CN204064765U - For detecting process in early stage, the sampler of industrial germanium tetrachloride - Google Patents

For detecting process in early stage, the sampler of industrial germanium tetrachloride Download PDF

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Publication number
CN204064765U
CN204064765U CN201420509809.2U CN201420509809U CN204064765U CN 204064765 U CN204064765 U CN 204064765U CN 201420509809 U CN201420509809 U CN 201420509809U CN 204064765 U CN204064765 U CN 204064765U
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Prior art keywords
bottle
germanium tetrachloride
nitrogen
sample cell
nitrogen pipeline
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CN201420509809.2U
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莫正辉
张爱华
祁君芳
孙凡
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WUHAN YUNJINGFEI OPTICAL FIBER MATERIAL Co Ltd
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WUHAN YUNJINGFEI OPTICAL FIBER MATERIAL Co Ltd
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Abstract

The utility model discloses a kind of for detect industrial germanium tetrachloride early stage process, sampler, comprise germanium tetrachloride bottle for material and sample cell, process bottle, receiving bottle and nitrogen pipeline, described germanium tetrachloride bottle for material, process bottle, sample cell, receiving bottle successively with nitrogen pipeline UNICOM.Adopt device of the present utility model, the foreign gases such as chlorine free in germanium tetrachloride sample and hydrochloric acid can be made to enter tail gas, its infrared spectrum 2985cm -1and 2835cm -1the saturated peak of connection separated, 3322cm -1peak is high-visible; The nitrogen simultaneously retained in sample cell can effectively avoid entering of air, makes the germanium tetrachloride in sample cell not easily produce hydrolysis reaction, advantageously in obtaining correct germanium tetrachloride liquid phase infrared spectrum, improves the accuracy detecting data.The utility model also has the features such as simple to operate, quick, and impurity in sample cell, nitrogen pipeline, process bottle or residue can be avoided completely to the interference of testing result.

Description

For detecting process in early stage, the sampler of industrial germanium tetrachloride
Technical field
The utility model relate to a kind of for detect industrial germanium tetrachloride early stage process, sampler.
Background technology
Germanium tetrachloride easily with water generation hydrolysis reaction, run into soft air and to be fuming immediately generation hydrolysis reaction release HCl gas.
GeCl 4+4H 2O→Ge(OH) 4+4HCl↑
When detecting the quality of industrial germanium tetrachloride, owing to there is the gases such as a small amount of free chlorine and hydrochloric acid in germanium tetrachloride material, when adopting liquid phase infrared spectroscopic determination germanium tetrachloride, if directly sampled from bottle for material with sample cell, serious interference will be produced, particularly at wave number 2985cm to testing result -1and 2835cm -1be connected to form one saturated through peak, at wave number 3322cm -1, 3301cm -1not too obvious through peak, cause and cannot read wave number 2985cm in germanium tetrachloride material detection sample -1, 2835cm -1, and 3322cm -1peak value, can not get the correct detection data of germanium tetrachloride material.
Summary of the invention
The purpose of this utility model is to remove impurity in industrial germanium tetrachloride material to the interference of testing result, obtaining correct industrial germanium tetrachloride liquid phase infrared spectrum, thus improves the accuracy detecting data.For this reason we provide a kind of for detect industrial germanium tetrachloride early stage process, sampler.
Above-mentioned purpose is achieved through the following technical solutions:
A kind of early stage for detecting industrial germanium tetrachloride processes, sampler, comprise germanium tetrachloride bottle for material and sample cell, also comprise process bottle, receiving bottle and nitrogen pipeline, described germanium tetrachloride bottle for material, process bottle, sample cell, receiving bottle successively with nitrogen pipeline UNICOM
Described germanium tetrachloride bottle for material is in parallel with nitrogen pipeline, draft tube and drain pipe is provided with in germanium tetrachloride bottle for material, the mouth of pipe of described drain pipe is positioned at the bottom of germanium tetrachloride bottle for material, and described draft tube and drain pipe are equipped with for the two-port valve in parallel with nitrogen pipeline;
Described receiving bottle is in parallel with nitrogen pipeline, is provided with feed tube and escape pipe in receiving bottle, and the mouth of pipe of described escape pipe is positioned at the top of receiving bottle, and described feed tube and escape pipe are equipped with for the two-port valve in parallel with nitrogen pipeline;
Described sample cell is in parallel with nitrogen pipeline, and sample cell is provided with feed pipe and discharge nozzle, and described feed pipe and discharge nozzle are equipped with for the two-port valve in parallel with nitrogen pipeline;
Described process bottle is connected with nitrogen pipeline, and process bottle is provided with charging aperture and discharging opening, and described charging aperture is positioned at the bottom of process bottle, and described discharging opening is positioned at the top of process bottle.
Preferably, the inlet end of described nitrogen pipeline is provided with the valve for controlling nitrogen flow.
Preferably, the mouth of pipe of the draft tube in described germanium tetrachloride bottle for material is positioned at the top of germanium tetrachloride bottle for material.
Preferably, the mouth of pipe of the feed tube in described receiving bottle is positioned at the bottom of receiving bottle.
In order to ensure the accuracy of the infrared detection data of germanium tetrachloride, adopt device of the present utility model, high pure nitrogen can be passed into the detection sample of industrial germanium tetrachloride material to purge (referred to as nitrogen flushing), the foreign gases such as chlorine free in germanium tetrachloride sample and hydrochloric acid are made to enter tail gas, germanium tetrachloride sample through nitrogen flushing early stage process after, its infrared spectrum 2985cm -1and 2835cm -1the saturated peak of connection separated, 3322cm -1peak is high-visible; The nitrogen simultaneously retained in sample cell can effectively avoid entering of air, makes the germanium tetrachloride in sample cell not easily produce hydrolysis reaction, advantageously in obtaining correct germanium tetrachloride liquid phase infrared spectrum, improves the accuracy detecting data.
The utility model also has the features such as simple to operate, quick, and impurity in sample cell, nitrogen pipeline, process bottle or residue can be avoided completely to the interference of testing result.
Accompanying drawing explanation
Fig. 1 is the structural representation of the utility model device.
Fig. 2 is the infrared spectrum not carrying out industrial germanium tetrachloride sampling process in early stage.
Fig. 3 is the infrared spectrum after carrying out industrial germanium tetrachloride sampling process in early stage.
In figure: 1-germanium tetrachloride bottle for material, 2-sample cell, 3-process bottle, 4-receiving bottle, 5-nitrogen pipeline, 6-valve.
Embodiment
Below in conjunction with accompanying drawing and embodiment, the utility model is described in detail.
Embodiment: as shown in Figure 1, a kind of early stage for detecting industrial germanium tetrachloride processes, sampler, comprise germanium tetrachloride bottle for material 1 and sample cell 2, process bottle 3, receiving bottle 4 and nitrogen pipeline 5, described germanium tetrachloride bottle for material 1, process bottle 3, sample cell 2, receiving bottle 4 successively with nitrogen pipeline 5 UNICOM.
Described germanium tetrachloride bottle for material 1 is in parallel with nitrogen pipeline 5, draft tube and drain pipe is provided with in germanium tetrachloride bottle for material 1, the mouth of pipe of described drain pipe is positioned at the bottom of germanium tetrachloride bottle for material 1, the mouth of pipe of draft tube is positioned at the top of germanium tetrachloride bottle for material 1, and described draft tube and drain pipe are equipped with for the two-port valve in parallel with nitrogen pipeline 5.
Described receiving bottle 4 is in parallel with nitrogen pipeline 5, feed tube and escape pipe is provided with in receiving bottle 4, the mouth of pipe of described escape pipe is positioned at the top of receiving bottle 4, and the mouth of pipe of feed tube is positioned at the bottom of receiving bottle 4, and described feed tube and escape pipe are equipped with for the two-port valve in parallel with nitrogen pipeline 5.
Described sample cell 2 is in parallel with nitrogen pipeline 5, and sample cell 2 is provided with feed pipe and discharge nozzle, and described feed pipe and discharge nozzle are equipped with for the two-port valve in parallel with nitrogen pipeline 5.
Described process bottle 3 is connected with nitrogen pipeline 5, and process bottle 3 is provided with charging aperture and discharging opening, and described charging aperture is positioned at the bottom of process bottle 3, and described discharging opening is positioned at the top of process bottle 3.
The inlet end of described nitrogen pipeline 5 is provided with the valve 6 for controlling nitrogen flow.
The process in early stage, the sampling method that detect industrial germanium tetrachloride are:
1. the pre-service of nitrogen pipeline and process bottle
For getting rid of air in nitrogen pipeline 5 and process bottle 3 and pollutant, avoid it to enter the sample cell 2 pairs of testing results when sampling and produce interference, before sampling, first need carry out the pre-service of nitrogen flushing and rinse to nitrogen pipeline 5 and process bottle 3, disposal route is as follows:
The purging of 1.1 nitrogen pipelines and process bottle
Before cleaning, need purge nitrogen pipeline 5.(namely two-port valve is opened to the direction of nitrogen pipeline 5 two-port valve on germanium tetrachloride bottle for material 1, sample cell 2, receiving bottle 4 to be all arranged on short-circuit condition, nitrogen pipeline 5 is directly communicated with, nitrogen is not by germanium tetrachloride bottle for material 1, sample cell 2 and receiving bottle 4), open nitrogen and control nitrogen flow by valve 6,10min is purged to nitrogen pipeline 5.
1.2 germanium tetrachloride bottle for material fill nitrogen pressurization
After blowing pipeline terminates, close nitrogen, receiving bottle 4 pressure release 30s, then the two-port valve on germanium tetrachloride bottle for material 1 drain pipe is arranged on short-circuit condition, two-port valve in draft tube is arranged on channel status, and (namely two-port valve is opened to the direction of germanium tetrachloride bottle for material 1, nitrogen pipeline 3 can not be directly communicated with, nitrogen enters germanium tetrachloride bottle for material 1), open nitrogen and nitrogen 10 ~ 15s is mended to germanium tetrachloride bottle for material 1, the nitrogen pressure in germanium tetrachloride bottle for material 1 is made to be 1 ~ 2Bar, the excessive binder excessive velocities easily causing the later stage of pressure, more germanium tetrachloride material can be wasted on the one hand, process bottle 3 can be made to be impacted when shifting germanium tetrachloride material to process bottle 3 on the other hand and break, jeopardize personal safety.
Germanium tetrachloride material is pressed onto process bottle by 1.3
Germanium tetrachloride bottle for material 1 is mended after nitrogen terminates, nitrogen is closed by valve 6, two-port valve in germanium tetrachloride bottle for material 1 draft tube is switched to short-circuit condition, two-port valve on germanium tetrachloride bottle for material 1 drain pipe is slowly opened, makes the germanium tetrachloride material in germanium tetrachloride bottle for material 1 under the effect of pressure reduction, enter process bottle 3.
The rinse of 1.4 process bottles
When the press-in of germanium tetrachloride material processes 20% place of bottle 3 volume, carry out the cleaning processing bottle 3.Two-port valve on germanium tetrachloride bottle for material draft tube and drain pipe is all set to short-circuit condition, slow Open valve 6, after germanium tetrachloride material residual in nitrogen pipeline 5 being all pressed into process bottle 3, closing nitrogen, process bottle 3 is rocked gently and carries out rinse.
After rinse completes, two-port valve on receiving bottle 4 feed tube and escape pipe is all switched to channel status, opens nitrogen, process bottle 3 is tilted, make the discharging opening of the germanium tetrachloride material submerged impinging jet bottle 3 in process bottle 3, the germanium tetrachloride material rinse liquid of cleaning treatment bottle 3 is all pressed in receiving bottle 4, closes nitrogen, after receiving bottle 4 pressure release 30s, again the two-port valve on receiving bottle 4 feed tube and escape pipe is switched to short-circuit condition, open nitrogen, nitrogen pipeline 5 is purged, then closes nitrogen.
2. process the early stage of germanium tetrachloride, sample
For ensureing the accuracy of germanium tetrachloride material sample detection result, need carry out nitrogen flushing process in early stage to the detection sample of germanium tetrachloride material, the operation steps of process is:
Germanium tetrachloride material is pressed onto process bottle by 2.1
Two-port valve on germanium tetrachloride bottle for material 1 drain pipe is slowly opened, makes the germanium tetrachloride material in germanium tetrachloride bottle for material 1 under the effect of pressure reduction, enter process bottle 3.
2.2 pairs of germanium tetrachloride materials carry out nitrogen flushing process
After 50 ~ 80% of germanium tetrachloride sample press-in process bottle 3 volume, the two-port valve on germanium tetrachloride bottle for material 1 draft tube and drain pipe is arranged on short-circuit condition.Open nitrogen, according to the flow velocity of germanium tetrachloride material in nitrogen pipeline 5, control valve 6, germanium tetrachloride material in pipe is all pressed in process bottle 3, and by control valve 6, make the germanium tetrachloride material in process bottle 3 remain micro-and seethe state, duration of ventilation is 30 ~ 60min, realizes the nitrogen flushing to germanium tetrachloride material in process bottle 3.
The rinse of 2.3 sample cells
In order to avoid the impurity in sample cell 2 or detection residue are to the interference of testing result, need before sampling to carry out rinse to sample cell 2.First by germanium tetrachloride bottle for material 1, two-port valve on receiving bottle 4 is all arranged on short-circuit condition, then the two-port valve on sample cell 2 feed pipe and discharge nozzle is arranged on channel status, open nitrogen, process bottle 3 is tilted, the germanium tetrachloride material in process bottle 3 is made to flood discharging opening, germanium tetrachloride material in process bottle 3 is compressed into sample cell 2, after sample cell 2 discharge nozzle has germanium tetrachloride material to flow out, close nitrogen, two-port valve on receiving bottle 4 feed tube and escape pipe is switched to channel status, open nitrogen again, nitrogen is closed after germanium tetrachloride rinse liquid in sample cell 2 is all pressed into receiving bottle 4, on receiving bottle 4 two two-port valve is switched to short-circuit condition again.
2.4 sample cell samplings
Again open nitrogen, process bottle 3 is tilted, the germanium tetrachloride material in process bottle 3 is made to flood gas outlet, germanium tetrachloride material in process bottle 3 is compressed into sample cell 2, after the discharge nozzle of sample cell 2 has germanium tetrachloride material to flow out, the two-port valve on sample cell 2 feed pipe and discharge nozzle is all switched to short-circuit condition, remaining germanium tetrachloride material in bottle 3 and nitrogen pipeline 5 will be processed with nitrogen and be pressed in receiving bottle 4, close nitrogen, switch to short-circuit condition to after receiving bottle 4 pressure release 30s.Finally regulate all valves on germanium tetrachloride bottle for material 1, sample cell 2, receiving bottle 4 to be in short-circuit condition, open nitrogen, 15min is purged to nitrogen pipeline 5 and clears up.
Testing result is as follows:
According to GB/T 6040 infrared spectrum analysis general rule, use Fourier infrared spectrograph to carry out infrared detection to the germanium tetrachloride material in sample cell 2, detect spectrogram as shown in Figure 2,3.
Wherein Fig. 2 is the infrared spectrum not carrying out germanium tetrachloride sampling process in early stage, as can see from Figure 2: wave number 2985cm -1to 2710cm -1peak connect into one saturated through peak, wave number 3322cm -1, 3301cm -1slightly highlight through peak, cause and cannot judge wave number 2985cm -1and 2710cm -1, 3322cm -1, 3301cm -1the transmitance through peak.
Fig. 3 uses device of the present utility model to carry out the infrared spectrum after process in early stage to thick germanium tetrachloride sample, wave number 2985cm -1, 2710cm -1what connect is saturated obvious through peak through separating in two of peak, 3322cm -1, 3301cm -1wave number high-visible through peak, reading that therefore can be correct, through peak value, obtains sample and detects data accurately.
Therefore, after adopting the detection sample of method to industrial germanium tetrachloride material passing into nitrogen to carry out process in early stage, effectively can eliminate the foreign gases such as chlorine free in sample and hydrochloric acid to the interference measured, make the detection data that obtain more accurately and reliably, thus have laid a good foundation for the quality testing analysis of industrial germanium tetrachloride.

Claims (4)

1. one kind for detect industrial germanium tetrachloride early stage process, sampler, comprise germanium tetrachloride bottle for material (1) and sample cell (2), it is characterized in that: also comprise process bottle (3), receiving bottle (4) and nitrogen pipeline (5), described germanium tetrachloride bottle for material (1), process bottle (3), sample cell (2), receiving bottle (4) successively with nitrogen pipeline (5) UNICOM
Described germanium tetrachloride bottle for material (1) is in parallel with nitrogen pipeline (5), germanium tetrachloride bottle for material is provided with draft tube and drain pipe in (1), the mouth of pipe of described drain pipe is positioned at the bottom of germanium tetrachloride bottle for material (1), and described draft tube and drain pipe are equipped with for the two-port valve in parallel with nitrogen pipeline (5);
Described receiving bottle (4) is in parallel with nitrogen pipeline (5), receiving bottle is provided with feed tube and escape pipe in (4), the mouth of pipe of described escape pipe is positioned at the top of receiving bottle (4), and described feed tube and escape pipe are equipped with for the two-port valve in parallel with nitrogen pipeline (5);
Described sample cell (2) is in parallel with nitrogen pipeline (5), and sample cell (2) is provided with feed pipe and discharge nozzle, and described feed pipe and discharge nozzle are equipped with for the two-port valve in parallel with nitrogen pipeline (5);
Described process bottle (3) is connected with nitrogen pipeline (5), process bottle (3) is provided with charging aperture and discharging opening, described charging aperture is positioned at the bottom of process bottle (3), and described discharging opening is positioned at the top of process bottle (3).
2. according to claim 1 for detect industrial germanium tetrachloride early stage process, sampler, it is characterized in that: the inlet end of described nitrogen pipeline (5) is provided with the valve (6) for controlling nitrogen flow.
3. according to claim 1 for detect industrial germanium tetrachloride early stage process, sampler, it is characterized in that: the mouth of pipe of the draft tube in described germanium tetrachloride bottle for material (1) is positioned at the top of germanium tetrachloride bottle for material (1).
4. according to claim 1 for detect industrial germanium tetrachloride early stage process, sampler, it is characterized in that: the mouth of pipe of the feed tube in described receiving bottle (4) is positioned at the bottom of receiving bottle (4).
CN201420509809.2U 2014-09-05 2014-09-05 For detecting process in early stage, the sampler of industrial germanium tetrachloride Active CN204064765U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104236973A (en) * 2014-09-05 2014-12-24 武汉云晶飞光纤材料有限公司 Pre-treatment and sampling device and method for detecting industrial germanium tetrachloride
CN106153565A (en) * 2016-07-29 2016-11-23 攀钢集团攀枝花钢铁研究院有限公司 Measure TiOCl in titanium tetrachloride2the apparatus and method of content

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104236973A (en) * 2014-09-05 2014-12-24 武汉云晶飞光纤材料有限公司 Pre-treatment and sampling device and method for detecting industrial germanium tetrachloride
CN106153565A (en) * 2016-07-29 2016-11-23 攀钢集团攀枝花钢铁研究院有限公司 Measure TiOCl in titanium tetrachloride2the apparatus and method of content

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