA-80 SOFTWARE 640/1640 and PC 71


Milestone DMA-80 Operator Manual – Revision 1/2010

Interface cable Cable with RJ45 plug at the terminal. For Precisa balances a 1:1
cable can be used.

Plug position

PIN Signal

2 RxT
5 GND
6 TxD

Pin1 isonthe right of the terminal connections.

3.12 MESSAGES AND INQUIRIES

Status Messages

STATUS LINE
In the system main menu there is the status line of the currente status of the unit. .

DMA_NO_ERROR
The system is in Standby-Mode and is ready for sample measurement.

DMA_MEASURE_IN_PROGRESS
Measurement is under process.

DMA_MOVE_IN_PROGRESS
The rotating plate or the pneumatic cylinders are moving.

TREAD STOPPED
This message appears only for very short time after the measuring has
been broken off pushing the Stop button.
Push the red-green Start button and the system is again ready to start.

ERROR MESSAGES

INIT
When an error has been recognized by the software, an error message
appears on the screen. After acknowledgement, the error message will also
appear in the status line.
After repair of the error (by the user if this is possible) the unit must be re-
initialized clicking on Init (The Init button appears over the Start button).

COMMUNICATION ERROR
If the communication between DMA and terminal is disturbed, or the DMA
does not react to an instruction from the terminal, communication error is
indicated.
1 Check if the connecting cable from DMA-80 ⇔ Terminal is correctly
plugged in.

3 DMA-80 SOFTWARE 640/1640 and PC 72


Milestone DMA-80 Operator Manual – Revision 1/2010

LOOKING FOR PARAMETER


If a sandclock appears on Start it means that the parameters have
not yet been reached. The related Parameter will be blinking on the
System-Page.

DMA_LIGHT_BARRIER_ERROR
The DMA-System controls at all times the Autosampler
turntable. When the software is started, it will look for and
find the reference position (double hole in tray at position
31).
Taking out the sample tray, it will interfere with the
position light sensor and the software will display the error
message. This means that the position of the turntable is
no more known to the system.
Verify that the turntable is inserted correctly and initialize
the unit with Init.

DMA_CALIBRATION_ERROR
Initialization Error:
During initialization of the autosampler, if the reference
position of the turntable (double hole at pos. 31) is not
found within one complete turn (360°), the calibration error
is displayed.
Make sure that the sample tray is correctly inserted and re-
initialize the equipment clicking on "init" start button.

DMA_PNEUMATIC_ERROR
Pneumatic Error:
The pneumatic actuators did not move after the command
was sent from the terminal.
The reason may be due to a blocked or disconnected
oxygen line (empty bottle or incorrect setting of the
pressure regulator) or the pneumatic actuators are
blocked.
Check the oxygen line and re-initialize the equipment.

DMA_T1_FAILURE
This message indicates that the measured temperature
increase was too low if compared with the required value.
This means that the heating coil for drying/decomposition
is not functioning, or the required value is too high.
Initialize the equipment from the System-Page.

DMA_MOVE_ERROR
Move Error:
No signal was sent to the light barrier within a certain
time, although the sample tray should move.
Make sure that the sample tray is not blocked.
See also Initialization Error.

3 DMA-80 SOFTWARE 640/1640 and PC 73


Milestone DMA-80 Operator Manual – Revision 1/2010

INCORRECT CALIBRATION FACTOR


This error means that measuring a reference sample the
calibration factor is outside the pre-set limits.
The limits are set in the Administration Panel/ Settings.

INCORRECT EXTINCTION
The extinction [A] (height) of the measuring signal of the
2nd cuvette is larger than 0.8. The measured value is
therefore invalid and is not evaluated.

INCORRECT TIME OF THE PEAK RISE


This error is due to a peak of sample outside the pre-set
limits. Limits are set in the Administration
Panel/Settings/Setup 1.
If this error appears repeatedly, check the settings of
Peak control and gas flow.

WRONG SOFTWARE OF CONTROLLER


BOARD
The terminal does not connect with the CPU of
the Controller-Board of the DMA-80.
If the terminal is correctly installed and
connected to the DMA-80, it means that a
wrong software version is loaded on the CPU.
Try to restart the system or call the local
Milestone representative for service.

MA_CONTROLLER_ERROR
There is a small CPU/controller board installed inside the DMA-80. When the system is
switched on the board boots and checks the system. This error message indicates that the
CPU/controller board is not working correctly.
Re-start the system or call the local Milestone representative fort service.

DMA_HARDWARE_VERIFY_ERROR
The signal of the light barrier is controlled several times by the controller board before it is
recognized as valid. Thus it is guaranteed that no electrical disturbance falsifies the signal.
The error message means that the signal was not received correctly.

3.12.1 TECHNICAL SUPPORT

Contact your local Milestone representative for any technical support, application advice and
supplemental operator training.

3 DMA-80 SOFTWARE 640/1640 and PC 74


Milestone DMA-80 Operator Manual – Revision 01/2010

4 OPERATING THE UNIT

4.1 CALIBRATION STANDARDS

Before using the Direct Mercury Analyzer for the first time, the instrument must be calibrated using prepared
Standard solutions of Hg or Standard Reference Materials (SRM or CRM). The instrument does not have to be
re-calibrated every time, but the calibration curve must be checked every morning prior to analyze unknown
samples. The instrument has to be recalibrated only if the calibration check results in 10% higher or 10% lower
than expected recoveries.
The instrument has to be also recalibrated when any of the major components are replaced. For example,
calibration must be performed when the catalyst and/or the amalgamator are replaced, or when the oxygen
tank or gas regulator is changed.
The Direct Mercury Analyzer can be calibrated using solid Standard Reference Materials or diluted aqueous
standards. Diluted aqueous standards (or working standards) may be prepared by diluting either 1,000 ppm or
100 ppm Hg standards (stock solutions). Both standards are commercially available. Use the equation below to
dilute the standards.

Working standard (ppm) = Stock solution (ppm) x (Volume of the stock solution (mL)/Total
volume (mL)
Total volume is the volume of the working standard.

For Example:
To prepare 1,000 µg/Kg(1 ppm) working standard, take 100 µl of the 1,000 ppm Stock solution and dilute up
to 100 mL.
To prepare 2,000 µg/Kg(2 ppm) working standard, take 200 µL of the 1,000 ppm Stock solution and dilute
up to 100 mL.
To prepare 5,000 µg/Kg(5 ppm ) working standard, take 500 µL of the 1,000 ppm Stock solution and dilute
up to 100 mL.
To prepare 7,000 µg/Kg(7 ppm) working standard, take 700 µL of the 1,000 ppm Stock solution and dilute
up to 100 mL.
To prepare 10,000 µg/Kg(10 ppm) working standard, take 1,000 µL of the 1,000 ppm Stock solution and
dilute up to 100 mL.

The diluted aqueous standards for low and medium concentration (ppb range) are prepared from the 1 and 5
ppm solution.
To prepare 5 µg/Kg(5 ppb) working standard, take 0.5 mL of the 1 ppm solution and dilute up to 100 mL.
To prepare 10 µg/Kg(10ppb) working standard, take 1 mL of the 1 ppm solution and dilute up to 100 mL.
To prepare 20 µg/Kg(20 ppb) working standard, take 2 mL of the 1 ppm solution and dilute up to 100 mL.
To prepare 30 µg/Kg(30 ppb) working standard, take 3 mL of the 1 ppm solution and dilute up to 100 mL.
To prepare 50 µg/Kg(50 ppb) working standard, take 1 mL of the 5 ppm solution and dilute up to 100 mL.
To prepare 100 µg/Kg(100 ppb) working standard, take 2 mL of the 5 ppm solution and dilute up to 100 mL.
To prepare 200 µg/Kg(200 ppb) working standard, take 4 mL of the 5 ppm solution and dilute up to 100 mL.
To prepare 500 µg/Kg(150 ppb) working standard, take 5 mL of the 10 ppm solution and dilute up to 100 mL.

There are three different working range responses that the instrument may be calibrated on:

1. the low range is 0- 10 ng Hg


2. the medium range 10-20 ng Hg
3. the high range is 20-1000 ng Hg.

To calibrate the instrument for its full range, prepare 5 ppb up to 10 ppm Hg working standards as described
above. Use 0.5 % - 5 % (1 % suggested) dilute hydrochloric for the dilutions.
Make sure the stock standard is not old or contaminated. As soon as the working standards are prepared,
transfer them into brown glass bottles. Aqueous standards with low Hg concentration are very unstable when
stored in plastic or regular clear bottles. Do not expose the Hg standards to the air for any length of time. Mix
the aqueous samples each time prior the analysis. As soon as the sample is pipetted out, close the storage
container. Don’t leave the solution bottles open on the bench and at the end store them into a fridge at 5-10°C.

4 OPERATING WITH THE UNIT 75


Milestone DMA-80 Operator Manual – Revision 01/2010

4.2 HOW TO PREPARE AQUEOUS Hg STANDARDS

Introduce some distilled water into the rounded


bottom flasks of 100 ml volume.

Add 1ml of HCl conc. 37% used for stabilization.

Place it on an analytical balance and get the


tare.

Make the injection of the standard/stock


solution (see the standards list reported at
chapter 4.1) and take the weight of it.

Now apply the following formula in order to get the correct concentration value of new standard.

Working standard (ppm) = [Stock solution (ppm) x Weight of injection (g)] / Total volume (mL)

As example:

- 1000 mg/Kg (ppm): take 100 µl from 1000 ppm Stock solution and dilute up to 100 ml.

[1000 ppm (stock sol.) x 0.100 g (Weight of injection)] / 100 ml (total volume of flask)= 1ppm

4 OPERATING WITH THE UNIT 76


Milestone DMA-80 Operator Manual – Revision 01/2010

If standards at ppb level, remember: 1 ppm = 1000 ppb.

-25 µg/Kg (ppb): take 0.5 µl from 5 ppm (5000 ppb) solution and dilute up to 100 ml

[5 ppm (standard sol.) x 0.500 g (Weight of injection)] / 100 ml (total volume of flask)= 0.025 ppm (25 ppb)

4.3 CALIBRATION PROCESS USING AQUEOUS Hg STANDARD

Open the “Methods”, type a new method name, description and assign the working parameters of the
instrument, such as drying and decomposition time and save the new method file.
Drying time varies with the volume of the sample and has to be calculated using the following equation:
Drying time (sec) = Sample Volume (µ µL) × 0.6
Decomposition time is 150 sec

Open the “DMA-80 Measurement ” click the button to obtain a new empty data file, type a new data name,
description and save new data file.

Open the “DMA-80 Calibration”, click the button for provide new empty calibration file, type a new data name,
description and save the new calibration file.

Return to the “DMA-80 Measurement ”, and load the data file saved.
Open “Sample” table of “Data”. Click “magic wand” button to build a new line. Click in the “Sample name” field
and type sample name. Under the “Weight” column, enter the weight in units of gram (or volume in mL) of the
working Hg standard that will be used for calibration (if 100 µL is used, then enter 0.1).
Open “Result” table and clicking the “Calibration” button appears under State “C”. Enter with the concentration
of your working standard solution in units of µg/Kg(ppb) or mg/Kg(ppm). For example, 100 µg/Kg (see Figure
1).

1 ppm = 103 ppb (1,000 ppb) = 106 ppt (1,000,000 ppt)


10-3 ppm = 1 ppb = 103 ppt
10-6 ppm = 10-3 ppb = 1 ppt

Figure 1. “ Result” table:

Ignore the “Hg (ng)”, the “Calibration Factor” and the Cal file. Nanograms of mercury will be plotted against
absorbance in the “Calibration” panel (see Figure 3).

Figure 2. “Result” panel after analysis

4 OPERATING WITH THE UNIT 77


Milestone DMA-80 Operator Manual – Revision 01/2010

Figure 3. “Calibration” panel of Cell 0 (only for DMA-80 Tricell)

When performing a calibration, the instrument first has to be calibrated for 0 ng of mercury. To do it, firstly, run
an analysis of several empty boats (this cleans the system and the boats). Empty boats must be repeatedly
processed until a low, stable absorbance is obtained. Then, follow the calibration procedure that has been
described above, running one of the clean empty boats. In the “Result” table, enter 0.0000 in the “C (µg/Kg)”
column and 0.1 g in the “Weight” column.

The calibration may be performed using two different approaches: Type A or Type B (the most commonly
used).

Calibration type A
Performing calibration using three standard solutions via different volumes

Use the following Table 1 as a guide to calibrate the instrument. Always start with the lowest amount of
mercury. Make sure that the sample boat is at room temperature before introducing the sample into it.

Use the following equation to determine the volumes of various working standards you should use to calibrate
the instrument.

Hg (ng)= Hg concentration in the sample (ppm) x Sample weight (mg)

Use variable volumes of the 0.1 ppm (100ppb) , 1 ppm, 10 ppm working Hg standards, and the following
equation, to calibrate the instrument i.e for low range, Hg (ng) = 0.1 ppm x Sample weight (mg). For 0.1
ppm(100 ppb) Hg standard liquid solutions, 10 µL solution contains 1 ng of Hg.

Table 1

To calibrate for … ng of Hg Standards size to be weighed…


to get desired ng of Hg
0.5 ng (low range) 5 µL of 100 ppb
1 ng (low range) 10 µL of 100 ppb
2 ng (low range) 20 µL of 100 ppb
3 ng (low range) 30 µL of 100 ppb
5 ng (medium range) 50 µL of 100 ppb
10 ng (medium range) 100 µL of 100 ppb
20 ng (medium range) 20 µL of 1 ppm
50 ng (high range) 50 µL of 1 ppm
100 ng (high range) 100 µL of 1 ppm
200 ng (high range) 200 µL of 1 ppm
500 ng (high range) 50 µL of 10 ppm
700 ng (high range) 70 µL of 10 ppm
1000 ng (high range) 100 µL of 10 ppm

4 OPERATING WITH THE UNIT 78


Milestone DMA-80 Operator Manual – Revision 01/2010

Figure 4. Complete cal. of Cell 0 Figure 5. Complete cal. of Cell 1 Figure 6. Complete cal. of Cell 2
(only for DMA-80 Tricell)

After calibration, the user can select different calibration algorithms: linear, s-curve or square.
Clicking on the button of Cell 0 you can force the curve to 0 (when yellow, the function is activated).
Clicking on the button of magnifying lens the ultratrace range is selected (when yellow, the function is
activated); see chapter 3 (ultratrace range) for more details.

Calibration type B

Perform calibration using the same volume but different standards solutions.
To calibrate the instrument use the following Table 2 as a guide. Always start with the lowest amount of
mercury. Make sure that the sample boat is at room temperature prior to introducing the sample into the boat.

Note: the type B is one of the most used

Use the following equation to determine the volumes of various working standard to use to calibrate the
instrument:

Hg (ng) = Hg concentration in the sample (ppm) x 100 mg

Use a fixed volume of 100 µL aliquots from various concentrations of standard solutions, and the following
equation, to calibrate the instrument for the low range, i.e., Hg (0.5 ng) = 0.005 ppm (25 µg/Kg) x Sample
weight (100 mg), etc... For standard solutions at room temperature, 100 mg is equivalent to 100 µl.

Table 2.

To calibrate for … ng of Hg Standards solutions ... to get desired ng of Hg


0.5 ng 100 µL of 5 ppb std
1 ng 100 µL of 10 ppb std
2 ng 100 µL of 20 ppb std
3 ng 100 µL of 30 ppb std
5 ng 100 µL of 50 ppb std
10 ng 100 µL of 100 ppb std
20 ng 100 µL of 200 ppb std
50 ng 100 µL of 500 ppb std
100 ng 100 µL of 1 ppm std
200 ng 100 µL of 2 ppm std
500 ng 100 µL of 5 ppm std
700 ng 100 µL of 7 ppm std
1000 ng 100 µL of 10 ppm std

4 OPERATING WITH THE UNIT 79


Milestone DMA-80 Operator Manual – Revision 01/2010

Figure 7. Complete cal. of Cell 0 Figure 8. Complete cal. of Cell 1 Figure 9. Complete cal. of Cell 2
(only for DMA-80 Tricell)

After calibration, the user can select different calibration algorithms: linear or square etc...
Clicking on the button of Cell 0 you can force the curve to 0 (when yellow, the function is activated).
Clicking on the button of magnifying lens the ultratrace range is selected (when yellow, the function is
activated); see chapter 3 (ultratrace range) for more details.

4.4 CALIBRATION SAMPLE MEASUREMENT


(1) To create a new calibration curve, you have to create a new calibration file on the “DMA-80
Calibration”.
(2) If you want to add new calibration points to an existing calibration file, click the curve that you
want to edit in the list on the “DMA-80 Calibration”.
(3) Change to the “Data” table and use the calibration function to enter a calibration sample to the
table.

For measuring a calibration sample, you have to select a new line in the “Results” table of “DMA-80
Measurement\Data” and click the “Calibration” button. All calibration samples are stored in the table on the
Calibration in the software.
Activating the calibration function appears under state “C”, type sample name in the field of “Sample name”.

After editing the “Weight” field of the sample, it is absolutely required to edit the “Concentration” field of the
measured sample in the “Result” table. Without editing the “Concentration” field, the sample will be used as a
calibration sample of 0 ng.

Note: The concentration needs to be entered in units of “µg/kg” (ppb) or mg/Kg (ppm).

The Result field is normally blocked: no entry is allowed when measuring a sample. This field can be edited only
when working with Calibration and Reference sample functions.

Figure 15. Result panel

You have to enter “0.00” in the Result field only when measuring the “Blank” value as a “Calibration” point. The
software requires an entry in the weight field that differs from “0.0000” to enable the measurement of this
sample, e.g. “1.0000”.

Figure 16. Result panel after analysis

4 OPERATING WITH THE UNIT 80


Milestone DMA-80 Operator Manual – Revision 01/2010

After measuring the calibration sample, the data are written in the “Result” table and into the Calibration table
panel.

If this calibration function is activated, the measured result will be automatically added to the active calibration
table. To add the samples to a new or different calibration curve, firstly, create a new table.

To abort the Calibration function, click again the “Calibration” button. This is possible only before the sample is
processed. After the measurement, the data can not be changed any more by the operator.

4.5 RUNNING SAMPLES

This is an example of a standard procedure for running unknown samples:

(1) Start the software and turn on the “System” of “DMA-80 Measurement” and
allow some time to warm up

(2) Select a pre-stored method in the “Methods” , or create a new method for
your samples.
If you create a sample file first, the actual selected method file is stored
automatically. Therefore, first select the method file!

(3) Create a new sample file for saving the data from your samples. Select
between Auto or Single mode.
Note: It is recommended to measure liquid samples only in Single mode
using metal boat.

(4) Check if the correct calibration file is selected.


By switching on the software, the previously used calibration file is load
automatically.

(5) Run some “blank” measurements to make sure the system is clean.
If no calibration is selected, the system cannot calculate the result of the
measurement.

(6) Check the calibration of the system by measuring a “Reference” sample.

(7) Measure your samples. For unknown samples introduce small amount(<5mg)
in order to avoid DMA contamination.

(8) Measure some blank values in between your samples to see if the system is
contaminated or not.

4 OPERATING WITH THE UNIT 81


Milestone DMA-80 Operator Manual – Revision 01/2010

4.6 BLANK / AUTO-BLANK MEASUREMENTS

Blank measurement
It is recommended to run a number of “Blank” values before starting to measure unknown samples. The
measurement of the “Blank” determines if the system is clean and has no contamination of Hg inside.
Moreover, water condensation or dust can give an undefined absorption in the spectrometer. This can be
eliminated by running some blank values.

To enable a sample measurement with the software, it is required to enter a weight different than “0,0000” in
the “Result” table of “DMA-80 Measurement\Data”. If the entry in the weight field is “0.0000” the measurement
can not be started. Any entry different than “0,0000” will enable the measurement. e.g. “1.0000”

Figure 17. Blank panel

The measured value in the height field shows the result of the blank run. e.g. 0,0015 abs. This gives the
absolute amount of detected Hg, shown in the field “Hg” e.g. 0,05 ng Hg absolute
The calculated concentration depends on the entry for the weight.

Depending on the concentration of the sample to measure, a higher or lower blank value can be tolerated. A
blank run should be performed without any sample boat to test the system itself.
If the blank run is done with an empty sample boat, it is not possible to determine if the measured signal is
coming from the DMA system or if there is some residue in the sample boat. The sample boats should be
cleaned in a separate cleaning step. With liquid samples, a film may appear on the sample boat which can be
removed with a laboratory spatula. For solid samples, a brush can be used to remove any combustion residue.
It is recommend to clean the sample boats after every run to ensure correct analysis.

Auto-blank measurement
This function allows to automatically start blanks when the Hg amount detected is over a set limit.
More information about settings in chapter 3.8.3.

4.7 REFERENCE SAMPLE MEASUREMENT

For the measurement of a Reference sample, select a new line in the “Result” table of DMA-80
Measurement\Data” and click the “Reference” button. A Reference sample is used to check the validity of the
calibration curve. Measuring this sample will calculate a calibration factor for correction of the curve. This factor
is displayed in a separate column of the “Results” of “Data” screen. The standard calibration factor is “1.00”.

Once activated, the Reference function appears under state “R”. After editing the weight of the sample, it is
absolutely required to edit the concentration of the measured sample in the “Result” field. Without editing the
concentration, the sample can not be used as a reference sample for calculating the calibration factor.

Note: The concentration needs to be entered in units of “µg/kg” (ppb) or “mg/Kg”(ppm).

The “Result” field is normally locked when measuring a sample. This field need to be edited only for Calibration
and Reference Samples.

4 OPERATING WITH THE UNIT 82


Milestone DMA-80 Operator Manual – Revision 01/2010

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.

Figure 18. Reference panel after analysis

Factor 0,97 result from reference sample is 3 % higher than the calibration value
Factor 1,00 result from reference sample is equal to the calibration value
Factor 1,12 result from reference sample is 12 % lower than the calibration value

To abort processing a Reference sample, click again the Reference button. It is possible to do it only before the
sample is processed.

4.8 CONCENTRATE SAMPLE MEASUREMENT

To measure an unknown sample, the maximum volume is limited by the size of the sample boats for the
autosampler.

Using the Concentrate function, a large volume sample can be split into several aliquots and processed in the
system separately. This means the amount of Hg is collected in the system until the end of concentration
function is selected.

To measure a Concentrate, for instance, create: three new lines in the “Results” table of “DMA-80
Measurement\Data”. Weigh the samples normally and type the amount of each one in each “Weight” field of
“Sample” table. Return to “Result” table, select the first sample line and click the “Concentrate” button. The first
two samples will be automatically selected. By clicking on the second sample and then on “Concentration”
button, the first three samples will be selected. For first and second line the setting of the program will change
to Amalgam time = “0” and Recording time = “0”.

Figure 19. Concentrate panel

The sample is processed (thermally decomposed) in the system and all the Hg is collected on the amalgamator,
without measurement of the Hg in the absorption cell. This procedure is repeated for all the subsequent
samples marked with the Concentrate function. All the collected Hg is measured together with the last sample
of the concentration process.
To abort both functions, click again the corresponding button. This is possible only before the sample is
processed.

4.9 ANALYSIS

To start analysis, first make sure that calibration curve is loaded. Open the “DMA-80 Calibration” and choose
the curve to use.

Return to the “ Methods” table.


Use a pre-stored method or create a new method. In “Method name” line, type in a name of the new method.
Change method parameters if needed and save.

4 OPERATING WITH THE UNIT 83


Milestone DMA-80 Operator Manual – Revision 01/2010

Under “Program” table (Fig. 20) change working parameters of the instrument for every sample, such as drying,
decomposition and waiting time, if needed. Drying time varies with the volume of the sample or with
percentage of the water in the sample and has to be calculated using the following equation:

Max start temperature: Measurement starts only when temperature T1 (drying- and
decomposition furnace) is under the maximum Start-Temperature. This prevents the sample
boats to be exposed to high temperatures especially when working with flammable sample.

µL) × 0.6. or
Drying time (sec) = Sample Volume (µ
Drying time (sec) = Sample weight (mg) × 0.6 x % H2O.
For dry inorganic samples
Drying time =10 sec
For high organic samples
Drying time =30 sec - 1 min 30 sec

Drying temperature = 200°C for most samples.


Reduce the drying temperature if you are working with flammable sample ( see applications notes).

Decomposition time is 3 min. for most samples.


Increase decomposition time if analysis resulted in high rsd (> 5 %)
Add 30 sec and analyze samples determining rsd again.
For Example, coal requires 300 sec(for others see application notes).

Decomposition temperature = 650°C for most samples (see also applications notes)

Purge time is 60 sec for most samples

After all samples are loaded into the sample tray (in case of automode) and the data entered in the “DMA
Measurement”, open the “Results” table of “DMA-80 Measurement\Data” and press the “Start” button.

As samples are analyzed, the absorbance will appear in “Result” table under “Height” column, absolute amount
of Hg in the sample under “Hg (ng)” column and Hg concentration in the “C(µg/kg)” (Fig. 2).

Figure 20. Method table

4 OPERATING WITH THE UNIT 84


Milestone DMA-80 Operator Manual – Revision 01/2010

5. EASYDOC SOFTWARE 3.3 FOR DMA-80

5.1 SOFTWARE

5.1.1 LICENSE AGREEMENT


This Software is protected by the copyright law and the International Copyright Agreement. Users are
bound to use this Software as a book. However users are authorized to download the Software for use in
a Computer, and are authorized to make copies provided they are required as backup copies or for the
protection of your investment.
The assimilation of the Software to a book means, for example, that, as it is not possible its simultaneous
use by several persons, the Software may be used by any number of persons, that it may be copied by a
computer or another, or may be moved from one operating place to another. Like a book cannot be read
by two different persons in two different places at the same time, so the software cannot be used by
different persons at different places without authorization (this would be a copyright infringiment).
You can increase the number of users with the acquisition of further individual software packages as
desired.

TRANSFER OF THE SOFTWARE


You can transfer your rights to use the software altogether to a third person. To do this it is required that
you transfer the complete software together with disks and documentation, therefore all components of
this software package and all copies thereof, or the not transferred copies must be destroyed. We remind
you that – once you have transferred the software to a third party, you are no more authorized to use it.
Also the person to whom you transferred the software, is entitled to use it in accordance with the
copyright law, the international copyright agreement and these prescriptions.
If you acquire an "Upgrade" of the Software, this will be based on an unit with the original software. For
example the Upgrade and the original software cannot be used by two different users at the same time
and the two versions cannot be transferred as separate one from another.

LIMITED WARRANTY
The manufacturing company MLS GmbH fully guarantee for 90 days from purchase that memory media
and documentation are free from material and labour defects. MLS / MILESTONE shall replace defective
memory media and documentation provided they are.
The aforementioned warranty is limited to being the defect funded. It is limited to the replacement of the
defective memory media or documentation. The replacement of other damages is excluded. This applies
in particular to loss of profit, loss of data, or non-usability of the software as well as indirect damages.
This limitation is valid also in case MLS had particular knowledge of the possibilities of damages. In any
case the responsibility of MLS for damages occurred to the user or to a third person is limited to an
amount which is the minimum paid according to price list for software package.
MLS / MILESTONE hereby expressly exclude all express or tacitly given warranties,
guarantees, or properties in particular all warranties related with usability of the software
for use in the frame of a planned contract. Any contrary conditions are not valid.
MLS / MILESTONE particularly do not take over any special warranty for the "defect-free" software or
documentation and also is not responsible for matching customers standards or special requirements. In
any case all express and tacitly given warranties on the properties of the memory media and
documentation are limited to a validity period of 90 days.
It is excluded any warranty for products, memory media, software or documentation not supplied nor
delivered by MLS / MILESTONE. This is particularly valid for programs of these parties which are intended
for use in connection with MLS-Software or which contain MLS-Programs or Files.

5 EASYDOC SOFTWARE FOR DMA-80


5 85
Milestone DMA-80 Operator Manual – Revision 01/2010

5.1.2 REGISTRATION

Read very carefully the License Agreement. The installation of the Software or issue of safety
copies of the program mean that you accepted the terms of the license agreement.

REGISTRATION
When started for the first time the Software must be
registered before use.
Click on Registration. The easyDOC Registration form will be
opened.

Registration screenshot

5 EASYDOC SOFTWARE FOR DMA-80


5 86
Milestone DMA-80 Operator Manual – Revision 01/2010

Name/Organization Enter your name and your company/organization

Registration No. Note the number on the yellow field

Online Registration Connect in Internet to the address www.preptec.net auf

Under Registration select Software

(Screen may be slightly different)


Fill in the form that will be opened. Enter the previously noted number into the
Registration field.

Key After sending out the form you will get via e-mail your Key-Number.
Enter this number into the Key field.

OK
As soon as you have filled all fields including the Key-Number, click
on OK. The Software is now ready to operate.

FAX REGISTRATION
You can also register the software via fax. A form will be opened
to be filled in and returned by fax to MLS.
Telefax: 0049-7561-981812

CANCEL
To quit the Menu without saving.

5 EASYDOC SOFTWARE FOR DMA-80


5 87
Milestone DMA-80 Operator Manual – Revision 01/2010

5.2 DOWNLOADING OF DATA FILES

5.2.1 GENERAL
The easyDOC software enables the downloading of all measured values and system parameters as well as
copies of screenshots from the terminal to a Windows-PC. All data can then be saved and filed on the PC,
opened, printed out and exported.
With easyDOC all data files can be displayed both in the form of graphics and tables.
The data files can be saved in Excel, ASCII, PDF and JPG formats.
No manipulations of the original data files are possible.
1 Install the easyDOC software on your PC or Laptop: Start the Setup-file and follow the
instructions for installation.

5.2.2 CONNECTION TERMINAL-PC

TERMINAL 1024

1 Connect your PC or Laptop via 0-Modem-cable with the PC-interface of the terminal 1024.

Terminal 1024 Connection for PC

TERMINAL 640/1640

1 With Terminal 640 all data are saved on a flash card. This
Flash card is read with a card reader connected to the PC.
Card types: Flash Cards Type PC-Card or CF-Card (Compact
Flash Card) can be used.
Memory capacity: the Terminal is supplied complete with a Flash
Card with minimum 128MB. All memory capacities can be used.
Since the files are very small, some MB are sufficient.

2 Milestone supply an USB pen for data transfer

5.2.3 START DOWNLOADING

1 Switch on the DMA with Terminal.


2 Start the easyDOC-Software on your PC.
3 Make in the Setup-Menu of the easyDOC-Software the relevant appropriate settings
(see Setup-Menu Chapter for more information).
4 Press Download, to start downloading

5 EASYDOC SOFTWARE FOR DMA-80


5 88
Milestone DMA-80 Operator Manual – Revision 01/2010

DOWNLOAD

DOWNLOAD
This operation will download the selected data-files
displayed by the easyDOC-Software from the terminal to the
PC. The data files can then be saved.

Download-screenshot

1 Select under Port the COM-interface of the PC for connection to the terminal.
After successful connection the listing structure of the terminal will be displayed.
2 Select the files to be downloaded to the PC and confirm with OK. The file is shown in the
easyDOC software and the question Save under will appear. The standard path for memory is
indicated in the Set-up settings.
3 Save the file.

5.2.4 SETUP

SETUP
The Setup Menu is started from the upper line of the menu

5 EASYDOC SOFTWARE FOR DMA-80


5 89
Milestone DMA-80 Operator Manual – Revision 01/2010

OK
To save settings.

CANCEL
To quit without saving.

PATH

Path Settings-screen

1 Here are selected the directories for the single file types.

RS232 COMMUNICATION

RS232 Communication-screenshot

1 To select the COM-port of the PC for the Terminal.

5 EASYDOC SOFTWARE FOR DMA-80


5 90
Milestone DMA-80 Operator Manual – Revision 01/2010

5.2.5 BACKUP

BACKUP
With the Backup-Tool it is possible to download and save
simultaneously multiple files on the PC.

Backup-screenshot

1 Select in the right window (under Save to) the directory path under which the files should be
saved.
2 Press the Synchronization button. If in the list there are files that were already downloaded
from the Terminal and are still present in the terminal, they will be displayed in the right
window.
3 Mark in the left window with a check-mark all the files to be downloaded.
4 Press the double arrow (in case only one file has to be downloaded, the single arrow must be
operated), to be able to download the files.

SYNCHRONIZATION
If the Terminal is synchronized with the PC-Directory, it will check which
files can be downloaded.

DOWNLOAD OF SINGLE FILES


The x-marked file will be downloaded.

DOWNLOAD OF MULTIPLE FILES


All files that are check-marked will be downloaded.

5 EASYDOC SOFTWARE FOR DMA-80


5 91
Milestone DMA-80 Operator Manual – Revision 01/2010

5.3 EASYDOC

After Start, the main easyDOC menu will be displayed.

Start-screenshot

5.3.1 END PROGRAM / EXIT

Touch Exit to end the program.

The program can also be ended via File ⇒ Exit .

5.3.2 MAIN BUTTONS

OPEN FILES
This opens the Explorer, which can open an existing file.
The path selected in Setup will appear. Select the desired Folder and
File.

A file can also be opened with File ⇒ Open.

MAKE SCREENSHOT
This will generate a copy of the terminal screen.

The point in the menu can also be recalled with


Communication ⇒ Screenshot

5 EASYDOC SOFTWARE FOR DMA-80


5 92
Milestone DMA-80 Operator Manual – Revision 01/2010

DOWNLOAD
The selected file will be downloaded from the terminal to the PC and
will be announced in the easyDOC-Software. The file can then be
saved.

The point in the menu can also be recalled with


Communication ⇒ Download.

See also File Dowmnloading chapter.

PRINT
Pressing the Print button the print preview will appear. The document
can then be printed out.

Files can also be printed via File ⇒ Print.

Print screen

5 EASYDOC SOFTWARE FOR DMA-80


5 93
Milestone DMA-80 Operator Manual – Revision 0/2009

PDF
This will generate a PDF of the current document.
Operating this button will open Explorer.
Indicate a name for the document and select the directory in which it
should be saved.

A PDF can also be generated with File ⇒ PDF.

BACKUP
With the Backup-Tool it is possible to download and save
simultaneously multiple files on the PC.

The point in the menu can also be recalled with File ⇒


Backup.

See also chapter of downloading of files.

5 EASYDOC SOFTWARE FOR DMA-80 94


Milestone DMA-80 Operator Manual – Revision 0/2009

TYPES OF FILES

DMA Calibration file


Detailed information on calibration of ths sytem is contained in the DMA
Operator Manual.

DMA Measurement file


Information about the DMA-80 measurements, like sample data,
measurement results and signal run.

DMA Method file


Information about methods.

System Protocol
Status of the system and modifications of settings.

5.3.3 CALIBRATION

CALIBRATION
System Parameters and diagram of the calibration are
represented.
1 Open or download a file with extension *.c80.

Calibration-screnshot

5 EASYDOC SOFTWARE FOR DMA-80 95


Milestone DMA-80 Operator Manual – Revision 0/2009

The heading of the columns may be different, depending on the way it was set in the DMA-
Software. Instead of Peak (Maximum value) the column can be designated as Area (Integral).

ZOOM

The graphic representation can only be zoomed within the axles.

Draw a rectangle from upper left to Increase cutout


lower right direction (keep left mouse ⇒
button pressed)

Draw a rectangle from lower right to Return to original size


upper left direction (keep left mouse ⇒
button pressed) (opposite directions)

Move in the diagram (keep right mouse Shift the diagram



button pressed)

FADE IN/OUT OF CURVES

Use the following buttons to fade in or out the corresponding curves.

SHOW CALIBRATION POINT


The numerical value at the corresponding calibration point will be
indicated.

SHOW CALIBRATION POINT OUT OF CALCULATION


The numerical value at the corresponding calibration point out of the
curve will be indicated.
The points marked with red x are not used to calculate the regression
coefficient. See DMA 80 Operator Manual.

Depending where the calibration point is, it is necessary to switch to the


other cuvette to show the related value.

GRAPHIC BUTTONS

COPY TO CLIPBOARD
The diagram is saved in the clipboard.

5 EASYDOC SOFTWARE FOR DMA-80 96


Milestone DMA-80 Operator Manual – Revision 0/2009

GRAPHIC EXPORT

EXPORT GRAPHIC
Data or diagrams can be exported in different formats.

Data/diagrams are copied in the clipboard.

Data/diagrams are saved in memory.

Data/diagrams are sent by e-mail.

Quit the screen.

Register Picture
▪ Bitmap, GIF, JPEG: image formats
Options: specify resolution
▪ Metafile: Format for 32-Bit-Windows-
Systems; Options: Activation of enhanced
with Win95 and over
Size: specify size
Keep aspect ratio: maintain aspect ratio with
scale.

Register Data
▪ Text: Text format
▪ XML: Extensible Markup Language,
Standard for definition of language.
▪ HTML: Hyper Text Markup Language,
Document format for definition of Hypertext
in World Wide Web
▪ Excel: Microsoft Office Excel-Tabele calcu-
lation program
Series: definition of data to be saved together
Include: definition of additional data to be
saved together.
Delimiter: Specify column separation

5 EASYDOC SOFTWARE FOR DMA-80 97


Milestone DMA-80 Operator Manual – Revision 0/2009

PRINT GRAPHIC/DIAGRAM

PRINT GRAPHIC
Print window will be opened
The window shows a side view of the easyDOC Report.This contains the
data of the current project.

Graphic print screenshot

SAVE AS

SAVE SAMPLE TABLE AS EXCEL FILE


Data will be exported as Excel file.
The marked calibration points (column P) are used to calculate the
calibration curve. These points are marked „True“ in the Excel Table.

SAVE SAMPLE TABLE AS ASCII


Data are exported as ASCII-files.

5 EASYDOC SOFTWARE FOR DMA-80 98


Milestone DMA-80 Operator Manual – Revision 0/2009

5.3.4 SAMPLE

SAMPLE
Data files with extension *.d80 can be opened.
The screen on the left will show the data for Sample, Program
and Results. The right side shows the signal process of the
selected sample.

Sample-screenshot

1 Click on overview selection to sort out the column in ascendent or


descendent order.

SAVE SAMPLE TABLE (SIGNAL) AS EXCEL FILE


Data are exported as Excel-file.

SAVE SAMPLE TABLE (SIGNAL) AS ASCII


Data are exported as ASCII-file.

5 EASYDOC SOFTWARE FOR DMA-80 99


Milestone DMA-80 Operator Manual – Revision 0/2009

COPY SAMPLE TABLE (SIGNAL) TO CLIPBOARD


The values are saved in the clipboard.

PRINT SIGNAL
Print window will be opened.

PROCESS FADE-IN AND OUT

SHOW GRAPHIC
The signal diagram can be faded in or out with the following buttons.

SHOW GRAPHIC MARKS


With the following buttons you can fade-in or out signal height, retention
time and half widths.

CHANGE SCALE

CHANGE SCALE
The axle scale can be changed to preset values for a better view.

Register Graphic Setting


1 Enter the values for axle scaling directly
into the corresponding fields.

Quit the menu without saving.

The values are applied and the window remains open.

Values are saved.

AUTO SCALING
Axles are automatically adjusted to the optimal scale.

5 EASYDOC SOFTWARE FOR DMA-80 100


Milestone DMA-80 Operator Manual – Revision 0/2009
STATISTICS

SHOW STATISTIC
This will open a window to show statistics. The currently opened file can
now be downloaded with Refresh Resuls..
▪ The file is shown as a table in the upper part of the screen.
▪ In the center of the screen are shown the numerical values of maximum
and minimum, average and absolute or relative standard deviation.
▪ In the lower part of the screen is shown the diagram of the marked
single values and the average. The single values are shown as a curve of
the marked numbers.

1 Click on Refresh Results, to transfer the currently opened file.


2 Check-Mark the values to be shown.

Sample-Bildschirm

REFRESH RESULTS
The currently opened file will be transferred to statistics elaboration.

5 EASYDOC SOFTWARE FOR DMA-80 101


Milestone DMA-80 Operator Manual – Revision 0/2009

SAVE RESULT TABLE (CHART) AS EXCEL FILE


The file is exported as Excel file.

SAVE RESULT TABLE (CHART) AS ASCII


The file is exported as ASCII-file; or the diagram will be exported as
graphic file.

COPY RESULT TABLE (CHART) TO CLIPBOARD


The results will be copied in the clipboard.

PRINT GRAPHIC
The print window will be opened.

CHANGE UNIT
To switch from [µg/kg] to [mg/kg].

SHOW GRAPHIC MARKS


With the following buttons the results can be faded in or out.

CHANGE SCALE
The axle scale for R Results can be changed to preset values for better
view.

AUTO SCALING
The axles are automatically adjusted to the best scale.

CLOSE STATISTIC
The statistic window will be closed.

5 EASYDOC SOFTWARE FOR DMA-80 102


Milestone DMA-80 Operator Manual – Revision 0/2009

5.3.5 PARAMETER

PARAMETER
Here are shown the parameters for calibration and sample
measurement.

Depending on the type of file that is open (Calibration or Sample) the calibration parameters
are shown on the left and the sample parameters on the right.

Parameter-Bildschirm

5.3.6 DISPLAY

DISPLAY
This generates a copy of the Terminal screen.
A dialog is shown for downloading of the screen.
 Select an interface port (e.g. COM1) and press OK to
confirm. The downloading will be started.

SAVE SCREENSHOT AS
The file will be saved as image file (*.jpg).

5 EASYDOC SOFTWARE FOR DMA-80 103


Milestone DMA-80 Operator Manual – Revision 0/2009

COPY CAPTURE
The file will be saved to the clipboard.

PRINT GRAPHIC
The print window will be opened.

5.3.7 TRAIL

TRAIL
This will collect the protocol of the system (Trail files *.trl). All
changes are noted in the MLS Terminal.

SAVE DEVICE TRAIL AS


The file is saved as ASCII.

COPY DEVICE TRAIL


The file is saved in the clipboard.

5.3.8 METHOD

METHOD
Methods, i.e. Files with extension *.m80 can be opened.

Method-screenshot

SAVE DMA METHOD AS ASCII FILE


The file is exported as Excel file

COPY DMA METHOD GRAPH TO CLIPBOARD


The graphic is saved in the clipboard.

5 EASYDOC SOFTWARE FOR DMA-80 104


Milestone DMA-80 Operator Manual – Revision 01/2010

6 DMA-80 MAINTENANCE

6.1 HOW TO REMOVE THE CATALYST AND THE AMALGAMATOR

During routine maintenance of the DMA-80, both the unit and the labTerminal should
be turned OFF and disconnected from the power supply. The oxygen supply must be
turned OFF at the tank. Change the internal consumables only after the unit has
cooled to room temperature.
Wear body protection during the maintenance!

Open the unit using housing key.

Lift the hinged chassis cover to expose the internal


components.

Remove the red screw and the amalgamator cover to


provide access to the amalgamator.

6 DMA-80 MAINTENANCE 105


Milestone DMA-80 Operator Manual – Revision 01/2010

Using a razor blade, cut the silicon joint between the


cuvette and the amalgamator, on the left side of the
amalgamator.

Use a new razor, the silicon tube is flexible


and the heater coil is fragile and may
become deformed.

Cut the silicon joint between the amalgamator and the


catalyst tube, on the right side of the amalgamator.

Loosen the red screw located on the cuvette module and


remove it.

Move the cuvette module left.

6 DMA-80 MAINTENANCE 106


Milestone DMA-80 Operator Manual – Revision 01/2010

Clean the amalgamator tube from the residue of


junctions tube using the razor – see next picture.

Completely remove any residual silicon


joint material from the right end of the
amalgamator using the razor blade,
otherwise the fragile
heater coil could be deformed or damaged.

Remove the amalgamator from the heating coil.

Remove any residual silicon joint material from the


catalyst tube using the razor.

The ceramic support between the catalyst


tube and the ceramic cylinder may be
damaged -
our suggestion is when using the razor
move it horizontally from left to right,
removing (shaving) a small piece with each
pass.

6 DMA-80 MAINTENANCE 107


Milestone DMA-80 Operator Manual – Revision 01/2010

The next picture shows the cleaned left end of the


catalyst tube.

Remove any residual silicon joint material from the


cuvette block. Below is a picture of the cleaned block.

Unscrew the two red screws from the


drying/decomposition oven cover.

Remove the shield.

6 DMA-80 MAINTENANCE 108


Milestone DMA-80 Operator Manual – Revision 01/2010

Close the oxygen gas flow before


performing the following operation!

Remove the oxygen supply connector, on the rear of the


instrument, by pushing in the connector on the unit with
your hand and then pulling on the gas tube.
Now the internal gas pressure is relieved and it is
possible to manually move the pneumatic actuators from
left to right.

The next picture shows the actuators in the fully


retracted (open) position.

Unscrew the red screws located on the left and right of


the catalyst module.
Gently pull the oven forward on the tracks until it stops.

Loosen the screws to free the module, but


do not completely remove the screws.

6 DMA-80 MAINTENANCE 109


Milestone DMA-80 Operator Manual – Revision 01/2010

The next picture shows the oven in the fully open


position.

The next picture shows the flange, on the right hand


side of the oven module, that holds the catalyst tube.

Remove the flange using the 4 mm hexdriver.

Separate the flange from the catalyst tube.

Using your finger, gently push and hold


the catalyst tube in place during this
process.

6 DMA-80 MAINTENANCE 110


Milestone DMA-80 Operator Manual – Revision 01/2010

Remove the Silicon o-ring from the catalyst tube.

The next picture shows the silicon O-ring enclosed in


the package of the spare parts of the catalyst tube P/N
8333.

When replacing the catalyst and


amalgamator, the silicon joints and all the
o-rings should be changed to ensure
proper operation of the instrument.

Gently remove the catalyst tube by pulling straight out.

After removing the o-rings, clean inside


of the flange with a tissue to remove
any combustion or sample processing
residues.

If the “ceramic insulating disc” on the left hand side of


the oven is cracked, proceed to the next step. If it is
fine, proceed to Chapter 6.2, “How to install the
catalyst and Amalgamator”.

6 DMA-80 MAINTENANCE 111


Milestone DMA-80 Operator Manual – Revision 01/2010

Remove the drying decomposition coil.

Use the long screw driver to push the “ceramic insulator


disc” out of the catalyst oven. Insert the new “ceramic
insulator disc” from the right side of the catalyst oven
Clean the drying /decomposition coil leads with
sandpaper to ensure good electrical contact. Then
reinstall those leads into their original positions in the
bottom of the ceramic connector block. The coil leads
are in series with electrical power wires (red wires)
already connected to the ceramic connector block from
the top. Tighten the coil leads firmly.

6.2 HOW TO INSTALL THE CATALYST AND THE AMALGAMATOR

Remove the stoppers from the new catalyst tube.

Introduce the new catalyst tube avoiding contact with


the heating coil.

6 DMA-80 MAINTENANCE 112


Milestone DMA-80 Operator Manual – Revision 01/2010

The next picture shows the correct position of the


catalyst and the “ceramic insulator disc” inside the
catalyst module.
To the amalgamtor

The left end of the catalyst tube will emerge as


shown, check the correct position between the
catalyst tube and the “ceramic insulator disc” from the
left side of the catalyst module.

Put a new silicon joint on the catalyst tube.

Avoid direct contact of the silicon


joint with either the “ceramic
insulator disc” or the steel support,
the high operating temperature will
damage the silicon joint, causing
problems with the gas flow.

Introduce the Silicon o-ring onto the catalyst tube.

6 DMA-80 MAINTENANCE 113


Milestone DMA-80 Operator Manual – Revision 01/2010

Install gently the steel flange on right hand end of the


catalyst tube and secure it using 4 mm hex driver.
Make sure that there is no gap between catalyst and
flange lip. The end of the catalyst tube should be fully
in contact with the flange.
Using your finger, gently push and hold the catalyst
tube in place during this process.

Push the catalyst oven module back to its fully


installed position and secure the module.

Make sure the module does not rise


up as the screws are being tightened.
A rising oven indicates that the screws
are not in their proper path.

The picture below shows the correct position of the


amalgamator in the unit.

To the cuvette From the


catalyst

Gas flow

Introduce the new amalgamator as shown.

6 DMA-80 MAINTENANCE 114


Milestone DMA-80 Operator Manual – Revision 01/2010

Connect the amalgamator with a new silicon joint.

The filling of the amalgamator must be


completely and uniformly covered by the
heater coil.
If needed, the coils can be slightly
stretched to cover the amalgamator.

Make sure that the unit is


disconnected from the power supply
before performing this operation!

Now connect the cuvette block to the amalgamator


using another new silicon joint, then, tighten the red
screw on the cuvette module to secure the module.
The amalgamator tube should not be in direct contact
with either the cuvette block or the catalyst tube. It
should essentially float in the silicon joints with a gap
of 2 mm at each end between the amalgamator and
the cuvette / catalyst tube.

Replace the drying/decomposition coil shield as well


as the amalgamator cover using the red screws. Now
the catalyst and the amalgamator are correctly
installed.

Manually move the pneumatic actuators from right to


left, making sure that it is aligned correctly, see
chapter “How to do the alignment of the pneumatic
actuators”.

Close the chassis using the housing key to lock the


housing. Replace the sample tray. Connect the power
cord and oxygen. Now open the oxygen flow.
After approx. 15 minutes the message “READY” will
indicate that the DMA-80 is ready to work.

To avoid damage to the regulator


diaphragm, open the tank valve only
when the DMA-80 unit and Terminal
or PC are comunicating, then make
adjustments to the pressure from 0 to
4 bar (60 psig).

6 DMA-80 MAINTENANCE 115


Milestone DMA-80 Operator Manual – Revision 01/2010

Before starting the calibration, a procedure for catalyst/amalgamator’s activation is necessary:

Tri-cell DMA 80 – procedure for catalyst/amalgamator’s activation


Run Reagent/ Sample Max START Drying/Ashing Drying/Ashing Purge Time
Sample type amount Temperature Time Temperature
n.1 Flour 1 minute 200°C
100 mg 200°C 60sec
n.2 HNO3 5% * 2 minutes 650°C
1 minute 650°C

*: quartz boat (suggested)

Repeat at least 5 times the above procedure, up to absorbance < 0.0030

After conditioning a stability test is required.


Repeat 5 times: a fresh aqueous standard of 100ppb, the RSD must be <1.5%.
For this evaluation is not important the recovery but only the DMA stability so the previous calibration curve can be
used.

If the stability test is according to the specs, please proceed making new calibration (see user manual), otherwise
repeat the conditioning procedure again.

If the unit is not used for long time, the procedure for catalyst/amalgamator’s activation is
suggested!

It is suggested that the mercury sample boats be cleaned before starting to work with the samples. To do
this, bake them out collectively in a muffle furnace or use the following program:

Max START Drying/Ashing Time Drying/Ashing Purge


Temperature Temperature Time
2 minute 650°C
200°C 60 sec
1 minute 650°C

Repeat this cleaning procedure until the absorbance is a stable, low number < 0.003

Note: consult the available Application Notes before starting to work with the unit; some samples, such as
crude oil, require a dedicated or specific configuration of the system.

You are now ready to work!

6 DMA-80 MAINTENANCE 116


Milestone DMA-80 Operator Manual – Revision 01/2010

6.3 HOW TO DO ORDINARY MAINTENANCE TO THE PNEUMATIC ACTUATORS

Release the oxygen as explained in the first part of the


Maintenance chapter.
Open the horizontal pneumatic actuator (sample boat
delivery arm).

The next picture shows how to clean the sample boat


holding forks of the actuator using sand paper.

Replace the O-ring ∅ 20x3mm seal for the boat holder


P/N OR0024.

Put a very minor quantity of the maintenance grease on


the O-ring. The quantity should barely “wet” the surface
of the o-ring. There should be no visible “gobs” of
lubricant.

6 DMA-80 MAINTENANCE 117


Milestone DMA-80 Operator Manual – Revision 01/2010

Spread the maintenance grease on the o-ring using your


finger. It may be easier to first remove the o-ring.

Also, periodically use the maintenance grease to lightly


lubricate all the exposed steel rods of the horizontal and
vertical actuators, as shown.

6 DMA-80 MAINTENANCE 118


Milestone DMA-80 Operator Manual – Revision 01/2010

6.4 HOW TO PROPERLY ALIGN THE HORIZONTAL ACTUATORS

Release the oxygen as explained in the first part of the


Maintenance chapter. Fully retract the horizontal
actuators. Check the alignment position between the
sample boat holder and the flange. Check that the
sealing o-ring on the boat holder is making uniform
contact all around the flange. If it is not centered, see
the procedure below.

To perform vertical adjustment of the horizontal


actuator, do the following:

The horizontal actuator is secured to a steel platform


connected to the bottom plate of the instrument
chassis. Use a 4 mm hex driver to loosen the two
screws that secure the actuator platform to the bottom
plate. Use a 7 mm wrench to perform the alignment by
adjusting the hex nut shown in the figure.

Turning the alignment nut clockwise will raise the


actuator slightly with each turn. Turning the alignment
nut counterclockwise will lower the actuator slightly
with each turn. Remember to secure the two hex
screws to the bottom plate when finished making the
adjustment.

6 DMA-80 MAINTENANCE 119


Milestone DMA-80 Operator Manual – Revision 01/2010

The horizontal actuator must also be properly aligned


front to back with respect to the instrument platform.
The picture shows the correct alignment resulting in a
uniform closing of the sealing o-ring.

The next picture shows poor contact of the sealing o-


ring toward the back side of the flange. The actuator is
positioned too far forward.

The next picture shows poor contact of the sealing o-


ring toward the front side of the flange. The actuator is
positioned too far back.

6 DMA-80 MAINTENANCE 120


Milestone DMA-80 Operator Manual – Revision 01/2010

Use a 3 mm hexdriver to make the adjustment. Each


time an adjustment is made, both screws should always
be turned, in opposite directions, and to the same
extend of rotation. Turning the left screw clockwise
(and the right screw counterclockwise) will move the
actuator, in the horizontal plane toward the front of the
chassis. Turning the right screw clockwise (and the left
screw counterclockwise) will move the actuator in the
horizontal plane toward the back of the chassis.

The last picture shows the actuator in the fully closed


position under oxygen flow. Note that the sample boat
holder is completely inserted into the flange and that
the sealing o-ring is not visible.

6 DMA-80 MAINTENANCE 121


Milestone DMA-80 User Manual – Revision 01/2010

7 APPENDIX “21 CFR 11 COMPLIANCE”

7.1 DESCRIPTION OF COMPLIANCE OF DMA-80 SOFTWARE WITH FDA 21 CFR-11

The Tri-cell DMA-80 System with control software fulfils the requirements of a “Closed System“.

21 CFR 11 Requirement DMA-80 Software Approach


Subpart B Data records in electronic form
11.10 Controls for "Closed Systems"

11.10 (a) Validation of systems The Owner / Operator of the Tri-cell DMA-80 can
establish a Validation of the Tri-cell DMA-80 software,
if one is desired. On request "Milestone" can provide
detailed documentation on the software development,
test, update, administration and filing.

11.10 (a) Ability to discern invalid or The Tri-cell DMA-80 Software controls the validity of
altered data records. the data on the basis of check sums. Altered records
cannot be opened or used.

11.10 (b) Ability to generate accurate All data records can be viewed, copied and printed
and complete copies of data with the Tri-cell DMA-80 Software and the PC utility
records program “easyWAVE”. With the utility program
"easyVIEW" the data can be exported in any standard
Windows Text format.

11.10 (c) Protection of records to The data records can always be viewed and printed,
enable their accurate and using the same version of Tri-cell DMA-80 Software
ready retrieval that was used for their recording.
Additionally they can be exported with the PC utility
program "easyVIEW" in any standard Windows Text
Format. These files can be viewed with every text
editor.

11.10 (d) Limited system access to The Tri-cell Dma-80 system fulfils the requirements of
authorized persons a "Closed System". Access to the system is divided
into 3 levels
- Supervisor + Service
- Administrator
- User
Access to the appropriate level is only possible by
using a write-protected electronic access card and an
additional password.
Every access level has different rights on the system
and control parameters which cannot be modified.

11.10 (e) Complete and secure A Process Report (History trail) captures all changes
recording of changes on the on the system that have influence on the analytical
system results or data recording.
The Process Report includes date, time, user name
and access level, and the kind of action that was

DMA-80 Software with 21CFR, PART 11 122


Milestone DMA-80 User Manual – Revision 01/2010

accomplished.

11.10 (f) Operational System checks The Owner / Operator of the Tri-cell DMA-80 System
to enforce permitted can establish and enforce Standard Operating
sequencing of steps. Procedures (SOP) for permitted sequencing of steps,
within the context of the “closed system” features and
functions of the System as delivered by the
Manufacturer. Calibration Checks, and Blank
Determination, as described in the System
documentation, are the only Operational Performance
checks provided by the Manufacturer.

11.10 (g) Use of authority checks The Tri-cell DMA-80 System fulfils the requirements of
a "Closed System". Access to the system is divided
into 3 levels
- Supervisor + Service
- Administrator
- User
Access to the appropriate level is only possible by
using a write-protected electronic access card and an
additional password.
Every access level has different rights on the system
and control parameters which cannot be modified.

11.10 (h) Use of device checks… In the Tri-cell DMA-80 System, data are generated by
validity of source data a Tri-cell DMA-80 Direct Mercury Analyzer directly
connected to the related control terminal with control
software. The terminal and software are dedicated to
the task. There are no other data sources
communicating with the terminal or software. For this
reason device checks are not necessary.

11.10 (i) Training of the persons All persons with access authorization for Service
according to their assigned and/or Supervisor level receive appropriate Education
access authorization. and Training by the Manufacturer. Education and
training of system operators (Administrator and User
level) is provided by the Manufacturer’s
Representative within the context and at the time of
the initial on-site installation of the system. Education
And Training of additional system operators is the
responsibility of the Owner / Operator of the Tri-cell
DMA-80. On request, supplemental Education and
Training courses can be provided by the
Manufacturer’s Representative.

11.10 (j) Responsibility for the The Owner / Operator of the Tri-cell DMA-80 System
execution of electronic can establish policies that hold individuals accountable
signatures. and responsible for all actions initiated under their
electronic signatures.

11.10 (k)(1) Controls over distribution The Owner/Operator of the Tri-cell DMA-80 System is
and access of the system responsible for establishing and using appropriate

DMA-80 Software with 21CFR, PART 11 123


Milestone DMA-80 User Manual – Revision 01/2010

documentation. controls over system documentation including access


to and use of Tri-cell DMA-80 System Documentation
for operation and maintenance.

11.10 (k)(2) Controls over System The Owner/Operator of the Tri-cell DMA-80 System
Document Revisions and are responsible for establishing and using appropriate
Change Control Procedures. controls over Tri-cell DMA-80 System Documentation
revisions and Change Control procedures.
11.50 Signature manifestations

11.50 (a)(1) Data records with electronic Together with the Signature; the complete Name /
signature must show the Identification of the person is printed out.
complete, printed names.

11.50 (a)(2) Data records with electronic Together with the signature; the date and time of the
signature must include the execution of the signature are printed out...
date and the time of the
execution of the signature.

11.50 (a)(3) Data records with electronic Together with the signature; the meaning of the
signature must contain the signature is printed out.
meaning of the signature.

11.50 (b) For the electronic signature The electronic signature is part of the Tri-cell DMA-80
the same controls as for data record and therefore undergoes the same
electronic data records must controls as the data records themselves.
be applied.

11.70 Signature / record linking

11.70 Secure linking of the The electronic signature is imbedded as part of the
signature with the data Tri-cell DMA-80 data record and cannot be separated,
record copied or transferred from the data record by ordinary
means.
Subpart C Electronic Signatures

11.100 (a) Unique identification of each The Tricell DMA-80 System prevents the repeated use
Person of the same password for different users.
Each user must identify him using a write-protected
electronic access card and an additional password.

11.100 (b) Verification of the identity of The Owner / Operator of the Tri-cell DMA-80 System
the signature must verify the identity of the individual prior to
assigning a write-protected electronic access card and
password.

11.100 (c) Certification of electronic The Owner / Operator of the Tri-cell DMA-80 System
signatures. is responsible for communicating with the Agency
regarding the use, authenticity, and intended
equivalence of electronic signatures for hand written
signatures.

DMA-80 Software with 21CFR, PART 11 124


Milestone DMA-80 User Manual – Revision 01/2010

11.200 Electronic Signature Components and Control

11.200 (a)(1) Use of two different To access the Tri-cell DMA-80 System and for
components for the executing the electronic signature, unique
identification. identification is required using a write-protected
electronic access card and an additional password.

11.200 Signature components used To gain access to the Tri-cell DMA-80 System, unique
(a)(1)(i) for a series of signings identification must be made by the write-protected
during a continuous access electronic access card and an additional password.
period. During a single continuous period of controlled access,
the presence of the electronic access card installed in
the system, is sufficient for repeatedly executing the
signature. The presence of the electronic access card
is polled for automatically.

11.200 Signature components used To gain access to the Tri-cell DMA-80 System, unique
(a)(1)(ii) during discontinuous access identification must be made by the write-protected
periods. electronic access card and an additional password. If
the electronic access card is removed from the
system, then the access period is terminated. To
regain access to the Tri-cell DMA-80 System, the
unique identification must again be made using the
write-protected electronic access card and the
additional password.

11.200 (a)(2) Signature Components used Each user of the Tri-cell DMA-80 System chooses their
only by the genuine owner own unique password to associate with the write-
protected electronic card assigned to them for their
personal use by the Owner / Operator of the System.

11.200 (a)(3) Attempted misuse of The Owner / Operator of the Tri-cell DMA-80 System
Signature Components. is responsible for administering and executing
electronic signature components in such a way that
the collaboration of two or more individuals is required
in any attempt to misuse the electronic signature
owned by another user.

11.300 Controls for identification codes / passwords

11.300 (a) Combination of The Tri-cell DMA-80 System prevents the use of the
identification and password same password in association with different electronic
must be unique. cards. Each user of the Tri-cell DMA-80 System must
identify himself to the system using a write-protected
electronic access card and a unique additional
password.

11.300 (b) Periodic checks of the The Owner /Operator of the Tri-cell DMA-80 System
passwords. are responsible for periodic review, maintenance and

DMA-80 Software with 21CFR, PART 11 125


Milestone DMA-80 User Manual – Revision 01/2010

reissue of electronic access cards and passwords.

11.300 (c) Loss management Access to the Tri-cell DMA-80 System is in 3 levels
procedures - Supervisor + Service
- Administrator
- User
A superior level can, at any time, administer and also
delete the subordinate levels.

11.300 (d) Transaction Safeguards to If more than three (3) consecutive attempts to access
prevent unauthorized use of the system fail due to incorrect combination of
passwords electronic access card and password time, the incident
will be indicated in the Process Report (History trail).
The Owner / Operator of the Tri-cell DMA-80 System
must ensure that the Process Reports are evaluated at
reasonable time intervals.

11.300 (e) Periodic test of the function During each access to the system the functioning of
of the system security the write-protected electronic access card and
checks. associated password are checked.
If damage is present in the electronic access card or
the card reader, access will be denied.
The software with the administration of the password
points cannot be deleted or installed by the user.
For this reason this point cannot be used.

DMA-80 Software with 21CFR, PART 11 126


Milestone DMA-80 Operator Manual – Revision 01/2010

8 DMA EC SAFETY DATA

8.1 AMALGAMATOR FOR DMA-80 EC SAFETY DATA

Identification Amalgamator for DMA-80

Trade name Gold-based absorber

Hazardous ingredients Gold content about 3% hazard symbols : -


silicate hazard symbols : -

Hazards identification Not identified according directive 67/548/EWG

First aid measures


after inhalation not applicable
after contact with skin no risk
after contact with eyes remove particles by rinsing with water
after ingestion when swallowed do induce vomiting

Accident release
measures
Personal precaution no special protection required
Methods for cleaning up mechanical cleaning

Storage The material is delivered inside of a quartz tube.


Store the tube in a cool, dry, well-ventilated place

Handling Contact to the human body is only possible when the


quartz tube is broken. No special protection required

Physical and chemical


properties
Appearance Solid particles, with reddish colour, odourless
Flash point not applicable
explosion limit not applicable
solubility in water insoluble

Ecological Do not discharge product unmonitored into the


considerations environment

Disposal considerations No special regulations available

8 DMA-80 SAFETY DATA 127


Milestone DMA-80 Operator Manual – Revision 01/2010

8.2 CATALYST FOR Tri-cell DMA-80 (optional) EC SAFETY DATA

Identification Catalyst for DMA-80


Trade name Co-Mn-oxyde catalyst
Hazardous ingredients Potassium hydroxide, hazard symbols C
Cobaltoxid, hazard symbols Xn
Hazards identification Harmful if swallowed
Causes severe burns
Possible risks of irreversible effects.
May cause sensitization by skin contact

First aid measures:


after inhalation Remove the casualty into fresh air and keep him calm.
after contact with skin In case of contact with skin wash off immediately
with plenty of water.
after contact with eyes In case of contact with eyes rinse thoroughly
with plenty of water and seek medical advice.
after ingestion When swallowed, allow water to be drunk.
Do not induce vomiting.
Summon a doctor immediately
hints for the physician Allergic symptoms

Accident release
measures:
Personal precaution Ensure adequate ventilation
Use personal protective clothing
Methods for cleaning up Avoid raising dust
Take up with absorbent material (e.g. sand, kieselguhl,
universal binder)
Pick for disposal in tightly closed container
Storage The material is delivered inside of a catalytic tube.
Store the tube in a cool, dry, well-ventilated place.
Handling Contact to the human body is only possible when the
catalyst tube is broken. Wear goggles, rubber gloves,
protective clothing. Ensure adequate ventilation
Physical and chemical
properties
Appearance Solid, with black – brown colour, odourless
Flash point not applicable
explosion limit not applicable
solubility in water partly soluble, alkaline solution is formed
Ecological Do not discharge product unmonitored into the
considerations environment
Disposal considerations In accordance with regulations for special waste
Must be taken to a special waste disposal site

8 DMA-80 SAFETY DATA 128


Milestone Srl Material Safety Data Sheet
Date Updated: 08th February, 2012

1 - Product and Company Information Wear self-contained breathing apparatus and protective
clothing
Product Name SAMPLE ADDITIVE A to prevent contact with skin and eyes.
Product Number DMA-80 - SFA
Company Milestone S.r.l. 6 - Accidental Release Measures
Via Fatebenefratelli, 1-5
I-24010 Sorisole (BG) PROCEDURE(S) OF PERSONAL PRECAUTION(S)
Technical Phone # 39-035 573857 Wear respirator, chemical safety goggles, rubber boots,
Fax 39-035 575498 and heavy rubber gloves.
E-mail address application@milestonesrl.com METHODS FOR CLEANING UP
Sweep up, place in a bag and hold for waste disposal.
2 - Hazards Identification Avoid
raising dust. Ventilate area and wash spill site after
SPECIAL INDICATION OF HAZARDS TO HUMANS material pickup is complete.
AND THE ENVIRONMENT
Irritating to eyes and respiratory system. 7 - Handling and Storage

3 - Composition/Information on Ingredients HANDLING


Directions for Safe Handling: Do not breathe dust. Avoid
Product Name EC no Annex I contact
Index Number with eyes, skin, and clothing. Avoid prolonged or
Hydratated Aluminasilicated minerals None None repeated exposure.
STORAGE
Conditions of Storage: Keep tightly closed.
4 - First Aid Measures
SPECIAL REQUIREMENTS: Hygroscopic.
AFTER INHALATION
If inhaled, remove to fresh air. If not breathing give 8 - Exposure Controls / Personal Protection
artificial respiration. If breathing is difficult, give
oxygen. ENGINEERING CONTROLS
AFTER SKIN CONTACT Safety shower and eye bath. Mechanical exhaust
In case of contact, immediately wash skin with soap and required.
copious GENERAL HYGIENE MEASURES
amounts of water. Wash thoroughly after handling.
AFTER EYE CONTACT PERSONAL PROTECTIVE EQUIPMENT
In case of contact, immediately flush eyes with copious Respiratory Protection: Use respirators and components
amounts tested and
of water for at least 15 minutes. approved under appropriate government standards such
AFTER INGESTION as NIOSH (US)
If swallowed, wash out mouth with water provided or CEN (EU). Where risk assessment shows air-purifying
person is respirators
conscious. Call a physician. are appropriate use a dust mask type N95 (US) or type P1
(EN 143) respirator.
Hand Protection: Compatible chemical-resistant gloves.
5 - Fire Fighting Measures
Eye Protection: Chemical safety goggles.
EXTINGUISHING MEDIA
Suitable: Water spray. Carbon dioxide, dry chemical 9 - Physical and Chemical Properties
powder, or
appropriate foam. Appearance Physical State: Solid
SPECIAL RISKS Property Value At Temperature or Pressure
Specific Hazard(s): Emits toxic fumes under fire pH N/A
conditions. BP/BP Range N/A
SPECIAL PROTECTIVE EQUIPMENT FOR MP/MP Range N/A
FIREFIGHTERS Flash Point N/A
Flammability N/A

Sample Additive A - Page 129/130 - Rev. 01/2012


Autoignition Temp N/A 13 - Disposal Considerations
Oxidizing Properties N/A
Explosive Properties N/A SUBSTANCE DISPOSAL
Explosion Limits N/A Contact a licensed professional waste disposal service to
Vapor Pressure N/A dispose of this material.
SG/Density N/A Dissolve or mix the material with a combustible solvent
Partition Coefficient N/A Miscellaneous Data N/A and burn in a
Viscosity N/A Solubility N/A chemical incinerator equipped with an afterburner and
Vapor Density N/A scrubber.
Saturated Vapor Conc. N/A Observe all federal, state, and local environmental
Evaporation Rate N/A regulations.
Bulk Density N/A
Decomposition Temp. N/A 14 - Transport Information
Solvent Content N/A
Water Content N/A
RID/ADR
Surface Tension N/A
Non-hazardous for road transport.
Conductivity N/A
IMDG
Non-hazardous for sea transport.
10 - Stability and Reactivity IATA
Non-hazardous for air transport.
STABILITY
Stable: Stable. 15 - Regulatory Information
Conditions to Avoid: Moisture.
Materials to Avoid: Hydrogen fluoride, Strong acids,
CLASSIFICATION AND LABELING ACCORDING
Strong bases,
TO EU DIRECTIVES
Strong oxidizing agents.
INDICATION OF DANGER: Xi
HAZARDOUS DECOMPOSITION PRODUCTS
Irritant.
Hazardous Decomposition Products: Nature of
R-PHRASES: 36/37
decomposition products not known.
Irritating to eyes and respiratory system.
HAZARDOUS POLYMERIZATION
S-PHRASES: 26
Hazardous Polymerization: Will not occur
In case of contact with eyes, rinse immediately with
plenty of water and seek medical advice.
11 - Toxicological Information
16 - Other Information
SIGNS AND SYMPTOMS OF EXPOSURE
To the best of our knowledge, the chemical, physical, and
WARRANTY
toxicological properties have not been
The above information is believed to be correct but does
thoroughly investigated.
not
ROUTE OF EXPOSURE
purport to be all inclusive and shall be used only as a
Skin Contact: May cause skin irritation.
guide. The
Skin Absorption: May be harmful if absorbed through the
information in this document is based on the present state
skin.
of our
Eye Contact: Causes eye irritation.
knowledge and is applicable to the product with regard to
Inhalation: May be harmful if inhaled. Material is
appropriate safety precautions. It does not represent any
irritating to mucous membranes and upper respiratory
guarantee of the properties of the product. Milestone Srl,
tract.
shall not be held liable for any damage resulting from
Ingestion: May be harmful if swallowed.
handling or
from contact with the above product.
12 - Ecological Information

No data available.

DISCLAIMER
For R&D and chemical laboratory use only. Not for drug, household or other uses.

Sample Additive A - Page 130/130 - Rev. 01/2012


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

You might also like