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Hamid
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To everyone who has helped us with support,
http://www.milestonesrl.com/
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• Introduction
• Hardware
• System initialization
• Software
• Analysis
• Applications
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Direct Mercury Analyzer for analysis of liquid, solid and gaseous samples
thermal decomposition.
preparation.
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• Results in 5 minutes.
field analysis.
matrices.
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• Elemental mercury
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• Solid, liquid or gas samples are weighed and
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The DMA-80 produces accurate results over a wide dynamic range and on a variety of different matrices.
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• The DMA-80 produces matrix independent results.
• The instrument is calibrated with aqueous standards and analyzes organic and inorganic solid samples.
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Front View
Back View
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1. Sample dosing system.
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• The DMA-80 has a built-in 40 positions
pre-concentration on amalgamator.
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• Purpose of the pneumatic section is to take
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Auto-sampler motor
plate.
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• The samples are weighed and carried for
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• After the loading and positioning steps the
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• Moisture removal from solid samples, bulk
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• keep the temperature of the catalyst tube
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• Hg is trapped in the amalgamator and all the other
gases are flushed out of the system before Hg is
measured in the cuvette.
• The amalgamator coil has a double purpose: to keep the
amalgamator tube at the stand-by temperature of
around 170°C/150°C and then to quickly heat it up to
850°C.
• The temperature is measured with an infrared sensor.
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• The spectrometer works with a single
beam system with sequential flow through
measurement cells.
• It is composed of:
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• Normal system: The spectrometer works
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• Tricell system: The spectrometer
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• Light source is a low pressure mercury
vapor lamp.
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• Cuvette system with quartz window.
condensation.
• Clean the windows using a very soft tissue and some acetone.
• Dry them very well, in order not to left any mark on the quartz.
• Tricell DMA-80: The first and long one cuvette is used for
• The second medium one (10-20ng), the third and short one for
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• Detector is UV enhanced Si- photodiodes.
• Detection limit:
0.005 ng of Hg (dual-cell)
0.0015 ng of Hg (tri-cell)
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Terminals 660 ( 1660)
or Vista.
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Function Carrier and decomposition gas
“Research” grade
Purity
(O2 > 99,95%)
Internal oxygen
3.1 bar
pressure
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• The required Oxygen must have a flow rate
at 3,1 bar.
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• Oxygen/Air connection,
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• Mercury trap to be located at
DMA-80 outlet.
• Activated charcoal.
• Safe operation.
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• The DMA-80 system must be installed in a
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System initialization steps:
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• Click on DMA-80 Measurement icon and wait
the amalgamator.
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Create a new working method (sample path and temperatures) in according to the
information you can find in the table.
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• In the calibration page load the
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Proceed with this method:
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• The solution (100 µl of 100ppb) must be fresh • Go to Meas. Page and press the white paper to
and stabilized with 1-2% of HCL(ultrapure). create a new measurement file and save it as
• Create a new working method “stability”.
1) 00:00:10 200°C • Quartz sample boat required.
4) 00:01:30 650°C
• Purge time P: 60 s
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• Once the analyse has ended, you have to verify:
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• Evolution of previous Windows™ based
DMA-80 software.
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Item Symbol Function
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DMA-80 MEASUREMENTS
1. Method
2. Calibration
3. Measurement
4. System
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• To create a new method its Program
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Item Symbol Function
Go back Go back to the start screen, save any changes before quitting.
Start If there is a sand clock on, this means that a Current procedure
must first be accomplished (e.g. Heating of furnace and cuvette).
Stop The current measurement is interrupted and the sample boats
are taken back to the auto sampler tray.
Restart The stop-button must then be re-set Touching the red-green stop-
button.
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No. Function Meaning
5 Amalgam Heater Time The time required by the amalgam heater to completely
release the Hg collected in the absorption cell.
6 Recording Time Time for Noted and evaluated the measuring signal of the
spectrometer.
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Temperature Typical
Step Time range Typical time
range temperature
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• Purpose is to administer the calibration
files.
• From a calibration file you can select the
used measuring points and specify the
regression curves for each cuvette.
• Different calibration files can be opened,
created and saved.
• All cuvettes are always used for
measurement.
• If the maximum peek of the first signal is
over 1.0 A (standard setting), the maximum
of the second signal will be used to
calculate the result.
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Item Symbol Function
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Low value used for 1st cell
calibration 0 – 35 ng.
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High value used for 2nd cell of
calibration35 – 600 ng.
• Stock solution of 1000 ppm can be Standard 1000 ppm HCl 36% Deionized
solution in ml in ml water in ml
stored for one year if maintained in
1 ppm 0.1 1 Up to 100
its original tightly sealed bottle away
from sunlight and intense sources of 2 ppm 0.2 1 Up to 100
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• The extinction process can be monitored in
real time.
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Item Symbol Function
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• Sample name, The Name is taken over from the selected record and can be changed/modified.
• Pos, Consists of two numbers: If Simple sample processing is activated, and a sample is added,
the number over the selected record will be taken, alternatively the sample can be selected (from
pos. 1 to 40), as in this operating mode each sample can be measured individually.
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In this Register you can select the calibration file (Cal-Date) and Methods to be used for the
process.
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• On the left of the screen there is a
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• Check the signal for a typical good
peak:
(6,85s) = 15 seconds
from 5 to 8 L/h.
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• The average final result with the relative standard deviation is shown in the headline of the
multiple measurements. Individual values can be disabled removing the sigma sign.
• Hg [ng], Absolute quanty of Hg in the sample (calculated from active calibration) c[μg/kg] or
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Here the system is supervised (Autosampler, heating elements, spectrometer)
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After the start of the system all Standby functions are activated:
• Catalyst, amalgamator unit and absorption cells are heated up to Standby temperatures.
• HEATING 1: for drying and decomposition of the sample. Here also the oxygenation takes place.
condensation water. Heating to high temperature is then used to release very rapidly the
accumulated Hg.
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• Working range: from 0.05 ng up to 600 ng absolute value of Hg.
• Eliminate any source of contamination coming from environmental dust or from the
samples.
• Clean the laboratory tools such as spatula, balance plate, tweezers, etc.
• The working standards solution must be freshly prepared before every calibration.
• Stock solution of 1000 ppm can be stored for one year if maintained in its original tightly
sealed bottle away from sunlight and intense sources of radiation, in a refrigerator at 10°C.
• Note: It is recommended to measure liquid samples only in Single mode using metal boat.
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• Diluted liquid standard solution can be stored for one month.
• The curve comprises the entire range of interest, working range 0.5– 600 ng.
• The quality of the calibration curve can be also improved by using quartz boats,
• Quartz boat are completely inert; they have no memory effect, and do not interact
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• Increase the decomposition time will reduce the memory effect.
• Increase the recovery from difficult inorganic sample matrices, such as metal oxide, by
• Reduce the drying temperature and extend the time if strong exothermic reaction
persists.
• With liquid samples, metal boats can be used only in single mode, to minimize the loss
of mercury due to chemical interaction between the acid matrix and the metal boat.
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• Drying time (sec) = Sample Volume (μL) × 0.6 or
• Reduce the drying temperature if you are working with flammable sample
• For Example, coal requires 300 sec(for others see application notes).
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Working standard (ppm) = Stock solution (ppm) x (Volume of the stock solution (mL)
Total volume (mL).
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Different volumes of same standard solution
Same volume (100 μL) of above 3 solutions in three 100 ml measuring flask gives
Dual-cell:
Tri-cell:
Low range: 0 to 10 ng
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• The instrument is calibrated using aqueous
different matrices .
1,5 mL of liquids
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• Simply sample the gas, through a dedicated
easy to operate.
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• More adsorption tubes can be tied up,
according to requirement.
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• Switch on the DMA-80 System it requires approx. 15 minutes of pre-heating time before run.
• Open the “Methods - parameter”, type a new method name, description and assign the working
parameters of the instrument, such as drying and decomposition time and save the new method
file.
• Open the “DMA-80 Measurement - sample ” click the button to obtain a new empty data file, type
a new data name, number of sample and weight, description and save new data file, Select the
operating mode, either automatic or simple.
• Open the “DMA-80 Calibration”, click the button for provide new empty calibration file, type a new
data name, description and save the new calibration file.
• Return to the “DMA-80 Measurement ”, and load the data file saved. Open “Sample” table of
“Data”. Click “magic wand” button to build a new line, fill the data.
• Open “ Measurement - Result” table and clicking the “Calibration” button appears under State “C”.
Enter with the concentration of your working standard solution.
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• Carry on an blank (several empty boats) measurement to make sure that the system is free
from Hg contaminations, (this cleans the system and the boats).
• Then, follow the calibration procedure that has been described above, running one of the
clean empty boats. In the “Result” table, enter 0.0000 in the “C (μg/Kg)” column and 0.1 g in
the “Weight” column.
• Check calibration of the system measuring a reference sample. At the end also the signal
curve can be tested in the Measurement/Signal menu.
• Add the data necessary for the measurement. Be careful that measurement can be started
only when weight is indicated for all data records.
• Enter the sample weight, put the sample in the Autosampler and start measurement.
• Verify the results, If the samples show heavily different Hg values, it is recommended to carry
out blank measurements after samples with high values.
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• An initial calibration verification standard is checked once per run after calibration.
• An initial calibration verification blank is checked once per run after calibration.
• A matrix spike is analyzed with each sample batch, or one per 20 samples (5%)
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• Control standards for checking the stability of the instrument
±10%.
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• Biological
Blood, urine, hair, tissue, plankton
• Liquids
Waste water, crude oil, heavy oil, detergents, paints
• Solids
Coal, fly ash, soil, sediment, sludge, minerals, food, feed,
plastic, wood, vegetables, leaves, waxes
• Medicinal
Pharmaceuticals, gelatin capsules, lipstick, lotions
• Gas
natural gas, biogas, gases processing, safety and health
occupational hygiene, hazardous waste inspection
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• Clinical, 6 applications . • Pharmaceutical , 11 applications .
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