CN110455598A - The sample treatment of impurity in a kind of detection stannic oxide - Google Patents
The sample treatment of impurity in a kind of detection stannic oxide Download PDFInfo
- Publication number
- CN110455598A CN110455598A CN201910820513.XA CN201910820513A CN110455598A CN 110455598 A CN110455598 A CN 110455598A CN 201910820513 A CN201910820513 A CN 201910820513A CN 110455598 A CN110455598 A CN 110455598A
- Authority
- CN
- China
- Prior art keywords
- sample
- stannic oxide
- solution
- impurity
- potassium hydroxide
- 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
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
Abstract
The present invention relates to a kind of sample treatments of impurity in detection stannic oxide, it is characterised in that: (1) drying to constant weight for sample；(2) stannic oxide sample and potassium hydroxide quality ratio 1:3,2/3 potassium hydroxide amount is weighed respectively is laid on silver crucible, 3 parts of stannic oxide samples are weighed to spread, 3 part of 1/3 potassium hydroxide amount is weighed to be placed on sample, silver crucible is placed at firn-jet head, and heating makes sample melted, cooling, with ultrapure water by transfer of melt to 250 mL beakers, it is shifted again with 10mL concentrated hydrochloric acid, heating beaker dissolution；A blank test solution is done in the same way；(3) beaker, cooling are removed, 100 mL volumetric flasks is transferred to respectively, mixes；(4) 1 group of sample solution and blank solution constant volume are taken, respectively as prepare liquid and blank solution.The invention has the advantages that can quickly carry out sample treatment to the stannic oxide of different process production, efficient analysis goes out impurity content；Easy to operate, safety, result are accurate, will not block instrument pipeline.
Description
Technical field
The invention belongs to glass substrate detection technique fields, are related to a kind of sample treatment side for detecting impurity in stannic oxide
Method.
Background technique
In glass industry production, stannic oxide is critically important one of raw material, stannic oxide impurity content number
It will have a direct impact on the quality of glass substrate, so reinforcing the detection and analysis to stannic oxide impurity component content, to glass substrate
Quality it is most important.Stannic oxide fusing point is high, any acid solution is not readily dissolved in, so in the detection of impurity component at sample
Extremely difficult, the production technology difference of stannic oxide is managed, the dissolution analysis of stannic oxide is also influenced in many big degree.
After the detection of impurity content uses chloroazotic acid or excellent pure grade high chloro acid dissolution mostly in stannic oxide in the prior art,
It recycles filter paper to be filtered for multiple times, takes supernatant using ICP checked for impurities ingredient, however such method utilizes chloroazotic acid (a variety of strong acid
Mixing), excellent pure grade perchloric acid (strong acid), risk is bigger, it is difficult to ensure that solution is clarified through being filtered for multiple times, is easy stifled
Instrument sample channel is filled in, equipment damage is caused.
Summary of the invention
The purpose of the present invention is to solve sample treatment in the detection of existing stannic oxide difficult (a variety of strong acid mixing, danger
Dangerous big and need to be filtered for multiple times, instrument sample feeding pipe easily blocked, equipment damage is caused), impurity component measurement is inaccurate in stannic oxide
The problem of, provide a kind of sample treatment for detecting impurity in stannic oxide.
To achieve the goals above, The technical solution adopted by the invention is as follows:
The sample treatment of impurity in a kind of detection stannic oxide, including existing plasma emission spectrum detecting step, it is special
Sign is: the processing of stannic oxide sample before plasma emission spectrum detects；
Specifically includes the following steps:
(1) sample stannic oxide is put into clean glass weighing bottle, 105 DEG C ~ 115 DEG C drying to constant weight, it is subsequently placed at dry
It is cooling stand-by in dry device；
(2) it is no more than ± 0.0002 by stannic oxide sample sample weighting amount and excellent pure grade potassium hydroxide sample weighting amount ratio 1:3(deviation
G), it weighs 2/3 potassium hydroxide amount respectively to tile three clean, dry silver crucible bottoms, then after accurately weighing 3 parts of drying
Stannic oxide sample is separately added into above-mentioned silver crucible, and the potassium hydroxide amount for finally accurately weighing 3 part of 1/3 weight again is placed on sample
Silver crucible is placed at firn-jet head by top, is heated to sample all meltings (uniform fusant), is stopped heating, be cooled to room
Stannic oxide alkali fusion object will be transferred to respectively in three 250 mL beakers in silver crucible with ultrapure water, then used respectively by temperature
10mL concentrated hydrochloric acid (excellent pure grade, concentration 36.0-38.0%) rinses silver crucible and washing lotion is transferred in corresponding three beakers, with
Beaker is dissolved by heating afterwards；A blank test solution is done in the same way；
(3) beaker is removed, is cooled to room temperature, is transferred in 100 mL volumetric flasks respectively, is slowly shaken volumetric flask, make in volumetric flask
Solution is uniformly mixed；
(4) 1 group of sample solution and blank solution is taken in step (3) to be settled to graticule, and using this as prepare liquid and blank
Solution.
Further, the partial size of the stannic oxide sample to be measured is less than 100 μm.
Because sodium hydroxide is by heat of solution, it is affected by temperature larger, easily solidification, so taking sample and excellent pure grade potassium hydroxide
Mixed dissolution；Again because when potassium hydroxide sample weighting amount increases, easily in thermal histories, spilling is boiled, therefore the method for the present invention is adopted
Take sample sample weighting amount and excellent pure grade potassium hydroxide sample weighting amount optimum sample weighting amount ratio 1:3(sample weighting amount deviation be no more than ±
0.0002g).
Advantages of the present invention: this method is directed to the stannic oxide of different process production, can very easily carry out at sample
Reason, and then quickly analyze the impurity content of stannic oxide；Acid (chloroazotic acid) the processing filtration method processing sample more now used, process
It is easy to operate, as a result accurately, and meanwhile it is also comparatively safe, pipeline will not be blocked because of particle remaining in filtrate.
Specific embodiment
The sample treatment of impurity in a kind of detection stannic oxide, specific steps are as follows:
Embodiment 1
1, with ICP-OES method, instrument parameter is set
(1) host power supply is opened, 0.5h or more is preheated；
(2) circulating water device is opened, confirms 20 DEG C of set temperature, confirms 0.31 MPa -0.55 MPa of output pressure；Connect argon
Gas, pressure are controlled in 0.7 MPa -0.8 MPa；Air compressor machine is opened, confirms 0.55 MPa -0.825 MPa of output pressure；It opens
Ventilator cowling；
(3) it opens computer and enters ICP operating system, whether normal, new folder is then established, according to measurement if looking first at instrument
Need to impose a condition: plasma gas 12L/min assists gas 0.23/min-0.4L/min, atomization gas 0.65L/min-0.75L/
min；
(4) plasma flame is lighted, optics initialization is carried out, until numerical value is in allowed band (± 50) (if exceeding model
Value is enclosed, then carries out axial and orientation alignment observation bit respectively with the Mn standard solution of 1ppm)；
2, the preparation of stannic oxide solution
(1) by stannic oxide to be measured, (raw material of standard needed for meeting TFT-LCD base plate glass production technology, partial size are not more than
100 μm) sample be put into advance with ultrapure water clean drying glass weighing bottle (50 mm × 30mm) in, at 105 DEG C ~ 110 DEG C
Baking 1h is placed in drier cooling stand-by in baking oven；
(2) 3 part of 2.0000 g potassium hydroxide solid is accurately weighed, is respectively put into three clean, dry silver crucibles, then accurately
The stannic oxide sample after 3 parts of 1.0000g(deviations g) are dried no more than ± 0.0002 is weighed, above-mentioned silver crucible is separately added into
In, then 3 parts of 1.0000g potassium hydroxide solids are weighed, it is laid on the sample in silver crucible；Silver crucible is placed at firn-jet head,
Sample all meltings (well-proportioned fusant) are heated to, heating is stopped, into silver crucible first using a small amount of multiple after cooling
Ultrapure water is added, is stirred evenly with glass bar, stannic oxide alkali fusion object is transferred in 250mL beaker, then respectively with 10 mL
The a small amount of multiple flushing silver crucible of concentrated hydrochloric acid (excellent pure grade, concentration 36.0-38.0%), and washing lotion is transferred to corresponding three burnings
In cup, finally beaker (fill stannic oxide alkali and melt precipitation liquid) is transferred on electric furnace, is dissolved by heating；One is done in the same way
Blank test solution；
(3) beaker is removed, is cooled to room temperature, is transferred in 100 mL volumetric flasks respectively, is slowly shaken volumetric flask, make in volumetric flask
Solution is uniformly mixed；
(4) wantonly 1 group of sample solution and blank solution is taken in step (3) to be settled to graticule, and using this as prepare liquid and sky
White solution.
3, impurity content in stannic oxide is surveyed
(1) selection scanning wavelength 180nm-800nm carries out qualitative scanning to the sample to be tested solution of above-mentioned steps (4), according to fixed
Property the impurity element components and semi-quantitative results (referring to table 1) that scan, formulate mixed standard solution preparation table (referring to table 2),
And set the conditions (referring to table 3) such as impurity element detection spectral line；
The qualitative scanning result of table 1
2 mixed standard solution preparation table of table
The detection line wavelength of each impurity element of table 3
(2) standard addition method is used, reference table 2 pipettes standard solution respectively and fills stannic oxide lysate in other 2
In 100mL volumetric flask, ultrapure water constant volume is used respectively, is shaken up, stand to be measured:
(3) by first blank testing solution, then survey prepare liquid, finally detect the titer of 2 groups of high-concentration and low-concentrations of configuration, establish to
The standard curve of micrometer secondary element；
(4) after measuring, first extinguish torch flame, close argon gas valve, turn off power supply.
(5) data processing, according to the standard curve of microelement to be measured, corresponding microelement intensity is corresponding in prepare liquid
Value is the concentration of each microelement of impurity in stannic oxide, and each microelement is calculated according to method (referring to formula 1)
Content (referring to table 4).
Formula illustrates: the percentage composition of element to be measured in W- sample；
C- determines the concentration of element to be measured in the sample solution come, unit ug/mL；
C0- determines the concentration of element to be measured in the blank solution come, unit ug/mL；
V- determines solution product, Unit/mL；
M- sample weighting amount, unit g.
The percentage composition of each impurity element of table 4
This experimental method, since stannic oxide purity is relatively high, impurity element is microelement or trace element, so only adding
Enter the element standard liquid for needing to detect, reduces the high tin element interference of content；For generally existing spectral line interference problem, we
Method can separately test influential element according to constituent content, illustrate that the detection method accuracy is high；By to same sample
Continuous 10 parallel analysis obtain the relative standard deviation (referring to table 5) of each element, can illustrate this method test precision
It is high.
Comparative example 1
Using the sample treatment of embodiment 1, the difference is that being examined using calibration curve method using plasma emission spectrum
The content that instrument detects all impurity elements in the solution to be measured is surveyed, standard liquid series preparation is shown in Table 6；To sample into
After ten parallel analysis of row, averaging of income test result and standard deviation are shown in Table 5.
Table 6
Comparative example 2
Stannic oxide sample is handled using perchloric acid, the specific steps are as follows:
(1) by stannic oxide to be measured, (raw material of standard needed for meeting TFT-LCD base plate glass production technology, partial size are not more than
100 μm) sample be put into advance with ultrapure water clean drying glass weighing bottle (50 mm × 30mm) in, at 105 DEG C ~ 110 DEG C
Baking 1h is placed in drier cooling stand-by in baking oven；
(2) 3 part of 1.0000 g(deviation is accurately weighed no more than the stannic oxide sample after ± 0.0002g) drying, is separately added into
In 250mL beaker, then 15mL perchloric acid (excellent pure grade, concentration 70.0-72.0%) is separately added into three beakers, will finally burn
Cup (filling stannic oxide sample and perchloric acid reagent) is transferred on electric furnace, is dissolved by heating；Blank examination is done in the same way
Liquid；
(3) then repeated filtration processing, takes filtrate to use standard addition method again, utilizes plasma emission spectrum detector test institute
The content of all impurity elements in solution to be measured is stated, standard liquid series preparation is identical as embodiment allocation list, is shown in Table
2；After carrying out ten parallel analysis to sample, averaging of income test result and standard deviation are shown in Table 5.
5 each element relative standard deviation of table
Impurity content in stannic oxide is detected using sample treatment of the present invention, easy to operate, precision
High, high-efficient, credible result can meet the detection demand of impurity element in stannic oxide.
Claims (3)
1. the sample treatment of impurity in a kind of detection stannic oxide, including existing plasma emission spectrum detecting step,
It is characterized in that: the processing of stannic oxide sample before plasma emission spectrum detects；
Specifically includes the following steps:
(1) sample stannic oxide is put into clean glass weighing bottle, 105 DEG C ~ 115 DEG C drying to constant weight, it is subsequently placed at dry
It is cooling stand-by in dry device；
(2) by stannic oxide sample sample weighting amount and excellent pure grade potassium hydroxide sample weighting amount ratio 1:3,2/3 hydroxide is weighed respectively
Three clean, dry silver crucible bottoms of potassium amount tiling, then the stannic oxide sample accurately weighed after 3 parts of drying are separately added into
It states in silver crucible, the potassium hydroxide amount for finally accurately weighing 3 part of 1/3 weight again is placed on sample top, and silver crucible is placed in flame
Head place, be heated to sample all melt, stop heat, be cooled to room temperature, with ultrapure water by silver crucible by stannic oxide alkali fusion
Melt object to be transferred to respectively in three 250 mL beakers, then rinses silver crucible simultaneously with the concentrated hydrochloric acid of 10mL concentration 36.0-38.0% respectively
Washing lotion is transferred in corresponding three beakers, is then dissolved by heating beaker；A blank test solution is done in the same way；
(3) beaker is removed, is cooled to room temperature, is transferred in 100 mL volumetric flasks respectively, is slowly shaken volumetric flask, make in volumetric flask
Solution is uniformly mixed；
(4) 1 group of sample solution and blank solution is taken in step (3) to be settled to graticule, and using this as prepare liquid and blank
Solution.
2. a kind of sample treatment for detecting impurity in stannic oxide according to claim 1, it is characterised in that: the title
It measures deviation and is no more than ± 0.0002g.
3. according to claim 1 it is a kind of detection stannic oxide in impurity sample treatment, it is characterised in that: it is described to
The partial size of stannic oxide sample is surveyed less than 100 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910820513.XA CN110455598A (en) | 2019-09-02 | 2019-09-02 | The sample treatment of impurity in a kind of detection stannic oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910820513.XA CN110455598A (en) | 2019-09-02 | 2019-09-02 | The sample treatment of impurity in a kind of detection stannic oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110455598A true CN110455598A (en) | 2019-11-15 |
Family
ID=68490313
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910820513.XA Pending CN110455598A (en) | 2019-09-02 | 2019-09-02 | The sample treatment of impurity in a kind of detection stannic oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110455598A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102998300A (en) * | 2012-11-19 | 2013-03-27 | 中国船舶重工集团公司第七二五研究所 | Analysis method for impurity elements in tin-oxide-containing nanopowder |
| CN103543141A (en) * | 2013-09-25 | 2014-01-29 | 中国科学院上海光学精密机械研究所 | Analytical method of trace impurity elements Fe and Cu in tin oxide electrode |
| CN103868911A (en) * | 2014-04-03 | 2014-06-18 | 河南科技学院 | Method for dissolving aluminum oxide and determining trace metal elements in aluminum oxide |
| CN104297024A (en) * | 2013-10-31 | 2015-01-21 | 东旭集团有限公司 | Method for detecting stannic oxide main content and impurity content |
| CN104677883A (en) * | 2015-02-02 | 2015-06-03 | 海南中航特玻科技有限公司 | Analytical method for measuring impurity content in tin sample |
| CN105628683A (en) * | 2015-12-29 | 2016-06-01 | 东旭科技集团有限公司 | Method determining impurity content in stannic oxide electrode material |
| CN108956585A (en) * | 2018-05-16 | 2018-12-07 | 柘城惠丰钻石科技股份有限公司 | The detection method of metallic element in a kind of diadust |
-
2019
- 2019-09-02 CN CN201910820513.XA patent/CN110455598A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102998300A (en) * | 2012-11-19 | 2013-03-27 | 中国船舶重工集团公司第七二五研究所 | Analysis method for impurity elements in tin-oxide-containing nanopowder |
| CN103543141A (en) * | 2013-09-25 | 2014-01-29 | 中国科学院上海光学精密机械研究所 | Analytical method of trace impurity elements Fe and Cu in tin oxide electrode |
| CN104297024A (en) * | 2013-10-31 | 2015-01-21 | 东旭集团有限公司 | Method for detecting stannic oxide main content and impurity content |
| CN103868911A (en) * | 2014-04-03 | 2014-06-18 | 河南科技学院 | Method for dissolving aluminum oxide and determining trace metal elements in aluminum oxide |
| CN104677883A (en) * | 2015-02-02 | 2015-06-03 | 海南中航特玻科技有限公司 | Analytical method for measuring impurity content in tin sample |
| CN105628683A (en) * | 2015-12-29 | 2016-06-01 | 东旭科技集团有限公司 | Method determining impurity content in stannic oxide electrode material |
| CN108956585A (en) * | 2018-05-16 | 2018-12-07 | 柘城惠丰钻石科技股份有限公司 | The detection method of metallic element in a kind of diadust |
Non-Patent Citations (4)
| Title |
|---|
| 刘淑萍等: "《分析化学实验》", 31 October 2010 * |
| 张文清: "《分离分析化学（第二版）》", 29 February 2016, 华东理工大学出版社 * |
| 肖柳婧等: "碱熔-电感耦合等离子体原子发射光谱(ICP—AES)法测定锡矿石中锡", 《中国无机分析化学》 * |
| 金献忠等: "碱熔融-电感耦合等离子体原子发射光谱法测定铬矿石中铬铝铁镁硅", 《冶金分析》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101718720B (en) | Method for detecting content of carborundum impurities by applying X-ray fluorescent spectrometry | |
| CN102539511B (en) | Method for detecting content of bromine in fire retardant through automatic potentiometric titration | |
| CN104034722B (en) | Content of material assay method in a kind of complex silicon carbide | |
| CN109142412A (en) | The X-fluorescence measuring method of zinc, iron, Ti content during a kind of blast furnace dry method dust is grey | |
| CN111504982A (en) | Method for measuring boron content in glass by inductively coupled plasma emission spectrometry | |
| CN101644678A (en) | Method for detecting content of titanium dioxide in emulsion or milk powder | |
| CN107389494B (en) | The measuring method of SBS content in SBS modified pitch | |
| CN112858361A (en) | Detection method for measuring slag pressing agent by melting method sample preparation X-ray fluorescence spectrometry | |
| CN110455598A (en) | The sample treatment of impurity in a kind of detection stannic oxide | |
| CN106187884B (en) | 2- [2- hydroxyls -5- (4- nitroazobenzenes) styryl] -8-hydroxyquinoline colorimetric reagents and preparation and application | |
| CN101788464B (en) | Solution concentration on-line detection method in solventing-out crystallization process and special device thereof | |
| CN105044275B (en) | The method of testing of alumina content in aluminium metaphosphate | |
| CN109613169A (en) | A kind of method of lead molybdate precipitating in ferro-molybdenum chemical analysis | |
| CN106990098A (en) | The method of each element content in simultaneous determination aluminium electrolyte | |
| CN102192922A (en) | Heat conductivity coefficient measuring device for high temperature material | |
| CN106338534B (en) | The method of Calcium Fluoride Content in fluorite is quickly measured using Xray fluorescence spectrometer | |
| CN105606717B (en) | The detection method in Buddhist nun's bulk drug about material is replaced in the life of two p-methyl benzenesulfonic acid edge | |
| CN106290438B (en) | A kind of method that X-ray fluorescence spectra fusion method measures Calcium Fluoride Content in fluorite | |
| CN106568643B (en) | Method for determining impurity content in alumina sample and sample pretreatment method | |
| CN110146490A (en) | A method of with micro ruthenium element in ICP-OES measurement drug | |
| CN104062285A (en) | Determination method for contents of calcium, aluminum and silicon elements in solid surface materials | |
| CN104215541B (en) | Efficiently, high purity aluminium oxide content and the method for impurity content are accurately detected | |
| CN107356618A (en) | A kind of method of covering agent component content in x-ray fluorescence spectrometry | |
| CN107860721A (en) | With the method for sulfur content in ICP test sample product | |
| CN107247051A (en) | A kind of method of quick detection phospholipid in lipid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191115 |
|
| RJ01 | Rejection of invention patent application after publication |