CN103185715A - Analytical method of ferroporphyrin in ore biological leaching liquid - Google Patents

Analytical method of ferroporphyrin in ore biological leaching liquid Download PDF

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Publication number
CN103185715A
CN103185715A CN2011104566575A CN201110456657A CN103185715A CN 103185715 A CN103185715 A CN 103185715A CN 2011104566575 A CN2011104566575 A CN 2011104566575A CN 201110456657 A CN201110456657 A CN 201110456657A CN 103185715 A CN103185715 A CN 103185715A
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Prior art keywords
leachate
ore
analytical approach
volumetric flask
leaching liquid
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CN2011104566575A
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屈伟
刘爽
蔡镠璐
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Beijing General Research Institute for Non Ferrous Metals
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Beijing General Research Institute for Non Ferrous Metals
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Abstract

The invention relates to an analytical method of Fe<2+> in ore biological leaching liquid, which comprises the following steps: moving the leaching liquid to be tested in a volumetric flask, adding phenanthroline, an acetic acid-natrium aceticum buffer solution and a masking agent in order, developing for 10-15 minutes, and measuring the absorbance of Fe<2+> at wavelength of 510nm by using a spectrophotometer. The analytical method has good practical applicability, can effectively eliminate the interference of frequent ions and greatly enlarge the application scope of the method, and is more suitable for analyzing and determining the ore biological leaching liquid sample, and the obtained result has good accuracy and precision.

Description

Ferrous analytical approach in the ore biology leachate
Technical field
The present invention relates to ferrous analytical approach in a kind of ore biology leachate, specifically, relate to a kind ofly develop the color in brown volumetric flask with the phenanthroline spectrophotometric method, and adjust the addition sequence of developer, buffer solution, screening agent, measure ore biology leachate Central Asia analysis of iron content method.
Background technology
Ferrous analytical approach mainly contains dichromate method and phenanthroline spectrophotometric method.Dichromate method is traditional ferrous method of mensuration high-load, and it has advantages such as method is simple, quick, but concentration ferrous in the solution is lower than the sample of 0.20g/L, and its analysis result is difficult to satisfactory.Be lower than the sample of 0.20g/L for ferrous iron concentration, generally use the phenanthroline spectrophotometric method, under the condition of pH2-9, with oxammonium hydrochloride with Fe 3+Be reduced to Fe 2+, Fe 2+Generate stable salmon pink complex compound Fe (phen) with phenanthroline again 3 2+, use spectrophotometry Fe 2+Content.This method only is applicable to the total iron in the sample, and forms Fe in the sample simple, that interfering material is few 2+Mensuration, for Fe in the ore biology leachate 2+Mensuration certain difficulty is arranged.
Summary of the invention
The objective of the invention is to, provide a kind of easy fast, be easy to grasp, practicality is good, has Fe in the ore biology leachate of good accuracy and precision 2+Analytical approach.Especially provide a kind of under illumination condition, be applicable to Fe in the general ore biology leachate more 2+Analytical approach.
For achieving the above object, the present invention is by the following technical solutions:
Fe in a kind of ore biology leachate 2+Analytical approach, its step comprises: pipette leachate to be measured in volumetric flask, add phenanthroline, acetic acid-sodium acetate buffer solution and screening agent successively, developed the color 10-15 minute, measure Fe at 510nm wavelength place with spectrophotometer 2+Absorbance.
Fe in the aforesaid ore biology leachate 2+Analytical approach, wherein preferably, described volumetric flask is brown volumetric flask, purpose is to guarantee that chromogenic reaction finishes under the lucifuge condition, prevents Fe 3+Fe (phen) with the phenanthroline generation 3 3+Complex generation photoreduction.
Fe in the aforesaid ore biology leachate 2+Analytical approach, wherein saidly add successively, be point to add a kind of reagent in the volumetric flask after, add the next one again, and the addition sequence of three kinds of reagent can not change, its objective is to make screening agent shelter interfering ion effectively, and do not influence Fe 2+Chromogenic reaction with phenanthroline.
Fe in the aforesaid ore biology leachate 2+Analytical approach, wherein preferably, get described leachate 5.00-25.00mL to be measured.
Fe in the aforesaid ore biology leachate 2+Analytical approach, wherein preferably, described phenanthroline concentration is 0.25wt%, addition is 1.0-3.0mL.
Fe in the aforesaid ore biology leachate 2+Analytical approach, wherein preferably, the pH value of described acetic acid-sodium acetate buffer solution is 3, addition is 10mL.
Fe in the aforesaid ore biology leachate 2+Analytical approach, wherein preferably, described screening agent is EDTA, its concentration is 5wt%, addition is 1.0-7.0mL, purpose is to eliminate Fe in the ore biology leachate 3+, Cu 2+, Ni 2+, Co 2+, Mn 2+Interference Deng nonferrous metal ion.
Beneficial effect of the present invention is:
The present invention has good practicability, and is easy to be quick, is easy to grasp.The inventive method has been eliminated Fe effectively 3+, Cu 2+, Ni 2+, Co 2+, Mn 2+Deng the interference of nonferrous metal ion, expanded the scope of application of method; Realized under illumination condition Fe in the ore biology leachate 2+Mensuration.The gained result has good accuracy and precision.
The present invention will be further described below by embodiment, but and do not mean that limiting the scope of the invention.
Description of drawings
Fig. 1 is the Fe that makes under three kinds of different situations 2+Typical curve.
Embodiment
Analytical procedure
Accurately pipette leachate 5.00-25.00mL to be measured in the brown volumetric flask of 50mL, add 1.0-3.0mL 0.25wt% phenanthroline successively, 10mL pH3 acetic acid-sodium acetate buffer solution, 1.0-7.0mL 5wt%EDTA, developed the color 10-15 minute, on spectrophotometer, with the cuvette of 1cm-3cm, as reference, measure Fe with blank test solution at 510nm wavelength place 2+Absorbance.
Embodiment 1
Pipette 5.00mL leachate to be measured in the 250mL volumetric flask, be diluted with water to scale, divide and get the 5.00mL dilution in the brown volumetric flask of 50mL, add 1.0mL 0.25wt% phenanthroline successively, 10mL pH3 acetic acid-sodium acetate buffer solution, 6.0mL 5wt%EDTA, developed the color 10-15 minute, and on spectrophotometer, used the 3cm cuvette, as reference, measure Fe with leachate to be measured at 510nm wavelength place 2+Absorbance be 0.323, Fe 2+Concentration be 0.295g/L.
Embodiment 2
Pipette 10.00mL leachate to be measured in the 100mL volumetric flask, be diluted with water to scale, divide and get the 10.00mL dilution in the 100mL volumetric flask, be diluted with water to scale again, divide and get the 5.00mL dilution in the brown volumetric flask of 50mL, add 2.0mL 0.25wt% phenanthroline successively, 10mL pH3 acetic acid-sodium acetate buffer solution, 5.0mL 5wt%EDTA, developed the color 10-15 minute, and on spectrophotometer, used the 2cm cuvette, as reference, measure Fe with leachate to be measured at 510nm wavelength place 2+Absorbance be 0.414, Fe 2+Concentration be 1.201g/L.
Embodiment 3
Pipette 10.00mL leachate to be measured in the 100mL volumetric flask, be diluted with water to scale, divide and get the 5.00mL dilution in the 100mL volumetric flask, be diluted with water to scale again, divide and get the 5.00mL dilution in the brown volumetric flask of 50mL, add 3.0mL 0.25wt% phenanthroline successively, 10mL pH3 acetic acid-sodium acetate buffer solution, 3.0mL 5wt%EDTA, developed the color 10-15 minute, and on spectrophotometer, used the 2cm cuvette, as reference, measure Fe with leachate to be measured at 510nm wavelength place 2+Absorbance be 0.429, Fe 2+Concentration be 2.490g/L.
Comparative example 1
Pipette 10.00mL leachate to be measured in the 250mL beaker, add 20mL hydrochloric acid (1+1), 15-20mL sulphur-phosphorus acid mixture is diluted with water to about 100mL, adds 3 0.5% diphenylamine sulfonic acid sodium salt indicator, uses T Fe/K2Cr2O7Potassium dichromate standard solution titration to the purple of=2.00mg/mL is terminal point, and consuming potassium dichromate standard solution volume is 12.37mL, Fe 2+Concentration be 2.474g/L.
Fe 2+Typical curve
Get 10.00,20.00,30.00 and 40.00 μ g Fe 2+Standard solution is made standard curve I~III for each three parts.
Standard curve I: add phenanthroline successively in the standard solution and acetic acid-sodium acetate buffer solution is chromogenic assay.
Standard curve I I: add chromogenic assay behind phenanthroline, acetic acid-sodium acetate buffer solution and the EDTA in the standard solution successively.
Standard curve I II: in standard solution, add 1.00mg Fe respectively 3+, add chromogenic assay behind phenanthroline, acetic acid-sodium acetate buffer solution and the EDTA afterwards successively.
By Fig. 1 and referential coloured picture as seen, standard curve I and standard curve I I overlap fully, and II overlaps substantially with standard curve I, i.e. EDTA and Fe 3+Adding do not influence the sensitivity of the inventive method.
Method contrast experiment
To the Fe in four kinds of ore biology leachate samples 2+, adopt the inventive method and potassium bichromate titrimetric method to measure and comparison respectively, relative deviation shows that the inventive method has good accuracy, sees Table 1 in 3% as a result; And, measured four kinds of artificial synthetic samples, Fe with the inventive method 2+The recovery in the 99.6%-100.8% scope, the prescription of four kinds of artificial synthetic samples and experimental result show that referring to table 2 the inventive method has good precision.
Table 1
Table 2

Claims (6)

1. Fe in the ore biology leachate 2+Analytical approach, it is characterized in that its step comprises: pipette leachate to be measured in volumetric flask, add phenanthroline, acetic acid-sodium acetate buffer solution and screening agent successively, developed the color 10-15 minute, measure Fe at 510nm wavelength place with spectrophotometer 2+Absorbance.
2. Fe in the ore biology leachate as claimed in claim 1 2+Analytical approach, it is characterized in that described volumetric flask is brown volumetric flask.
3. Fe in the ore biology leachate as claimed in claim 1 or 2 2+Analytical approach, it is characterized in that, get described leachate 5.00-25.00mL to be measured.
4. Fe in the ore biology leachate as claimed in claim 1 or 2 2+Analytical approach, it is characterized in that described phenanthroline concentration is 0.25wt%, addition is 1.0-3.0mL.
5. Fe in the ore biology leachate as claimed in claim 1 or 2 2+Analytical approach, it is characterized in that the pH value of described acetic acid-sodium acetate buffer solution is 3, addition is 10mL.
6. Fe in the ore biology leachate as claimed in claim 1 or 2 2+Analytical approach, it is characterized in that described screening agent is EDTA, its concentration is 5wt%, addition is 1.0-7.0mL.
CN2011104566575A 2011-12-30 2011-12-30 Analytical method of ferroporphyrin in ore biological leaching liquid Pending CN103185715A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102928345A (en) * 2012-11-26 2013-02-13 芜湖东旭光电科技有限公司 Method for removing deposits and suspended matters during measurement of total iron content in high-calcium material
CN103411968A (en) * 2013-07-31 2013-11-27 南京梅山冶金发展有限公司 Method for detecting total iron content of steel slag
CN105628694A (en) * 2015-12-24 2016-06-01 大连理工大学 Test paper and method for detecting integrity of copper coating or chromium coating on steel surface

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57172248A (en) * 1981-04-17 1982-10-23 Toshiba Corp Pretreating method for measurement of heavy metal in sample water
EP0718629A1 (en) * 1994-12-20 1996-06-26 Fuji Photo Film Co., Ltd. Method of spotting sample liquid on dry chemical analysis film
CN1757767A (en) * 2005-11-08 2006-04-12 昆明理工大学 Shielding iron removing method in high purity aluminium oxide preparation process
CN101713740A (en) * 2009-12-31 2010-05-26 中国原子能科学研究院 Method for spectrophotometry measuring boron content in BNCT medicament in biological sample
CN102095727A (en) * 2010-12-14 2011-06-15 常德力元新材料有限责任公司 Method for carrying out non-destructive qualitative detection on copper

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57172248A (en) * 1981-04-17 1982-10-23 Toshiba Corp Pretreating method for measurement of heavy metal in sample water
EP0718629A1 (en) * 1994-12-20 1996-06-26 Fuji Photo Film Co., Ltd. Method of spotting sample liquid on dry chemical analysis film
CN1757767A (en) * 2005-11-08 2006-04-12 昆明理工大学 Shielding iron removing method in high purity aluminium oxide preparation process
CN101713740A (en) * 2009-12-31 2010-05-26 中国原子能科学研究院 Method for spectrophotometry measuring boron content in BNCT medicament in biological sample
CN102095727A (en) * 2010-12-14 2011-06-15 常德力元新材料有限责任公司 Method for carrying out non-destructive qualitative detection on copper

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
董文宾等: "1 , 1 0 一邻菲啰啉分光光度法同时测定玻璃中的亚铁和总铁", 《硅酸盐通报》 *
赵梦月等: "Fe(II)(III)-EDTA体系研究(IV)——邻菲啰啉光度法测铁价态", 《郑州工学院学报》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102928345A (en) * 2012-11-26 2013-02-13 芜湖东旭光电科技有限公司 Method for removing deposits and suspended matters during measurement of total iron content in high-calcium material
CN103411968A (en) * 2013-07-31 2013-11-27 南京梅山冶金发展有限公司 Method for detecting total iron content of steel slag
CN103411968B (en) * 2013-07-31 2016-07-06 南京梅山冶金发展有限公司 A kind of detection method of all iron content suitable in slag
CN105628694A (en) * 2015-12-24 2016-06-01 大连理工大学 Test paper and method for detecting integrity of copper coating or chromium coating on steel surface

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Application publication date: 20130703