Digestion Block Application Notes - LabTech

DigiBlock Sample Preparation Systems
APPLICATION NOTES
LABTECH S.r.l.
DigiBlock Application Notes
CONTENT
1 ENVIRONMENTAL ................................................................................................5
1.1 SOIL ...................................................................................................................5
1.2 WASTE WATER ...................................................................................................6
2 FOOD .....................................................................................................................7
2.1 WINE…………………………………………………………………………………7
2.2 RICE ..................................................................................................................8
2.3 FISH ...................................................................................................................8
2.4 MILK ...................................................................................................................9
2.5 RAISIN ..............................................................................................................10
3 AGRICULTRAL....................................................................................................11
3.1 VEGETABLE ......................................................................................................11
3.2 EXTRACTIVE FROM THE LEAF OF GINGKO ............................................................12
3.1 TEA LEAF ..........................................................................................................13
4 CHEMICAL...........................................................................................................15
4.1 COSMETIC …………………………………………………………………………..15
4.2 SILICONE ..........................................................................................................16
5 INDUSTRIAL ........................................................................................................17
5.1 PAINT CHIP .......................................................................................................17
5.2 OIL ...................................................................................................................18
6 GEOLOGICAL .....................................................................................................19
6.1 COAL ASH .........................................................................................................19
7 CLINICAL .............................................................................................................21
7.1 BLOOD .............................................................................................................21
8 ACID SPECIFICATION ........................................................................................23
8.1 EASY SAMPLE ...................................................................................................23
8.2 COMMON SAMPLE .............................................................................................24
8.3 DIFFICULT SAMPLE ............................................................................................24
9 SERVICE ..............................................................................................................25
-3-
NOTE: This procedure is a guideline, developed on a specific

sample. It may need to be modified or changed to obtain the required results
on your sample.
We plan to update DigiBlock application notes periodically. If your interested

samples are not included in this application notes, please send your
application request to our Customer Service Center. We do our best support
you.
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Chapter
1
1 ENVIRONMENTAL
1.1 SOIL
Application field: Soil
Summary
This method provides for the acid digestion of soil sample using hot block digester
for the metal determination of spectroscopic methods.
Equipment
LabTech DigiBlock hot block digester and digestion tube (PTFE)
Reagent
1. HCl: ρ=1.19g/ml, GR
2. HNO3: ρ=1.42g/ml, GR
3. HF: ρ=1.49g/ml
Procedure
4. Add 0.5g sample and 10mL HCI to digestion tube and close the tube.
5. Insert the digestion tube into the cavity of DigiBlock.
6. Setting DigiBlock temperature to 100℃ and run the heating program.
7. Keep 10min at 100℃ after reach 100℃.
8. If the sample do not digest completely. Let the tube cool to room temp. and
add 5mL HNO3 and 5mL HF.
9. Check the DigiBlock temperature is 100℃.
10. Continuously heating 1h and reset DigiBlock temperature to 150℃ and open
the tube
11. Run the heating program till the digestion tube is filled with heavy white smoke.
12. Continuously heating till the solution is approx. 2mL and transparent.
Notes
If the soil sample completely digested, the solution is transparent. Please repeat
above procedure if the sample is not completely digested.
-5-
Appropriate digestion time and acid proportion are both important for good
digestion result due to the organic component are quite various in different soil
samples.
DigiBlock can precisely control the digestion temperature and provide high sample-
to-sample uniformity. It’s a kind of easy and simple way to digest multiple soil
samples.
1.2 WASTE WATER
Application field: Waste water
Summary
This method provides for the acid digestion of waste water sample using hot block
digester for the metal determination of spectroscopic methods.
Equipment
LabTech DigiBlock hot block digester and digestion tube (glass or polypropylene)
Reagent
1. HNO3: ρ=1.42g/ml, GR
2. H2SO4: ρ=1.84g/ml, AR
3. KMnO4: 5%
Procedure
1. Add 20mL sample, 0.5mL HNO3 and 1mL H2SO4 to digestion tube.
2. Add 3mL 5% KMnO4 to digestion tube and let stand for 15min.
3. Add additional 2mL 5% KMnO4 to digestion tube if purple or brown solution
fade.
4. Close the digestion tube and keep a little gap for vent.
5. Insert the digestion tube into DigiìBlock cavity.
7. Continuously heating 2h and keep the solution un-boiling. Acid refluxing and
rinse the wall of tube during the heating program.
8. Let solution cool to room temp. and the solution is ready for analysis.
-6-
Chapter
2
2 FOOD
2.1 WINE
Application field : Determination of metals in wine samples
Summary
This method provide for the acid digestion of wine samples using hot block digester
of wine samples using hot block digester for the metal determination of
spectroscopic methods.
Equipment
Labtech DigiBlock hot block digester and digestion tube (glass/plastic)
Reagent
1. HNO3: ρ=1.42g/ml, GR
2. H2O2: 30%, AR
Procedure
1. Add 5 mL of wine sample and into digestion tube (horniness glass).
2. Add to the digestion tube 3mL HNO3 and 2mL H2O2.
3. Insert the digestion tube into the cavity of DigiBlock.
5. Maintain 15min at 65℃.
6. Setting DigiBlock temperatute to 130℃ then maintain 30min at 130℃.
7. Continuously heating until the solution is transparent and canary.
8. The final solution is clear without color.
Notes
The refluxing in the condenser save a large mount of acid and automatically rinse
the residual on the wall of digestion tube simultaneously. Circling heating brings
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uniformity. Avoid liquid splash and precise control the temperature. It’s a kind of
easy and simple way to digest multiple rice samples.
2.2 RICE
Application field: Rice
Summary
This method provides for the acid digestion of rice sample using hot block digester
Equipment
LabTech DigiBlock hot block digester and digestion tube (glass)
Reagent
1. HNO3: ρ=1.42g/ml, GR
2. HClO4 : ρ=1.68g/ml, GR
Procedure
9. Grind rice sample and pass through 100 screen.
10. Add 1.0g sample and 10mL mixing acids (HNO3:HClO4=4:1) to digestion tube
(horniness glass) and close the tube.
11. Let the sample stand over 12h before insert the digestion tube into the cavity of
DigiBlock.
13. Maintain 15min at 65℃.
14. The tube is filled with red brown color after reach 100℃, then maintain 30min
at 100℃.
16. Reset DigiBlock temperature to 190℃.
17. Open the tube and dry the unwanted acids by heating to 190℃.
18. The final solution is 2mL and clear without color.
Notes
easy and simple way to digest multiple rice samples.
2.3 FISH
Application field: Fish
Summary
This method provides for the acid digestion of fish sample using hot block digester
Equipment
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Reagent
1. HNO3: ρ=1.42g/ml, GR
Procedure
1. Dry the fish sample at 120℃ and grind the sample by agate mortar.
2. Add 0.5g sample and 8mL HNO3 to digestion tube (horniness glass) and close
the tube.
3. Insert the digestion tube into DigiBlock cavity.
4. Setting DigiBlock temperature to 130℃ and run the heating program. Approx.
15min from room temp. to 130℃.
5. After reach 130℃, make the acid refluxing and rinse the wall of tube.
6. Keep 20min refluxing and the solution basically clear.
7. Let the tube cool to room temp. and add 2mL HClO4.
8. Reset DigiBlock temperature to 190℃ and place the tube into unit cavity.
9. Continue heating sample to no white smoke and the solution is 2mL,
transparent and colorless.
Notes
If the fish samples are totally digested, the solution is transparent. If used for
AAS&ICP-AES analysis, please choose appropriate acidity of medium. It’s
available for testing when the medium is diluted to scale.
uniformity. The total procedure is approx. 1 hour by LabTech DigiBlock hot block
digester. It’s a kind of very easy and simple way to digest multiple fish samples
2.4 MILK
Application field: Milk
Summary
This method provides for the acid digestion of milk sample using hot block digester
Equipment
Reagent
1. HNO3: ρ=1.42g/ml, GR
Procedure
1. Add 0.5g sample and 10mL HNO3 to digestion tube and close the tube.
2. Insert the digestion tube into unit cavity.
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4. Acid refluxing and rinse the wall of tube during the heating program.
5. Maintain 60min after reach 120℃ until the solution basically clear.
6. Let the tube cool to room temp. and add 2mL HCIO4. Then insert the digestion
tube into unit cavity.
7. Reset DigiBlock temperature to 190℃ and run the heating program until the
solution no white smoke.
Notes
The grease, which comes from milk digestion, reacts to HCIO4 will bring explosion.
Compare with hotplate beaker digestion, when the residual solution is small, the
sample could not be vaporized to solid phase due to the small bottom of digestion
tube.
Prolong the digestion time at 120℃ will dissolve most part of organic substances.
Then add HCIO4 to avoid explosion.
If using H2SO4 to carbonize the sample, and then add a little of H2SO4 and HCIO4 to
dissolve carbonization substance. The result is also good.
2.5 RAISIN
Application field: Raisin
Summary
This method provides for the acid digestion of raisin sample using hot block
Equipment
Reagent
HNO3: ρ=1.42g/ml, GR
Procedure
1. Add 0.5g sample and 8mL HNO3 to glass digestion tube and close the tube.
4. Acid refluxing and rinse the wall of tube 30min after reach 130℃.
5. Run the heating program until the solution is clear.
Notes
The sample amount, reagent amount, setting temp., etc. are all reference data.
Please adjust the digestion temp., digestion time and acid concentration to
guarantee the best digestion result for specific sample.
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Chapter
3
3AGRICULTURAL
3.1 VEGETABLE
Application field: Vegetable
Summary
This method provides for the acid digestion of vegetable samples using hot block
Equipment
Reagent
1. HNO3: ρ=1.42g/ml, GR
Procedure
1. Take the edible part of fresh vegetable and clean it by tap water and quadric
distilled water successively. Dry the surface of sample and place it in oven for
drying at 100℃. Then grind the sample and place it on desiccator.
2. Add 0.5g sample and 15mL mixing acids (HNO3:HClO4=4:1) to digestion tube
and close the tube.
3. Let the sample stand over 12h before insert the digestion tube into unit cavity.
5. Maintain 10min acid refluxing and rinse the wall of tube.
6. Reset DigiBlock temperature to 100℃ and run the heating program.
7. Keep 30min under 100℃ after the digestion tube is filled with red brown color.
8. If the sample do not digest completely. Let the tube cool to room temp. and
add 5mL mixing acid (HNO3:HClO4=4:1).
10. Let the tube cool to room temp. and add 2mL distilled water.
11. Reset DigiBlock temperature to 190℃and run the heating program till white
smoke appears. The solution is colorless or tiny yellow.
-11-
Notes
uniformity. It’s a kind of easy and simple way to digest multiple vegetable samples.
3.2 EXTRACTIVE FROM THE LEAF OF GINGKO
Application field: Extractive from the Leaf of Gingko
Summary
This method provides for the acid digestion of extractive from the leaf of gingko
using hot block digester for the metal determination of spectroscopic methods.
Equipment
Reagent
HNO3: ρ=1.42g/ml, GR
Procedure
1. Add 0.5g sample and 8mL HNO3 to digestion tube and close the tube.
12~15min from room to setting point.
4. After reach 120℃, make the acid refluxing and rinse the wall of tube.
5. Keep 20min refluxing and the solution basically clear.
6. Continue heating 1.5~2h until the solution changes to canary and transparent.
7. Reset DigiBlock temperature to 160℃ and drive away the acid.
8. Let the digestion tube cool to room temp. Then fix the volume of the sample.
Notes
This method is also available for the digestion of Chinese traditional medicine. The
result will be better if soak the Chinese traditional medicine in nitric acid before
digestion. Digest sample at 95℃ low temperature for testing Hg element. For Pb,
Cd, etc. heavy metal elements, you can increase temperatue and make them
dissolving totally. At the same time, please adjust the proportion of oxidant and add
appropriate H2O2 (30%) and HCIO4 according to sample and interested element.
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3.3 TEA LEAF
Application field: Tea leaf
Summary
This method provides for the acid digestion of tea leaf sample using hot block
Equipment
Reagent
1. HNO3: ρ=1.42g/ml, GR
3. H2O2: 30%, AR
Procedure
4. Grind tea-leaf sample and pass through 120 screen.
5. Add 0.5g sample and 10mL HNO3 to digestion tube (horniness glass) and
close the tube.
6. Place the sample over 12h before insert the digestion tube into unit cavity.
8. Maintain 15min at 65℃ after reach 65℃.
9. Reset DigiBlock temperature to 135℃and maintain 2h at 135℃ after reach 135
℃.
10. Let the tube cool to room temp. if the solution is not clear, add 5mL mixing
acids (HNO3:HClO4=4:1) or H2O2.
11. Continuously heating until the solution is transparent.
13. Open the tube and dry the unwanted acids by heating at 160℃.
14. The final solution is 2mL and clear.
Notes
easy and simple way to digest multiple tea-leaf samples.
-13-
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Chapter
4
4 CHEMICAL
4.1 COSMETIC
Application field: Cosmetic
Summary
This method provides for the acid digestion of cosmetic sample using hot block
Equipment
Reagent
1. HNO3: ρ=1.42g/ml, GR
2. H2SO4 : ρ=1.84g/ml, GR
Procedure
1. Add 1.0g sample into digestion tube and close the tube.
2. Insert the digestion tube into the cavity of EHD36.
3. Setting DigiBlock temperature to 90℃. Run 5-10min to volatilize the organic
solvents.
4. Let the digestion tube cool to room temp. Add 5mL water and 10~15mL HNO3.
Then close the digestion tube.
5. Insert the digestion tube into unit cavity and waiting for several minutes.
6. Continuously heating 5min on 90℃.
7. Let the digestion tube cool to room temp. Add 5mL H2SO4 and insert tube into
unit cavity.
8. Reset the temp. to 350℃ and continuously heating sample till the tube filled
with white smoke.
9. Let the digestion tube cool to room temp. and fix the volume of solution.
Notes
The cosmetic samples ordinarily have organic compounds, such as ethanol and
glycerin. Need to volatilize organic solvents firstly.
-15-
Must adjust an appropriate time for volatilization due to the content of organic
component are different in cosmetic samples. If the cosmetic samples are cream,
please heating the sample by low temp. firstly and melt the sample adhere in the wall
to the bottom of digestion tube.
In addition, please add acid slowly if the cosmetic samples include calcium carbonate,
etc. power. This manipulation can prevent the violent expansion of caused carbon
dioxide gas.
4.2 SILICONE
Application field: Silicone
Summary
This method provides for the acid digestion of silicone sample using hot block
Equipment
LabTech DigiBlock hot block digester and digestion tube (PTFE)
Reagent
1. HF: ρ=1.49g/ml
2. HNO3: ρ=1.42g/ml, GR
Procedure
1. Grind 0.5g of silicone sample.
2. Add silicone sample into PTFE digestion tube
3. At room temperature add 3mL of HF + 3mL HNO3 + 3 mL HClO4
4. Insert the digestion tube into the DigiBlock cavity.
6. Continuously heating for 30 minutes.
7. Reset the temp. to 190℃ and continuously heating until sample is totally
dissolved.
8. Open the tube and dry the unwanted acids
9. The final solution is 2mL and clear.
10. Let the digestion tube cool to room temp. and fix the volume of solution.
Note
The finally solution is turbid maybe due to some inorganic additives in silicone
sample, which available for testing after filtration.
-16-
Chapter
5
5INDUSTRIAL
5.1 PAINT CHIP
Application field: Paint Chip
Summary
This method provides for the acid digestion of paint chip sample using hot block
Equipment
Reagent
1. HNO3: ρ=1.42g/ml, GR
3. H2O2: 30%, AR
Procedure
1. Add 0.5g dried sample and 10mL HNO3 to digestion tube and close the tube.
4. During the heating process, add 1~2mL H2O2 time after time. Finally add 1mL
HClO4 until the sample basically dissolving.
6. Continue heating sample until the solution is small. Then fix the volume of the
sample.
Notes
The finally solution is turbid maybe due to some inorganic additives in paint chip
sample, which available for testing after filtration.
-17-
5.2 OIL
Application field: Oil
Summary
This method provides for the acid digestion of oil sample using hot block digester
Equipment
Reagent
1. HNO3: ρ=1.42g/ml, AR
2. H2SO4 : ρ=1.84g/ml, AR
3. HClO4 : ρ=1.68g/ml, AR
4. H2O2: 30%, AR
Procedure
1. Add 0.5g sample, 10mL mixing acids (HNO3:H2SO4=3:1), and 1.5mL HClO4 to
digestion tube (horniness glass) and close the tube.
2. Let the sample stand over 12h.
3. Add 2 pcs of furbished beading to the digestion tube and insert the digestion
tube into unit cavity.
4. Setting DigiBlock temperature to 50℃ and run the heating program. Slowly
heating the sample and see the bubble boiling.
5. Keep 20min under 50℃. Make sure the bubble boiling is complete and this will
prevent the sample splash from the digestion vessel.
6. Reset DigiBlock temperature to 120℃ and continuously heating 30min.
7. Reset DigiBlock temperature to 145℃ and run the heating program.
8. Let the digestion tube cool to room temp. if the solution darken and unclear.
9. Add 5mL mixing acids (HNO3:HClO4=4:1) or H2O2 to digestion tube.
10. Continuously heating till the solution is transparent.
11. Reset DigiBlock temperature to 150℃ and run the heating program until the
solution is 2mL.
Notes
DigiBlock can precisely control the digestion temperature and provide high sample-
to-sample uniformity. It’s a kind of easy and simple way to digest multiple soil
samples.
-18-
Chapter
6
6 GEOLOGICAL
6.1 COAL ASH
Application field: Coal Ash
Summary
This method provides for the acid digestion of coal ash sample using hot block
Equipment
Reagent
1. HNO3: ρ=1.42g/ml, GR
2. H2SO4 : ρ=1.84g/ml, AR
3. HCI : ρ=1.19g/ml, AR
4. HF: ρ=1.49g/ml
5. H3BO3
Procedure
1. Add 0.5g sample, 10mL mixing acids （HNO3:HCl=1:3）and 4mL HF to

digestion tube and close the tube.
3. Setting DigiBlock temperature to 100℃ and run the heating program for
approx. 120min.
4. Let the tube cool to room temp. and add 2g H3BO3 to it.
-19-
5. Insert the digestion tube into unit cavity and continuously run the heating
program for approx. 10min.
6. The solution is available for analysis after filtration.
-20-
Chapter
7
7 CLINICAL
7.1 BLOOD
Application field: Blood
Summary
This method provides for the acid digestion of blood sample using hot block
Equipment
Reagent
1. HNO3: ρ=1.42g/ml, GR
Procedure
1. Take 20mL sample and place it on 37℃ water bath for 10min.
2. Transfer sample to centrifuge and run 10min under 3000rpm. Collect serum for
following digestion.
3. Add 5mL serum to digestion tube, and add 2mL mixing acids
(HNO3:HClO4=20:1) successively. Shaking the tube slowly when add the acid.
4. Place 10min after insert the digestion tube into unit cavity.
6. After nitric acid break down, reset DigiBlock temperature to 190℃.
7. Continue heating until no white smoke and solution changes to small volume.
8. Add 1mL distilled water and drive away the acid by heating solution.
-21-
9. Turn off the unit and take away the digestion tube.
10. Let the tube cool to room temp. and add distilled water to dissolve residual
substance.
11. Shake up the solution before analysis.
Notes
This method is also available for the digestion of urine sample.
-22-
Chapter
8
8ACID SPECIFICATION
The sample amount, 8.1 EASY SAMPLE

reagent amount, setting
temp., etc. are all
reference data. Please
adjust the digestion Sample
Drinking-water, waste water, etc.
temp., digestion time and Type
acid concentration to Sample
guarantee the best Solid sample ＜2g and liquid sample is 20mL
digestion result due to Amount
the diversity of sample. Reagent
8-10mL
Amount
Acid HCl HNO3 HCl+HNO3
Strong non-oxidizing Strong oxidizing Extremely strong
Acid Type
mineral acid mineral acid oxidizing mineral acid
Digestion
65-95℃ 65-95℃ 65-95℃
Temp.
Setting
70-100℃ 70-100℃ 70-100℃
Temp.
Available
Glass and Glass and Glass and
Digestion
Polypropylene Polypropylene Polypropylene
Vessel
Available
All DigiBlock models All DigiBlock models All DigiBlock models
Digester
Note Especially suitable for Hg determination
-23-
8.2 COMMON SAMPLE
Sample Type Vegetable, soil, food, etc.

Sample
＜2g
Amount
Reagent
8-10mL
Amount
Acid HCl HNO3 HCl+HNO3
Extremely strong
Strong non-oxidizing Strong oxidizing
Acid Type oxidizing mineral
mineral acid mineral acid
acid
Digestion
＜80℃ 80-120℃ 95-110℃
Temp.
Setting Temp. 90-95℃ 90-130℃ 100-120℃
Available
Glass, Polypropylene
Digestion Glass Glass
and PTFE
Vessel
Available
All DigiBlock models All DigiBlock models All DigiBlock models
Digester
If the sample is not digested completely, please let the vessel cool to
Note
room temp. and add H2O2, then repeat former steps.
8.3 DIFFICULT SAMPLE
Sample
Feed, oil, polymer and component unknown sample
Type
Sample
＜2g
Amount
Reagent
10mL
Amount
Acid HCl HNO3 HCl+HNO3 H2SO4 HF H2SO4+ HNO3 HNO3+HClO4
Strong non-
Strong Extremely Strong
Strong oxidizing
non- strong oxidized Charring
Acid oxidizing mineral acid Extremely
oxidizing oxidizing and firstly, and
Type mineral ideal for strong acid
mineral mineral dehydrated then digestion
acid samples
acid acid acid
such as SiO2
Add H2SO4 at
Digestion 220°C firstly,
＜80°C 80-120°C 95-110°C 230°C ＜95°C 145-200°C
Temp. and then 80-
120°C
260°Cfirstly
Setting
90-95°C 90-130°C 100-120°C 260-400°C ＜110°C and then 90- 160-210°C
Temp.
130°C
Available Glass
Digestion and Glass Glass Glass PTFE Glass Glass
Vessel PTFE
Available All All
All Models EHD36 All Models EHD36 All Models
Digester Models Models
The dosage of acid is quite big during high temp. digestion. Please add acid according to specific
Note sample. If the sample is not digested completely, please add acid to dissolve the sample time after
time.
-24-
Chapter
9
9 SERVICE
The LABTECH worldwide technical support network consists of highly trained Field
Service Engineers, Technical Support Specialists and Service Coordinators who
are ready to quickly assist customers with answers and solutions to service needs
and application questions.
If you need any help, please feel free to tell LABTECH, and we will do our
best to support you.
LABTECH Srl
Via Fatebenefratelli 1/5
24010 Sorisole (BG)
Italy
Tel : +39 035 576614

Fax : +39 035 4729414
E-mail: [email protected]
www.labtechsrl.com
-25-

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DigiBlock Sample Preparation Systems

NOTE: This procedure is a guideline, developed on a specific

We plan to update DigiBlock application notes periodically. If your interested

Application field: Soil

1.2 WASTE WATER

Application field: Waste water

Application field : Determination of metals in wine samples

Application field: Rice

Application field: Fish

LabTech DigiBlock hot block digester and digestion tube (glass)

Application field: Milk

Application field: Raisin

Application field: Vegetable

3.2 EXTRACTIVE FROM THE LEAF OF GINGKO

Application field: Extractive from the Leaf of Gingko

3.3 TEA LEAF

Application field: Tea leaf

Application field: Cosmetic

Application field: Silicone

5.1 PAINT CHIP

Application field: Paint Chip

Application field: Oil

6.1 COAL ASH

Application field: Coal Ash

LabTech DigiBlock hot block digester and digestion tube (glass)

1. Add 0.5g sample, 10mL mixing acids （HNO3:HCl=1:3）and 4mL HF to

Application field: Blood

LabTech DigiBlock hot block digester and digestion tube (glass)

This method is also available for the digestion of urine sample.

The sample amount, 8.1 EASY SAMPLE

8.2 COMMON SAMPLE

Sample Type Vegetable, soil, food, etc.

8.3 DIFFICULT SAMPLE

Tel : +39 035 576614

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