Escolar Documentos
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SOP
Milestone
March 2009
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SOP for Microwave Digestion
Microwave digestion has been used in this project to quantify total metals in water and sediment
samples. The following procedure is modified from standardized EPA procedures and digestion
procedure was developed after reviewing the ETHOS D labstation Microwave Digestor
Instructions.
Safety measures must be taken when working with digestion procedure, proper laboratory
attire is needed, gloves and goggles. Sample preparation should take place under a laboratory
extraction hood.
Temperature
probe sleeve
Teflon liner
1
Valve
Vessel Vessel
Teflon liner
2
Figure 2. Temperature Probe Sleeve
Figure 4. Vessel Teflon liner, Teflon cap and temperature probe sleeve.
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Figure 5. Ethos D Labstation Microwave digestor.
The vessels are numbered starting at number zero, vessel “zero” will be always used to
monitor the temperature inside of the vessels. To achieve this, the temperature probe sleeve is
introduced through the Teflon cap; the vessel cap used is different from the rest as this will not
have a Teflon valve on the inside. The vessel Teflon liner used to monitor temperature is also
different from the rest as it will have a thicker bottom, of about 1/8 of an inch. The sample used
in this vessel is prepared with the same procedure as the rest of the samples.
When preparing all types of samples the vessels are to be used in an orderly way.
1. Samples will be weighed and prepared inside the vessel Teflon liners (Figure 4).
2. When digesting sediment samples the vessel Teflon liner needs to be weighed in the
balance and the sample poured carefully to avoid exceeding the amount specified (Figure
6).
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Figure 6. Preparation of sediment sample
3. When adding the acids, these have to be slowly poured letting them slide gently on the
4. After preparing samples cover them with parafilm and swirl gently, allow time to
predigest.
5. The vessel Teflon liners are to be introduced inside the vessels then covered with a
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6. After covering the vessel with the Teflon cap, check the valve and Teflon liner are
secured in place, then screw and tighten the vessel cap (Figure 8).
7. When transferring the vessels to the microwave digestor verify first the gas exhaust is
Gas
Exhaust
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8. A carousel comprised of a base and upper support is fixed inside the digestor, take this
carousel out of the digestor and disassemble to arrange the vessels (Figure 10).
9. Vessel “zero” will always be in position number 2, the rest of the vessels need to be
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10. The vessels are then secured with the upper support and the temperature probe is
introduced inside of vessel “zero” through the opening found at the upper part of the
11. The carousel is then introduced and fixed inside the microwave (it might have to be
12. The temperature probe is then connected to the opening found on the left wall inside the
From the options given select Edit (F2), the following options will be displayed:
1. Edit-Program: select program using the F1 and F2 buttons, then press F3 to confirm
the choice.
2. If the program number exists the screen will display “Program # Exist!”, we are then
3. Afterwards, the program requires setting up the time, power, pressure and
4. After selecting all the stages needed, we are able to select the twist option (ON/OFF)
5. The ventilation time is then required. Remember this is related to the amount of
6. After the program is ready the screen sends you to the initial display, this time select
Work a program.
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7. The screen displays the options of starting the program or turning the rotor, before
running the program verify the rotor will work appropriately to avoid further
problems.
8. After verifying the proper performance of the rotor, start the program.
9. After completing digestion, samples are taken out of the microwave digestor and
for further analysis and kept refrigerated at 4°C. Samples duration is six months after
Program Specifications
Temperature 1 Temperature 1
Stage Time (min) Watts
(°C) (°C)
Stage 1 3 600 165 160
Stage 2 5 900 165 160
Stage 3 5 800 165 160
Vent 15 - - -
Sample Amount: 0.5 gr. Of air dried, crushed and homogenized sediment.
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Acid Addition: 9mL Nitric Acid and 3mL Hydrochloric Acid.
Temperature 1 Temperature 1
Stage Time (min) Watts
(°C) (°C)
Stage 1 6 700 175 170
Stage 2 6 900 175 170
Stage 3 6 800 175 170
Vent 25 - - -
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