CN106769916A - A kind of Determination of Hexavalent Chromium method in water - Google Patents
A kind of Determination of Hexavalent Chromium method in water Download PDFInfo
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- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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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
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.
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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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CN201611036559.5A CN106769916A (en) | 2016-11-23 | 2016-11-23 | A kind of Determination of Hexavalent Chromium method in water |
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Cited By (1)
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)
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 |
-
2016
- 2016-11-23 CN CN201611036559.5A patent/CN106769916A/en active Pending
Patent Citations (4)
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)
Title |
---|
隋庆云: "《水质及常见毒物快速检验法》", 31 August 1983 * |
Cited By (1)
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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