CN107907536A - A kind of improved method of EDTA titration measurings calcium content - Google Patents

A kind of improved method of EDTA titration measurings calcium content Download PDF

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Publication number
CN107907536A
CN107907536A CN201711345690.4A CN201711345690A CN107907536A CN 107907536 A CN107907536 A CN 107907536A CN 201711345690 A CN201711345690 A CN 201711345690A CN 107907536 A CN107907536 A CN 107907536A
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China
Prior art keywords
edta
calcium
measurings
titration
improved method
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CN201711345690.4A
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Inventor
池明
石佳波
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Dagong Qingdao New Energy Material Technology Research Institute Co Ltd
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Dagong Qingdao New Energy Material Technology Research Institute Co Ltd
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Priority to CN201711345690.4A priority Critical patent/CN107907536A/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
    • G01N21/79Photometric titration

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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 Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The present invention proposes a kind of improved method of EDTA titration measurings calcium content, the ionic calcium soln of concentration known is prepared first, titrated with quantitative EDTA, the sky blue of titration end-point is reference colour, the solution of reference colour is detected with uv-spectrophotometric agent, the signal of blueness is converted into light absorbing strength signal.As titrimetric standard, and then eliminate different people and have the problem of different color differentiation abilities, artificial experimental error is substantially reduced.The present invention improves traditional titration method, test result indicates that more people's test results are almost consistent.

Description

A kind of improved method of EDTA titration measurings calcium content
Technical field
The present invention relates to analytical chemistry field, more particularly to a kind of improved method of EDTA titration measurings calcium content.
Background technology
Calcium constituent is a kind of tellurian basic element, and the content of calcium is about 5.1%, and the form that is primarily present is carbon The forms such as sour calcium.In the water cycle process of the earth, calcium constituent can be dissolved in water, therefore substantially all containing calcium member in surface water Element, based on, since everyone sensitivity to color is different, the result that may be titrated is multifarious when titrating detection.
ISO 6059-1984《Water quality calcium and the measure EDTA titrations of magnesium total amount》It is a kind of general national standard inspection Survey method, its basic procedure are under conditions of pH=10, with EDTA solution complexometry calcium ions, are given instruction with eriochrome black T Agent, purplish red solution is generated with calcium ion, and the calcium ion to dissociate in titration is reacted with EDTA first, molten after arrival titration end-point The color of liquid becomes sky blue by purple.But due to everyone for color resolution capability it is multifarious, become by purple It is undoubtedly a kind of fuzzy standard concept into sky blue.
The content of the invention
The present invention proposes a kind of improved method of EDTA titration measurings calcium content, solve due to people to debate aberration different Caused error problem.
The technical proposal of the invention is realized in this way:
1st, a kind of improved method of EDTA titration measurings calcium content, includes the following steps:
(1) the calcium ion storing solution of 1~2g/L is prepared;
(2) the EDTA titers of 0.2~1g/L are prepared;
(3) ISO 6059-1984 are used《Water quality calcium and the measure EDTA titrations of magnesium total amount》Step (1) is prepared Calcium ion storing solution is titrated;
(4) the calcium ion storing solution of step (1) is measured, required step is calculated according to the dosage of calcium ion storing solution (2) dosage of EDTA titers, and then the volume for needing EDTA is calculated, titrated according to volume is calculated, solution is by purple Become au bleu;
(5) the solution UV-3600Plus type UV spectrophotometer measurings after step (4) being become basket, by what is scanned The absorption intensity of the most strong characteristic peak of characteristic peak is standard absorption intensity;
(6) more people are allowed to use ISO 6059-1984 respectively《Water quality calcium and the measure EDTA titrations of magnesium total amount》Titrate unknown The ionic calcium soln of concentration, by the solution after titration with after UV-3600Plus type UV spectrophotometer measurings, inhales with standard After receiving intensity contrast adjustment titration results three times, according to EDTA content calculations calcium ion concentration used, the contrast of result is carried out.
Further, detection wave band is 300~800nm in the step (5).
In order to make result more accurate, more artificial at least 5 people in the step (6).
Further, the step (1) is specially to weigh 0.5~1g calcium hydroxides constant volume in 500mL volumetric flasks.
Further, the step (2) is specially to weigh 0.1~0.5g EDTA constant volumes in 500mL volumetric flasks.
The beneficial effects of the invention are as follows:
(1) solution of reference colour is detected by the present invention with uv-spectrophotometric agent, and the signal of blueness is converted into suction The strength signal of light is received, as titrimetric standard, and then different people is eliminated and has the problem of different color differentiation abilities, it is right Traditional titration method is improved, and artificial experimental error is substantially reduced;
(2) more people's test results are almost consistent.
Embodiment
The technical solution in the embodiment of the present invention is clearly and completely described below, it is clear that described implementation Example is only part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this area is general Logical technical staff all other embodiments obtained without making creative work, belong to protection of the present invention Scope.
Embodiment 1
(1) preparation of calcium ion storing solution:Calcium hydroxide 0.5g constant volumes are weighed in 500mL volumetric flasks.
(2) preparation of EDTA titers:It is stand-by in 500mL volumetric flasks to weigh EDTA 0.1g constant volumes.
(3) ISO 6059-1984 are used《Water quality calcium and the measure EDTA titrations of magnesium total amount》By above-mentioned concentration known Ionic calcium soln is titrated.
(4) content of required known EDTA is calculated, is titrated according to volume is calculated, solution is become by purple at this time Au bleu.
(5) by the UV-3600Plus type UV spectrophotometer measurings of solution at this time, detection wave band for 300~ 800nm, is standard absorption intensity by the absorption intensity of the most strong characteristic peak of the characteristic peak scanned.
(6) 5 people are allowed to use ISO 6059-1984 respectively《Water quality calcium and the measure EDTA titrations of magnesium total amount》Titrate unknown The ionic calcium soln of concentration, by the solution after titration with after UV-3600Plus type UV spectrophotometer measurings, inhales with standard After receiving intensity contrast adjustment titration results three times, according to EDTA content calculations calcium ion concentration used, the contrast of result is carried out, Test data is as follows:
Sample This law test result National standard measurement result
1 0.51mmol/L 0.53mmol/L
2 0.50mmol/L 0.57mmol/L
3 0.51mmol/L 0.60mmol/L
4 0.49mmol/L 0.47mmol/L
5 0.50mmol/L 0.52mmol/L
It can be seen that by data in table after the standard of final titration results is set, the test of 5 different people As a result it is almost identical, up-down error 0.2mmol/L, but it is substantially bigger than normal without the method titration results error of established standards.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention With within principle, any modification, equivalent replacement, improvement and so on, should all be included in the protection scope of the present invention god.

Claims (5)

1. a kind of improved method of EDTA titration measurings calcium content, it is characterised in that include the following steps:
(1) the calcium ion storing solution of 1~2g/L is prepared;
(2) the EDTA titers of 0.2~1g/L are prepared;
(3) ISO 6059-1984 are used《Water quality calcium and the measure EDTA titrations of magnesium total amount》The calcium ion prepared to step (1) Storing solution is titrated;
(4) the calcium ion storing solution of step (1) is measured, required step (2) is calculated according to the dosage of calcium ion storing solution The dosage of EDTA titers, and then the volume for needing EDTA is calculated, titrated according to volume is calculated, solution is become by purple Blueness;
(5) solution after step (4) being become basket is with UV-3600Plus type UV spectrophotometer measurings, the feature that will be scanned The absorption intensity of the most strong characteristic peak in peak is standard absorption intensity;
(6) more people are allowed to use ISO 6059-1984 respectively《Water quality calcium and the measure EDTA titrations of magnesium total amount》Titrate unknown concentration Ionic calcium soln, by the solution after titration with after UV-3600Plus type UV spectrophotometer measurings, with standard absorption intensity After contrast adjusts titration results three times, according to EDTA content calculations calcium ion concentration used, the contrast of result is carried out.
2. the improved method of EDTA titration measurings calcium content as claimed in claim 1, it is characterised in that the step (5) Middle detection wave band is 300~800nm.
3. the improved method of EDTA titration measurings calcium content as claimed in claim 1, it is characterised in that the step (6) In more artificial at least 5 people.
4. the improved method of EDTA titration measurings calcium content as claimed in claim 1, it is characterised in that the step (1) 0.5~1g calcium hydroxides constant volume is specially weighed in 500mL volumetric flasks.
5. the improved method of EDTA titration measurings calcium content as claimed in claim 1, it is characterised in that the step (2) 0.1~0.5g EDTA constant volumes are specially weighed in 500mL volumetric flasks.
CN201711345690.4A 2017-12-15 2017-12-15 A kind of improved method of EDTA titration measurings calcium content Pending CN107907536A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111751162A (en) * 2020-01-17 2020-10-09 浙江农林大学 Urban water quality detection method
CN113414009A (en) * 2021-05-20 2021-09-21 安徽开发矿业有限公司 Flotation method for crude ore containing filler specularite

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1046604A (en) * 1989-04-16 1990-10-31 云南省锅炉压力容器安全检测中心 A kind of water hardness quickly measuring agent
CN1677091A (en) * 2004-03-30 2005-10-05 三浦工业株式会社 Hardness measurement reagent
CN101701914A (en) * 2009-10-29 2010-05-05 江西稀有金属钨业控股集团有限公司 Analysis detection method for calcium element in ore
CN104977295A (en) * 2015-06-25 2015-10-14 天津工业大学 Method for detecting trace heavy metal ions in water body

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1046604A (en) * 1989-04-16 1990-10-31 云南省锅炉压力容器安全检测中心 A kind of water hardness quickly measuring agent
CN1677091A (en) * 2004-03-30 2005-10-05 三浦工业株式会社 Hardness measurement reagent
CN101701914A (en) * 2009-10-29 2010-05-05 江西稀有金属钨业控股集团有限公司 Analysis detection method for calcium element in ore
CN104977295A (en) * 2015-06-25 2015-10-14 天津工业大学 Method for detecting trace heavy metal ions in water body

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* Cited by examiner, † Cited by third party
Title
李桂伶 等: "3种测定钙制品中钙含量方法的比较", 《检测分析》 *
王军 等: "铬黑T作显色剂兼络合剂分光光度法测定钙的研究", 《陕西科技大学学报》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111751162A (en) * 2020-01-17 2020-10-09 浙江农林大学 Urban water quality detection method
CN113414009A (en) * 2021-05-20 2021-09-21 安徽开发矿业有限公司 Flotation method for crude ore containing filler specularite

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Application publication date: 20180413