CN102564841A - Method for preparing analysis solution for inductively coupled plasma-atomic emission spectrometry (ICP-AES) and atomic absorption spectroscopy (AAS) by using lithium metaborate - Google Patents
Method for preparing analysis solution for inductively coupled plasma-atomic emission spectrometry (ICP-AES) and atomic absorption spectroscopy (AAS) by using lithium metaborate Download PDFInfo
- Publication number
- CN102564841A CN102564841A CN2012100351117A CN201210035111A CN102564841A CN 102564841 A CN102564841 A CN 102564841A CN 2012100351117 A CN2012100351117 A CN 2012100351117A CN 201210035111 A CN201210035111 A CN 201210035111A CN 102564841 A CN102564841 A CN 102564841A
- Authority
- CN
- China
- Prior art keywords
- sample
- icp
- aes
- aas
- lithium metaborate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a method for preparing an analysis solution for inductively coupled plasma-atomic emission spectrometry (ICP-AES) and atomic absorption spectroscopy (AAS) by using lithium metaborate. The method comprises the following steps of: melting and decomposing an oxidative sample to be inspected in a platinum or platinum yellow crucible by using lithium metaborate; directly pouring molten liquid into dilute acid; and heating to ensure that the molten liquid of the oxidative sample is completely dissolved in the dilute acid to obtain the analysis solution. According to the method, the problem about sample dissolution of antiacid oxide is effectively solved by using the strong melting and decomposition characteristic of the lithium metaborate on the oxide, and the good demoulding effect of the lithium metaborate in the platinum or platinum yellow crucible and is generally used for common oxide; and the obtained analysis solution is suitable for ICP-AES and AAS. By using the method, operation steps are simplified, the pollution possibility of samples is reduced, and a sodium element can be determined. The method is completely suitable for analysis of ICP-AES and AAS, and has the characteristics of short sample preparation time and high repeatability, and is easy to operate.
Description
Technical field
The invention belongs to technical field of analysis and detection, especially a kind ofly produce ICP-AES and AAS method with analytical solution with lithium metaborate.
Background technology
In whole physical and chemical inspection process; The sample survey of being made up of oxide or composite oxides has occupied a very big ratio of whole work for inspection, like the check of the dedusting ash in various geology class samples, all kinds of slag, part steelmaking ingredient, the blast furnace secondary product, gas ash etc.General, during micro-in adopting ICP-AES and AAS working sample, at first need process sample the WS of clarification, all be dissolved in the WS to guarantee all elements to be measured, otherwise test job is insignificant.Carrying out ICP-AES and AAS when carrying out element determination, for the dissolving sample preparation of sample, generally adopt acid mixture to dissolve appearance at present, nitric acid, hydrochloric acid, sulfuric acid, phosphoric acid and dangerous acid+hydrofluoric acid and perchloric acid unites use often.However, marquis's solute effect is also also not fully up to expectations sometimes, such as the dissolving sample preparation of iron ore, dedusting ash, gas ash etc., unite use various acid after, still have deposition in the sample and exist.For this reason, general solution is to adopt the sodium borate alkali fusion; Together with carrying out acidleach in the crucible input beaker, process is loaded down with trivial details after the fusion, and owing to be the acidleach of carrying out together with crucible; Pollute probability and also obviously increase, simultaneously because the use of sodium borate has also limited the mensuration of sodium element.
Summary of the invention
The technical matters that the present invention will solve provides a kind of lithium metaborate and produces ICP-AES and the AAS method with analytical solution, solving some molten appearance problems with sour indissoluble sample, and is common to general oxide.
For solving the problems of the technologies described above, the technical scheme that the present invention taked is: it carries out fusion and decomposition to the oxidisability sample that will check with lithium metaborate earlier in platinum or platinum yellow crucible; Directly pour fused solution into then and fill among the diluted acid; Heating at last is dissolved among the diluted acid fused solution of oxidisability sample fully, promptly obtains described analytical solution.
The further processing step of the present invention is:
(1) get lithium metaborate and oxidisability sample and put into platinum or platinum yellow crucible, add release agent, 900～1100 ℃ of following fusions, rotation crucible in fusing back makes the fusion of oxidisability sample fully;
(2) pouring the fused solution of the oxidisability sample that obtains after the fusion into percent by volume is among 3～15% the rare nitric acid or watery hydrochloric acid;
(3) heating contains the rare nitric acid or the watery hydrochloric acid of fused solution, among fused solution is dissolved in rare nitric acid or watery hydrochloric acid fully, can obtain described analytical solution.
Oxidisability sample according to the invention is the composite oxides of oxide or disassembled one-tenth oxide.
The mass ratio of lithium metaborate according to the invention and sample is preferably 1:3～10.
The preferred release agent of the present invention is iodide or bromide solution, and concentration is 30g/100mL.
The consumption of the preferred oxidisability sample of the present invention is 0.1000～0.5000g, and the addition of release agent is 0.5～3mL.
The diluted acid heating for dissolving 2～15min that contains fused solution according to the invention.
Adopt the beneficial effect that technique scheme produced to be: the present invention utilizes the lithium metaborate fusion and decomposition characteristic strong to oxide; And lithium metaborate good stripping result in platinum or platinum yellow crucible, can adopt fused solution directly to pour the method that generates analytical solution in the diluted acid fast into; The present invention has effectively solved the molten appearance problem of antiacid oxide, and is common to general oxide; Gained analytical solution be applicable to inductively coupled plasma atomic emission spectrometry and atomic absorption spectrum.The difference of the general sodium borate alkali fusion of the inventive method is to adopt a step tipping, has simplified operation steps, has reduced the contaminated probability of sample, and has realized the mensuration of sodium element.
Be applicable to ICP-AES and AAS that the inventive method adopts a small amount of lithium metaborate and single dilute acid soln (salpeter solution as 3%) to be clarified fully analyze the solution of usefulness; Reduced the use of dangerous acid (hydrofluorite, perchloric acid etc.); What discharge also is the minimum waste liquid of harm; Therefore can effectively reduce and detect the pollution that produces, have the characteristics of green, environmental protection.
Adopt the inventive method can make the analytical solution of the no any deposition of clarification fully, be applicable to that fully ICP-AES and AAS analyze usefulness; Characteristics with short, simple to operate, favorable reproducibility of sample preparation time, the analysis result that obtains accurately and reliably, analysis data is rapid, the needs of accuracy to detecting to meet modern enterprise, has also widened the range of application of ICP-AES and AAS.
Embodiment
Lithium metaborate of the present invention produce ICP-AES and AAS with the method for analytical solution comprise the molten appearance of lithium metaborate, topple over, step such as dissolving; Use through lithium metaborate; Make the structure of separating material with sour indissoluble destroy fully, be easy to make the fluid sample of clarifying fully.In the method, related sample is an oxide, so can not cause damage to platinum or platinum yellow crucible, in the fused solution toppling process, because the use of release agent in the high-temp liquid moment entering diluted acid, can not cause splash, whole process is safe and reliable.
Further specify the inventive method through specific embodiment below.
Embodiment 1: this fusion method for making sample is accomplished through following steps:
1, take by weighing 0.2000g iron ore sample, the 0.8000g lithium metaborate is put into platinum or platinum yellow crucible, adds 1mL liquor kalii iodide (concentration 30g/100mL), 1000
oFusion under the C, rotation crucible twice in fusing back makes the fusion of iron ore sample fully;
2, the liquid after the fusion is poured into fast filled in the beaker that volumn concentration is 8% dilute nitric acid solution;
3, be placed on beaker on the electric hot plate, heating 2～15min dissolves to the iron ore sample fully;
4, be transferred to constant volume in the volumetric flask to the solution in the beaker, promptly get and be applicable to that ICP-AES and AAS analyze the solution of usefulness.
Embodiment 2: this fusion method for making sample is accomplished through following steps:
1, take by weighing 0.3000g magnesia sample, the 1.0000g lithium metaborate is put into platinum or platinum yellow crucible, adds the 0.5mL bromination and receives solution (concentration 30g/100mL), 1000
oFusion under the C, rotation crucible twice in fusing back makes the fusion of magnesia sample fully;
2, the liquid after the fusion is poured into fast filled in the beaker that volumn concentration is 5% dilute nitric acid solution;
3, be placed on beaker on the electric hot plate, heating 2～15min dissolves to the magnesia sample fully;
4, be transferred to constant volume in the volumetric flask to the solution in the beaker, promptly get and be applicable to that ICP-AES and AAS analyze the solution of usefulness.
Embodiment 3: this fusion method for making sample is accomplished through following steps:
1, take by weighing 0.4000g ferrous acid manganese sample, the 1.5000g lithium metaborate is put into platinum or platinum yellow crucible, adds 1.5mL sodium iodide solution (concentration 30g/100mL), 1100
oFusion under the C, rotation crucible twice in fusing back makes the fusion of ferrous acid manganese sample fully;
2, the liquid after the fusion is poured into fast filled in the beaker that volumn concentration is 10% dilute hydrochloric acid solution;
3, be placed on beaker on the electric hot plate, heating 2～15min dissolves to ferrous acid manganese sample fully;
4, be transferred to constant volume in the volumetric flask to the solution in the beaker, promptly get and be applicable to that ICP-AES and AAS analyze the solution of usefulness.
Embodiment 4: this fusion method for making sample is accomplished through following steps:
1, take by weighing the 0.1000g clay sample, the 1.0000g lithium metaborate is put into platinum or platinum yellow crucible, adds 3.0mL potassium bromide solution (concentration 30g/100mL), 900
oFusion under the C, rotation crucible twice in fusing back makes the clay sample fusion fully;
2, the liquid after the fusion is poured into fast filled in the beaker that volumn concentration is 3% dilute nitric acid solution;
3, be placed on beaker on the electric hot plate, heating 2～15min dissolves to clay sample fully;
4, be transferred to constant volume in the volumetric flask to the solution in the beaker, promptly get and be applicable to that ICP-AES and AAS analyze the solution of usefulness.
Embodiment 5: this fusion method for making sample is accomplished through following steps:
1, take by weighing 0.5000g calcium titanate sample, the 1.5000g lithium metaborate is put into platinum or platinum yellow crucible, adds 2.0mL liquor kalii iodide (concentration 30g/100mL), 1000
oFusion under the C, rotation crucible twice in fusing back makes the fusion of calcium titanate sample fully;
2, the liquid after the fusion is poured into fast filled in the beaker that volumn concentration is 15% dilute hydrochloric acid solution;
3, be placed on beaker on the electric hot plate, heating 2～15min dissolves to the calcium titanate sample fully;
4, be transferred to constant volume in the volumetric flask to the solution in the beaker, promptly get and be applicable to that ICP-AES and AAS analyze the solution of usefulness.
Test Example 1: utilize this method to produce the magnesia WS, be used for ICP-AES and analyze, with accuracy and the stability of verifying this method.
(1) foundation of typical curve:
Select magnesia series standard sample as shown in table 1 for use, after employing the method for the invention is prepared the WS that is used for the ICP-AES analysis, measure each element-intensities and draw calibration curve.
(2) mensuration of sample:
Stability of this method and replica test are accomplished through same sample being carried out continuous 5 same operation, and the result is as shown in table 2.Can find out that the relative standard deviation of each element is all very little, explain that the whole process of this method is reliable and stable.
The accuracy of this method through and the comparison of x ray fluorescence spectrometry (GB/T 21114-2007) accomplish; The result is as shown in table 3; The measurement result that two kinds of distinct methods draw is very approaching, and within the error range that allows, the measured value that this method is described is accurately and reliably fully.
Test Example 2: utilize this method to produce the iron ore WS, be used for icp analysis, with accuracy and the stability of verifying this method.
(1) foundation of directrix curve:
Select iron ore series standard sample as shown in table 4 for use, after employing the method for the invention is prepared the WS that is used for icp analysis, measure each element-intensities and draw calibration curve, carry out the mensuration of K, Na and Zn in the iron ore.
(2) mensuration of sample:
Stability of this method and replica test are accomplished through same sample being carried out continuous 5 same operation, and the result is as shown in table 5.Can find out that the relative standard deviation of each element is all very little, explain that the whole process of this method is reliable and stable.
With the accuracy of standard model checking this method of having neither part nor lot in calibration curve, the result is as shown in table 6, can find out, measurement result and standard value are very approaching, within the error range of permission, explain that this method is accurately and reliably fully.
Claims (7)
1. a lithium metaborate is produced ICP-AES and AAS with the method for analytical solution, and it is characterized in that: it carries out fusion and decomposition to the oxidisability sample that will check with lithium metaborate earlier in platinum or platinum yellow crucible; Directly pour fused solution into then and fill among the diluted acid; Heating at last is dissolved among the diluted acid fused solution of oxidisability sample fully, promptly obtains described analytical solution.
2. lithium metaborate according to claim 1 is produced ICP-AES and AAS with the method for analytical solution, it is characterized in that its processing step is:
(1) get lithium metaborate and oxidisability sample and put into platinum or platinum yellow crucible, add release agent, 900～1100 ℃ of following fusions, rotation crucible in fusing back makes the fusion of oxidisability sample fully;
(2) pouring the fused solution of the oxidisability sample that obtains after the fusion into percent by volume is among 3～15% the rare nitric acid or watery hydrochloric acid;
(3) heating contains the rare nitric acid or the watery hydrochloric acid of fused solution, among fused solution is dissolved in rare nitric acid or watery hydrochloric acid fully, can obtain described analytical solution.
3. lithium metaborate according to claim 1 and 2 is produced ICP-AES and AAS with the method for analytical solution, and it is characterized in that: said oxidisability sample is the composite oxides of oxide or disassembled one-tenth oxide.
4. lithium metaborate according to claim 1 and 2 is produced ICP-AES and AAS with the method for analytical solution, and it is characterized in that: the mass ratio of said lithium metaborate and oxidisability sample is 1:3～10.
5. lithium metaborate according to claim 2 is produced ICP-AES and AAS with the method for analytical solution, and it is characterized in that: described release agent is iodide or bromide solution, and concentration is 30g/100mL.
6. produce ICP-AES and AAS with the method for analytical solution according to claim 2 or 5 described lithium metaborates, it is characterized in that: the consumption of said oxidisability sample is 0.1000～0.5000g, and the addition of release agent is 0.5～3mL.
7. lithium metaborate according to claim 1 and 2 is produced ICP-AES and AAS with the method for analytical solution, it is characterized in that: the said diluted acid heating for dissolving 2～15min that contains fused solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100351117A CN102564841A (en) | 2012-02-16 | 2012-02-16 | Method for preparing analysis solution for inductively coupled plasma-atomic emission spectrometry (ICP-AES) and atomic absorption spectroscopy (AAS) by using lithium metaborate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100351117A CN102564841A (en) | 2012-02-16 | 2012-02-16 | Method for preparing analysis solution for inductively coupled plasma-atomic emission spectrometry (ICP-AES) and atomic absorption spectroscopy (AAS) by using lithium metaborate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102564841A true CN102564841A (en) | 2012-07-11 |
Family
ID=46410846
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012100351117A Pending CN102564841A (en) | 2012-02-16 | 2012-02-16 | Method for preparing analysis solution for inductively coupled plasma-atomic emission spectrometry (ICP-AES) and atomic absorption spectroscopy (AAS) by using lithium metaborate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102564841A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111521467A (en) * | 2020-06-04 | 2020-08-11 | 河北省地质实验测试中心 | Graphite detection method |
| CN115389489A (en) * | 2022-08-04 | 2022-11-25 | 江苏沙钢集团淮钢特钢股份有限公司 | Method for detecting element content in iron ore |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101923016A (en) * | 2009-06-17 | 2010-12-22 | 华东电力试验研究院有限公司 | Blade deposit sediment measuring method for turbine |
-
2012
- 2012-02-16 CN CN2012100351117A patent/CN102564841A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101923016A (en) * | 2009-06-17 | 2010-12-22 | 华东电力试验研究院有限公司 | Blade deposit sediment measuring method for turbine |
Non-Patent Citations (4)
| Title |
|---|
| JEAN CARLOS MONTERO-SERRANO 等: "Sedimentary evidence of deglacial megafloods in the northern Gulf of Mexico (Pigmy Basin)", 《QUATERNARY SCIENCE REVIEWS》 * |
| 刘虎生 等: "偏硼酸锂熔样ICP-MS法测定土壤样品中15种痕量稀土元素", 《光谱学与光谱分析》 * |
| 张卫东 等: "高频熔解ICP-AES法测定镁砂中硅铁铝钙锰", 《现代科学仪器》 * |
| 马生凤 等: "偏硼酸锂碱熔-电感耦合等离子体发射光谱法测定硫化物矿中硅酸盐相的主成分", 《岩矿测试》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111521467A (en) * | 2020-06-04 | 2020-08-11 | 河北省地质实验测试中心 | Graphite detection method |
| CN111521467B (en) * | 2020-06-04 | 2023-08-29 | 河北省地质实验测试中心 | Graphite detection method |
| CN115389489A (en) * | 2022-08-04 | 2022-11-25 | 江苏沙钢集团淮钢特钢股份有限公司 | Method for detecting element content in iron ore |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105223050B (en) | Method for measuring scandium in bauxite by microwave digestion inductively coupled plasma spectrometry | |
| CN105136975B (en) | A kind of method of Calcium Fluoride Content in measure fluorite | |
| CN106018666A (en) | Oxygen bomb combustion method for testing content of halogens and content of sulphur in industrial solid waste | |
| CN103344587B (en) | Method for determination of molybdenum trioxide and/or tungsten trioxide content of high-molybdenum tungsten ore | |
| CN103115916B (en) | A kind of method measuring content of niobium in ferrocolumbium | |
| CN103439213B (en) | The system detecting method of industry carborundum component | |
| CN103954617B (en) | Method for detecting content of lithium carbonate | |
| CN102590255A (en) | Method for detecting main content of glass raw material | |
| CN104730139B (en) | The analysis method of fluorinion concentration under a kind of radioactivity | |
| CN104101572A (en) | Method for detecting content of heavy metals in inner liner for cigarette | |
| CN106645122A (en) | Determination method of content of zirconium in uranium-zirconium alloy | |
| CN102564841A (en) | Method for preparing analysis solution for inductively coupled plasma-atomic emission spectrometry (ICP-AES) and atomic absorption spectroscopy (AAS) by using lithium metaborate | |
| CN102928271A (en) | Sample treatment method for measuring niobium, tungsten and zirconium in steel | |
| CN104089957A (en) | Method for determining phosphorus pentoxide in phosphorite by molybdenum blue colorimetric method | |
| CN103543080B (en) | The assay method of tailings composition after potassium feldspar decomposition | |
| CN104111305A (en) | Novel method for determination of total iron of iron ore by potassium dichromate volumetric method | |
| CN103616473B (en) | The assay method of all iron content in steelmaking ingredient DRI | |
| CN104215634A (en) | Method for determining content of tin in tungsten concentrate | |
| CN103543141B (en) | The analytical approach of tin oxide electrode micro impurity element Fe and Cu | |
| CN106338505A (en) | Method for determination of rare earth content in red mud | |
| CN112129744B (en) | Chemical phase analysis method for lithium in ore | |
| CN100535637C (en) | Continuous detecting method for lead-cadmium in plastic sample | |
| CN104155267A (en) | Method for chemically analyzing content of boron nitride in nickel-based powder material | |
| CN104006993A (en) | Preparation method of sample for testing content of sulfur in fuel oil by ID-ICP-MS (isotope dilution inductively coupled plasma mass spectrometry) method | |
| CN106979946A (en) | The quick determination method of protein in a kind of milk |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120711 |