CN106769916A - A kind of Determination of Hexavalent Chromium method in water - Google Patents

A kind of Determination of Hexavalent Chromium method in water Download PDF

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Publication number
CN106769916A
CN106769916A CN201611036559.5A CN201611036559A CN106769916A CN 106769916 A CN106769916 A CN 106769916A CN 201611036559 A CN201611036559 A CN 201611036559A CN 106769916 A CN106769916 A CN 106769916A
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China
Prior art keywords
chromium
water
developer
colorimetric cylinder
determination
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CN201611036559.5A
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Chinese (zh)
Inventor
马丽
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SHANGHAI LEICI ENVIRONMENTAL ENGINEERING Co Ltd
INESA SCIENTIFIC INSTRUMENT CO Ltd
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SHANGHAI LEICI ENVIRONMENTAL ENGINEERING Co Ltd
INESA SCIENTIFIC INSTRUMENT CO Ltd
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Application filed by SHANGHAI LEICI ENVIRONMENTAL ENGINEERING Co Ltd, INESA SCIENTIFIC INSTRUMENT CO Ltd filed Critical SHANGHAI LEICI ENVIRONMENTAL ENGINEERING Co Ltd
Priority to CN201611036559.5A priority Critical patent/CN106769916A/en
Publication of CN106769916A publication Critical patent/CN106769916A/en
Pending legal-status Critical Current

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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
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material 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

A kind of Determination of Hexavalent Chromium method in water, with Cr VI in diphenyl carbazide spectrophotometry measurement water, whole method determination step is easy;Reagent convenient storage, storage period is long, and volume of water sample is contracted to original 1/5th, sampling amount is reduced, volume of water sample is not required to accurate quantification, eliminate the error produced because sampling is inaccurate, measurement range and linear dependence are improve, sensitivity and anti-interference is improve.

Description

A kind of Determination of Hexavalent Chromium method in water
Technical field
It is exactly specifically to be related to a kind of Determination of Hexavalent Chromium method in water the invention belongs to species analysis detection technique field.
Background technology
Chromium is one of trace element necessary to organism, and it is relevant that the toxicity of chromium has valence state with it, it is generally recognized that sexavalence The toxicity of chromium is higher than trivalent chromium 100 times, and Cr VI is easily absorbed by the body and accumulates in vivo, it can by digestion, respiratory tract, Skin and mucous membrane invade human body, and skin contact may cause sensitivity, more likely cause inherited genetic defects, and suction may be caused Cancer, there is lasting danger to environment.
The industrial source of chromium is mainly processing, Treatment of Metal Surface, leather tanning, textile printing and dyeing, the oil of chromium-containing ore The industries such as chemical industry, medical treatment and pharmacy.Current Cr VI is generally measured using diphenyl carbazide spectrophotometry.It determines former Manage as in an acidic solution, Cr VI reacts with diphenylcarbazide, generate aubergine compound, carried out at wavelength 540nm Spectrophotometry.Traditional measuring method is more accurate to measurement raw material sampling needs, and interference free performance is poor, the sample of consumption Amount is more.
The content of the invention
The purpose of the present invention is poor aiming at Determination of Hexavalent Chromium method interference free performance in existing water, the sample size of consumption More technological deficiency, there is provided a kind of Determination of Hexavalent Chromium method in water, with six in diphenyl carbazide spectrophotometry measurement water Valency chromium, whole method determination step is easy;Reagent convenient storage, storage period is long, and volume of water sample is contracted to original 1/5th, Sampling amount is reduced, volume of water sample is not required to accurate quantification, eliminate the error produced because sampling is inaccurate, improve measurement range And linear dependence, improve sensitivity and anti-interference.
Technical scheme
In order to realize above-mentioned technical purpose, Determination of Hexavalent Chromium method in a kind of water of present invention design, it is characterised in that it Including following steps:
(I) preparation method of reagent
(1) prepared by chromium developer
8.0g potassium pyrosulfates are weighed first, 2.0g anhydrous magnesium sulfates grind mentioned reagent, mix, then weigh 0.05g bis- Dinitrodiphenyl carbazide, adds in said mixture, is slightly ground;
Then the above-mentioned mix reagents of 0.1g are weighed, is packaged in moisture barrier bag, stored protected from light is in cleaning, shady and cool, dry, ventilation Place, it is to avoid direct sunlight and high temperature;
(2) density p (Cr6+The preparation of)=100.0mg/L chromium calibration solutions
Weigh in advance in 110 DEG C of top pure grade 0.2829 ± 0.0001g of potassium bichromate of drying 2 hours, after water dissolves, move Enter in 1000mL volumetric flasks, be diluted with water to graticule, shake up.
(3) density p (Cr6+)=1.00mg/L chromium demarcates the preparation of liquid
Draw 1mL ρ (Cr6+In)=100.0mg/L chromium calibration solution to 100mL volumetric flasks, graduation mark is settled to water.
(II) in water content of 6-valence Cr ions measure
10mL water samples to be measured, pure water and 1.00mg/L chromium are taken respectively to demarcate in liquid to colorimetric cylinder, are walked to being added in colorimetric cylinder Suddenly 0.1g chromium developers in (1), screw colorimetric lid, rock colorimetric cylinder, dissolve chromium developer, in course of reaction, rock ratio Colour tube, makes solution mix and eliminate the bubble adhered on colour developing tube wall, after reaction 5min, absorbance is measured at 540nm wavelength, And the hexavalent chromium concentration of sample is calculated according to the absorbance demarcated.
Beneficial effect
Determination of Hexavalent Chromium method in a kind of water that the present invention is provided, with six in diphenyl carbazide spectrophotometry measurement water Valency chromium, whole method determination step is easy;Reagent convenient storage, storage period is long, and volume of water sample is contracted to original 1/5th, Sampling amount is reduced, volume of water sample is not required to accurate quantification, eliminate the error produced because sampling is inaccurate, improve measurement range And linear dependence, improve sensitivity and anti-interference.
Specific embodiment
With reference to embodiment, the present invention is elaborated.
Embodiment
(I) preparation method of reagent
Unless otherwise indicated, agents useful for same is the AR for meeting national standard.
1st, chromium developer
Accurately weigh 8.0g potassium pyrosulfates (K2S2O7), 2.0g anhydrous magnesium sulfates (MgSO4), mentioned reagent is ground, mix It is even.0.05g diphenylcarbazides (C is weighed again13H14N4O), add in said mixture, be slightly ground.
Weigh the above-mentioned mix reagents of 0.1g, be packaged in moisture barrier bag (respective labels are printed on moisture barrier bag), stored protected from light in Cleaning, shady and cool, dry, ventilation, it is to avoid direct sunlight and high temperature.
2nd, chromium calibration solution:ρ(Cr6+)=100.0mg/L
Accurately weigh top pure grade potassium bichromate (K2Cr2O7, dry 2h at 110 DEG C in advance) and 0.2829 ± 0.0001g, uses water After dissolving, move into 1000mL volumetric flasks, be diluted with water to graticule, shake up.
3rd, chromium demarcates liquid:ρ(Cr6+)=1.00mg/L
It is accurate to draw 1mL chromium calibration solution (ρ (Cr6+)=100.0mg/L) in 100mL volumetric flasks, scale is settled to water Line.
(II) in running water content of 6-valence Cr ions measure
10mL running water, pure water and 1.00mg/L chromium are taken respectively to demarcate in liquid to colorimetric cylinder, are wrapped to adding one in colorimetric cylinder Chromium developer, screws colorimetric lid, rocks colorimetric cylinder, chromium developer is dissolved (if having a small amount of undissolved, belong to normal phenomenon).Instead During answering, colorimetric cylinder is rocked in good time, solution is mixed and eliminate the bubble adhered on colour developing tube wall.After reaction 5min, Absorbance is measured at 540nm wavelength, and the hexavalent chromium concentration of sample is calculated according to the absorbance demarcated.
Wherein:Measured again after must reacting at least 5min after sample addition developer, be otherwise easily caused measurement inaccurate.It is dense Degree sample higher can the proper extension reaction time, if containing vanadium in sample, the reaction time can be extended to 10min, to eliminate Interference.

Claims (1)

1. a kind of Determination of Hexavalent Chromium method in water, it is characterised in that it includes following steps:
(I) preparation method of reagent
(1) prepared by chromium developer
8.0g potassium pyrosulfates are weighed first, 2.0g anhydrous magnesium sulfates grind mentioned reagent, mix, then weigh 0.05g hexichol carbon The hydrazine of acyl two, adds in said mixture, is slightly ground;
Then the above-mentioned mix reagents of 0.1g are weighed, are packaged in moisture barrier bag, stored protected from light in cleaning, it is shady and cool, dry, ventilation, Avoid direct sunlight and high temperature;
(2) density p (Cr6+The preparation of)=100.0mg/L chromium calibration solutions
Weigh in advance in 110 DEG C of top pure grade 0.2829 ± 0.0001g of potassium bichromate of drying 2 hours, after water dissolves, move into In 1000mL volumetric flasks, graticule is diluted with water to, shaken up.
(3) density p (Cr6+)=1.00mg/L chromium demarcates the preparation of liquid
Draw 1mL ρ (Cr6+In)=100.0mg/L chromium calibration solution to 100mL volumetric flasks, graduation mark is settled to water.
(II) in water content of 6-valence Cr ions measure
Take 10mL water samples to be measured, pure water and 1.00mg/L chromium respectively to demarcate in liquid to colorimetric cylinder, to addition step (1) in colorimetric cylinder Middle 0.1g chromium developer, screws colorimetric lid, rocks colorimetric cylinder, dissolves chromium developer, in course of reaction, rocks colorimetric cylinder, Solution is mixed and eliminate the bubble adhered on colour developing tube wall, after reaction 5min, absorbance, and root are measured at 540nm wavelength The hexavalent chromium concentration of sample is calculated according to the absorbance demarcated.
CN201611036559.5A 2016-11-23 2016-11-23 A kind of Determination of Hexavalent Chromium method in water Pending CN106769916A (en)

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CN201611036559.5A CN106769916A (en) 2016-11-23 2016-11-23 A kind of Determination of Hexavalent Chromium method in water

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Application Number Priority Date Filing Date Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109557087A (en) * 2018-10-29 2019-04-02 中国第汽车股份有限公司 A kind of detection method of metal surface Cr VI

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009104551A1 (en) * 2008-02-21 2009-08-27 矢崎総業株式会社 Method for simply quantitatively determining hexavalent chromium
US20090286323A1 (en) * 2008-05-19 2009-11-19 Hitachi High -Technologies Corporation Determination method and instruments of hexavalent chromium
CN102253039A (en) * 2011-04-25 2011-11-23 湖北神舟化工有限公司 Detection method of hexavalent chromium content
CN104792777A (en) * 2015-01-16 2015-07-22 深圳市环境科学研究院 An economical and rapid type test pack for colorimetric determination of a concentration of hexavalent chromium in water and a determination method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009104551A1 (en) * 2008-02-21 2009-08-27 矢崎総業株式会社 Method for simply quantitatively determining hexavalent chromium
US20090286323A1 (en) * 2008-05-19 2009-11-19 Hitachi High -Technologies Corporation Determination method and instruments of hexavalent chromium
CN102253039A (en) * 2011-04-25 2011-11-23 湖北神舟化工有限公司 Detection method of hexavalent chromium content
CN104792777A (en) * 2015-01-16 2015-07-22 深圳市环境科学研究院 An economical and rapid type test pack for colorimetric determination of a concentration of hexavalent chromium in water and a determination method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
隋庆云: "《水质及常见毒物快速检验法》", 31 August 1983 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109557087A (en) * 2018-10-29 2019-04-02 中国第汽车股份有限公司 A kind of detection method of metal surface Cr VI

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