CN103018183A - Kit and method used for monitoring hexavalent chromium online - Google Patents
Kit and method used for monitoring hexavalent chromium online Download PDFInfo
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- CN103018183A CN103018183A CN2011102839120A CN201110283912A CN103018183A CN 103018183 A CN103018183 A CN 103018183A CN 2011102839120 A CN2011102839120 A CN 2011102839120A CN 201110283912 A CN201110283912 A CN 201110283912A CN 103018183 A CN103018183 A CN 103018183A
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Abstract
The invention discloses a kit and a method used for monitoring hexavalent chromium online. The kit is composed of a sulfuric acid and phosphoric acid solution and a chromogenic agent solution. The sulfuric acid and phosphoric acid solution comprises concentrated sulfuric acid, concentrated phosphoric acid, and water with a volume ratio of (0.5-1.5):(0.5-1.5):(135-160). The chromogenic agent solution comprises a chromogenic agent, anhydrous ethanol, and water. According to the invention, the chromogenic agent is dissolved by using anhydrous ethanol, such that an acetone solvent is not needed, and the kit is environment-friendly. Also, the acid content in the kit provided by the invention is low, such that a monitoring result is ensured, harm brought by acid upon human body is reduced, and resource is saved. The invention also provides a method used for monitoring hexavalent chromium. According to the method, only two reagents which are the sulfuric acid and phosphoric acid solution and the chromogenic agent solution are needed. Compared with prior arts that three reagents are respectively fed, error caused by wide range of feed of an online monitoring instrument is reduced, and a monitoring result is accurate.
Description
Technical field
The present invention relates to the on-line monitoring technique field, more particularly, relate to a kind of be used to monitoring chromic kit and method.
Background technology
Chromium is one of necessary trace element of biosome, and chromium deficiency can cause the metabolic disorder of the materials such as sugar, fat, and still, the too high meeting of cr intake brings adverse effect to biological and the mankind.The toxicity of chromium and the form of its existence have very large relation, mainly exist with trivalent chromium and chromic form at occurring in nature chromium, in general, chromic toxicity is that trivalent chromium is more than 100 times, wherein, trivalent chromium stable chemical nature and almost non-toxic is the essential element of human body and animal; On the contrary, the chemical property of hexavalent chromium compound is active, usually exists with ionic species, and strong oxidizing property and larger toxicity are arranged, and human body is had extremely strong carcinogenic and mutagenesis characteristic.China's water environment quality standard has strict restriction to sexavalent chrome, sexavalent chrome belongs to first kind pollutant in the integrated wastewater discharge standard, trivalent chromium maximum permissible concentration in the day water is 0.5mg/L, sexavalent chrome is 0.1mg/L, the maximum permissible concentration of sexavalent chrome in drinking water is 0.05mg/L, the content of 6-valence Cr ions of therefore, accurately monitoring in the water has important practical significance.
At present, chromic monitoring method mainly comprises spectrophotometric method, dynamics photometry and flow injection photometry etc., and wherein, spectrophotometric method is to being main monitoring method.In addition, compare the laboratory and detect sexavalent chrome, the on-line monitoring instrument can be realized hexavalent chromium polluted situation in the unattended long term monitoring water quality.In the prior art, take the on-line monitoring instrument as monitoring device, utilize the chromic kit in the water by Spectrophotometry matter to comprise at least sulfuric acid solution, phosphoric acid solution, developer and acetone etc.In the mentioned reagent box, because acetone has toxicity, thereby bring harm and polluted environment to human body; In addition, the acid content of mentioned reagent box is larger, has wasted resource when easily bringing harm to human body; And, utilizing the mentioned reagent box to carry out in the process of on-line monitoring, sulfuric acid solution, phosphoric acid solution and developer are distinguished sample introductions as three kinds of reagent, thereby can bring considerable influence to the monitoring result of on-line monitoring instrument, and error is larger.
Summary of the invention
In view of this, it is a kind of be used to monitoring chromic kit that the technical problem to be solved in the present invention is to provide, and it is less as solvent and acid content that this kit need not acetone.In addition, it is a kind of be used to monitoring chromic method that the technical matters that the present invention also solves also is to provide, and the method monitoring result is accurate.
In order to solve above technical matters, the invention provides a kind of be used to monitoring chromic kit, be comprised of sulphur phosphoric acid solution and chromogenic reagent solution, described sulphur phosphoric acid solution comprises that volume ratio is (0.5～1.5): (0.5～1.5): the concentrated sulphuric acid of (135～160), strong phosphoric acid and water; Described chromogenic reagent solution comprises developer, absolute ethyl alcohol and water.
Preferably, the mass volume ratio of developer and water is (0.05～0.1g): 1L in the described chromogenic reagent solution.
Preferably, the mass volume ratio of developer and water is 0.08g: 1L in the described chromogenic reagent solution.
Preferably, described sulphur phosphoric acid solution comprises that volume ratio is 1: 1: 148 the concentrated sulphuric acid, strong phosphoric acid and water.
Preferably, the volume ratio of described sulphur phosphoric acid solution and chromogenic reagent solution is 1: (1～2).
Preferably, described developer is diphenylcarbazide, and the concentration of the described concentrated sulphuric acid is 98%, and the concentration of described strong phosphoric acid is 85%.
Accordingly, it is a kind of be used to monitoring chromic method that the present invention also provides, and may further comprise the steps:
Take the on-line monitoring instrument as monitoring device, the sulphur phosphoric acid solution is contacted with water sample to be detected with chromogenic reagent solution, and described sulphur phosphoric acid solution comprises that volume ratio is (0.5～1.5): (0.5～1.5): the concentrated sulphuric acid of (135～160), strong phosphoric acid and water; Described chromogenic reagent solution comprises developer, absolute ethyl alcohol and water;
The absorbance of monitoring chromogenic reagent solution changes, and determines the content of 6-valence Cr ions in the water sample to be detected.
Preferably, the volume ratio of described sulphur phosphoric acid solution, chromogenic reagent solution and water sample to be detected is (1～2): (1～2): (1～2).
Preferably, the volume ratio of described sulphur phosphoric acid solution, chromogenic reagent solution and water sample to be detected is 1: 1: 1.
Preferably, described sulphur phosphoric acid solution comprises that volume ratio is 1: 1: 148 the concentrated sulphuric acid, strong phosphoric acid and water.
The invention provides a kind of be used to monitoring chromic kit, be comprised of sulphur phosphoric acid solution and chromogenic reagent solution, described sulphur phosphoric acid solution comprises that volume ratio is (0.5～1.5): (0.5～1.5): the concentrated sulphuric acid of (135～160), strong phosphoric acid and water; Described chromogenic reagent solution comprises developer, absolute ethyl alcohol and water.Compared with prior art, the present invention adopts the anhydrous alcohol solution developer, need not acetone as solvent, and is more friendly to environment.And kit acid content provided by the invention is less, when having guaranteed monitoring result, reduces acid and brings harm to human body, has saved resource.
Accordingly, the present invention provides also that a kind of the method only needs sulphur phosphoric acid solution and two kinds of reagent of chromogenic reagent solution be used to monitoring chromic method, with in the prior art with three kinds of reagent respectively sample introduction compare, reduced the on-line monitoring instrument owing to the sample introduction error that produces of a great variety, monitoring result is accurate.
Embodiment
The below is clearly and completely described the technical scheme in the embodiment of the invention, and obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that obtains under the creative work prerequisite.
The invention discloses a kind of be used to monitoring chromic kit, be comprised of sulphur phosphoric acid solution and chromogenic reagent solution, described sulphur phosphoric acid solution comprises that volume ratio is (0.5～1.5): (0.5～1.5): the concentrated sulphuric acid of (135～160), strong phosphoric acid and water; Described chromogenic reagent solution comprises developer, absolute ethyl alcohol and water.In chromic mensuration, prior art mainly with acetone as solvent, the Main Function of acetone is the dissolving developer, and the existence of acetone for the reaction of sexavalent chrome and developer without impact.The present invention adopts absolute ethyl alcohol as solvent, and the reaction for sexavalent chrome and developer when can dissolve developer there is no impact.The more important thing is, as the reagent of sexavalent chrome on-line monitoring, absolute ethyl alcohol is far smaller than acetone to the impact of environment, and is more friendly to environment.
As preferred implementation, described sulphur phosphoric acid solution comprises that volume ratio is 1: 1: 148 the concentrated sulphuric acid, strong phosphoric acid and water; The volume ratio of described sulphur phosphoric acid solution and chromogenic reagent solution is preferably 1: (1～2), more preferably 1: 1.The purity of the concentrated sulphuric acid that the present invention adopts is preferably the AR level, most preferably is the GR level, and concentration is 98%; The purity of described strong phosphoric acid is preferably the AR level, most preferably is the GR level, and concentration is 85%.
Compared with prior art, kit provided by the invention has reduced sour use amount, and acidity is less, thereby when having guaranteed monitoring result, has reduced acid and brought harm to human body, has saved resource.
The developer that the present invention adopts is preferably diphenylcarbazide, but is not limited only to this.When containing sexavalent chrome in the water sample to be detected, under acid condition, sexavalent chrome can form mauve complex with hexichol phosphinylidyne two traps, and this complex has characteristic absorption peak at the 540nm place, is used for detecting chromic concentration.The mass volume ratio of developer and water is preferably (0.05～0.1g): 1L, more preferably 0.08g:1L in the described chromogenic reagent solution.The present invention has changed the concentration of developer in the classic method, has namely adopted the developer of low concentration, thereby has avoided in to chromic observation process because the residual error of bringing of high concentration developer.In addition, include the water of certain content in described sulphur phosphoric acid solution and the described chromogenic reagent solution, it is preferably the water that pure water or ultrapure water etc. do not contain chromium ion.
Of the present inventionly preferably be prepared as follows be used to monitoring chromic kit: the concentrated sulphuric acid, strong phosphoric acid and water are (0.5～1.5) by volume: (0.5～1.5): mix (135～160), obtains the sulphur phosphoric acid solution; Developer, absolute ethyl alcohol and water are mixed, obtain chromogenic reagent solution.
Accordingly, it is a kind of be used to monitoring chromic method that the present invention also provides, and may further comprise the steps:
Take the on-line monitoring instrument as monitoring device, the sulphur phosphoric acid solution is contacted with water sample to be detected with chromogenic reagent solution, and described sulphur phosphoric acid solution comprises that volume ratio is (0.5～1.5): (0.5～1.5): the concentrated sulphuric acid of (135～160), strong phosphoric acid and water; Described chromogenic reagent solution comprises developer, absolute ethyl alcohol and water;
The absorbance of monitoring chromogenic reagent solution changes, and determines the content of 6-valence Cr ions in the water sample to be detected.
Above-mentioned to chromic observation process in, the volume ratio of described sulphur phosphoric acid solution, chromogenic reagent solution and water sample to be detected is preferably (1～2): (1～2): (1～2), preferred, the volume ratio of described sulphur phosphoric acid solution, chromogenic reagent solution and water sample to be detected is 1: 1: 1.Wherein, volume of water sample is one of important factor in the sexavalent chrome observation process, and volume of water sample is excessive or too small, all can cause the accuracy of chromic monitoring is descended.The reagent and the inconsistent problem of water sample sample size that exist for the chromic method of water by Spectrophotometry matter in the open source literature, the present invention changes the sample introduction ratio of reagent concentration and water sample to be detected, most preferably making the volume ratio of sulphur phosphoric acid solution, chromogenic reagent solution and water sample to be detected is 1: 1: 1, has solved the on-line monitoring instrument because the relatively less error that produces of reagent sample size.
As preferred implementation, described sulphur phosphoric acid solution comprises that volume ratio is 1: 1: 148 the concentrated sulphuric acid, strong phosphoric acid and water; The volume ratio of described sulphur phosphoric acid solution and chromogenic reagent solution is preferably 1: (1～2), more preferably 1: 1.
In the present invention, this is monitored chromic method and only needs sulphur phosphoric acid solution and two kinds of reagent of chromogenic reagent solution, with in the prior art with three kinds of reagent respectively sample introduction compare, reduced the on-line monitoring instrument because the sample introduction error that produces of a great variety, convenient and swift, monitoring result is accurate.
In order to further specify technical scheme of the present invention, below in conjunction with embodiment the preferred embodiment of the invention is described, but should be appreciated that these describe just as further specifying the features and advantages of the present invention, rather than to the restriction of claim of the present invention.
The chemical reagent that adopts in the embodiment of the invention is commercial.
Embodiment 1
The raw materials that is used for monitoring chromic kit is: concentration is that 98% the concentrated sulphuric acid, concentration are 85% strong phosphoric acid, absolute ethyl alcohol, developer (diphenylcarbazide) and pure water.
The preparation of sulphur phosphoric acid solution: pipette respectively the concentrated sulphuric acid, strong phosphoric acid is dissolved in a small amount of pure water, places the 1000ml volumetric flask, uses the pure water constant volume, mixing is for subsequent use, and the volume ratio of the described concentrated sulphuric acid, strong phosphoric acid and pure water is 1: 1: 148;
The preparation of chromogenic reagent solution: accurately take by weighing developer (diphenylcarbazide) and be dissolved in the absolute ethyl alcohol, be stirred to fully dissolving, add again the pure water dilution, be settled to 1000ml, mixing, be kept in the brown volumetric flask for subsequent usely, the mass volume ratio of described developer (diphenylcarbazide) and pure water is 0.08g:1L;
The drafting of typical curve: the chromium standard solution that accurately pipette 0,0.5,1,1.5,2.0,2.5,3.0,3.5,4.0,4.5,5.0ml concentration is 1mg/L is in the 25ml color comparison tube, add 5ml sulphur phosphoric acid, shake up, add pure water and be settled to 10ml, fully shake up, add the 5ml chromogenic reagent solution, shake up, left standstill 3 minutes, take ultrapure water as blank reference, with the cuvette of 30mm light path, measure absorbance and drawing standard curve at 540nm wavelength place.
Embodiment 2,
With the online water quality sexavalent chrome monitor automatic sucking 5ml of Tianrui water white transparency water sample, 0.5mg/L chromium mark liquid 5ml, automatic sucking 5ml sulphur phosphoric acid solution successively again, the 5ml chromogenic reagent solution, fully after the reaction, in the cuvette of 30mm light path, absorbance is measured at 540nm wavelength place, and the result of seven measurements is respectively 0.497,0.499,0.498,0.499,0.500,0.500,0.500, and relative standard deviation RSD is 0.214%.
By the present embodiment as seen, adopt the chromic kit monitoring of the monitoring sexavalent chrome of the present invention's preparation, measured result precision, accuracy are all fine, have solved because the residual error of bringing of auto injection pipeline.
Embodiment 3
With the online water quality sexavalent chrome monitor automatic sucking 5ml of Tianrui water white transparency water sample, 0.04mg/L chromium mark liquid 5ml, automatic sucking 5ml sulphur phosphoric acid solution successively again, the 5ml chromogenic reagent solution, fully after the reaction, in the cuvette of 30mm light path, absorbance is measured at 540nm wavelength place, and the result of seven measurements is respectively 0.037,0.037,0.037,0.038,0.037,0.038,0.037.
By the present embodiment as seen, adopt agents useful for same of the present invention and water sample that proportioning is surveyed to detect lower limit and be low to moderate 0.04mg/L, reach the GB requirement.
Embodiment 4
With the online water quality sexavalent chrome monitor automatic sucking 5ml of Tianrui water white transparency water sample, 5mg/L chromium mark liquor 5ml, automatic sucking 5ml sulphur phosphoric acid solution successively again, the 5ml chromogenic reagent solution, fully after the reaction, in the cuvette of 30mm light path, absorbance is measured at 540nm wavelength place, and the result of seven measurements is respectively 4.993,5.032,5.025,5.025,5.032,5.032,5.032, and RSD is 0.262%.
From then on as seen example adopts agents useful for same of the present invention and water sample that proportioning is surveyed to detect the upper limit and can up to 5mg/L, can solve the full-automatic on-line monitoring problem that industrial waste water etc. contains the higher water quality of sexavalent chrome.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be apparent concerning those skilled in the art, and General Principle as defined herein can be in the situation that do not break away from the spirit or scope of the present invention, in other embodiments realization.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. one kind is used for monitoring chromic kit, is comprised of sulphur phosphoric acid solution and chromogenic reagent solution, and described sulphur phosphoric acid solution comprises that volume ratio is (0.5～1.5): (0.5～1.5): the concentrated sulphuric acid of (135～160), strong phosphoric acid and water; Described chromogenic reagent solution comprises developer, absolute ethyl alcohol and water.
2. kit according to claim 1 is characterized in that, the mass volume ratio of developer and water is (0.05～0.1g): 1L in the described chromogenic reagent solution.
3. kit according to claim 2 is characterized in that, the mass volume ratio of developer and water is 0.08g:1L in the described chromogenic reagent solution.
4. kit according to claim 1 is characterized in that, described sulphur phosphoric acid solution comprises that volume ratio is 1: 1: 148 the concentrated sulphuric acid, strong phosphoric acid and water.
5. kit according to claim 1 is characterized in that, the volume ratio of described sulphur phosphoric acid solution and chromogenic reagent solution is 1: (1～2).
6. kit according to claim 1 is characterized in that, described developer is diphenylcarbazide, and the concentration of the described concentrated sulphuric acid is 98%, and the concentration of described strong phosphoric acid is 85%.
7. one kind is used for monitoring chromic method, may further comprise the steps:
Take the on-line monitoring instrument as monitoring device, the sulphur phosphoric acid solution is contacted with water sample to be detected with chromogenic reagent solution, and described sulphur phosphoric acid solution comprises that volume ratio is (0.5～1.5): (0.5～1.5): the concentrated sulphuric acid of (135～160), strong phosphoric acid and water; Described chromogenic reagent solution comprises developer, absolute ethyl alcohol and water;
The absorbance of monitoring chromogenic reagent solution changes, and determines the content of 6-valence Cr ions in the water sample to be detected.
8. method according to claim 1 is characterized in that, the volume ratio of described sulphur phosphoric acid solution, chromogenic reagent solution and water sample to be detected is (1～2): (1～2): (1～2).
9. method according to claim 8 is characterized in that, the volume ratio of described sulphur phosphoric acid solution, chromogenic reagent solution and water sample to be detected is 1: 1: 1.
10. method according to claim 1 is characterized in that, described sulphur phosphoric acid solution comprises that volume ratio is 1: 1: 148 the concentrated sulphuric acid, strong phosphoric acid and water.
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| CN2011102839120A CN103018183A (en) | 2011-09-22 | 2011-09-22 | Kit and method used for monitoring hexavalent chromium online |
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| CN2011102839120A CN103018183A (en) | 2011-09-22 | 2011-09-22 | Kit and method used for monitoring hexavalent chromium online |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104007078A (en) * | 2014-06-18 | 2014-08-27 | 宁波市环境监测中心 | Method for rapidly detecting total concentration of chromium in water and detection kit |
| CN105223147A (en) * | 2015-10-19 | 2016-01-06 | 攀钢集团攀枝花钢铁研究院有限公司 | The assay method of content of 6-valence Cr ions in chromium type high iron ore |
| CN106092921A (en) * | 2016-05-31 | 2016-11-09 | 无锡伊佩克科技有限公司 | The detection method of hexavalent chromium content in a kind of passivating solution |
| CN106770249A (en) * | 2016-12-28 | 2017-05-31 | 云南昆钢水净化科技有限公司 | A kind of water quality Cr VI mixed color developing agent and its compound method |
| CN110672540A (en) * | 2019-11-19 | 2020-01-10 | 长春黄金研究院有限公司 | Method for determining hexavalent chromium in solid waste |
| CN112630172A (en) * | 2020-11-26 | 2021-04-09 | 宝钢湛江钢铁有限公司 | Method for monitoring concentration of hexavalent chromium in high-content chromium-containing wastewater |
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| CN101900670A (en) * | 2010-05-25 | 2010-12-01 | 深圳市清时捷科技有限公司 | Reagent for determining hexavalent chromium by spectrophotometry |
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| CN101900670A (en) * | 2010-05-25 | 2010-12-01 | 深圳市清时捷科技有限公司 | Reagent for determining hexavalent chromium by spectrophotometry |
Non-Patent Citations (1)
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| 国家环境保护局规划标准处，北京市环境监测中心，尚邦懿，: "《GB/7467-87：中华人民共和国国家标准-水质六价铬的测定二苯碳酰二肼分光光度法》", 1 August 1987 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104007078A (en) * | 2014-06-18 | 2014-08-27 | 宁波市环境监测中心 | Method for rapidly detecting total concentration of chromium in water and detection kit |
| CN104007078B (en) * | 2014-06-18 | 2016-09-14 | 宁波市环境监测中心 | Total chromium method for quick and detection kit in a kind of water |
| CN105223147A (en) * | 2015-10-19 | 2016-01-06 | 攀钢集团攀枝花钢铁研究院有限公司 | The assay method of content of 6-valence Cr ions in chromium type high iron ore |
| CN106092921A (en) * | 2016-05-31 | 2016-11-09 | 无锡伊佩克科技有限公司 | The detection method of hexavalent chromium content in a kind of passivating solution |
| CN106770249A (en) * | 2016-12-28 | 2017-05-31 | 云南昆钢水净化科技有限公司 | A kind of water quality Cr VI mixed color developing agent and its compound method |
| CN110672540A (en) * | 2019-11-19 | 2020-01-10 | 长春黄金研究院有限公司 | Method for determining hexavalent chromium in solid waste |
| CN112630172A (en) * | 2020-11-26 | 2021-04-09 | 宝钢湛江钢铁有限公司 | Method for monitoring concentration of hexavalent chromium in high-content chromium-containing wastewater |
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Application publication date: 20130403 |