DE19815753C2 - Process for the production of filtering silica gel for trace analysis - Google Patents

Process for the production of filtering silica gel for trace analysis

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Publication number
DE19815753C2
DE19815753C2 DE1998115753 DE19815753A DE19815753C2 DE 19815753 C2 DE19815753 C2 DE 19815753C2 DE 1998115753 DE1998115753 DE 1998115753 DE 19815753 A DE19815753 A DE 19815753A DE 19815753 C2 DE19815753 C2 DE 19815753C2
Authority
DE
Germany
Prior art keywords
silica gel
acetone
silver nitrate
water
production
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.)
Expired - Fee Related
Application number
DE1998115753
Other languages
German (de)
Other versions
DE19815753A1 (en
Inventor
Andreas Buslaps
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.)
BUSLAPS, ANDREAS, 88677 MARKDORF, DE
Original Assignee
Andreas Buslaps
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Filing date
Publication date
Application filed by Andreas Buslaps filed Critical Andreas Buslaps
Priority to DE1998115753 priority Critical patent/DE19815753C2/en
Publication of DE19815753A1 publication Critical patent/DE19815753A1/en
Application granted granted Critical
Publication of DE19815753C2 publication Critical patent/DE19815753C2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157—After-treatment of gels

Description

Die Erfindung betrifft ein Verfahren zur Herstellung filternden Kieselgels für die Spurenanalytik.The invention relates to a method for manufacturing filtering silica gel for trace analysis.

Kieselgel, insbesondere solches, das mit Silbernitrat imprägniert ist, dient in der Spurenanalytik zur Entfer­ nung besonders von störendem Schwefel und Schwefelver­ bindungen sowie polarer Störsubstanzen aus zu untersu­ chenden Proben.Silica gel, especially those containing silver nitrate impregnated is used in trace analysis for removal particularly disruptive sulfur and sulfur ver bonds and polar interfering substances to be examined samples.

Bisher wird das hierzu benötigte Kieselgel stets frisch hergestellt, da es nicht lagerfähig ist.So far, the silica gel required for this has always been fresh made because it is not storable.

Aus der DE 44 29 644 A1 ist ein Jodabsorbtionsmittel bekannt, das Silber oder ein Silbersalz auf einem porö­ sen, anorganischen Träger, beispielsweise SiO2 enthält und bestimmte Eigenschaften aufweist. Dabei wird der an­ organische Träger getrocknet und anschließend mehrfach mit einer wässrigen Silbernitratlösung imprägniert. Nach Abblasen der noch anhaftenden Silbernitratlösung werden die imprägnierten Trägerkügelchen getrocknet. DE 44 29 644 A1 discloses an iodine absorbent which contains silver or a silver salt on a porous, inorganic carrier, for example SiO 2 , and has certain properties. The organic carrier is dried and then impregnated several times with an aqueous silver nitrate solution. After blowing off the still adhering silver nitrate solution, the impregnated carrier beads are dried.

Aus der EP 0 034 037 A1 ist ein Mittel zu Absorbtion von Jod bekannt, daß einen porösen Träger beispielsweise Kieselgel, der mit einem Metallsalz imprägniert ist, aufweist. Dabei wird zunächst der poröse Träger herge­ stellt und dieser dann mit einer wässrigen Silbernitrat­ lösung imprägniert.EP 0 034 037 A1 describes a means for absorbing Iodine is known to be a porous carrier, for example Silica gel impregnated with a metal salt, having. First, the porous carrier is produced and then this with an aqueous silver nitrate impregnated solution.

Aus der JP 59196743 A ist ein Katalysator bekannt, der einen mit einer wässrigen Silbernitratlösung imprägnier­ ten Träger, beispielsweise Siliciumdioxid, aufweist.From JP 59196743 A a catalyst is known which impregnate one with an aqueous silver nitrate solution th carrier, for example silicon dioxide.

Aufgabe der Erfindung ist es, ein lagerfähiges Kieselgel und ein Verfahren zu seiner Herstellung zu schaffen.The object of the invention is a storable silica gel and to create a process for its manufacture.

Erfindungsgemäß wird dies durch die Merkmale des Haupt­ anspruches gelöst, die Unteransprüche geben vorteilhafte Ausführungsformen des Verfahrens wieder.According to the invention, this is due to the features of the main solved claim, the sub-claims give advantageous Embodiments of the method again.

Im folgenden wird anhand eines Beispiels die Herstellung eines über mindestens vier Monate haltbaren Produktes beschrieben:The following is the production using an example a product that can be kept for at least four months described:

Beispielexample

Zur Aktivierung wird Kieselgel (Kieselgel 60, 70-230 mesh) über fünf Stunden bei 550°C geglüht. Nach dem Ab­ kühlen wird das Kieselgel unter Feuchtigkeitsausschluß aufbewahrt und kann anschließend durch Imprägnierung weiter bearbeitet werden. Zur Bereitung von 100 g im­ prägniertem Kieselgel werden folgende Substanzen verwen­ det:
For activation, silica gel (silica gel 60, 70-230 mesh) is annealed at 550 ° C. for five hours. After cooling, the silica gel is stored in the absence of moisture and can then be further processed by impregnation. The following substances are used to prepare 100 g in the impregnated silica gel:

  • - 100 g geglühtes Kieselgel 60,- 100 g of annealed silica gel 60,
  • - 11,11 g Silbernitrat - 11.11 g of silver nitrate  
  • - 22,22 ml Aceton- 22.22 ml acetone
  • - 44,44 ml bidestilliertes Wasser- 44.44 ml of double distilled water

Das Silbernitrat wird zunächst vollständig in Wasser ge­ löst und anschließend das Aceton (im Verhältnis zum Was­ ser 1 : 2 nach Volumen) so zugegeben, daß sich beide Flüssigkeiten vollständig mischen. Die Lösung wird zu dem Kieselgel gegeben und alles 20 min kräftig geschüt­ telt, bis das Kieselgel eine einheitliche Konsistenz hat. Danach wird das Kieselgel eine Stunde geschüttelt, bzw. durchmischt.The silver nitrate is initially completely in water dissolves and then the acetone (in relation to what ser 1: 2 by volume) added so that both Mix liquids completely. The solution becomes too given the silica gel and vigorously poured everything for 20 min until the silica gel has a uniform consistency Has. Then the silica gel is shaken for an hour, or mixed.

Um das Aceton wieder zu entfernen, wird das Kieselgel fünf Stunden bei vermindertem Druck (20 mbar) am Rotati­ onsverdampfer rotiert. Das Kieselgel wird vorsichtig belüftet und im Trockenschrank innerhalb von fünf Stun­ den von 70 auf 125°C aufgeheizt. Zur Aktivierung wird das Kieselgel ca. weitere 16 Stunden auf 125°C erhitzt.In order to remove the acetone again, the silica gel five hours at reduced pressure (20 mbar) on the Rotati on evaporator rotates. The silica gel becomes careful ventilated and in the drying cabinet within five hours heated from 70 to 125 ° C. To activate the silica gel is heated to 125 ° C. for a further 16 hours.

Das nun erhältliche weiße Endprodukt wird in braune Glasflaschen gefüllt und hat sich als mindestens sechs- Monate haltbar bewiesen, während herkömmlich erstelltes Kieselgel ohne beigegebenes Aceton lediglich im Bereich von 14 Tagen haltbar ist.The now available white end product turns brown Filled glass bottles and has proven to be at least six Proven for months while conventionally created Silica gel without added acetone only in the area is stable for 14 days.

Claims (4)

1. Verfahren zur Herstellung filternden Kieselgels für die Spurenanalytik mit den Schritten:
  • - Aktivierung des Kieselgels durch Glühen,
  • - Lösen von Silbernitrat in Wasser,
  • - Beigabe von Aceton in die Wassersilbernitratlösung, Vermischen der Wassersilbernitratlösung mit dem ge­ glühten Kieselgel,
  • - Entfernen des Acetons durch Ausgasen.
1. Method for the production of filtering silica gel for trace analysis with the steps:
  • Activation of the silica gel by annealing,
  • - dissolving silver nitrate in water,
  • - adding acetone to the water silver nitrate solution, mixing the water silver nitrate solution with the annealed silica gel,
  • - Remove the acetone by degassing.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Verhältnis Wasser zu Aceton 2 : 1 nach Volumenan­ teilen ist.2. The method according to claim 1, characterized in that that the ratio of water to acetone 2: 1 by volume is to share. 3. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß auf 100 g geglühtes Kieselgel 22,22 ml Aceton und 44,44 ml bidestilliertes Wasser, in denen 11,11 g Sil­ bernitrat gelöst sind, verwendet werden.3. The method according to claim 1, characterized in that on 100 g of annealed silica gel 22.22 ml of acetone and 44.44 ml of double-distilled water, in which 11.11 g of Sil bernitrate are used. 4. Verfahren nach einem der vorangehenden Ansprüche, gekennzeichnet durch Belüften und anschließendes weite­ res Aktivieren des Kieselgels durch Aufheizen auf mehr als 100°C.4. The method according to any one of the preceding claims, characterized by ventilation and subsequent wide res Activate the silica gel by heating to more than 100 ° C.
DE1998115753 1998-04-08 1998-04-08 Process for the production of filtering silica gel for trace analysis Expired - Fee Related DE19815753C2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE1998115753 DE19815753C2 (en) 1998-04-08 1998-04-08 Process for the production of filtering silica gel for trace analysis

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE1998115753 DE19815753C2 (en) 1998-04-08 1998-04-08 Process for the production of filtering silica gel for trace analysis

Publications (2)

Publication Number Publication Date
DE19815753A1 DE19815753A1 (en) 1999-10-14
DE19815753C2 true DE19815753C2 (en) 2003-05-28

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Application Number Title Priority Date Filing Date
DE1998115753 Expired - Fee Related DE19815753C2 (en) 1998-04-08 1998-04-08 Process for the production of filtering silica gel for trace analysis

Country Status (1)

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DE (1) DE19815753C2 (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0034037A1 (en) * 1980-02-04 1981-08-19 Hitachi, Ltd. Method of preparation of material for adsorbing iodine
JPS59196743A (en) * 1983-04-21 1984-11-08 Mitsui Toatsu Chem Inc Silver catalyst for preparation of ethylene oxide
DE4429644A1 (en) * 1994-08-20 1996-02-22 Sued Chemie Ag iodine adsorbent

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0034037A1 (en) * 1980-02-04 1981-08-19 Hitachi, Ltd. Method of preparation of material for adsorbing iodine
JPS59196743A (en) * 1983-04-21 1984-11-08 Mitsui Toatsu Chem Inc Silver catalyst for preparation of ethylene oxide
DE4429644A1 (en) * 1994-08-20 1996-02-22 Sued Chemie Ag iodine adsorbent

Also Published As

Publication number Publication date
DE19815753A1 (en) 1999-10-14

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Legal Events

Date Code Title Description
OP8 Request for examination as to paragraph 44 patent law
8304 Grant after examination procedure
8327 Change in the person/name/address of the patent owner

Owner name: BUSLAPS, ANDREAS, 88677 MARKDORF, DE

8364 No opposition during term of opposition
8339 Ceased/non-payment of the annual fee