CN106932388B - A kind of Cr VI detection indicator solution, preparation method and its application method - Google Patents
A kind of Cr VI detection indicator solution, preparation method and its application method Download PDFInfo
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Abstract
The invention belongs to Cr VI field of fast detection, specially a kind of Cr VI detection indicator solution, preparation method and its application method, including diphenylcarbazide, solvent, pH adjusting agent and diluent；The solvent is the mixture of the two of one of dimethyl acetamide, dimethylformamide or any percent mass ratio.It effectively solves the technical problems such as current diphenylcarbazide process for preparation is cumbersome, dissolved efficiency is low, while improving the concentration of diphenylcarbazide in Cr VI indicator solution and increasing its validity period.
Description
Technical field
The invention belongs to Cr VI field of fast detection, specially a kind of Cr VI detection indicator solution, preparation method and
Its application method.
Background technique
Cr VI has very strong toxicity, and very big to human health damage, in modern industry, Cr VI is widely present in
In metal material, or polluted the environment in the form of solution etc..Cr VI indicator solution is applied to detection metal material, coating material
Material etc. whether there is Cr VI, while can carry out qualitative, quantitative measurement to content of 6-valence Cr ions in each medium.
In the prior art, has relevant report about Cr VI indicator solution, as Chinese patent CN104483307A is provided
Diphenylcarbazide is dissolved in methanol, ethyl alcohol, in acetone, lipid dissolution is added by a kind of configuration method of Cr VI developing solution
Agent adjusts acidity using sulfuric acid when in use, but it is in dissolution hexichol phosphinylidyne to increase its shelf-life
The equipment such as stirring auxiliary is needed when two hydrazines, and dissolution time at least needs 5 minutes, therefore increase its guarantor using lipid lytic agent
The matter phase.Chinese patent CN101900670A discloses the reagent of determining hexavalent chromium by spectrophotometry, uses dehydrated alcohol conduct
Lytic agent dissolve diphenylcarbazide, and using the concentrated sulfuric acid as acidulant adjust pH value, but itself the problem is that invention instead
It is long between seasonable, and concentrated sulfuric acid corrosivity is strong, and oxidisability is high, is easy to influence experimental result.Also there is Chinese patent CN1570607A
The special agent and preparation method of Cr VI, by 100 mg color developing agents, 1900 mg buffers and 2000 mg dispersing agents are protected from light and grind
Mill is uniformly mixed it.Wherein color developing agent is two navel of hexichol phosphinylidyne, and buffer is sulfosalicylic acid, and dispersing agent is sodium chloride, is used
0.1g standard sample spoon dispenses its mixture in capsule, after be put into bottle, seal, in refrigerator l-6 DEG C preservation, when in use
It takes portion to be dissolved in 10ml water, 5min is stood after mixed dissolution, Portable color comparator (for DR890 type) is used to measure, it is main suitable
For the portable measurement in non-laboratory.For another example Chinese patent CN102411001A provides one kind and quickly detects Cr VI in sewage
The method of ion, diphenylcarbazide is dissolved in acetone, and sulfuric acid phosphoric acid mixed liquor is as acidulant.Diphenylcarbazide is third
Solubility is lower in ketone and solution rate is slow, influences conventional efficient.
To sum up, in the prior art, that there are process for preparation is cumbersome, it is longer to prepare the time for Cr VI instruction liquid making method
Defect, specifically, indicator use diphenylcarbazide, and organic solvent mostly uses ethyl alcohol and acetone, and course of dissolution normally needs
1 h or more is wanted, 10-20 min is needed under physical agitation, considerably increases detection time.Meanwhile diphenylcarbazide is in second
Alcohol and the solubility in acetone are lower, cause diphenylcarbazide proportion in indicator system lower, affect sexavalence
The detection limit and detection effect of chromium.
Summary of the invention
The present invention provides a kind of Cr VI detection indicator solution, preparation method and its application method, effectively solves existing
The technical problems such as diphenylcarbazide process for preparation is cumbersome in technology, dissolved efficiency is low, while improving two in Cr VI indicator solution
The concentration of dinitrodiphenyl carbazide simultaneously increases its validity period.
To realize the above-mentioned technical purpose, the specific technical solution that the present invention takes is a kind of Cr VI detection indicator solution,
Including diphenylcarbazide, solvent, pH adjusting agent and diluent；The solvent is dimethyl acetamide, dimethylformamide
One of or any percent mass ratio the two mixture.
As the improved technical solution of the present invention, the pH adjusting agent is phosphoric acid.
As the improved technical solution of the present invention, diluent is ultrapure water.
As the improved technical solution of the present invention, the mass percent of each substance are as follows: diphenylcarbazide 0.5-3%, molten
Agent 20-30%, pH adjusting agent 20-60%, surplus are diluent.
As the improved technical solution of the present invention, the Cr VI that Cr VI detection indicator solution can be used for different medium quantitatively divides
Analysis.
Another object of the present invention is to provide a kind of preparation methods of Cr VI detection indicator solution, include the following steps:
Step 1: first diphenylcarbazide is dissolved in solvent, just solution is obtained；Step 2: disperse pH adjusting agent in diluent,
Obtain uniform mixed solution；Step 3: being added mixed solution into first solution, and will be shaken for being uniformly mixed up to solution,
Indicator solution is detected up to Cr VI.
Another object of the present invention is to provide a kind of application methods of Cr VI detection indicator solution, include the following steps:
When Cr VI detection indicator solution is for detecting the coat of metal with the presence or absence of Cr VI, Cr VI is taken to detect indicator solution with dropper,
And drip 1-2 drop Cr VI on the coat of metal and detect indicator solution, observe whether its liquid purple occurs, if metal coating surface goes out
Existing purple, then there are Cr VIs for the coat of metal, conversely, Cr VI is then not present；When Cr VI detection indicator solution is for detecting liquid
It when body sample, takes Cr VI to detect indicator solution with dropper, 1-2 drop Cr VI is dripped into fluid sample and detects indicator solution, observes liquid
Body sample is instilling at Cr VI detection indicator solution whether purple occur, if there is purple, there are Cr VIs in fluid sample.
Beneficial effect
Indicator of the diphenylcarbazide as Cr VI in the application can be shown obvious with Cr VI complexing colour developing
Purple effect, convenient for observation colour developing phenomenon；Dimethyl acetamide, dimethylformamide want the solubility of diphenylcarbazide
Much higher than common solvent ethyl alcohol and acetone, a large amount of diphenylcarbazide, regular quality (1 g can be dissolved in the shorter time
Left and right) diphenylcarbazide dissolution time less than 10 s, and in course of dissolution without stirring, shorten indicator solution prepare when
Between；Use phosphoric acid for diluent, for phosphoric acid without strong oxidizing property, no strong corrosive can be to avoid acid with strong oxidizing property to measurement result
Interference, compared to sulfuric acid, nitric acid using safe, while phosphoric acid has good corrosivity to the coat of metal, being capable of corrosion dissolution
Cr VI in coating material out；Impurity metal ion is free of in ultrapure water, can substantially reduce third party's factor and experiment is tied
The interference of fruit, by the dilution of ultrapure water, Cr VI detection indicator solution can achieve the optimal item of diphenylcarbazide chromogenic reaction
Part；And be greater than 7 days the validity period of the Cr VI prepared detection indicator solution.
To sum up, the Cr VI detection indicator solution of the application effectively solve current Cr VI detection indicator solution process for preparation it is numerous
Trivial, the low lamp technical problem of dissolved efficiency, while improving the concentration of diphenylcarbazide in Cr VI indicator solution and increasing it effectively
Phase.
Detailed description of the invention
Fig. 1: the standard curve schematic diagram of gained Cr VI indicator determination of hexavalent chromium in the embodiment of the present invention 3.
Specific embodiment
To keep purpose and the technical solution of the embodiment of the present invention clearer, below in conjunction with the attached of the embodiment of the present invention
Figure, is clearly and completely described the technical solution of the embodiment of the present invention.Obviously, described embodiment is of the invention
A part of the embodiment, instead of all the embodiments.Based on described the embodiment of the present invention, those of ordinary skill in the art
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of being not necessarily to creative work.
Those skilled in the art of the present technique are appreciated that unless otherwise defined, all terms used herein (including technology art
Language and scientific term) there is meaning identical with the general understanding of those of ordinary skill in fields of the present invention.Should also
Understand, those terms such as defined in the general dictionary, which should be understood that, to be had and the meaning in the context of the prior art
The consistent meaning of justice, and unless defined as here, it will not be explained in an idealized or overly formal meaning.
A kind of Cr VI detection indicator solution, including diphenylcarbazide, solvent, pH adjusting agent and diluent；Each substance
Mass percent are as follows: diphenylcarbazide 0.5-3%, solvent 20-30%, pH adjusting agent 20-60%, surplus are diluent.It is excellent
It is selected as the mass percent of each substance are as follows: diphenylcarbazide 1-3%, solvent 20-25%, pH adjusting agent 40-50%, surplus are dilute
Release agent.The mass percent of more preferably each substance are as follows: diphenylcarbazide 1-2%, solvent 20-25%, pH adjusting agent 40-
50%, surplus is diluent.
This patent is using dimethylformamide with dimethyl acetamide as the organic molten of indicator (diphenylcarbazide)
Agent replaces traditional solvent acetone and ethyl alcohol, overcomes that traditional Cr VI detection indicator solution dissolution time is long, validity period is short
Disadvantage.Specifically contain ketone group for diphenylcarbazide, is in polarity, and dimethylformamide, dimethyl acetamide are that polarity is molten
Agent, and polarity is better than ethyl alcohol acetone, according to similar compatibility principle, diphenylcarbazide is more soluble in dimethylformamide, diformazan
Yl acetamide.And in ethanol, since ethyl alcohol is protonic solvent, ketone group is oxidized easily, so as to cause indicator solution failure, and
Dimethylformamide and dimethyl acetamide are aprotic solvents, and contain aldehyde radical, and aldehyde radical is easier to be oxidized compared to ketone group,
So diphenylcarbazide is dissolved in dimethylformamide, dimethyl acetamide and can save longer time (> 7 days).
The present invention avoids acid with strong oxidizing property from doing measurement result as acidulant using phosphoric acid with no strong oxidizing property
It disturbs, no strong corrosive, compared to sulfuric acid, nitric acid, uses safe advantage.
A kind of preparation method of Cr VI detection indicator solution, includes the following steps: Step 1: first that diphenylcarbazide is molten
In solvent, just solution is obtained；Step 2: dispersing pH adjusting agent in diluent, uniform mixed solution is obtained；Step
Three, mixed solution is added into first solution, and will be shaken for until solution, which is uniformly mixed, detects indicator solution to get Cr VI.
A kind of application method of Cr VI detection indicator solution includes the following steps: when Cr VI detection indicator solution is for examining
When surveying the coat of metal with the presence or absence of Cr VI, Cr VI is taken to detect indicator solution with dropper, and drip 1-2 drop sexavalence on the coat of metal
Chromium detects indicator solution, observes whether its liquid purple occurs, if purple occurs in metal coating surface, there are sexavalences for the coat of metal
Chromium, conversely, Cr VI is then not present；When Cr VI detection indicator solution with dropper for taking Cr VI to examine when detecting fluid sample
Indicator solution is surveyed, and drips 1-2 drop Cr VI into fluid sample and detects indicator solution, observation fluid sample refers in instillation Cr VI detection
Show at liquid whether purple occur, if there is purple, there are Cr VIs in fluid sample.
On the other hand, Cr VI of the invention detection indicator solution can be used for the Cr VI quantitative analysis of different medium.
Embodiment 1
Organic solvent is dimethyl acetamide, and the percent mass ratio of each component is 0.5% diphenylcarbazide；30%
Organic reagent；60% orthophosphoric acid, remaining is ultrapure water.Diphenylcarbazide is added in dimethyl acetamide, is shaken several seconds with hand
It can dissolve, add the mixed liquor of orthophosphoric acid and ultrapure water, rock uniformly.The Cr VI detection instruction drop completed will be prepared
The metal coating surface containing Cr VI is added to, the liquid of dropwise addition is observed after 2 min, becomes purple from colorless and transparent, it was demonstrated that
It is effective that the Cr VI detects indicator solution.
Embodiment 2
Organic solvent is dimethylformamide, and the percent mass ratio of each component is 3% diphenylcarbazide；10% has
Machine reagent；20% orthophosphoric acid, remaining is ultrapure water.Diphenylcarbazide is added in dimethylformamide, shakes several seconds i.e. with hand
It can dissolve, add orthophosphoric acid, ultrapure water is added after mixing and rocks uniformly.The Cr VI completed will be prepared and detect instruction
Drop adds to the metal coating surface containing Cr VI, and the liquid of dropwise addition is observed after 2 min, becomes purple from colorless and transparent,
Prove that Cr VI detection indicator solution is effective.
Embodiment 3
Organic solvent is dimethylformamide and dimethyl acetamide mixed solvent, and the percent mass ratio of each component is 1 %
Diphenylcarbazide；10% dimethylformamide；10% dimethyl acetamide；50% orthophosphoric acid, remaining is ultrapure water.It will
Dimethylformamide is mixed in proportion with dimethyl acetamide, then mixed organic solvent is added in diphenylcarbazide
In, it can dissolve with hand shake several seconds, the mixed liquor of orthophosphoric acid and ultrapure water be then added, rocks uniformly and is kept in dark place.It will
The Cr VI detection indicator solution of preparation is used for Cr VI quantitative detection.
Embodiment 4
Organic solvent is ethyl alcohol, and the percent mass ratio of each component is 0.5% diphenylcarbazide；25% ethyl alcohol；50%
Orthophosphoric acid, remaining is ultrapure water.Diphenylcarbazide is added in organic solvent, then positive phosphorus is added in stirring half an hour dissolution
The mixed liquor of acid and ultrapure water rocks uniformly.The Cr VI detection indicator solution of preparation is kept in dark place.
Cr VI detection indicator solution prepared by embodiment 3 and embodiment 4 is protected from light and is saved with shady place, Yu Yitian, three
It, Cr VI quantitative detection is used for after seven days, the Cr VI detection indicator solution prepared by embodiment 4 fails after 1 day, and implements
Cr VI detection indicator solution prepared by example 3 is used equally for Cr VI quantitative detection in 7 days, and validity period is greater than 7 days.
Reach 0.999 or more according to the standard curve linear coefficient of 3 gained indicator determination of hexavalent chromium of optimum embodiment, it is full
The requirement of sufficient content of 6-valence Cr ions measurement.See Fig. 1.Data see the table below 1.
The standard solution absorbance data of 1 optimum embodiment of table, 3 gained indicator determination of hexavalent chromium
| Serial number | Chromium standard solution concentration (mg/L) | Absorbance (Abs) |
| 1 | 0 | 0 |
| 2 | 0.033 | 0.02 |
| 3 | 0.059 | 0.04 |
| 4 | 0.086 | 0.06 |
| 5 | 0.116 | 0.08 |
| 6 | 0.136 | 0.1 |
| 7 | 0.276 | 0.2 |
The above is only embodiments of the present invention, and the description thereof is more specific and detailed, and but it cannot be understood as right
The limitation of the invention patent range.It should be pointed out that for those of ordinary skill in the art, not departing from the present invention
Under the premise of design, various modifications and improvements can be made, these are all belonged to the scope of protection of the present invention.
Claims (6)
1. a kind of Cr VI detects indicator solution, including diphenylcarbazide, solvent, pH adjusting agent and diluent；Its feature exists
In the solvent is the mixing of the two of one of dimethyl acetamide, dimethylformamide or any percent mass ratio
Object；The pH adjusting agent is phosphoric acid.
2. a kind of Cr VI according to claim 1 detects indicator solution, which is characterized in that diluent is ultrapure water.
3. a kind of Cr VI according to claim 1 or 2 detects indicator solution, which is characterized in that the quality percentage of each substance
Than are as follows: diphenylcarbazide 0.5-3%, solvent 20-30%, pH adjusting agent 20-60%, surplus are diluent.
4. a kind of Cr VI according to claim 1 or 2 detects indicator solution, which is characterized in that Cr VI detects indicator solution
It can be used for the Cr VI quantitative analysis of different medium.
5. a kind of preparation method of Cr VI detection indicator solution as claimed in claim 1 or 2, which is characterized in that including as follows
Step: Step 1: first diphenylcarbazide is dissolved in solvent, just solution is obtained；Step 2: dispersing dilution for pH adjusting agent
In agent, uniform mixed solution is obtained；Step 3: being added mixed solution into first solution, and will be shaken for until solution mixes
Uniformly indicator solution is detected to get Cr VI.
6. a kind of application method of Cr VI detection indicator solution as claimed in claim 1 or 2, which is characterized in that work as Cr VI
When detection indicator solution is for detecting the coat of metal with the presence or absence of Cr VI, Cr VI is taken to detect indicator solution with dropper, to metal-plated
1-2 drop Cr VI is dripped on layer and detects indicator solution, observes whether its liquid purple occurs, if there is purple in metal coating surface,
There are Cr VIs for the coat of metal, conversely, Cr VI is then not present；When Cr VI detection indicator solution is used to detect fluid sample,
It takes Cr VI to detect indicator solution with dropper, and drips 1-2 drop Cr VI into fluid sample and detect indicator solution, observation fluid sample exists
It instills at Cr VI detection indicator solution and whether purple occurs, if there is purple, there are Cr VIs in fluid sample.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104148009A (en) * | 2014-06-17 | 2014-11-19 | 厦门出入境检验检疫局检验检疫技术中心 | Composite bentonite material capable of quickly identifying hexavalent chromium ions in water with naked eyes as well as preparation method and application of material |
| CN104830312A (en) * | 2015-04-07 | 2015-08-12 | 济南大学 | Fluorescence-enhanced probe compound preparation method and trivalent chromium ion detection method |
| CN106248641A (en) * | 2016-07-17 | 2016-12-21 | 徐伟鹏 | Chromic fluorescent optical sensor of a kind of detection and preparation method thereof |
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| KR101290508B1 (en) * | 2011-10-28 | 2013-07-26 | 현대제철 주식회사 | Test sheet for analysis of hexavalent chromium and method for manufacturing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104148009A (en) * | 2014-06-17 | 2014-11-19 | 厦门出入境检验检疫局检验检疫技术中心 | Composite bentonite material capable of quickly identifying hexavalent chromium ions in water with naked eyes as well as preparation method and application of material |
| CN104830312A (en) * | 2015-04-07 | 2015-08-12 | 济南大学 | Fluorescence-enhanced probe compound preparation method and trivalent chromium ion detection method |
| CN106248641A (en) * | 2016-07-17 | 2016-12-21 | 徐伟鹏 | Chromic fluorescent optical sensor of a kind of detection and preparation method thereof |
Non-Patent Citations (1)
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| 《环境样品中六价铬的光度法测定》;蔡慧华等;《广东化工》;20061231;第33卷(第154期);正文第50页 * |
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