CN105372230A - Method for measuring tin in titanium tetrachloride through ICP-AES - Google Patents
Method for measuring tin in titanium tetrachloride through ICP-AES Download PDFInfo
- Publication number
- CN105372230A CN105372230A CN201510638121.3A CN201510638121A CN105372230A CN 105372230 A CN105372230 A CN 105372230A CN 201510638121 A CN201510638121 A CN 201510638121A CN 105372230 A CN105372230 A CN 105372230A
- Authority
- CN
- China
- Prior art keywords
- tin
- solution
- icp
- aes
- titanium tetrachloride
- 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)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to a tin detection method, in particular to a method for measuring tin in titanium tetrachloride through an ICP-AES. According to the method, an inductive coupling plasma atomic emission spectrometer is mainly utilized for detecting and recycling a sample solution under the set instrument working condition and analysis wavelength, and the sample solution is calibrated simultaneously. The method is simple and fast in operation, feasible and high in recycling rate, accuracy degree and precision degree, interference of titanium on tin detection is eliminated, and measurement of tin in titanium tetrachloride is fully satisfied.
Description
Technical field
The present invention relates to the detection method of tin, be specifically related to a kind of method that ICP-AES measures tin in titanium tetrachloride.
Background technology
Along with the continuous expansion of titanium sponge industry and titanium white industry, the demand of titanium tetrachloride is surged, and the kind of producing titanium tetrachloride raw material also gets more and more, and therefore, causes impurity component in titanium tetrachloride to become increasingly complex.
Tin chloride or oxychloride are one of impurity in titanium tetrachloride, after usual production, Theil indices detection can be carried out to titanium tetrachloride, to judge whether titanium tetrachloride meets standard, and then ensure the quality of titanium sponge, in titanium tetrachloride, the method for tin mostly is traditional chemical analysis, such as, and compleximetry, its step is simple, easy to operate, but degree of accuracy is lower, easy contaminated environment; Spectrophotometric method, its accuracy in detection is high, but process is complicated, and hand sequence is loaded down with trivial details, takes time and effort, and easily causes sample to stain, and then contaminated environment; Nuclear magnetic resonance method, its degree of accuracy is high, easy to operate, but equipment requirement is high, energy consumption is large, testing cost is high, in addition, conventional at present detection method, the interference of titanium, aluminium, vanadium, iron, silicon metallic element is comparatively large on testing result impact, and especially titanium elements interference is maximum.
Therefore, set up a kind of easy to operate, pollution-free, detection method that accuracy is high, be conducive to the production of titanium tetrachloride, and then be conducive to the development of titanium industry.
Summary of the invention
The object of the present invention is to provide the method for tin in a kind of easy to operate, pollution-free, cost is low, accuracy is high detection titanium tetrachloride.
Be achieved especially by following scheme:
ICP-AES measures a method for tin in titanium tetrachloride, comprises the following steps:
(1) condition of work of ICP-AES, as shown in table 1:
Table 1
| Radio-frequency generator power | 1250-1350w |
| Plasma gas flow rate | 10-20L/min |
| Auxiliary argon flow | 0.15-0.25L/min |
| Nebulizer flow | 0.75-0.85L/min |
| Observed altitude | 15mm |
| Sample size | 1.5mL/min |
| Flush time | 40s |
| Analysis spectral line | 189.928nm |
(2) preparation of tin standard reserving solution: the tin standard solution and the ultrapure water that by concentration are 1000 μ g/mL, compound concentration is 40 μ gmL
-1tin standard reserving solution;
(3) preparation of sample solution: be the TiCl of 1.73g/mL by HCl solution, density
4, ultrapure water mixes, preparation sample solution, wherein, density is the TiCl of 1.73g/mL
4the consumption of solution accounts for 1/100 of solution total amount;
(4) tin standard reserving solution is placed in inductively coupled plasma atomic emission spectrometer, under the condition of work of table 1, standardization is carried out to inductively coupled plasma atomic emission spectrometer, sample solution is placed in inductively coupled plasma atomic emission spectrometer and measures;
(5) remaining sample solution is reclaimed, contain with vinyon bucket is airtight, after refining, chlorination, distillation, enter titanium sponge production technique;
(6) result analytic method:
According to step (4) measurement result, adopt using standard samples recovery, calculate the recovery of tin element.
The volumetric concentration of described HCl solution is 40-60%, and further preferably, the volumetric concentration of HCl solution is 50%.
In described sample solution, the volumetric concentration of HCl is 5-15%, and further preferably, in sample solution, the volumetric concentration of HCl is 10%.
Described density is the TiCl of 1.73g/mL
4the equal < 0.1% of the massfraction of aluminium, vanadium, iron, silicon in solution.
Beneficial effect of the present invention
ICP-AES is adopted to measure tin in titanium tetrachloride, the lower limit that detects of its Theil indices is 0.01 μ g/mL, illustrate: precision of the present invention is good and accuracy is high, its recovery is 98.67%-100.50%, illustrate that feasibility of the present invention is high, and the way of recycling of combination seal, recycling, make test not cause environmental pollution; By detecting the tin standard working solution of sample solution, titanium based sols, obtain the linear relationship coefficient of tin element more than 0.99, illustrate that the disturbing factor of the present invention program is little, especially titanium almost disturbs without detection tin, and then contributes to improving accuracy; The present invention, by strictly controlling solution acidity, effectively prevents the hydrolysis of titanium tetrachloride, controls reaction rate again, and then avoid the impact of flue gas on measurement result; So this method is fast simple to operate, method is feasible, and the recovery, accuracy and degree of accuracy are high, meets the mensuration of tin in titanium tetrachloride completely.
Accompanying drawing explanation
Fig. 1 represents the tin element linearly dependent coefficient figure of embodiment 1.
Fig. 2 represents the tin element linearly dependent coefficient figure of embodiment 2.
Embodiment
Below in conjunction with concrete embodiment, further restriction is done to technical scheme of the present invention, but claimed scope is not only confined to done description.
Embodiment 1
ICP-AES measures a method for tin in titanium tetrachloride, comprises the following steps:
Step 1: instrument prepares
Start Optima7000DV inductively coupled plasma atom generation spectrometer, after carrying out initialization, by following setting parameter condition of work:
Radio-frequency generator power: 1300w
Plasma gas flow rate: 10L/min
Auxiliary argon flow: 0.2L/min
Nebulizer flow: 0.8L/min
Observed altitude: 15mm
Sample size: 1.5mL/min
Flush time: 40s
Analysis spectral line: 189.928nm
Step 2: solution preparation
Step 2.1: tin standard reserving solution is prepared
Pipette 10mL concentration be the tin standard solution of 1000 μ g/mL in 250mL volumetric flask, ultrapure water constant volume, shakes up;
Step 2.2: sample solution is prepared
Get respectively 10mL, 20mL, 30mL volumetric concentration be the hydrochloric acid of 50% in 100mL volumetric flask, often organize and slowly add the TiCl that 1.00mL density is 1.73g/mL
4solution, covers rapidly capacity bottle stopper, and shake to smokelessly, after cooling, ultrapure water constant volume, shakes up, and counts sample 1, sample 2, sample 3 successively;
Step 2.3: titanium based sols is prepared
Get respectively 20mL volumetric concentration be the hydrochloric acid of 50% in 6 100mL volumetric flasks, often organize and slowly add 1.00mLw
snbe the TiCl of 0.0001%
4solution, covers rapidly capacity bottle stopper, shakes to after smokeless, counts titanium based sols 1, titanium base 2, titanium base 3, titanium base 4, titanium base 5, titanium base 6 successively;
Step 3: spectral measurement and calculating
Step 3.1
Under the condition of work of the inductively coupled plasma atomic emission spectrometer described in step 1, step 2.1 tin Standard Stock solutions is adopted to carry out standardization to instrument, drawing line, sample 1, sample 2, sample 3 are placed in inductively coupled plasma atomic emission spectrometer respectively and measure, the tin standard reserving solution that Theil indices is 2 μ g, 4 μ g, 6 μ g is added respectively in sample 3,1,2, measure, adopt using standard samples recovery, its result is as shown in table 2:
Table 2
Step 3.2
Under the condition of work of the inductively coupled plasma atomic emission spectrometer described in step 1, adopt and step 2.3 titanium based sols 1, titanium based sols 2, titanium based sols 3, titanium based sols 4, titanium based sols 5, titanium based sols 6 are added step 2.1 tin standard reserving solution preparation working solution respectively and carry out standardization to instrument, in its working solution, tin mass concentration is as shown in table 3, these 6 groups of working solutions are placed in inductively coupled plasma atomic emission spectrometer respectively measure, its tin element linearly dependent coefficient as shown in Figure 1;
Table 3
Step 3.3
Under the condition of work of the inductively coupled plasma atomic emission spectrometer described in step 1, after adopting the working solution of step 3.2 to carry out standardization to instrument, same sample is made into 10 parts of identical sample solutions according to the preparation method of sample 2, namely sample solution 1, sample solution 2, sample solution 3, sample solution 4, sample solution 5, sample solution 6, sample solution 7, sample solution 8, sample solution 9, sample solution 10 are placed in inductively coupled plasma atomic emission spectrometer respectively and measure, and result is as shown in table 4:
Table 4
By Fig. 1: tin element linearly dependent coefficient is 0.999973, close to 1, illustrates that linear relationship is better; Associative list 3 again, knows that the actual measurement mean value of Sn is 3.89 μ gg
-1, standard deviation is 0.18, calculates further and knows: the lower limit that detects of tin is 0.01 μ g/ml, and relative standard deviation (RSD) is about 4.63%, to sum up illustrates, the present invention can detect the solution compared with low tin content, and it is high to detect degree of accuracy; Last associative list 2 is known, the inventive method has feasibility, and sample recovery rate is high, reaches 98.67%-100.5%.
Step 4: solution reclaims
Contain airtight for remaining for step 3 sample solution vinyon bucket, after refining, chlorination, distillation, enter titanium sponge production technique.
Embodiment 2
ICP-AES measures a method for tin in titanium tetrachloride, comprises the following steps:
Step 1: instrument prepares
Start Optima7000DV inductively coupled plasma atom generation spectrometer, after carrying out initialization, by following setting parameter condition of work:
Radio-frequency generator power: 1350w
Plasma gas flow rate: 20L/min
Auxiliary argon flow: 0.25L/min
Nebulizer flow: 0.85L/min
Observed altitude: 15mm
Sample size: 1.5mL/min
Flush time: 40s
Analysis spectral line: 189.928nm
Step 2: solution preparation
Step 2.1: tin standard reserving solution is prepared
Pipette 10.00mL concentration be the tin standard solution of 1000 μ g/mL in 250mL volumetric flask, ultrapure water constant volume, shakes up;
Step 2.2: sample solution is prepared
Get respectively 10mL, 20mL, 30mL volumetric concentration be the hydrochloric acid of 50% in 100mL volumetric flask, often organize that slowly to add 1.00mL density be 1.73gmL
-1tiCl
4solution, covers rapidly capacity bottle stopper, and shake to smokelessly, after cooling, ultrapure water constant volume, shakes up, and counts sample 1, sample 2, sample 3 successively;
Step 2.3: titanium based sols is prepared
Take 0.436g titanium 6 parts, wherein, in titanium, the mass percent of tin is 0.0001%, be placed in 150mL polytetrafluoroethylene beaker respectively, add the HCl solution that 5mL volumetric concentration is 50%, 2mL volumetric concentration is the hydrofluoric acid solution of 50%, be 30 DEG C by temperature and be heated to test portion dissolving completely, proceed in 6 100mL volumetric flasks after cooling, add the HCl that 15mL volumetric concentration is 50% more respectively, shake up, count titanium based sols 1, titanium based sols 2, titanium based sols 3, titanium based sols 4, titanium based sols 5, titanium based sols 6 successively;
Step 3: spectral measurement and calculating
Step 3.1
Under the condition of work of the inductively coupled plasma atomic emission spectrometer described in step 1, step 2.1 tin Standard Stock solutions is adopted to carry out standardization to instrument, drawing line, sample 1, sample 2, sample 3 are placed in inductively coupled plasma atomic emission spectrometer respectively and measure, the tin standard reserving solution that Theil indices is 2 μ g, 4 μ g, 6 μ g is added respectively in sample 3,1,2, measure, adopt using standard samples recovery, its result is as shown in table 5:
Table 5
Step 3.2
Under the condition of work of the inductively coupled plasma atomic emission spectrometer described in step 1, adopt and step 2.3 titanium based sols 1, titanium based sols 2, titanium based sols 3, titanium based sols 4, titanium based sols 5, titanium based sols 6 are added step 2.1 tin standard reserving solution preparation working solution respectively and carry out standardization to instrument, in its working solution, tin mass concentration is as shown in table 6, these 6 groups of working solutions are placed in inductively coupled plasma atomic emission spectrometer respectively measure, its tin element linearly dependent coefficient as shown in Figure 1;
Table 6
Step 3.3
Under the condition of work of the inductively coupled plasma atomic emission spectrometer described in step 1, after adopting the working solution of step 3.2 to carry out standardization to instrument, same sample is made into 10 parts of identical sample solutions according to sample 1 preparation method, namely sample solution 1, sample solution 2, sample solution 3, sample solution 4, sample solution 5, sample solution 6, sample solution 7, sample solution 8, sample solution 9, sample solution 10 are placed in inductively coupled plasma atomic emission spectrometer respectively and measure, and result is as shown in table 7:
Table 7
By Fig. 2: tin element linearly dependent coefficient is 0.999968, close to 1, illustrates that linear relationship is better; Associative list 7 again, knows that the actual measurement mean value of Sn is 3.96 μ gg
-1, standard deviation is 0.18, calculates further and knows: the lower limit that detects of tin is 0.01 μ g/mL, and relative standard deviation (RSD) is about 4.46%, to sum up illustrates, the present invention can detect the solution compared with low tin content, and it is high to detect degree of accuracy; Last associative list 5 is known, the inventive method has feasibility, and sample recovery rate is high, reaches 99.33%-100.25%.
Step 4: solution reclaims
Contain airtight for remaining for step 3 sample solution vinyon bucket, after refining, chlorination, distillation, enter titanium sponge production technique.
Claims (6)
1. measure a method for tin in titanium tetrachloride with ICP-AES, it is characterized in that, comprise the following steps:
(1) condition of work of ICP-AES, as shown in table 1:
Table 1
(2) preparation of tin standard reserving solution: the tin standard solution and the ultrapure water that by concentration are 1000 μ g/mL, compound concentration is 40 μ gmL
-1tin standard reserving solution;
(3) preparation of sample solution: be the TiCl of 1.73g/mL by HCl solution, density
4solution, ultrapure water mix, and preparation sample solution, wherein, density is the TiCl of 1.73g/mL
4the consumption of solution accounts for 1/100 of solution total amount;
(4) tin standard reserving solution is placed in inductively coupled plasma atomic emission spectrometer, under the condition of work of table 1, standardization is carried out to inductively coupled plasma atomic emission spectrometer, sample solution is placed in inductively coupled plasma atomic emission spectrometer and measures;
(5) remaining sample solution is reclaimed, contain with vinyon bucket is airtight, after refining, chlorination, distillation, enter titanium sponge production technique;
(6) result analytic method:
According to step (4) measurement result, adopt using standard samples recovery, calculate the recovery of tin element.
2. measure the method for tin in titanium tetrachloride as claimed in claim 1 with ICP-AES, it is characterized in that, the volumetric concentration of described HCl solution is 40-60%.
3. measure the method for tin in titanium tetrachloride as claimed in claim 1 or 2 with ICP-AES, it is characterized in that, the volumetric concentration of described HCl solution is 50%.
4. measure the method for tin in titanium tetrachloride as claimed in claim 1 with ICP-AES, it is characterized in that, in described sample solution, the volumetric concentration of HCl is 5-15%.
5. the method measuring tin in titanium tetrachloride with ICP-AES as described in claim 1 or 4, it is characterized in that, in described sample solution, the volumetric concentration of HCl is 10%.
6. measure the method for tin in titanium tetrachloride as claimed in claim 1 with ICP-AES, it is characterized in that, described density is the TiCl of 1.73g/mL
4the equal < 0.1% of the massfraction of aluminium, vanadium, iron, silicon in solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510638121.3A CN105372230A (en) | 2015-09-30 | 2015-09-30 | Method for measuring tin in titanium tetrachloride through ICP-AES |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510638121.3A CN105372230A (en) | 2015-09-30 | 2015-09-30 | Method for measuring tin in titanium tetrachloride through ICP-AES |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105372230A true CN105372230A (en) | 2016-03-02 |
Family
ID=55374621
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510638121.3A Pending CN105372230A (en) | 2015-09-30 | 2015-09-30 | Method for measuring tin in titanium tetrachloride through ICP-AES |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105372230A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1870377A1 (en) * | 2006-06-20 | 2007-12-26 | E.I.Du pont de nemours and company | Method for quantification of analytes in a titanium, tin or silicon tetrachloride sample |
| CN101349646A (en) * | 2007-07-19 | 2009-01-21 | 北京有色金属与稀土应用研究所 | Method for measuring impurity in high pure gold by plasma atomic emission spectrometer |
| CN103424399A (en) * | 2013-07-19 | 2013-12-04 | 中国船舶重工集团公司第七二五研究所 | Analytic method for simultaneously determining percentage content of nine impurity elements in titanium sponge |
-
2015
- 2015-09-30 CN CN201510638121.3A patent/CN105372230A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1870377A1 (en) * | 2006-06-20 | 2007-12-26 | E.I.Du pont de nemours and company | Method for quantification of analytes in a titanium, tin or silicon tetrachloride sample |
| CN101349646A (en) * | 2007-07-19 | 2009-01-21 | 北京有色金属与稀土应用研究所 | Method for measuring impurity in high pure gold by plasma atomic emission spectrometer |
| CN103424399A (en) * | 2013-07-19 | 2013-12-04 | 中国船舶重工集团公司第七二五研究所 | Analytic method for simultaneously determining percentage content of nine impurity elements in titanium sponge |
Non-Patent Citations (3)
| Title |
|---|
| 成勇: "ICP-AES法直接测定70钛铁中V，Sn", 《冶金分析》 * |
| 成勇: "电感耦合等离子体原子发射光谱法测定四氯化钛液体中杂质元素", 《理化检验（化学分册）》 * |
| 谢绍金 等: "ICP-AES法测定钛基复合材料中的Sn，Zr，Nb，Ta，Nd和Fe的研究", 《航空材料学报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101315316B (en) | Digestion method and detection method of titanium-rich material | |
| CN103604800B (en) | A kind of analytical approach measuring titanium vanadium tungsten manganese silicon in K25 refractory Cr-base alloy | |
| CN102866046B (en) | Method for determining contents of heavy metals in sample | |
| CN104713870A (en) | Method for determining trace elements in Ti-AL-V-base titanium alloy | |
| CN102590184A (en) | Method for determining high-content potassium and sodium in iron and dust-containing mud | |
| CN103234954A (en) | Method for measuring content of metal element cadmium Cd by ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) method | |
| CN106153654A (en) | Method for analyzing ludwigite by X-ray fluorescent powder tabletting method | |
| CN102590108B (en) | Micro-wave digestion rapidly and efficiently detects the method for silica sand medium trace element content | |
| CN107525799A (en) | The method of chromium content in inductively coupled plasma mass spectrometry measure indium | |
| CN106383108A (en) | Method for simultaneously detecting multiple components of cement sample by ICP-AES (inductively coupled plasma-atomic emission spectrometry) process and application thereof | |
| CN103698176B (en) | The assay method of Holo-Al content in a kind of iron and steel and alloy | |
| CN104897623A (en) | Method for determining aluminium oxide content of aluminous castable | |
| CN106990098A (en) | The method of each element content in simultaneous determination aluminium electrolyte | |
| CN105372230A (en) | Method for measuring tin in titanium tetrachloride through ICP-AES | |
| CN111239240B (en) | Method for determining harmful elements in iron ore | |
| CN104330389A (en) | Method for detecting content of various components in stannic oxide electrode block | |
| CN110095419A (en) | The detection method of lead, cadmium in automotive material | |
| CN102914513A (en) | Analysis detection method of iron element in vanadium carbide | |
| CN109632769A (en) | Rutile type TiO in titanium ore2Method (2) | |
| CN107462567B (en) | A method of lithium content in measurement zirconium and zircaloy | |
| CN105758844B (en) | The measuring method of trace silicon in a kind of cobaltosic oxide | |
| CN104048951B (en) | Method for measuring contents of silicon, calcium and aluminum in additives and co-solvents of permanent magnetic ferrites through ICP (Inductively Coupled Plasma) emission spectroscopy | |
| CN105954262A (en) | {0><}0{>ICP-AES method for measuring sulfur content of lead sulfate in waste storage battery | |
| CN103344628A (en) | ICP-AES (inductively coupled plasma-atomic emission spectrometer) measurement method for content of arsenic in steel | |
| CN107389778A (en) | Niobium, vanadium, the assay method of titanium elements content in nitro-alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160302 |
|
| RJ01 | Rejection of invention patent application after publication |