application report mws-3 - onlinecas.com berghof/micro...berghof products + instruments gmbh...

V. 4.0

Application Report

Microwave Pressure Digestion

Food, Pharma, Cosmetics

MWS-3+

BERGHOF Products + Instruments GmbHLabor-Technik

Harretstr. 1 • 72800 Eningen • GermanyTel.: +49 7121 894-0 • Fax: +49 7121 894-300http://www.berghof-instruments.de

Contact:Dr. Dieter Gutwerk Tel.: +49 7121 894-127 • E-Mail: [email protected]. Rainer Krämer Tel.: +49 7121 894-142 • E-Mail: [email protected]

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MICROWAVE DIGESTION OF BLOOD

Summary Blood and similar samples are digested in a acid solution using a Berghofmicrowave digestion system

Equipment Type ManufacturerMWS-3 Berghof Products + Instruments, GermanyDAP-60S or DAQ-20S Berghof Products + Instruments, Germany

Reagents HNO3 65%

Procedure* Weigh 2.0 ml of the sample into the digestion vessel and add 5 ml of nitricacid and shake the mixture carefully or stirr with a clean teflon or a glass bar.Wait at least 20 minutes before the vessel is closed. Heat in the microwaveoven with the following program.

Temperature Program Step 1 2 3 4 5 6T [°C] 160 190 100 100Ta [min] 5 1 1 1Time [min] 5 10 10 10To avoid foaming and splashing wait until the vessels have cooled to room temperature (about20 min). Carefully open the digestion vessel in a fume hood wearing hand, eye and bodyprotection since a large amount of gas will be produced during the digestion process.

Results Clear solution

Notes: This application serves only as a guide line and may need to be optimised for yoursample.*When the Berghof quatz-liner DAQ-20S is used, the sample weight must be reduced to lessthan 750µl. The sample is digested in 3 ml nitric acid.




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MICROWAVE DIGESTION OF BODY LOTION

Summary Body lotion and similar samles are digested in a acid solution using a Berghofmicrowave digestion system. Spontanous reactions are avoided by heating insteps.


Reagents HNO3 65%

Procedure* Weigh 300 mg of the sample into the digestion vessel and add 5ml of nitricacid and shake the mixture carefully or stirr with a clean teflon or a glass bar.Wait at least 10 minutes before the vessel is closed. Heat in the microwaveoven with the following program.

Temperature Program Step 1 2 3 4T [°C] 170 190 100Ta [min] 2 5 1Time [min] 5 30 15To avoid foaming and splashing wait until the vessels have cooled to room temperature (about20 min). Carefully open the digestion vessel in a fume hood wearing hand, eye and bodyprotection since a large amount of gas will be produced during the digestion process.

Results clear solution.If the sample contains pigments, 2 ml hydrofluoric acid (40%) must be addedto obtain a clear solution.

Notes: This application serves only as a guide line and may need to be optimised for yoursample.*When the Berghof quartz liner DAQ-20S is used, the sample weight must be reduced to lessthan 100 mg. The sample is digested in 3ml nitric acid.




M W S - 3

MICROWAVE DIGESTION OF BONES

Summary Digestion of bones with a mixture of nitric acid and hydrochloric acid using aBerghof microwave digestion system.

Equipment Type ManufacturerMWS-3 Berghof Products + Instruments, GermanyDAP-60S Berghof Products + Instruments, Germany

Reagents HNO3 65%HCl 37%

Procedure Weigh 300 mg of the sample into the digestion vessel. Add 8 ml of nitric acid,2 ml of hydrochloric acid and shake the mixture carefully or stirr with a cleanteflon or a glass bar. Wait at least 2 min before the vessel is closed. Heat inthe microwave oven with the following program.

Temperature Program Step 1 2 3 4 5 6T [°C] 160 180 190Ta [min] 10 5 3Time [min] 10 10 10Wait until the vessels have cooled to room temperature. Carefully open the digestion vessel ina fume hood wearing hand, eye and body protection..

Results The samples are digested completely.

Notes: This application serves only as a guide line and may need to be optimised for yoursample.




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MICROWAVE DIGESTION OF BRAN

Summary Bran is digested in a acid solution using a Berghof microwave digestionsystem. Spontanous reactions are avoided by heating in steps.


Reagents HNO3 65%H2O2 30%

Procedure Weigh 300 mg of the sample into the digestion vessel. Add 5 ml of nitric acidand 2 ml hydrogen peroxide. Close the vessel and heat in the microwaveoven with the following program.







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MICROWAVE DIGESTION OF CALCIUM STEARATE

Summary Calcium stearate is digested in a acid solution using a Berghof microwavedigestion system. Spontanous reactions are avoided by heating in steps.



Procedure Weigh 100mg of the sample into the digestion vessel. Add 5 ml of nitric acidand 2 ml hydrogen peroxide. Close the vessel and heat in the microwaveoven with the following program.

Temperature Program Step 1 2 3 4T [°C] 145 170 100 100Ta [min] 10 5 5 1Time [min] 5 10 10 10To avoid foaming and splashing wait until the vessels have cooled to room temperature (about20 min). Carefully open the digestion vessel in a fume hood wearing hand, eye and bodyprotection since a large amount of gas will be produced during the digestion process.

The solution is transfered to volumetric flask and filled to 25 ml with water.






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MICROWAVE DIGESTION OF CASTOR OIL

Summary Castor oil is digested in a acid mixture with a Berghof microwave digestionsystem. Spontanous reactions are avoided by heating in steps.

Equipment Type ManufacturerMWS-3 Berghof Products + Instruments, GermanyDAP-60 Berghof Products + Instruments, Germany


Procedure Weigh 100 mg of the sample into the digestion vessel. Add 6 ml of nitric acidand 2 ml of hydrogen peroxide. Close the vessel and heat in the microwaveoven with the following program.







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MICROWAVE DIGESTION OF COCONUT FAT

Summary Coconut fat is digested in a acid solution using a Berghof microwavedigestion system. Spontanous reactions are avoided by heating in steps.



Procedure Weigh 100mg of the sample into the digestion vessel. Add 5 ml of nitric acidand 2 ml hydrogen peroxide. Close the vessel and heat in the microwaveoven with the following program.


The solution is transfered to volumetric flask and filled to 25 ml with water.






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MICROWAVE DIGESTION OF COFFEE

Summary Coffee and similar samples are digested in a acid solution using a Berghofmicrowave digestion system


Reagents HNO3 65%

Procedure Weigh 300 mg of the sample into the digestion vessel and add 7.5 ml of nitricacid. Heat in the microwave oven with the following program.







M W S - 3


Summary Coffee is digested in a acid solution using a Berghof microwave digestionsystem



Procedure Weigh 300 mg of the sample into the digestion vessel and add 3 ml of nitricacid and 3 ml hydrogenperoxide. Shake the mixture carefully or stirr with aclean teflon or glass bar. Wait at least 20 min. before the vessel is closed.Heat in the microwave oven with the following program.







M W S - 3


Summary Coffee is digested in a acid solution using a Berghof microwave digestionsystem


Reagents HNO3 65%

Procedure Weigh 300 mg of the sample into the digestion vessel and add 5 ml of nitricacid. Shake the mixture carefully or stirr with a clean teflon or glass bar. Waitat least 20 min. before the vessel is closed. Heat in the microwave oven withthe following program.







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MICROWAVE DIGESTION OF COGNAC

Summary Cognac is digested in a acid solution using a Berghof microwave digestionsystem. Spontanous reactions are avoided by heating in steps.



Procedure Weigh 0.5 ml of the sample into the digestion vessel. Add 5 ml of nitric acidand 5 ml hydrogen peroxide. Close the vessel and heat in the microwaveoven with the following program.







M W S - 3

MICROWAVE DIGESTION OF FACE CREME

Summary Face cremes and similar samles are digested in a acid solution using aBerghof microwave digestion system. Spontanous reactions are avoided byheating in steps.


Reagents HNO3 65%








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MICROWAVE DIGESTION OF FARINE

Summary Farine is digested in a acid solution using a Berghof microwave digestionsystem. Spontanous reactions are avoided by heating in steps.










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MICROWAVE DIGESTION OF FEED

Summary Feed and similar samples are digested in a acid solution using a Berghofmicrowave digestion system


Reagents HNO3 65%








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MICROWAVE DIGESTION OF FEED

Summary Feeds and similar samples are digested in a acid solution using a Berghofmicrowave digestion system










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MICROWAVE DIGESTION OF FISHMEAL

Summary Fishmeal is digested in an acid solution with a BERGHOF microwavedigestion system.



Procedure Weigh 500 mg of the sample into the digestion vessel. Add 8ml of nitric acidand 2ml of hydrogen peroxide. Close the vessel and heat in the microwaveoven with the following program.

Temperature Program Step 1 2 3 4T [°C] 200 100 100 100Ta [min] 15 1 1 1Time [min] 40 10 0 10Wait until the vessels have cooled to room temperature (about 20 min). Carefully open thedigestion vessel in a fume hood wearing hand, eye and body protection since a large amountof gas will be produced during the digestion process.






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MICROWAVE DIGESTION OF FRUIT JUICES

Summary Fruit juices are digested in a acid solution using a Berghof microwavedigestion system.



Procedure Weigh 5 ml of the sample into the digestion vessel and add 5 ml of nitric acidand 1.0 ml hydrogenperoxide. Shake the mixture carefully or stirr with a cleanteflon or glass bar before closing the vessels. Heat in the microwave ovenwith the following program.


Results clear solution





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MICROWAVE DIGESTION OF FRUITES

Summary Fruites (dried) are digested in a acid solution using a Berghof microwavedigestion system.



Procedure Weigh 250 mg of the sample into the digestion vessel and ad 6 ml of nitricacid and 1.0 ml hydrogenperoxide. Shake the mixture carefully or stirr with aclean teflon or glass bar before closing the vessels. Heat in the microwaveoven with the following program.







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MICROWAVE DIGESTION OF KOREA GINGSENG

Summary Korea Gingseng is digested in a acid solution using a Berghof microwavedigestion system.


Reagents HNO3 65% H2O2 30%



Transfer the solution to a volumetric flask and dilute with water to 25ml.

Results Clear solutionAll elements are determined by GF-AAS.

Element Limit of detection[µg/g]

Result[µg/g]

Variation Coefficient[%]

Cd 0.01 0.088 ± 0.005 5.7

Pb 0.05 0.250 ± 0.018 7.4

Cu 0.05 7.75 ± 0.244 3.1

Cr 0.05 0.256 ± 0.009 3.6

Ni 0.05 1.73 ± 0.137 7.9

Hg 0.01 < 0.01 -





M W S - 3

MICROWAVE DIGESTION OF HAIR

Summary Hair and similar samples are digested in a acid solution using a Berghofmicrowave digestion system

Equipment Type ManufacturerMWS-3 Berghof Products + Instruments, GermanyDAP-60S or DAQ-20H Berghof Products + Instruments, Germany

Reagents HNO3 65%

Procedure* Weigh 250 mg of the sample into the digestion vessel and add 5 ml of nitricacid and shake the mixture carefully or stirr with a clean teflon or aglass bar.Wait at least 20 minutes before the vessel is closed. Heat in the microwaveoven with the following program.



Notes: This application serves only as a guide line and may need to be optimised for yoursample.*When the Berghof quatz-liner DAQ-20S is used, the sample weight must be reduced to lessthan 100 mg. The sample is digested in 3 ml nitric acid.




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MICROWAVE DIGESTION OF LIME

Summary Lime is digested in a acid solution using a Berghof microwave digestionsystem. Spontanous reactions are avoided by heating in steps.










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MICROWAVE DIGESTION OF LINE SEED

Summary Line seed and similar samples are digested in a acid solution using a Berghofmicrowave digestion system


Reagents HNO3 65%

Procedure Weigh 500 mg of the sample into the digestion vessel and add 10 ml of nitricacid. Heat in the microwave oven with the following program.

Temperature Program Step 1 2 3 4 5 6T [°C] 160 190 100 100Ta [min.] 5 1 1 1Time [min] 5 10 10 10To avoid foaming and splashing wait until the vessels have cooled to room temperature (about40 min.). Carefully open the digestion vessel in a fume hood wearing hand, eye and bodyprotection since a large amount of gas will be produced during the digestion process.






M W S - 3


Summary Line seed is digested in a acid solution using a Berghof microwave digestionsystem










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Summary Line seed is digested in a acid solution using a Berghof microwave digestionsystem


Reagents HNO3 65%








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MICROWAVE DIGESTION OF LIPSTICK

Summary Lipsticks and similar samles are digested in a acid solution using a Berghofmicrowave digestion system. Spontanous reactions are avoided by heating insteps.


Reagents HNO3 65%HF 40%

Procedure* Weigh 250 mg of the sample into the digestion vessel and add 5ml of nitricacid, 2 ml of hydrofluoric acid and shake the mixture carefully or stirr with aclean teflon or a glass bar. Wait at least 10 minutes before the vessel isclosed. Heat in the microwave oven with the following program.


Results clear solution.

Notes: This application serves only as a guide line and may need to be optimised for yoursample.*When the Berghof quartz liner DAQ-20S is used, the sample weight must be reduced to lessthan 100 mg. The sample is digested in 3ml nitric acid and 1.0 ml hydrofluoric acid.




M W S – 3

MICROWAVE DIGESTION OF MILK POWDER

Summary Milk powder is digested in a acid solution using a Berghof microwavedigestion system


Reagents HNO3 65%








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Procedure Weigh 200 mg of the sample into the digestion vessel and add 4 ml of nitricacid and 1 ml hydrochloric acid. Shake the mixture carefully or stirr with aclean teflon or glass bar. Wait at least 20 min. before the vessel is closed.Heat in the microwave oven with the following program.







M W S - 3


Summary Reference Material Skim Milk Powder BCR 151 is digested in a acid solutionusing a Berghof microwave digestion system.







Validation All elements are determined by GF-AAS.


Result[µg/g]

Certified Value[µg/g]

Cd 0.01 0.090 ± 0.010 0.101 ± 0.010Cu 0.1 5.46 ± 0.04 5.23 ± 0.10Hg 0.03 0.094 ± 0.003 0,101 ± 0,012





M W S - 3

MICROWAVE DIGESTION OF MUFFINS

Summary Muffins are digested in an acid solution with a Berghof microwave digestionsystem.



Procedure Weigh 1000 mg of the sample into the digestion vessel. Add 10ml of nitricacid 2ml hydrogen peroxide. Close the vessel and heat in the microwaveoven with the following program.


Results Clear solution.





M W S - 3

MICROWAVE DIGESTION OF MULTI VITAMIN ANDMINERAL TABLETS

Summary Different multi-vitamin and multi-mineral tablets (gelatine tablets or dragees)are digested in a acid solution using a Berghof microwave digestion system

Equipment Type ManufacturerMWS-3 Berghof Products + Instruments, GermanyDAC-100 Berghof Products + Instruments, Germany


Procedure One tablet is weighed (350 – 1000 mg) into the digestion vessel. Add 15 ml ofnitric acid, 3 ml hydrogenperoxide and 25 ml water. Shake the mixturecarefully or stirr with a clean teflon or glass bar. Wait at least 5 min. beforethe vessel is closed. Heat in the microwave oven with the following program.


The solution is transfered to a volumetric flask and and diluted with water to250 ml.

Results Clear, colourless solution.





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MICROWAVE DIGESTION OF OLIVE LEAVES

Summary Reference Material Olive Leaves BCR 62 is digested in a acid solution usinga Berghof microwave digestion system.








Result[µg/g]


Cd 0.01 0.080 ± 0.024 0.10 ± 0.02Pb 0.05 29.3 ± 1.5 25 ± 1.5Cu 0.05 48.9 ± 3.4 46.6 ± 1.8Hg 0.01 0.33 ± 0.02 0.28 ± 0.02





M W S - 3

MICROWAVE DIGESTION OF OLIVE OIL

Summary Olive oil is digested in a acid solution using a Berghof microwave digestionsystem. Spontanous reactions are avoided by heating in steps.



Procedure Weigh 0,75 ml (about 700 mg) of the sample into the digestion vessel. Add10 ml of nitric acid and 2 ml hydrogen peroxide. Close the vessel and heat inthe microwave oven with the following program.







M W S - 3

MICROWAVE DIGESTION OF OLIVE OIL

Summary Olive oil is digested in a acid solution using a Berghof microwave digestionsystem. Spontanous reactions are avoided by heating in steps.










M W S - 3

MICROWAVE DIGESTION OF PAPRIKA POWDER

Summary Paprika powder is digested in a acid solution using a Berghof microwavedigestion system


Reagents HNO3 65%








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MICROWAVE DIGESTION OF PAPRIKA POWDER

Summary Paprika powder is digested in a acid solution using a Berghof microwavedigestion system










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MICROWAVE DIGESTION OF PIG FEED

Summary Pig feed and similar samples are digested in a acid solution using a Berghofmicrowave digestion system


Reagents HNO3 65%








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MICROWAVE DIGESTION OF DRIED PLANTS

Summary Dried plants are digested in a acid solution using a Berghof microwavedigestion system










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MICROWAVE DIGESTION OF PLANT SAMPLES

Summary Plant samples (dried) are digested in a acid solution using a Berghofmicrowave digestion system. This digestion procedure is usually used for thedetermination of phosphourous and nitrogen.


Reagents H2SO4 95-97%H2O2 30%

Procedure Weigh 150 mg of the sample into the digestion vessel and ad 4.5 ml ofsulfuric acid and 4.5 ml hydrogenperoxide. Shake the mixture carefully or stirrwith a clean teflon or glass bar before closing the vessels. Heat in themicrowave oven with the following program.







M W S - 3

MICROWAVE DIGESTION OF PLANT SAMPLES

Summary Plant samples (dried) are digested in a acid solution using a Berghofmicrowave digestion system


Reagents HNO3 65%

Procedure Weigh 300 mg of the sample into the digestion vessel and add 7.5 ml of nitricacid. Shake the mixture carefully or stirr with a clean teflon or glass bar. Heatin the microwave oven with the following program.







M W S - 3

MICROWAVE DIGESTION OF RICE

Summary Whole Rice grains are digested in an acid solution with a Berghof microwavedigestion system.










M W S - 3

MICROWAVE DIGESTION OF SHAMPOO

Summary Shampoos and similar samles are digested in a acid solution using a Berghofmicrowave digestion system. Spontanous reactions are avoided by heating insteps.


Reagents HNO3 65%








M W S - 3

MICROWAVE DIGESTION OF SOAP

Summary Soap and similar samles are digested in a acid solution using a Berghofmicrowave digestion system. Spontanous reactions are avoided by heating insteps.










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MICROWAVE DIGESTION OF SUGAR

Summary Sugar is digested in a acid solution using a Berghof microwave digestionsystem










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MICROWAVE DIGESTION OF SUN PROTECTION CREME

Summary Sun Protection cremes and similar samles are digested in a acid solutionusing a Berghof microwave digestion system. Spontanous reactions areavoided by heating in steps.










M W S - 3

MICROWAVE DIGESTION OF TEA

Summary Tea and similar samples are digested in a acid solution using a Berghofmicrowave digestion system


Reagents HNO3 65%


Temperature Program Step 1 2 3 4 5 6T [°C] 150 160 190Ta [min] 5 5 5Time [min] 10 10 20To avoid foaming and splashing wait until the vessels have cooled to room temperature (about30 min). Carefully open the digestion vessel in a fume hood wearing hand, eye and bodyprotection since a large amount of gas will be produced during the digestion process.






M W S - 3

MICROWAVE DIGESTION OF MOTHER TINCTURES

Summary Pharmaceutical mother tinctures are digested in a acid solution using aBerghof microwave digestion system.


Reagents HNO3 65% H2O2 30%






Result[µg/g]

Variation Coefficient[%]

Cd 0.01 <0.01 -Pb 0.05 <0.05 -Cu 0.05 0.36 ± 0.033 9.2

Cr 0.05 0.109 ± 0.013 12.1

Ni 0.05 0.094 ± 0.016 17.5

Hg 0.01 < 0.01 -





M W S - 3

MICROWAVE DIGESTION OF TISSUE

Summary Tissue and similar samles are digested in a acid solution using a Berghofmicrowave digestion system. Spontanous reactions are avoided by heating insteps.


Reagents HNO3 65%

Procedure* Weigh 250 mg of the sample into the digestion vessel and add 5ml of nitricacid and shake the mixture carefully or stirr wirh a clean teflon or a glass bar.Wait at least 20 minutes before the vessel is closed. Heat in the microwaveoven with the following program.







M W S - 3

MICROWAVE DIGESTION OF TOMATO LEAVES

Summary Tomato Leaves and similar samples are digested in a acid solution using aBerghof microwave digestion system.

Equipment Type ManufacturerMWS-3 Berghof Products + Instruments, GermanyDAC-60S Berghof Products + Instruments, Germany

Reagents H2SO4 95-97%H2O2 30%

Procedure Weigh 50 mg of the sample into the digestion vessel. 5 ml of sulfuric acid and2 ml hydrogenperoxide are added dropwise. Shake the mixture carefully orstirr with a clean teflon or glass bar before closing the vessels. Heat in themicrowave oven with the following program.


If the sample is not dissolved completely, add again 1-2 ml hydrogenperoxideand heat again.

Results The samples are digested completely. The solution can be used forphotometric determination of phosphate with ascorbic acid and molybdate-reagent at 880 nm.





M W S - 3

MICROWAVE DIGESTION OF TOMATO LEAVES

Summary Reference Material Tomato Leaves 1573a is digested in a acid solution usinga Berghof microwave digestion system.








Result[µg/g]


Cd 0.01 1.52 ± 0.10 1.52 ± 0.04Cr 0.05 1.94 ± 0.23 1.99 ± 0.06Ni 0.05 1.49 ± 0.10 1.59 ± 0,07Hg 0.01 0.036 ± 0.004 0.034 ± 0.004





M W S - 3

MICROWAVE DIGESTION OF TOOTHPASTE

Summary Toothpastes and similar samles are digested in a acid solution using aBerghof microwave digestion system. Spontanous reactions are avoided byheating in steps.










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MICROWAVE DIGESTION OF VANILLA DESSERT

Summary Vanilla dessert and similar samples are digested in a acid solution using aBerghof microwave digestion system


Reagents HNO3 65%

Procedure* Weigh 400 mg of the sample into the digestion vessel and add 7.5 ml of nitricacid. Shake the mixture carefully or stirr with a clean teflon or glass bar. Waitat least 20 min. before the vessel is closed. Heat in the microwave oven withthe following program.







M W S - 3

MICROWAVE DIGESTION OF VEGETABLES

Summary Vegetables (dried) are digested in a acid solution using a Berghof microwavedigestion system.



Procedure Weigh 250 mg of the sample into the digestion vessel and ad 6 ml of nitricacid and 1.0 ml hydrogenperoxide. Shake the mixture carefully or stirr with aclean teflon or glass bar before closing the vessels. Heat in the microwaveoven with the following program.







M W S - 3

MICROWAVE DIGESTION OF WHEAT

Summary Whole wheat grains are digested in an acid solution with a Berghofmicrowave digestion system.










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MICROWAVE DIGESTION OF YOGURT

Summary Yogurt is digested in an acid solution using a Berghof microwave digestionsystem:



Procedure Weigh 500mg of the sample into the digestion vessel and add 5ml water, 5mlnitric acid and 2ml hydrochloric acid. Shake the mixture carefully or stirr witha clean teflon bar. Wait at least 20 min. before the vessel is closed. Heat inthe microwave oven with the following program with SOFTSTART switchedON:


Results Clear, colourless solution


application report mws-3 - onlinecas.com berghof/micro...berghof products + instruments gmbh...

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