CN104569123A - Extraction separation-inductive coupling plasma mass-spectrometry for determining impurity elements in high-purity aluminum - Google Patents
Extraction separation-inductive coupling plasma mass-spectrometry for determining impurity elements in high-purity aluminum Download PDFInfo
- Publication number
- CN104569123A CN104569123A CN201310517052.1A CN201310517052A CN104569123A CN 104569123 A CN104569123 A CN 104569123A CN 201310517052 A CN201310517052 A CN 201310517052A CN 104569123 A CN104569123 A CN 104569123A
- Authority
- CN
- China
- Prior art keywords
- plasma mass
- add
- sample
- spectrometry
- purity aluminum
- 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
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses an extraction separation-inductive coupling plasma mass-spectrometry for determining impurity elements in high-purity aluminum. Aluminum is extracted and separated by adopting APDC-MIBK, and Co, Ni, Cu, Mo, Cd, Pb and Bi in the high-purity aluminum are determined by an inductive coupling plasma mass-spectrometry (ICP-MS) at the same time. Working parameters of an instrument, internal standard elements, separation and enrichment conditions and interferences on a sample base body are discussed in details so that optimal determination conditions of an experiment are determined. A result shows that the detection limit of the method is 0.011 microgram/liter-0.052 microgram/liter, the yield is 92.2%-103.0% and the relative standard deviation (RSD) is less than 2.3%. The method is accurate, rapid and simple and convenient, and is applied to the determination of the impurity elements in the high-purity aluminum, such as Co, Ni, Cu, Mo, Cd, Pb and Bi.
Description
Technical field
The invention belongs to casting technology field, be specifically related to a kind of extract and separate-inductively coupled plasma mass spectrometry of the impurity element measured in rafifinal.
Background technology
As starting material, high pure metal aluminium is widely used in the hi-tech industries such as computing machine, communication, light transmitting fiber, semiconductor material, and the contamination accurately understanding its impurity element is significant.Impurities analysis many employings ICP-AES (ICP-AES) in current Al and Alalloy, but due to the restriction by instrumental sensitivity, to the ultimate analysis of trace impurity in high pure metal, its accuracy and precision are all unsatisfactory.
Summary of the invention
In order to overcome the above-mentioned technical matters that prior art field exists, the object of the invention is to, provide a kind of extract and separate-inductively coupled plasma mass spectrometry of the impurity element measured in rafifinal, the method is easy and simple to handle, quick, accurate, reproducible.
Extract and separate-the inductively coupled plasma mass spectrometry of the impurity element in mensuration rafifinal provided by the invention, comprises the following steps:
(1) preparing standard solution: Co, Ni, Cu, Mo, Cd, Pb and Bi standard reserving solution (800 ~ 1000mgL
-1) Al standard reserving solution (20 ~ 50mgL
-1) adopt rafifinal preparation;
(2) Co, Ni, Cu, Mo, Cd, Pb and Bi mixed standard solution of obtained variable concentrations is progressively diluted by above-mentioned standard reserving solution;
(3) instrument is: Hewlett-Packard HP4500series300 plasma mass spectrometry, Milli-pore company of U.S. ultrapure water machine (Milli-Q), instrument parameter is: high-frequency emission power: 1200 ~ 1400W, sampling depth: 7 ~ 8mm, plasma flow speed: 12.0 ~ 15.0Lmin
-1, assisted gas flow velocity: 0.8 ~ 1.2Lmin
-1, flow rate of carrier gas: 1.0 ~ 1.2Lmin
-1, atomizer: Rabington type, atomization temperature: 3 DEG C, sample lifting capacity: 0.3 ~ 0.6mLmin
-1, sampling spiroid and intercepting cone: Ni, the measurement point residence time: 0133s, measuring point number/quality: 3, multiplicity: 3 times.
(4) take 1.0000g metallic aluminium sample in 100mL beaker, add the moistening sample of a small amount of ultrapure water, then in beaker, add 15mLHCl (when sample is not soluble, appropriate HNO can be added
3), low-temperature heat dissolved samples, dissolves completely, moves in separating funnel, after being adjusted to pH2.5 ~ 3.0 with HCl, add 5mLAPDC and 10mLMIBK, violent jolting 4min, after stratification, organic layer is moved in 100mL beaker, after heating water bath removing MIBK, add 1mL30%H
2o
2with the HNO of 1mL65%
3repeat to clear up 3 times, cooling is transferred in 50mL volumetric flask, is diluted with water to scale, measures 7 kinds of impurity contents, do blank assay simultaneously under optimization experiment condition by ICP-MS method.
Extract and separate-the inductively coupled plasma mass spectrometry of the impurity element in mensuration rafifinal provided by the invention, its beneficial effect is, detecting of this method is limited to 0.011 ~ 0.052 μ gL
-1, the recovery is 92.2% ~ 103.0%, and relative standard deviation (RSD) is less than 2.3%.Method is accurate, quick, easy, and be applied to the mensuration of the impurity element such as Co, Ni, Cu, Mo, Cd, Pb and Bi in rafifinal, analytical precision is 0.8% ~ 2.3%.This law is easy, quick, sensitive, accurate, for actual sample analysis.
Embodiment
Below in conjunction with an embodiment, the extract and separate-inductively coupled plasma mass spectrometry of the impurity element in mensuration rafifinal provided by the invention is described in detail.
Embodiment
Extract and separate-the inductively coupled plasma mass spectrometry of the impurity element in the mensuration rafifinal of the present embodiment, comprises the following steps:
(1) preparing standard solution: Co, Ni, Cu, Mo, Cd, Pb and Bi standard reserving solution (1000mgL
-1) Al standard reserving solution (50mgL
-1) adopt rafifinal preparation;
(2) Co, Ni, Cu, Mo, Cd, Pb and Bi mixed standard solution of obtained variable concentrations is progressively diluted by above-mentioned standard reserving solution;
(3) instrument is: Hewlett-Packard HP4500series300 plasma mass spectrometry, Milli-pore company of U.S. ultrapure water machine (Milli-Q), instrument parameter is: high-frequency emission power: 1350W, sampling depth: 7.8mm, plasma flow speed: 14.0Lmin
-1, assisted gas flow velocity: 1.0Lmin
-1, flow rate of carrier gas: 1.1Lmin
-1, atomizer: Rabington type, atomization temperature: 3 DEG C, sample lifting capacity: 0.4mLmin
-1, sampling spiroid and intercepting cone: Ni, the measurement point residence time: 0133s, measuring point number/quality: 3, multiplicity: 3 times.
(4) take 1.0000g metallic aluminium sample in 100mL beaker, add the moistening sample of a small amount of ultrapure water, then in beaker, add 15mLHCl (when sample is not soluble, appropriate HNO can be added
3), low-temperature heat dissolved samples, dissolves completely, moves in separating funnel, after being adjusted to pH2.5 ~ 3.0 with HCl, add 5mLAPDC and 10mLMIBK, violent jolting 4min, after stratification, organic layer is moved in 100mL beaker, after heating water bath removing MIBK, add 1mL30%H
2o
2with the HNO of 1mL65%
3repeat to clear up 3 times, cooling is transferred in 50mL volumetric flask, is diluted with water to scale, measures 7 kinds of impurity contents, do blank assay simultaneously under optimization experiment condition by ICP-MS method.
Claims (1)
1. measure extract and separate-inductively coupled plasma mass spectrometry of the impurity element in rafifinal, it is characterized in that:
(1) preparing standard solution: Co, Ni, Cu, Mo, Cd, Pb and Bi standard reserving solution (800 ~ 1000mgL
-1) Al standard reserving solution (20 ~ 50mgL
-1) adopt rafifinal preparation;
(2) Co, Ni, Cu, Mo, Cd, Pb and Bi mixed standard solution of obtained variable concentrations is progressively diluted by above-mentioned standard reserving solution;
(3) instrument is: Hewlett-Packard HP4500series300 plasma mass spectrometry, Milli-pore company of U.S. ultrapure water machine (Milli-Q), instrument parameter is: high-frequency emission power: 1200 ~ 1400W, sampling depth: 7 ~ 8mm, plasma flow speed: 12.0 ~ 15.0Lmin
-1, assisted gas flow velocity: 0.8 ~ 1.2Lmin
-1, flow rate of carrier gas: 1.0 ~ 1.2Lmin
-1, atomizer: Rabington type, atomization temperature: 3 DEG C, sample lifting capacity: 0.3 ~ 0.6mLmin
-1, sampling spiroid and intercepting cone: Ni, the measurement point residence time: 0133s, measuring point number/quality: 3, multiplicity: 3 times;
(4) take 1.0000g metallic aluminium sample in 100mL beaker, add the moistening sample of a small amount of ultrapure water, then in beaker, add 15mLHCl (when sample is not soluble, appropriate HNO can be added
3), low-temperature heat dissolved samples, dissolves completely, moves in separating funnel, after being adjusted to pH2.5 ~ 3.0 with HCl, add 5mLAPDC and 10mLMIBK, violent jolting 4min, after stratification, organic layer is moved in 100mL beaker, after heating water bath removing MIBK, add 1mL30%H
2o
2with the HNO of 1mL65%
3repeat to clear up 3 times, cooling is transferred in 50mL volumetric flask, is diluted with water to scale, under optimization experiment condition, measures 7 kinds of impurity contents by ICP-MS method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310517052.1A CN104569123A (en) | 2013-10-29 | 2013-10-29 | Extraction separation-inductive coupling plasma mass-spectrometry for determining impurity elements in high-purity aluminum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310517052.1A CN104569123A (en) | 2013-10-29 | 2013-10-29 | Extraction separation-inductive coupling plasma mass-spectrometry for determining impurity elements in high-purity aluminum |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104569123A true CN104569123A (en) | 2015-04-29 |
Family
ID=53085685
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310517052.1A Pending CN104569123A (en) | 2013-10-29 | 2013-10-29 | Extraction separation-inductive coupling plasma mass-spectrometry for determining impurity elements in high-purity aluminum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104569123A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105823821A (en) * | 2015-12-29 | 2016-08-03 | 中核北方核燃料元件有限公司 | Determination method for contents of impurity elements in thorium tetrafluoride powder |
| CN106525745A (en) * | 2015-09-09 | 2017-03-22 | 南京理工大学 | Method for analyzing and detecting trace metal ion impurities in dimethyl diallyl ammonium chloride monomers |
| CN108760454A (en) * | 2018-06-01 | 2018-11-06 | 广西壮族自治区海洋环境监测中心站 | A kind of preparation method of low-heavy metal content seawater |
| CN109991304A (en) * | 2017-12-29 | 2019-07-09 | 东莞东阳光科研发有限公司 | A method of measurement high-voltage electricity sub-light foil surface layer different-thickness lead content |
| CN111239199A (en) * | 2020-03-03 | 2020-06-05 | 宁波江丰电子材料股份有限公司 | Method for distinguishing high-purity aluminum from aluminum alloy |
| CN111398257A (en) * | 2020-04-15 | 2020-07-10 | 首钢京唐钢铁联合有限责任公司 | Method for measuring content of trace elements in silicon-aluminum alloy |
| CN113237871A (en) * | 2021-05-19 | 2021-08-10 | 宁波江丰电子材料股份有限公司 | Method for detecting AlSc alloy components |
| CN113791132A (en) * | 2021-09-03 | 2021-12-14 | 山东非金属材料研究所 | Isotope dilution determination method for hafnium in nickel-based superalloy |
-
2013
- 2013-10-29 CN CN201310517052.1A patent/CN104569123A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106525745A (en) * | 2015-09-09 | 2017-03-22 | 南京理工大学 | Method for analyzing and detecting trace metal ion impurities in dimethyl diallyl ammonium chloride monomers |
| CN106525745B (en) * | 2015-09-09 | 2019-10-18 | 南京理工大学 | The detection method of trace metal ion in dimethyldiallylammonchloride chloride monomer |
| CN105823821A (en) * | 2015-12-29 | 2016-08-03 | 中核北方核燃料元件有限公司 | Determination method for contents of impurity elements in thorium tetrafluoride powder |
| CN109991304A (en) * | 2017-12-29 | 2019-07-09 | 东莞东阳光科研发有限公司 | A method of measurement high-voltage electricity sub-light foil surface layer different-thickness lead content |
| CN108760454A (en) * | 2018-06-01 | 2018-11-06 | 广西壮族自治区海洋环境监测中心站 | A kind of preparation method of low-heavy metal content seawater |
| CN111239199A (en) * | 2020-03-03 | 2020-06-05 | 宁波江丰电子材料股份有限公司 | Method for distinguishing high-purity aluminum from aluminum alloy |
| CN111398257A (en) * | 2020-04-15 | 2020-07-10 | 首钢京唐钢铁联合有限责任公司 | Method for measuring content of trace elements in silicon-aluminum alloy |
| CN113237871A (en) * | 2021-05-19 | 2021-08-10 | 宁波江丰电子材料股份有限公司 | Method for detecting AlSc alloy components |
| CN113791132A (en) * | 2021-09-03 | 2021-12-14 | 山东非金属材料研究所 | Isotope dilution determination method for hafnium in nickel-based superalloy |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104569123A (en) | Extraction separation-inductive coupling plasma mass-spectrometry for determining impurity elements in high-purity aluminum | |
| CN105823772B (en) | The detection method of impurity element in a kind of measurement tungsten carbide | |
| CN102735678B (en) | Method for determining chromium content and aluminum content in nickel-chromium-aluminum coated diatomite | |
| CN103604800B (en) | A kind of analytical approach measuring titanium vanadium tungsten manganese silicon in K25 refractory Cr-base alloy | |
| CN102854179B (en) | Method for analyzing and detecting cadmium impurity element in tungsten or tungsten compound | |
| CN103115916B (en) | A kind of method measuring content of niobium in ferrocolumbium | |
| CN104713870A (en) | Method for determining trace elements in Ti-AL-V-base titanium alloy | |
| CN105548331A (en) | Method for simultaneous determination of multiple trace elements in iron ore | |
| CN104568916A (en) | Inductive coupling plasma atomic emission spectrometry for determining elements in nuclear-grade zirconium alloy | |
| CN104949961B (en) | The ICP AES detection methods of Ge element content in Pb-free solder material | |
| CN105136777A (en) | Method for measuring trace element content in aluminium alloy by ICP method | |
| CN104020157A (en) | Method for measuring elemental niobium content of titanium-niobium alloy | |
| CN103674932A (en) | Method for determining content of Cu, Mn and Sn in Cu-Mn-Sn alloyed powder through ICP (inductively coupled plasma) | |
| CN103344629B (en) | The ICP-AES measurement method of lead content in water | |
| CN103149196A (en) | Method for determining content of silicon, phosphor and aluminium in ferrocolumbium through inductive coupling plasma emission spectroscopy | |
| CN104316590A (en) | Inductively coupled plasma mass spectrometry method for simultaneous determination of chromium, nickel, arsenic and lead in hot melt adhesive for cigarette | |
| CN102928271A (en) | Sample treatment method for measuring niobium, tungsten and zirconium in steel | |
| CN104132933B (en) | A kind of measure the method for free aluminum content in Tercod | |
| CN105388142A (en) | Method for detecting silicon content in titanium sponge, titanium and titanium alloy | |
| CN103837381A (en) | Method for detecting lithium ion content of anodization tank liquid | |
| CN107632011A (en) | The assay method of impurity content in a kind of high purity bismuth | |
| CN103954610A (en) | Method for measuring arsenic in high-chromium high-nickel steel | |
| CN105911049A (en) | Method for determining calcium oxide in rare earth concentrate | |
| CN105021692A (en) | Method for simultaneously determining multiple inorganic elements in cigarette liquid of electronic cigarette | |
| CN102914513A (en) | Analysis detection method of iron element in vanadium carbide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150429 |