CN104142312A - Method for rapidly measuring content of silicon in catalyst - Google Patents
Method for rapidly measuring content of silicon in catalyst Download PDFInfo
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- CN104142312A CN104142312A CN201310657318.2A CN201310657318A CN104142312A CN 104142312 A CN104142312 A CN 104142312A CN 201310657318 A CN201310657318 A CN 201310657318A CN 104142312 A CN104142312 A CN 104142312A
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Abstract
The invention relates to a method for rapidly measuring the content of silicon in a catalyst. The method comprises the following steps: rapidly dissolving a catalyst sample and a high-purity silicon dioxide standard substance in an alkali solution at high temperature, adding an ethanol-acetone mixed solution serving as a stabilizer under an acidic condition, and then adding ammonium molybdate for color reaction so as to generate yellow silicon molybdenum yellow heteropolyacid; and performing reduction on silicon molybdenum yellow heteropolyacid to obtain silicon molybdenum blue heteropolyacid, making up to the constant volume, measuring the absorbancy at the wavelength of 810nm, and calculating the content of silicon in the sample according to a standard curve of silicon dioxide concentration and absorbancy value. Compared with a conventional silicon dioxide alkali fusion method, the method has the advantages that the sample treatment temperature is low, the treatment speed is high, and silicon in the catalyst is simply measured by a spectrophotometric method.
Description
Technical field
The present invention relates to catalyst chemical analysis examination survey technology field, the particularly rapid assay methods of silicone content in a kind of catalyzer.
Background technology
The analytical test of dioxide-containing silica is mainly divided into chemical analysis and instrumental analysis two class methods, instrumental analysis speed, but it is more difficult to face sample dissolution, and error and interference are larger, and making to measure directly and accurately dioxide-containing silica with instrument has great difficulty.At present, dioxide-containing silica analysis mainly still adopts chemical analysis, includes gravimetric method, volumetric method and colourimetry.Gravimetric method is converted into silicic acid sediment after being mostly with hydrofluorite or alkali, sample to be dissolved again, and high temperature sintering makes it to become SiO
2after weighing, measure content, operation steps is more, is not suitable for express-analysis and measures; Volumetric method generally first will be converted into silicon potassium fluosilicate precipitation, and this uses aqueous slkali titration after being deposited in the hydrofluorite that is hydrolyzed and generates respective quality in hot water, and operation requirements is high, and influence factor is more; Colourimetry can be divided into again molybdenum yellow and silicon molybdenum blue colourimetry, and the latter is more sensitive, and other chemical method operation stepss are few relatively for colourimetry, and method is simple, is generally applicable to the sample that silicone content is not high.
For the mensuration of dioxide-containing silica in catalyzer, also there is no at present corresponding standard method.Adopt colourimetry the silicone content in molecular sieve to be measured to (Zhang Zhi is red etc. though have been reported, Beijing Institute of Petrochemical Technology's journal, 2010,18(3): 43-46), but what in document, adopt is that sodium hydrate solid reacts the rear acid-soluble solution of using with sample for a long time at 150 DEG C, process more consuming time, not carefully operation may cause sample difficulty dissolve completely or lose.In addition, in colorimetric method for determining silicone content process, colour developing and method of reducing and condition are more, although existing a lot of successfully application in the silica test of the samples such as cement, pottery, metal alloy and water body, but directly measure and may cause larger measured deviation because of the difference of properties of samples with reference to these conditions in catalyzer, reduce the accuracy of result, therefore, need to set up the rapid assay methods of dioxide-containing silica in a kind of catalyzer.
Summary of the invention
Silicone content in catalyzer is measured with reference to the Determination of Silicon Content of the samples such as cement, pottery, metal alloy and water body for solving in above-mentioned prior art, may cause larger measured deviation because of the difference of properties of samples, reduce the accuracy of result, the invention provides the rapid assay methods of silicone content in a kind of catalyzer, to overcome the deficiency in existing the Determination of Silicon Content, realize the Accurate Measurement to silicone content in catalyzer.
The present invention is achieved through the following technical solutions:
A rapid assay methods for silicone content in catalyzer, comprises the following steps:
(1) dissolve high-purity silicon dioxide and the testing sample of drying with strong base solution;
(2) the silicon dioxide standard solution of absorption different volumes, develop the color and reduce, measure absorbance, and the reagent that deducts not add silicon dioxide standard solution develop the color as blank and reduce after measured absorbance as the actual absorbance of silicon dioxide standard solution, and draw the typical curve of silica concentration and actual absorbance;
(3) under same condition, use the method identical with step (2), draw appropriate testing sample lysate, develop the color and reduce, measure absorbance, and the reagent that deducts not add testing sample solution develops the color as blank and reduce the actual absorbance of measured afterwards absorbance as testing sample;
(4) look into silicon dioxide standard working curve according to the actual absorbance of testing sample solution, be converted into the percentage composition of silicon dioxide in testing sample.
Further, step (1) is specially:
The NaOH that is 20%～40% by mass concentration or potassium hydroxide solution in polytetrafluoroethylcontainer container with cover between 140 DEG C～250 DEG C, constant temperature 20min～30min dissolves respectively appropriate high-purity silicon dioxide and testing sample, to be cooled proceed to respectively during to normal temperature after 250mL plastics volumetric flask constant volume to be measured.
Further, step (2) is specially:
Use 1g/L silicon dioxide standard solution that calibrated pipettor draws respectively 0 μ L, 20 μ L, 40 μ L, 60 μ L, 80 μ L, 100 μ L, 150 μ L, 200 μ L, 300 μ L to 50mL plastics volumetric flask, adding respectively 4mL volume ratio is the absolute ethyl alcohol of 1:1 and the mixed solution of anhydrous propanone, and 4mL distilled water, regulate pH value to 0.9～1.5 of solution in each volumetric flask with the 6mol/L hydrochloric acid solution of 2mL, adding 3mL mass concentration is that 3% ammonium molybdate solution carries out chromogenic reaction again, after colour developing 15～40min, generates stable molybdenum yellow heteropoly acid;
Adding 2mL mass concentration to the solution in each volumetric flask of color stability is 2% ascorbic acid solution and the 6mol/L hydrochloric acid solution of 10～13mL, and adjusting acidity is 1.3 ~ 1.6mol/L, is diluted to scale mark, reductase 12 0min～1h;
Final solution through reduction constant volume in each volumetric flask is measured to absorbance record with absorption cell 810nm place on spectrophotometer of 1cm.
Further, in step (4), the computing formula of conversion silicon dioxide percentage composition is:
Wherein
c samplefor the unit being calculated by the typical curve linear equation sample concentration that is mg/L,
v samplethe sample solution volume that the unit pipetting for chromogenic reaction is mL,
m samplefor the weighed unit testing sample quality that is g.
The present invention can be dissolved sample with aqueous slkali within a short period of time fast, adopts the silicone content in silicon molybdenum blue colorimetry for quick analysis catalyzer, and sample preparation temperature is low, and method is reliable and stable, highly sensitive, measures the range of linearity wide, simple to operation.
Brief description of the drawings
Fig. 1 is the visible spectrum curve of the blue solution of medium-Si, Mo of the present invention;
Fig. 2 is concentration and the absorbance relation curve of silicon dioxide standard solution in the present invention.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
1, preparing experiment instrument and medicament:
Instrument: SPECORD 200 ultraviolet-visible pectrophotometers;
Medicament: 30% sodium hydroxide solution, 3% ammonium molybdate solution, 2% ascorbic acid solution, 6mol/L hydrochloric acid solution, 99.99% high-purity silicon dioxide, absolute ethyl alcohol and acetone.
2, prepare silicon dioxide standard solution and testing sample test solution:
Respectively high-purity silicon dioxide and testing sample are dried at 200 DEG C to 1h to stand-by in being placed on exsiccator after constant weight.
Accurately take the treated high-purity silicon dioxide of 0.25g, add teflon reactor and add a cover with together with 30% sodium hydroxide solution of 10mL, in 180 DEG C of baking ovens, place 30min, take out after cooling, add suitable quantity of water, add the 6mol/L hydrochloric acid solution of 20mL again, quantitatively proceed to constant volume in 250mL plastics volumetric flask, this solution is the silicon dioxide standard solution of concentration 1g/L.
Equally accurately take testing sample 0.25g, under the same conditions, after operating with step as stated above, be settled in 250mL plastics volumetric flask to be measured.
In above-mentioned course of reaction, reactant is silica solid and strong base solution reaction, and silicon dioxide molecules is converted into silicate.Molecule collision probability increase when reaction, compares conventional silicon dioxide and highly basic solid high-temperature fusion temperature of reaction reduces greatly, and reaction velocity speeds, and therefore the sample dissolution time shortens greatly, has saved whole analysis time.Use teflon reactor and plastics volumetric flask to ensure can not introduce the interference of silicate ion in sample dissolution and constant volume process, guarantee the accuracy of testing.
3, the drafting of typical curve:
Get the plastics volumetric flask of 9 50mL, use respectively calibrated pipettor accurately to draw the 1g/L silicon dioxide standard solution of 0 μ L, 20 μ L, 40 μ L, 60 μ L, 80 μ L, 100 μ L, 150 μ L, 200 μ L, 300 μ L, adding respectively 4mL volume ratio is that the absolute ethyl alcohol of 1:1 and the mixed solution of anhydrous propanone are as color stability agent, and 4mL distilled water, regulate the pH value to 1.2 of solution in each volumetric flask with the hydrochloric acid solution of 2mL 6mol/L, then develop the color with the ammonium molybdate solution that 3mL mass concentration is 3%, react as follows:
After colour developing 30min, the yellow silicomolybdic acid colour stable of generation is constant.Then adding 2mL mass concentration is 2% ascorbic acid solution and the 6mol/L hydrochloric acid solution of 10mL, is diluted to scale mark and reduces, and reacts as follows:
Reduce after 30min, using distilled water as reference, instrument is carried out to absorbance zeroing at mensuration wavelength place and proofread and correct, use the absorbance of absorption cell sequentially determining silicon dioxide standard solution in 810nm place on spectrophotometer of 1cm, this value can preserve value to stablize and not change.Fig. 1 is the visible spectrum curve of the blue solution of medium-Si, Mo of the present invention, and its maximum absorption wavelength is 810nm place.
Taking the mass concentration of the silicon dioxide in above-mentioned bioassay standard solution as horizontal ordinate, the actual absorbance not adding taking reducing of correspondence after the absorbance of blank reagent of silicon dioxide is ordinate, drawing standard curve.As shown in Figure 2.
The equation of linear regression of matching is:
A=0.2832C-0.0151
Wherein A is the actual absorbance of reducing after blank reagent absorbance, the concentration that C is testing sample: mg/L, linearly dependent coefficient R=0.9998.
4, sample determination
The testing sample solution of accurately drawing 0.10mL, is placed in after 50mL plastics volumetric flask, adds medicament to develop the color and reduces according to above-mentioned steps and consumption.Similarly, using distilled water as reference, instrument is carried out to absorbance zeroing at mensuration wavelength place and proofread and correct, use the absorption cell of 1cm to measure the absorbance of testing sample solution at 810nm place, and deduct blank reagent absorbance, as the actual absorbance of sample.
5, result is calculated
According to the equation of linear regression of the dioxide-containing silica in above-described embodiment and actual absorbance, calculate after the concentration of silicon dioxide in surveyed sample solution, calculate according to the following formula the quality percentage composition of silicon dioxide in institute's test sample product:
Wherein C
samplefor be mg/L sample concentration, the V of the unit being calculated by typical curve linear equation
samplethe sample solution volume that the unit pipetting for chromogenic reaction is mL, m
samplefor the weighed unit testing sample quality that is g.
Respectively two kinds of samples are measured according to the step and method of above-described embodiment, in two kinds of samples, silicon dioxide quality mark is listed in the table below:
| Catalyst sample | Silicon dioxide quality mark % | Relative standard deviation (n=5) % |
| Sample A | 85.95 | 0.32 |
| Sample B | 35.76 | 0.18 |
Claims (4)
1. the rapid assay methods of silicone content in catalyzer, is characterized in that, comprises the following steps:
(1) dissolve high-purity silicon dioxide and the testing sample of drying with strong base solution;
(2) the silicon dioxide standard solution of absorption different volumes, develop the color and reduce, measure absorbance, and the reagent that deducts not add silicon dioxide standard solution develop the color as blank and reduce after measured absorbance as the actual absorbance of silicon dioxide standard solution, and draw the typical curve of silica concentration and actual absorbance;
(3) under same condition, use the method identical with step (2), draw appropriate testing sample lysate, develop the color and reduce, measure absorbance, and the reagent that deducts not add testing sample solution develops the color as blank and reduce the actual absorbance of measured afterwards absorbance as testing sample;
(4) look into silicon dioxide standard working curve according to the actual absorbance of testing sample solution, be converted into the percentage composition of silicon dioxide in testing sample.
2. the rapid assay methods of silicone content in catalyzer according to claim 1, is characterized in that, described step (1) is specially:
Respectively high-purity silicon dioxide and testing sample are dried to constant weight at 200 DEG C, the NaOH that is 20%～40% by mass concentration or potassium hydroxide solution in polytetrafluoroethylcontainer container with cover between 140 DEG C～250 DEG C, constant temperature 20min～30min dissolves respectively appropriate high-purity silicon dioxide and testing sample, to be cooled proceed to respectively during to normal temperature after 250mL plastics volumetric flask constant volume to be measured.
3. the rapid assay methods of silicone content in catalyzer according to claim 1, is characterized in that, described step (2) is specially:
Use 1g/L silicon dioxide standard solution that calibrated pipettor draws respectively 0 μ L, 20 μ L, 40 μ L, 60 μ L, 80 μ L, 100 μ L, 150 μ L, 200 μ L, 300 μ L to 50mL plastics volumetric flask, adding respectively 4mL volume ratio is the absolute ethyl alcohol of 1:1 and the mixed solution of anhydrous propanone, and 4mL distilled water, regulate pH value to 0.9～1.5 of solution in each volumetric flask with the 6mol/L hydrochloric acid solution of 2mL, adding 3mL mass concentration is that 3% ammonium molybdate solution carries out chromogenic reaction again, after colour developing 15～40min, generates stable molybdenum yellow heteropoly acid;
Adding 2mL mass concentration to the solution in each volumetric flask of color stability is 2% ascorbic acid solution and the 6mol/L hydrochloric acid solution of 10～13mL, and adjusting acidity is 1.3 ~ 1.6mol/L, is diluted to scale mark, reductase 12 0min～1h;
Final solution through reduction constant volume in each volumetric flask is measured to absorbance record with absorption cell 810nm place on spectrophotometer of 1cm.
4. the rapid assay methods of silicone content in catalyzer according to claim 1, is characterized in that, in described step (4), the computing formula of conversion silicon dioxide percentage composition is,
Wherein
c samplefor the unit being calculated by the typical curve linear equation sample concentration that is mg/L,
v samplethe sample solution volume that the unit pipetting for chromogenic reaction is mL,
m samplefor the weighed unit testing sample quality that is g.
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| CN105424687A (en) * | 2015-11-11 | 2016-03-23 | 中国科学院水生生物研究所 | Method for detecting biogenic silicon content in bottom sediment |
| CN108414461A (en) * | 2018-02-05 | 2018-08-17 | 佛山科学技术学院 | A method of improving silicate component measuring accuracy |
| CN110631874A (en) * | 2019-09-17 | 2019-12-31 | 全球能源互联网研究院有限公司 | Sample pretreatment method for determining content of silicon element in polymer and method for determining content of silicon element in polymer |
| CN112986165A (en) * | 2021-02-20 | 2021-06-18 | 珠海格力电工有限公司 | Enameled wire and method for measuring silicon content in auxiliary materials for production of enameled wire and application of enameled wire |
| CN113670895A (en) * | 2021-08-20 | 2021-11-19 | 江苏扬农化工集团有限公司 | Method for improving element determination accuracy in heteropoly acid catalyst |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105424687A (en) * | 2015-11-11 | 2016-03-23 | 中国科学院水生生物研究所 | Method for detecting biogenic silicon content in bottom sediment |
| CN108414461A (en) * | 2018-02-05 | 2018-08-17 | 佛山科学技术学院 | A method of improving silicate component measuring accuracy |
| CN110631874A (en) * | 2019-09-17 | 2019-12-31 | 全球能源互联网研究院有限公司 | Sample pretreatment method for determining content of silicon element in polymer and method for determining content of silicon element in polymer |
| CN110631874B (en) * | 2019-09-17 | 2022-06-10 | 全球能源互联网研究院有限公司 | Sample pretreatment method for determining content of silicon element in polymer and method for determining content of silicon element in polymer |
| CN112986165A (en) * | 2021-02-20 | 2021-06-18 | 珠海格力电工有限公司 | Enameled wire and method for measuring silicon content in auxiliary materials for production of enameled wire and application of enameled wire |
| CN113670895A (en) * | 2021-08-20 | 2021-11-19 | 江苏扬农化工集团有限公司 | Method for improving element determination accuracy in heteropoly acid catalyst |
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Application publication date: 20141112 |