CN102539197A - Sampling method implemented during process of analyzing metal-element content of high-purity silicon tetrachloride product used for fibers - Google Patents
Sampling method implemented during process of analyzing metal-element content of high-purity silicon tetrachloride product used for fibers Download PDFInfo
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- CN102539197A CN102539197A CN2012100109109A CN201210010910A CN102539197A CN 102539197 A CN102539197 A CN 102539197A CN 2012100109109 A CN2012100109109 A CN 2012100109109A CN 201210010910 A CN201210010910 A CN 201210010910A CN 102539197 A CN102539197 A CN 102539197A
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Abstract
The invention relates to a sampling method for high-purity silicon tetrachloride products, and particularly relates to a sampling method implemented during a process of analyzing the metal-element content of a high-purity silicon tetrachloride product used for fibers. The method sequentially comprises the following steps: cleaning sampling bottles, drying the sampling bottles, sampling the sampling bottles, and gathering impurities of metal elements.
Description
Technical field
The present invention relates to the sampling method of high purity silicon tetrachloride product, be specifically related to a kind of sampling method when analyzing optical fiber with high purity silicon tetrachloride resultant metal constituent content.
Background technology
Silicon tetrachloride (SiCl
4) normal temperature, normal pressure is liquid down, 57.6 ℃ of boiling points, volatile; Be prone to vaporization, steam has faintly acid, and the smell of suffocating is arranged; Facile hydrolysis forms silicic acid and hydrogen chloride in humid air; Emit heat simultaneously, white cigarette takes place, be mainly used in system silicate class, organic silicon monomer, organic silicone oil, high temperature insulating material, silicones, silicon rubber etc.And the silicon tetrachloride that is used for the optical fiber manufacturing is very high to the purity requirement of raw material, and China's optical fiber mainly relies on import with the silicon tetrachloride raw material at present.In order to reduce fiber transmission attenuation, silicon tetrachloride must pass through strict the purification as the primary raw material of optical fiber, to remove harmful transition metal ion.China does not formulate standard to optical fiber with the analysis of silicon tetrachloride, and sampling process is not seen relevant patent report yet.The optical fiber of formulating by German Merck company is with the requirement of high purity silicon tetrachloride commercial quality, and transition metal ion impurity content standard is:
| Metallic element | V | Cr | Mn | Fe | Co | Ni | Cu | Ge |
| Quality standard (ng/g) | ≤2 | ≤1 | ≤0.5 | ≤5 | ≤1 | ≤1 | ≤1 | ≤3 |
Adopt ICP-MS to analyze various metallic elements simultaneously, can obtain reasonable result, but this character and detection of trace (ng/g level) metallic element to the silicon tetrachloride sample has proposed very high requirement.
In the sampling pollution of sample from baking oven air-flow in the unclean property of sampling jar, the baking bottle to bottle pollution, pipeline and valve pollute, the pollution of moisture and dust in the extraneous surrounding air in the sampling process, environmental pollution and wave in the silicon excessive temperature metallic element is taken away with gas etc. in the impurity enriched process.In view of silicon tetrachloride character and determination of trace element requirement, the sample sampling must be accomplished sampling jar cleaning, pipeline and valve cleaning, sampling process sealing, and low temperature seal is waved silicon, could guarantee by the true and reliable property of sample thief.
Summary of the invention
The object of the present invention is to provide a kind of sampling method when analyzing optical fiber with high purity silicon tetrachloride resultant metal constituent content, this method guarantees that institute's sample thief adopts ICP-MS analyzing metal elements result's true and reliable property.
The present invention realizes through following technical scheme: the sampling method when analyzing optical fiber with high purity silicon tetrachloride resultant metal constituent content, this method comprise cleaning sampling jar, oven dry sampling jar, sampling jar sampling, four steps of metallic element impurity enriched successively.
Above-mentioned cleaning sampling jar step comprise following 2 step by step:
1) sampling jar to be cleaned is placed in the container, analytically pure oxydol of injection and concentration are 10% analytical pure sulfuric acid formation mixed liquor in container, let sampling jar be immersed in this mixed liquor until lather collapse;
2) sampling jar is taken out from above-mentioned mixed liquor, soaked 4～5 hours with deionized water, clean with deionized water rinsing 4～5 times then up to acid solution.
Above-mentioned sampling jar is for adopting the sampling jar that covers of teflon barred body material monolithic making.
Above-mentioned analytically pure oxydol and concentration are that 10% analytical pure sulfuric acid volume ratio is 2:1.
Above-mentioned oven dry sampling jar step comprise following 3 step by step:
1) sampling jar is inserted in the cleaning oven, dried by the fire 24 hours down at 60 ℃;
2) oven temperature is reduced to 50 ℃, dried by the fire 2 hours, reduce to 40 ℃ again, dried by the fire 2 hours, cut off the electricity supply then;
3) treat after sampling jar cools off fully it to be taken out from baking oven, building bottle cap, to put into freshness protection package sealing for use.
Above-mentioned sampling jar sampling procedure comprise following 5 step by step:
1) connect, each sampling equipment such as fixing, cleaning and drying duct valve;
2) form the air chamber that seals on every side at sample tap and sampling bottleneck, air chamber was poured high pure nitrogen about 10 minutes;
3) turn on the sampling bottle cap, rapidly sampling jar is positioned over sample tap and takes a sample, confirm that through illumination sample takes out scale;
4) treat that sampling finishes after, take out sampling jar and change waste liquid bottle, sampling jar seals rapidly;
5) if will continue other sample tap sampling is repeated above 4 steps.
Above-mentioned metallic element impurity enriched step comprise following 3 step by step:
1) takes a sample from sample bottle in the nitrogen environment of drying with transfer pipet rapidly, put into 3 and wave the silicon bottle;
2) connect and wave the silicon device; The above-mentioned silicon bottle of waving is heated under 57 ℃ of waters bath with thermostatic control; Adopt optical fiber to carry secretly and make the volatilization of silicon tetrachloride matrix with the big Lip river of the generation gram gas filter filtration low temperature of 99.999% high purity nitrogen warp 0.5 μ m; Till the noresidue silicon tetrachloride liquid, the matrix silicon tetrachloride of volatilization discharges with the back in lime water;
3) after matrix volatilization is accomplished, will wave the silicon bottle rapidly and unload and add a cover, and send ICP-MS instrumental analysis, each sample is by 1)-3) enrichment three times step by step.
Compare with existing public technology, the present invention has following advantage:
A kind of cleaning sampling jar effective method is provided;
Avoided sampling jar dry run drying box air-flow that sampling jar is polluted;
One cover sampling flow process has been avoided the pollution to sample of pipeline, valve and external environment;
Impurity enriched process airtight, low temperature avoided present ICP-MS analyze in the uncovered heating of ultra close-table (150 ℃) wave silicon, external environmental and metallic element high temperature entrainment loss phenomenon.
Description of drawings
Fig. 1 is the sampling process synoptic diagram;
Wherein: 1-sampling dish, 2-distributor pipe, 3-T-valve, 4-air chamber, 5-removable hose, 6-friction top, 7-sampling jar, 8-lifting table, 9-sampling bench, 10-holding tank;
Fig. 2 is for waving silicon process synoptic diagram;
Fig. 3 is the sampling process process flow diagram.
Embodiment
Like Fig. 1, shown in Figure 3, the present invention includes following four processes:
Process one: sampling jar cleans
It is that 120ml covers sampling jar that step 1, employing teflon barred body material monolithic are made volume.
Step 2, elder generation are placed on sampling jar to be cleaned in the big plastic cup, carefully pour oxydol (AR) and 10% sulfuric acid (AR) into along wall of cup successively, and oxydol and sulfuric acid blending ratio are 2:1, let article be immersed in the mixed liquor until lather collapse.
Step 3, sampling jar were soaked 4～5 hours with deionized water, and it is clean to arrive pickling for 4～5 times with deionized water rinsing then.
Above Principle of Process be adopt various acid and oxydol can with each metal ion species generation oxidation reaction of being with in the sampling jar, clean sampling jar.
Process two: oven dry
Step 1, baking oven is cleaned up, sampling jar is put into the tailormadepiston baker dry, regulating oven temperature is 60 ℃, keeps 24 hours.
After step 2, the oven dry oven temperature is transferred to 50 ℃, lowered the temperature 2 hours, transfer to 40 degree again, lowered the temperature 2 hours, cut off the electricity supply then.
Step 3, treat that sampling jar cools off fully after, with clean gloves sampling jar is taken out, add a cover that to put into freshness protection package sealing for use.
Above process can guarantee that in drying course intrinsic metallic ion does not pollute sample bottle in the baking oven air-flow.
Process three: sampling (sampling method is seen Fig. 1)
Step 1, the preceding elder generation of sampling be clean dry sampling assemble 4,6 fixedly, connects removable hose 5.
Step 2, on production line material pipeline, bypass to be set be sample tap, opens sample cock in the bypass, makes it to coil 1 set distributor pipe 2 through sampling and link to each other with sampling three-way valve 3.
Step 3, unlatching T-valve wash pipeline, simultaneously air chamber 4 are poured high pure nitrogen, about 10 minutes of this process.
Step 4, turn on the sampling bottle cap after the oven dry, rapidly sampling jar is positioned over sample tap, sample tap and friction top are fixed through lifting table 8.
Step 5, open three-way valve 3 and take a sample, confirm that through illumination sample takes out scale, sample size is about 100ml.
After step 6, the end of waiting to take a sample, open three-way valve 3 feed liquid is blown off to holding tank 10, take out sample bottle simultaneously and change waste liquid bottle, sample bottle seals rapidly.
After step 7, pipeline blow off, through three-way valve 3 adjustings removable hose 5 is blown off, feed liquid is collected by waste liquid bottle.
Step 8, close T-valve 3 and all nitrogen pipelines, take off removable hose 5 and sampling assemble 4,6, clean for use.
Step 9, if will continue to the sampling of other sample tap, repeating step 1～8.
Process four: metallic element impurity enriched (method is seen Fig. 2)
Step 1, rapidly will take a sample transfer pipet in the nitrogen environment of drying from sample bottle sampling 30ml, put into 3 and wave silicon bottle 11;
Step 2, connect by Fig. 2 and to wave silicon device (wave silicon device comprise wave silicon bottle 11 and absorption bottle 12); Wave 57 ℃ of water bath with thermostatic control heating of silicon bottle 11 usefulness; Adopt optical fiber to carry secretly through the big Lip river gram gas filter filtration of generation (0.5 μ m) and make the volatilization of silicon tetrachloride matrix with 99.999% high purity nitrogen; Till the noresidue silicon tetrachloride liquid, the lime water of the matrix silicon tetrachloride of volatilization in absorption bottle 12 receives, the discharging of neutralization back;
Step 3, silicon tetrachloride matrix are evaporated completely back (about 24h), will wave the silicon bottle rapidly and unload and add a cover, and send ICP-MS instrumental analysis.
Each sample is by above step enrichment three times.
Below in conjunction with four sampling procedures and accompanying drawing 1, Fig. 2, further the present invention will be described for embodiment, but the present invention is not limited to this.
By process one method sample bottle is cleaned, sample bottle is toasted, take a sample, impurity in the sample is carried out enrichment by process four directions method by process three methods by process two methods.Analytical instrument is the ICP-MS of U.S. Thermo Electron company, and model is X-7.To different samples, the different time sample analysis can both obtain the authentic sample analysis result.
Embodiment 1:
Provide German Merck company optical fiber to use SiCl to Wuhan optical fiber cable company limited
4Commodity about 100ml that takes a sample adopts ICP-MS to analyze, and analyzes three times with an appearance 30ml at every turn, and average result is seen table 1.
Embodiment 2:
To by-product SiCl in the production of polysilicon of our purchase
4Raw material carries out sample analysis, and this raw material ships with special-purpose tank car from certain polysilicon factory purifying plant, adopts nitrogen to be pressed onto head tank and stores.From the head tank sampling, the about 30m of extraction pipeline wherein has 4 valves, sampling 100ml.Adopt ICP-MS to analyze, each appearance 30ml that uses analyzes three times, and average result is seen table 2.
Embodiment 3:
Adopt purifying column extraction regular grade product No. 1, the about 30m of extraction pipeline wherein has 4 valves, and sampling 110ml adopts ICP-MS to analyze, and each appearance 30ml that uses analyzes three times, and average result is seen table 3.
Embodiment 4:
Produce high-purity grade of product, the about 0.2m of product tank volume
3, the about 20m of sampling line wherein has 3 valves, and jar outlet sampling 115ml adopts ICP-MS to analyze, and with appearance 30ml, analyzes three times at every turn, and average result is seen table 4.This product through Wuhan one tame optical fiber company on probation at the PCVT bed, optical fiber each item index of being produced is qualified, has proved the accuracy of analytical approach.
Embodiment 5:
Factory's relay tank material, this raw material can be made the regular grade product export, and also can continue to purify is optical fiber level product.The about 12m3 of tank volume, the about 25m of sampling line wherein has 3 valves, sampling 112ml.Adopt ICP-MS to analyze, each appearance 30ml that uses analyzes three times, and average result is seen table 5.
Embodiment 6:
With U.S. a company check analysis: raw material is the by-product SiCl of polysilicon factory
4, contain SiCl
4Be 99%.After the steady production 7 days, in the product jar, take a sample simultaneously A, B, one kind of article send U.S. optical fiber enterprise specialty to detect, and another sample oneself detects and contrasts, and analysis result is seen table 6.Can know that by table 6 result is basic identical.
Table 1 embodiment 1 product analysis result
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Table 2 embodiment 2 analysis results
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Table 3 embodiment 3 product analysis results
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Table 4 embodiment 4 product analysis results
"/" expression does not detect
Table 5 embodiment 5 analysis results
"/" expression does not detect
Table 6 and U.S. optical fiber enterprise check analysis
| Element | Max (ng/g) | External detect (ng/g) | Domestic check (ng/g) |
| Iron | 15 | 2.13 | 1.32 |
| Chromium | 5 | <0.2 | 0.01 |
| Copper | 5 | <0.1 | / |
| Manganese | 5 | <0.2 | / |
| Nickel | 5 | <0.2 | / |
| Aluminum | 5 | <0.2 | / |
"/" expression does not detect.
Claims (9)
1. the sampling method when analyzing optical fiber with high purity silicon tetrachloride resultant metal constituent content is characterized in that, this method comprises successively cleans sampling jar, oven dry sampling jar, sampling jar sampling, four steps of metallic element impurity enriched.
2. the sampling method of analysis optical fiber as claimed in claim 1 during with high purity silicon tetrachloride resultant metal constituent content is characterized in that, said cleaning sampling jar step comprise following 2 step by step:
1) sampling jar to be cleaned is placed in the container, analytically pure oxydol of injection and concentration are 10% analytical pure sulfuric acid formation mixed liquor in container, let sampling jar be immersed in this mixed liquor until lather collapse;
2) sampling jar is taken out from above-mentioned mixed liquor, soaked 4～5 hours with deionized water, clean with deionized water rinsing 4～5 times then up to acid solution.
3. the sampling method of analysis optical fiber as claimed in claim 2 during with high purity silicon tetrachloride resultant metal constituent content is characterized in that: said sampling jar is for adopting the sampling jar that covers that teflon barred body material monolithic makes.
4. the sampling method of analysis optical fiber as claimed in claim 3 during with high purity silicon tetrachloride resultant metal constituent content is characterized in that: used analytically pure oxydol and concentration are that 10% analytical pure sulfuric acid volume ratio is 2:1.
5. the sampling method of analysis optical fiber as claimed in claim 1 during with high purity silicon tetrachloride resultant metal constituent content is characterized in that, said oven dry sampling jar step comprise following 3 step by step:
1) sampling jar is inserted in the cleaning oven, dried by the fire 24 hours down at 60 ℃;
2) oven temperature is reduced to 50 ℃, dried by the fire 2 hours, reduce to 40 ℃ again, dried by the fire 2 hours, cut off the electricity supply then;
3) treat after sampling jar cools off fully it to be taken out from baking oven, building bottle cap, to put into freshness protection package sealing for use.
6. the sampling method of analysis optical fiber as claimed in claim 1 during with high purity silicon tetrachloride resultant metal constituent content is characterized in that, said sampling jar sampling procedure comprise following 5 step by step:
1) connects, fixes, cleans and dry sampling equipment;
2) form the air chamber that seals on every side at sample tap and sampling bottleneck, air chamber was poured high pure nitrogen about 10 minutes;
3) turn on the sampling bottle cap, rapidly sampling jar is positioned over sample tap and takes a sample, confirm that through illumination sample takes out scale;
4) treat that sampling finishes after, take out sampling jar and change waste liquid bottle, sampling jar seals rapidly;
5) if will continue other sample tap sampling is repeated above 4 steps.
7. the sampling method of analysis optical fiber as claimed in claim 1 during with high purity silicon tetrachloride resultant metal constituent content is characterized in that, said metallic element impurity enriched step comprise following 3 step by step:
1) takes a sample from sample bottle in the nitrogen environment of drying with transfer pipet rapidly, put into 3 and wave the silicon bottle;
2) connect and wave the silicon device, wave silicon bottle water bath with thermostatic control heating with above-mentioned, make the volatilization of silicon tetrachloride matrix, till the noresidue silicon tetrachloride liquid, the matrix silicon tetrachloride of volatilization discharges with the back in lime water;
3) after matrix volatilization is accomplished, will wave the silicon bottle rapidly and unload and add a cover, and send ICP-MS instrumental analysis, each sample is by 1)-3) enrichment three times step by step.
8. the sampling method of analysis optical fiber as claimed in claim 7 during with high purity silicon tetrachloride resultant metal constituent content is characterized in that above-mentioned water bath with thermostatic control is heated to be 57 ℃.
9. the sampling method of analysis optical fiber as claimed in claim 8 during with high purity silicon tetrachloride resultant metal constituent content; It is characterized in that above-mentioned step by step 2) the gram gas filter filters low temperature and carries secretly the silicon tetrachloride matrix is volatilized through the big Lip river of the generation of 0.5 μ m with 99.999% high purity nitrogen to adopt optical fiber.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105784459A (en) * | 2016-03-15 | 2016-07-20 | 亚洲硅业（青海）有限公司 | Pretreatment method for trace impurity element on chlorosilane and polycrystalline silicon body surface metal |
| CN106568775A (en) * | 2016-10-24 | 2017-04-19 | 洛阳中硅高科技有限公司 | Online detection apparatus of tetrachlorosilane for optical fibers |
| CN107024527A (en) * | 2016-01-29 | 2017-08-08 | 安捷伦科技有限公司 | Plasma spectroscopy device |
| CN107101850A (en) * | 2017-04-06 | 2017-08-29 | 洛阳中硅高科技有限公司 | On-line period method |
| CN107643281A (en) * | 2017-09-29 | 2018-01-30 | 通标标准技术服务有限公司 | Industrial silicon dirt content test method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6142024A (en) * | 1997-10-23 | 2000-11-07 | Huls Aktiengesellschaft | Apparatus and method for sampling and IR-spectroscopic analysis of high-purity, hygroscopic liquids |
| 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 |
-
2012
- 2012-01-13 CN CN2012100109109A patent/CN102539197A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6142024A (en) * | 1997-10-23 | 2000-11-07 | Huls Aktiengesellschaft | Apparatus and method for sampling and IR-spectroscopic analysis of high-purity, hygroscopic liquids |
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| 方志青等: "气相色谱法测定四氯化硅的纯度", 《理化检验(化学分册)》, vol. 47, no. 5, 31 December 2011 (2011-12-31) * |
| 郭峰: "海绵钛生产中回收副产物四氯化硅纯度分析方法研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》, no. 4, 15 October 2007 (2007-10-15) * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107024527A (en) * | 2016-01-29 | 2017-08-08 | 安捷伦科技有限公司 | Plasma spectroscopy device |
| CN107024527B (en) * | 2016-01-29 | 2022-04-12 | 安捷伦科技有限公司 | Plasma spectrum analyzer |
| CN105784459A (en) * | 2016-03-15 | 2016-07-20 | 亚洲硅业（青海）有限公司 | Pretreatment method for trace impurity element on chlorosilane and polycrystalline silicon body surface metal |
| CN105784459B (en) * | 2016-03-15 | 2019-05-21 | 亚洲硅业（青海）有限公司 | The pretreating device of chlorosilane and polysilicon body surface metal trace impurity element |
| CN106568775A (en) * | 2016-10-24 | 2017-04-19 | 洛阳中硅高科技有限公司 | Online detection apparatus of tetrachlorosilane for optical fibers |
| CN107101850A (en) * | 2017-04-06 | 2017-08-29 | 洛阳中硅高科技有限公司 | On-line period method |
| CN107643281A (en) * | 2017-09-29 | 2018-01-30 | 通标标准技术服务有限公司 | Industrial silicon dirt content test method |
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Application publication date: 20120704 |