CN106770249A - A kind of water quality Cr VI mixed color developing agent and its compound method - Google Patents

A kind of water quality Cr VI mixed color developing agent and its compound method Download PDF

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Publication number
CN106770249A
CN106770249A CN201611238809.3A CN201611238809A CN106770249A CN 106770249 A CN106770249 A CN 106770249A CN 201611238809 A CN201611238809 A CN 201611238809A CN 106770249 A CN106770249 A CN 106770249A
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China
Prior art keywords
color developing
mixed color
water
developing agent
water quality
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CN201611238809.3A
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Chinese (zh)
Inventor
张燕玲
张海涛
史花丽
杨雪景
曹海燕
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Yunnan Kunming Iron & Steel Water Purification Technology Co Ltd
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Yunnan Kunming Iron & Steel Water Purification Technology Co Ltd
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Priority to CN201611238809.3A priority Critical patent/CN106770249A/en
Publication of CN106770249A publication Critical patent/CN106770249A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N2021/775Indicator and selective membrane

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The present invention discloses a kind of water quality Cr VI mixed color developing agent and its compound method, and following component is contained in every 100mL mixed color developing agents:Diphenylcarbazide 0.2g, ethanol 70mL, 6~12mL of SPA, 18~24mL of water.The present invention replaces acetone with ethanol as solvent, environmentally friendly and harmless to the human body, does not pollute the environment.When developer of the invention is used, it is measured by being directly added into after 2mL mixed color developing agents, and adds SPA to carry out Controlled acidity in mixed color developing agent, the influence that ferric iron in water sample is determined to content of 6-valence Cr ions can be eliminated, this invention simplifies operating procedure is determined, accuracy is determined high.

Description

A kind of water quality Cr VI mixed color developing agent and its compound method
Technical field
The present invention relates to a kind of water quality Cr VI mixed color developing agent and its compound method, belong to water quality Cr VI detection technique Field.
Background technology
The valence state that the compound of chromium is common has trivalent and sexavalence.Murder by poisoning of the Cr VI to health is very big, to fish, three The toxicity of valency chromium compound is bigger than Cr VI.In water body, Cr VI is typically with CrO4 2-、Cr2O7 2-、HCrO4 -Three kinds of anion Form is present, and is influenceed by the condition such as pH value, organic matter, redox materials, temperature and hardness in water, trivalent chromium and Cr VI Compound can be changed mutually.
The assay method of current water quality Cr VI is diphenyl carbazide spectrophotometry, and the preparation of its developer is by two Dinitrodiphenyl carbazide is dissolved in acetone, is then diluted with water to required volume.It has the disadvantage that acetone is that a kind of poisonous, high volatility have Machine reagent, there is certain murder by poisoning to human body, pollutes the environment.
The content of the invention
To solve the above problems, the present invention provides a kind of water quality Cr VI mixed color developing agent and its compound method, uses ethanol It is nontoxic and do not pollute the environment instead of acetone as primary solvent, and with Determination of Hexavalent Chromium in control the SPA of color acidity Mixed preparing developer, simplifies operating procedure.
The present invention is realized by following technical proposal:A kind of water quality Cr VI mixed color developing agent, it is characterised in that:Often Contain following component in 100mL mixed color developing agents:Diphenylcarbazide 0.2g, ethanol 70mL, 6~12mL of SPA, water 18~ 24mL。
The ethanol is absolute ethyl alcohol.
The mass concentration of the SPA is 85%.
The water is distilled water.
Another object of the present invention is also resided in and provides a kind of compound method of water quality Cr VI mixed color developing agent, by following Operation:First SPA is dissolved in appropriate water, diphenylcarbazide, ethanol is subsequently adding, residue is added after shaking up dissolving Water, contain following component in making gained per 100mL water quality Cr VI mixed color developing agents:Diphenylcarbazide 0.2g, ethanol 70mL, 6~12mL of SPA, 18~24mL of water, that is, obtain water quality Cr VI mixed color developing agent.
The application method of gained water quality Cr VI mixed color developing agent is:50mL water samples to be measured are taken to be placed in 50mL colorimetric cylinders, 2mL gained water quality Cr VI mixed color developing agents are added, is shaken up, after 5min, at 540nm wavelength, surveyed with 30mm cuvettes It is fixed, by conventionally calculation, that is, obtain the content of 6-valence Cr ions of water sample to be measured.
Advantage and effect that the present invention possesses:Water quality Cr VI mixed color developing agent of the invention be by diphenylcarbazide, Ethanol, SPA, water mixed preparing are formed.The present invention replaces acetone with ethanol as solvent, environmentally friendly and harmless to the human body, no Pollute the environment.The application method of traditional developer, i.e. water quality Determination of Hexavalent Chromium standard《GB7467-87》Regulation, water sample is advance Add 0.5mL(1+1)H3PO4Solution and 0.5mL(1+1)H2SO4Solution carrys out Controlled acidity, is subsequently adding 2mL developers and is surveyed It is fixed.When developer of the invention is used, be measured by being directly added into after 2mL mixed color developing agents, and in mixed color developing agent plus Enter SPA and carry out Controlled acidity, the influence that ferric iron in water sample is determined to content of 6-valence Cr ions can be eliminated, this invention simplifies survey Determine operating procedure, determine accuracy high.
Brief description of the drawings
Fig. 1 is the standard working curve of embodiment 1.
Specific embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1
First 8mL SPAs are dissolved in appropriate water, 0.2g diphenylcarbazides, 70mL ethanol is subsequently adding, after shaking up dissolving Remaining water is added, following component is contained in making gained per 100mL water quality Cr VI mixed color developing agents:Diphenylcarbazide 0.2g, ethanol 70mL, SPA 8mL, water 22mL, that is, obtain water quality Cr VI mixed color developing agent.Wherein, ethanol is anhydrous second Alcohol, the mass concentration of SPA is 85%, and water is distilled water.
The drafting of standard working curve:
0,0.20,0.50,1.00,2.00,4.00,6.00,8.00 and 10.00mL1 μ are separately added into 9 50mL colorimetric cylinders The chromium standard solution of g/mL, is diluted with water to graticule, adds the mixed color developing agent of the above-mentioned preparations of 2mL, shakes up, after placing 10min, It is measured at 540nm wavelength, as shown in Figure 1.
As can be seen from Figure 1, the correlation coefficient r of the standard working curve drawn with the mixed color developing agent prepared is 0.9998, accurate Exactness is high.
The measure of recovery of standard addition:
The measure of water sample:Gone out by the second pond to coking secondary clarifier effluent and the chromium standard solution for adding a certain amount of 10 μ g/mL The measure of content of 6-valence Cr ions in water, calculates recovery of standard addition, the degree of accuracy of further validation criteria curve.
The recovery testu result of table 1
As seen from Table 1, recovery of standard addition is 91~110%, further demonstrates and determines water quality six using the mixed color developing agent prepared Valency chromium content exactness is high.
Embodiment 2
First 6mL SPAs are dissolved in appropriate water, 0.2g diphenylcarbazides, 70mL ethanol is subsequently adding, after shaking up dissolving Remaining water is added, following component is contained in making gained per 100mL water quality Cr VI mixed color developing agents:Diphenylcarbazide 0.2g, ethanol 70mL, SPA 6mL, water 24mL, that is, obtain water quality Cr VI mixed color developing agent.Wherein, ethanol is anhydrous second Alcohol, the mass concentration of SPA is 85%, and water is distilled water.
Embodiment 3
First 12mL SPAs are dissolved in appropriate water, 0.2g diphenylcarbazides, 70mL ethanol is subsequently adding, after shaking up dissolving Remaining water is added, following component is contained in making gained per 100mL water quality Cr VI mixed color developing agents:Diphenylcarbazide 0.2g, ethanol 70mL, SPA 12mL, water 18mL, that is, obtain water quality Cr VI mixed color developing agent.Wherein, ethanol is anhydrous second Alcohol, the mass concentration of SPA is 85%, and water is distilled water.
To a certain cleaning surface water, it is measured using two methods.Determination step and result are as follows:
The method of the present invention:Take 50mL water samples to be placed in 50mL colorimetric cylinders, add the gained water quality Cr VI mixing of 2mL embodiments 2 Developer, shakes up, and after 5min, at 540nm wavelength, is measured with 30mm cuvettes, and by calculating, the Cr VI of water sample contains It is 0.885mg/L to measure.
《GB7467-87》Diphenyl carbazide spectrophotometry:Take 50mL water samples to be placed in 50mL colorimetric cylinders, add 0.5mL(1+1)H3PO4Solution and 0.5mL(1+1)H2SO4Solution, shakes up, and adds 2mL developers (I), shakes up, after 5min, in At 540nm wavelength, it is measured with 30mm cuvettes, by calculating, the content of 6-valence Cr ions of water sample is 0.895mg/L.
By contrasting the measurement result of two methods, measurement result without significant difference, but from determination step, the present invention Simplify operating procedure, and only use phosphoric acid Controlled acidity, it is not necessary to phosphoric acid and sulfuric acid co- controlling acidity, save reagent into This.

Claims (6)

1. a kind of water quality Cr VI mixed color developing agent, it is characterised in that:Contain following component in per 100mL mixed color developing agents:Two Dinitrodiphenyl carbazide 0.2g, ethanol 70mL, 6~12mL of SPA, 18~24mL of water.
2. water quality Cr VI mixed color developing agent according to claim 1, it is characterised in that:The ethanol is absolute ethyl alcohol.
3. water quality Cr VI mixed color developing agent according to claim 1, it is characterised in that:The mass concentration of the SPA It is 85%.
4. water quality Cr VI mixed color developing agent according to claim 1, it is characterised in that:The water is distilled water.
5. a kind of compound method of water quality Cr VI mixed color developing agent, it is characterised in that by following operation:It is first that SPA is molten In appropriate water, diphenylcarbazide, ethanol are subsequently adding, remaining water is added after shaking up dissolving, make gained per 100mL Contain following component in water quality Cr VI mixed color developing agent:Diphenylcarbazide 0.2g, ethanol 70mL, 6~12mL of SPA, water 18~24mL, that is, obtain water quality Cr VI mixed color developing agent.
6. compound method according to claim 5, it is characterised in that:The user of gained water quality Cr VI mixed color developing agent Method is:Take 50mL water samples to be measured to be placed in 50mL colorimetric cylinders, add 2mL gained water quality Cr VI mixed color developing agents, shake up, 5min Afterwards, at 540nm wavelength, it is measured with 30mm cuvettes, by conventionally calculation, that is, the Cr VI for obtaining water sample to be measured contains Amount.
CN201611238809.3A 2016-12-28 2016-12-28 A kind of water quality Cr VI mixed color developing agent and its compound method Pending CN106770249A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110296947A (en) * 2019-07-30 2019-10-01 杭州鑫月建材有限公司 A kind of cement Cr VI test powder indicator and preparation method thereof
CN116429760A (en) * 2023-03-27 2023-07-14 广州伊创科技股份有限公司 Color reagent for monitoring total chromium content in water and method for online monitoring total chromium content in water

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Publication number Priority date Publication date Assignee Title
CN2757123Y (en) * 2004-12-23 2006-02-08 广东环凯微生物科技有限公司 Quick detecting reagent box for sexavalence chromium
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
CN102411001A (en) * 2011-08-08 2012-04-11 山东汇金彩钢有限公司 Method for rapid detection of hexavalent chromium ions in sewage
CN103018183A (en) * 2011-09-22 2013-04-03 江苏天瑞仪器股份有限公司 Kit and method used for monitoring hexavalent chromium online

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2757123Y (en) * 2004-12-23 2006-02-08 广东环凯微生物科技有限公司 Quick detecting reagent box for sexavalence chromium
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
CN102411001A (en) * 2011-08-08 2012-04-11 山东汇金彩钢有限公司 Method for rapid detection of hexavalent chromium ions in sewage
CN103018183A (en) * 2011-09-22 2013-04-03 江苏天瑞仪器股份有限公司 Kit and method used for monitoring hexavalent chromium online

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110296947A (en) * 2019-07-30 2019-10-01 杭州鑫月建材有限公司 A kind of cement Cr VI test powder indicator and preparation method thereof
CN110296947B (en) * 2019-07-30 2022-02-08 杭州鑫月建材有限公司 Cement hexavalent chromium test powder indicator and preparation method thereof
CN116429760A (en) * 2023-03-27 2023-07-14 广州伊创科技股份有限公司 Color reagent for monitoring total chromium content in water and method for online monitoring total chromium content in water

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Address after: 650399 Kunming City, Yunnan Province, Anning City, Baihua East Road extension line 26

Applicant after: Yunnan Tianlong Environment Technology Co., Ltd.

Address before: 650399 Kunming City, Yunnan Province, Anning City, Baihua East Road extension line 26

Applicant before: Yunnan Kunming Iron & Steel Water Purification Technology Co., Ltd.

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Application publication date: 20170531