CN104198466A - Method for determining content of Ti in TiO2 photocatalyst - Google Patents
Method for determining content of Ti in TiO2 photocatalyst Download PDFInfo
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- CN104198466A CN104198466A CN201410436070.1A CN201410436070A CN104198466A CN 104198466 A CN104198466 A CN 104198466A CN 201410436070 A CN201410436070 A CN 201410436070A CN 104198466 A CN104198466 A CN 104198466A
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Abstract
The invention discloses a method for determining the content of Ti in a TiO2 photocatalyst and belongs to the field of chemical testing. The method comprises the following steps: adding 10-100mg of carrier catalyst into a polytetrafluoroethylene microwave digestion tube, adding 1-10ml of 98% concentrated sulfuric acid and 1-10ml of 30% hydrogen peroxide, and performing heating digestion reaction in a microwave digester, wherein the reaction temperature is controlled within 140-200 DEG C, and the reaction time is controlled within 25-55min; after the reaction is finished, a digestion solution is obtained, filtering the digestion solution, making up to the volume to 50ml, and determining the content of the Ti in a liquid supernatant by virtue of ICP-OES. The carrier TiO2 catalyst is acidized and subjected to microwave digestion pretreatment, TiO2 is converted into the Ti in a soluble ionic state, and the quick, simple and convenient method is provided for the determination of the content of the Ti in the TiO2 photocatalyst. The method is suitable for determining the content of the Ti in a TiO2 nano-sheet colloid, a TiO2 nano-tube, a thin TiO2 film and catalysts in other forms, is suitable for being used for determining the content of the Ti in the TiO2 photocatalyst after repeated reaction, and is wide in application range.
Description
Technical field
The present invention relates to test chemical field, is a kind of to TiO
2 the assay method of Ti content in photocatalyst.
Background technology
In recent years, water pollutes, atmospheric pollution is day by day serious, in order effectively to remove various pollutants as hardly degraded organic substance, SO
2, NO
xdeng, absorption method, chemical oxidization method and bioanalysis have been applied to every field.TiO
2photocatalysis technology is subject to extensive concern as a kind of high-level oxidation technology, and its cost is low, safety non-toxic, stable, under normal temperature, can react, and does not need to add other chemical reagent, to environmental pollutants almost can be without selective oxidation, and final product is CO
2, H
2o, NO
3 -and SO
4 2-deng, do not cause secondary pollution, it is more and more come into one's own as a kind of good photocatalyst.
The TiO of catalyst active center
2content be an important indicator weighing catalyst activity.In general Study, the TiO in different shape catalyzer
2content is normally controlled the TiO of the photocatalyst of preparation according to the presoma content of the Ti such as titanium alkoxide that add in its preparation process
2content, but in preparation process, there is unavoidably loss of material, thereby cause cubage deviation.
At present, TiO
2assay method have colourimetry, titrimetry and inductively coupled plasma emission spectrography, for example GB/T3654.8-2008 adopts the Ti content in chromotropic acid spectrphotometric method for measuring ferro-niobium, GB/T6730.23-2006 adopts ferrous ammonium sulfate titration Ti content, but titrimetry and colorimetric method for determining result are disturbed many factors, error is larger, especially be unsuitable for the mensuration of low content titanium, and test period is long, is not suitable with the express-analysis of batch samples; And in the preprocessing process of sample, conventionally adopt add strong acid acidifying associating electric hot plate heating means (huge power pendant etc., 2013) or adopt highly basic melting-metal deoxidization (number of patent application 2012103888190), consuming time longer.
This method of testing is intended to set up a kind of Quick Pretreatment TiO
2photocatalyst also carries out the method for Ti assay, specifically by strong acid acidifying-Microwave Digestion to TiO
2photocatalyst pre-service, by solid-state TiO
2all be converted into the Ti of dissolubility ionic state, so that use inductive coupling plasma emission spectrograph (ICP-OES) to measure.
Summary of the invention
For TiO
2in catalyzer, Ti content is directly measured difficult problem, the invention provides a kind of strong acid and dissolves United microwave resolution method, and catalyzer is carried out to pre-service, measures Ti content subsequently by ICP-OES method, and this method is easy and in enforcement.Described method realizes in the following way:
In teflon micro-wave digestion pipe, add 10 ~ 100 mg TiO
2catalyzer, then add the hydrogen peroxide that the concentrated sulphuric acid that 1 ~ 10 ml concentration is 98% and 1 ~ 10 ml concentration are 30%, be then placed in microwave dissolver, (condition is: step 1 under 800W heating power, to clear up reaction, heating-up times 5 ~ 15 min, 120 ~ 160 ℃ of target temperatures, do not keep; Step 2,170 ~ 200 ℃ of target temperatures, insulation 20 ~ 40 min), cooling rear digestion solution is filtered and is settled to 50 ml, utilize ICP-OES to carry out the mensuration of titanium elements.
The present invention compares and has the following advantages with conventional determining method:
(1) propose the pre-service of strong acid acidifying United microwave resolution method and processed TiO
2photocatalyst, simple, convenient and rapid;
(2) this law is not only applicable to TiO in carried catalyst
2the mensuration of content is also suitable for other forms as TiO simultaneously
2nanometer sheet colloid, TiO
2nanotube, TiO
2the mensuration of the Ti content such as film, applied widely;
(3) this law can be determined the rear TiO of repeatedly reaction
2the content of Ti in catalyzer.
Embodiment
embodiment reagent used comprises:
98% concentrated sulphuric acid, top grade is pure;
30% hydrogen peroxide, top grade is pure;
titania (100%), analyzes pure;
pure water;
titanium standard solution, 1000 mg/ml(country's non-ferrous metal and electronic material Institute of Analysis);
65% red fuming nitric acid (RFNA), top grade is pure.
embodiment 1:
Embodiment 1 relates to the preparation of Ti standard solution, the drafting of standard working curve and contain carried catalyst TiO
2mensuration, specific as follows:
(1) preparation titanium standard solution, drawing standard working curve: titanium standard solution is diluted to constant volume with 2% nitric acid, be mixed with the serial titanium standard operation liquid that titanium ion concentration is respectively 0.1 mg/ml, 0.5 mg/ml, 1 mg/ml, 2 mg/ml, 5 mg/ml, 10 mg/ml, the linear regression coeffficient R of the standard working curve obtaining
2=0.9999;
(2) clear up carried catalyst sample: take and take the TiO that flyash is carrier
2photocatalyst is placed in teflon micro-wave digestion pipe, adds the hydrogen peroxide that the concentrated sulphuric acid that 6 ml concentration are 98% and 4 ml concentration are 30%, and (condition is: step 1,5 min that heat up, 140 ℃ of target temperatures in microwave dissolver, to carry out micro-wave digestion; Step 2,190 ℃ of target temperatures, insulation 25 min), reaction finishes rear filtration and is settled to 50 ml;
(3) measure: get the solution after step constant volume, cross the polyethersulfone filter membrane of 0.45 mm, utilize inductive coupling plasma emission spectrograph (ICP-OES) to detect, by the typical curve wherein obtaining, calculate titanium elements content in sample.
embodiment 2:
(1) preparation titanium standard solution, drawing standard working curve: single mark solution of titanium is diluted to constant volume with 2% nitric acid, be mixed with the serial titanium standard operation liquid that titanium ion concentration is respectively 0.1 mg/ml, 0.5 mg/ml, 1 mg/ml, 2 mg/ml, 5 mg/ml, 10 mg/ml, the linear regression coeffficient R of the standard working curve obtaining
2=0.9999;
(2) clear up TiO
2nanometer sheet colloidal solution: get variable concentrations TiO
2nanometer sheet colloidal solution 1 ml, in teflon micro-wave digestion pipe, adds the hydrogen peroxide that the concentrated sulphuric acid that 5 ml concentration are 98% and 3 ml concentration are 30%, reacts that (condition is: step 1,8 min that heat up, 150 ℃ of target temperatures in microwave dissolver; Step 2,170 ℃ of target temperatures, insulation 35 min), be settled to 50 ml after cooling;
(3) measure: get the solution after step constant volume, utilize inductive coupling plasma emission spectrograph (ICP-OES) to detect, by the typical curve wherein obtaining, calculate titanium elements content in colloidal solution.
Claims (6)
1. one kind to TiO
2the assay method of Ti content in photocatalyst, that application strong acid acidifying United microwave resolution method is carried out pre-service to carried catalyst, and then titanium ion concentration is measured, it is characterized in that described method concrete steps are: first in teflon micro-wave digestion pipe, add 10 ~ 100 mg TiO
2catalyzer, then add the hydrogen peroxide that the concentrated sulphuric acid that 1 ~ 10 ml concentration is 98% and 1 ~ 10 ml concentration are 30%, be then placed in microwave dissolver, (condition is: step 1 under 800W heating power, to clear up reaction, heating-up times 5 ~ 15 min, 140 ~ 160 ℃ of target temperatures, do not keep; Step 2,170 ~ 200 ℃ of target temperatures, insulation 20 ~ 40 min), digestion solution is filtered and is settled to 50 ml after cooling, utilize ICP-OES to carry out the mensuration of titanium elements.
2. a kind of mensuration TiO according to claim 1
2the assay method of Ti content in catalyzer, is characterized in that the catalyzer amount of clearing up is 10 ~ 100 mg.
3. a kind of mensuration TiO according to claim 1
2the assay method of Ti content in catalyzer, is characterized in that in described acidification that 98% concentrated sulphuric acid addition is 1 ~ 10 ml, and the addition of 30% hydrogen peroxide is 1 ~ 10 ml.
4. a kind of mensuration TiO according to claim 1
2the assay method of Ti content in catalyzer, micro-wave digestion temperature of reaction is 140 ~ 200 ℃.
5. a kind of mensuration TiO according to claim 1
2the assay method of Ti content in catalyzer, the micro-wave digestion reaction time is 25 ~ 55 min.
6. a kind of mensuration TiO according to claim 1
2the assay method of Ti content in catalyzer, constant volume test again after reaction finishes rear digestion solution and need filter.
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| CN201410436070.1A CN104198466A (en) | 2014-08-29 | 2014-08-29 | Method for determining content of Ti in TiO2 photocatalyst |
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| CN201410436070.1A CN104198466A (en) | 2014-08-29 | 2014-08-29 | Method for determining content of Ti in TiO2 photocatalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105388141A (en) * | 2015-12-23 | 2016-03-09 | 中国科学院兰州化学物理研究所 | Method for measuring gold element content in core-shell type gold-magnetic nano composite catalyst through inductively coupled plasma emission spectrum |
| CN106525953A (en) * | 2016-12-02 | 2017-03-22 | 北京工业大学 | Method for accurately determining quality of titanium dioxide nanotube array |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008116233A2 (en) * | 2007-03-20 | 2008-09-25 | Sasol Technology (Pty) Ltd | A method for determining the content of metallic elements in fischer-tropsch waxes |
| CN103808558A (en) * | 2014-03-03 | 2014-05-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Digestion method and detection method for vanadium-nitrogen-titanium-iron mixed alloy conductor |
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2014
- 2014-08-29 CN CN201410436070.1A patent/CN104198466A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008116233A2 (en) * | 2007-03-20 | 2008-09-25 | Sasol Technology (Pty) Ltd | A method for determining the content of metallic elements in fischer-tropsch waxes |
| CN103808558A (en) * | 2014-03-03 | 2014-05-21 | 攀钢集团攀枝花钢铁研究院有限公司 | Digestion method and detection method for vanadium-nitrogen-titanium-iron mixed alloy conductor |
Non-Patent Citations (2)
| Title |
|---|
| AMJAD H. EL-SHEIKH 等: "A rapid and simple microwave-assisted digestion procedure for spectrophotometric determination of titanium dioxide photocatalyst on activated carbon", 《TALANTA》 * |
| 张洁 等: "微波消解-电感耦合等离子发射光谱测定鸡肉中9种元素", 《食品科学》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105388141A (en) * | 2015-12-23 | 2016-03-09 | 中国科学院兰州化学物理研究所 | Method for measuring gold element content in core-shell type gold-magnetic nano composite catalyst through inductively coupled plasma emission spectrum |
| CN106525953A (en) * | 2016-12-02 | 2017-03-22 | 北京工业大学 | Method for accurately determining quality of titanium dioxide nanotube array |
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Application publication date: 20141210 |