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LabAnalyzer 254

Operating Manual
English
Version 5.2

Manufacturer: Mercury Instruments GmbH


Liebigstrasse 5
85757 Karlsfeld / Germany

service@mercury-instruments.de

© 2016 by Mercury Instruments GmbH, Karlsfeld (Germany)


LabAnalyzer 254

General information
for safe operation

• Do not operate instrument if it is damaged.


• When connecting the photometer unit (basically a VM-3000) of the
LabAnalyzer 254 to a power source please note the related safety
regulations.
• The photometer unit of the LabAnalyzer 254 must be operated from
the type of power source indicated on the rating plate.
• Make sure that plugs and power cord are not damaged.
• Regulations for prevention of accidents are to be observed.
• Before opening the photometer unit of the LabAnalyzer 254
disconnect it from the mains supply.
• Repairs and maintenance on the opened and powered instrument
must be carried out by trained personnel only.
• Operate the LabAnalyzer 254 on a stable and dry surface. The interior
of the photometer unit must never get moist or wet. In case it does get
wet or moist consult an expert.
• The LabAnalyzer 254 is dedicated for the measurement of mercury
concentrations in liquids and digested solid samples. Do obey the
related dangers while working with toxic or harmful substances. Make
sure that the emitted gas is lead back into an appropriate absorption
device and that gas leading parts are not leaking while measuring.

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LabAnalyzer 254

Table of Contents

1. GENERAL DESCRIPTION. ........................................................................8


1.1 Fields of application ................................................................................... 8
1.2 Measuring principle .................................................................................... 8
2. PREPARATION FOR OPERATION..........................................................10
2.1 U npacking and start- up. .............................................................................10
2.2 Power supply ...............................................................................................11
2.2.1 Operation on mains........................................................................................11
2.2.2 Battery operation............................................................................................11
2.2.3 Battery charger.............................................................................................. 12
2.2.4 Charging operation. . ...................................................................................... 12
2.2.5 Features of the battery charger...................................................................... 13
2.2.6 LEDs.. ............................................................................................................ 13
2.2.7 Charging times.. ............................................................................................. 13
2.2.7 Safety............................................................................................................. 13
2.2.8 Environment.................................................................................................. 13
2.2.9 Technical specifications................................................................................. 13
2.3 Fuses . ..........................................................................................................14
2.4 Operation and display components. ...........................................................15
2.5 C onnection of the electrical outputs ......................................................15
2.5.1 Analogue signal 4-20 mA............................................................................... 15
2.5.2 Serial data output (RS 232/ USB).................................................................. 15
2.5.3 Connecting a printer...................................................................................... 16
3. OPERATING THE LABANALYZER 254...................................................17
3.1 Turning on the LabA nalyzer 254.. .............................................................17
3.2 Entering the name of the analyst.............................................................17
3.3 Main menu...................................................................................................18
3.4 Analyze sample...........................................................................................19
3.4.1 Set air flow. . ................................................................................................... 20
3.4.2 Entering sample identification....................................................................... 21
3.4.3 Entering a dilution factor ............................................................................. 23
3.4.4 Start measurement......................................................................................... 23
3.4.5 Printout of results.......................................................................................... 24
3.4.6 Data transfer to a PC or Laptop..................................................................... 25
3.5 C alibration .................................................................................................31
3.5.1 Check stored calibration data........................................................................ 31
3.5.2 Perform new calibration................................................................................ 32
3.5.3 Delete calibration.. ......................................................................................... 34
3.6 R ecall data . ...............................................................................................35
3.6.1 Selecting data.. ............................................................................................... 35
3.6.2 Print data....................................................................................................... 35
3.6.3 Transfer data to a PC or laptop...................................................................... 36
3.6.4 Delete data..................................................................................................... 36

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LabAnalyzer 254

3.7 S ervice menu ...............................................................................................36


3.7.1 Setting date and time..................................................................................... 37
3.7.2 Device data.................................................................................................... 37
3.7.3 Printer port.................................................................................................... 37
3.7.4 Set language.................................................................................................. 38
3.7.5 Check heating of the optical cell.................................................................... 38
3.7.6 Test of 4-20 mA signal output........................................................................ 38
3.7.7 Show error records........................................................................................ 39
3.7.8 Set calibration data manually........................................................................ 39
4. MAINTENANCE.......................................................................................40
4.1 Error messages ..........................................................................................40
4.1.1 Error messages during start-up.................................................................... 40
4.1.1.1 WARNING EEP INIT check parameters.................................................. 40
4.1.1.1 WARNING EEP INIT check parameters.................................................. 40
4.1.1.2 WARNING check memory batt................................................................ 40
4.1.1.2 WARNING check memory batt................................................................ 40
4.1.1.3 WARNING Check Calibration P-Sensor (LA -VM Combi only)................ 40
4.1.1.4 Photometer Malfunction Check Optical Cell........................................... 41
4.1.1.4 Photometer Malfunction Check Optical Cell........................................... 41
4.1.2 Error messages after start-up......................................................................... 41
4.1.2.1 Replace carbon filters............................................................................ 41
4.1.2.2 Reset of operational Hours and total absorbed Hg................................. 41
4.1.3 Error messages during operation.................................................................. 42
4.1.3.1 Lamp . . ................................................................................................... 42
4.1.3.2 AD 0-7 .................................................................................................. 42
4.1.3.3 Temp. opt. cell. . ...................................................................................... 42
4.2 Particle filter. ..........................................................................................43
4.3 R eplacement of the carbon cartridges . ...................................................43
4.3.1 Replacing the internal carbon cartridge for zero air..................................... 43
4.3.2 Replacing the carbon cartridge of the reaction unit..................................... 44
4.3.3 Replacing the carbon cartridge of the gas outlet.......................................... 44
4.4 C leaning the bubbler .................................................................................44
4.5 R eplacement of the bubbler ......................................................................44
4.6 C leaning the optical cell. ........................................................................45
4.7 Preventive maintenance.............................................................................46
4.8 Troubleshooting. .......................................................................................46
4.8.1 Fuses.. ............................................................................................................ 46
4.8.2 Loss of air flow.............................................................................................. 46
5.1 Technical specifications............................................................................47
5.2 Operating conditions . ................................................................................47
5.3 S torage and transport...............................................................................47
5.4 S pare parts and accessories.......................................................................48
5.5 Block diagram of electrical parts ...........................................................49
5.6 D iagrams of components ...........................................................................50

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LabAnalyzer 254

6. APPENDIX A: WORKING WITH THE LABANALYZER 254........................53


6.1 S ample preparation . ...................................................................................53
6.2 R eagents for analyses . ..............................................................................54
6.3 S hort instructions for performing an analysis ........................................55
6.4 R ecord of signal........................................................................................56
6.5 S ome commonly used sample preparation methods....................................57
6.5.1 Water. . ............................................................................................................ 57
6.5.2 Biological samples......................................................................................... 57
6.5.3 Food. . ............................................................................................................. 57
6.5.4 Drinks (wine)................................................................................................. 58
6.5.5 Liquid waste and ground water...................................................................... 58
6.5.6 Natural gas.................................................................................................... 58
6.5.7 Microwave oven sample decomposition.......................................................... 58
6.5.8 Sewage sludge, sediments, soil, construction rubble and............................... 59
6.5.9 Hair............................................................................................................... 59
contaminated glass................................................................................................. 59
6.5.10 Flue gas / stack gas. . .................................................................................... 60
6.5.11 Petroleum and petroleum products............................................................... 60
7. APPENDIX B: STATISTICAL PERFORMANCE DATA. . ............................61
7.1 D etection Limit and Limit of determination. ...........................................61
7.2 U ncertainty ................................................................................................61
8. APPENDIX C: EC-DECLARATION OF CONFORMITY.............................63
INDEX.........................................................................................................64
FLOWCHARTS...........................................................................................67

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LabAnalyzer 254

1. General description
The LabAnalyzer 254 consists of a reaction unit and a photometer unit.
The photometer unit is basically a VM-3000. It comes in two options:
Operation as LabAnalyzer 254 only and operation as LabAnalyzer 254 as well as VM-3000.
For operation as VM-3000 please refer to the VM-3000 manual.

1.1 Fields of application


The LabAnalyzer 254 is used for manual measurement of mercury concentrations in liquid
samples and digested solid samples.

Typical samples are:

• water, like surface and ground water


• process waters from chlorine-alkali-electrolysis plants
• industrial effluents (chemical industry, incinerators, power-plants)
• caustic solutions and acids (NaOH, KOH, H2SO4)
• biological samples like plants, urine, saliva
• food
• geological samples (minerals, soil, sediments)
• refuse (construction rubble, broken glass, wood, sludges, ...)
• flue gas analysis (according to VDI 3868-2 VE)
• petrochemical samples

1.2 Measuring principle


Basis for determination of the mercury concentration is the resonance absorption of the
Hg-atoms at a wavelength of 253,7nm at room temperature. This analytical technique is
known as the „cold vapor method“ (see Fig. 1, p. 9) Mercury contained in the sample is
reduced to its elementary state by a reductant (Tin-II-chloride or Sodium-tetrahydroborate
(Sodium-borohydride)).
A stream of air, which is produced by a built-in membrane pump, strips the mercury from
the sample and draws it into the optical cell. In this cell the concentration of mercury is
determined by measuring light absorption at a wavelength of 253.7 nm (see Fig. 2, p. 9) .
A built-in computer performs the quantitative evaluation of the results. In order to get an
extremely stable baseline, the UV-light source is controlled by the reference beam method.
In addition to that, the UV-detectors of the LabAnalyzer are thermostatically stabilized.
Heating of the optical cell prevents sensitivity for water vapor. Thus the use of a desiccant or
dryer tube, which always show adsorption of mercury vapor, is avoided.

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LabAnalyzer 254

h.u

UV Source (EDL) k=253,7 nm


Hg Optical Cell

Air Air + Hg

Hg
Hg
Hg

Sample

Fig. 1: Measuring principle: Cold Vapor Method

Activated Carbon Filter

Reference Detector

Optical Cell Membrane Pump

UV Source (EDL) UV-Detector

Carbon Filter Cell Heating

Zero-Air Photometer Unit

Flowmeter

Reaction Unit

Air in
Reduction bottle Activated Carbon Filter

Fig. 2: Schematic gas flow

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LabAnalyzer 254

2. Preparation for operation

2.1 Unpacking and start-up

• The photometer unit is unpacked and placed on a flat surface. For more comfortable
operation, the instrument can be positioned with the adjustable front feet (in combination
with the VM-3000 option there is an adjustable handle instead, see manual of the VM-
3000).
• The reaction unit is unpacked as well and placed on the left side of the photometer unit.
• Both components (photometer and reaction unit) are connected with the included Tygon
tubing as shown in figure 3 below.
• The included activated carbon cartridge (A) is also unpacked and attached to the gas
outlet on the rear side of the photometer unit (see figure 4 below).

A
LabAnalyzer 254

Gas Flow MERCURY INSTRUMENTS

le
in 1 2 3 ENT
Date Time Cal.Factor
mp

F2 4 5 6
Sa

ESC

F3 7 8 9

F4 0

MERCURY INSTRUMENTS

Fig. 3: Connection of the reaction unit (A) and the photometer unit (B)

Fig. 4: Installation of the activated carbon cartridge (A) on rear panel of photometer unit.

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LabAnalyzer 254

2.2 Power supply

The 12 Volt version of the LabAnalyzer 254 can be operated with mains as well as with 12
Volt rechargeable batteries.

2.2.1 Operation on mains

One end of the included power cord has to be connected to the power cord socket on
the back of the photometer unit. The opposite end has to be plugged into an appropriate
power outlet. For operation turn on the photometer unit by pushing the switch on the rear
panel to position „I“. The voltage of the power source is detected automatically (90 V
AC-132 V AC or 187 V AC - 264 V AC, 47-63 Hz).

2.2.2 Battery operation

The photometer unit of the LabAnalyzer 254 can be run on rechargeble batteries for
approximately five to six hours if the option VM-3000 is installed. If „Low Battery” is
indicated on the display the LabAnalyzer 254 (VM-3000) can still operate a few minutes
in order to give you time to finish measurements and recharge the batteries or change to
operation on mains power.
If the LabAnalyzer 254 is not in use for a longer period of time, it should be connected
to the battery charger every four to eight weeks to maintain full capacity of the batteries.

Temperature sensor
PT-100

Bat. PT-100

USB/RS232

Mercury Instruments

Ser. No.

Voltage

output 4 - 20 mA
12V DC connection
Back label
sample gas out
Serial output for PC, USB = standard activated
power cord receptable ( internal switchable to RS 232, if needed)

power ON / OFF Status output

fuses Printer output (parallel)


Fig. 5: Rear panel of photometer unit. To charge connect the battery charger to
the „Bat.“ input.

(The temperature sensor PT-100 is only available when the photometer unit is
equipped with the VM-3000 option.)

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LabAnalyzer 254

2.2.3 Battery charger

The LabAnalyzer/VM-3000 must not be operated on mains while


charging batteries
(Turn off the photometer or disconnect mains cable).

The charger ACS 110 Traveller is designed to quick charge the NiMH battery pack of the
VM-3000. Charging time of empty battery packs is approximately 10 hours.
Note that new battery packs or packs that have not been used over a longer period of time,
will reach their full capacity only after a certain time.

2.2.4 Charging operation


1. Switch off the Mercury Vapor Monitor.
2. Disconnect Mercury Vapor Monitor from mains power supply by pulling the power
plug.
3. Put primary plug of the battery charger into wall socket. The red LED „Power“ will
light up.
4. Connect the Mercury Vapor Monitor by means of the included cable observing correct
polarity; in case of wrong connection the green LED „Charge“ will keep flashing.
5. The green LED will flash for about 1 Minute. (battery contact detection - test phase).
6. Charging of the NiMH power packs will start automatically once being properly
connected.

If the green LED „Ready“ keeps flashing after the test phase
and the red LED „Charge“ is off,
check the polarity of the battery pack (+/- switched).
If polarity is right and the green LED keeps flashing after the test
phase, the battery pack must be replaced.

The test phase is followed by the charging procedure (red LED „Charging“ on). After
termination of the charging time the device will automatically switch over to impulse-
trickle-charge. This is indicated by a flashing green LED, red LED „Charging“ off.

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LabAnalyzer 254

2.2.5 Features of the battery charger


• for NiCd and NiMH battery packs
• capacity: 500 mAh to 5000 mAh
• micro-controller controlled charging
• battery test phase at the start of each charging cycle to detect broken battery packs,
charging current cut off
• short circuit detection
• electronic protection against reversed polarity
• battery charging state at the start of the charging cycle is of no importance
• automatic switching over to trickle charge
• button for discharging automatically followed by charging
To avoid memory effect (loss of capacity due to frequent partly discharging), you have to
discharge the battery pack every now and then. After the test phase, press the „PRESS”
button for approximately 2 seconds (green LED flashing). After discharging and after a
power interruption the charger automatically switches over to charging.

2.2.6 LEDs
Green LED flashing: battery contact detection (test phase)
battery pack reversed
battery pack broken or unsuitable amount of cells
discharging after pressing the PRESS button
Red LED „Charging“ on: Charging
Green LED on: Battery fully charged, trickle charge

2.2.7 Charging times


Number of cells: 1-10
Capacity: 800 - 7200 mAh
Charging time: approx. 10h

2.2.7 Safety
Do not charge dry batteries. Danger of explosion!
Only charge rechargeable NiMH battery packs.
Do not open the charger. Repairs may only be done by the manufacturer.
For indoor use only.

2.2.8 Environment
Batteries are small chemical waste. Throw away broken or used up batteries in a special
container or hand them in at a recycling centre.

2.2.9 Technical specifications


Prim: 100 -240 V AC, 50-60 Hz.
Sec: 1,45 - 14,5 DC, max 800 mA 9,6 VA

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LabAnalyzer 254

2.3 Fuses

The fuse compartment is located on the rear of the photometer unit between the power cord
receptacle and the power switch. It can be opened with a small screw driver and contains two fuses.

Disconnect instrument from electrical mains supply before opening the


fuse compartment !

Fuse type: 230V / 115V operation voltage: fuse type T 1.250 mA T (time lag) (2x)

Further fuses:
• A Type 3.15 A MT is located on
the power supply board. It is
accessed by removing the top of
the case (opening the photometer
unit (see chapter 4.3.1, p. 43),
position of power supply board
(see Figure 20, p. 50 and Figure
21, p. 51).
• A Type 2.5 mA MT is also located
on the power supply board (only
for LA / VM-3000 combi with
optional rechargeable battery
pack). Fig. 6:
Position of the 3.15 A T fuse and 2.5 A MT fuse
• A Type 400 mA T is located inside (optional) on the power supply board
the UV lamp unit.

Fig. 7: Lamp Unit containing the HF-


board and position of 400 mA T fuse
on the HF-board

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LabAnalyzer 254

2.4 Operation and display components

The LabAnalyzer 254 features a waterproof IP66 keypad and a graphic LCD with background
illumination for comfortable communication with the operator.

2.5 Connection of the electrical outputs


2.5.1 Analogue signal 4-20 mA

The socket for the analogue output signal is located on the rear panel of the photometer
unit.
To transmit the signal the optional cable (part No. 202-06) is connected with the BNC-
plug to the socket marked with „SIGNAL“. Maximum load is 400 Ohms.

GND
Fig. 8: Signal output socket (BNC)
+4 ... 20 mA

2.5.2 Serial data output (RS 232/ USB)

To connect the LabAnalyzer 254 with a PC there are two possibilities provided: a USB-
socket and a 9-pin DSUB-socket on the rear panel of the instrument. The serial port of the
PC has to be connected to one of them with an appropriate cable (RS 232: part No. 202-07
pins 2-3-5 are 1:1/ USB: 202-07a). The two ports of the photometer cannot be activated
simultaneously, there is a dip-switch on the inner back panel of the instrument (see Fig.
10, p. 16) which allows to select either USB or RS232.
All data are transferred from the LabAnalyzer 254 as ASCII-characters. They can be
transferred to the PC with a terminalprogram like Windows® Hyper-Terminal or with the
included HG-Transfer software.
Factory setting is: USB activated. For being able to use this port you have to install
the USB-driver (CDM Driver) which you will find on the HG-Transfer CD-ROM.
For installation and configuration of the HG-Transfer software see chapter 3.4.6, p. 25 ff.

RS 232
5 1 Pin Nr 5 3 2
GND RxD TxD

9 6
Fig. 9: RS232 serial output socket

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LabAnalyzer 254

The parameters for data transfer are:


9600 Baud / 8 Data bits/ 1 Stop bit/ no Parity and Xon/ Xoff.
The following data will be available:
• name of analyst
• sample number
• date
• time
• peak height
• concentration Hg
• equation of the calibration graph
• dilution factor.

Fig. 10:
Dip switch for selecting
USB or RS 232

2.5.3 Connecting a printer


A printer (EPSON - compatible) can be connected to the 25-pin DSUB-socket installed
on the rear panel of the photometer unit.

If you want to use a printer directly with the LabAnalyzer you have
to set the parameter „Set printer Mode“ to parallel in the Service
menu (see chapter 3.7.3, p. 37). Factory setting is serial

Printer
13 1

25 14

Pin No. 1 2 3 4 5 6 7 8 9 11 18
PSTROBE D0 D1 D2 D3 D4 D5 D6 D7 BUSY DGND

Fig. 11: Parallel output socket for printer connection

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LabAnalyzer 254

3. Operating the LabAnalyzer 254


3.1 Turning on the LabAnalyzer 254
After turning on the LabAnalyzer 254 the mercury lamp is ignited and warmed up to operation
temperature. This indicated by the follwing displays:

Display No. 1 Display No. 2

3.2 Entering the name of the analyst


After the instrument has stabilized, which
typically takes 3-10 minutes (depending on the
ambient temperature), the input mask for the
analyst’s name appears on the display.
By pressing the numbered keys shown on the
display a previously stored name can be selected.
Pressing F1 lets you enter a new name
(maximum 20 characters), pressing F4 will Display No. 3-1
delete the selected name.
The letters can be chosen by entering the
assigned number. Repeat pressing the number
until right letter appears on entering line. To
go to the next position press ▲ and select next
letter.
With ▼ you can go back to a previously entered
letter and either change or delete it. Delete
function is ◄. Display No. 3-2
Space between first and second name is created
by pressing the triangle ▲. Repeat until name
is completed and press ENT.

In the next menu the operator can decide if


the entered name should either be deleted or
saved after measuring. Maximum is ten names,
when entering an eleventh name, you will be
prompted to select the name to be overwritten. Display No. 3-3

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LabAnalyzer 254

The name to be overwritten can be selected by


presing the ▼ or ▲ keys.

Presst the corresponding numerical key to


overwrite the selected name (in this case
„SAP”).

Display No. 3-6

A selected name can also be deleted by pressing F4 (see above) before entering a new name.
(Deleting a name has to be confirmed by pressing F1.)

Display No. 3-1 Displays No.3-4 and 3-5

3.3 Main menu

After entering the analysts name the main menu


is displayed automatically:

Display No. 4-1


The following sub-menus are available:
F1: „Analyze Sample“ = analysis mode
F2: „Calibration“ = calibration of instrument with standard solutions
F3: „Recall data“ = display or print results from previous measurements
F4: „Service“ = set date/time/ device data/printer mode/choose language/
check heating of the optical cell/set 4-20mA output, check or
delete error record
ESC = Select analyst or enter a new analyst name

If your LabAnalyzer comes with the option VM-3000 as stand-alone


instrument, pressing ESC lets you choose between operation as
LabAnalyzer 254 or VM-3000 (“Select Mode”).

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LabAnalyzer 254

Display No. 4-2 Display No. 6

If your LabAnalyzer comes with the option VM-3000 as stand-alone


instrument selecting or entering another analyst name
cannot be done directly after measuring:

Press ESC in the main menu to enter the „Select Operation Mode“ menu,
then press F2 „LabAnalyzer 254“ to get to the „Name of Analyst“ menu.

3.4 Analyze sample


Press F1 „Analyze Sample“ in the main menu (chapter 3.3, p.18).

Press F1 „Select calibration“ if you want to


use a stored calibration.

Press F2 „Perform new calibration“ to enter


a new calibration. The program will jump into
calibration mode (see chapter 3.5, p. 31).

Display No.5-1

If there are no calibrations stored yet, or all have


been deleted, press „ESC”, then press Press
F2 „Perform new calibration“ in Sample
Analysis Mode (Display No. 5-1) to enter a
new calibration. The program will switch to
calibration mode (see chapter 3.5, p. 31).

Display No.5-2

After pressing F1 „Select calibration“ in Sample


Analysis Mode you can choose between up to
three calibrations previously stored. Pressing the
numerical keys 1, 2 or 3 recalls the corresponding
calibration. (If you want to view the calibration
data of the stored calibrations go to the calibration
mode (see chapter 3.5.1, p. 31).
Display No. 5-3

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LabAnalyzer 254

3.4.1 Set air flow

With start-up procedure completed, the LabAnalyzer 254 will automatically call for an
adjustment of the correct airflow before calibrations or analysis can be started.

Fill the reaction bottle with 10 ml of water


and fit it onto the bubbler (step 1 and 2 in
fig. 12-1).

Pull the securing clamp forward to secure the


reaction flask. Press F1 „Ready“ to proceed.

Display No. 6-1


LabAnalyzer 254

read
3 adjust MERCURY INSTRUMENTS
Gas Flow

Bubbler

10 ml water push back


2 securing clamp
and attach
reaction flask to
1 bubbler Fig. 12-2: Securing the
reaction flask (reactor)
Fig. 12-1: Adjusting the air flow

Then adjust the


airflow to 30 by
turning the needle
valve (step 3 in fig.
12-1). The airflow
is indicated by the
middle of the ball in
the flow meter.
Fig. 12-3: Flow meter Display No. 6-2
Press F1 „Ready“
to proceed.

Remove the reaction bottle and empty it.

Press F1 „Ready“ to proceed.

Display No. 6-3

If the flow has been adjusted before calibration, readjustment before or


during measurements is not advised.

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LabAnalyzer 254

3.4.2 Entering sample identification

After pressing F1 „Ready“ in „Empty Reactor“ you will be prompted to enter a sample
name (up to 5 characters).
The letters can be chosen by entering the
assigned number. Repeat pressing the
number until the right letter appears on
entering line. To go to the next position press
▲ and select next letter.
With ▼ you can go back to a previously
entered letter and either change or delete it.
Delete function is ◄. Space is created by Display No. 7-1
pressing the triangle ▲ twice.

Repeat until the name of the sample is completed and press ENT.

Now a number (up to 9 digits) may be entered


to complete the sample identification.

To correct a certain digit, delete it by pressing


◄.

When finished, press ENT.


Display No. 7-2

Now you can either:

• change the sample identification (if it should


not be correct) by pressing F1 „Sample Nr“
• enter a dilution factor by pressing F2
(see chapter 3.4.3, p. 23)
• or start the measurement by pressing F3.
Display No .7-3

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LabAnalyzer 254

When measuring numerous samples that differ only in numbers but


have an identical name, proceed as noted below:

After you have chosen the calibration (or


after pressing F1 „Next“ after a completed
analysis, (see Display No. 9-2, p. 23),
display No. 7-1 will appear.

Display No.7-1 (Shortcut)


Press ESC:

The name of the last analyzed sample will


appear, followed by either 0 (if you have
started a new analysis) or the last number
used (after pressing F1 „Next“ following a
completed analysis, (see Display No. 9-2, p.
23).

Display No.7-3 (Shortcut)

Press F1 , don‘t edit the name and press


Enter.

Delete the old number by pressing ◄ and


enter the new number.

Press Enter when finished.

Display No.7-2 (Shortcut)

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LabAnalyzer 254

3.4.3 Entering a dilution factor

The dilution factor of the sample can be set


by pressing F2-„Dilution factor“.
For example: If 1 ml of the sample is
diluted up to the 10 ml mark with water,
a dilution factor of 10 has to be entered.
The LabAnalyzer 254 automatically
determines the correct concentration
of mercury in the undiluted sample.
The measuring range is automatically Display No.7-3 (Entering diltion factor)
increased to 100 µg/l Hg (100 ppb) in this
example.

Press F3 „Start Measurement“ to begin the analysis of the sample.

3.4.4 Start measurement

Measurement is started by pressing F3


„Start Measurement“.
The following instructions will appear on the
display: „Fill in sample No.#, + add reagent
+ close reactor”.
Fill in precisely 10 ml of sample volume (see
chapter 6.3, p. 55 ff).
Display No. 8

After pressing F3 „Start Measurement“ again,


air is drawn through the reaction flask and a
time-absorbance graph is shown on the display.
The values are also given out to the analogue
signal output.

Display No. 9-1

An acoustic signal will sound when


measurement is completed, absorbance peak
height and calculated mercury concentration
are shown on the display.
Press F1- „Next” if you want to analyze
another sample.
Press F2- End if no further analyses should
follow.
Display No. 9-2

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LabAnalyzer 254

3.4.5 Printout of results

If a printer is connected the analysis data will be printed automatically at the end of each
measurement. Calibration data will be given with the first printout and every time the
calibration is changed. On the printout also appear: date and time of analysis, name of
analyst, sample number, dilution factor, peak height, mercury concentration in µg/l.
A printout can also be started in the „Recall Data“ menu (see chapter 3.6.2, p. 35).

Please note:
If you want to connect a printer directly to the LabAnalyzer 254, you
have to choose „parallel“ in the „Set Printer Mode“ menu
(see chapter 3.7.3, p. 37).
Factory setting is „serial”.

When the printer is not Epson compatible,


direct printing might not function properly.

LabAnalyzer 254 Mercury Instruments


Analysis Report 01.09.13, 09:29:36 Software Release 31.04.2013

Calibration: STANDARD
--------------
prepared by INDERST BRIGITTE

Date : 01.09.13 Time : 09:29:36


Linear equation: Y= 0.03120 X + 0.00017
Correlation : 0.99951

Cal.point Conc .Hg Absorb. Peak


1 0.100 µg/l 0.0031
2 0.200 µg/l 0.0060
3 0.300 µg/l 0.0095
4 0.400 µg/l 0.0129
5 0.500 µg/l 0.0162
6 0.600 µg/l 0.0191
7 0.700 µg/l 0.0225
8 0.800 µg/l 0.0252

point 9: outlier
0.900 µg/l 0.0274

Results:
-----------------------
Sample Nr: 1 01.09.97 , 09:29:36 Analyst: INDERST BRIGITTE
Dilution: 1 Peak H: 0.0221 Conc.Hg: 0.703 ug/l

Sample Nr: 2 01.09.97 , 09:31:12 Analyst: INDERST BRIGITTE


Dilution: 1 Peak H: 0.0031 Conc.Hg: 0.095 ug/l

Sample Nr: 3 01.09.97, 09:31:41 Analyst: INDERST BRIGITTE


Dilution: 1 Peak H: 0.0002 Conc.Hg: 0.000 ug/l

Fig.13: LabAnalyzer 254 - direct printout of results

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3.4.6 Data transfer to a PC or Laptop

All calibration and analysis data will be sent as ASCII-signals to the serial output (USB or
RS 232) of the LabAnalyzer 254. To enable the photometer unit to communicate with a
PC you have to install the program Hg-Transfer on your PC or laptop first.
Data stored in the photometer unit can then be imported into Hg-Transfer to be permanently
saved or printed.
Two sockets are available on the instrument back panel (see chapter 2.5.2, p. 15): a
9-pin D-Sub socket (RS 232) for connecting the photometer unit to a COM-port of the PC
and a USB socket for connecting the photometer unit to a USB port of the PC. You can
switch between USB and RS 232 (see Fig. 10, p. 16). Factory setting is USB.
If the USB connection is used you have to install a USB driver (CDM Driver) on your PC
or laptop first. You will find the USB-driver on the CD-ROM containing the Hg-Transfer
software. A suitable USB cable is included on delivery.

202-07a

USB USB

PT-100

USB/RS232

Fig. 13 Connecting the photometer unit to a PC

When starting the Hg-Transfer-software the main window will appear. By clicking
parameters > Set language you can first . For being able to transfer data from the
LabAnalyzer 254 you have to select „serial“ in the „Set Printer Mode“ menu of the
photometer unit (see chapter 3.7.3, p. 37).

Screenshot No.1 Main window of Hg-Transfer with menu “Parameters” dropped down

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LabAnalyzer 254

Clicking „Port Settings“ lets you


select the port of your computer to
be used for communication with
the LabAnalyzer 254 and the data
transfer.
Normally it is found automatically. Screenshot No. 2: Port settings

By choosing „Configuration“ you can select the type of analyzer and the type of transfer
mode (LA = LabAnalyzer):

Transfer mode:
Record data =
continuous transfer of
the measured values.

Make sure this value


is set to “1”
Screenshot No. 3-1: Setting the configuration: Record.

Transfer mode:
Print data =
transfer of data must
be started from the
LabAnalyzer
With „Select printer“
you can choose a Screenshot No. 3-2: Setting the configuration: Print
connected printer.
If „Print data“ is selected, the printer icon in the main menu will blink, otherwise it will
stay grey.

Screenshot No.3-3: Main window with “Print data” selected

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Klick this icon to start data transfer from the LabAnalyzer to a PC or laptop.

Data transfer mode set to „Record data:“


Transfer of calibration data before first measurement
Automatic transfer of each measurement.

Data transfer mode set to „Print data“ and „Automatic print“ deactivated:
Transfer of calibration data of the selected measurements
Transfer of the selected measurements.

It is advised to deactivate „Automatic print“

Data selection and transfer of the selected data has to be started from
the „Recall Data“ menu
of the LabAnalyzer (see chapter 3.6, p. 35).
Format of data shown in the main window is identical to the format of the saved *.txt file
(see printout example 1, p. 29 and example 2, p. 29).

Screenshot No. 4: Data displayed.

Calibration data incl. name of analyst

Results of measurements incl. date, analyst, dilution factor, peak height, concentration
(Hg) [μg/l]

Save Logfile: The data displayed in the Hg-Transfer window can be saved
as EXCEL® or *.txt format files.

Save Continuously: If „Record Data“ is selected in the configuration menu


all running measurements are saved to a defined file. Format is EXCEL®
or *.txt.

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LabAnalyzer 254

If „Print Data“ is selected in the „Configuration“ window, the „Print View“


window will open with the first incoming block of data.
Each new incoming block of data will open in a separate page.

Features of the „Print View“ window:

• Tastefully predefined template for each block of incoming data, including


information about date, time, analyst and calibration data

• Pages can be printed seperately or all at once

• „Save page“ lets you export each page as a separate *.jpg file.

Screenshot No.5: Print View

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Please note:
Data that have been imported in the „Record Mode“ cannot be
imported to the print preview. To print those data, they have to be saved
as *.txt or Excel files first and then printed from a word processing
program or Excel.

LabAnalyzer 254,Mercury Instruments,Analysis Report,18.02.14,11:46:00,Software Release 28.02.2013;


Calibration: PHOTO,prepared by D,Date: 17.02.14,Time: 16:42:35,Linear equation: Y= 0.03617 X + 0.00
590,Correlation: 0.99946,Cal.point,Conc.Hg,Absorb. Peak,1:, 1.00 ug/l,0.0400,2:, 2.00 ug/l,0.0784,
3:, 3.00 ug/l,0.1158,4:, 4.00 ug/l,0.1536,5:, 6.00 ug/l,0.2206;Point: 5 --> outlier, 5.00 ug/l,0.17
62;
Results:,
Sample Nr PHOT1,17.02.14,17:09:29,Analyst: D,Dilution 1.0,Peak H 0.0374,Conc.Hg 0.87 ug/l;
Sample Nr PHOT2,17.02.14,17:13:14,Analyst: D,Dilution 1.0,Peak H 0.0781,Conc.Hg 2.00 ug/l;
Sample Nr PHOT3,17.02.14,17:19:12,Analyst: D,Dilution 1.0,Peak H 0.1166,Conc.Hg 3.06 ug/l;
Sample Nr PHOT4,17.02.14,17:24:10,Analyst: D,Dilution 1.0,Peak H 0.0919,Conc.Hg 2.38 ug/l;
Sample Nr PHOT5,17.02.14,17:27:11,Analyst: D,Dilution 1.0,Peak H 0.1422,Conc.Hg 3.77 ug/l;

Printout example 1: Unformatted *.txt file

LabAnalyzer 254,Mercury Instruments,Analysis Report,18.02.14,11:32:08


Software Release 28.02.2013;
Calibration: PHOTO,prepared by D,
Date: 17.02.14,Time: 16:42:35,
Linear equation: Y= 0.03617 X + 0.00590,
Correlation: 0.99946,
Cal.point,Conc.Hg,Absorb.
Peak,1:, 1.00 ug/l,0.0400,
2:, 2.00 ug/l,0.0784,
3:, 3.00 ug/l,0.1158,
4:, 4.00 ug/l,0.1536,
5:, 6.00 ug/l,0.2206;
Point: 5 --> outlier, 5.00 ug/l,0.1762;

Results:,
Sample Nr PHOT1,17.02.14,17:09:29,Analyst: D,Dilution 1.0,Peak H 0.0374,Conc.Hg 0.87 ug/l;
Sample Nr PHOT2,17.02.14,17:13:14,Analyst: D,Dilution 1.0,Peak H 0.0781,Conc.Hg 2.00 ug/l;
Sample Nr PHOT3,17.02.14,17:19:12,Analyst: D,Dilution 1.0,Peak H 0.1166,Conc.Hg 3.06 ug/l;
Sample Nr PHOT4,17.02.14,17:24:10,Analyst: D,Dilution 1.0,Peak H 0.0919,Conc.Hg 2.38 ug/l;
Sample Nr PHOT5,17.02.14,17:27:11,Analyst: D,Dilution 1.0,Peak H 0.1422,Conc.Hg 3.77 ug/l;

Printout example 2: Processed *.txt file

An example of a formatted EXCEL-file is given in chapter 7.2 on page 62.

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LabAnalyzer 254

Clicking this button will erase all data from the main window of
Hg-Tansfer.

This cannot be undone !


Be sure to have saved your data beforehand.

Data stored in the RAM of the photometer unit will not be affected.

By clicking on About
(i) you can check which
version of Hg-Transfer
-Software you are using.

Choosing Exit closes the Hg-Transfer software.

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3.5 Calibration

To enter „Calibration Mode“ press F2


„Calibration“ in the main menu (chapter 3.3,
p. 18).
Up to three different calbrations can be stored.
F1: Lets you view the stored calibrations
F2: Lets you perform a new calibration
F3: Lets you delete a stored calibration

Display No. 10

3.5.1 Check stored calibration data

Press F1 „Show Calibrations“ in Display


No. 10.

Press one of the numerical keys 1 - 3 to select


a calibration.

Display No. 11-1


Data of the selected calibration will be
shown on the display including a graph
showing calibration points and outliers ( )
(Display 11-4).
Points that have been marked as outliers are
underlayed black in Display No. 11-3.
Navigate through the pages with the arrow
keys (▼▲).
Display No. 11-2

Display No. 11-3 Display No. 11-4

In case a calibration has been entered manualy


(see chapter 3.7.8, p. 39), dispays 11-3 and 11-4 will show no
calibration points

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3.5.2 Perform new calibration

For a new calibration, press F2 „Calibration“ in the main menu (see chapter 3.3, p.
18), then press F2 „Perform new Calibration“ in the Calibration menu.

Enter the concentration of the first calibration


standard. Confirm by pressing ENT.

Display No. 12-1


Concentrations of calibration standards should be in the range of
0 - 5 µg/l Hg.
Calibration points should be chosen equidistant. For measurements at
the lower range calibration between 0 - 1µg/l Hg is recommended.

Fill 10 ml of calibration standard into


reaction bottle, add reductant (see “Tin-II-
chloride”, p. 54) and attach reaction bottle
to the standard ground cone of the bubbler.

Press F3 to start measurement of the first


calibration point.
Display No. 12-2

An air stream is drawn through the reaction


flask and the measurement of the first
calibration point begins (scaling of the peak
height is carried out automatically).

Display No. 12-3

An acoustic signal will indicate the end of


the measurement and the results will be
displayed.

Press F1 „Next“ for more calibration points.


A total of up to 9 points can be measured.

Press F2 “End“ to finish calibration.


Display No. 12-4

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The values of concentration and absorbance


for the measured calibration points are now
displayed.

Press ▲or▼to view the calibration graph,


or the resulting equation for the calibration
graph.
Display No. 13-4: No outlier marked

Display No. 13-3 (no outlier) Display No. 13-5: resulting equation when
no point is marked as outlier

In Display 13-4 it is possible to mark one


or more points as outliers by pressing the
corresponding numerical key. Confirm by
pressing ENT. To deselect a point as an
outlier select again and press ENT. Outliers
are underlayed in black.

By using the the arrow keys you can now Display No. 13-4: Point 3 and 4: Outliers.
scroll between the three pages showing the
results of defining certain points as outliers. The equation for the calibration curve will
change accordingly.

Display No. 13-3: with outliers Display No. 13-5: new equation taking into
account that points 3 and 5 are ignored.
You can go back to Display No. 13-4 and redefine other points as outliers.
When you press F1 „End“ in Display No. 13-5 calibration is completed (selection of
outliers is now stored and cannot be altered any more).

You will be prompted to store the calibration.

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F1 „Yes“: the new calibration will be stored.

F2 „No“: the new calibration is discarded

Display No. 13-6

Saving the calibration:

The calibration may be stored under a name


which has to be entered now.

Navigation when entering the name is the


same as described in chapter 3.2, p. 17.
Display No. 13-7

Only three calibrations can be stored. If there


are already three calibrations stored, the user
is asked which calibration should be deleted.
Select the calibration to be deleted by
pressing one of the numerical keys 1 to 3.

Display No. 13-8

3.5.3 Delete calibration

Press F3 „Delete calibration“ in the


Calibration menu (chapter 3.5).

Now you can delete one or all stored


calibrations by pressing the numerical keys
1 to 3.

(You will be asked to confirm the deletion


of the selected calibration, see Flowchart.) Display No. 14

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3.6 Recall data

The LabAnalyzer has the capacity to store up to 100 measurements. Each data set includes
name of sample, dilution factor, concentration, and absorption, as well as date and time,
number and name of calibration and name of the analyst.

3.6.1 Selecting data

Press F3 „Recall Data“ in the main menu to view results from previous measurements.
Sample number, dilution factor, concentration in µg/l Hg and the absorbance will be
displayed in a table.

Selecting (or deselecting) a sample is done


by scrolling with the arrow keys (▲▼) and
pressing Enter. Select as many samples as
you wish.

Pressing ESC brings you back to the main


menu.
Display No. 15-1

3.6.2 Print data

Press F1 „Print“ in the „Recall Data“ menu (display No 15-1).

Make sure that a printer is connected to the LabAnalyzer 254


and that „port setting“ is set to „parallel“ (see chapter 3.7.3, p. 37).

Press F4 „Print marked data“ to print the


values of the selected samples.

Display No. 15-2

All data are tansfered as ASCII characters.


The calibration data used for measuring the
selected samples is always sent before the
values of the selected samples.

Display No. 15-3

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3.6.3 Transfer data to a PC or laptop

Make sure that a computer or laptop is connected to the LabAnalyzer 254


and that „port setting“ is set to „serial“ (see chapter 3.7.3, p. 37).

Selecting data and transfering them to a PC or laptop is done the same way as printing
data (see chapter 3.6.1, p. 35) , the only difference being that the data are sent to the
serial output (USB /RS 232) instead of the parallel port (Centronics).

Select data to be transfered:


Press F1 „Print“ in the „Recall Data“ menu (display no. 15-1).
Press F4 „Print marked data“ in the „Print Data“ menu (display no. 15-2) to transfer the
values of the selected samples.

3.6.4 Delete data


Press F2 „Delete“ in the „Recall Data“ menu (see Display No. 15-1, p. 35).

This cannot be undone.


All data selected will be definitely lost if you have not transfered
them to a PC or Laptop beforehand.

Press F4 „Delete marked data“ to delete the


selected measurements.
Only selected measurements are deleted.
The associated calibration is not affected.
There will be NO confirmation prompt !

Display No. 15-4


If no data are selected (see chapter 3.6.1, p. 35)
ALL
measurements will be deleted.
You will be prompted to confirm the deletion of all data.

3.7 Service menu


Press F4 „Service“ in the main menu (see
chapter 3.3, p. 18)to get into Service Mode.

After entering the code 321 [Enter], you have


access to the Service Mode:
The service mode has two pages. Switch
between them by pressing the arrow buttons
(▼▲).
Display No. 16

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Display No. 17-1 Display No. 17-2

3.7.1 Setting date and time


In page 1 of the Service Mode. press F1 „Set Date/
Time“.
Press F1 to edit the date.
Press F2 to edit the time.
In the right bottom corner of the display the day of the
week is shown.
Display No. 18-1

By presssing F1 (or F2) you can consecutively choose


between day, month and year (F2: hour, minutes and
seconds respectively).
Change the values by pressing▲or ▼.
Confirm by pressing [ENTER].
Display No. 18-2

3.7.2 Device data


Press F2 „Device Data“ in page 1 of the
service menu.

You will get information about the


operational hours, the current voltage of the
lamp and the stored software version. The
standard operation range of lamp voltage is
3.0 – 9.0 V
Display No. 19

3.7.3 Printer port

Press F3 „Set Printer Mode“ in page 1 of


the service menu.

You can switch between the serial (transfer


to a PC or Laptop) and the parallel interface
port (transfer to a printer) at the back panel
of the instrument by pressing F1.
Display No. 20

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3.7.4 Set language

Press F4 „Set Language” on <Page 1> of


the service menu.

By pressing either F1 or F2 you can select


the desired language.

Display No. 21

3.7.5 Check heating of the optical cell


The heating of the optical cell can be controlled. This will be effective only 20 min after
powering on the analyzer. After this warming up period you will get an alarm if during 20
minutes there will be no heating impulse. Following alarm message will be shown on the
display: „Chk. heating opt. cell”

The control of the optical cell heating can be


deactivated in the service menu:
Enter the Service Mode (see chapter 3.7, p.
36)) and select <Page 2>.
By pressing F1 „Chk. Heating opt. cell“
you can switch between ON/OFF.
Display No. 17-2

If the LabAnalyzer is running on battery power, the heatig of the


optical cell is automatically turned off because of high energy
consumption. The
„Chk. Heating opt. cell“
function must be set to „off” manually,
otherwise there will be constant error messages.

3.7.6 Test of 4-20 mA signal output


The 4-20mA output can be tested in the service menu. Enter the Service Mode (see
chapter 3.7, p. 36)and select <Page 2>.

Select F2 „Set 4-20 mA“

Delete the current value by pressing the


arrow-left key (◄). Enter any value between
4 and 20 and press „Enter“.

Test the value with a multimeter at the outlet.


Display No. 17-2 (3)

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3.7.7 Show error records


Enter the Service Mode (see chapter 3.7, p.
36) and select <Page 2>.

Press F3 „Show Error Records“ to view the


chronicle of error messages. Up to 100 error
messages can be stored. When this limit is
reached, the oldest errors will be overwritten.
Press F4 „Delete“ to delete the list of errors.
Display No. 51
(You will be asked to confirm this step.)

Please note that turning


the instrument off and on
again will result in an error
message:
„System Reset“

Display No. 52

3.7.8 Set calibration data manually


It is possible to enter the values for the calibration directly. Enter the Service Mode (see
chapter 3.7, p. 36) and select <Page 2>.
Press F4 „Set Calibration Data“.
Press F1 to enter the gradient. Confirm by
pressing „Enter“.
Press F2 to enter the constant.
The sign of the constant can be switched
by pressing F2 again. Confirm by pressing
„Enter“.
Display No. 49: Input mask
After gradient and constant have been
entered, press ESC.
You will be asked whether to store the calibration or not (see chapter 3.5.3, p. 34).

Display No. 49: Entering constant Display No. 49: Input completed

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LabAnalyzer 254

4. Maintenance

4.1 Error messages


4.1.1 Error messages during start-up
In case of a serious malfunction or after the microprocessor has been exchanged the
following warnings will appear on the display after turning on the LabAnalyzer 254.

4.1.1.1 WARNING EEP INIT check parameters


This warning is usually given after
exchanging the internal eprom due to
software updates and/or replacement of
the buffer battery.
Press Enter to complete the start-up
procedure. Since all previously stored
names of analysts and all calibrations are
lost you will have to enter a new name for
the analyst and perform a new calibration. Display No. 2: Warning during start-up
(You can also enter a new calibration
manually, see chapter 3.7.8, p. 39).
4.1.1.2 WARNING check memory batt

When turning on the LabAnalyzer


254, the current date is checked.
Should „year” read „00”, there is a
malfunction concerning the battery of
the internal memory. Check or replace
the battery.

Display No. 2: Warning during start-up

4.1.1.3 WARNING Check Calibration P-Sensor (LA -VM Combi only)

This warning can only occur if the


photometer is warming up as VM-3000.
and the PT-correction is ON (refer to
VM-3000 manual).

Display No. 2: Warning during start-up

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4.1.1.4 Photometer Malfunction Check Optical Cell


If the optical cell is polluted, two different error messages will appear duriing start-up .
Turn off the instrument and clean the optical cell (see chapter 4.6, p. 45).

Display No. 1: Display No. 2:


Error message during lamp ignition Error message during lamp stabilizing

4.1.2 Error messages after start-up

4.1.2.1 Replace carbon filters

The carbon filters of the LabAnalyzer should be replaced annually. In addtion the
LabAnalyzer calculates the cumulative amount of mercury that has passed the outlet
filter. When the activated carbon filter has absorbed more than 50 000 μg of mercury
(or after more than 5000 hours of operation), the following reminder will appear after
start-up:

Press F1 „Replacement done” after


having changed the filter.

Press F2 „Continue” if you want to


continue without changing the filter.

Display No. 31

4.1.2.2 Reset of operational Hours and total absorbed Hg


If the outlet filter is replaced before
the above warning is shown, values of
operational hours and total absorbed Hg
can be reset manually. Enter the service
code 987 [Enter] in the „Service Menu“
(see chapter 3.7, p. 36). Pressing F4
twice resets the values to zero.
The reset has to be confirmed.
Display No. 30

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LabAnalyzer 254

4.1.3 Error messages during operation

Error messages during measurement will


appear blinking on the measuring display:

Measurement will continue however,


there will be an entry in the error record
and a status output <Malfunction>.

Display No. 9-1:


Error messages, eg.: Temp opt. cell

4.1.3.1 Lamp
The installed electrodeless mercury lamp is monitored permanently. If its performance
drops under a certain limit (lamp voltage >10 V) the warning „LAMP” will show on
the display. → Replace lamp within the next weeks.

4.1.3.2 AD 0-7
This message is displayed in the case of malfunction of the analog/digital converter.
The numbers show the channel which is defect and gives wrong values (measurement
is proceeding however)
0 = pressure
1 = temperature
4 = lamp voltage
7 = battery voltage (accu-version only)
→ Replace AD converter.

4.1.3.3 Temp. opt. cell


This warning is given in case the optical cell heating has not been turned off or on
within twenty minutes (see chapter 3.7.5, p. 38).
If „Temp. opt. cell” appears on the display while the photometer is operating on
battery power, turn off the function for controlling the heating of the optical cell, since
the cell heating is only active when the photometer is running on mains power.
If „Temp. opt. cell ” appears on the display while the LabAnalyzer is running on
mains power, call the service.

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4.2 Particle filter


Under normal operation conditions, the sample gas particle filter has to be inspected regularly.
If a deposit of particulate matter is visible, the filter membrane has to be replaced. Expected
time interval for a filter replacement is 1 ... 6 months. For filter replacement carefully screw
out the front part of the filter holder. Remove sealing ring and filter membrane. Insert spare
filter membrane so that the PTFE coated side faces towards the user and the fibrous side
toward the instrument. Insert sealing ring and screw in front part of the filter holder. Make
sure everything is gas tight.

Sealing
Filter

Figure 14:
Particle filter replacement

4.3 Replacement of the carbon cartridges


All carbon cartridges of the LabAnalyzer 254 unit should be replaced annually.

4.3.1 Replacing the internal carbon cartridge for zero air


Place the instrument on a flat surface with its rear panel facing to you. Then loosen the
two screws on the back of the photometer unit and remove the top of the case by pulling
it towards you. The carbon cartridge is now visible and can be removed from its holding
clamps. To replace the carbon cartridge the tubing has to be pulled off.

pull out cartridge


and remove tubing

Photometer Unit
3 Figure 15:
replacement of
top view activated carbon
cartridge for
remove top
2 Zero Air
unscrew with
3mm Allen key
1

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LabAnalyzer 254

4.3.2 Replacing the carbon cartridge of the reaction unit

The carbon cartridge of the reaction unit is positioned


in its rear upper part. For replacement pull it from its
holding clamps and remove the tubing.

Fig. 16-1: Activated carbon


cartridge of the reaction unit

4.3.3 Replacing the carbon cartridge of the gas outlet

The carbon cartridge at the gas outlet of the photometer


unit is replaced by simply pulling it from its tubing.
The operational hours and the calculated cumulative
Hg amount can be manually reset (see chapter 4.1.2.2,
p. 41).
Fig. 16-2: Activated carbon
cartridge at the gas outlet

4.4 Cleaning the bubbler


After a certain amount of analyses, precipitation from samples and chemicals, mainly
consisting of tin-II-oxide, may cover the bubbler (and the reaction flask as well). These
sedimentation can cause mercury adsorption and a high blank. Due to this the bubbler should
be cleaned with hydrochloric acid (concentrated HCl diluted 1 : 1 with water) occasionally.
If a white clouding of the sample appears during measuring, the acid concentration of the the
tin-II-chloride reagent should be raised. This reduces sedimentation in both the bubbler and
the reaction flask.
4.5 Replacement of the bubbler
The bubbler can be removed from its fitting if desired. This may
2
be necessary for purpose of cleaning or if damaged.
1
Proceed as follows:
• remove reaction flask (only if pump is not running!)
• pull off Tygon tubings 3

• loosen the screw on the right side of the holder (1)


• carefully turn the bubbler until its angled connecting nozzle
faces the operator (2)
• remove bubbler by tilting it and pulling it down carefully.

Inserting of the cleaned or new bubbler is done in the reversed


order.

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4.6 Cleaning the optical cell

When liquid has entered the sample-in filter of the photometer it may be necessary to clean
the optical cell.

• Disconnect the photometer from mains power and open the top cover following the
instructions of chapter 4.3.1, p. 43.

• Hold the optical cell on both connector nozzles and pull it carefully up with the tubes
still attached. The optical cell can now be lifted out from its support and pulled towards
the front side of the photometer. Now the tubes from the inlet and outlet can be pulled
off and the optical cell can be taken out from the photometer. Be careful not to touch the
glassware with bare fingers, use gloves or a clean tissue.

• The optical cell should be rinsed with distilled water first and then dried. Drying can
be done in a laboratory oven at mild temperatures (max. 85 °C) or/and by purging with
clean air, nitrogen or argon.

• Depending on the composition of the soiling of the optical cell, cleaning with water may
be not sufficient. In this case the cleaning has to be repeated with diluted hydrochloric
acid (ca. 10 – 15 %). If the precipitation still remains, higher acid con­­centrations or
concentrated hydroxide solutions (NaOH) may be used.

• If the optical cell is soiled with organic substances cleaning may be performed with pure
ethanol or acetone.
lift up clamps Fig. 18:-1:
Lifting the holding
clamps for removing the
optical cell

lift

Fig. 18:-2:
Holding the optical cell

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4.7 Preventive maintenance

• The LabAnalyzer 254 should be maintained regularly once a year.

• The tubing of the pinch valve for zero air (part No. 203-12) has to be replaced.

• The interior tubing as well as the optical cell should be checked for contamination.

• The lamp frequency should be checked. It is recommended that this control is carried out
by trained service personnel.

4.8 Troubleshooting

4.8.1 Fuses
If the display is not illuminated or the pump is not working, check the fuses.

Location of the fuses is described in chapter 2.3, page 14.

4.8.2 Loss of air flow


Loss of airflow can be due to different causes:

• Air pump is not working correctly (it produces an audible sound while in operation).
Readjust the pump (call the service) or replace the pump.

• Zero air pinch valve does not close tight during measurement. This will
cause a flow of “false” air from the zero cartridge bypassing the bubbler.
Replace valve and/or tubing.

• Leakage of the tubing or fitting between flowmeter and sample inlet of the photometer.
Check for leakage or damage of tubings and fittings. Replace if necessary.

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5. Technical Information

5.1 Technical specifications


Instrument type Mercury Vapor Monitor VM-3000
Manufacturer Mercury Instruments GmbH
Measuring component Mercury vapor Hg°
Measurement principle Atom absorption
Wavelength 253,7 nm
UV-source electrodeless mercury discharge lamp
Method of stabilising optically with reference beam; thermally
Optical cell entirely of fused silica Suprasil, l= 230 mm
Cell temperature 45 °C (+/- 0.3 °C)
Measuring ranges
0,01 - 10 µg/l at 10 ml sample volume
liquid sample
0,1 ng/g - 0,1 µg/g at 1 g sample weight
solid sample
Sensitivity ca. 5 ng/l resp. 0,05 ng absolutely
Air flow 30 l/h
Analogue output Absorption; 4 - 20 mA
Serial (RS 232 and USB) for PC connection,
Digital outputs
parallel (Centronics) for printer connection
Electrical power consumption max. ca. 40 W
90 V AC-132 V AC and 187 V AC - 264 V AC, 47-63 Hz;
Power supply
12 V DC (option)
45 x 15 x 35 cm (WxHxD) photometer unit
Dimensions
24 x 48 x 27 cm (WxHxD) reaction unit
Weight ca. 10 kg

5.2 Operating conditions


Operating temperature 0 °C ... 40 °C
Operating humidity ca. 90 % max. R.H.
according to 89/336/EEC and
CE approval
73/23/EEC

5.3 Storage and transport


The interior of the photometer unit should be kept save from moisture and hard shocks.
All glass parts of the reaction unit should be packed with care when transporting the
LabAnalyzer.Vibrations caused by transport in a car or an airplane do not harm the photometer
unit.

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5.4 Spare parts and accessories


ID Item Description
201-01 Reaction flask, with 10 ml mark, standard ground cone NS 24
201-02 Bubbler, with glass frit and standard ground cone NS 24
201-03 Connection tubing photometer - reaction unit, Tygon R3603

Tygon tubing, 4/7,


201-03m
internal tubing for photometer or sample tubing

Activated Carbon Filter


201-04
filled with sulphurized activated carbon, 11,5 cm³

Bubbler, with glass frit and standard ground cone NS 24,


201-05
with septum for NaBH4-method
201-06 Spare septa set (100 pcs.) incl. 10 syringes
201-07 Rack for reaction flasks
201-11 Y-piece, glass, for the connection tubes between pinch valve and optical cell
201-12 Tubing-connector (PTFE) at pinch valve
Membrane Filter
202-05
PTFE, 47 mm diameter, 1µ, pack of 25 pcs.
202-06 Signal cable with BNC plug, l = 180 cm
202-07/7a PC connection cable to transfer Data to a PC via RS 232 / via USB
202-08 Printer connection cable (Centronics)
203-01 Membrane pump complete pump
Optical cell
203-02
l= 230 mm, completely made of synthetic fused silica (Suprasil)
203-03 Pinch valve complete unit, 2 valves unit
203-08 LC-Display with LED backlight
Fitting, for connection of a 4 mm (ID) x 6 mm OD) sample tubing to the sample inlet
203-10
filter
203-12 Tubing for the pinch valve
203-60a Filter holder, clear plastic holds 47 mm diameter filters
203-61 UV Lamp, electrodeless spare lamp bulb
301-10 Buffer battery for RAM, Li-battery
301-11 4-20 mA-IC with cooler
301-12 Battery charger ACS 110
301-15a Charger cable for battery pack
350-01a Rechargeable battery pack, 12 V, for ca. 4-5 h operation, charge / discharge function
Conversion kit to upgrade the LabAnalyzer with mercury vapor monitor VM-3000
200-03
function

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5.5 Block diagram of electrical parts

Fig. No.19: Electrical block diagram of the photometer unit

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5.6 Diagrams of components

Figure 20: Diagram of components and tubing (different to the LA / VM-3000 version)

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11b
10 11 13 12 14 15
19 11a 11a

7 4c 5
17 4d
4b 3 4e 4a 6

16 1 18 2

No. in fig. Description Ref. No.


No. in fig. Description Ref. No.
1 Filter holder 203-60
1 2 Filter holder
Front panel with keypad 203-60a203-50
2 3 Front panel
Displaywith keypad 203-50203-05
3 4a DisplayInterface board 203-08300-62
4a 4b Interface board
Computer board 300-62o203-52
4b 4c Computer board
Eprom with software 203-52 -
4c 4d Eprom Li-battery
with software
for microprocessor
-
301-10
4d Li-battery for microprocessor 301-10
4e
4e P-sensorP-sensor
(LA / VM (LAcombi / VM
only)combi only) 650-40c650-40c
5 5 MembraneMembrane
pump pump 203-01203-01
6 6 Power Power supply with transformer
supply switch 203-53203-53
7 7 Pinch valve
Pinch valve for zero air
for zero air 203-03203-03
8 8 Activated carbon for zero air
Activated carbon for zero air 201-04201-04
9 9 UV detector
UV detector 203-54203-54
10 Optical cell 203-02
10 Optical cell 203-02
11 Complete optical bench 203-55
11a
11 Complete optical
Fixing clamps for optical cell bench 203-88203-55
11b 11aHoldingFixing bracketclamps
for optical forcell
optical cell - 203-88
11bincludingHolding
heater bracket for optical cell -
12 Outputincluding
signal board heater 203-66
13 12 Lamp Unit
Outputcontaining
signal board 203-66
13 a) UV lamp
Lamp Unit containing 203-61
b) HF board 203-67
a) UV lamp
Gas exit fitting 203-16
203-61
14
15 b) HF board
230 V / 110 V power cord receptable 203-59203-67
16 14 Filter membrane,
Gas exit PTFE fitting 202-05203-16
17 15 Transformer
230 Vfor/ heating
110 V power opt. cell cord receptable203-56203-59
18 16 Fitting for
Filter membrane,
sample gas inlet PTFE 203-10202-05
19 17 T-sensor (PT-100) (LA / VM combi
Transformer for heating opt. cell only) 203-51203-56
18 Fitting for sample gas inlet 203-10
19 T-sensor (PT-100) (LA / VM combi 203-51
only)
Figure 21: Part numbers of components (photometer unit)

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LabAnalyzer 254

LabAnalyzer 254

8
MERCURY INSTRUMENTS
Gas Flow
1

2
6

No. in fig. Description Ref. No.

1 Flowmeter 203-04
2 Activated carbon filter 201-04
3 Reaction flask 201-01
4 Bubbler 201-02
5 Drain pan 201-63
6 Connection tubing 201-03
7 Securing clamp 203-21
8 Connection tubing 201-20
Fig. 22: Modules and part numbers of the reaction unit

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6. Appendix A: Working with the LabAnalyzer 254


6.1 Sample preparation

The preparation of samples for mercury analysis is in fact as important as the measurement
itself. An extensive discourse on this subject would go beyond the scope of this manual.
However, the following pages may give some useful hints for carrying out mercury analyses.

The preparation of samples to be analysed with the LabAnalyzer


254 requires handling of more or less hazardous substances.
Therefore only qualified and trained persons should carry out
sample digestion.

Mercury Instruments is taking no responsibility for material or


physical damages due to improper handling of chemicals !

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1. For its determination the mercury in the sample has to be reduced with tin-II-chloride (or
sodium-tetra-hydroborate) into the elemental form.
2. Before this step all the mercury in the sample must be oxidised to the bivalent state. In
order to achieve this, the sample is treated with strong oxidizing reagents. Examples
for these reagents are: potassium permanganate solution + hydrochloric or sulphuric
acid, potassium dichromate solution + sulphuric acid, sodium peroxodisulphate solution,
hydrogen peroxide solution + UV irradiation, concentrated nitric acid, aqua regia,
mixtures of perchloric acid + nitric acid + sulphuric acid.
3. Subsequently to the oxidation step excess of reagent is reduced by addition of
hydroxylamine-hydrochloride solution.
4. This step is followed by addition of tin-II-chloride solution and stripping of the mercury
from the sample.

6.2 Reagents for analyses


A) Calibration standard:

Solutions for calibration are prepared from a mercury standard solution with a
concentration of 1 g/l Hg (can be purchased for example from Merck, ref. No. 1.70226).
This solution is stable for at least 2 years.
To 1 ml of this standard ca. 100 ml of reagent water and then 10 ml concentrated
nitric acid are added in a 1000 ml- volumetric flask. Then fill up with reagent water
to the mark. Concentration now is 1 mg/l Hg (= 1 ppm). This solution is stable for ca.
2 months. From this solution the calibration solution for each calibration is prepared
freshly.
Example: Transfer 1 ml of the 1 ppm solution into a 100 ml volumetric flask, add a
few drops of potassium dichromate solution until color is light yellow, and make up
with reagent water to the mark. The concentration of this solution is 10 µg/l (10 ppb).
For calibration 0,1 - 1 ml of this 10 ppb solution (corresponding to 0,1 - 1 ppb Hg)
are filled in the reaction flask of the LabAnalyzer and made up with water to the 10
ml-mark.

B) Hydroxylamine hydrochloride solution:


10 g HONH3Cl (eg Merck Nr. 1.04619, max. 0,000001% Hg) are dissolved in 100
ml water.

C) Tin-II-chloride (stannous chloride) solution:


30 ml concentrated hydrochloric acid are diluted with ca. 30 ml water. 10 g SnCl2*2
H20 (eg Merck Nr. 1.07814, max. 0,000001% Hg) are added and dissolved. The
solution is made up with water to 100 ml.

D) Potassium dichromate solution:


About 0,5g K2Cr2O7 (eg. Merck ref. no. 104865) are diluted in 25ml HNO3 conc
(eg. Merck ref. no. 100452, 65% HNO3). Fill up with water to the 100 ml mark.

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6.3 Short instructions for performing an analysis

In order to get familiar with handling of the instrument we recommend first to follow the
instructions given in the main part of this manual.

A) Switch on photometer at least 30 minutes before.

B) Enter or select name of analyst. Select „Analyze Sample” by pressing F1. Select
calibration. Adjust air flow following the instructions on the screen.

C) Enter sample number (letters and numerals) and (if applicable) dilution factor, then
press F3. The sample should have a concentration within the range of calibration. For
samples of unknown concentration level it is recommended to use a smaller volume of
sample (0.1 to 1 ml) and fill up to 10 ml with water (risk of overrange). Example: if a
1 ml sample is diluted to 10 ml the dilution factor is 10.
D) Open reaction flask.

Fig. 23: To open reaction flask push securing clamp backwards


and pull flask carefully down (a slight turning movement helps in
some cases)

Remove reaction flask only if pump is not running!


Because of underpressure the force required for removing the flask
is too big and may damage glass parts!

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E) Fill digested sample up to mark (10


ml). In case of smaller sample volumes
sample
fill up to the mark with water and
enter corresponding dilution factor as
mentioned earlier.
For very precise analysis use either a
10 ml narrow-necked volumetric flask
10 ml of sample 10ml

or a graduated pipette to get exactly 10


ml of sample volume into the reactor.
Fig. 24
F) Add some drops of hydroxylamine
hydrochloride solution (the purple
color of previously added potassium
permanganate should fade to a very
light or colorless hue)

G) Add 0,5 ml tin-II-chloride solution, connect reaction flask with bubbler and secure
with clamp.

H) Press F3 to start measurement.

I) A beeping sound announces end of measurement. The result of the analysis is displayed
on the screen. If a printer is connected to the LabAnalyzer the printout of the analysis
is automatically performed.
Open reaction flask and empty it. Rinse with water to clean it for next analysis.

6.4 Record of signal


The figure below shows a record of the analogue measuring signal from a 0,1 µg/l sample.
Width of the peak is ca. 65 seconds.

Fig. 25: Analogue 4 - 20 mA signal (0,1 µg/l sample

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6.5 Some commonly used sample preparation methods

If you have already made good experience with a special sample preparation procedure you
can use it of course also for analyses with the LabAnalyzer 254.

6.5.1 Water

For determination of mercury in water standard methods according to current regulations


are recommended (method DIN 38 406/12 in Germany, European standard EN 1483).
References see http://www.din.de.

6.5.2 Biological samples

Example: Digestion according to Höllerer and Hoffmann (G. Höllerer, J. Hoffmann,


Zeitschrift für Lebensmittel-Untersuchung und -Forschung, 150, 277-280 (1973).
For flesh, fish, hair, claw and nails, fresh plant material.

For materials with high content of cellulose like wood you should use only concentrated
sulphuric acid instead of the acid mixture described below.

Transfer the homogenised and exactly weighed sample (ca. 0,5 g for a measuring range
of 0,001 to 0,1 mg/kg Hg) into a 60 ml digestion vessel (made of PFA or FEP). Add 10
ml of an acid mixture (concentrated sulphuric acid and concentrated nitric acid in equal
parts) and close digestion vessel. Then heat sample for 2 hours in a water bath to max. 60
°C or leave standing at room temperature for 12 hours. A clear solution should develop.
Cool in an ice bath and open
c a r e f u l l y (possibility of pressure in the digestion vessel), dilute with 15 ml ice-cooled
distilled water and add 0.75 g potassium permanganate. Samples with a high COD may
require more permanganate. Close digestion vessel again and heat to 60 °C until gas
development stops. Let cool to room temperature.

Comment: dry material should be moistened with water first.

6.5.3 Food

Digestion with HNO3 at 180 °C in an autoclave vessel. 200 mg of the solid or 2 ml of the
liquid sample are treated with 2 ml nitric acid (min. 65 %).

More details see: Amtliche Sammlung von Untersuchungsverfahren nach § 35 LMGB:


Untersuchung von Lebensmitteln, Aufschlußverfahren zur Bestimmung von Blei und
Cadmium in Lebensmitteln, Druckaufschluß. Ausgabe L 00.00-19 vom Dezember 1989.

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LabAnalyzer 254

6.5.4 Drinks (wine)

According to Cacho & Castells (J. Cacho, J. Enrique Castelles), Atomic Spectroscopy, 10,
No. 3, 85-88 (1989).
Place 5 ml of the liquid sample in a 100 ml Erlenmeyer flask. Add 2 ml concentrated
nitric acid, cover the opening of the flask with a laboratory sealing film (for example
Parafilm™) and leave standing for one hour. Then, while shaking, slowly add 5 ml 5%
chromic acid solution; keep flask cool in an ice water bath. Once cold, remove flask from
the ice water bath, cover again with sealing film and leave standing at room temperature
for 60 minutes, shaking every 10 minutes. Then add 0,5 g hydroxylamine hydrochloride,
cool, and transfer the contents to the reaction flask of the analyzer.

6.5.5 Liquid waste and ground water

According to EPA method 7470A.

Transfer 100 ml, or an aliquot diluted to 100 ml, containing < 1 mg of mercury, to a 300
ml BOD bottle or equivalent. Add 5 ml of H2SO4 and 2.5 ml of concentrated HNO3,
mixing after each addition. Add 15 ml of potassium permanganate (5 g/100 ml) solution
to each sample bottle. Sewage samples may require additional permanganate. Ensure
that equal amounts of permanganate are added to standards and blanks. Shake and add
additional portions of potassium permanganate solution, if necessary, until the purple
color persists for at least 15 min.
Add 8 ml of potassium persulfate to each bottle and heat for 2 hours in a water bath
maintained at 95 °C. Cool and add 6 ml of sodium chloride-hydroxylamine sulfate to
reduce the excess permanganate.
After a delay of at least 30 sec, add 5 ml of stannous sulfate solution and immediately
attach the bottle to the aeration apparatus.

Comment: The volumes of sample and reagents should be reduced as the LabAnalyzer
254 requires only 10 ml for an analysis. The mercury concentration can be much lower
than described in the method above due to the high sensitivity of the instrument.

6.5.6 Natural gas

Sample preparation according to ISO 6978. Publication can be ordered from:


International Organization for Standardization, Case Postale 56, CH-1211 Genève 20

6.5.7 Microwave oven sample decomposition

Acid decompositions with nitric and sulphuric acid. Follow instructions of manufacturers.

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6.5.8 Sewage sludge, sediments, soil, construction rubble and


contaminated glass

a) Aqua regia digestion according to the German standard “DIN 38 414 S7 /


Klärschlammverordnung von 1992”.
3 g of the homogenized and weighed sample are transfered into the digestion flask of the
digestion apparatus.
Then step by step 21 ml concentrated HCl (32 - 36 %) and 7 ml concentrated HNO3 (65 %)
are added. If foam develops, the acids are added carefully drop by drop. The absorption
reservoir of the apparatus is filled with 10 ml HNO3 (0.5 mol/l). The digestion flask and
the absorption reservoir are connected with a condenser and left standing for several
hours at room temperature.
Subsequently the digestion flask is heated and maintained at boiling temperature for
2 hours. After cooling the liquid in the absorption reservoir is filled through the condenser
into the digestion flask.
Absorption reservoir and condenser are rinsed with a few ml of HNO3 (0.5 mol/l)
collecting the acid in the digestion flask. The content of the digestion flask is transferred
into a 100 ml volumetric flask and made up with water to the mark.

Comment: In order to prevent losses of mercury, the sample should not be dried as
described in the original of the method.

b) Simplified digestion with aqua regia according to EPA method 7471A:


Weigh triplicate 0.2 g portions of untreated sample and place in the bottom of a BOD
bottle. Add 5 ml of reagent water and 5 ml of aqua regia. Heat 2 min in a water bath at
95 °C. Cool.
Then add 50 ml reagent water and 15 ml potassium permanganate solution (5 g/ 100 ml)
to each sample bottle. Mix thoroughly and place in the water bath for 30 min at 95 °C.
Cool and add 6 ml of sodium chloride-hydroxylamine sulfate to reduce excess
permanganate.
Before analysis add 55 ml of reagent water. Caution: do this under a fume hood, as
chlorine could be evolved.

6.5.9 Hair

According to Giovanoli-Jakubczak, Greenwood, Smith and Clarkson (Clin. Chem. 20/2,


222-229 (1974).
To the weighed sample (up to 100 mg), 2 ml of a solution of NaOH (11,2 mol/l) is added;
the vial is placed on a hot plate at 125 °C and heated, with occasional agitation until the
hair just dissolves. Care should be taken not to boil the sample.
After dissolution of the hair, the vial is immediately placed in ice water and 8 ml of NaCl
solution (dissolve 1g NaCl in 100 ml of reagent water) are added. The vial is closed with
a cap and mixed. Analysis is carried out immediately.
The method described under “Biological Samples” is also suitable.

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6.5.10 Flue gas / stack gas

According to the German standard method VDI 3868 Blatt 2 or the European Standard
EN 13211 (proposal).
The gas is drawn through a sulphuric acid / nitric acid / potassium permanganate solution
contained in a bottle with bubbler insert. Two or three of these bottles are set in a row.
After collecting a known volume of gas, the acid solutions are mixed, hydroxylamine
hydrochloride is added, and the sample is analyzed.

Comment: Special care must be taken to avoid adsorption of mercury and mercury-II-
chloride on the inner surface of the sampling apparatus.

6.5.11 Petroleum and petroleum products

The whole organic matrix of these sample materials has to be decomposed by oxidation.
One method used is acid decomposition with sulfuric and nitric acid in a closed system;
the another method uses combustion of the sample in an oxygen/hydrogen combustion
apparatus (Wickbold apparatus) and collecting the volatilized mercury in acidic
permanganate solution.

Lit.: Henry E. Knauer, George E. Milliman, Analytical Chemistry, 47, 8, 1263-1268


(1975).

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7. Appendix B: Statistical Performance Data

7.1 Detection Limit and Limit of determination


For method validation and quality control statistical data deriving from calibration data are
used.
A typical calibration report using data achieved from measurement of calibration standards
is shown on the following page.

7.2 Uncertainty
Following table shows the statistical uncertainty of measurement results for a low-range
calibration at a significance level of 99 %.

99 %Significance
! !
Reading Concentration
Uncertainty Uncertainty Sample ID
Absorbance µg/l Hg
µg/l Hg %
0.0010 0.018 0.005 29.6 CAL-10
0.0015 0.039 0.005 13.6 CAL-15
0.0020 0.081 0.005 6.4 CAL-20
0.0030 0.122 0.005 4.3 CAL-30
0.0040 0.163 0.005 3.4 CAL-40
Table 1: Uncertainty of measurement results.

Following table shows the statistical uncertainty of measurement results for a medium-range
calibration at a significance level of 99 %.

99 %Significance
! !
Reading Concentration
Uncertainty Uncertainty Sample ID
Absorbance µg/l Hg
µg/l Hg %
0.0020 0.078 0.027 34.4 CAL-20
0.0050 0.190 0.026 14,0 CAL-50
0.0100 0.373 0.026 7.1 CAL-100
0.0200 0.740 0.030 4.1 CAL-200
Table 2: Uncertainty of measurement results.

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LabAnalyzer 254

Calibration Report created 03-Apr-2003

General Data

Raw Data C:\EXCEL\QC_Data\Cal-LabAnalyzer.txt


Date 01.04.03
Analyst A. Sauerer
Analyte Hg
Matrix Water
Anaytical Instrument LabAnalyzer-254; Serial No. 1102/252
Remarks none

Calibration Points
Calibrator Reading
0,0060
No. µg/l Hg Absorbance
1 0,000 0,0001
2 0,020 0,0005 0,0050
3 0,040 0,0010
4 0,060 0,0015
5 0,080 0,0020 0,0040
6 0,100 0,0025
7 0,120 0,0029
f(X)

8 0,140 0,0035 0,0030


9 0,160 0,0040
10 0,180 0,0044
11 0,200 0,0049 0,0020
12
13
0,0010
14
15
16 0,0000
0,000 0,050 0,100 0,150 X 0,200 0,250

Characteristical Data

Slope 0,0240 Number of Repetitions 1


Achsenabschnitt 0,0000 Reststandardabweichung 0,0000
Linear Correlation Coeff. 0,9998 Verfahrensstandardabweichung 0,0010
Uncertainty 33,33 % Summe der Abweichungsquadrate 0,0440
Irrtumswahrscheinlichkeit 1,00 % Quantile (einseitig) 2,8210
Quantile (zweiseitig) 3,2500

Analytical Performance Data according to DIN 32645

Detection Limit 0,005 µg/l Hg


Erfassungsgrenze 0,009 µg/l Hg
Limit of Determination 0,016 µg/l Hg

Fig. 26 : Example for a statistical evaluation of LabAnalyzer 254 calibration data according to DIN 32645

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8. Appendix C: EC-Declaration of Conformity

EC-Declaration of Conformity
The Company: Mercury Instruments GmbH
Liebigstrasse 5
D-85757 Karlsfeld
Germany
Declares that the product: VM-3000 Mercury Vapor Monitor
Intended purpose: Automatic measurement of mercury at trace
concentration levels in air and other gases
conforms with the basic requirements of the relevant EC directives.

A conformity assessment method as provided in the directives has been executed.

The following harmonized standards were applied:

EN 50 081-1: 1992 EN 61000-3-2: 1998


EN 50 081-2: 1993 EN 61000-3-3: 1996
EN 50 082-2: 1995 EN 61000-4-2: 1995
EN 55 011: 1991 EN 61000-4-3:1996, 2006 +A1:2008 + A2:2010
EN 55 011: 1991 EN 61000-4-4: 1995
ENV 50 204: 1995 EN 61000-4-6: 1996
EN 61326-1:2006 EN 61000-4-11:2004
EN 61010-1 + A1:1993 + A2:1995

The tests regarding above standards have been conducted by Intertek Deutschland GmbH,
Kaufbeuren/Germany (Test Reports No. 97KFE163/98-01-14, 00KFE1188/00-11-21 and
2218843KAU-001).

The test documents are available for inspection.

This declaration is submitted by:

Karlsfeld, 7th May, 2013 Dr. Brigitte Inderst


(CEO)

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LabAnalyzer 254

Index

A Cleaning.................................................................. 44
~ the bubbler......................................................... 44
Accessories............................................................. 48 ~ the optical cell................................................... 45
AD 0-7.................................................................... 42 Cold vapor method................................................... 8
Adjusting the air flow............................................. 20 Commonly used sample preparation methods........ 57
after start-up........................................................... 41 Configuration.......................................................... 26
Air flow................................................................... 20 Connecting a printer............................................... 16
Analogue signal 4-20 mA....................................... 15 Connection of the electrical outputs....................... 15
Analyze sample...................................................... 19 Construction rubble................................................ 59
Analyze Sample...................................................... 18 Contaminated glass................................................. 59
Appendix
A: Working with the LabAnalyzer 254.................. 53
B: Statistical Performance Data.......................... 61 D
C: EC-Declaration of Conformity........................ 63
Aqua regia digestion............................................... 59 Data
ASCII characters.................................................... 35 delete..................................................................... 36
Automatic print....................................................... 27 erase all (Hg-Tansfer).......................................... 30
print............................................................... 26, 35
recall....................................................... 18, 27, 35
B record.................................................................... 26
transfer to a PC or Laptop............................ 25, 36
Battery charger....................................................... 12 Date........................................................................ 37
features of the ~.................................................... 13 Delete
Battery operation.................................................... 11 calibration............................................................ 34
Biological samples................................................. 57 data....................................................................... 36
Block diagram of electrical parts............................ 49 error records......................................................... 39
Bubbler................................................................... 44 name of analyst..................................................... 18
Detection Limit....................................................... 61
Device data............................................................. 37
C Diagrams of components........................................ 50
Calibration....................................................... 18, 31 Dilution factor........................................................ 23
constant................................................................. 39 Display components............................................... 15
data....................................................................... 31 Drinks..................................................................... 58
delete..................................................................... 34 during start-up........................................................ 40
equation................................................................ 33
gradient................................................................. 39
graph.................................................................... 33
E
perform new ~....................................................... 32 Entering
Set ~ data manually.............................................. 39 dilution factor....................................................... 23
store...................................................................... 34 name of the analyst............................................... 17
Calibration standard............................................... 54 sample identification............................................. 21
Charging sample identification (short cut)........................... 22
operation............................................................... 12 sample name......................................................... 21
times...................................................................... 13 service code 321................................................... 36
Check service code 987................................................... 41
Calibration P-Sensor............................................ 40
heating of the optical cell..................................... 38
Memory Batt......................................................... 40
Optical Cell.......................................................... 41
Parameters........................................................... 40
stored calibration data......................................... 31

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LabAnalyzer 254

equation.................................................................. 33 L
Error messages....................................................... 40
after start-up Lamp....................................................................... 42
Replace carbon filters....................................... 41 Lamp Unit............................................................... 14
during operation LEDs....................................................................... 13
AD 0-7............................................................... 42 Limit of determination............................................ 61
Lamp................................................................. 42 Liquid waste........................................................... 58
Temp. opt. cell................................................... 42 Loss of air flow....................................................... 46
during start-up
Photometer Malfunction Check Optical Cell... 41
WARNING Check Calibration P-Sensor........... 40
M
WARNING check memory batt.......................... 40 Main menu.............................................................. 18
WARNING EEP INIT check parameters........... 40 Maintenance........................................................... 40
Error records Measuring principle.................................................. 8
delete..................................................................... 39 Microwave oven sample decomposition................ 58
show...................................................................... 39 Modules and part numbers of the reaction unit...... 52
Excel....................................................................... 29

N
F
Name of analyst
Features of the battery charger............................... 13 delete ~................................................................. 18
Fields of application................................................. 8 enter new ~........................................................... 17
Flow meter.............................................................. 20 select ~.................................................................. 17
Flue gas................................................................... 60 store ~................................................................... 17
Food........................................................................ 57 Natural gas.............................................................. 58
Fuses................................................................ 14, 46

O
G
Operating conditions.............................................. 47
Gas flow.................................................................... 9 Operating the LabAnalyzer 254............................. 17
General description................................................... 8 Operation................................................................ 11
General information for safe operation.................... 3 Battery~................................................................ 11
Glass....................................................................... 59 on mains............................................................... 11
Ground water.......................................................... 58 operational Hours................................................... 41
Operation and display components........................ 15
Optical cell...................................................... 38, 45
H Outliers............................................................ 31, 33
Hair......................................................................... 59 Output socket
HF-board................................................................ 14 parallel ~ for printer connection.......................... 16
Hg-Transfer............................................................ 15 serial ~ RS 232..................................................... 15
configuration......................................................... 26 USB....................................................................... 15
main window......................................................... 25
port settings.......................................................... 26
select language..................................................... 25
transfer mode - print data..................................... 26
transfer mode - reord data.................................... 26
Hydroxylamine hydrochloride solution.................. 54

J
jpg file..................................................................... 28

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LabAnalyzer 254

P S
Parallel output socket for printer connection......... 16 Sample
Particle filter........................................................... 43 identification......................................................... 21
Part numbers of components name..................................................................... 21
Photometer unit.................................................... 51 number.................................................................. 21
Reaction unit......................................................... 52 Sample decomposition........................................... 58
Performing an analysis........................................... 55 Sample preparation................................................. 53
Perform new calibration......................................... 19 ~ methods.............................................................. 57
Petroleum and petroleum products......................... 60 Save
Photometer Malfunction......................................... 41 continuously.......................................................... 27
Photometer Malfunction Check Optical Cell......... 41 logfile.................................................................... 27
Photometer unit............................................... 10, 51 page...................................................................... 28
Port setting....................................................... 26, 35 Schematic gas flow................................................... 9
Potassium dichromate solution............................... 54 Sediments............................................................... 59
Power supply.......................................................... 11 Select
Preparation for operation........................................ 10 calibration............................................................ 19
Preventive maintenance.......................................... 46 data....................................................................... 35
Print data.......................................................... 26, 35 name of analyst..................................................... 17
Printer port.............................................................. 37 Operation Mode.................................................... 19
Printout of results................................................... 24 printer................................................................... 26
Print View window................................................. 28 Select language
PT-100.................................................................... 11 Hg-Transfer.......................................................... 25
LabAnalyzer.......................................................... 38
Serial data output.................................................... 15
R Service.................................................................... 18
Reaction unit.................................................... 10, 52 Service code
Reagents for analyses............................................. 54 321........................................................................ 36
Rear panel........................................................ 10, 11 987........................................................................ 41
Recall data................................................ 18, 27, 35 Service menu.......................................................... 36
Record data............................................................. 26 Set
Record Mode................................................... 26, 29 air flow.................................................................. 20
Record of signal...................................................... 56 calibration data manually.................................... 39
Replace carbon filters............................................. 41 date and time........................................................ 37
Replacement language (LA)....................................................... 38
of the bubbler........................................................ 44 printer mode........................................... 16, 24, 25
of the carbon cartridges....................................... 43 Sewage sludge........................................................ 59
Replacing the carbon cartridge Short instructions for performing an analysis........ 55
~ of the gas outlet................................................. 44 Show Calibrations.................................................. 31
~ of the internal cartridge for zero air................. 43 Show error records................................................. 39
~ of the reaction unit............................................ 44 Significance............................................................ 61
Reset of operational Hours and soil.......................................................................... 59
total absorbed Hg................................................. 41 Spare parts.............................................................. 48
Resonance absorption............................................... 8 Stack gas................................................................. 60
Rreference beam....................................................... 8 Start measurement........................................... 21, 23
RS 232.................................................................... 15 Start-up................................................................... 10
Rubble.................................................................... 59 Statistical
~ evaluation of LabAnalyzer 254
calibration data................................................ 62
~ performance data.............................................. 61
Storage and transport.............................................. 47

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LabAnalyzer 254

T W
Technical Information............................................ 47 WARNING
Technical specifications Check Calibration P-Sensor................................. 40
Battery charger..................................................... 13 check memory batt................................................ 40
VM-3000............................................................... 47 EEP INIT check parameters................................. 40
Temperature sensor................................................. 11 WARNING check memory batt............................. 40
Temp. opt. cell........................................................ 42 WARNING EEP INIT check parameters............... 40
Test of 4-20 mA signal output................................ 38 Water....................................................................... 57
Time........................................................................ 37 Wine....................................................................... 58
Tin-II-chloride (stannous chloride) solution.......... 54 Working with the LabAnalyzer 254....................... 53
total absorbed Hg.................................................... 41
Transfer data to a PC or laptop........................ 25, 36
Transfer mode
print data.............................................................. 26
record data............................................................ 26
Troubleshooting
Fuses..................................................................... 46
Loss of air flow..................................................... 46
Ttransport............................................................... 47
Turning on the LabAnalyzer 254........................... 17
Tygon...................................................................... 10

U
Uncertainty............................................................. 61
Unpacking.............................................................. 10
USB........................................................................ 15

Flowcharts
Flowcharts 1a and 1b (folded) will give you a structural overview for:
Start-up displays
Select Analyst displays
Calibration
Sample analysis

Flowchart 2 (folded) will give you a structural overview for:


Start-up displays
Select Analyst displays
Recall data
Service

Lab_Analyzer_E__V_5_2.indd 11 - 08 - 2016 Page 67


Flowchart 1a: Start-up & Main Menu
Display No. 1 Display No. 2 Display No. 3-1

Analyse ample

Calibration
Back to Main Menu
Display No. 3-2 Display No. 3-4

Back to Main Menu

Display No. 4-1:


Display No. 3-3 Display No. 3-5 Main Menu
LA only

Display No. 4-2:


Main Menu
LA / VM Combi

Display No. 6
RE ME
AD

Flow Chart
-2-
Recall Data
&
Service

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