CN102928345A - Method for removing deposits and suspended matters during measurement of total iron content in high-calcium material - Google Patents
Method for removing deposits and suspended matters during measurement of total iron content in high-calcium material Download PDFInfo
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- CN102928345A CN102928345A CN2012104838377A CN201210483837A CN102928345A CN 102928345 A CN102928345 A CN 102928345A CN 2012104838377 A CN2012104838377 A CN 2012104838377A CN 201210483837 A CN201210483837 A CN 201210483837A CN 102928345 A CN102928345 A CN 102928345A
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Abstract
The invention discloses a method for removing deposits and suspended matters during the measurement of the total iron content in high-calcium material. The method includes the steps of firstly preparing a high-calcium material solution, and adding an acid solution into the high-calcium material solution after the color development is completed, wherein the solution prepared firstly is a solution of 50 ml to 80 ml prepared in a 100 ml volumetric flask, the time for completing the color development lasts for 20-30 min, the acid solution is an acid solution of 50 ml to 1 ml with the pH value of 2.5-4 and is an acidic solution with ionized H<+>, and the acid solution and the acid solution for dissolving the high-calcium material are the same type and have the same concentration but different pH values. Through the adoption of the method, deposits and suspension particles generated during the measurement can be reduced and removed, the depositing time is shortened, and the measurement precision is improved.
Description
Technical field
The present invention relates to the chemical analysis technology field, relate in particular to a kind of removing method of measuring in the high calcareous material deposition and suspension in the total iron content process.
Background technology
Total iron is a kind of easier measuring method in the use Phen metric measurement material.
The Phen spectrophotometric method be utilize to measure iron content in the material be utilize ferrous iron pH value be in 2～9 the solution with the orange red complex compound of Phen reflection generation, use again spectrophotometer and measure at the 510nm place, thereby obtain a kind of method of iron content.
Routine techniques is in using Phen metric measurement material in the total iron content, the typical curve of model di-iron trioxide, then sample is carried out dissolution process, insert the 100ml volumetric flask, add successively 4ml tartrate, 1～2 paranitrophenol, it is yellow to drip the modulation of (1+1) ammoniacal liquor, drip immediately hydrochloric acid to colourless (this moment, the pH value approximate 5), add 2ml hydrochloric acid hydrogen amine, 10ml Phen solution, be diluted with water to scale mark, shake up, after placing 20min, on spectrophotometer, do reference with blank, select 1 centimetre of cuvette, carry out absorbance measurement at wavelength 510nm place.
Use at present the high calcareous material of Phen metric measurement to have: lime stone, rauhkalk, kalzit, calcium carbonate etc.
In measuring the high calcium metallic substance during total iron content, the pH value approximates in 5 and can separate out a large amount of precipitations and suspension in course of reaction, can not reach precipitation in the time of 20min fully leaving standstill, generally precipitate and realize the fully general meeting of precipitation in the more situation between 3～8 hours, and precipitation also can produce new suspension in the situation that solution fluctuates.These suspensions have increased the extinction degree Spectrophotometric the time using, and affects accuracy of measurement results, and the while is corresponding to have prolonged the work stand-by period.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of removing method of measuring in the high calcareous material deposition and suspension in the total iron content process.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: measure in the high calcareous material removing method of deposition and suspension in the total iron content process, dispose first high calcareous material solution, adding acid solution after colour developing fully.
As preferably, the high calcareous material solution of configuration is the high calcareous material solution that disposes 50ml～80ml in the 100ml volumetric flask first.
As preferably, wait for and develop the color completely that the time is 20～30 minutes.
As preferably, acid solution is that the pH value is 2.5～4 acid solution.
As preferably, acid solution is 50ml～1ml.
As preferably, acid solution is to ionize out H
+Acid solution.
As preferably, acid solution is that the concentration from the used acid solution of the high calcareous material of dissolving is identical but same acid solution that the pH value is different.
In said method, configuration 50ml～80ml high calcareous material solution to be measured, with the pH value that after developing the color fully, adds 50ml～1ml be 2.5～4 acid solution, in the specific implementation will be according to what of precipitation and suspension, according to circumstances and decision amount of preparation and addition how much.
Principle of work:
Be about in 5 in adjusting pH value, can separate out a large amount of sediments and suspension, it is Ca (OH) in fact
2, with its elimination, so be to add acid after its complex compound colour developing fully, reaction equation is 2H to the use acid again in the situation that does not affect colour developing
++ Ca (OH)
2=Ca
2++ 2H
2O.
Wherein dispose the pH value and be 2.5～4 acid solution and be the stable pH value scope according to complex compound, the pH value is too small can destroy Stability of Metal Complexes, and the pH value is excessive, does not reach the elimination deposition effect.
Adding after developing the color fully of mentioning is the time length of considering colour developing, and the pH value is too small, Fe
2+Facile hydrolysis, the pH value is excessive, and the time of colour developing is just longer, can play the effect that does not have influence on developing time and colour developing result so add afterwards acid solution in colour developing.
Will slowly add when adding acid solution, it is violent to avoid local acidity to change, and affects the stability of complex compound.
The acid solution that adds afterwards is that concentration from the used acid solution of the high calcareous material of dissolving is identical but same acid solution (such as being both hydrochloric acid solution or being both sulfuric acid solution) that pH value is different, and purpose is the introducing of minimizing impurity.
The invention has the beneficial effects as follows:
Can reduce and eliminate high calcareous material solution to be measured produces in measurement sediment and suspended particle, reduce and wait for sedimentation time, improve the accuracy of measurement.
Embodiment
Embodiment 1
1) typical curve of configuration di-iron trioxide;
2) with dissolving with hydrochloric acid high calcareous material to be measured;
3) in the 100ml volumetric flask, dispose 50ml solution to be measured according to the Phen spectrophotometric method;
4) leave standstill 20min, the pH value that slowly adds 30ml after developing the color fully is 3 hydrochloric acid solution;
5) after deposition was eliminated fully, constant volume was to 100ml;
6) taking into account known di-iron trioxide curve with spectrophotometric detects sample.
Embodiment 2
1) typical curve of configuration di-iron trioxide;
2) with sulfuric acid dissolution high calcareous material to be measured;
3) in the 100ml volumetric flask, dispose 80ml solution to be measured according to the Phen spectrophotometric method;
4) leave standstill 30min, the pH value that slowly adds 10ml after developing the color fully is 2.5 sulfuric acid solution;
5) after deposition was eliminated fully, constant volume was to 100ml;
6) taking into account known di-iron trioxide curve with spectrophotometric detects sample.
Above-described embodiment of the present invention does not consist of the restriction to protection domain of the present invention.Any modification of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., all should be included within the claim protection domain of the present invention.
Claims (7)
1. measure in the high calcareous material removing method of deposition and suspension in the total iron content process, it is characterized in that, dispose first high calcareous material solution, adding acid solution after colour developing fully.
2. the removing method of deposition according to claim 1 and suspension is characterized in that, the high calcareous material solution of configuration is the high calcareous material solution that disposes 50ml～80ml in the 100ml volumetric flask first.
3. the removing method of deposition according to claim 1 and suspension is characterized in that, described wait develops the color completely that the time is 20～30 minutes.
4. the removing method of deposition according to claim 1 and suspension is characterized in that, described acid solution is that the pH value is 2.5～4 acid solution.
5. the removing method of deposition according to claim 1 and suspension is characterized in that, described acid solution is 50ml～1ml.
6. the removing method of any one described deposition and suspension is characterized in that according to claim 1-5, and described acid solution is to ionize out H
+Acid solution.
7. the removing method of any one described deposition and suspension is characterized in that according to claim 1-5, and described acid solution is that the concentration from the used acid solution of the high calcareous material of dissolving is identical but same acid solution that the pH value is different.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012104838377A CN102928345A (en) | 2012-11-26 | 2012-11-26 | Method for removing deposits and suspended matters during measurement of total iron content in high-calcium material |
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| CN2012104838377A CN102928345A (en) | 2012-11-26 | 2012-11-26 | Method for removing deposits and suspended matters during measurement of total iron content in high-calcium material |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539345A (en) * | 2010-12-21 | 2012-07-04 | 湖南晟通科技集团有限公司 | Method for measuring and analyzing Fe content of carbon material |
| CN102590108A (en) * | 2012-01-06 | 2012-07-18 | 安徽省石英砂及制品质量监督检验中心 | Method for quickly and efficiently detecting content of trace elements in quartz sand through microwave digestion |
| CN103185715A (en) * | 2011-12-30 | 2013-07-03 | 北京有色金属研究总院 | Analytical method of ferroporphyrin in ore biological leaching liquid |
-
2012
- 2012-11-26 CN CN2012104838377A patent/CN102928345A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102539345A (en) * | 2010-12-21 | 2012-07-04 | 湖南晟通科技集团有限公司 | Method for measuring and analyzing Fe content of carbon material |
| CN103185715A (en) * | 2011-12-30 | 2013-07-03 | 北京有色金属研究总院 | Analytical method of ferroporphyrin in ore biological leaching liquid |
| CN102590108A (en) * | 2012-01-06 | 2012-07-18 | 安徽省石英砂及制品质量监督检验中心 | Method for quickly and efficiently detecting content of trace elements in quartz sand through microwave digestion |
Non-Patent Citations (5)
| Title |
|---|
| 刘晓婷: "邻菲罗啉分光光度法测定白云岩中的铁", 《新疆有色金属》 * |
| 宋洪: "磷灰石中微量氧化亚铁的测定", 《四川建材》 * |
| 李江蔓: "长石精矿中钾、钠、铁、铝的系统分析", 《江西有色金属》 * |
| 杨华根: "氨分子对钴的亚硝基红盐法的干扰研究", 《稀有金属》 * |
| 程建国主编: "《无机及分析化学》", 30 September 2006 * |
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Application publication date: 20130213 |