DE2546290A1 - Determination of chlorine in air - with the help of a silver chromate impregnated paper and prior removal of hydrogen sulphide and hydrogen cyanide from the gas - Google Patents
Determination of chlorine in air - with the help of a silver chromate impregnated paper and prior removal of hydrogen sulphide and hydrogen cyanide from the gasInfo
- Publication number
- DE2546290A1 DE2546290A1 DE19752546290 DE2546290A DE2546290A1 DE 2546290 A1 DE2546290 A1 DE 2546290A1 DE 19752546290 DE19752546290 DE 19752546290 DE 2546290 A DE2546290 A DE 2546290A DE 2546290 A1 DE2546290 A1 DE 2546290A1
- Authority
- DE
- Germany
- Prior art keywords
- hydrogen
- gas
- air
- silver chromate
- determination
- 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.)
- Pending
Links
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 title claims description 30
- 239000007789 gas Substances 0.000 title claims description 16
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims description 15
- OJKANDGLELGDHV-UHFFFAOYSA-N disilver;dioxido(dioxo)chromium Chemical compound [Ag+].[Ag+].[O-][Cr]([O-])(=O)=O OJKANDGLELGDHV-UHFFFAOYSA-N 0.000 title claims description 10
- 239000000460 chlorine Substances 0.000 title description 2
- 229910052801 chlorine Inorganic materials 0.000 title description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title 1
- 238000000034 method Methods 0.000 claims abstract description 19
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 12
- 229910000039 hydrogen halide Inorganic materials 0.000 claims description 9
- 239000012433 hydrogen halide Substances 0.000 claims description 9
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 150000004820 halides Chemical class 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000004458 analytical method Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000004868 gas analysis Methods 0.000 abstract 1
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 5
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000002452 interceptive effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- -1 hydrogen halides Chemical class 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002926 oxygen Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
- G01N31/223—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for investigating presence of specific gases or aerosols
- G01N31/224—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for investigating presence of specific gases or aerosols for investigating presence of dangerous gases
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Molecular Biology (AREA)
- Dispersion Chemistry (AREA)
- Biophysics (AREA)
- Toxicology (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
Verfahren zur Beseitigung des Störeinflusses von Schwefelwasser-Procedure for eliminating the interference of sulphurous water
stoff und Cyanwasserstoff bei der Silberchromatmeßmethode zur Erfassung der Halogenwasserstoffe HCl. HBr und HJ Die Erfindung betrifft ein Verfahren zur Beseitigung des Störeinflusses von Schwefelwasserstoff und Cyanwasserstoff bei der Silberchromatmeßmethode zur Erfassung der Halogenwasserstoffe flcl, HBr und HJ.substance and hydrogen cyanide for the determination of the silver chromate measuring method of the hydrogen halides HCl. HBr and HJ The invention relates to a method for Elimination of the interference of hydrogen sulfide and hydrogen cyanide in the Silver chromate measuring method for the determination of the hydrogen halides flcl, HBr and HJ.
In der Hauptanmeldung P 25 34 367.3 wird ein Verfahren zur Messung von Chlorgas-Spuren in Luft beschrieben, wobei sich ein mit Silberchromat Ag2CrO4 als Reagenzstoff imprägniertes Indikatorpapier auf Grund der Einwirkung der gasförmigen Halogenwasserstoffe HCl, HBr und HJ je nach Konzentration, Gasdurchsatz und Begasungszeit verfärbt und der Grad der Verfärbung ein Maß für deren Konzentration darstellt.In the main application P 25 34 367.3 a method for measurement of chlorine gas traces in air, whereby a silver chromate Ag2CrO4 Indicator paper impregnated as a reagent due to the action of the gaseous Hydrogen halides HCl, HBr and HJ depending on concentration, gas throughput and gassing time discolored and the degree of discoloration is a measure of their concentration.
Die Umsetzungen finden dabei nach folgenden Reaktionsgleichungen statt (X = Cl, Br oder J): Je nach Art und Konzentration des Halogenwasserstoffs treten Verfärbungen des Reagenzpapiers von rotbraun nach gelbweiß bis weiß auf.The reactions take place according to the following reaction equations (X = Cl, Br or J): Depending on the type and concentration of the hydrogen halide, the reagent paper changes color from red-brown to yellow-white to white.
Es hat sich gezeigt, daß das mit Silberchromat imprägnierte Reagenzpapier auch auf Schwefelwasserstoff H2S und Cyanwasserstoff HCN empfindlich reagiert. Dadurch wird eine Verfärbung bewirkt, die beim H2S dem Halogenwasserstoff-Meßwert entgegenwirkt und damit eine zu niedrige Halogenwasserstoffanzeige hervorruft oder sie gänzlich unterdrückt. HCN wirkt umgekehrt: es wird eine höhere Halogenwasserstoff-Konzentration vorgetäuscht.It has been shown that the test paper impregnated with silver chromate also reacts sensitively to hydrogen sulfide H2S and hydrogen cyanide HCN. Through this This causes a discoloration that counteracts the hydrogen halide measured value in the case of H2S and thus causes a hydrogen halide reading that is too low or completely suppressed. HCN works the other way round: there will be a higher concentration of hydrogen halide faked.
Die Reaktionsgleichungen der Störkomponenten H2S und HCN entsprechen den Gln. (1)+ Aufgabe der Erfindung ist es somit, ein Verfahren zu schaffen, bei dem die Störeinflüsse von Schwefelwasserstoff H2S und Cyanwasserstoff HCN bei der Silberchromat-Meßmethode zur Erfassung der Halogenwasserstoffe HCl, HBr und HJ vermieden werden.The reaction equations of the interfering components H2S and HCN correspond the Eqs. (1) + The object of the invention is therefore to create a method for where the interfering influences of hydrogen sulfide H2S and hydrogen cyanide HCN in the Silver chromate measuring method for the detection of the hydrogen halides HCl, HBr and HJ avoided will.
Das erfindungsgemäße Verfahren muß folgenden Anforderungen genügen: 1. Die Cyanwasserstoff- bzw. die Schwefelwasserstoffanteile müssen entweder quantitativ aus dem Meßgas entfernt werden oder quantitativ in solche Verbindungen umgewandelt werden, die keine Verfärbung des mit Silberchromat imprägnierten Reagenzpapiers hervorrufen.The method according to the invention must meet the following requirements: 1. The hydrogen cyanide or hydrogen sulfide components must either be quantitative can be removed from the measurement gas or converted quantitatively into such compounds that do not discolour the test paper impregnated with silver chromate cause.
2. Die zu messenden Halogenwasserstoffanteile dürfen durch die Behandlung des Meßgases zwecks Beseitigung der Schwefelwasserstoff- bzw. Cyanwasserstoffanteile nicht beeinflußt werden. 2. The proportions of hydrogen halide to be measured are allowed to pass through the treatment of the measuring gas for the purpose of eliminating the hydrogen sulfide or hydrogen cyanide components are not influenced.
3. Das Verfahren soll möglichst ohne Reagenzien oder Reagenzlözungen arbeiten, so daß ein Ansetzen von Reagenzien bzw. 3. The procedure should be carried out without reagents or reagent solutions if possible work so that a preparation of reagents or
Reagenzlösungen und ein Nachfüllen von verbrauchten Reagenzien entfällt und nach dem Verfahren arbeitende Vorrichtungen somit wartungsarm sind. There is no need for reagent solutions or refilling of used reagents and devices operating according to the method are therefore low-maintenance.
Diese Aufgaben werden dadurch gelöst, daß das vom Schwefelwasserstoff bzw. Cyanwasserstoff zu befreiende,Halogenwassrstoff enthaltende Meßgas vor Eintritt in das Indikatorpapier-Analysengerät erhitzt und anschließend gekühlt wird.These objects are achieved in that the hydrogen sulfide or hydrogen cyanide to be freed and containing hydrogen halide before entry heated in the indicator paper analyzer and then cooled.
Vorzugsweise wird das Meßgas vor Eintritt in das Indikatorpapier-Analysengerät auf ca. 1200 K erwärmt.The measurement gas is preferably fed into the indicator paper analyzer before it enters heated to approx. 1200 K.
Im folgenden soll das Verfahren noch näher erläutert werden.The method is to be explained in more detail below.
Dem Verfahren liegt der Gedanke zugrunde, die störenden Meßgasbestandteile Schwefelwasserstoff und Cyanwasserstoff nach folgenden Reaktionen umzusetzen: Für zwei Raumteile Schwefelwasserstoff sind somit drei Raumteile Sauerstoff und für vier Raumteile Cyanwasserstoff neun Raumteile Sauerstoff zur vollständigen Oxidation erforderlich. Dieser Sauerstoffbedarf wird durch den Sauerstoffgehalt des Meßgases für H2S- und HCN-Konzentrationen im ppm-Bereich im allgemeinen gedeckt. Besonders geeignet ist das Verfahren zur Umsetzung von H2S- und HCN-Spuren bei der Halogenwasserstoff-Messung in Luft.The process is based on the idea of converting the interfering measuring gas components hydrogen sulfide and hydrogen cyanide according to the following reactions: For two parts of hydrogen sulfide, three parts of oxygen and four parts of hydrogen cyanide nine parts of oxygen are required for complete oxidation. This oxygen requirement is generally covered by the oxygen content of the measuring gas for H2S and HCN concentrations in the ppm range. The process is particularly suitable for converting traces of H2S and HCN when measuring hydrogen halide in air.
Die bei den Reaktionen (2) und (3) entstehenden Verbindungen C02, N02, S02 und H20 ergeben mit dem Silberchromat-Reagenzpapier keine Farbreaktion. Der im Meßgas vorhandene Halogenwasserstoff, z. B.The compounds C02 formed in reactions (2) and (3), N02, S02 and H20 do not produce a color reaction with the silver chromate test paper. The hydrogen halide present in the gas to be measured, e.g. B.
Chlorwasserstoff, wird durch den Erwärmungsprozeß nicht verändert und kann anschließend nach der Silberchromat-Methode mit dem Reagenzpapier-Gasanalysengerät gemessen werden.Hydrogen chloride, is not changed by the heating process and can then after the silver chromate method with the test paper gas analyzer be measured.
Damit das Analysengerät nicht mit den heißen Gasen in Berührung kommt, wird das Meßgas zuvor durch einen Glas-Luftkühler geleitet und wieder auf Raumtemperatur abgekühlt.So that the analyzer does not come into contact with the hot gases, the gas to be measured is previously passed through a glass air cooler and back to room temperature cooled down.
Für ein nach diesem Verfahren aufbereitetes Gasgemisch wird bei einer Chlorwasserstoff-Konzentration von 10 ppm in Luft und einem Gasdurchfluß von ca. 30 l/h eine Begasungszeit von 5 Minuten benötigt, um einen Vollausschlag des Papierband-Gasanalysengerätes zu erreichen.For a gas mixture prepared according to this process, a Hydrogen chloride concentration of 10 ppm in air and a gas flow of approx. 30 l / h a gassing time of 5 minutes is required to reach a full scale of the paper tape gas analyzer to reach.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19752546290 DE2546290A1 (en) | 1975-10-16 | 1975-10-16 | Determination of chlorine in air - with the help of a silver chromate impregnated paper and prior removal of hydrogen sulphide and hydrogen cyanide from the gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19752546290 DE2546290A1 (en) | 1975-10-16 | 1975-10-16 | Determination of chlorine in air - with the help of a silver chromate impregnated paper and prior removal of hydrogen sulphide and hydrogen cyanide from the gas |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE2546290A1 true DE2546290A1 (en) | 1977-04-21 |
Family
ID=5959259
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19752546290 Pending DE2546290A1 (en) | 1975-10-16 | 1975-10-16 | Determination of chlorine in air - with the help of a silver chromate impregnated paper and prior removal of hydrogen sulphide and hydrogen cyanide from the gas |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE2546290A1 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4650839A (en) * | 1986-01-23 | 1987-03-17 | Allied Corporation | Thermosettable modified phenolic imide resins |
| US4757118A (en) * | 1986-01-23 | 1988-07-12 | Allied Corporation | Thermosettable modified phenolic polyester imide resins |
| US4771113A (en) * | 1986-01-23 | 1988-09-13 | Allied Corporation | Thermosettable modified phenolic polyester imide resins |
-
1975
- 1975-10-16 DE DE19752546290 patent/DE2546290A1/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4650839A (en) * | 1986-01-23 | 1987-03-17 | Allied Corporation | Thermosettable modified phenolic imide resins |
| US4757118A (en) * | 1986-01-23 | 1988-07-12 | Allied Corporation | Thermosettable modified phenolic polyester imide resins |
| US4771113A (en) * | 1986-01-23 | 1988-09-13 | Allied Corporation | Thermosettable modified phenolic polyester imide resins |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| OHW | Rejection |