CN103940807B - Method for determining content of silicon in potassium fluotantalate - Google Patents
Method for determining content of silicon in potassium fluotantalate Download PDFInfo
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Abstract
The invention relates to a method for determining the content of silicon in potassium fluotantalate. The method adopts an ICP (Inductively Coupled Plasma) spectrometer and a hydrofluoric acid resistant sampling system; purified electronic-grade nitric acid and hydrofluoric acid are adopted, and the heights of a center pipe of an ICP spectrometer quarter bend and an inner pipe are adjusted to enable a distance between the bottom of a flame and an outer quartz pipe of the ICP spectrometer quarter bend to be increased by about 50% compared with a standard distance; solution prepared by a surfactant (Triton-X100) is used as washing liquid for washing the sampling system of the ICP spectrometer before each time of determination. The method overcomes the technological barrier existing in the industry, and realize the determination of the content of silicon in potassium fluotantalate through ICP spectrum analysis through comprehensive technical schemes of introducing the hydrofluoric acid (HF) resistant sampling system, adjusting the positions of the center pipe of the ICP spectrometer quarter bend and the inner pipe, setting special parameters, developing the washing liquid, preparing a standard sample, purifying and selecting reagents and the like, and the determination limit can reach 0.0005%; therefore, the method is initiative in domestic peers.
Description
Technical field:
The present invention relates to potassium floutaramite impurity content assay method technical field, refer in particular to the assay method of silicone content in a kind of potassium floutaramite.
Background technology:
Potassium floutaramite is the primary raw material producing tantalum powder, and its purity height directly affects the quality of tantalum powder, and therefore the requirement of enterprise to potassium floutaramite purity is more and more higher.Containing tens kinds of impurity elements such as Al, B, Ca, Cr, Mn, Cu, Fe, Mg, Mo, Nb, Ni, Ti, Si, W in potassium floutaramite, for other impurity except Si element, have at present and adopt ICP spectrophotometer method (inductively coupled plasma emission spectrography) to measure, Determination Limit can reach 0.0005%, can meet enterprise requirements.
And for Si element, because the quartz outer tube of quarter bend in ICP spectrometer, interior pipe contain a large amount of Si element, therefore background concentration is too high, and sample is easily polluted, and reagent blank is too high, said method therefore still cannot be adopted at present to measure Si constituent content in potassium floutaramite.Silicon in current domestic each producer chemical method or arclight spectrometry fluorine analysis potassium tantalate, silicon blank is high, poor stability, and the change of analytic process hollow white value causes greatly analyzes sample without reappearance.
Summary of the invention:
The object of the invention is to overcome the deficiencies in the prior art part, the assay method of silicone content in a kind of ICP spectroscopic assay potassium floutaramite is provided.
The technical scheme that the present invention realizes the employing of its object is: the assay method of silicone content in a kind of potassium floutaramite, and this assay method adopts ICP spectrometer, and adopt HF acid resistant device; Select the electronic grade nitric acid after purification and hydrofluorite; The height of adjustment ICP spectrometer quarter bend pipe core, interior pipe makes the distance of flame base and the quartz outer tube of ICP spectrometer quarter bend than gauged distance increase about 50%; And the solution selecting surfactant Triton-X100 to prepare between measuring each mensuration and next time is as washing lotion, cleans the sampling system of ICP spectrometer.
In this assay method, the running parameter of ICP spectrometer is: plasma generator power 1200W, cooling gas flow 14L/min, carrier gas flux 0.3L/min, nebulizer flow 0.69L/min, atomizing pressure 2.88bars, analysis of line wavelength 251.611nm.
These assay method concrete steps are:
Step one, regent purification and ICP spectrometer regulate: electronic grade nitric acid and hydrofluorite are purified further; By described running parameter setting ICP spectrometer, and regulate the height of ICP spectrometer quarter bend pipe core, interior pipe, make the distance of flame base and the quartz outer tube of ICP spectrometer quarter bend than gauged distance increase about 50%;
Step 2, Specification Curve of Increasing and blank assay: take the potassium floutaramite standard model that 4 groups of 0.2000g silicone contents are 0.0005% respectively, add the electronic grade nitric acid after 1.5mL purification respectively, electronic-stage hydrofluoric acid after 0.5mL purifies and 8mL pure water, heating for dissolving, be cooled to normal temperature, then wherein three components is selected not add the silicon standard solution 0.1mL of 10 μ g/mL, the silicon standard solution 1.0mL of 10 μ g/mL, the silicon standard solution 1.0mL of 100 μ g/mL, be settled to 20mL, successively 4 groups of standard model solution are introduced ICP spectrometer from HF acid resistant device to measure, record the standard model intensity level of mensuration respectively, and with the standard model intensity level measured for ordinate, with the content of Si in test solution for horizontal ordinate drawing standard curve, (Si in test solution comprises the Si in standard model, the Si in added silicon standard solution and the Si element (i.e. blank value) in system),
In company with doing blank test, namely when not adding sample, with ICP spectrophotometer blank solution, obtaining blank intensity level, on typical curve, finding corresponding Si content with this blank intensity level, being blank value;
Often group is cleaned with the sampling system of solution to ICP spectrometer that surfactant Triton-X100 prepares between measuring;
Step 3: clean with the sampling system of solution to ICP spectrometer that surfactant Triton-X100 prepares after blank test completes;
Step 4: take sample 0.2000g to be determined, add the electronic-stage hydrofluoric acid after the electronic grade nitric acid after 1.5mL purification, 0.5mL purification and 8mL pure water successively, 20mL is settled to after heating for dissolving, finally sample liquids is introduced from HF acid resistant device and measure, obtain corresponding sample solution intensity level, on typical curve, corresponding sample solution (containing blank) middle Si content is found with sample solution intensity level, deduct blank value, be Si content in sample (μ g/g), and be convertible into the percentage composition of silicon in sample.
The concentration of the solution that described surfactant Triton-X100 prepares is 4%.
The inventive method overcomes technology barriers consistent in the industry, by comprehensive technological schemes such as the development of the setting of the introducing of resistance to HF acid sampling system, ICP spectrometer quarter bend pipe core, the adjustment of interior pipe position, special parameter, washing lotion, the preparation of standard model, the purification of reagent and selections, realize with the silicon content in ICP spectral analysis potassium floutaramite, and Determination Limit reaches 0.0005%, method has reappearance and mensuration relative standard deviation is little, belongs to pioneering at home in colleague.
Embodiment:
Below in conjunction with specific embodiment, the present invention is further described.
Of the present invention is the assay method of silicone content in a kind of potassium floutaramite, and this assay method adopts ICP spectrometer, and adopt HF acid resistant device; Select the electronic grade nitric acid after purification and hydrofluorite; The pipe core of adjustment ICP spectrometer quarter bend, the height of interior pipe make flame base increase about 50% with the distance of the quartz outer tube of ICP spectrometer quarter bend than gauged distance (i.e. the standard conditions of instrument); And the solution selecting surfactant Triton-X100 to prepare between measuring each mensuration and next time is as washing lotion, cleans the sampling system of ICP spectrometer.
The further purification of nitric acid and hydrofluorite is conducive to the reduction of detectability;
Under a large amount of fluorine exists, by the adjustment pipe core of quarter bend, the height of interior pipe, make the distance of flame base and the quartz outer tube of quarter bend than standard value increase about 50%, more effectively reduce the quartz outer tube of hydrofluorite to quarter bend, the corrosion of interior pipe, thus effectively reduce the blank value of system silicon;
By selecting surfactant Triton-X100, prepare suitable concentration and do washing lotion, preferably concentration is 4%, after guaranteeing that each sample analysis completes, before system blank value returns to sample determination rapidly, makes analysis result have reappearance.
The present invention is by comprehensive technological schemes such as the development of the setting of the introducing of resistance to HF acid sampling system, ICP spectrometer quarter bend pipe core, the adjustment of interior pipe position, special parameter, washing lotion, the preparation of standard model, the purification of reagent and selections, realize with the silicon content in ICP spectral analysis potassium floutaramite, and Determination Limit reaches 0.0005%, method has reappearance and mensuration relative standard deviation is little.
Specifically, in this assay method, the running parameter of ICP spectrometer is: plasma generator power 1200W, cooling gas flow 14L/min, carrier gas flux 0.3L/min, nebulizer flow 0.69L/min, atomizing pressure 2.88bars, analysis of line wavelength 251.611nm.
These assay method concrete steps are:
Step one, regent purification and ICP spectrometer regulate: select electronic grade nitric acid and hydrofluorite to purify further; By described running parameter setting ICP spectrometer, and regulate the height of the pipe core of ICP spectrometer quarter bend, interior pipe, make the distance of flame base and the quartz outer tube of ICP spectrometer quarter bend than gauged distance increase about 50%;
Step 2, Specification Curve of Increasing and blank assay: take the potassium floutaramite standard model that 4 groups of 0.2000g silicone contents are 0.0005% respectively, add the electronic grade nitric acid after 1.5mL purification respectively, electronic-stage hydrofluoric acid after 0.5mL purifies and 8mL pure water, heating for dissolving, be cooled to normal temperature, then wherein three components is selected not add the silicon standard solution 0.1mL of 10 μ g/mL, the silicon standard solution 1.0mL of 10 μ g/mL, the silicon standard solution 1.0mL of 100 μ g/mL, be settled to 20mL, successively 4 groups of standard models are introduced ICP spectrometer from HF acid resistant device to measure, record the standard model intensity level of mensuration respectively, and with the standard model intensity level measured for ordinate, with the content of Si in test solution (unit μ g/g) for horizontal ordinate drawing standard curve, (Si in test solution comprises the Si in standard model, the Si in added silicon standard solution and the Si element (i.e. blank value) in system),
Typical curve test figure form is as follows:
In company with doing blank test, namely when not adding sample, with ICP spectrophotometer blank solution, obtaining blank intensity level, on typical curve, finding corresponding Si content with this blank intensity level, being blank value;
Often group is cleaned with the sampling system of solution to ICP spectrometer that the concentration that surfactant Triton-X100 prepares is 4% between measuring;
Step 3: clean with the sampling system of solution to ICP spectrometer that surfactant Triton-X100 prepares after blank test completes;
Step 4: take sample 0.2000g to be determined, add the electronic-stage hydrofluoric acid after the electronic grade nitric acid after 1.5mL purification, 0.5mL purification and 8mL pure water successively, 20mL is settled to after heating for dissolving, finally sample liquids is introduced from HF acid resistant device and measure, obtain corresponding sample solution intensity level, on typical curve, corresponding sample solution (containing blank) middle Si content is found with sample solution intensity level, deduct blank value, be Si content in sample (μ g/g), and be convertible into the percentage composition of silicon in sample.
Test result comparative analysis:
One, the analysis result adopting the inventive method and ordinary chemical method to measure silicone content in potassium floutaramite sample contrasts as following table:
| Sample lot number | ICP spectroscopic methodology (%) | Chemical method (%) |
| 2013-1-1 | 0.0005 | ＜0.0015 |
| 2013-5-1 | 0.001 | ＜0.0015 |
| 2013-6-1 | 0.0015 | 0.0017 |
As can be seen from the above table, 5ppm can be reached by the silicon Monitoring lower-cut value in ICP spectral analysis potassium floutaramite.
Two, mark-on recovery test result is as following table:
As seen from the above table, recovery of standard addition is between 90%-110%.
Three, 11 method reappearance tests and RSD (relative standard deviation) result are as following table:
As can be seen here, to have the relative standard deviation of reappearance and mensuration little for the inventive method.
Claims (4)
1. the assay method of silicone content in potassium floutaramite, is characterized in that: this assay method adopts ICP spectrometer, and adopt HF acid resistant device; Select the electronic grade nitric acid after purification and hydrofluorite; The pipe core of adjustment ICP spectrometer quarter bend, the height of interior pipe make the distance of flame base and the quartz outer tube of ICP spectrometer quarter bend than gauged distance increase about 50%; And the solution selecting surfactant Triton-X100 to prepare between measuring each mensuration and next time is as washing lotion, cleans the sampling system of ICP spectrometer.
2. the assay method of silicone content in potassium floutaramite according to claim 1, it is characterized in that: in this assay method, the running parameter of ICP spectrometer is: plasma generator power 1200W, cooling gas flow 14L/min, carrier gas flux 0.3L/min, nebulizer flow 0.69L/min, atomizing pressure 2.88bars, analysis of line wavelength 251.611nm.
3. the assay method of silicone content in potassium floutaramite according to claim 2, is characterized in that: its concrete steps are:
Step one, regent purification and ICP spectrometer regulate: to purify out electronic grade nitric acid through method of purification, to purify out electronic-stage hydrofluoric acid through method of purification; By described running parameter setting ICP spectrometer, and regulate the height of the pipe core of ICP spectrometer quarter bend, interior pipe, make the distance of flame base and the quartz outer tube of ICP spectrometer quarter bend than gauged distance increase about 50%;
Step 2, Specification Curve of Increasing and blank assay: take the potassium floutaramite standard model that 4 groups of 0.2000g silicone contents are 0.0005% respectively, add the electronic grade nitric acid after 1.5mL purification respectively, electronic-stage hydrofluoric acid after 0.5mL purifies and 8mL pure water, heating for dissolving, be cooled to normal temperature, then wherein three components is selected not add the silicon standard solution 0.1mL of 10 μ g/mL, the silicon standard solution 1.0mL of 10 μ g/mL, the silicon standard solution 1.0mL of 100 μ g/mL, be settled to 20mL, successively 4 groups of standard models are introduced ICP spectrometer from HF acid resistant device to measure, record the standard model intensity level of mensuration respectively, and with the standard model intensity level measured for ordinate, with the content μ g/g of Si in test solution for horizontal ordinate drawing standard curve,
In company with doing blank test, namely when not adding sample, with ICP spectrophotometer blank solution, obtaining blank intensity level, on typical curve, finding corresponding Si content with this blank intensity level, being blank value;
Often group is cleaned with the sampling system of solution to ICP spectrometer that surfactant Triton-X100 prepares between measuring;
Step 3: clean with the sampling system of solution to ICP spectrometer that surfactant Triton-X100 prepares after blank test completes;
Step 4: take sample 0.2000g to be determined, add the electronic-stage hydrofluoric acid after the electronic grade nitric acid after 1.5mL purification, 0.5mL purification and 8mL pure water successively, 20mL is settled to after heating for dissolving, finally sample liquids is introduced from HF acid resistant device and measure, obtain corresponding sample solution intensity level, on typical curve, find corresponding Si content with sample solution intensity level, deduct blank value, be Si content μ g/g in sample, and be convertible into the percentage composition of silicon in sample.
4. the assay method of silicone content in potassium floutaramite according to claim 3, is characterized in that: the concentration of the solution that described surfactant Triton-X100 prepares is 4%.
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Citations (4)
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| JP2012032171A (en) * | 2010-07-28 | 2012-02-16 | Sharp Corp | Icp analysis method |
| CN102565026A (en) * | 2010-12-15 | 2012-07-11 | 鞍钢股份有限公司 | Method for determination of silicon content in ferro-aluminum manganese |
| CN103149196A (en) * | 2013-02-25 | 2013-06-12 | 内蒙古包钢钢联股份有限公司 | Method for determining content of silicon, phosphor and aluminium in ferrocolumbium through inductive coupling plasma emission spectroscopy |
| CN103278493A (en) * | 2013-05-17 | 2013-09-04 | 株洲硬质合金集团有限公司 | Method for analyzing and detecting thirty impurity elements in tantalum and tantalum-based compound |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012032171A (en) * | 2010-07-28 | 2012-02-16 | Sharp Corp | Icp analysis method |
| CN102565026A (en) * | 2010-12-15 | 2012-07-11 | 鞍钢股份有限公司 | Method for determination of silicon content in ferro-aluminum manganese |
| CN103149196A (en) * | 2013-02-25 | 2013-06-12 | 内蒙古包钢钢联股份有限公司 | Method for determining content of silicon, phosphor and aluminium in ferrocolumbium through inductive coupling plasma emission spectroscopy |
| CN103278493A (en) * | 2013-05-17 | 2013-09-04 | 株洲硬质合金集团有限公司 | Method for analyzing and detecting thirty impurity elements in tantalum and tantalum-based compound |
Non-Patent Citations (2)
| Title |
|---|
| Determination of Silicon in Tantalum and its Compounds Using ICP-OES;G.ANIL等;《Chemical Papers》;20041231;第58卷(第3期);195-199 * |
| 氟钽酸钾中杂质的直接光谱测定;华锋;《分析试验室》;19901231;第9卷(第1期);67 * |
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Address after: 510900 Conghua Province, Guangzhou City, the town of red grass Patentee after: Guangdong Guangsheng photoelectric rare metal new material Co Ltd Address before: 510900 Conghua Province, Guangzhou City, the town of red grass Patentee before: CONGHUA TANTALUM & NIOBIUM SMELTERY |
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