CN111398266A - Rapid detection method of cerium-containing rare earth carbonate - Google Patents

Rapid detection method of cerium-containing rare earth carbonate Download PDF

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Publication number
CN111398266A
CN111398266A CN202010303988.4A CN202010303988A CN111398266A CN 111398266 A CN111398266 A CN 111398266A CN 202010303988 A CN202010303988 A CN 202010303988A CN 111398266 A CN111398266 A CN 111398266A
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sample
rare earth
cerium
carbonate
treo
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李颖毅
李永绣
杜国平
刘兵发
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Nanchang University
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Nanchang University
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems 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
    • G01N21/78—Systems 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems 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
    • G01N2021/775—Indicator and selective membrane

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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)
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  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention discloses a rapid detection method of cerium-containing rare earth carbonate, which utilizes the reaction of trivalent cerium and hydrogen peroxide to generate brown cerium peroxide, and carries out qualitative analysis on the components of a sample by observing the color change of a rare earth carbonate sample to be detected after the hydrogen peroxide is added. The method disclosed by the invention is simple to operate, is rapid and efficient, can visually reflect the existence of the rare earth cerium in the rare earth sample, is suitable for rapid detection of a production field of a rare earth workshop, and effectively solves the problem of long detection period of the existing industrial cerium-containing carbonate qualitative analysis detection method.

Description

Rapid detection method of cerium-containing rare earth carbonate
Technical Field
The invention relates to the field of rare earth qualitative analysis, in particular to a rapid detection method of cerium-containing rare earth carbonate.
Background
At present, no effective method exists for qualitative analysis of the cerium-containing carbonate of the rare earth, and with the high efficiency and the high speed of rare earth production, the method has great demand for on-site rapid detection. Typically, rare earth assay analysis takes at least 1-4 hours and takes sample time. The invention provides a rapid detection method of cerium-containing rare earth carbonate by combining with rare earth workshop production. The method is very simple, rapid and efficient, and the detection of the rare earth sample can be completed within 1-10 minutes.
Disclosure of Invention
The technical scheme adopted by the invention is as follows:
a rapid detection method of cerium-containing rare earth carbonate comprises the following steps:
s1, weighing 2-50g of rare earth carbonate sample to be detected, putting the rare earth carbonate sample into a 50-200ml beaker, and dripping 20-50% of analytically pure H by using a rubber head dropper2O22-20 ml; standing the sample for 1-10min, and observing whether the color of the sample changes;
s2, when the color of the sample is observed to be changed from white to tan, the sample to be detected contains rare earth cerium; when no obvious color change of the sample is observed, the sample does not contain rare earth cerium.
Weighing 20g of rare earth carbonate sample to be detected, putting the rare earth carbonate sample into a 100ml beaker, and dropwise adding 30% of analytically pure H by using a rubber head dropper2O210ml, standing for 10min, wherein the mass fraction of the sample is L a if the sample is not discolored2O3/TREO>99.9 percent of high-purity lanthanum carbonate, and the sample is changed from white to tan to be lanthanum cerium carbonate.
Weighing 2g of rare earth carbonate sample to be detected, putting the rare earth carbonate sample into a 50ml beaker, and dropwise adding 30% of analytically pure H by using a rubber head dropper2O22 ml; standing for 10min, wherein the mass fraction of CeO is determined when the color of the sample is changed from white to tan2/TREO>50 percent of cerium lanthanum carbonate, and the mass fraction of the sample without color change is L a2O3/TREO>99.9 percent of high-purity lanthanum carbonate.
Weighing 50g of rare earth carbonate sample to be detected, putting the rare earth carbonate sample into a 200ml beaker, and dropwise adding 30% of analytically pure H by using a rubber head dropper2O220ml of the solution; standing for 10min, wherein the mass fraction of CeO is determined when a sample has little brownish brown2/TREO =1% and L a2O3TREO =99% lanthanum cerium carbonate, CeO when a large amount of the sample turns tan2/TREO =10% and L a2O3/TREO =90% lanthanum cerium carbonate.
The detection range of the rare earth carbonate sample in the step S1 is mass fraction CeO2Rare earth carbonate sample with TREO (specific reaction temperature) more than or equal to 1 percent
The invention has the beneficial effects that:
1. the color change in the process of generating cerium peroxide by the reaction of trivalent cerium and hydrogen peroxide is utilized to carry out qualitative analysis on the rare earth sample to be detected, and the existence of rare earth cerium in the rare earth sample can be reflected visually.
2. The method disclosed by the invention is simple to operate, is quick in reaction, is suitable for quick detection of a production field of a rare earth workshop, and effectively solves the problem of long detection period of the existing industrial cerium-containing carbonate qualitative analysis detection method.
Detailed Description
The present invention will be further described with reference to the following examples.
A rapid detection method of cerium-containing rare earth carbonate comprises the following steps:
s1, weighing 2-50g of rare earth carbonate sample to be detected, putting the rare earth carbonate sample into a 50-200ml beaker, and dripping 20-50% of analytically pure H by using a rubber head dropper2O22-20 ml; standing the sample for 1-10min, and observing whether the color of the sample changes;
s2, when the color of the sample is observed to be changed from white to tan, the sample to be detected contains rare earth cerium; when no obvious color change of the sample is observed, the sample does not contain rare earth cerium.
The detection range of the rare earth carbonate sample in the step S1 is mass fraction CeO2/TREO>1% of a sample of rare earth carbonate.
EXAMPLE 1L a2O3/TREO>99.9% high purity lanthanum carbonate and CeO2/TREO =10% and L a2O3Qualitative distinction of lanthanum cerium carbonate/TREO =90%
20g of each sample was taken and put into a 100ml beaker, and 30% of analytically pure H was added dropwise with a rubber dropper2O210ml, mass fraction L a if the sample did not change color2O3/TREO>99.9 percent of high-purity lanthanum carbonate, and the mass fraction of CeO is determined when the color of the sample is changed from white to tan2/TREO =10% and L a2O3/TREO =90% lanthanum cerium carbonate.
Example 2: CeO (CeO)2/TREO =10% and L a2O3/TREO =90% lanthanum cerium carbonate and CeO2/TREO =1% and L a2O3Qualitative distinction of lanthanum cerium carbonate/TREO =99%
Respectively taking 50g of samples, putting the samples into a 200ml beaker, and using a rubber headDripping 30% analytically pure H into a dropper2O220 ml. The mass fraction of CeO is determined when the sample has a small amount of brownish brown2/TREO =1% and L a2O3/TREO =99% lanthanum cerium carbonate, mass fraction CeO if there is a large amount of white to tan2/TREO =10% and L a2O3/TREO =90% lanthanum cerium carbonate.
Example 3: CeO (CeO)2/TREO>50% cerium lanthanum carbonate and L a2O3/TREO>Qualitative distinction of 99.9% high purity lanthanum carbonate
2g of each sample was taken and placed in a 50ml beaker, and 30% of analytically pure H was added dropwise with a rubber-tipped dropper2O22 ml. The sample color is changed from white to brown and is CeO in percentage by mass2/TREO>50 percent of cerium lanthanum carbonate, and the mass fraction of the sample is L a when the sample is not discolored2O3/TREO>99.9 percent of high-purity lanthanum carbonate.
Example 4: qualitative differences between CeO2/TREO =5% LaCe-Pr-Nd carbonate and CeO2/TREO =0.1% Pr-Nd carbonate
20g of each sample was taken and put into a 100ml beaker, and 30% of analytically pure H was added dropwise with a rubber dropper2O25 ml. The sample is CeO in mass fraction if no color change occurs2/TREO =0.1% praseodymium neodymium carbonate, the sample color changed to tan, and mass fraction CeO2/TREO =5% lanthanum cerium praseodymium neodymium carbonate.
Although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention.

Claims (5)

1. A rapid detection method of cerium-containing rare earth carbonate is characterized by comprising the following steps:
s1, weighing 2-50g of rare earth carbonate sample to be detected, putting the rare earth carbonate sample into a 50-200ml beaker, and dripping 20-50% of analytically pure H by using a rubber head dropper2O22-20 ml; standing the sample for 1-10min, and observing whether the color of the sample changes;
s2, when the color of the sample is observed to be changed from white to tan, the sample to be detected contains rare earth cerium; when no obvious color change of the sample is observed, the sample does not contain rare earth cerium.
2. The method for rapidly detecting cerium-containing rare earth carbonate as claimed in claim 1, wherein 20g of a rare earth carbonate sample to be detected is weighed and placed in a 100ml beaker, and 30% analytically pure H is added dropwise with a rubber dropper2O210ml, standing for 10min, wherein the mass fraction of the sample is L a if the sample is not discolored2O3/TREO>99.9 percent of high-purity lanthanum carbonate, and the mass fraction of CeO is determined when the color of the sample is changed from white to tan2/TREO =10% and L a2O3/TREO =90% lanthanum cerium carbonate.
3. The method for rapidly detecting cerium-containing rare earth carbonate as claimed in claim 1, wherein 2g of a rare earth carbonate sample to be detected is weighed and placed in a 50ml beaker, and 30% analytically pure H is added dropwise with a rubber dropper2O22 ml; standing for 10min, wherein the mass fraction of CeO is determined when the color of the sample is changed from white to tan2/TREO>50 percent of cerium lanthanum carbonate, and the mass fraction of the sample without color change is L a2O3/TREO>99.9 percent of high-purity lanthanum carbonate.
4. The method for rapidly detecting cerium-containing rare earth carbonate as claimed in claim 1, wherein 50g of a rare earth carbonate sample to be detected is weighed and placed in a 200ml beaker, and 30% analytically pure H is added dropwise with a rubber dropper2O220ml of the solution; standing for 10min, wherein the mass fraction of CeO is determined when a sample has little brownish brown2/TREO =1% and L a2O3TREO =99% lanthanum cerium carbonate, CeO when a large amount of the sample turns tan2/TREO =10% and L a2O3/TREO =90% lanthanum cerium carbonate.
5. The method of claim 1, wherein the rare earth carbonate sample is detected in the mass fraction CeO of the rare earth carbonate sample in step S12the/TREO is more than or equal to 1 percent of the rare earth carbonate sample.
CN202010303988.4A 2020-04-17 2020-04-17 Rapid detection method of cerium-containing rare earth carbonate Pending CN111398266A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1138586A (en) * 1996-01-22 1996-12-25 宝山钢铁(集团)公司 Rare-earth developer, its prepn. and use in determing micro-cerium group rare-earth
CN101633516A (en) * 2008-07-23 2010-01-27 甘肃稀土新材料股份有限公司 Preparation method of high-purity cerium hydroxide
CN102507535A (en) * 2011-10-28 2012-06-20 内蒙古包钢钢联股份有限公司 Determination method of lanthanum and cerium content in rare earth silicon aluminum iron
US20160002751A1 (en) * 2013-01-18 2016-01-07 Rare Element Resources Ltd. Selective extraction of cerium from other metals
CN108051385A (en) * 2017-12-11 2018-05-18 中国科学院长春应用化学研究所 It is a kind of to measure the method for mixing cerium content in cerium mischmetal silicate scintillation crystal

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1138586A (en) * 1996-01-22 1996-12-25 宝山钢铁(集团)公司 Rare-earth developer, its prepn. and use in determing micro-cerium group rare-earth
CN101633516A (en) * 2008-07-23 2010-01-27 甘肃稀土新材料股份有限公司 Preparation method of high-purity cerium hydroxide
CN102507535A (en) * 2011-10-28 2012-06-20 内蒙古包钢钢联股份有限公司 Determination method of lanthanum and cerium content in rare earth silicon aluminum iron
US20160002751A1 (en) * 2013-01-18 2016-01-07 Rare Element Resources Ltd. Selective extraction of cerium from other metals
CN108051385A (en) * 2017-12-11 2018-05-18 中国科学院长春应用化学研究所 It is a kind of to measure the method for mixing cerium content in cerium mischmetal silicate scintillation crystal

Non-Patent Citations (2)

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Title
乔军 等: "高纯氢氧化铈制备工艺研究", 《湿法冶金》 *
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