DE3422360A1 - Nitrogen heating apparatus for volatilisation of solutions - Google Patents

Nitrogen heating apparatus for volatilisation of solutions

Info

Publication number
DE3422360A1
DE3422360A1 DE19843422360 DE3422360A DE3422360A1 DE 3422360 A1 DE3422360 A1 DE 3422360A1 DE 19843422360 DE19843422360 DE 19843422360 DE 3422360 A DE3422360 A DE 3422360A DE 3422360 A1 DE3422360 A1 DE 3422360A1
Authority
DE
Germany
Prior art keywords
nitrogen
solutions
evaporation
volatilisation
heating apparatus
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
DE19843422360
Other languages
German (de)
Inventor
Dieter Dr. 8042 Oberschleißheim Jahr
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to DE19843422360 priority Critical patent/DE3422360A1/en
Publication of DE3422360A1 publication Critical patent/DE3422360A1/en
Ceased legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N30/12—Preparation by evaporation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/14—Evaporating with heated gases or vapours or liquids in contact with the liquid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44—Sample treatment involving radiation, e.g. heat
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/84—Preparation of the fraction to be distributed

Abstract

To ensure a rapid, gentle and loss-free volatilisation of solutions, surface evaporation using nitrogen as a heat transfer medium is used. The apparatus is used for sample preparation in instrumental analytical chemistry. Amongst a multiplicity of applications, derivatisation in gas chromotography and solvent change in HPLC/MS transfer can be emphasised. The nitrogen heating apparatus contains devices for flow control, for electrical heating of the gas and for removal of the evaporated solvent by suction.

Description

Beschreibung:Description:

Stickstoff-Heizgerät zum Abdampfen von Lösungen Die Erfindung betrifft eine einfache Möglichkeit zum Abdampfen von Lösungen nach den Ansprüchen 1 und 2. Die Apparatur findet Verwendung zur Probenvorbereitung in der instrumentellen analytischen Chemie (GC, HPLC, MS, DC). Dabei ist es häufig notwendig, Extraktlösungen einzuengen (zur Anreicherung der zu untersuchenden gelösten Stoffe) oder vollständig abzudampfen (z.B. vor der Derivatisierung zur Gaschromatographie oder zum Lösungsmittelwechsel beim HPLC/MS-Transfer).Nitrogen heater for evaporation of solutions The invention relates to a simple way of evaporating solutions according to claims 1 and 2. The apparatus is used for sample preparation in the instrumental analytical field Chemistry (GC, HPLC, MS, TLC). It is often necessary to concentrate extract solutions (for the enrichment of the dissolved substances to be examined) or to evaporate completely (e.g. before derivatisation for gas chromatography or for changing the solvent for HPLC / MS transfer).

Diese Aufgabe wird bisher durch Aufheizen des Proben gefäßes in einem gebohrten Metall-Heizblock oder in einem Wasserbad (evtl. unterstützt durch Abblasen mit ungeheiztem Stickstoff) bewältigt. Auch ein Abdampfen unter vermindertem Druck im Rotationsverdampfer ist möglich. Beide Methoden haben den Nachteil, daß insbesondere bei wasserhaltigen Lösungen Stoßen und Spritzen durch Siedeverzüge und damit Substanzverluste eintreten. Beim Eindampfen in einem gebohrten Metall-Heizblock oder in einem Wasserbad muß die ganze Lösung auf Siedetemperatur gehalten werden. Diese thermische Belastung ist bei empfindlichen chemischen Stoffen von Nachteil, zumal der Endpunkt des Abdampfens schlecht von außen zu erkennen ist und daher leicht zu lange erhitzt wird.This task is so far by heating the sample vessel in one drilled metal heating block or in a water bath (possibly assisted by blowing off with unheated nitrogen). Also evaporation under reduced pressure in a rotary evaporator is possible. Both methods have the disadvantage that in particular In the case of water-based solutions, bumping and spraying due to delayed boiling and thus loss of substance enter. When evaporating in a drilled metal heating block or in a water bath the whole solution must be kept at the boiling point. This thermal load is a disadvantage for sensitive chemical substances, especially the end point of evaporation is difficult to see from the outside and is therefore easily heated for too long.

Der Erfindung liegt die Aufgabe zugrunde, den Abdampfvorgang zügig und verlustfrei durchzuführen. Dabei soll die thermische Belastung der gelösten Stoffe so gering wie möglich gehalten werden.The invention is based on the task of the evaporation process quickly and to be carried out without loss. The thermal load of the dissolved Substances are kept as low as possible.

Diese Aufgabe wird gelöst durch Oberflächenverdampfung mit Stickstoff als Wärmeüberträger wie in Anspruch 1 beschrieben.This problem is solved by surface evaporation with nitrogen as a heat exchanger as described in claim 1.

Die mit der Erfindung erzielten Vorteile bestehen darin, daß der Verdampfungsvorgang zügig und ohne Verluste durch Siedeverzüge abläuft. Die Verdampfung findet nur an der Flüssigkeitsoberfläche statt, das Probenvolumen selbst bleibt bei Raumtemperatur. Besonders bei empfindlichen chemischen Stoffen ist diese Methode von Vorteil, zumal der Vorgang unter Stickstoff als Schutzgas stattfindet. Der Endpunkt des Abdampfens kann ungehindert von außen beobachtet werden. Ein unnötig langes Erhitzen der Probe kann daher leicht vermieden werden.The advantages achieved by the invention are that the evaporation process expires quickly and without losses due to delayed boiling. The evaporation only takes place the surface of the liquid, the sample volume itself remains at room temperature. This method is particularly advantageous when it comes to sensitive chemical substances the process takes place under nitrogen as a protective gas. The end point of the evaporation can be observed from the outside unhindered. Heating the sample for an unnecessarily long time can therefore be easily avoided.

Die Temperatur des Heizgases kann in Grenzen beliebig eingestellt und für die zu untersuchende Stoffklasse optimiert werden.The temperature of the heating gas can be set arbitrarily within limits and optimized for the class of substances to be examined.

Ein Ausführungsbeispiel des Stickstoff-Heizgerätes, das für die vorgeschlagene Lösung erforderlich ist, ist in Zeichnung 1 dargestellt. Es enthält Einrichtungen zur Einstellung der erforderlichen Stickstoffströmung von 1,5 1/min (Nadelventil und Schwebekörper-Strömungsmesser) sowie elektrische Einrichtungen zur Messung und Einstellung der gewünschten Heizspannung. Die Aufheizung des Stickstoffstroms erfolgt indirekt in einem Heizgehäuse (siehe Zeichnung 2) durch einen elektrischen Heizwiderstand. Die Temperatur des Stickstoffs an der Austrittsöffnung beträgt maximal 1800C. Ein Ventilator sorgt für die schnelle Absaugung der verdampften Lösungsmittel. Das Gefäß mit der Lösung kann durch eine Hebebühne in eine günstige Lage unter die Auslaßöffnung des Heizgases gebracht werden. Durch ein zusätzliches Verteilerstück ist auch das gleichzeitige Abdampfen mehrerer Probengefäße möglich.An embodiment of the nitrogen heater that is proposed for the Solution is required is shown in drawing 1. It contains facilities for setting the required nitrogen flow of 1.5 1 / min (needle valve and variable area flow meters) as well as electrical devices for measuring and Setting the desired heating voltage. The nitrogen stream is heated indirectly in a heating housing (see drawing 2) through an electrical heating resistor. The temperature of the nitrogen at the outlet opening is a maximum of 1800C. A The fan ensures that the evaporated solvents are extracted quickly. The container the solution can be placed in a convenient position under the outlet opening through a lifting platform of the heating gas are brought. This is also possible with an additional distributor simultaneous evaporation of several sample vessels possible.

Claims (2)

Patentansprüche: 1. Apparatur zur Erzeugung eines heißen Stickstoffstroms zum Abdampfen von Lösungen im Maßstab von wenigen Millilitern durch Oberflächenverdampfung.Claims: 1. Apparatus for generating a hot nitrogen stream for evaporation of solutions on a scale of a few milliliters by surface evaporation. Die Vorrichtung ist dadurch gekennzeichnet, daß der elektrisch beheizte Stickstoffstrom von oben her auf die Flüssigkeitsoberfläche im Probengefäß gerichtet ist und eine zügige Verdampfung gewährleistet. The device is characterized in that the electrically heated Stream of nitrogen directed from above onto the surface of the liquid in the sample vessel and quick evaporation is guaranteed. 2. Vorrichtung nach Anspruch 1, dadurch gekennzeichnet, daß die Temperatur des ausstömenden Heizgases je nach den Erfordernissen des gelösten Stoffes in Grenzen frei einstellbar ist.2. Apparatus according to claim 1, characterized in that the temperature of the emitted heating gas within limits depending on the requirements of the dissolved substance is freely adjustable.
DE19843422360 1984-06-15 1984-06-15 Nitrogen heating apparatus for volatilisation of solutions Ceased DE3422360A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE19843422360 DE3422360A1 (en) 1984-06-15 1984-06-15 Nitrogen heating apparatus for volatilisation of solutions

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19843422360 DE3422360A1 (en) 1984-06-15 1984-06-15 Nitrogen heating apparatus for volatilisation of solutions

Publications (1)

Publication Number Publication Date
DE3422360A1 true DE3422360A1 (en) 1984-11-08

Family

ID=6238500

Family Applications (1)

Application Number Title Priority Date Filing Date
DE19843422360 Ceased DE3422360A1 (en) 1984-06-15 1984-06-15 Nitrogen heating apparatus for volatilisation of solutions

Country Status (1)

Country Link
DE (1) DE3422360A1 (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3632245A1 (en) * 1986-09-23 1988-04-07 Siemens Ag Method for concentrating aqueous solutions from production processes and apparatus for carrying out the method
FR2656540A1 (en) * 1990-01-03 1991-07-05 Rhone Poulenc Agrochimie EVAPORATION DEVICE AND SAMPLE WEIGHTING
WO2007104824A1 (en) * 2006-03-16 2007-09-20 Universidad Técnica Federico Santa María Semi-automatic device for the evaporation of solvents by analytical gas for concentration of atmospheric samples, which is designed to identify and quantify organic chemical compounds with toxic properties
WO2010076580A1 (en) * 2006-09-21 2010-07-08 Mariana Arce-Osuna Iris digester-evaporator interface

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2653902A1 (en) * 1976-11-27 1978-06-01 Schmidt Gayk Heinrich Eduard D Multiple specimen evapn. chamber - with injection cannulae for multiple gas outlets to micro-titration plate
DE2903008A1 (en) * 1979-01-25 1980-07-31 Schering Ag METHOD FOR EVAPORATION AND, IF NECESSARY, RECOVERY OF WATER FROM AQUEOUS SOLUTIONS

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2653902A1 (en) * 1976-11-27 1978-06-01 Schmidt Gayk Heinrich Eduard D Multiple specimen evapn. chamber - with injection cannulae for multiple gas outlets to micro-titration plate
DE2903008A1 (en) * 1979-01-25 1980-07-31 Schering Ag METHOD FOR EVAPORATION AND, IF NECESSARY, RECOVERY OF WATER FROM AQUEOUS SOLUTIONS

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3632245A1 (en) * 1986-09-23 1988-04-07 Siemens Ag Method for concentrating aqueous solutions from production processes and apparatus for carrying out the method
FR2656540A1 (en) * 1990-01-03 1991-07-05 Rhone Poulenc Agrochimie EVAPORATION DEVICE AND SAMPLE WEIGHTING
WO2007104824A1 (en) * 2006-03-16 2007-09-20 Universidad Técnica Federico Santa María Semi-automatic device for the evaporation of solvents by analytical gas for concentration of atmospheric samples, which is designed to identify and quantify organic chemical compounds with toxic properties
WO2010076580A1 (en) * 2006-09-21 2010-07-08 Mariana Arce-Osuna Iris digester-evaporator interface

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OAV Applicant agreed to the publication of the unexamined application as to paragraph 31 lit. 2 z1
OP8 Request for examination as to paragraph 44 patent law
8131 Rejection