CN108490112A - The assay method of basic magnesium chloride in a kind of water-free magnesium chloride granule - Google Patents
The assay method of basic magnesium chloride in a kind of water-free magnesium chloride granule Download PDFInfo
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- CN108490112A CN108490112A CN201810227257.9A CN201810227257A CN108490112A CN 108490112 A CN108490112 A CN 108490112A CN 201810227257 A CN201810227257 A CN 201810227257A CN 108490112 A CN108490112 A CN 108490112A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
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Abstract
The invention discloses a kind of assay method of basic magnesium chloride in water-free magnesium chloride granule, magnesia exists at suspended state in the electrolyte, and the magnesium globule of part is entered by magnesia entrainment in slag.Depositing to the magnesia of cathodic work piece makes magnesium globule be difficult to assemble on cathode plane and grow up, and magnesium globule excessively disperses, and increases the chance of secondary response, seriously affects cathodic process.The detection method of industrial basic magnesium chloride has the molten method of water-soluble acid extracting, alcohol, but when both methods is very low for basic magnesium chloride content, and the data error of measurement is larger, makes troubles for Precise control；The present invention is reacted using chemical reaction and titration, that is, basic magnesium chloride with quantitative hydrochloric acid, it is excessive sour and with KI KIO3Reaction generates iodine, and iodine is reacted with sodium thiosulfate again to be titrated with starch as indicator, and referred to as iodimetric titration, iodimetric titration can detect basic magnesium chloride micro in anhydrous magnesium chloride, and precision is relatively high.
Description
Technical field
The present invention relates to the assay method field of basic magnesium chloride in water-free magnesium chloride granule, specifically a kind of anhydrous chlorination
The assay method of basic magnesium chloride in magnesium granules.
Background technology
Qinghai Chaerhan salt lakes are the chloride type potassium sodium magnesium salts mineral deposits of Largest In China, have large storage capacity, grade height, type
Entirely, it is distributed Relatively centralized, the features such as combination of resources is good, wherein 55,500,000,000 tons of sodium chloride reserves, 1.5 hundred million tons of potassium chloride reserves, chlorination
4,900,000,000 tons of magnesium, and the national strategies resource such as have abundant lithium, rubidium, caesium, are the salt lake of domestic most Development volue, potential economic valence
It is worth up to more than 12 trillion yuans.
The old halogen generated when the potash fertilizer enterprise production potash fertilizer in Cha Er Han area is largely still discharged into salt lake, these old halogen are such as
Fruit is not used, and both results in waste of resources, and also results in environmental pollution, therefore Qinghai Salt Lake Mei Ye Co., Ltds introduce generation in due course
Magnesium technology is refined in the advanced electrolysis in boundary, is raw material using the abundant brine in salt lake by innovation, is built a phase and produce per year
100000 tons of electrolysis magnesium smelting devices.The device is divided into brine refining, evaporation, granulation, air dehydration, hydrogen chloride dehydration, supplies water, supplies
The processes such as electricity, gas supply, wherein 1,250,000 tons of bischofites of consumption every year, accordingly produce 440,000 tons of anhydrous magnesium chlorides and 100,000 tons of gold
Belong to magnesium, this technology transfer efficiently solves the bottleneck problem of salt lake resources comprehensive development and utilization, it will generate prodigious economic effect
Benefit and social benefit.
For bischofite in 400 DEG C of dehydration material below, hydrolysate MgOHCl, the country is usually to be indicated with water soluble magnesium
MgCl in primary dewatering material2Content, the content of MgO is indicated with the insoluble magnesium of water.Measured solvable magnesium is chlorine in sample in this way
Change magnesium and is transformed by basic magnesium chloride.Thus, using solvable magnesium as the MgCl in sample2, more higher than real content；Not
Molten magnesium is relatively low more a lot of than the practical content for being MgOHCl as the MgO in sample.Domestic coastal certain brine Lian Mei little factories are de-
The primary dewatering material MgCl of water material2Content is mostly 70% hereinafter, some is less than 60%；And the content of MgOHCl is in 10-20%
Between.Magnesium metal is produced with this material Direct Electrolysis, total quantity of slag is up to 1-2 tons of magnesium/ton magnesium, and current efficiency is only 60-75%, always
Power consumption is ten thousand KWhs/ton of magnesium of 5-7, the main reason is that the dehydration aqueous and MgOHCl of material compared with plateau because.So the detection that selection is suitable
Method can obtain accurate, reliable detection data in time, and parameter adjustment, control basic magnesium chloride content are provided for production line
Foundation is provided.
Contain multiple element in salt lake bittern, have Li, Na, K, Mg, Ca, Si, Ba, Pb, P, S, Cl, Br, Fe, B, Ni, Cu,
Tens kinds of compositions such as Zn, Al, some of which element also have the substances such as basic magnesium chloride, boride, magnesia to magnesium eletrolysis process
Harmful, basic magnesium chloride can be converted into magnesia in a cell, and magnesia can cause cathode to be passivated, and so that magnesium is collected bad.
Magnesia exists at suspended state in electrolyte, and the magnesium globule of part is entered by magnesia entrainment in slag.Deposit to cathodic work piece
Magnesia make magnesium globule be difficult to assemble on cathode plane and grow up, magnesium globule excessively disperses, and increases the chance of secondary response, serious shadow
Ring cathodic process.Therefore, it is extremely important that basic magnesium chloride content is controlled in production.
The detection method of industrial basic magnesium chloride has the molten method of water-soluble acid extracting, alcohol, etc. quality two parts of samples, a sample
Product can use sour sample dissolution to measure Mg2+ (acid is molten) % amounts, the water-soluble measurement Mg of another sample2+(water-soluble) %, acid are molten and water-soluble
MgOHCl and MgCl in sample is calculated according to the following formula out in sample respectively2。
MgOHCl%=[Mg2+(acid is molten) %-Mg2+(water-soluble) %] × 2 × 3.157
MgCl2%=MgCl2(water-soluble) -0.6196 × MgOHCl%
In formula：2x 3.157=2M MgOHCl/M Mg2+
0.6196=M MgCl2/2M MgOHCl
But when both methods is very low for basic magnesium chloride content, the data error of measurement is larger, is Precise control
It makes troubles.
Invention content
The purpose of the present invention is to provide a kind of assay methods of basic magnesium chloride in water-free magnesium chloride granule, in solution
State the problem of being proposed in background technology.
To achieve the above object, the present invention provides the following technical solutions：Basic magnesium chloride in a kind of water-free magnesium chloride granule
Assay method, include the following steps：
S1:The water-free magnesium chloride granule that quality is 5 ± 0.1000g is weighed to be placed in 250ml iodine flasks, it is then accurate to be added
The hydrochloric acid solution of a concentration of 15ml0.05mol/L carries out the liquid in bottle wall with a small amount of level-one water after particle is completely dissolved
It rinses, is then cooled to room temperature solution；
S2:The Na of a concentration of 0.025mol/L of 10ml is added into solution2S2O3Then solution shakes up；
S3:Then the KI-KIO of 2ml volumes is added into solution3Solution；
S4:Immediately after with the Na of a concentration of 0.025mol/L2S2O3Solution titrates, light yellow until occurring in solution；
S5:Then 1ml starch indicators are added into solution；
S6:Continue to titrate, until solution becomes colorless, and keeps 15s；
S7:Blank test is done by the same way；
S8:As a result it calculates：
In formula：M-weighs the quality of water-free magnesium chloride granule.
Compared with prior art, the beneficial effects of the invention are as follows：The present invention is to utilize chemical reaction and titration i.e. alkali formula
Magnesium chloride is reacted with quantitative hydrochloric acid, excessive acid and and KI-KIO3Reaction generates iodine, and iodine is reacted with sodium thiosulfate again uses starch
It is titrated as indicator, referred to as iodimetric titration, iodimetric titration can detect basic magnesium chloride micro in anhydrous magnesium chloride, precision
It is relatively high.
Description of the drawings
Fig. 1 is a kind of step schematic diagram of the assay method of basic magnesium chloride in water-free magnesium chloride granule.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Referring to Fig. 1, in the embodiment of the present invention 1, the assay method of basic magnesium chloride, packet in a kind of water-free magnesium chloride granule
Include following steps：
S1:It weighs the water-free magnesium chloride granule that quality is 4.9000g to be placed in 250ml iodine flasks, then accurately be added dense
Degree is that the hydrochloric acid solution of 15ml0.05mol/L rushes the liquid in bottle wall with a small amount of level-one water after particle is completely dissolved
It washes, is then cooled to room temperature solution；
S2:The Na of a concentration of 0.025mol/L of 8ml is added into solution2S2O33 solution, then shake up；
S3:Then the KI-KIO of 1ml volumes is added into solution3Solution；
S4:Immediately after with the Na of a concentration of 0.025mol/L2S2O3Solution titrates, light yellow until occurring in solution；
S5:Then 1ml starch indicators are added into solution；
S6:Continue to titrate, until solution becomes colorless, and keeps 15s；
S7:Blank test is done by the same way；
S8:As a result it calculates：
In formula：M-weighs the quality of water-free magnesium chloride granule.
In the embodiment of the present invention 2, the assay method of basic magnesium chloride in a kind of water-free magnesium chloride granule, including following step
Suddenly：
S1:It weighs the water-free magnesium chloride granule that quality is 5.1000g to be placed in 250ml iodine flasks, then accurately be added dense
Degree is that the hydrochloric acid solution of 15ml0.05mol/L rushes the liquid in bottle wall with a small amount of level-one water after particle is completely dissolved
It washes, is then cooled to room temperature solution；
S2:The Na of a concentration of 0.025mol/L of 12ml is added into solution2S2O33 solution, then shake up；
S3:Then the KI-KIO of 3ml volumes is added into solution3Solution；
S4:Immediately after with the Na of a concentration of 0.025mol/L2S2O3Solution titrates, light yellow until occurring in solution；
S5:Then 1ml starch indicators are added into solution；
S6:Continue to titrate, until solution becomes colorless, and keeps 15s；
S7:Blank test is done by the same way；
S8:As a result it calculates：
In formula：M-weighs the quality of water-free magnesium chloride granule.
In the embodiment of the present invention 3, the assay method of basic magnesium chloride in a kind of water-free magnesium chloride granule, including following step
Suddenly：
S1:It weighs the water-free magnesium chloride granule that quality is 5.0000g to be placed in 250ml iodine flasks, then accurately be added dense
Degree is that the hydrochloric acid solution of 15ml0.05mol/L rushes the liquid in bottle wall with a small amount of level-one water after particle is completely dissolved
It washes, is then cooled to room temperature solution；
S2:The Na of a concentration of 0.025mol/L of 10ml is added into solution2S2O33 solution, then shake up；
S3:Then the KI-KIO of 2ml volumes is added into solution3Solution；
S4:Immediately after with the Na of a concentration of 0.025mol/L2S2O3Solution titrates, light yellow until occurring in solution；
S5:Then 1ml starch indicators are added into solution；
S6:Continue to titrate, until solution becomes colorless, and keeps 15s；
S7:Blank test is done by the same way；
S8:As a result it calculates：
In formula：M-weighs the quality of water-free magnesium chloride granule.
The present invention operation principle be：The present invention is to utilize chemical reaction and titration i.e. basic magnesium chloride and quantitative hydrochloric acid
Reaction, excessive acid and and KI-KIO3Reaction generates iodine, and iodine is reacted with sodium thiosulfate and dripped as indicator with starch again
Fixed, referred to as iodimetric titration, iodimetric titration can detect basic magnesium chloride micro in anhydrous magnesium chloride, and precision is relatively high.
MgOHCl+xHCl→MgCl2+H2O+yHCl
Excessive hydrogen ion and KI-KIO3Reaction generates iodine, the iodine and Na of generation2S2O3Reaction, with starch make indicator into
Row titration.
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art,
It still can be with technical scheme described in the above embodiments is modified, or is carried out to which part technical characteristic etc.
With replacing, all within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in this
Within the protection domain of invention.
Claims (10)
1. the assay method of basic magnesium chloride in a kind of water-free magnesium chloride granule, which is characterized in that include the following steps：
S1:It weighs the water-free magnesium chloride granule that quality is 5 ± 0.1000g to be placed in iodine flask, then accurately be added a concentration of
Then solution is cooled to room temperature by the hydrochloric acid solution of 15ml0.05mol/L after particle is completely dissolved；
S2:The Na of a concentration of 0.025mol/L is added into solution2S2O3Then solution shakes up；
S3:Then the KI-KIO of volume is added into solution3Solution；
S4:Immediately after with the Na of a concentration of 0.025mol/L2S2O3Solution titrates, light yellow until occurring in solution；
S5:Then 1ml starch indicators are added into solution；
S6:Continue to titrate, until solution becomes colorless, and keeps 15s；
S7:Blank test is done by the same way；
S8:As a result it calculates：
2. the assay method of basic magnesium chloride in water-free magnesium chloride granule according to claim 1, which is characterized in that described
After particle is completely dissolved, the liquid in bottle wall is rinsed with a small amount of level-one water, is then cooled to room temperature solution.
3. the assay method of basic magnesium chloride in water-free magnesium chloride granule according to claim 1, which is characterized in that described
Water-free magnesium chloride granule is weighed using electronic balance in S1, uses glass bar molten to water-free magnesium chloride granule and hydrochloric acid in the S1
Liquid is to accelerate to dissolve.
4. the assay method of basic magnesium chloride in water-free magnesium chloride granule according to claim 1, which is characterized in that described
Solution is cooled down by the method for natural cooling in S1.
5. the assay method of basic magnesium chloride in water-free magnesium chloride granule according to claim 1, which is characterized in that described
In step 3 KI-KIO is measured using graduated cylinder3Solution.
6. the assay method of basic magnesium chloride in water-free magnesium chloride granule according to claim 1, which is characterized in that described
It is titrated using buret and volumetric flask in S4.
7. the assay method of basic magnesium chloride in water-free magnesium chloride granule according to claim 1, which is characterized in that described
Starch indicator is now with the current in S5.
8. the assay method of basic magnesium chloride in water-free magnesium chloride granule according to claim 1, which is characterized in that described
Timing is carried out by stopwatch in step S6.
9. the assay method of basic magnesium chloride in water-free magnesium chloride granule according to claim 1, which is characterized in that described
Blank assay in step S7 refers to quantitatively being divided with the identical method of determination sample, step in the case where being not added with sample
Analysis, using acquired results as blank value, is deducted from the analysis result of sample.
10. the assay method of basic magnesium chloride in water-free magnesium chloride granule according to claim 1, which is characterized in that institute
It states in step S8, m is the quality for weighing water-free magnesium chloride granule.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102706868A (en) * | 2012-06-04 | 2012-10-03 | 哈尔滨医科大学 | Quick salt iodine quantitative detection equipment |
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2018
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102706868A (en) * | 2012-06-04 | 2012-10-03 | 哈尔滨医科大学 | Quick salt iodine quantitative detection equipment |
Non-Patent Citations (4)
| Title |
|---|
| I.M.科尔索夫 等: "《定量化学分析》", 30 April 1987, 高等教育出版社 * |
| 李迅 等: "一种氯化镁的简易脱水工艺及分析方法"", 《现代化工》 * |
| 河南省农村厅教材编辑委员会: "《无机化学及分析化学》", 30 September 1958, 河南人民出版社 * |
| 胡湖生等: "EDTA滴定法直接测定水氯镁石脱水产品中氧化镁", 《冶金分析》 * |
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