CN104048895B - A kind of assay method of titanium dioxide surface hydroxy radical content - Google Patents
A kind of assay method of titanium dioxide surface hydroxy radical content Download PDFInfo
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- CN104048895B CN104048895B CN201310577762.3A CN201310577762A CN104048895B CN 104048895 B CN104048895 B CN 104048895B CN 201310577762 A CN201310577762 A CN 201310577762A CN 104048895 B CN104048895 B CN 104048895B
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Abstract
The present invention relates to a kind of can the method for quantitative measurement titanium dioxide sample the adsorbed hydroxyl content, steps of the method are: the titanium dioxide sample of A, accurately weighing m quality, dry to constant weight m
1, described bake out temperature is 220 ~ 250 DEG C; B, accurately weighing m
2the steps A gained titanium dioxide sample of quality is dispersed in water; C, under heating stirring reaction condition, homodisperse for step B described titanium dioxide sample to be contacted with hydrochloric acid standard solution or nitric acid standard solution; D, the potpourri of gained after step C contact is carried out Separation of Solid and Liquid, obtain separation solution; E, by the separation solution constant volume in step D to certain volume, obtain solution after constant volume; The pH value of solution after constant volume described in F, determination step E.The content of titanium dioxide surface hydroxyl is calculated according to formula 1 and formula 2.Method energy accurate quantitative analysis of the present invention measures the content of titanium dioxide sample surface hydroxyl, and simple to operate.
Description
Technical field
The present invention relates to a kind of method measuring titanium dioxide surface hydrogen bonding hydroxy radical content, and a kind of method measuring titanium dioxide surface hydroxyl total content.
Background technology
Titania, because of advantages such as chemical stability are good, nontoxic, inexpensive, is widely used in various fields such as multiphase photocatalysis, solar cell, antibacterial building materials and light therapies, has broad prospects.Titanium dioxide surface contains abundant oh group, thermal stability, be mainly divided into two kinds, and a kind of is the hydrogen bonding hydroxyl that thermal stability is lower, and another kind is the isolated hydroxyl that thermal stability is higher.The classification of surface hydroxyl and character have very important meaning to the absorption of research titania and photocatalysis essence.At present, the research of titanium dioxide surface hydroxyl mainly concentrate on utilize in-situ ft-ir effects on surface hydroxyl qualitative on, there is no open source literature to measuring titanium dioxide surface hydroxyl analysis method by measuring hydrogen bonding hydroxy radical content and isolated hydroxy radical content respectively.
Summary of the invention
The object of this invention is to provide a kind of can the method for Accurate Determining titanium dioxide sample Surface Hydrogen bonded hydroxy content and the method for titanium dioxide sample total surface hydroxy radical content.
According to an aspect of the present invention, the invention provides a kind of method measuring titanium dioxide surface hydrogen bonding hydroxy radical content, the method comprises the following steps:
The titanium dioxide sample of A, accurately weighing m quality, dries to constant weight m
1, described bake out temperature is 220-250 DEG C;
B, determine Surface Hydrogen bonded hydroxy content in described titanium dioxide sample according to following computing formula:
In formula: the quality of the titanium dioxide sample of m-take, g;
M
1-dry the quality of titanium dioxide sample to constant weight, g.
According to a further aspect in the invention, the invention provides a kind of method measuring titanium dioxide sample surface hydroxyl total content, the method comprises the following steps:
The titanium dioxide sample of A, accurately weighing m quality, dries to constant weight m
1, described bake out temperature is 220-250 DEG C;
B, accurately weighing m
2the steps A gained titanium dioxide sample of quality is dispersed in water;
C, under heating stirring reaction condition, homodisperse for step B described titanium dioxide sample to be contacted with hydrochloric acid standard solution or nitric acid standard solution;
D, the potpourri of gained after step C contact is carried out Separation of Solid and Liquid, obtain separation solution;
E, by the separation solution constant volume in step D to certain volume, obtain solution after constant volume;
The pH value of solution after constant volume described in F, determination step E, determine surface hydroxyl total content in described titanium dioxide sample according to following computing formula:
In formula: C
1-hydrochloric acid standard solution or nitric acid concentration of standard solution, mol/L;
V
1-add hydrochloric acid standard solution or nitric acid standard solution volume, mL;
V
2volume after-constant volume, mL;
The molal weight of 17.01-surface hydroxyl, g/mol;
The pH value that pH-step F records;
The quality of the titanium dioxide sample of m-take, g;
M
1-dry the quality of titanium dioxide sample to constant weight, g;
M
2-the quality of titanium dioxide sample that is dispersed in water, g.
Method of the present invention can measure the content of titanium dioxide sample Surface Hydrogen bonded hydroxy and the content of titanium dioxide sample total surface hydroxyl by accurate quantitative analysis, and the method is simple to operate, and agents useful for same is easy to get, and experimental apparatus used is conventional.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
One aspect of the present invention provides a kind of method measuring titanium dioxide surface hydrogen bonding hydroxy radical content, and the method comprises the following steps:
The titanium dioxide sample of A, accurately weighing m quality, dries to constant weight m
1, described bake out temperature is 220-250 DEG C;
B, determine Surface Hydrogen bonded hydroxy content in described titanium dioxide sample according to following computing formula:
In formula: the quality of the titanium dioxide sample of m-take, g;
M
1-dry the quality of titanium dioxide sample to constant weight, g.
The present invention provides a kind of method measuring titanium dioxide surface hydroxyl total content on the other hand, and the method comprises the following steps:
The titanium dioxide sample of A, accurately weighing m quality, dries to constant weight m
1, described bake out temperature is 220-250 DEG C;
B, accurately weighing m
2the steps A gained titanium dioxide sample of quality is dispersed in water;
C, under heating stirring reaction condition, homodisperse for step B described titanium dioxide sample to be contacted with hydrochloric acid standard solution or nitric acid standard solution;
D, the potpourri of gained after step C contact is carried out Separation of Solid and Liquid, obtain separation solution;
E, by the separation solution constant volume in step D to certain volume, obtain solution after constant volume;
The pH value of solution after constant volume described in F, determination step E, determine surface hydroxyl total content in described titanium dioxide sample according to following computing formula:
In formula: C
1-hydrochloric acid standard solution or nitric acid concentration of standard solution, mol/L;
V
1-add hydrochloric acid standard solution or nitric acid standard solution volume, mL;
V
2volume after-constant volume, mL;
The molal weight of 17.01-surface hydroxyl, g/mol;
The pH value that pH-step F records;
The quality of the titanium dioxide sample of m-take, g;
M
1-dry the quality of titanium dioxide sample to constant weight, g;
M
2-the quality of titanium dioxide sample that is dispersed in water, g.
According to method of the present invention, wherein, in steps A, described bake out temperature is 220-250 DEG C, and titanium dioxide surface hydrogen bonding hydroxyl thermal stability is lower, generally can disappear about 200 DEG C process; Isolated hydroxyl thermal stability is higher, character is comparatively stable, generally just can disappear when 350 DEG C or higher temperature, therefore, have chosen at 220-250 DEG C of baking titanium dioxide sample to constant weight in determination step A of the present invention, temperature is too low, and hydrogen bonding hydroxyl not easily disappears, temperature is too high, and isolated hydroxyl may disappear.In order to measure titanium dioxide surface hydrogen bonding hydroxy radical content more accurately, preferably, described bake out temperature is 230-240 DEG C.
Described oven dry is preferably carried out in electric heating constant-temperature blowing drying box.
According to method of the present invention, wherein, in step B, the consumption of water can be selected in relative broad range, as long as titanium dioxide sample can be made dispersed, under preferable case, relative to the titanium dioxide sample that 0.5000g is dispersed in water, the volume of water is 50-200mL, is more preferably 100mL.
According to method of the present invention, wherein, in step B, described dispersion can be carried out under any known method, as long as titanium dioxide sample can be made to be dispersed in water uniformly, under preferable case, it is suspension that described dispersion first stirs titania solution with glass bar, then under ultrasound wave exists, carry out continuation dispersion.
Described hyperacoustic frequency can be existing various ultrasonic frequency, and in order to make titanium dioxide sample disperse fully in water, under preferable case, described ultrasonic frequency is 30-80kHz; The time of ultrasound wave dispersion is 2-3min.
According to method of the present invention, wherein, in step C, as long as described heating stirring reaction condition can make the hydroxyl complete reaction of titanium dioxide surface and sour surplus can in measurement range at accurate pH meter, under preferable case, described mixing time is 1-1.5h; Described heating-up temperature is 30-35 DEG C.
The consumption of described hydrochloric acid or nitric acid standard solution can be selected in relative broad range, as long as can make the hydroxyl complete reaction of titanium dioxide surface and sour surplus can in measurement range at accurate pH meter.Preferably, the concentration of described hydrochloric acid or nitric acid standard solution is 0.005-0.008mol/L; Relative to the titanium dioxide sample that 0.5000g is dispersed in water, the volume of described hydrochloric acid or nitric acid standard solution is 5-10mL.
According to method of the present invention, wherein, in step D, the mode of described Separation of Solid and Liquid can be carried out under any known method, as long as finally can obtain the filtrate of clarifying.Under preferable case, the mode of described Separation of Solid and Liquid comprises carries out standing sedimentation and filtration successively by step C contact gained potpourri, and filtrate is carried out centrifuging.
The described standing sedimentation time is 3-10 hour, be preferably 5-8 hour, described filtration is preferably Filter paper filtering, be more preferably fast grade filter paper to filter, described centrifuging is preferably centrifuge and is separated, be more preferably supercentrifuge centrifuging, rotating speed is 5000-10000r/min, finally obtains settled solution; Settled solution is cooled to room temperature, is convenient to accurate constant volume in step e.
According to method of the present invention, wherein, relative to the titanium dioxide sample that 0.5000g is dispersed in water, in step e, centrifugal rear settled solution, the volume of constant volume can be 50-200mL, is preferably 100mL.
As long as can the pH value of Accurate Determining filtrate in step e, under preferable case, the assay method of described pH value be that pH meter measures, and is preferably the pH value that Accurate pH measures solution after constant volume, accurate Calculation after being convenient to.The mensuration of pH value can be carried out according to operation steps described in corresponding analytical approach GB/T6920-1986 " the mensuration glass electrode method of water pH value ".
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
The invention will be further described by the following examples.
The titanium dioxide sample of following examples and comparative example is commercially available product.
Embodiment 1
The present embodiment is for illustration of the content of titanium dioxide surface hydrogen bonding hydroxyl of the present invention and the assay method of hydroxyl total content.
Accurately take titanium dioxide sample 1.000g in evaporating dish, be placed in electric heating constant-temperature blowing drying box 230 DEG C and dry to constant weight and weigh.Accurately take and dry to constant weight titanium dioxide sample 0.5000g in 200mL beaker, add 100mL distilled water, be separated into suspension with glass bar agitating solution, titanium dioxide sample is placed in ultrasound wave and disperses 2min, hyperacoustic frequency is 80kHz, is cooled to room temperature; In titanium dioxide sample, drip hydrochloric acid standard solution (0.005mol/L) 8mL, and 30 DEG C of constant temperature stir 1h on magnetic stirring apparatus, titanium dioxide sample surface hydroxyl and hydrochloric acid standard solution are fully reacted, standing sedimentation 5 hours after reacting completely.Filter with fast grade filter paper, filtrate is placed in supercentrifuge and is separated, inclining supernatant liquor and is settled to 100mL, is transferred in 100mL beaker, adopts accurate pH meter to measure solution ph according to GB/T6920-1986.Then calculate the content of titanium dioxide surface hydrogen bonding hydroxyl according to following formula 1, calculate the total content of titanium dioxide surface hydroxyl according to following formula 2:
In formula: C
1-hydrochloric acid standard solution concentration, mol/L;
V
1-add hydrochloric acid standard solution volume, mL;
V
2volume after-constant volume, mL;
The molal weight of 17.01-surface hydroxyl, g/mol;
The pH value that pH-step F records;
The quality of the titanium dioxide sample of m-take, g;
M
1-dry the quality of titanium dioxide sample to constant weight, g;
M
2-the quality of titanium dioxide sample that is dispersed in water, g.
Carry out 11 times according to the method described above to same titanium dioxide sample independent to measure, the described content of titanium dioxide surface hydrogen bonding hydroxyl and the measurement result of total content of hydroxyl and the precision of statistical method, as shown in table 1.
Table 1
Good, reliable and stable by table 1 visual method precision.
Embodiment 2
The present embodiment is for illustration of the content of titanium dioxide surface hydrogen bonding hydroxyl of the present invention and the assay method of hydroxyl total content.
Accurately take titanium dioxide sample 1.000g in evaporating dish, be placed in electric heating constant-temperature blowing drying box 240 DEG C and dry to constant weight and weigh.Accurately take the titanium dioxide sample 0.5000g that dries to constant weight and be placed in 200mL beaker, add 100mL distilled water, be separated into suspension with glass bar agitating solution, titanium dioxide sample is placed in ultrasound wave and disperses 3min, hyperacoustic frequency is 30kHz, is cooled to room temperature; Nitric acid standard solution (0.005mol/L) 8mL is dripped in titanium dioxide sample, and 35 DEG C of constant temperature stir 1.5h on magnetic stirring apparatus, titanium dioxide sample surface hydroxyl and nitric acid standard solution are fully reacted, after reacting completely, titanium dioxide sample standing sedimentation 5 hours.Filter with fast grade filter paper, filtrate is placed in supercentrifuge and is separated, inclining supernatant liquor and is settled to 100mL, is transferred in 100mL beaker, adopts accurate pH meter to measure solution ph according to GB/T6920-1986.Then calculate the content of titanium dioxide surface hydrogen bonding hydroxyl according to following formula 1, calculate the total content of titanium dioxide surface hydroxyl according to following formula 2:
In formula: C
1-nitric acid concentration of standard solution, mol/L;
V
1-add nitric acid standard solution volume, mL;
V
2volume after-constant volume, mL;
The molal weight of 17.01-surface hydroxyl, g/mol;
The pH value that pH-step F records;
The quality of the titanium dioxide sample of m-take, g;
M
1-dry the quality of titanium dioxide sample to constant weight, g;
M
2-the quality of titanium dioxide sample that is dispersed in water, g.
Carry out 11 times according to the method described above to same titanium dioxide sample independent to measure, the described content of titanium dioxide surface hydrogen bonding hydroxyl and the measurement result of total content of hydroxyl and the precision of statistical method, as shown in table 2.
Table 2
Good, reliable and stable by table 2 visual method precision.
Embodiment 3
The present embodiment is for illustration of the content of titanium dioxide surface hydrogen bonding hydroxyl of the present invention and the assay method of hydroxyl total content.
Accurately take titanium dioxide sample 1.000g in evaporating dish, be placed in electric heating constant-temperature blowing drying box 250 DEG C and dry to constant weight and weigh.Accurately take the titanium dioxide sample 0.5000g that dries to constant weight and be placed in 200mL beaker, add 100mL distilled water, be separated into suspension with glass bar agitating solution, titanium dioxide sample is placed in ultrasound wave and disperses 2.5min, hyperacoustic frequency is 40kHz, is cooled to room temperature; Nitric acid standard solution (0.008mol/L) 5mL is dripped in titanium dioxide sample, and 33 DEG C of constant temperature stir 1.2h on magnetic stirring apparatus, titanium dioxide sample surface hydroxyl and nitric acid standard solution are fully reacted, after reacting completely, titanium dioxide sample standing sedimentation 8 hours.Filter with fast grade filter paper, filtrate is placed in supercentrifuge and is separated, inclining supernatant liquor and is settled to 100mL, is transferred in 100mL beaker, adopts accurate pH meter to measure solution ph according to GB/T6920-1986.Then calculate the content of titanium dioxide surface hydrogen bonding hydroxyl according to following formula 1, calculate the total content of titanium dioxide surface hydroxyl according to following formula 2:
In formula: C
1-nitric acid concentration of standard solution, mol/L;
V
1-add nitric acid standard solution volume, mL;
V
2volume after-constant volume, mL;
The molal weight of 17.01-surface hydroxyl, g/mol;
The pH value that pH-step F records;
The quality of the titanium dioxide sample of m-take, g;
M
1-dry the quality of titanium dioxide sample to constant weight, g;
M
2-the quality of titanium dioxide sample that is dispersed in water, g.
Carry out 11 times according to the method described above to same titanium dioxide sample independent to measure, the described content of titanium dioxide surface hydrogen bonding hydroxyl and the measurement result of total content of hydroxyl and the precision of statistical method, as shown in table 3.
Table 3
Good, reliable and stable by table 3 visual method precision.
As can be seen from showing the data of 1-3 relatively, the content of titanium dioxide sample Surface Hydrogen bonded hydroxy of the present invention and the assay method precision of hydroxyl total content good, reliable and stable, to measure the analysis result of the content of titanium dioxide sample total surface hydroxyl basically identical with adding nitric acid standard solution to add hydrochloric acid standard solution.
Therefore, use described method of the present invention can measure the content of titanium dioxide sample Surface Hydrogen bonded hydroxy and the content of titanium dioxide sample total surface hydroxyl by accurate quantitative analysis, and the method is simple to operate, agents useful for same is easy to get, and experimental apparatus used is conventional.
The present invention is not limited to the detail in above-mentioned embodiment, and within the scope of technical conceive of the present invention, can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.It should be noted that in addition, each the concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode.In order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.In addition, also can carry out combination in any between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (7)
1. measure a method for titanium dioxide sample surface hydroxyl total content, the method comprises the following steps:
The titanium dioxide sample of A, accurately weighing m quality, dries to constant weight m
1, described bake out temperature is 220-250 DEG C;
B, accurately weighing m
2the steps A gained titanium dioxide sample of quality is dispersed in water;
C, under heating stirring reaction condition, homodisperse for step B described titanium dioxide sample to be contacted with hydrochloric acid standard solution or nitric acid standard solution;
D, the potpourri of gained after step C contact is carried out Separation of Solid and Liquid, obtain separation solution;
E, by the separation solution constant volume in step D to certain volume, obtain solution after constant volume;
The pH value of solution after constant volume described in F, determination step E, determine surface hydroxyl total content in described titanium dioxide sample according to following computing formula:
In formula: C
1-hydrochloric acid standard solution or nitric acid concentration of standard solution, mol/L;
V
1-add hydrochloric acid standard solution or nitric acid standard solution volume, mL;
V
2volume after-constant volume, mL;
The molal weight of 17.01-surface hydroxyl, g/mol;
The pH value that pH-step F records;
The quality of the titanium dioxide sample of m-take, g;
M
1-dry the quality of titanium dioxide sample to constant weight, g;
M
2-the quality of titanium dioxide sample that is dispersed in water, g.
2. method according to claim 1, wherein, in steps A, described bake out temperature is 230-240 DEG C, and described oven dry is carried out in electric heating constant-temperature blowing drying box.
3. method according to claim 1, wherein, in step B, described in be dispersed in ultrasound wave exist under carry out, hyperacoustic frequency is 30-80kHz, and the time of dispersion is 2-3min.
4. method according to claim 1, wherein, in step C, described heating stirring reaction condition comprises: mixing time is 1-1.5h; Described heating-up temperature is 30-35 DEG C.
5. method according to claim 1, wherein, in step C, the concentration of described hydrochloric acid standard solution or nitric acid standard solution is 0.005-0.008mol/L.
6. method according to claim 5, wherein, in step C, the volume of described hydrochloric acid or nitric acid standard solution is 5-10mL.
7., according to the method in claim 1-6 described in any one, wherein, in step F, use Accurate pH measurement to determine the pH value of solution after the constant volume that step e obtains.
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