GB2227314A - Preparing reagent indicator paper - Google Patents
Preparing reagent indicator paper Download PDFInfo
- Publication number
- GB2227314A GB2227314A GB8830326A GB8830326A GB2227314A GB 2227314 A GB2227314 A GB 2227314A GB 8830326 A GB8830326 A GB 8830326A GB 8830326 A GB8830326 A GB 8830326A GB 2227314 A GB2227314 A GB 2227314A
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- United Kingdom
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- paper
- reagent
- indicator
- iron
- indicator paper
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- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
- G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
- G01N33/84—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing involving inorganic compounds or pH
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- Chemical & Material Sciences (AREA)
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- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Hematology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Urology & Nephrology (AREA)
- Pathology (AREA)
- Physics & Mathematics (AREA)
- Biomedical Technology (AREA)
- Inorganic Chemistry (AREA)
- Cell Biology (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
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- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Description
1 METHOD OF PREPARING REAGENT INDICATOR PAPER The present invention
relates to the art of analytical chemistry and, more particularly, to reagent indi- cator papers and may be useful for a rapid determination of microamounts of the total of bi- and trivalent iron ions.
Known In the art is a method of preparing a reagent indicator paper 11Merckoquant iron-(Pe2+) -test" for a semiquantitative determination oj-" iron (II) with the paper colour change into red by way of fixation, on the paperg of 2,21-bipyridine and a buffer substance, followed by drying (FRGReagenzien Merekoquant Test zur halbquantitativen Bestimung von Ionen und Verbindungen.
Darmstadt$ 19829 p.23).
According to this method, the ultimate detected content of Iron (II) Ions Is 3x10 -4 % by mass. This method, due to the adsorptive'fixation of the reagent on the paper, does not ensure an adequate strength of their retention under different conditions of the contact of the reagent paper with the analyzed solution which, in turn, does not make it possible to attain a lower limit of determination of iron (II) (1-5)x10-511"0 In effluents and natural waters. as well as in process solutions. Furthermore 2,21-bipyridine does not make it possible to determine ions of iron (III) which should be preferably converted to iron (II) ions by means of ascorbic acid; thirdly, the resulting reagent indicator paper is not sufficiently selective, since it also gives colour reactions with copper (II),cobalt(I1), and vanadyl (II).
Known in the art is a method for preparing a reagent indicator paper comprising treatment of a chromatographic paper with a solution of Oupferron for the determination of iron (III)q followed by drying and cutting into strips (Abstract Journal 'Thimiya", No.1919679 VINITI, Moscow; Japanese Patent No. 18298, No.1 G 24 P).
The main drawback of this method for preparing a reagent indicator paper resides in that use is made of a non-selective reagent Cupferron whichq apart from iron (III). forms intracomplex compounds with copper, aluminium, bismuth, mercury, manganese, niobium, tin, thorium, titaniums vanadium, zirconium and others. For this reason, the interfering metals should be masked.
Known in the art is a method of preparing a reagent paper comprising treatment of a modified chromatographic paper based on aldehyde cellulose with a solution of hydrazine derivative (heterylhyclrazine) and then with an aromatic amine in dimethylformamide and an aqueous buffer solution (SU, Ay 1178819). By means of the reagent paper produced by this method it is possible to determine iron with the ultimate detection of 0. 5 mg/1 (5x10-5,,:'.).
A disadvantage of this method for the preparation of a reagent indicator paper resides in that it does not ensure the production of a reagent indicator paper with a high selectivity and a low limit of detection of iron (II,III) ions, since the reagent paper forms intensi.rely coloured and durable complexes with a number of other metals. Thus, a reagent paper based on 4 1(5)-phenyl-(5-b.romopyrimidin-2-yl)-formazan-6-cellulose has a yellow colour and forms complexes with iron (I1) of a brown colour, with iron (III) - beige. with copper blue, palladium - green, mercury brick-brown. cobalt grey colour. These metals disturb the determination of iron. The reactive paper based on 1-(5)-phenyl-[4-(2hydroxyphenyl)-pyrimidin-6-yll-formazan- 6-cellulose forms at a pHa.,5 with iron (II) a compound of a brown colourlwith iron (III) - a light-brown compound, but this reaction is disturbed by ions of metals with which the reagent paper forms intensively coloured and more durable compounds: at a pH;,- 1 with palladium - a compound of green colour; at a pHasl.5 with copper - a dark- blue compound; at a pH-.r-2 with mercury (II) - a red- -brown compound; at a pH-Y 4 with cobalt - a grey-brown compound; at a pH. > 5 with nickel - a brown colour, with zinc - a red-brown compound-.
It is an object of the present invention to provide a reagent indicator paper with a high selectivity and a low limit of detection of iron (II,III) ions and to simplify the process of its preparation.
This object is accomplished by that in a process for preparing a reagent indicator paper comprising treatment of a modified chromatographic paper based on aldehyde cellulose with a solution of a derivative of hydrazine, washing and drying thereof, in accordance with the present invention, as the derivative of hydrazine use is made of its derivatives of the -eneral formula:
A-NM2 9 wherein:
r, H A N C, C C, - N 0C N H 0 / cl 0 0 R ct wherein: R, R RJ, OWN R' M. PA CH The method according to the present invention makes it possible to produce a reagent indicator paper."
with a high selectivity relative to iron (II and III) ions within different pH ranges and with the limits of detection of ions of iron (11) and (III) of at least 0.5 mg/l (5x10-576) and to simplify the process for the preparation of a reagent indicator paper due to the elimination of the additional stage of the treatment of a reagent paper with dilazotated amine.
Furthermoreg the method according to the present invention makes it possible to use thrice a spent re- action solution of the derivative Of hydrazine without impairing quality of the resulting reagent paper.Owing to a covalent fixation of chromogenous analytical rea- gent3employed in the method according to the present invention - nitrogen-containing heterocyclic compounds.
It becomes possible to selectiveY concentrate iron (11,111) ions which, in turng makes it possible to extend the limits of their detection to 0.1-0.2 mg/1 (1x10-5 to 2x10-5-0).
t 1 The methid according to the present invention Is implemented in the following manner.
Into a reactor a modified chromatographic paper based on aldehyde cellulose is charged, poured with a solution of a derivative of hydrazine employed in the method according to the present invention having the general formula:
A-NWR2, wherein:
c HA cl 0 c A=0 H C-CJ HC N.,.-he--ein:
HC the mixture is allowed to stand, the solution is decan ted, the paper is successively washed with distilled water,acetone ethanol and dried.
The resulting reagent indicator paper is tested for its metal-indicator properties. The thus-produced reagent indicator paper forms coloured compounds only with iron ions.
For a better understanding of the present inventi on some specific examples illustrating the embodiments of the method for preparing a reagent indicator paper are given hereinbelow.
Example 1 g of a modified chromatographic paper based on monoaldehyde cellulose are placed into a titanium reac tor, poured with a solution of 0.3 g of 2-hydrazino- CH 1, c H 0 b -5,7-dichloro-8-quinolinol (M.p. 217OC) and 200 ral of dimethylformamide and allowed to stand overnight. The solution Is decanted, the paper is successively washed three times with distilled waterl acetone, ethanol, dried in the air or in a drying cabinet at a temperature -of up to 6000 to obtain a reagent paper of a pale-yellow colour which is tested for metal-indicator properties. The test results are shown in the Table hereinbelow. Example 2 A reagent indicator paper is produced as in Example 1, but 2.5 g of P modified chromatographic paper are treated with a solution of 0.1 g of 2-hydrazino-4-phenyl-8- quinolinol (m.p. 167-17UOG) in 50 ml of a 2.5% acetic acid to obtain a reagent paper of a light-yellow paper which is tested for metal-indicator properties as in Example 1. The test results are shown in the Table hereinbelow. Example 3 A reagent indicator paper is pl?oduced in a manner similar to that described in Example 1 hereinbefore, except that it is treated with a solution of 2-hydrazino-4-phenylpyrimidine-6-carboxylic acid (m.p. 214-216OC) in dimethylformamide. The paper has a paleyellow colour. Its metal-indicator properties are tes- ted as in Example 1. The test results are shown in the Table hereinbelow. Example 4 A reagent indicator paper is pruduced as in Example! -1 C with the only difference that it is treated with a solution of 2- hydrazino-4-(4-methoxyphenyl)-pyrimidine-6-carboxylic acid (m.p. 213- 21700) in dimethylformamide.
The paper has a light-yellow colour. It is tested for metal-indicator properties in a manner similar to that described in Example 1. The test results are shown in the Table hereinbelow.
Example 5
A reagent paper is produced as in Example 2 herein before,except that it is treated with a solution of 4 hydroxy-l-oxo-192-dehydroisoquinoIY1-3-carbohyd.razide (1 g, ra.p. 261-2630C. decomposition temperature 310C) in 360 mI of dimethylformamide. The paper has a light yellow colour, when treated with a solution of pH 13 it changes its colour into light-brown. The paper is subjected to tests for its metal-indicator properties as in Example 1. The test results are shown in the Table hereinbelow.
Example 6
A reagent indicator paper is produced in a manner similar to that described in Example 1. except that it is treated with a solution of 1 g of 1-oxo-4-chloro 112-dihydroisoquinolYl-3-carbohydrazide (m.p. 225 -227OC) in 180 mi of dimethylformamide in a mixture with 20 ml of ethanol and 10 al of water. A white paper is obtained (at pH 13 it changes its colour into yellow) and its metal-indicator properties are tested as described in Example 1. The test results are shown in the Table hereinbelow.
Example 7 A reagent indicator paper is prepared in a manner similar to that described in Example 1 hereinbefore and tested for metal- indicator properties by way of sucking through it 5 ml of potable water with tle pH of 6. If no grey-green spot of the diameter of 6 mm Is formed on the paperl the content of iron is less than 0.1 mg/1. The concentration of iron ions of 0.1 mg/1 and over is determined against the comparison colour scale.
Example 8 A reagent indicator paper is produced in a manner similar to that of Example 1 and tested for metal-indicator properties in analysis of washing waste water containing hydrochloric acid and dissolved boiler sediments after washing thereof (pH of 1-2) by placing a strip of the reagent paper into the washing waste water for 3---4seconds, followed by keeping it in the air for 2 minutes. The concentration of iron ions ranging from 10 mg/1 to 200 mg/1, is determined against the colour comparison scale.
Z.
T A B L B Comparison of a number of reagent papers for selectivity and ranges of detection of iron ions Reagent-indicator Colour of Colour of its com- Limits of detect- Disturbing No. paper reagent indi- _Plexes with ion. mgll effect of cator paper 2+ 3+ 2+ 3+ other ca- Fe Fe Fe Fe tions at the specified - PR- 1. Reagent indicator pa er "Merekoquant iron(FeMwhite -test" 2. Reagent indicator paper dark of Sug A 1178819 yellow 3. Reagent indicator paper pale- of Example 1 yellow deep red white 3 brown light- brown grey- grey- green green 0.5 0.5 pH=4-5 0.2 0.2 pH=3-6 interfere: copperocobalt,Yanadium copper-co- ebuarlyt. mzierepalladium Xn do not interfere:copper. cobalttmercury. zinc 9 palladium 4. Reagent indicator paper light grey- grey of Example 2 yellow green green. 0.5 PH=5-8 0.5 ditto lighter Reagent indicator paper pele- light- light- 0.25 0.5 ditto of Example 3 yellow brown brown pH=3-5 00I11 TABLE (cont.)
Colour of Colour of its com- Limits of detect- Disturbing No. Reagent-indicator reagent indi- plexes with ion, mg11 effect of paper cator paper 2+ 3+ other ca- Fe Fe Pe 2+ Fe3+ tions at the specif ied 6. Reagent indicator light- light- light- 0.25 0.5 do not inter paper of Example 4 yellow claret- claret fere:copper, orange orange PH=3-5 cobaltmercu- ry. zinc. palla- dium A Reagent indicator light- dark- dark0.25 0.5 -1 ditto 0 paper of Example 5 yellow grey grey PH=3-5 1 8. Reagent indicator white grey- grey- 0.25 0.25 ditt o paper of Example 6 violet violet PH=3-5 0
Claims (2)
1. A method of preparing a reagent indicator paper comprising treating a modified chromatographic paper based on aldehyde cellulose with a solution of a 1:ydra zine derivative. washing and drying, wherein as the hyd.razine derivative compounds are used, having the general formula: ANHNH29 wherein cl CZ---.
N11 if NI 'I N R 1 R Z.
c HG 014 where R, R1 are H. Cl; R2 is H, Ph.
2.k method of preparing.a reagent indicator paper according to Claim 1, substantially as described in the Specification and Examples herei. nbefore.
Published 1990 at The Patent Office. State House. 66 71 High Holborn. London WC1 R 4TP Purther copies maybe obtainedfrom The Patent Office Sales Branch. St Ma...y Crky. Orpington. Kent ERS 3Rr Printed bY Mult, Plex techniques ltd. St Mary Cray. Kent C= 2 8' - -- -- ------ --- -- - -, 11.). -- le- -. 1
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB8830326A GB2227314A (en) | 1988-12-29 | 1988-12-29 | Preparing reagent indicator paper |
| DE19893902453 DE3902453A1 (en) | 1988-12-29 | 1989-01-27 | METHOD FOR PRODUCING REAGENT PAPER |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB8830326A GB2227314A (en) | 1988-12-29 | 1988-12-29 | Preparing reagent indicator paper |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| GB8830326D0 GB8830326D0 (en) | 1989-02-22 |
| GB2227314A true GB2227314A (en) | 1990-07-25 |
Family
ID=10649231
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB8830326A Withdrawn GB2227314A (en) | 1988-12-29 | 1988-12-29 | Preparing reagent indicator paper |
Country Status (2)
| Country | Link |
|---|---|
| DE (1) | DE3902453A1 (en) |
| GB (1) | GB2227314A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160074379A1 (en) * | 2009-06-26 | 2016-03-17 | Northeastern University | Antimicrobial Compounds |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1178819A1 (en) * | 1981-07-10 | 1985-09-15 | Предприятие П/Я А-7815 | Method of producing reaction paper |
| EP0248312A1 (en) * | 1986-06-04 | 1987-12-09 | Bayer Ag | 4,6-Dinitro benzothiazolone-2-hydrazones |
-
1988
- 1988-12-29 GB GB8830326A patent/GB2227314A/en not_active Withdrawn
-
1989
- 1989-01-27 DE DE19893902453 patent/DE3902453A1/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1178819A1 (en) * | 1981-07-10 | 1985-09-15 | Предприятие П/Я А-7815 | Method of producing reaction paper |
| EP0248312A1 (en) * | 1986-06-04 | 1987-12-09 | Bayer Ag | 4,6-Dinitro benzothiazolone-2-hydrazones |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160074379A1 (en) * | 2009-06-26 | 2016-03-17 | Northeastern University | Antimicrobial Compounds |
Also Published As
| Publication number | Publication date |
|---|---|
| DE3902453A1 (en) | 1990-08-02 |
| GB8830326D0 (en) | 1989-02-22 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| WAP | Application withdrawn, taken to be withdrawn or refused ** after publication under section 16(1) |