CN109382047A - Molten titrant for depositing density of hydrogen and preparation method thereof in a kind of superior platinum nano-sized colloidal solution of high-concentration and stable, measurement water - Google Patents
Molten titrant for depositing density of hydrogen and preparation method thereof in a kind of superior platinum nano-sized colloidal solution of high-concentration and stable, measurement water Download PDFInfo
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- CN109382047A CN109382047A CN201811226162.1A CN201811226162A CN109382047A CN 109382047 A CN109382047 A CN 109382047A CN 201811226162 A CN201811226162 A CN 201811226162A CN 109382047 A CN109382047 A CN 109382047A
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0004—Preparation of sols
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- G—PHYSICS
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- 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
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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Abstract
The invention discloses molten titrant for depositing density of hydrogen in a kind of superior platinum nano-sized colloidal solution of high-concentration and stable, measurement water and preparation method thereof, are related to density of hydrogen detection technique field.Specifically, the superior platinum nano-sized colloidal solution of the high-concentration and stable, is used to prepare the molten titrant for depositing density of hydrogen in measurement water, the nano platinum particle concentration of the platinum nano-sized colloidal solution is high, stability is superior, and catalytic performance is good.React fast using the titrant that the platinum nano-sized colloidal solution is prepared, stability is good, can effectively improve the molten accuracy and efficiency for depositing hydrogen in titrant measurement water.
Description
Technical field
The present invention relates to density of hydrogen detection technique fields, in particular to a kind of superior platinum of high-concentration and stable
Molten titrant for depositing density of hydrogen and preparation method thereof in nano-sized colloidal solution, measurement water.
Background technique
In recent years with the development of hydrogen molecule medicine, hydrogen molecule health progresses into our visual field, in Japan and South Korea
Product etc. relevant hydrogen type is quickly grown, and many this kind of product also occurs in the major on-line off-line sales platform in China,
Middle hydrogen-rich cup, hydrogen-rich water dispenser, hydrogen-rich foot bath and hydrogen-rich facial mask are the most welcome.
During using hydrogen, either apply in scientific research or actual product, Accurate Determining hydrogen
Concentration is all the major issue for needing to face.For hydrogen molecule health product, producing agent and user must all be defined
Whether product can generate the amount of hydrogen and generation, this directly affects the sales volume and using effect of product.Measurement hydrogen at present
The standard method of concentration is gas chromatography and electrode method, but both methods needs more expensive instrument and equipment and complexity
Detection technique does not meet the demand of production agent and ordinary user.
Be used for the convenient measurement of density of hydrogen on the market is exactly the similar product of negative potential test pen, but this kind of test pen
Be easy to the interference by other substances, and accuracy it is high test pen it is expensive, the frequency of use of user is not high in addition, therefore
Cost performance is very low.Other than test pen, there are also the titrant for measuring density of hydrogen in water.But really effective and accuracy
Higher titrant is not only at high cost, price, and reacts slow, and stability is bad.
Therefore, how to provide that a kind of raw material is relatively cheap, synthesis is simple, stablize and molten water element titrant that effect is good is
Industry problem to be solved.
Summary of the invention
The first object of the present invention is to provide a kind of superior platinum nano-sized colloidal solution of high-concentration and stable, be used to prepare
The molten titrant for depositing density of hydrogen in water is measured, the nano platinum particle concentration of the platinum nano-sized colloidal solution is high, stability is superior, urges
Change performance is good, reacts fast using the titrant that the platinum nano-sized colloidal solution is prepared, stability is good, can effectively improve titration
Agent measures the molten accuracy and efficiency for depositing hydrogen in water.
The second object of the present invention is to provide the molten titrant for depositing density of hydrogen in a kind of measurement water comprising has above-mentioned
Platinum nano-sized colloidal solution, the titrant can quickly measure the density of hydrogen in solution, and the accuracy of measurement is high.
The third object of the present invention is to provide the molten preparation method for depositing density of hydrogen titrant in a kind of measurement water, energy
Enough quickly and easily prepare being capable of the molten titrant for depositing density of hydrogen in Accurate Determining water.
The fourth object of the present invention is to provide a kind of molten method for depositing density of hydrogen in measurement water comprising has using upper
It states titrant to be measured the hydrogen in solution, the determination efficiency of this method is high, and accuracy in detection is good.
The present invention is implemented as follows:
A kind of superior platinum nano-sized colloidal solution of high-concentration and stable, there is following steps synthesis:
Platinum acid chloride solution, PVP ethanol solution and distilled water are mixed, form the platinum nanometre glue of brownish black after agitating and heating
Liquid solution；Wherein, the volume ratio of platinum acid chloride solution, PVP ethanol solution and distilled water can for 1:200:10,1:200:20,
1:200:30,1:200:40,1:200:50,1:200:60,1:200:70,1:200:80,1:200:90,1:150:10,1:
150:20,1:150:30,1:150:40,1:150:50,1:150:60,1:150:70,1:150:80,1:150:90,1:170:
10,1:170:20,1:170:30,1:170:40,1:170:50,1:170:60,1:170:70,1:170:80,1:170:90,
1:230:10,1:230:20,1:230:30,1:230:40,1:230:50,1:230:60,1:230:70,1:230:80,1:
230:90,1:250:10,1:250:20,1:250:30,1:250:40,1:250:50,1:250:60,1:250:70,1:250:
80 or 1:250:90 etc., it should be noted that the volume ratio of platinum acid chloride solution, PVP ethanol solution and distilled water can be 1:
(50~400): selectively it is arranged in the range of (10~100).
Wherein, specifically, platinum acid chloride solution with distilled water is prepared to obtain by six hydration chloroplatinic acids, it is preferable that distilled water is
Secondary distilled water.The initial concentration of platinum acid chloride solution is 0.01gmL-1、 0.10g·mL-1、0.20g·mL-1、0.30g·
mL-1、0.40g·mL-1、0.50g·mL-1、0.60 g·mL-1、0.70g·mL-1、0.80g·mL-1、0.90g·mL-1Or
1g·mL-1, the initial concentration of PVP ethanol solution is 1mgmL-1、4mg·mL-1、5mg·mL-1、6mg·mL-1、 7mg·mL-1、8mg·mL-1、9mg·mL-1、10mg·mL-1、11mg·mL-1、12 mg·mL-1、13mg·mL-1、14mg·mL-1、
15mg·mL-1、16mg·mL-1、17 mg·mL-1、18mg·mL-1、19mg·mL-1、20mg·mL-1、21mg·mL-1、22
mg·mL-1、23mg·mL-1、24mg·mL-1、25mg·mL-1、26mg·mL-1、27 mg·mL-1、28mg·mL-1、29mg·
mL-1Or 30mgmL-1。
The platinum nano-sized colloidal solution prepared by said components can be used in the molten titration for depositing density of hydrogen in preparation measurement water
Agent, the nano platinum particle concentration of the platinum nano-sized colloidal solution is high, stability is superior, and catalytic performance is good, can effectively improve hydrogen
The accuracy and efficiency of measurement.
The embodiment of the present invention also provides the molten titrant for depositing density of hydrogen in a kind of measurement water comprising by above-mentioned platinum nanometer
Colloidal solution and the mixing of methylene blue ethanol solution.Specifically, the initial concentration of methylene blue ethanol solution is 0.5gL-1、
1g·L-1、1.5g·L-1、2.0g·L-1、 2.5g·L-1、3g·L-1、3.5g·L-1、4g·L-1、4.5g·L-1、5.0g·L-1、5.5g·L-1、 6.0g·L-1、6.5g·L-1、7.0g·L-1、7.5g·L-1、8.0g·L-1、8.5g·L-1、9.0g·L-1、 9.5g·L-1、10g·L-1、10.5g·L-1、11g·L-1、11.5g·L-1Or 12gL-1。
Further, in titrant, the volume ratio of methylene blue ethanol solution and platinum nano-sized colloidal solution can be 4:
1,10:1,15:1,16:1,17:1,18:1,19:1,20:1,25:1,30:1,35:1,40:1,45:1 or 51:1.
The titrant reaction being prepared by above-mentioned platinum nano-sized colloidal solution and said ratio is fast, and stability is good, can
The molten concentration for depositing hydrogen in Accurate Determining water.
The embodiment of the invention also provides a kind of preparation method of the molten titrant for depositing density of hydrogen in measurement water, the preparations
Method includes the preparation step of platinum nano-sized colloidal solution；
The preparation step includes: that platinum acid chloride solution, PVP ethanol solution and distilled water are mixed to get mixed liquor, will be mixed
It closes liquid and is heated to 80 DEG C, 82 DEG C, 84 DEG C, 86 DEG C, 88 DEG C, 90 DEG C, 92 DEG C, 94 DEG C or 95 DEG C, heating time 1h to 2h, formed
The platinum nano-sized colloidal solution of brownish black is to complete terminal.Wherein, the volume of platinum acid chloride solution, PVP ethanol solution and distilled water
Than that can be same as above, in 1:(50~400): selectively it is arranged in the range of (10~100).
Wherein, specifically, platinum acid chloride solution with distilled water is prepared to obtain by six hydration chloroplatinic acids, it is preferable that distilled water is
Secondary distilled water.The initial concentration of platinum acid chloride solution is same as above, in 0.01~1gmL-1In the range of be selectively arranged, preferably
Ground, the initial concentration of platinum acid chloride solution are 0.6~1gmL-1, the initial concentration of PVP ethanol solution is same as above, in 1mgmL-1~
30 mg·mL-1In the range of be selectively arranged, it is preferable that the initial concentration of PVP ethanol solution be 8~15mgmL-1。
The preparation method includes mixing platinum nano-sized colloidal solution with methylene blue ethanol solution.
Methylenum careuleum (MB, methylene blue) is a kind of common dyes and redox titration indicator.Due to hydrogen
The influence of covalent bond itself makes it be difficult to react at normal temperature with methylenum careuleum, if but using nano platinum particle as catalyst,
Then redox reaction can occur with the hydrogen of equivalent molecule amount, the oxidized form methylenum careuleum of blue is made to become colourless reduced form Asia
First is blue.Reaction equation are as follows:
In some implementations of the invention, the initial concentration of methylene blue ethanol solution is same as above, and is 0.5gL-1~
12g·L-1In the range of be arranged.In titrant, methylene blue ethanol solution and the volume ratio of platinum nano-sized colloidal solution can be
4:1,10:1,15:1,16:1,17:1,18:1,19:1,20:1,25:1,30:1,35:1,40:1,45:1 or 51:1.
In embodiments of the present invention, platinum nano-sized colloidal solution after being mixed with methylene blue ethanol solution manufactured titrant without
Precipitating, stability is fine, and reaction is fast, can be improved the accuracy and efficiency of density of hydrogen in measurement solution.
In addition, the present invention also provides a kind of molten method for depositing density of hydrogen in measurement water, including using above-mentioned titration
Agent titrates solution to be measured, until solution to be measured just becomes stable blue from colourless, records the drop number N that titrant is added dropwise, and
Calculate the molten concentration for depositing hydrogen in water.
Specifically, when calculating density of hydrogen, calculation formula isWherein, described to be measured
The volume of solution takes 6mL, mHFor the hydrogen quality of every drop titrant consumption, CHFor the density of hydrogen in aqueous solution.
The invention has the following advantages:
The embodiment of the present invention provides a kind of superior platinum nano-sized colloidal solution of high-concentration and stable, the platinum nano-sized colloidal solution
Nano platinum particle concentration is high, stability is superior, catalytic performance is good, is used to prepare the molten titrant for depositing density of hydrogen in measurement water
Long-term place also generates without precipitating, and reaction is fast, can effectively improve the accuracy and efficiency of hydrogen measurement.
The embodiment of the present invention also provides the molten titrant for depositing density of hydrogen, preparation method and use in a kind of measurement water
The titrant measures the molten method for depositing density of hydrogen in water.The titrant includes above-mentioned platinum nano-sized colloidal solution.The titrant
The density of hydrogen in solution can be quickly measured, the accuracy of measurement is high.The titrant is easy to use, easy to carry, stability
It is splendid.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the grain size distribution for the nano platinum particle that the embodiment of the present invention 1 provides；
Fig. 2 is the precipitation result figure for the titrant that comparative example 2 of the present invention provides.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of superior platinum nano-sized colloidal solutions of high-concentration and stable.
Addition 1mL secondary distilled water in chloroplatinic acid solid, which is hydrated, in 1g six is configured to 1g mL-1Platinum acid chloride solution it is spare；
The PVP (polyvinylpyrrolidone) of 96.5mg is dissolved in 10mL ethyl alcohol, obtain PVP ethanol solution (PVP's
Concentration is 9.65mgmL-1)；
It takes 50 μ L platinum acid chloride solutions to be added in PVP ethanol solution, 1mL secondary distilled water is added, then in round-bottomed flask
In be vigorously stirred, obtained after being heated to reflux brownish black nano platinum particle colloidal solution (in the present embodiment, platinum acid chloride solution, PVP
The volume ratio of ethanol solution and distilled water is 1:200:20).
The grain size distribution for detecting nano platinum particle in the nano platinum particle colloidal solution of the present embodiment synthesis, please refers to attached
Fig. 1, it is seen that the average grain diameter of nano platinum particle is 124.4nm.
Embodiment 2
The present embodiment provides the molten titrant for depositing density of hydrogen in a kind of measurement water.
Methylene blue 0.3g is weighed, is dissolved in it in ethyl alcohol, and is settled to 100mL, obtains the ethanol solution of methylene blue
(concentration 3gL-1), 9.5mL methylene blue ethanol solution is then taken, the platinum nano-sized colloidal solution of the embodiment 1 of 0.5mL is added
(volume ratio 19:1) is fitted into the small droplet bottles of 10mL, obtains the titrant (MB-PtNPs-C that ethyl alcohol is solvent2H5OH, MB second
Alcoholic solution).
Embodiment 3
The present embodiment provides a kind of molten methods for depositing density of hydrogen in measurement water, and steps are as follows:
The liquid water 6mL to be measured containing hydrogen is taken, titrant 1 is instilled and drips, blue is presented in liquid water, it jiggles uniformly,
Liquid water can become colorless and transparent by blue；It is further continued for being added dropwise, is terminal until solution becomes stable blue liquid water,
The hydrogen in solution is depleted substantially at this time, and recording solution is N by the drop number of the colourless titrant being added dropwise to blue, and is counted
Calculate the molten concentration for depositing hydrogen in water.
When calculating density of hydrogen, calculation formula isWherein, the body of the solution to be measured
Product takes 6mL, mHFor the hydrogen quality of every drop titrant consumption, CHFor the concentration of the hydrogen in aqueous solution.
Embodiment 4
The molten method measurement effect for depositing density of hydrogen in the measurement water that verifying embodiment 3 provides.
Various concentration hydrogen water is measured using the method that embodiment 3 provides, the hydrogen water of various concentration is by the way of electrolysis water
It is prepared, density of hydrogen CHIt is measured using electrode method.The results are shown in Table 1 for test.
1 test result of table
As shown in Table 1, embodiment 3 provide method measurement water in the molten measurement result for depositing density of hydrogen it is more stable, have compared with
Good repeatability, can effectively measure different density of hydrogen.
Comparative example 1
The proportion optimizing experiment of each component in the platinum nano-sized colloidal solution that embodiment 1 provides.
Platinum nano-sized colloidal solution is prepared using the component in embodiment 1, and compares 4 groups of comparative examples of setting, for surveying
Identical solution to be measured is tried, the difference condition and test result of comparative examples (serial number 1~4) and embodiment 1 (serial number 5) are such as
Shown in table 2.
The experiment of 2 proportion optimizing of table
As shown in Table 2, the volume and concentration of platinum nano-colloid will have a direct impact on the reaction speed of titrant.Nano platinum particle
Stability and its concentration and PVP in titrant have very big relationship, using the platinum nano-sized colloidal solution in embodiment 1
The molten titrant stability for depositing density of hydrogen is preferable in preparation measurement water, and color change is fast.
Comparative example 2
Verify the stability for the titrant that embodiment 2 provides.
The titrant that embodiment 2 provides is compared with commercially available 4 sections of titrant, places after a week, observes titrant
In precipitation status, observation result it is as shown in Figure 2.
As shown in Figure 2, it can be generated precipitating (part irised out) relative to other commercially available titrant, what embodiment 2 provided
Titrant does not precipitate generation, i.e., the nano platinum particle that embodiment 1 provides can be stabilized in the solution.
Comparative example 3
The molten method measurement precision for depositing density of hydrogen in the measurement water that verifying embodiment 3 provides.
The method provided using embodiment 3 compared with commercially available test pen, is tested identical dense using electrode method as standard
Solution to be measured is spent, test result is as shown in table 3.
The comparison of 3 distinct methods of table
As shown in Table 3, commercially available negative potential pen irregular, the expensive test pen that is equal to class testing accuracy
1 accuracy is high, but low compared to the accuracy of cheap test pen 2 and 3, and the stability of data is also bad.The present invention
The measuring method accuracy of offer is higher, and stability is preferable.
To sum up, it the embodiment of the invention provides a kind of superior platinum nano-sized colloidal solution of high-concentration and stable, is used to prepare
The molten titrant for depositing density of hydrogen in water is measured, the nano platinum particle concentration of the platinum nano-sized colloidal solution is high, stability is superior, urges
Change performance is good, and the titrant reaction speed being prepared using the platinum nano-sized colloidal solution is fast, and stability is good, can effectively improve
Titrant measures the molten accuracy degree for depositing hydrogen and efficiency in water.
The embodiment of the invention also provides the molten titrant for depositing density of hydrogen, preparation method in a kind of measurement water and adopt
With the molten method for depositing density of hydrogen in titrant measurement water, which includes above-mentioned platinum nano-sized colloidal solution.The titration
Agent can quickly measure the density of hydrogen in solution, and the accuracy of measurement is high.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of superior platinum nano-sized colloidal solution of high-concentration and stable, which is characterized in that it is synthesized by following steps:
It is 1:(50~400 by volume ratio): platinum acid chloride solution, PVP ethanol solution and the distilled water of (10~100) mix, and add
The platinum nano-sized colloidal solution of brownish black is formed after thermal agitation；
Wherein, the initial concentration of the platinum acid chloride solution is 0.01~1gmL-1, the initial concentration of the PVP ethanol solution is 1
~30mgmL-1。
2. platinum nano-sized colloidal solution according to claim 1, which is characterized in that it is synthesized by following steps:
It is 1:(150~250 by volume ratio): platinum acid chloride solution, PVP ethanol solution and the distilled water of (30~50) mix, and add
The platinum nano-sized colloidal solution of brownish black is formed after thermal agitation；
Wherein, the initial concentration of the platinum acid chloride solution is 0.6~1gmL-1, the initial concentration of the PVP ethanol solution is 8
~15mgmL-1。
3. the molten titrant for depositing density of hydrogen in a kind of measurement water, which is characterized in that it includes: methylene blue ethanol solution with
And platinum nano-sized colloidal solution of any of claims 1 or 2.
4. titrant according to claim 3, which is characterized in that the initial concentration of the methylene blue ethanol solution is
0.5~12gL-1。
5. titrant according to claim 4, which is characterized in that in the titrant, the methylene blue ethyl alcohol is molten
The volume ratio of liquid and the platinum nano-sized colloidal solution is (4~51): 1.
6. titrant according to claim 5, which is characterized in that in the titrant, the methylene blue ethyl alcohol is molten
The volume ratio of liquid and the platinum nano-sized colloidal solution is (17~20): 1.
7. the preparation method of the molten titrant for depositing density of hydrogen in a kind of measurement water, which is characterized in that it includes platinum nano-colloid
The preparation step of solution；
It is 1:(50~400 that the preparation step of the platinum nano-sized colloidal solution, which includes: by volume ratio): the chloroplatinic acid of (10~100)
Solution, PVP ethanol solution and distilled water mix, and the platinum nano-sized colloidal solution of brownish black is formed after heating stirring；
Wherein, the concentration of the platinum acid chloride solution is 0.01~1gmL-1, the concentration of the PVP ethanol solution is 1~30mg
mL-1。
8. preparation method according to claim 7, which is characterized in that the preparation method include by volume ratio be (4~
51): 1 platinum nano-sized colloidal solution and 0.5~12gL-1The mixing of methylene blue ethanol solution.
9. a kind of molten method for depositing density of hydrogen in measurement water, which is characterized in that it includes by any one of claim 3~6 institute
The titrant stated titrates solution to be measured until solution to be measured from colourless becomes stable blue, records the drop that the titrant is added dropwise
Number N, and calculate the molten concentration for depositing hydrogen in water.
10. according to the method described in claim 9, it is characterized in that, calculation formula is when calculating density of hydrogenWherein, the volume of the solution to be measured takes 6mL, mHFor the hydrogen matter of every drop titrant consumption
Amount, CHFor the concentration of the hydrogen in aqueous solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811226162.1A CN109382047A (en) | 2018-10-19 | 2018-10-19 | Molten titrant for depositing density of hydrogen and preparation method thereof in a kind of superior platinum nano-sized colloidal solution of high-concentration and stable, measurement water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811226162.1A CN109382047A (en) | 2018-10-19 | 2018-10-19 | Molten titrant for depositing density of hydrogen and preparation method thereof in a kind of superior platinum nano-sized colloidal solution of high-concentration and stable, measurement water |
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|---|---|
| CN109382047A true CN109382047A (en) | 2019-02-26 |
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| CN201811226162.1A Pending CN109382047A (en) | 2018-10-19 | 2018-10-19 | Molten titrant for depositing density of hydrogen and preparation method thereof in a kind of superior platinum nano-sized colloidal solution of high-concentration and stable, measurement water |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105784794A (en) * | 2014-12-25 | 2016-07-20 | 大连中鼎化学有限公司 | Method for calibrating hydrogen concentration of hydrogen-rich water by redox potential |
-
2018
- 2018-10-19 CN CN201811226162.1A patent/CN109382047A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105784794A (en) * | 2014-12-25 | 2016-07-20 | 大连中鼎化学有限公司 | Method for calibrating hydrogen concentration of hydrogen-rich water by redox potential |
Non-Patent Citations (1)
| Title |
|---|
| 黎慧: "液相还原法制备Pt胶体粒子", 《天津理工大学学报》 * |
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