CN114152710B - Method for detecting total iron content in iron ore - Google Patents

Method for detecting total iron content in iron ore Download PDF

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CN114152710B
CN114152710B CN202111462633.0A CN202111462633A CN114152710B CN 114152710 B CN114152710 B CN 114152710B CN 202111462633 A CN202111462633 A CN 202111462633A CN 114152710 B CN114152710 B CN 114152710B
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iron
iron ore
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concentration
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CN114152710A (en
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周杰强
崔向鹤
赵炎
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Henan Zihuan Mining Technology Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
    • 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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention belongs to the technical field of total iron content detection, and discloses a method for detecting the total iron content in iron ores, which comprises the following steps: s1, taking an iron ore sample, sequentially adding sodium fluoride, sodium bicarbonate and hydrochloric acid solution, heating and stirring until the iron ore sample is completely dissolved; adding sodium bicarbonate again, stirring for dissolving, and cooling to room temperature with running water synchronously; sequentially adding sulfur-phosphorus mixed acid and manganese sulfate solution, and uniformly mixing to obtain a pretreatment solution; s2, heating the pretreatment solution, adding the zinc chloride solution while stirring until the pretreatment solution becomes light yellow, and then continuing to heat for 2min; cooling the flowing water to room temperature, dropwise adding a sodium tungstate solution, and then adding a titanium trichloride solution while stirring until tungsten blue appears in the pretreatment solution to obtain a sample solution; s3, taking a sample solution with tungsten blue disappeared, dropwise adding indicator sodium diphenylamine sulfonate, then titrating a potassium permanganate standard solution, and recording the consumption volume V of the potassium permanganate standard solution when the sample solution turns purple and does not fade within 30 seconds; s4, calculating a result.

Description

Method for detecting total iron content in iron ore
Technical Field
The invention belongs to the technical field of total iron content detection, and particularly relates to a method for detecting total iron content in iron ores.
Background
At present, a potassium dichromate titration method of mercury chloride is generally adopted for measuring the total iron content in iron ore, and the method has strong applicability and high accuracy, but mercury and chromium used in the method are toxic substances, so that serious environmental pollution is caused in the detection process, and even the physical health of measuring staff is influenced.
In recent years, more and more reports about mercury-free detection methods are provided, wherein a zinc powder reduction potassium dichromate titration method is a typical mercury-free detection method, but the method still does not completely eliminate the application and pollution of chromium, so that a mercury-free and chromium-free green detection method is provided in the invention.
Disclosure of Invention
In view of the above, the invention aims to provide a method for detecting the total iron content in iron ore, which aims to solve the pollution problem of mercury and chromium in the existing detection method.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for detecting the total iron content in iron ore comprises the following steps:
s1, pretreatment
Taking an iron ore sample, sequentially adding sodium fluoride, sodium bicarbonate and hydrochloric acid solution according to a proportion, heating and stirring until the iron ore sample is completely dissolved;
adding sodium bicarbonate again, stirring for dissolving, and cooling to room temperature with running water synchronously;
sequentially adding sulfur-phosphorus mixed acid and manganese sulfate solution, and uniformly mixing to obtain a pretreatment solution;
s2, oxidation reduction
Heating the pretreatment solution to 90-100 ℃, adding zinc chloride solution while stirring until the pretreatment solution becomes light yellow, and then continuing to heat for 2min;
cooling the flowing water to room temperature, dropwise adding a sodium tungstate solution, and then adding a titanium trichloride solution while stirring until tungsten blue appears in the pretreatment solution to obtain a sample solution;
s3, titration
Taking a sample solution with tungsten blue disappeared, dropwise adding indicator sodium diphenylamine sulfonate, then titrating a potassium permanganate standard solution, and recording the consumption volume V of the potassium permanganate standard solution when the sample solution turns purple and does not fade within 30 seconds;
s4, calculating results
The percentage content of total iron in the iron ore is calculated,wherein:
t-total iron titration coefficient;
v-the consumption volume of the potassium permanganate standard solution when the iron ore sample is titrated, wherein the unit is mL;
m-mass of iron ore sample in g.
Preferably, in the step S1, the mixing mass ratio of the iron ore sample, sodium fluoride, sodium bicarbonate and hydrochloric acid solution is 2:5:10:12.
preferably, in the step S1, the concentration of the hydrochloric acid solution is 1.2g/mL.
Preferably, in the step S1, the mass ratio of the sodium bicarbonate added twice is 2:1.
preferably, in the step S1, the adding volume ratio of the hydrochloric acid solution, the sulfur-phosphorus mixed acid solution and the manganese sulfate solution is 2:3:4.
preferably, in said step S1: the sulfur-phosphorus mixed acid solution is formed by mixing sulfuric acid solution with the concentration of 1.84g/mL and phosphoric acid solution with the concentration of 1.7 g/mL; the concentration of the manganese sulfate solution is 150g/L.
Preferably, in the step S2, the concentration of the zinc chloride solution is 25g/L, the concentration of the sodium tungstate solution is 250g/L, and the concentration of the titanium trichloride solution is 1.5g/L.
Preferably, before the step S3, the potassium permanganate standard solution is dropped to the sample solution so that tungsten blue disappears, and the currently dropped potassium permanganate standard solution does not account for the consumption volume V in the step S3.
Preferably, before said step S3, the sample solution is left to stand at room temperature until the tungsten blue disappears.
Preferably, in said step S4, the total iron titration coefficientWherein:
c (Fe) -iron standard solution concentration, wherein the unit is mol/L;
V T the volume of potassium permanganate standard solution consumed in titrating the iron standard solution is in mL.
Compared with the prior art, the invention has the following beneficial effects:
in the detection method provided by the invention, a hydrochloric acid solution is adopted for pretreatment and dissolution of a sample, then zinc chloride-titanium trichloride is used for replacing mercury salt to reduce ferric iron in the pretreatment solution into ferrous iron, finally sodium diphenylamine sulfonate is used as an indicator, and potassium permanganate is used as a standard solution for titration detection, so that a mercury-containing reagent and a chromium-containing reagent are effectively avoided in the whole detection process, and the secondary pollution of mercury and chromium to the environment is effectively eliminated.
In addition, zinc chloride and titanium trichloride are matched under an acidic medium, so that ferric iron can be completely reduced into ferrous iron, the reduction efficiency is high, the reduction effect of chloride ions on potassium permanganate is effectively inhibited, and the accuracy of a detection result is effectively improved.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Method for detecting total iron content in iron ore
S1, pretreatment
Taking 0.2g of iron ore sample, sequentially adding 0.5g of sodium fluoride, 1g of sodium bicarbonate and 10mL of hydrochloric acid solution with the concentration of 1.2g/mL, heating and stirring until the solution is completely dissolved;
adding 0.5g of sodium bicarbonate again, stirring for dissolution, and cooling to room temperature with running water;
mixing a sulfuric acid solution with the concentration of 1.84g/mL with a phosphoric acid solution with the concentration of 1.7g/mL to prepare a sulfuric-phosphoric mixed acid solution, sequentially adding 15mL of the sulfuric-phosphoric mixed acid solution and 20mL of a manganese sulfate solution with the concentration of 150g/L, and uniformly mixing to obtain a pretreatment solution.
S2, oxidation reduction
Heating the pretreatment solution to 90-100 ℃, adding 25g/L zinc chloride solution while stirring until the pretreatment solution turns light yellow, and then continuing heating for 2min;
cooling the flowing water to room temperature, dropwise adding 15 drops of sodium tungstate solution with the concentration of 250g/L, and then adding titanium trichloride solution with the concentration of 1.5g/L while stirring until tungsten blue appears in the pretreatment solution to obtain a sample solution;
the tungsten blue of the sample solution is eliminated by dropping the potassium permanganate standard solution or by standing, wherein the currently dropped potassium permanganate standard solution does not account for the consumption volume V in step S3 when the potassium permanganate standard solution is dropped.
S3, titration
And (3) taking a sample solution with tungsten blue disappeared, dropwise adding 4-6 drops of indicator sodium diphenylamine sulfonate, then titrating a potassium permanganate standard solution, and recording the consumption volume V of the potassium permanganate standard solution when the sample solution turns purple and does not fade within 30 seconds.
S4, calculating results
The percentage content of total iron in the iron ore is calculated,wherein:
t-iron titration coefficient, andwherein, the concentration of the c (Fe) -iron standard solution is expressed in mol/L; v (V) T -the volume of potassium permanganate standard solution consumed in titrating the iron standard solution, in mL;
v-the consumption volume of the potassium permanganate standard solution when the iron ore sample is titrated, wherein the unit is mL;
m-mass of iron ore sample in g.
When the total iron titration coefficient is obtained, preparing an iron standard solution, and executing V based on the same principle of the method T Is detected:
1) Preparing an iron standard solution
2.1446g of ferric oxide is weighed and placed in a 200mL beaker, 125mL of hydrochloric acid solution with the concentration of 1.2g/mL is added, and the mixture is heated and stirred until the mixture is completely dissolved; and naturally cooling, and then adding deionized water to adjust the concentration of the iron standard solution to 6mg/mL.
2) Redox
Heating the iron standard solution to 90-100 ℃, adding 25g/L zinc chloride solution while stirring until the pretreatment solution turns light yellow, and then continuing heating for 2min;
cooling the flowing water to room temperature, dropwise adding 15 drops of sodium tungstate solution with the concentration of 250g/L, and then adding titanium trichloride solution with the concentration of 1.5g/L while stirring until tungsten blue appears in the pretreatment solution to obtain a sample solution;
the tungsten blue of the sample solution is eliminated by dripping the potassium permanganate standard solution or standing, wherein the currently dripped potassium permanganate standard solution does not account for the consumption volume V in the step S3 when the potassium permanganate standard solution is dripped;
s3, titration
Taking a sample solution with tungsten blue disappeared, dropwise adding 2-4 drops of indicator sodium diphenylamine sulfonate, then titrating a potassium permanganate standard solution, and recording the consumption volume V of the potassium permanganate standard solution when the sample solution turns purple and does not fade within 30 seconds T
S4, the total iron titration coefficient is obtained,wherein:
c (Fe) -iron standard solution concentration, wherein the unit is mol/L; v (V) T The volume of potassium permanganate standard solution consumed in titrating the iron standard solution is in mL.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (8)

1. A method for detecting the total iron content in iron ore, comprising the steps of:
s1, pretreatment
Taking an iron ore sample, sequentially adding sodium fluoride, sodium bicarbonate and hydrochloric acid solution according to a proportion, heating and stirring until the iron ore sample is completely dissolved;
adding sodium bicarbonate again, stirring for dissolving, and cooling to room temperature with running water synchronously;
sequentially adding sulfur-phosphorus mixed acid and manganese sulfate solution, and uniformly mixing to obtain a pretreatment solution;
s2, oxidation reduction
Heating the pretreatment solution to 90-100 ℃, adding zinc chloride solution while stirring until the pretreatment solution becomes light yellow, and then continuing to heat for 2min;
cooling the flowing water to room temperature, dropwise adding a sodium tungstate solution, and then adding a titanium trichloride solution while stirring until tungsten blue appears in the pretreatment solution to obtain a sample solution;
s3, titration
Taking a sample solution with tungsten blue disappeared, dropwise adding indicator sodium diphenylamine sulfonate, then titrating a potassium permanganate standard solution, and recording the consumption volume V of the potassium permanganate standard solution when the sample solution turns purple and does not fade within 30 seconds;
s4, calculating results
The percentage content of total iron in the iron ore is calculated,wherein:
t-total iron titration coefficient;
v-the consumption volume of the potassium permanganate standard solution when the iron ore sample is titrated, wherein the unit is mL;
m-mass of iron ore sample in g;
in the step S1, the mixing mass ratio of the iron ore sample, sodium fluoride, sodium bicarbonate and hydrochloric acid solution is 2:5:10:12;
in said step S4, the iron titration coefficientIn the middle of
c (Fe) -iron standard solution concentration, wherein the unit is mol/L;
V T the volume of potassium permanganate standard solution consumed in titrating the iron standard solution is in mL.
2. The method for detecting the total iron content in iron ore according to claim 1, wherein: in the step S1, the concentration of the hydrochloric acid solution is 1.2g/mL.
3. The method for detecting the total iron content in iron ore according to claim 1 or 2, wherein: in the step S1, the mass ratio of the two additions of sodium bicarbonate is 2:1.
4. the method for detecting the total iron content in the iron ore according to claim 2, wherein: in the step S1, the adding volume ratio of the hydrochloric acid solution, the sulfur-phosphorus mixed acid solution and the manganese sulfate solution is 2:3:4.
5. the method for detecting the total iron content in iron ore according to claim 4, wherein in the step S1:
the sulfur-phosphorus mixed acid solution is formed by mixing sulfuric acid solution with the concentration of 1.84g/mL and phosphoric acid solution with the concentration of 1.7 g/mL;
the concentration of the manganese sulfate solution is 150g/L.
6. The method for detecting the total iron content in iron ore according to claim 1, wherein: in the step S2, the concentration of the zinc chloride solution is 25g/L, the concentration of the sodium tungstate solution is 250g/L, and the concentration of the titanium trichloride solution is 1.5g/L.
7. The method for detecting the total iron content in iron ore according to claim 1, wherein: before the step S3, the tungsten blue of the potassium permanganate standard solution is dropped to the sample solution and the currently dropped potassium permanganate standard solution does not account for the consumption volume V in the step S3.
8. The method for detecting the total iron content in iron ore according to claim 1, wherein: prior to said step S3, the sample solution was left at room temperature until the tungsten blue disappeared.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102313771A (en) * 2010-06-29 2012-01-11 鞍钢股份有限公司 Method for determining metallic iron of iron-containing material
CN103472059A (en) * 2013-09-30 2013-12-25 武汉钢铁(集团)公司 Method for measuring total iron content in fly ash
CN104391077A (en) * 2014-12-17 2015-03-04 内蒙古包钢钢联股份有限公司 Method for determining total iron in vanadium titano-magnetite by using acid dissolution method
CN106908441A (en) * 2017-03-23 2017-06-30 攀枝花学院 Iron ore all iron content without mercury salt detection method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102313771A (en) * 2010-06-29 2012-01-11 鞍钢股份有限公司 Method for determining metallic iron of iron-containing material
CN103472059A (en) * 2013-09-30 2013-12-25 武汉钢铁(集团)公司 Method for measuring total iron content in fly ash
CN104391077A (en) * 2014-12-17 2015-03-04 内蒙古包钢钢联股份有限公司 Method for determining total iron in vanadium titano-magnetite by using acid dissolution method
CN106908441A (en) * 2017-03-23 2017-06-30 攀枝花学院 Iron ore all iron content without mercury salt detection method

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
氯化亚锡-三氯化钛-高锰酸钾 无汞无铬滴定法测定铁;叶青等;《冶金分析》;第25卷(第5期);94-95 *
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