DE4113212A1 - Cyanide standard soln. contg. complex cyanide, pref. tetra:cyano-zincate - easily releasing cyanide, which is stable and less toxic than alkali cyanide - Google Patents

Cyanide standard soln. contg. complex cyanide, pref. tetra:cyano-zincate - easily releasing cyanide, which is stable and less toxic than alkali cyanide

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Publication number
DE4113212A1
DE4113212A1 DE4113212A DE4113212A DE4113212A1 DE 4113212 A1 DE4113212 A1 DE 4113212A1 DE 4113212 A DE4113212 A DE 4113212A DE 4113212 A DE4113212 A DE 4113212A DE 4113212 A1 DE4113212 A1 DE 4113212A1
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Germany
Prior art keywords
cyanide
soln
stable
pref
complex
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.)
Withdrawn
Application number
DE4113212A
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German (de)
Inventor
Roland Bitsch
Helmut Bernius
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Merck Patent GmbH
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Merck Patent GmbH
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Application filed by Merck Patent GmbH filed Critical Merck Patent GmbH
Priority to DE4113212A priority Critical patent/DE4113212A1/en
Priority to ITRM920286A priority patent/IT1254324B/en
Priority to FR9204844A priority patent/FR2675905A1/en
Priority to NL9200732A priority patent/NL9200732A/en
Priority to JP4129347A priority patent/JPH05193929A/en
Publication of DE4113212A1 publication Critical patent/DE4113212A1/en
Withdrawn legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/50Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
    • G01N33/96Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing involving blood or serum control standard

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  • Life Sciences & Earth Sciences (AREA)
  • Hematology (AREA)
  • Engineering & Computer Science (AREA)
  • Molecular Biology (AREA)
  • Biomedical Technology (AREA)
  • Chemical & Material Sciences (AREA)
  • Immunology (AREA)
  • Urology & Nephrology (AREA)
  • Biotechnology (AREA)
  • Biochemistry (AREA)
  • Cell Biology (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Microbiology (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Pathology (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Cyanide standard soln. (I) contains complex cyanide (II). Pref. (II) consists of a complex cyanide of Zn, Ni or Cd, pref. an alkali metal tetracyanozincate. USE/ADVANTAGE - (I) is stable in storage and less toxic than the alkali metal cyanides normally used. The cyanide is in easily released but stable form. In an example, 1.25 g(19.2 mmole) KCN were dissolved in ca. 500 ml. distilled water, than 1.127 g (9.6 mmole) Zn(CN)2 were added and the soln. was made up to 11 with distilled water. The Zn(CN)2 was dissolved by stirring and any undissolved fraction was filtered off. The cyanide content was determined by argentometric titration in alkaline medium, using potentiometric indication with a Ag electrode. 1 ml AgNO3 soln. 0.1 mole/1 = 5.2036 mg CN-. Solns. with definite contents were prepd. from the stock soln. by diluting an aliqu

Description

Die Erfindung betrifft lagerstabile Cyanidstandardlösungen. Wäßrige Lösungen von Cyaniden, insbesondere von Alkalicyani­ den, sind nicht über längere Zeit stabil. Durch Oxidation, Wechselwirkung mit dem Kohlendioxid der Luft, aber auch durch Lichteinwirkung, verändert sich der Gehalt der Lösungen, abhängig von der Konzentration der Lösung an Cyanidionen, sehr schnell.The invention relates to storage-stable cyanide standard solutions. Aqueous solutions of cyanides, especially alkali cyanide are not stable over a long period of time. Through oxidation, Interaction with the carbon dioxide in the air, but also through Exposure to light, the content of the solutions changes, depending on the concentration of cyanide ions in the solution, very fast.

In der Analytik werden häufig Lösungen mit definiertem Gehalt als Standardlösungen zu Kalibrierzwecken benötigt. Hierzu wird eine Urtitersubstanz genau bekannten Gehaltes eingewogen und in einem bekannten Volumen Wasser gelöst. Im Falle des Cyanids werden hierzu in der Regel die leicht löslichen Alkalicyanide verwendet. Es muß also eine stark giftige Substanz gehandhabt werden, um eine Lösung mit definiertem Gehalt an Cyanid herzustellen. Diese Lösungen sind, je nach der Konzentration an Cyanid, nur über einen relativ kurzen Zeitraum stabil, insbesondere wenn die Cyanidkonzentration im bereich von mg/l liegt.In analytics, solutions with a defined content are often used required as standard solutions for calibration purposes. For this an original titer substance is weighed out with a precisely known content and dissolved in a known volume of water. In the case of For this purpose, cyanides are usually the most easily soluble Alkali cyanides used. So it must be a highly toxic one Substance can be handled to a solution with defined Cyanide content. These solutions are, depending on the concentration of cyanide, only over a relatively short one Period stable, especially when the cyanide concentration in the range of mg / l.

Der Erfindung liegt die Aufgabe zugrunde, eine lagerstabile Cyanidstandardlösung zur Verfügung zu stellen, die auch weniger giftig ist als das bisher zu diesem Zweck verwendete Alkalimetallcyanid. The invention has for its object a storage stable To provide cyanide standard solution that too is less toxic than that previously used for this purpose Alkali metal cyanide.  

Überraschenderweise wurde gefunden, daß bestimmte komplexe Cyanide diese Forderungen erfüllen.Surprisingly, it has been found that certain complex Cyanides meet these requirements.

Gegenstand der Erfindung ist eine Cyanidstandardlösung, die durch einen Gehalt an komplexen Cyaniden gekennzeichnet ist.The invention relates to a cyanide standard solution which is characterized by a content of complex cyanides.

Lösungen von Cyanokomplexen mit geringer Komplexstabilität, d. h. freien Cyanidionen, weisen eine hohe Stabilität bezüglich der Cyanidionenkonzentration auf. Vorzugsweise wäßrige Lösungen von komplexen Cyaniden von Zink, Nickel und Cadmium, insbesondere Alkalimetalltetracyanozinkat, zeigen auch nach längerer Lagerung eine ausgezeichnete Stabilität. Dies trifft sowohl für konzentrierte Lösungen (1-20 g/l Cyanid) als auch für verdünnte Lösungen im Bereich von etwa 500 mg/l Cyanid zu.Solutions of cyano complexes with low complex stability, d. H. free cyanide ions, have high stability regarding the cyanide ion concentration. Preferably aqueous solutions of complex cyanides of zinc, nickel and Cadmium, especially alkali metal tetracyanozinkat show excellent stability even after prolonged storage. This applies to both concentrated solutions (1-20 g / l Cyanide) as well as for dilute solutions in the range of about 500 mg / l cyanide too.

Neben Zink, Nickel und Cadmium bilden eine Reihe von Metallen ebenfalls komplexe Cyanide, wie z. B. Silber, Eisen, Quecksil­ ber, Kupfer, Cobalt usw. Diese sind jedoch teilweise so stabil, daß sich sowohl das Metall als auch das Cyanid dem Nachweis entziehen.In addition to zinc, nickel and cadmium, a number of metals form also complex cyanides, such as. B. silver, iron, mercury About copper, cobalt, etc. However, some of them are stable that both the metal and the cyanide Withdraw proof.

DIN 38 405, Teil 13, unterscheidet zwischen leicht freisetzba­ rem Cyanid und Gesamtcyanid. Leicht freisetzbar ist alles Cyanid, das bei einem pH-Wert von 4 mit dem beschriebenen Verfahren direkt bestimmt werden kann. Die Bestimmung des Gesamtcyanids erfordert einen Aufschluß durch Kochen mit verdünnter Salzsäure in Gegenwart von Kupfer(I)-Ionen.DIN 38 405, part 13, differentiates between easily releasable Rem cyanide and total cyanide. Everything is easy to release Cyanide, which is at a pH of 4 with that described Procedure can be determined directly. The determination of the Total cyanide requires digestion by cooking with dilute hydrochloric acid in the presence of copper (I) ions.

Für die erfindungsgemäßen Cyanidstandardlösungen muß das Cyanid in leicht freisetzbarer aber lagerstabiler Form vor­ liegen. Diese Voraussetzung wird von Lösungen der komplexen Cyanide von Nickel, Cadmium und Zink besonders gut erfüllt. Im Hinblick auf die zusätzliche Umweltbelastung durch Nickel und Cadmium wird zur Herstellung dieser Lösungen vorzugsweise das Zinksalz verwendet.For the standard cyanide solutions according to the invention Cyanide in an easily releasable but storage stable form lie. This requirement is met by solutions of complex  Nickel, cadmium and zinc cyanides particularly well met. With regard to the additional environmental pollution caused by nickel and cadmium is preferred for the preparation of these solutions uses the zinc salt.

Beispielexample Herstellung einer CyanidstandardlösungPreparation of a standard cyanide solution

In einem 1-1-Meßkolben werden 1,25 g (19,2 mmol) Kaliumcyanid in ca. 500 ml dest. Wasser gelöst. Anschließend gibt man 1,127 g (9,6 mmol) Zn(CN)2 hinzu und verdünnt mit dest. Wasser bis zur Eichmarke. Das Zn(CN)2 wird unter Rühren gelöst. Eventuell ungelöste Anteile werden über ein Faltenfilter abfiltriert. Der Cyanidgehalt der Lösung wird durch argen­ tometrische Titration mittels potentiometrischer Indikation im alkalischen Medium bestimmt. Elektrode: Silber-Einstab- Meßkette. 1 ml AgNO3-Lösung 0,1 mol/l = 5,2036 mg CN-. Aus der Stammlösung können durch Verdünnung eines Aliquots Lösungen definierten Gehaltes hergestellt werden.1.25 g (19.2 mmol) of potassium cyanide in approx. 500 ml of dist. Water dissolved. Then add 1.127 g (9.6 mmol) of Zn (CN) 2 and dilute with dist. Water up to the calibration mark. The Zn (CN) 2 is dissolved with stirring. Any undissolved portions are filtered off using a pleated filter. The cyanide content of the solution is determined by argentometric titration using potentiometric indication in an alkaline medium. Electrode: silver single-rod electrode. 1 ml AgNO 3 solution 0.1 mol / l = 5.2036 mg CN-. Defined content can be prepared from the stock solution by diluting an aliquot of solutions.

Claims (3)

1. Cyanidstandardlösung, gekennzeichnet durch einen Gehalt an komplexen Cyaniden.1. Cyanide standard solution, characterized by a content of complex cyanides. 2. Cyanidstandardlösung nach Anspruch 1, gekennzeichnet durch einen Gehalt an komplexen Cyaniden von Zink, Nickel oder Cadmium.2. cyanide standard solution according to claim 1, characterized due to the content of complex cyanides of zinc, nickel or cadmium. 3. Cyanidstandardlösung nach den Ansprüchen 1 und 2, gekenn­ zeichnet durch einen Gehalt an Alkalimetalltetracyano­ zinkat.3. cyanide standard solution according to claims 1 and 2, marked characterized by a content of alkali metal tetracyano zincate.
DE4113212A 1991-04-23 1991-04-23 Cyanide standard soln. contg. complex cyanide, pref. tetra:cyano-zincate - easily releasing cyanide, which is stable and less toxic than alkali cyanide Withdrawn DE4113212A1 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
DE4113212A DE4113212A1 (en) 1991-04-23 1991-04-23 Cyanide standard soln. contg. complex cyanide, pref. tetra:cyano-zincate - easily releasing cyanide, which is stable and less toxic than alkali cyanide
ITRM920286A IT1254324B (en) 1991-04-23 1992-04-17 CYANIDE SAMPLE SOLUTIONS STABLE FOR STORAGE
FR9204844A FR2675905A1 (en) 1991-04-23 1992-04-21 STANDARD CYANIDE SOLUTIONS STABLE ON STORAGE.
NL9200732A NL9200732A (en) 1991-04-23 1992-04-22 STORAGE STABLE CYANIDE STANDARD SOLUTIONS.
JP4129347A JPH05193929A (en) 1991-04-23 1992-04-23 Standard solution of cyanide stable to storage

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE4113212A DE4113212A1 (en) 1991-04-23 1991-04-23 Cyanide standard soln. contg. complex cyanide, pref. tetra:cyano-zincate - easily releasing cyanide, which is stable and less toxic than alkali cyanide

Publications (1)

Publication Number Publication Date
DE4113212A1 true DE4113212A1 (en) 1992-10-29

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DE4113212A Withdrawn DE4113212A1 (en) 1991-04-23 1991-04-23 Cyanide standard soln. contg. complex cyanide, pref. tetra:cyano-zincate - easily releasing cyanide, which is stable and less toxic than alkali cyanide

Country Status (5)

Country Link
JP (1) JPH05193929A (en)
DE (1) DE4113212A1 (en)
FR (1) FR2675905A1 (en)
IT (1) IT1254324B (en)
NL (1) NL9200732A (en)

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE782831A (en) * 1971-05-05 1972-08-16 Paris Rene A NEW COMPLEX METALLIC CYANIDES
US3850761A (en) * 1973-03-01 1974-11-26 Orion Research Cyanide decomplexing
US4026790A (en) * 1975-03-07 1977-05-31 The United States Of America As Represented By The United States Energy Research And Development Administration Removal of Zn or Cd and cyanide from cyanide electroplating wastes
CH621367A5 (en) * 1977-07-08 1981-01-30 Systemes Traitements Surfaces Electrolytic bath for plating gold-copper-cadmium alloys and its use in galvanoplasty
JPS635239A (en) * 1986-06-25 1988-01-11 Seiko Instr & Electronics Ltd Zinc-cadmium composite standard solution for atomic absorptiometric analysis

Also Published As

Publication number Publication date
ITRM920286A1 (en) 1993-10-17
IT1254324B (en) 1995-09-14
JPH05193929A (en) 1993-08-03
NL9200732A (en) 1992-11-16
FR2675905B1 (en) 1997-02-21
FR2675905A1 (en) 1992-10-30
ITRM920286A0 (en) 1992-04-17

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