CN102692407A - Method for analysis of metal impurity ions of organic solvent - Google Patents
Method for analysis of metal impurity ions of organic solvent Download PDFInfo
- Publication number
- CN102692407A CN102692407A CN2011100725661A CN201110072566A CN102692407A CN 102692407 A CN102692407 A CN 102692407A CN 2011100725661 A CN2011100725661 A CN 2011100725661A CN 201110072566 A CN201110072566 A CN 201110072566A CN 102692407 A CN102692407 A CN 102692407A
- Authority
- CN
- China
- Prior art keywords
- organic solvent
- icp
- impurity ions
- solution
- metal impurity
- 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
Images
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
The invention provides a method for analysis of metal impurity ions of an organic solvent. The method for analysis of metal impurity ions of an organic solvent realizes quantitative analysis of the content of metal impurity ions of an organic solvent by an inductively coupled plasma (ICP) method and comprises the following steps of 1, diluting a standard solution of a solvent needing to be detected by an organic system, 2, starting an instrument, correcting intensity values, setting an observation position according to a maximum intensity value, and carrying out optical initialization, 3, detecting the standard solution, and establishing a standard curve, wherein a correction coefficient is greater than 0.999, and 4, detecting an unknown solution. The method for analysis of metal impurity ions of an organic solvent can realize accurate measurement of the content of metal impurity ions of an organic solvent, reduce experimental errors caused by organic degradation and improve the accuracy of ICP detection.
Description
Technical field
The present invention relates to the analytical approach of metallic impurity ion in a kind of organic solvent, belong to technical field of analytical chemistry.
Background technology
In chemical industry, organic solvent is as a kind of comparatively general solvent, and its metals content impurity does not receive publicity always.Aspect test, AAS and ICP (inductively coupled plasma atomic emission) are generally adopted in the test of metallic impurity ion.Method of testing, but with regard to some transition metal ion, like Fe, it is with its content poor effect in organic solvent of AAS test; ICP has its special advantages at test metallic impurity ion concentration.It is many that ICP not only detects species of metal ion, and detectability is superior to AAS, and precision also is higher than the AAS method of testing.Traditional I CP test system is on the high side with aqueous systems, and organic system is the aviation kerosene system; But actual organic system be mostly to be not dissolved in water body or with aqueous systems can not complete miscibility; There are shortcomings such as carbon distribution is serious in inconvenient operation, the experimentation, experimental expenses is higher in the aviation kerosene system; Therefore, ICP has many restrictions in the Test Application of organic solvent foreign metal ion; Tradition utilizes the degraded of organic system can solve the Test Application of ICP metallic impurity ion in organic system to a certain extent; But the dust of part metal ion when the impurity metal ion in the novel solvent of introducing during degraded (like strong acid), burning; Reduce along with flowing of air-flow, or the burning dust is attached to vessel surface by force and reduces actual content.In essence, this indirect method is unfavorable for accurately testing the metal ion content in the organic system.Degraded has increased experimental error, and the analysis for trace in the organic system and trace metal impurities is quite disadvantageous especially.
Summary of the invention
In order to solve above-mentioned technical matters, the object of the present invention is to provide the analytical approach of metallic impurity ion in a kind of organic solvent.
In order to reach above-mentioned purpose, the present invention uses a kind of method of measuring some organic solvent metallic impurity with ICP.
The object of the invention is realized through following technical scheme:
The analytical approach of metallic impurity in a kind of organic solvent, said analytical approach are to use the content of metallic impurity ion in the ICP quantitative analysis organic solvent, comprise the steps,
Step 1: the standard solution that dilutes solvent to be measured with organic system;
Step 2: open instrument, the correction intensity value is provided with observation position according to the strongest intensity level, carries out the optics initialization;
Step 3: measurement standard solution, set up typical curve, correction coefficient reaches more than 0.999;
Step 4: measure unknown solution, obtain a result;
It is to adopt identical organic solvent with test system that ICP mark liquid is equipped with solvent;
The ICP that uses is Po Jinaiermo 7000DV;
The carbon remover device that ICP uses: flow accuracy removes carbon deposit device as the 0.1ml/min high purity oxygen;
The working gas that ICP uses: high-purity argon gas, high purity oxygen gas.
Further, organic system is meant high-purity organic solvent ethanol in the said step 1, acetonitrile, tetrahydrofuran, benzene, in the toluene any one, standard solution is HNO
3, water or aviation kerosene standard.
Further, proofread and correct intensity level in the said step 2 and carry out the correction of intensity level with the Mn solution of 1ppm.
Further, unknown solution is used with the standard solution system and is adopted identical organic solvent diluting in the step 4, and the metal concentration to be measured after it is diluted is within standard curve range.
Analytical approach provided by the invention can accurately be tested the metal ion content in the organic solvent, has reduced the experimental error that the organic degradation process is brought, and has increased the accuracy of ICP test.
Description of drawings
Fig. 1: through the figure as a result of ICP tested K ion concentration of the present invention.
Fig. 2: through the figure as a result of ICP test Fe ion concentration of the present invention.
Fig. 3: through the figure as a result of ICP test Li ion concentration of the present invention.
Fig. 4: through the figure as a result of ICP test Ca ion concentration of the present invention.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is elaborated.
Embodiment 1
Test foreign metal ion concentration in the dimethyl carbonate (DMC) with ICP, test M
N+=(K, Na, Ca, Fe, Pb etc.) (n=N).Use ethanol dilution ICP-26 element to mix mark liquid, weighing method (wt/wt) the accurately normal concentration of dilute concentration is: K=1ppm, M
N+=0.1ppm, M
N+=(Na, Ca, Fe, Pb etc.) (n=N); K=5ppm, M
N+=0.5ppm, M
N+=(Na, Ca, Fe, Pb etc.) (n=N); K=10ppm, M
N+=1ppm, M
N+=(Na, Ca, Fe, Pb etc.) (n=N).Use ethanol dilution dimethyl carbonate (DMC) to 20 times (wt/wt).
Using the ICP playpipe instead is 0.8mm, adopts relevant ICP accessory and gas condition of work that the present invention selected for use.Start is treated to calibrate observation bit with 1ppm Mn titer behind the instrument stabilizer, adjusts liquid apart from observation position according to the result.Observation position is adjusted the back and in water, ICP is carried out the optics initialization, tests after waiting to accomplish.Blank high straight alcohol, blank testing reagent, standard reagent and the sample successively of adopting.Fig. 1, Fig. 2 are respectively ICP tested K, Fe figure as a result, and solid-line curve is represented standard reagent, and dashed curve is represented test result.Containing K by the calculating derived sample is 35.1ppb, and it is 12.1ppb that sample contains Fe.
Embodiment 2
With Li ion concentration in certain solution of ICP test, use ethanol dilution ICP-Li element mark liquid, weighing method (wt/wt) accurately dilution standard liquid makes that to n times the concentration of mark liquid is (Li
+=0.1～1ppm); With ethanol dilution solution to n doubly, make Li in the solution
+Concentration is (Li
+=0.1～1ppm).
Using the ICP playpipe instead is 0.8mm, adopts relevant ICP accessory and gas condition of work that the present invention selected for use.Start is treated to calibrate observation bit with the 1ppmMn titer behind the instrument stabilizer, adjusts liquid apart from observation position according to the result.Observation position is adjusted the back and in water, ICP is carried out the optics initialization, tests after waiting to accomplish.Blank high straight alcohol, blank testing reagent, standard reagent and the sample successively of adopting.Fig. 3 tests Li ion concentration figure as a result for ICP, and solid-line curve is represented standard reagent, and dashed curve is represented test result.Li content by calculating derived sample is 1383ppm.
Embodiment 3
With Ca ion concentration in certain reagent of ICP test, test M
N+=Ca (n=N).Use ethanol dilution Ca element mark liquid, weighing method (wt/wt) is the normal concentration of dilute concentration accurately: M
N+=0.01ppm, M
N+=Ca, (n=N); M
N+=0.05ppm, M
N+=Ca (n=N); M
N+=0.1ppm, M
N+=Ca (n=N).Use this solvent to 20 of ethanol dilution times (wt/wt).
Using the ICP playpipe instead is 0.8mm, adopts relevant ICP accessory and gas condition of work that the present invention selected for use.Start is treated to calibrate observation bit with the Mn titer of 1ppm behind the instrument stabilizer, adjusts liquid apart from observation position according to the result.Observation position is adjusted the back and in water, ICP is carried out the optics initialization, tests after waiting to accomplish.Blank high straight alcohol, blank testing reagent, standard reagent and the sample successively of adopting.Fig. 4 tests Ca ion concentration figure as a result for ICP, and solid-line curve is represented standard reagent, and dashed curve is represented test result.Containing Ca by the calculating derived sample is 133.2ppb.
The present invention still has multiple concrete embodiment, and all employings are equal to replacement or equivalent transformation and all technical schemes of forming all drop within the scope of requirement protection of the present invention.
Claims (4)
1. the analytical approach of metallic impurity in the organic solvent is characterized in that: said analytical approach comprises the steps for using the content of metallic impurity ion in the ICP quantitative analysis organic solvent,
Step 1: the standard solution that dilutes solvent to be measured with organic system;
Step 2: open instrument, the correction intensity value is provided with observation position according to the strongest intensity level, carries out the optics initialization;
Step 3: measurement standard solution, set up typical curve, correction coefficient reaches more than 0.999;
Step 4: measure unknown solution, obtain a result;
It is to adopt identical organic solvent with test system that ICP mark liquid is equipped with solvent;
The ICP that uses is Po Jinaiermo 7000DV;
The carbon remover device that ICP uses: flow accuracy removes carbon deposit device as the 0.1ml/min high purity oxygen;
The working gas that ICP uses: high-purity argon gas, high purity oxygen gas.
2. the analytical approach of metallic impurity in a kind of organic solvent as claimed in claim 1, it is characterized in that: organic system is meant high-purity organic solvent ethanol in the said step 1, acetonitrile, tetrahydrofuran, benzene, in the toluene any one, standard solution is HNO
3, water or aviation kerosene standard.
3. like the analytical approach of metallic impurity in a kind of organic solvent of claim 1, it is characterized in that: proofread and correct intensity level in the said step 2 and carry out the correction of intensity level with the Mn solution of 1ppm.
4. like the analytical approach of metallic impurity in a kind of organic solvent of claim 1; It is characterized in that: unknown solution is used with the standard solution system and is adopted identical organic solvent diluting in the step 4, and the metal concentration to be measured after it is diluted is within standard curve range.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100725661A CN102692407A (en) | 2011-03-24 | 2011-03-24 | Method for analysis of metal impurity ions of organic solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100725661A CN102692407A (en) | 2011-03-24 | 2011-03-24 | Method for analysis of metal impurity ions of organic solvent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102692407A true CN102692407A (en) | 2012-09-26 |
Family
ID=46858004
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011100725661A Pending CN102692407A (en) | 2011-03-24 | 2011-03-24 | Method for analysis of metal impurity ions of organic solvent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102692407A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108614028A (en) * | 2018-04-09 | 2018-10-02 | 杉杉新材料（衢州）有限公司 | The analysis method of metal ion in a kind of lithium ion battery preparation process |
| CN110658183A (en) * | 2018-06-28 | 2020-01-07 | 张家港市国泰华荣化工新材料有限公司 | Method for measuring electrolyte content in nickel-hydrogen electrolyte |
| CN112147130A (en) * | 2020-09-29 | 2020-12-29 | 浙江巨化技术中心有限公司 | Method for determining content of metal elements in polyvinylidene fluoride resin |
| CN112858263A (en) * | 2021-01-15 | 2021-05-28 | 中国神华煤制油化工有限公司 | Method for measuring content of metal elements in organic solution |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003329584A (en) * | 2002-05-08 | 2003-11-19 | Santoku Corp | Method for analyzing metal contained in organic phase sample |
| CN101644677A (en) * | 2009-08-28 | 2010-02-10 | 中国北车集团大同电力机车有限责任公司 | Method for detecting element content in alloy or ore by utilizing ICP emission spectrometer |
| CN101726482A (en) * | 2009-12-24 | 2010-06-09 | 江苏天瑞仪器股份有限公司 | Method for detecting content of elements in oil with inductively coupled plasma (ICP) spectrometer |
-
2011
- 2011-03-24 CN CN2011100725661A patent/CN102692407A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003329584A (en) * | 2002-05-08 | 2003-11-19 | Santoku Corp | Method for analyzing metal contained in organic phase sample |
| CN101644677A (en) * | 2009-08-28 | 2010-02-10 | 中国北车集团大同电力机车有限责任公司 | Method for detecting element content in alloy or ore by utilizing ICP emission spectrometer |
| CN101726482A (en) * | 2009-12-24 | 2010-06-09 | 江苏天瑞仪器股份有限公司 | Method for detecting content of elements in oil with inductively coupled plasma (ICP) spectrometer |
Non-Patent Citations (3)
| Title |
|---|
| 李绍松等: "《ICP-AES有机进样测定润滑油中的S元素》", 《润滑油》, vol. 21, no. 5, 31 October 2006 (2006-10-31), pages 62 - 64 * |
| 陈迎霞: "《使用过得润滑油中添加剂、磨损和污染物元素的测定-ICP/AES有机溶剂稀释法》", 《光谱仪器与分析》, no. 1, 31 December 1999 (1999-12-31), pages 5 - 8 * |
| 黄宗平: "《ICP-AES法测定润滑油中微量元素的评述》", 《现代科学仪器》, 31 December 2005 (2005-12-31), pages 61 - 63 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108614028A (en) * | 2018-04-09 | 2018-10-02 | 杉杉新材料（衢州）有限公司 | The analysis method of metal ion in a kind of lithium ion battery preparation process |
| CN110658183A (en) * | 2018-06-28 | 2020-01-07 | 张家港市国泰华荣化工新材料有限公司 | Method for measuring electrolyte content in nickel-hydrogen electrolyte |
| CN112147130A (en) * | 2020-09-29 | 2020-12-29 | 浙江巨化技术中心有限公司 | Method for determining content of metal elements in polyvinylidene fluoride resin |
| CN112858263A (en) * | 2021-01-15 | 2021-05-28 | 中国神华煤制油化工有限公司 | Method for measuring content of metal elements in organic solution |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US8796032B2 (en) | Method for analyzing and detecting calcium element in ore | |
| CN103196880B (en) | Method for determining content of arsenic in iron ore by using hydride generation-atomic fluorescence spectroscopy | |
| CN102692407A (en) | Method for analysis of metal impurity ions of organic solvent | |
| Yang et al. | On-line determination of silver in sea-water and marine sediment by inductively coupled plasma mass spectrometry | |
| CN103674932A (en) | Method for determining content of Cu, Mn and Sn in Cu-Mn-Sn alloyed powder through ICP (inductively coupled plasma) | |
| CN103543133A (en) | Method for determining content of bismuth in iron ores by hydride generation-atomic fluorescence spectrometry method | |
| Kuznetsova et al. | How feasible is direct determination of rare earth elements in seawater by ICP-MS? | |
| CN111289499B (en) | Method for simultaneously detecting multiple trace elements in iron-containing waste acid | |
| CN106198495B (en) | The test method of lithium cobalt molar ratio in cobalt acid lithium | |
| CN102721676A (en) | Method for stably measuring arsenic and mercury in water by atomic fluorescence spectrometry | |
| CN101639443A (en) | Method for rapidly and accurately determining sulphur element content in fluorite | |
| US20090229995A1 (en) | Analysis of fluoride at low concentrations in acidic processing solutions | |
| CN103543134A (en) | Method for determining lead content in iron ore through hydride generation-atomic fluorescence spectrometry | |
| CN107367505B (en) | ICP-AES method for rapidly and accurately determining content of niobium element in heat-resistant steel | |
| CN102706848A (en) | Pretreatment method for sewage sample during measurement of arsenic and mercury in water by fluorescent spectrometry | |
| CN111595835A (en) | Method for measuring cerium content in high-silicon stainless steel | |
| CN104655610B (en) | The analysis method and assay method of vanadyl oxalate oxalate ion concentration | |
| Phukphatthanachai et al. | SI-traceable quantification of sulphur in copper metal and its alloys by ICP-IDMS | |
| CN103344628B (en) | The ICP-AES of Determination of Arsenic In Iron And Steel measures | |
| Mariet et al. | Relevance of NH4F in acid digestion before ICP-MS analysis | |
| CN112683611B (en) | Digestion solution and method for determining element content in refined aluminum ingot for remelting | |
| CN104713834A (en) | Quantitative method of atomic spectrometer | |
| CN105758844B (en) | The measuring method of trace silicon in a kind of cobaltosic oxide | |
| CN102072886B (en) | Method for measuring content of titanium in industrial silicon and buffer releasing agent thereof | |
| Anderlini et al. | Characterization of a 12 M KOH zincate fuel for green energy backup systems using flow injection coupled to inductively coupled plasma optical emission spectrometry |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C05 | Deemed withdrawal (patent law before 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120926 |