CN1090045A - A kind of method of measuring silicone content - Google Patents
A kind of method of measuring silicone content Download PDFInfo
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- CN1090045A CN1090045A CN 93100640 CN93100640A CN1090045A CN 1090045 A CN1090045 A CN 1090045A CN 93100640 CN93100640 CN 93100640 CN 93100640 A CN93100640 A CN 93100640A CN 1090045 A CN1090045 A CN 1090045A
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- chemiluminescence
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- silicone content
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Abstract
A kind of method of measuring silicone content, this method is based on chemiluminescence principle, adopts to contain the oxygen organic solvent and activate chemical reaction between water sample to be measured and detectable solution, forms binary or the siliceous system of ternary heteropoly acid fast, oxidation luminol or derivatives thereof produces chemiluminescence reaction.The present invention can add chemiluminescence intensifier simultaneously.This method has overcome that the check and analysis time that the traditional chemical luminescence method exists is long, and the shortcoming that sensitivity is low can make and detect 4～5 times of light intensity peak raisings, and detectability is 0.5 μ g/l.And it is good in 0～50 μ g/l scope internal linear.The present invention is suitable for detecting silicone content in steam, water and the metal, and testing process can in seconds be finished.
Description
The present invention relates to a kind of method of measuring silicone content, particularly relate to dioxide-containing silica in chemiluminescence fast measuring steam, water and the metal.
The method of silicone content is to adopt molybdenum Huang or molybdenum blue spectrophotometric method to detect in the known mensuration water.The lower limit that this kind method detects silicone content is generally 2 μ g/l, and need 15 minutes the analysis time of detection.
The method of silicone content is a chemoluminescence method in the another kind of detection water of using always, and the mode of this method employing has two kinds at present:
1. the silicomolybdic acid oxidation luminol with oxidation activity that utilizes silicate to form produces the content of chemical luminescent detecting silicon.The method in " analytical chemistry magazine " (the 585th page of 45 3 phase of volume of nineteen ninety) that USSR (Union of Soviet Socialist Republics) is published play-by-play its detection method and result.Other has Soviet Union's country's certificate of invention (SU-1357841-A1) also to introduce a kind of method that detects silicone content with chemoluminescence method.The said method detectability is 2.5 μ g/l SiO
2, the check and analysis shortest time is 7～10 minutes.
2. utilize silicate catalysis ammonium molybdate iodine oxide ion to produce the free-iodine reaction, borrow the iodine oxidation luminol that produces to produce the content of silicon in the chemiluminescence analysis test sample.The method sees " metallurgical analysis " (rolling up 7 pages of the 5th phases in 1988 the 8th), and its detectability is 2 μ g/l SiO
2, the analysis time that needs is longer, and wherein making iodide ion be oxidized to the free-iodine required time is 15 minutes.
The method of above-mentioned two kinds of known detection silicone contents is finished by the particular detection device, not only exists the sampling check and analysis reaction time long, detects the big problem of amount time lag as a result, has detectability height, the low problem of detection sensitivity simultaneously.Said method is difficult to satisfy the requirement that industrial chemistry is analyzed grab sample analysis, fast measuring result.
In view of above-mentioned problems of the prior art, the present invention utilize the chemoluminescence method purpose be to provide a kind of can fast measuring water sample to be measured in the method for silicone content height.
The present invention is based on and adopts ammonium molybdate to make reagent to be mixed with certain density solution in advance, reacts with silicon in the water sample to be measured, generates the siliceous system of binary heteropoly acid.With this binary heteropoly acid oxidation luminol or derivatives thereof, promptly produce chemiluminescence, reach the purpose of measuring silicone content in the water sample by specific pick-up unit.Above-mentioned in the past analytical reactions required time is very long, reason is that the binary heteropoly acid required time that generates with this method is long, cause determination and analysis time and sample time between the two the interval long, the actual silicon content that measurement result can't in time reflect industrial flow at all brings inconvenience and problem to commercial production.The present invention is still based on above-mentioned chemiluminescence principle, different is can be used alone or as a mixture to contain molybdenum or vanadium-containing compound, and contain antimony-molybdenum or vanadium-molybdenum compound is done detectable, and in the solution that contains above-claimed cpd that prepare in advance, certain density, add an amount of oxygen organic solvent that contains, be mixed with mixed solution A.Mixed solution A and water sample to be tested are mixed, contain under the oxygen organic solvent activation, can rapid reaction generate binary or the siliceous system of ternary heteropoly acid, comprise silicon-molybdenum system, silicon-vanadium system, silicon-antimony-molybdenum or silicon-vanadium-molybdenum system above-mentioned.Just produce chemiluminescence with above-mentioned binary heteropoly acid or the siliceous system oxidation of ternary heteropoly acid luminol or derivatives thereof.More than two kinds of chemical reactions finish in moment.Therefore use the method for mensuration silicone content provided by the invention that shortened analysis time greatly, almost can make sample time and determination and analysis time synchronized, make testing result can reflect commercial production reality fully.The present invention provides a kind of simple and direct, method of testing accurately for timely, METHOD FOR CONTINUOUS DETERMINATION silicone content.
The present invention adopts containing the oxygen organic solvent and can adopting alcohols, ketone, ethers etc. of activation, methyl alcohol, ethanol, the propyl alcohol etc. of comprising commonly used.Adopt ketone or ethers to do when containing the oxygen organic solvent, should manage to make mixed solution A to keep evenly, and in time use.
Said method of the present invention is the silicone content in the fast measuring water sample to be measured in time, but as the chemoluminescence method of routine, above-mentioned chemiluminescence usually a little less than, often need could measure silicone content in the water sample by high-sensitive detecting instrument.In order to improve chemiluminescence intensity of the present invention, in above-mentioned reaction system, also can be simultaneously separately or mix and add rhodamine and derivant, cumarin and derivant thereof or fluorescent prime system and be listed as the solution B that the reinforcing agent as the chemiluminescence agent is mixed with, to improve above-mentioned chemiluminescence intensity, improve detection sensitivity of the present invention.
Measured result of the present invention, SiO
2Detectability can reach 0.5 μ g/l, with existing detection method relatively, sensitivity can improve several times, and the check and analysis time only be various solution incorporation times, in several seconds, can finish determination and analysis, hundreds of times of raising finding speeds.The concentration of various solution and addition should be adjusted with the silicone content height is an amount of in the water sample to be measured among the present invention.
Measure the specific embodiment and the analytical approach thereof of low silicon content in the water sample below in conjunction with said method introduction of the present invention.
1. reagent preparation
Solution A: get the 2g ammonium molybdate, the 40mg potassium antimony tartrate is dissolved in the 50ml high-purity water, treat that mentioned reagent all after the dissolving, adds the 40ml absolute ethyl alcohol, be diluted to 100ml with high purity water again and shake all, use dense H
2SO
4It is standby in the special syringe to transfer pH value to 2～4 to pack into.
Solution B:, add rhodamine and make that rhodamine content is 1 * 10 in the solution with the NaOH aqueous solution of high purity water preparation 0.5N
-3Mol/l, the back that is mixed is standby.
Solution C: the NaOH aqueous solution with high purity water preparation 0.5N, add luminol again, luminol content is 1 * 10 in the solution
-3Mol/l.Standby after being mixed.
Solution D: solution B and solution G were mixed in by volume 1: 1, standby in another special syringe of packing into.
2. analytical approach:
Get water sample 2ml to be measured, inject the luminescence-producing reaction ware of special chemiluminescence reaction detector, inject solution A 0.35ml earlier, inject solution D 1ml immediately rapidly.At this moment, the chemiluminescence reaction detector promptly demonstrates the peak value of luminous intensity, and the registering instrument that is connected with detector writes down luminous intensity-time curve simultaneously, can directly determine the silicone content of water sample to be measured by this curve.
This method detectability is 0.5 μ g/l, SiO
2Concentration has good linearity in 0～50 μ g/l scope, wherein contained Na in the solution
+, Cl
-, NH
+ 4Noiseless to testing result.Phosphate is to SiO
2Interference can adopt the method for known tartarize or citric acid or oxalic acid to make it to disturb greatly to reduce.
The use and the compound concentration of the above-mentioned all ingredients of the present invention do not have specific (special) requirements, and the method with the embodiment introduction is identical substantially, introduces no longer one by one for this reason.Chemiluminescence method provided by the present invention is applicable to and detects silicone content in steam, water and the metal.
Claims (5)
1, a kind of method of measuring silicone content, this method is at first utilized the silicon in the water sample to be measured and is mixed with certain density detectable solution reaction in advance, generate the siliceous system of polynary heteropoly acid, carry out oxidation reaction with the luminol or derivatives thereof again and produce chemiluminescence, it is characterized in that having added in the said detectable solution that is mixed with in advance and contain the oxygen organic solvent in right amount and make mixed solution A, activate the siliceous system reaction of the polynary heteropoly acid of above-mentioned generation.
2, by the described method of claim 1, it is characterized in that the said oxygen organic solvent that contains is alcohols, ketone and ethers, wherein methyl alcohol, ethanol, propyl alcohol are the most commonly used.
3,, it is characterized in that in said chemiluminescence reaction, having added the reinforcing agent solution B of chemiluminescence agent by the described method of claim 1.
4, by claim 1 or 3 described methods, the reinforcing agent solution B that it is characterized in that adding in the chemiluminescence agent is to adopt rhodamine and derivant, cumarin and derivant thereof or fluorescent prime system row formulated.
5,, it is characterized in that said detectable can be used alone or as a mixture and contain molybdenum or vanadium-containing compound, and contain antimony one molybdenum or contain vanadium one molybdenum compound by the described method of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93100640 CN1090045A (en) | 1993-01-05 | 1993-01-05 | A kind of method of measuring silicone content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93100640 CN1090045A (en) | 1993-01-05 | 1993-01-05 | A kind of method of measuring silicone content |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1090045A true CN1090045A (en) | 1994-07-27 |
Family
ID=4983156
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93100640 Withdrawn CN1090045A (en) | 1993-01-05 | 1993-01-05 | A kind of method of measuring silicone content |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105866110A (en) * | 2016-03-28 | 2016-08-17 | 同济大学 | Detection agent for determining content of silica in water |
-
1993
- 1993-01-05 CN CN 93100640 patent/CN1090045A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105866110A (en) * | 2016-03-28 | 2016-08-17 | 同济大学 | Detection agent for determining content of silica in water |
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| C53 | Correction of patent for invention or patent application | ||
| CB02 | Change of applicant information |
Address after: 116001 No. 78, Kunming street, Zhongshan District, Liaoning, Dalian Applicant after: Yu Desheng Address before: 116013, Liaoning, Zhongshan, Dalian province Jiefang Road unite good alley No. 22-2-2 Applicant before: Chen Yixin |
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