UltraWAVE Application Guidelines

ULTRAWAVE
APPLICATION
BOOK
Application guidelines for

your UltraWAVE
Milestone Srl UltraWAVE – Application book
Milestone Srl
Via Fatebenefratelli, 1/5
24010 Sorisole (BG) Italy
Tel +39 035 573857 – Fax +39 035 575498
www.milestonesrl.com
THE ULTRAWAVE APPLICATION BOOK

1- Introduction and Applications for UltraWAVE ECR
MICROWAVE PROGRAM GUIDELINES

2- Sample weight
3- Acid mixture
4- Microwave program
GENERAL DIGESTION METHODS

5- General Digestion method for Food samples
6- General digestion method of Environmental samples
7- General digestion method for Polymers samples
8- General digestion method for Petrochemicals samples
9- General digestion method for Pharmaceutical samples
10- General digestion method for Biological samples
LIST OF TESTED SAMPLES IN MILESTONE ANALYTICAL LAB
APPLICATIONS FOR ALL ULTRAWAVE VERSIONS
UW-01 Mineral Oil

UW-02 Polyethylene loaded with Si (Total recover of Si)
UW-03 Terephtalic acid (PTA)
1
Milestone Srl UltraWAVE – Application book
UW-04 Toys samples (Paper and polymer)

UW-05 Boron Carbide
UW-06 Silicon Carbide
UW-07 Water based markers (Ink)
UW-08 EPA 3051 General digestion method for Soil
UW-09 EPA 3052 General digestion method of soil with Si
UW-10 SRM samples B5-B6 (Lake Sediment)
UW-11 Carbon Fibre
UW-12 Silica Sand
UW-13 Coal
UW-14 Textile sample (Cotton)
UW-15 SRM Sample NIST 1575 (Pine Needles)
UW-16 SRM Sample USGS G-2 (Granite)
UW-17 SRM Sample USGS BCR-2 (Basalt)
UW-18 SRM Sample NIST 2702 (Marine sediment)
UW-19 SRM sample NIST 2711 (Montana soil)
UW-20 SRM Sample NIST 2709a (San Joaquim soil)
UW-21 Fly ash
UW-22 Aluminium Titanate (Al2TiO5)
UW-23 High amount of Vegetable oil
UW-24 Sulphur
UW-25 Titanium Oxide (TiO2)
APPLICATIONS ONLY FOR ULTRAWAVE ECR VERSION
UW-ECR-01 Alumina
UW-ECR-02 Ferberite (Iron Wolframite mineral, FeWO4)
UW-ECR-03 Inorganic Fertilizers
UW-ECR-04 Manganese doped Zirconia
UW-ECR-05 Nickel-Chromium (NiCr)
UW-ECR-06 Calcium Tungstate Mineral, CaWO4 (Scheelite)
UW-ECR-07 Tantalite
UW-ECR-08 Iron Manganese Tungstate Mineral, FeMnO4 (Wolframite)
UW-ECR-09 Yttria Zirconia
UW-ECR-10 Zirconia with Rare Earth Oxide
UW-ECR-11 Zirconium Oxide or Zirconium Hydroxide
UW-ECR-12 Platinum and Rhodium Alloy
UW-ECR-13 Carbon Black with high Si content
2
Milestone Srl UltraaWAVE – Appliccation book
Milestone Srl
Via Fatebennefratelli, 1/5
24010 Sorissole (BG) Italy
Tel +3
39 035 5738557 – Fax +39 035 575498
www.mileestonesrl.com
THE ULTTRAWAVVE APPLICATIO

ON BOO
OK
Introducttion
The purpoose of the application

a book is too support you,
y in ordeer to find thhe proper method
m forr
your samples.
s
The lissted appliccation notees are a goood point too start wheen developping a new
w
methood for yourr samples.. These guuidelines are a the moost relevant methodss
develooped by Milestone Laaboratoriess, based onn real sam mples from Milestonee
worldwwide users.
Anywaay pleasee consider that some applications might neeed somee

modifiications, in order to fi t with yourr specific sample.
Applicatioons for UlttraWAVE ECR

E
The Appliccation book is divideed into twoo parts, whhere the seecond part is only deedicated too
UltraWAVEE systems with
w ECR (EEnhanced CChemical Resistance)
R ) kit.
The ECR vversion consists of pressure

p linnes made of a speciial alloy haaving an outstanding
o g
chemical rresistance to a broad range of ccorrosive media,
m suchh as:
• Applications that reqquire moree than 15 mL of hyddrochloric aacid, consiidering thee

complete rack (i.e. more
m than 1 mL in eaach 15-possitions rackk or 3 mL in each 5--
positions rack,
r etc…
…)
• Routine appplications with high volume of hydrochlorric acid.
• Applications that reqquire the usse of aqua regia (3:1 HCl:HNO3))
Alll UltraWAV
VE system
ms can be upgraded with the EECR kit
Alll applications in thee first partt of this ap

pplication book are of course
suuitable forr UltraWAVVE ECR as well.
3
M
MICROW
WAVE PPROGRA
AM GUID
DELINESS
UltraWAVEE allows tto digest a wide rrange of samples such s as eenvironmenntal, food,,
pharmaceutical, pettrochemicaal, polymerr, metals, ggeologicals, etc.
This guiddelines, willl help you to find the suitable microwavee digestionn
f all your samples.
method for
These aree only guiddelines, in case you need
n furtheer informatiion, pleasee
contact your
y local M Milestone distributor
d
Sample wweight
Sample wweight is an important parameterr especiallyy for digesttion of Orgaanic samplles.
Here below
w are somee guidelinees based onn sample tyypes.
Samples rreactivity Samp

ples type 15 positions
p ra
ack 5 positions rack
Soils, aqueeous solution s,

Not reaactive
environmeental sampless, Up to 1 g Up to 3 g
sampples
fertilizerss, feed, etc..
Food (fattty samples),

Samplees with
pharma, ingredients, Up to 0,5 g Up to 1,,5 g
medium rreactivity
feed
f
Highly reeactive Polymer, petrochemicaal,

Up to 0,3 g Up to 0,,8 g
sampples oils, solvents
s
Acid mixttures
The choosse of the acid
a mixtuure is a cruucial part of sample preparatioon especiaally for thee
inorganic samples.
w some inddications about acids , based on sample types.
Here below
Sam
mples Type Reag
gents
Orgaanic samplee HNO3, H2O2
Organic sam
mple with Silicates
S HNO3, H2O2,
H HF
4
HNO33, HCl.
Mettal samples (Aqua regiaa or reverse aquaregia.
a Inn some casess
HF is neecessary for a complete ddigestion)
HNO3, HF, H2SO4, etc...
Inorganic samplees (See the appplication bookk or contact the Milestonne
application
n specialist)
Saamples mu
ust be com
mpletely wet
w by the acid mixtuure.
Digestionn program
Most of thhe samples can be used simultaaneously wiith a standaard microw
wave prograam:
Steep 1 20 min 240°C
Steep 2 10 min 240°C
In some ccases, due to the reacctivity of thhe sampless or to the high tempperature reqquired, thee
microwavee program should bee slightly m modified. Below
B is reeported a ttable that gives
g clearr
indicationss of the appproach too be used for the diffferent sam mples. The table considers twoo
main paraameters:
- Reaactivity of the
t samplee
- Tarrget tempeerature
Samples rreactivity Samp ples type Targeet temperatu

ure Staandard ramping time
Soils, aqueeous solutionns, 10 min up too 180°C
Not reaactive
environmeental sampless, 180-220°C
1 or
sampples
fertilizerss, feed, etc.. 15 min up too 220°C
Food (fattty samples), 20 min up too 220°C
Samplees with
pharma ingredients, 200-240°C
2 or
medium rreactivity
feed
f 25 min up too 240°C
5 min to 100°C
Polymer, petrochemica
p al,
Highly rreactive 15 min to 180°C
1
large amoount of food,, 220-250°C
2
sampples 10 min to 220°C*
2
oils, solvents
*deppending on the
t target T
25 min up too 250°C
Geologiccal, metals,
High temperature 250-270°C
2 Or
ceramicss, inorganics
30 min up too 270°C
5

Application Note
General digestion method for food samples

Summary
With Oil or high fat samples, reduce the amount to
This method provides the acid digestion of the sample 1 g in the 5 positions rack and 0,3 g in the 15
in a Single Reactor Chamber (SRC) using temperature positions rack.
control and microwave heating for the metal
determination by spectroscopic methods. This method
is suitable for samples like: Infant formula, Milk
powder, Meat, vegetables, rice, etc…
Start Pressure
40 bar of Nitrogen
Instrumentation
Milestone UltraWAVE with internal temperature and
Procedure
pressure control in all vessels, 640 or 660 terminal 1. Switch ON the chiller
with easyCONTROL software installed. 2. Place the main TFM vessel with the basic load, into
the UltraWAVE chamber.
Nitrogen tank 3. Position the rack into the UltraWAVE
4. Close the UltraWAVE chamber trough the software
Basic Load 5. Tight the clamps
6. Run the microwave program.
Place the following basic load into the main 1 L 7. Wait the cooling and the pressure release
TFM vessel: 130 ml of H2O, 5 ml of HNO3 67% 8. Untight the clamps and open the main chamber.
9. Collect the solutions in a marked flask and dilute it.
Sample amount and Reagent
Microwave program
Add 2 - 3 drops of pure water into the empty vials
before weight, this will help to completely wet the Step Time T1 T2 P Power
powder sample. 1 00:20:00 220°C 60°C 110 1500W
2 00:10:00 220°C 60°C 110 1500W
Notes
*Milestone suggest Glass or Quartz vials.
THE CLEANING /MAINTENANCE PROCEDURE MUST

BE EXECUTED FOLLOWING THE USER MANUAL AND
INSTALLER INSTRUCTIONS.
Rack type Sample Amount Reagents
5 positions* 2g 10 ml of HNO3
This procedure is only a guideline and it may need to be modified
15 positions* 0,5 g 5 ml of HNO3 or changed to obtain the required results on your sample.
Milestone Srl – Helping Chemists www.milestonesrl.com application@milestonesrl.com

Application Note
General digestion method for environmental samples

Summary Start Pressure
This method provides the acid digestion of the sample 40 bar of Nitrogen
in a Single Reactor Chamber (SRC) using temperature
control and microwave heating for the metal Procedure
1. Switch ON the chiller
is suitable for samples like: Soils, Plant materials,
2. Place the main TFM vessel with the basic load, into
Waste water, etc… the UltraWAVE chamber.
3. Position the rack into the UltraWAVE
Instrumentation 4. Close the UltraWAVE chamber trough the software
5. Tight the clamps
Milestone UltraWAVE with internal temperature and 6. Run the microwave program.
pressure control in all vessels, 640 or 660 terminal 7. Wait the cooling and the pressure release
with easyCONTROL software installed. 8. Untight the clamps and open the main chamber.
Nitrogen tank
Microwave program
Basic Load
Step Time T1 T2 P Power
Place the following basic load into the main 1 L
1 00:15:00 220°C 60°C 110 1500W
TFM vessel: 130 ml of H2O, 5 ml of HNO3 67%
2 00:10:00 220°C 60°C 110 1500W
Sample amount and Reagent Notes
Rack type Sample Amount Reagents *Milestone suggest Glass or Quartz vials.
5 positions* 2g 10 ml of HNO3 THE CLEANING /MAINTENANCE PROCEDURE

MUST BE EXECUTED FOLLOWING THE USER
15 positions* 0,5 g 5 ml of HNO3
MANUAL AND INSTALLER INSTRUCTIONS.
In case of “foaming” of samples: This procedure is only a guideline and it may need to be modified
or changed to obtain the required results on your sample.
- ‘Pre-wet’ these samples with 1ml H2O in
these vials, then add the acids for your
digestions
- Add acid drop-by-drop
- Wait for the exothermic reaction to subside

to down
- Use Vortex system, before the digestion

run.

Application Note
General digestion method for polymers

Summary 5. Tight the clamps
This method provides the acid digestion of the sample 7. Wait the cooling and the pressure release
in a Single Reactor Chamber (SRC) using temperature 8. Untight the clamps and open the main chamber.
control and microwave heating for the metal 9. Collect the solutions in a marked flask and dilute it.
Microwave program
is suitable for samples like: Polyethylene, Polyester,
Polypropylene, etc... Step Time T1 T2 P Power
1 00:10:00 110°C 60°C 90 1500W
Instrumentation
2 00:15:00 180°C 60°C 90 1500W
Milestone UltraWAVE with internal temperature and 3 00:10:00 230°C 60°C 120 1500W
pressure control in all vessels, 640 or 660 terminal 4 00:05:00 230°C 60°C 120 1500W
with easyCONTROL software installed.
Nitrogen tank
Note
Basic Load
Milestone suggest to use glass or quartz vials
In case of high NOx production, it’s suggested
to use the High temperature PTFE disc (p/n
Sample amount and Reagent MCL0699A). See user manual for more details
or contact the Milestone specialist
8ml of HNO3, BE EXECUTED FOLLOWING THE USER MANUAL AND
5 positions Up to 600 mg*
1ml H2O de. INSTALLER INSTRUCTIONS.
4ml of HNO3,
1ml H2O de.
Pressure loading
40 bar of Nitrogen
Procedure

Application Note
General digestion method for petrochemical products

Summary Pressure loading
determination by spectroscopic methods. This method 1. Switch ON the chiller
is suitable for samples like: Fuel oil, heavy oil, Crude 2. Place the main TFM vessel with the basic load, into
oil, etc… the UltraWAVE chamber.
Instrumentation 4. Close the UltraWAVE chamber trough the software
5. Tight the clamps
Milestone UltraWAVE with internal temperature and 6. Run the microwave program.
pressure control in all vessels, 640 or 660 terminal 7. Wait the cooling and the pressure release
with easyCONTROL software installed. 8. Untight the clamps and open the main chamber.
Nitrogen tank
Microwave program
Basic Load
Place the following basic load into the main 1 L 1 00:10:00 110°C 60°C 90 1500W
TFM vessel: 150 ml of H2O, 5 ml of HNO3 65% 2 00:15:00 180°C 60°C 90 1500W
3 00:10:00 230°C 60°C 120 1500W
4 00:05:00 230°C 60°C 120 1500W
8ml of HNO3,
1ml H2O de. Note
5ml of HNO3, Milestone suggest to use glass or quartz vials
1ml H2O de.
In case of high NOx generation, it’s suggested
to use the High temperature PTFA disc (p/n
*For solvent samples (i.e. Naphtha) reduce MCL0699A). See user manual for more details
the sample amount to 300 mg in 5 positions or contact the Milestone specialist
rack and 150 mg in 15 positions rack
MILESTONE SUGGEST TO USE GLASS OR BE EXECUTED FOLLOWING THE USER MANUAL AND
QUARTZ VIALS. INSTALLER INSTRUCTIONS.


Application Note

General digestion method for pharmaceutical samples

Summary Pressure loading
Procedure
determination by spectroscopic methods. 1. Switch ON the chiller
Instrumentation the UltraWAVE chamber.
Milestone UltraWAVE with internal temperature and 4. Close the UltraWAVE chamber trough the software
pressure control in all vessels, 640 or 660 terminal 5. Tight the clamps
with easyCONTROL software installed. 6. Run the microwave program.
7. Wait the cooling and the pressure release
Nitrogen tank 8. Untight the clamps and open the main chamber.
Basic Load
Microwave program
TFM vessel: 130 ml of H2O, 5 ml of HNO3 65% Step Time T1 T2 P Power
1 00:20:00 240°C 60°C 110 1500W
2 00:10:00 240°C 60°C 110 1500W
5 positions Up to 800 mg* 8ml of HNO3

Note
15 positions Up to 500 mg* 5ml of HNO3
Milestone suggest to use glass or quartz vials



Application Note

General method for biological samples

Summary 7. Wait the cooling and the pressure release
8. Untight the clamps and open the main chamber.
This method provides the acid digestion of the sample 9. Collect the solutions in a marked flask and dilute it.
Microwave program
is suitable for samples like: Blood, human or animal
1 00:15:00 220°C 60°C 110 1500W
tissue, hairs, etc…
2 00:10:00 220°C 60°C 110 1500W
Instrumentation
Milestone UltraWAVE with internal temperature and Note
pressure control in all vessels, 640 or 660 terminal
with easyCONTROL software installed. *Milestone suggest Glass or quartz vials.
Nitrogen tank THE CLEANING /MAINTENANCE PROCEDURE MUST

Basic Load INSTALLER INSTRUCTIONS.

TFM vessel: 130 ml of H2O, 5 ml of HNO3 67%. This procedure is only a guideline and it may need to be modified
Sample amounts refers to dry matter
Pressure loading
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note

Mineral Oil

Summary 6. Run the microwave program.
This method provides the acid digestion of the sample 8. Untight the clamps and open the main chamber.
in a Single Reactor Chamber (SRC) using temperature 9. Collect the solutions in a marked flask and dilute it.
determination by spectroscopic methods.
Microwave program

Instrumentation
1 00:10:00 120°C 60°C 110 1500W
3 00:20:00 220°C 60°C 130 1500W
4 00:10:00 220°C 60°C 130 1500W
Nitrogen tank
Basic Load *Milestone suggest Quartz or Glass vials
Place the following basic load into the main 1 L THE CLEANING /MAINTENANCE PROCEDURE MUST
TFM vessel: 150 ml of H2O, 5 ml of HNO3 65%. BE EXECUTED FOLLOWING THE USER MANUAL AND
4 ml of HNO3,
15 positions* 0,2 g
2ml H2O
Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps


Application Note

Polyethylene loaded with Si (Total Si recovery)

Microwave program
determination by spectroscopic methods. Step Time T1 T2 P Power
1 00:25:00 220°C 60°C 110 bar 1500W
Instrumentation
2 00:10:00 220°C 60°C 110 bar 1500W
with easyCONTROL software installed. Note
Nitrogen tank *Milestone suggest PTFE vials.
Basic Load Use the PTFE protection for thermowell (P/N

MCL0664A)
TFM vessel: 150 ml of H2O, 5 ml of HNO3 65% THE CLEANING /MAINTENANCE PROCEDURE MUST
Sample amount and Reagent INSTALLER INSTRUCTIONS.

4 ml of HNO3 + 4 or changed to obtain the required results on your sample.
15 positions* 100 mg
ml of HF
Pressure loading
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note
Terephtalic acid (PTA)

Summary Procedure
This method provides the acid digestion of the sample 1. Switch ON the chiller
in a Single Reactor Chamber (SRC) using temperature 2. Place the main TFM vessel with the basic load, into
determination by spectroscopic methods. 4. Close the UltraWAVE chamber trough the software
5. Tight the clamps
Instrumentation 6. Run the microwave program.
Milestone UltraWAVE with internal temperature and 8. Untight the clamps and open the main chamber.
pressure control in all vessels, 640 or 660 terminal 9. Collect the solutions in a marked flask and dilute it.
Microwave program
Nitrogen tank
Basic Load
1 00:10:00 150°C 60°C 90 1500W
Place the following basic load into the main 1 L 2 00:05:00 150°C 60°C 90 1500W
TFM vessel: 130 ml of H2O, 5 ml of HNO3 3 00:10:00 250°C 60°C 120 1500W
4 00:10:00 250°C 60°C 120 1500W

Note
15 positions* 500 mg 8 ml of HNO3
*Milestone suggest glass or quartz vials.

Pressure loading INSTALLER INSTRUCTIONS.
40 bar of Nitrogen

Application Note

Toys samples (Paper and polymer)

Microwave program
determination by spectroscopic methods. Step Time T1 T2 P Power
1 00:10:00 110°C 60°C 90 1500W
Instrumentation
2 00:10:00 180°C 60°C 90 1500W
Nitrogen tank
Note
Basic Load
Milestone suggest to use glass or quartz
Place the following basic load into the main 1 L vials. Use PTFE vials with HF.
In case of high NOx generation, it’s suggested
Sample amount and Reagent to use the High temperature PTFE disc (p/n
MCL0699A). See user manual for more details
Rack type Sample Amount Reagents or contact the Milestone specialist
8ml of HNO3, THE CLEANING /MAINTENANCE PROCEDURE MUST
(1mL of HF) BE EXECUTED FOLLOWING THE USER MANUAL AND
5ml of HNO3,
(1mL of HF)
In case of Si presence, add 1 mL of HF

Pressure loading
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note

Boron Carbide

Summary
Microwave program
Instrumentation
Nitrogen tank
*Milestone suggest PTFE vials
Basic Load Use the PTFE (MCL0699A) discs for high

temperature applications
TFM vessel: 130 ml of H2O, 5 ml of HNO3 65%. THE CLEANING /MAINTENANCE PROCEDURE MUST

3 ml of HNO3, or changed to obtain the required results on your sample.
5 or 8 positions* 50 mg 1 ml HF,
1 ml H2SO4
Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps


Application Note

Silicon Carbide

Summary
Microwave program
Instrumentation
Nitrogen tank

TFM vessel: 130 ml of H2O, 5 ml of HNO3 65%. Use the PTFE protection for thermowell (P/N
MCL0664A)
Rack type Sample Amount Reagents INSTALLER INSTRUCTIONS.
3 ml of HNO3,
5 positions* 50 mg 3 ml HF,
6 ml H2SO4
Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps


Application Note

Water based marker (Ink)

Summary Microwave program
This method provides the acid digestion of the sample Step Time T1 T2 P Power
in a Single Reactor Chamber (SRC) using temperature 1 00:20:00 250°C 60°C 110 1500W
control and microwave heating for the metal 2 00:10:00 250°C 60°C 110 1500W
Instrumentation
Note
*Milestone suggest glass or quartz vials.
with easyCONTROL software installed. THE CLEANING /MAINTENANCE PROCEDURE MUST
Nitrogen tank INSTALLER INSTRUCTIONS.
Basic Load
Place the following basic load into the main 1 L or changed to obtain the required results on your sample.

4 ml of HNO3,
15 positions* 0,25 g
1 ml of H2O
Pressure loading
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note

EPA 3051 General digestion method of soil samples

Instrumentation
Note
*Milestone suggest Glass or quartz vials.
Basic Load
Place the following basic load into the main 1 L This procedure is only a guideline and it may need to be modified
TFM vessel: 130 ml of H2O, 5 ml of HNO3 67% or changed to obtain the required results on your sample.

15 positions* 0,5 g 10 mL of HNO3*
Pressure loading
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note

EPA 3052 Siliceous based compound

2 00:10:00 180°C 70°C 120 1200W
Instrumentation
Note
*Milestone suggest TFM vials for application with
HF.
Nitrogen tank BE EXECUTED FOLLOWING THE USER MANUAL AND
Basic Load
TFM vessel: 130 ml of H2O, 5 ml of HNO3 67% This procedure is only a guideline and it may need to be modified
4 ml of HNO3, 2
15 positions* 0,5 g
ml of HF
Pressure loading
40 bar of Nitrogen
Procedure
5. Tight the clamps
8. Un-tight the clamps and open the main chamber.

Application Note

SRM samples B5-B6 (Lake Sediment)

Summary 8. Un-tight the clamps and open the main chamber.
This method provides the acid digestion of the sample
in a Single Reactor Chamber (SRC) using temperature Microwave program
1 00:25:00 260°C 60°C 110 1200W
Instrumentation 2 00:15:00 260°C 60°C 110 1200W

Note
*Milestone suggest TFM vials for application with
Nitrogen tank HF.

TFM vessel: 130 ml of H2O, 5 ml of HNO3 67% THE CLEANING /MAINTENANCE PROCEDURE MUST
4 ml of HNO3, This procedure is only a guideline and it may need to be modified

2 ml of H3PO4, or changed to obtain the required results on your sample.
15 positions* 50 mg
2 ml of HBF4,
1 ml of H2SO4
Pressure loading
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note

Carbon Fibre
Instrumentation *Milestone suggest Quartz or glass vials
Milestone UltraWAVE with internal temperature and Use the PTFE (MCL0699A) discs for high
pressure control in all vessels, 640 or 660 terminal temperature applications
Basic Load
TFM vessel: 130 ml of H2O, 5 ml of HNO3 65%. or changed to obtain the required results on your sample.
15 positions* 100 mg 4 ml of HNO3
Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note

Silica Sand
Summary
1 00:15:00 240°C 60°C 110 1500W

pressure control in all vessels, 640 or 660 terminal *Milestone suggest PTFE vials
Use the PTFE protection for thermowell (P/N
Nitrogen tank MCL0664A)
Basic Load THE CLEANING /MAINTENANCE PROCEDURE MUST

Place the following basic load into the main 1 L INSTALLER INSTRUCTIONS.
TFM vessel: 130 ml of H2O, 5 ml of HNO3 65%.
Sample amount and Reagent This procedure is only a guideline and it may need to be modified
1 ml of HNO3,
15 positions* 100 mg
4 ml of HF
Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note
Coal
Instrumentation
Milestone UltraWAVE with internal temperature and 3. Position the rack into the UltraWAVE
Basic Load
Microwave program
1 00:20:00 240°C 60°C 110 1500W
2 00:10:00 240°C 60°C 110 1500W
Add 2 - 3 drops of pure water into the empty vials Notes
before weight, this will help to completely wet the
powder sample. * Milestone suggest Glass or quartz vials. If HF is
required, use TFM vials.
In case of big amount of NOx, it’s suggested to

use the High temperature PTFE disc (p/n
MCL0699A). See user manual for more details or
contact the Milestone specialist

Rack type Sample Amount Reagents INSTALLER INSTRUCTIONS.
5 ml of HNO3
15 positions* 0,5 g
(1 ml of HF)
In case of Si presence, add the HF. or changed to obtain the required results on your sample.

Application Note
Textile sample (Cotton)

Summary 9. Collect the solutions in a marked flask and dilute it.
This method provides the acid digestion of the sample Microwave program
1 00:15:00 220°C 60°C 110 1500W
2 00:15:00 220°C 60°C 110 1500W
Instrumentation
Notes
Milestone UltraWAVE with internal temperature and * Milestone suggest Glass or quartz vials.
Basic Load

5 positions* 1g 10 ml of HNO3
Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note
SRM Sample NIST 1575 (Pine Needles)

Summary 9. Collect the solutions in a marked flask and dilute it.
This method provides the acid digestion of the sample Microwave program
determination by spectroscopic methods. 1 00:15:00 230°C 60°C 110 1500W
2 00:10:00 230°C 60°C 110 1500W
Instrumentation Notes
Milestone UltraWAVE with internal temperature and * Milestone suggest Glass or quartz vials.
Basic Load

Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note
SRM sample USGS G-2 (Granite)

Summary 8. Untight the clamps and open the main chamber
1 00:20:00 260°C 60°C 110 1500W
Milestone UltraWAVE with internal temperature and Notes

pressure control in all vessels, 640 or 660 terminal * Milestone suggest PTFE vials.
Use the PTFE (MCL0699A) discs for high
Nitrogen tank temperature applications

2 ml of HNO3,
1 ml of HCl,
15 positions* 50 mg
2 ml of H3PO4,
2 ml of HBF4
Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note
SRM sample USGS BCR-2 (Basalt)

1 00:20:00 260°C 60°C 110 1500W


2 ml of HNO3,
1 ml of HCl,
15 positions* 50 mg
2 ml of H3PO4,
2 ml of HBF4
Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note
SRM sample NIST 2702 (Marine sediment)

1 00:20:00 260°C 60°C 110 1500W


3 ml of HNO3,
15 positions* 50 mg
2 ml of HBF4
Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note
SRM sample NIST 2711 (Montana soil)

1 00:20:00 260°C 60°C 110 1500W


3 ml of HNO3,
15 positions* 50 mg 2 ml of HBF4,
1 ml of HCl
Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note
SRM sample NIST 2709a (San Joaquin soil)

1 00:20:00 260°C 60°C 110 1500W


3 ml of HNO3,
15 positions* 50 mg 2 ml of HBF4,
1 ml of HCl
Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps

Application Note
Fly Ash
Instrumentation
Basic Load
Microwave program
1 00:25:00 250°C 60°C 110 1500W
2 00:10:00 250°C 60°C 110 1500W
powder sample. * Milestone suggest Glass or quartz vials. If HF is
required, use TFM vials.


0,4g H3BO3
15 positions* 0,5 g powder, 4 ml
HNO3, 2ml HF
Add the reagents sequentially, in the order how they are

written.

Application Note

Aluminium Titanate
(Al2TiO5)

Microwave program

Instrumentation
1 00:30:00 280°C 60°C 110 1500W
Nitrogen tank
Basic Load temperature applications
Place the following basic load into the main 1 L Use the PTFE protection for thermowell (P/N
TFM vessel: 130 ml of H2O, 5 ml of HNO3 65%. MCL0664A)

Sample amount and Reagent BE EXECUTED FOLLOWING THE USER MANUAL AND
5 ml HF, This procedure is only a guideline and it may need to be modified

5 positions* 50 mg
6 ml H3PO4
Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps


Application Note

High amount of Vegetable

oil

Microwave program

Instrumentation
1 00:10:00 120°C 60°C 110 1500W
3 00:08:00 160°C 60°C 150 1500W
4 00:05:00 160°C 60°C 150 1500W
Nitrogen tank 5 00:10:00 250°C 60°C 150 1500W
6 00:10:00 250°C 60°C 150 1500W
Basic Load
*Milestone suggest Quartz or Glass vials
TFM vessel: 170 ml of H2O, 5 ml of HNO3 65%.
Sample amount and Reagent BE EXECUTED FOLLOWING THE USER MANUAL AND
6 ml of HNO3, This procedure is only a guideline and it may need to be modified

5 positions* 1g
3 ml H2O or changed to obtain the required results on your sample.
Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps


Application Note
Sulphur
Instrumentation
Basic Load
Microwave program
1 00:20:00 250°C 60°C 130 1500W
2 00:10:00 250°C 60°C 130 1500W
powder sample. * Milestone suggest Glass or quartz vials.


4 ml of HNO3
15 positions* 0,2 g
1 ml of H2O

Application Note
Titanium Oxide (TiO2)

Notes
Instrumentation *Milestone suggest PTFE vials
Milestone UltraWAVE with internal temperature and Use the PTFE (MCL0699A) discs for high
pressure control in all vessels, 640 or 660 terminal temperature applications
Basic Load
TFM vessel: 130 ml of H2O, 5 ml of HNO3 67% or changed to obtain the required results on your sample.

4 ml of HNO3
15 positions* 0,1 g
1 ml of HF
Start Pressure
40 bar of Nitrogen
Procedure
5. Tight the clamps

UltraWAVE Application Guidelines

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UltraWAVE Application Guidelines

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ULTRAWAVE

Application guidelines for

THE ULTRAWAVE APPLICATION BOOK

MICROWAVE PROGRAM GUIDELINES

GENERAL DIGESTION METHODS

LIST OF TESTED SAMPLES IN MILESTONE ANALYTICAL LAB

APPLICATIONS FOR ALL ULTRAWAVE VERSIONS

UW-01 Mineral Oil

UW-04 Toys samples (Paper and polymer)

APPLICATIONS ONLY FOR ULTRAWAVE ECR VERSION

THE ULTTRAWAVVE APPLICATIO

The purpoose of the application

Anywaay pleasee consider that some applications might neeed somee

Applicatioons for UlttraWAVE ECR

The ECR vversion consists of pressure

• Applications that reqquire moree than 15 mL of hyddrochloric aacid, consiidering thee

Alll applications in thee first partt of this ap

Samples rreactivity Samp

Soils, aqueeous solution s,

Food (fattty samples),

Highly reeactive Polymer, petrochemicaal,

Orgaanic samplee HNO3, H2O2

Samples rreactivity Samp ples type Targeet temperatu

General digestion method for food samples

THE CLEANING /MAINTENANCE PROCEDURE MUST

Milestone Srl – Helping Chemists www.milestonesrl.com application@milestonesrl.com

General digestion method for environmental samples

5 positions* 2g 10 ml of HNO3 THE CLEANING /MAINTENANCE PROCEDURE

- Add acid drop-by-drop

- Wait for the exothermic reaction to subside

- Use Vortex system, before the digestion

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General digestion method for polymers

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General digestion method for petrochemical products

This procedure is only a guideline and it may need to be modified

Milestone Srl – Helping Chemists www.milestonesrl.com application@milestonesrl.com

General digestion method for pharmaceutical samples

5 positions Up to 800 mg* 8ml of HNO3

THE CLEANING /MAINTENANCE PROCEDURE MUST

This procedure is only a guideline and it may need to be modified

Milestone Srl – Helping Chemists www.milestonesrl.com application@milestonesrl.com

General method for biological samples

Nitrogen tank THE CLEANING /MAINTENANCE PROCEDURE MUST

Place the following basic load into the main 1 L

15 positions* 0,5 g 5 ml of HNO3

22 positions* 0,2 g 3 ml of HNO3

Sample amounts refers to dry matter

Milestone Srl – Helping Chemists www.milestonesrl.com application@milestonesrl.com

Step Time T1 T2 P Power

Basic Load *Milestone suggest Quartz or Glass vials

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Polyethylene loaded with Si (Total Si recovery)

Basic Load Use the PTFE protection for thermowell (P/N

Rack type Sample Amount Reagents

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Terephtalic acid (PTA)

Rack type Sample Amount Reagents

THE CLEANING /MAINTENANCE PROCEDURE MUST

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Toys samples (Paper and polymer)

In case of Si presence, add 1 mL of HF