CN105203385A - Sample dissolution device resistant to hydrofluoric acid and use method - Google Patents

Sample dissolution device resistant to hydrofluoric acid and use method Download PDF

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Publication number
CN105203385A
CN105203385A CN201510743705.7A CN201510743705A CN105203385A CN 105203385 A CN105203385 A CN 105203385A CN 201510743705 A CN201510743705 A CN 201510743705A CN 105203385 A CN105203385 A CN 105203385A
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China
Prior art keywords
molten
valve
sampling device
hydrofluoric acid
absorption cell
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CN201510743705.7A
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Chinese (zh)
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CN105203385B (en
Inventor
徐汝钦
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CHINA SHIPBUILDING INDUSTRY SPECIAL EQUIPMENT CO LTD
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CHINA SHIPBUILDING INDUSTRY SPECIAL EQUIPMENT CO LTD
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Priority to CN201510743705.7A priority Critical patent/CN105203385B/en
Publication of CN105203385A publication Critical patent/CN105203385A/en
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Abstract

The invention relates to a sample dissolution device resistant to hydrofluoric acid and a use method. According to the technical scheme, the upper end of a sample dissolution container (3) is embedded in an annular boss at the bottom of an absorption tank (2), and the lower end of a non-return pressure release valve (1) is put in an annular groove (10) in the bottom of the absorption tank (2); the sample dissolution container (3) is a short cylindrical container; the opening end of a tank body of the absorption tank (2) is integrally connected with an upper plane of the tank bottom of the absorption tank (2), a mounting hole (8) is formed in the closed end of the tank body, the non-return pressure release valve (1) is put in the absorption tank (2) from the mounting hole (8), and a vent hole (9) is formed in the center of the tank bottom; a valve element (6) of the non-return pressure release valve (1) is concentrically placed in a valve body (5), and waste gas discharge ports (7) are symmetrically formed in the edge of the valve body (5); a horizontal valve channel is formed in the upper end surface of a cylinder of the valve element (6) in the diameter direction, a vertical valve channel is formed upwards in the lower end surface of the cylinder along the center line, and the vertical valve channel is communicated with the horizontal valve channel. The sample dissolution device has the characteristics of simple structure, convenience in operation, reduction of the use amount of acid, low cost, capability of collecting waste acid and environmental protection.

Description

A kind of molten sampling device of hydrofluoric acid resistant and using method
Technical field
The invention belongs to the molten sampling device technical field of sample.Be specifically related to a kind of molten sampling device and using method of hydrofluoric acid resistant.
Background technology
At present, the molten sample acid of hydrofluoric acid containing is widely used in the sample of dissolution process containing silicon dioxide, elemental silicon and silicate, and the sample of dissolving is used for chemical composition and measures.Typical application is as the mensuration (YB/T175-2000) etc. of silit in conventional abrasive Wilicon carbide analytical approach (GB/T3045-2003), emery.Traditional acid-soluble sample vessel are the container opening wide or be with one-way exhaust gland bonnet (as lid formula funnel).Acid dissolution generally needs to maintain certain acidity and time, and in heating acid dissolution, a large amount of acid evaporations, not only makes the utilization ratio of acid reduce and discharge a large amount of spent acid gas simultaneously.When adding a cover formula funnel sealing dissolving, after stopping heating or stopping exhaust, sealing liquid meeting resorption; If when stoping resorption, the negative pressure that molten sampling device exists makes gland bonnet be difficult to open.
Said method problem is: 1, sour velocity of evaporation is fast at ambient pressure; 2, the consumption maintaining the required acid of certain reaction time is large, and waste is large; 3, the spent acid of evaporation directly enters air, difficult treatment.
Summary of the invention
The present invention is intended to overcome prior art defect, and object is to provide that simple, easy to operate, the sour consumption of a kind of structure is few, cost is low and is easy to the molten sampling device of hydrofluoric acid resistant and the using method of the process of spent acid gas collection.
For achieving the above object, the technical solution used in the present invention is: described molten sampling device is made up of non-return blowdown valve, absorption cell and molten sample container.The upper end of molten sample container is mutually embedding with the annular boss bottom absorption cell, and the lower end of non-return blowdown valve is inserted in the ring groove bottom absorption cell, and the center line of the center line of non-return blowdown valve, the center line of absorption cell and molten sample container is same straight line.
Molten sample container is short cylinder shape container, and described short cylinder shape container refers to that described cylinder heights is less than the container of drum diameter.
Absorption cell is made up of bottom land and cell body.Bottom land is in the form of annular discs, and the outer rim of bottom land lower plane is annular boss, and the internal diameter of annular boss is identical with the nominal size of molten sample its external diameter, and the center position of bottom land is provided with air hole, and the upper plane of bottom land is provided with ring groove concentrically; Cell body is identical with the shape of molten sample container, and the openend of cell body and the upper plane of bottom land are linked as entirety, and upward, the end face of blind end has mounting hole to the blind end of cell body.Non-return blowdown valve is inserted in absorption cell from described mounting hole.
Non-return blowdown valve is made up of valve body and spool, inserts in valve body spool is concentricity line.Cylindrically, down, the edge of nozzle has " U " shape or square exhaust vent to cylinder nozzle to valve body symmetrically, and the center position at the bottom of cylinder cylinder is provided with spool bore, and the valve rod of spool passes from described spool bore.Spool is the entirety of right cylinder and valve rod composition, be provided with valve rod cylindrical upper surface is concentricity line, diametrically having horizontal valve road near cylindrical upper end surface, cylindrical lower surface centrally alignment have vertical valve road, and described vertical valve road communicates with horizontal valve road.
The diameter d of described air hole 1for described vertical valve road diameter d 22 ~ 3 times.
The gap of described valve body and valve core chamber is 0.1 ~ 2mm.
The material of described absorption cell and molten sample container is teflon.
The volume of described absorption cell is 5 ~ 100mL.
The using method of the molten sampling device of described hydrofluoric acid resistant is: sample is put into molten sample container, adds the molten sample acid of 1 ~ 50ml, cover the absorption cell that non-return blowdown valve is housed, then add the absorbing liquid of 1 ~ 50ml to absorption cell in molten sample container; Then move on well heater by the molten sampling device of hydrofluoric acid resistant, heating, until course of dissolution completes; Take off the molten sampling device of hydrofluoric acid resistant, cooling, take out the product processed.
To be hydrofluorite mix with more than one in following acid in described molten sample acid, and described following acid is nitric acid, hydrochloric acid, perchloric acid and sulfuric acid.
Described absorbing liquid is the one in water, lime water and sodium hydroxide solution.
Owing to adopting technique scheme, the present invention compared with prior art, has following good effect:
1, this device is only made up of non-return blowdown valve, absorption cell and molten sample container, and structure is simple; In addition, the annular boss internal diameter of absorption cell is identical with the external diameter of molten sample container, and tension force synergy when relying on the gravity of absorption cell, non-return blowdown valve and absorbing liquid and molten sample container to be heated reaches sealing, and pressure limiting is vented, without the need to seal.
2, this device is when completing when course of dissolution or molten sample container stops heating, pressure drop in molten sample container, absorbing liquid liquid level in absorption cell declines, the buoyancy that spool is subject to reduces, spool falls automatically, and closed waste gas arranges its gas port, is communicated with air by vertical valve road, pressure release, thus easy to operate.
3, this device is under the effect of non-return blowdown valve, and acid vapor is subject to the pressure of absorbing liquid, and molten sample acid can reflux in molten sample container, and sour velocity of evaporation is slow, therefore can reduce sour consumption, reduces costs.
4, when the molten sample container of this device is heated, spool upwards holds out against by acid vapor, and steam enters absorption cell from waste gas round, therefore can collect waste gas and be conducive to environmental protection.
Therefore, the present invention has the advantages that simple, easy to operate, the sour consumption of structure reduces, cost is low, can collect spent acid and environmental protection.
Accompanying drawing explanation
Fig. 1 is a kind of structural representation of the present invention;
Fig. 2 is the structural representation of non-return blowdown valve 1 in Fig. 1;
Fig. 3 is the structural representation of absorption cell 2 in Fig. 1;
Fig. 4 is the use schematic diagram of Fig. 1.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described further, the restriction not to its protection domain.
embodiment 1
A kind of molten sampling device of hydrofluoric acid resistant and using method.As shown in Figure 1, described molten sampling device is made up of non-return blowdown valve 1, absorption cell 2 and molten sample container 3.The upper end of molten sample container 3 is mutually embedding with the annular boss bottom absorption cell 2, and the lower end of non-return blowdown valve 1 is inserted in the ring groove 10 bottom absorption cell 2, and the center line of the center line of non-return blowdown valve 1, the center line of absorption cell 2 and molten sample container 3 is same straight line.
As shown in Figure 1, molten sample container 3 is short cylinder shape container, and described short cylinder shape container refers to that described cylinder heights is less than the container of drum diameter.
As shown in figures 1 and 3, absorption cell 2 is made up of bottom land and cell body.Bottom land is in the form of annular discs, and the outer rim of bottom land lower plane is annular boss, and the internal diameter of annular boss is identical with the nominal size of molten sample container 3 external diameter, and the center position of bottom land is provided with air hole 9, and the upper plane of bottom land is provided with ring groove 10 concentrically; Cell body is identical with the shape of molten sample container 3, and the openend of cell body and the upper plane of bottom land are linked as entirety, and upward, the end face of blind end has mounting hole 8 to the blind end of cell body.Non-return blowdown valve 1 is inserted in absorption cell 2 from described mounting hole 8.
As depicted in figs. 1 and 2, non-return blowdown valve 1 is made up of valve body 5 and spool 6, inserts in valve body 5 spool 6 is concentricity line.Cylindrically, down, the edge of nozzle has " U " shape or square exhaust vent 7 to cylinder nozzle to valve body 5 symmetrically, and the center position at the bottom of cylinder cylinder is provided with spool bore 4, and the valve rod of spool 6 passes from described spool bore 4.Spool 6 is the entirety of right cylinder and valve rod composition, be provided with valve rod cylindrical upper surface is concentricity line, diametrically having horizontal valve road near cylindrical upper end surface, cylindrical lower surface centrally alignment have vertical valve road, and described vertical valve road communicates with horizontal valve road.
The diameter d of described air hole 9 1for described vertical valve road diameter d 22 ~ 2.5 times.
Gap between described valve body 5 and spool 6 is 1.0 ~ 2mm.
The material of described absorption cell 2 and molten sample container 3 is teflon.
The volume of described absorption cell 2 is 60 ~ 100mL.
The using method of the molten sampling device of described hydrofluoric acid resistant is as shown in Figure 4: sample 11 is put into molten sample container 3, the molten sample acid 12 of 30 ~ 50ml is added in molten sample container 3, cover the absorption cell 2 that non-return blowdown valve 1 is housed, then add the absorbing liquid 13 of 30 ~ 50ml to absorption cell 2; Then move on well heater by the molten sampling device of hydrofluoric acid resistant, heating, until course of dissolution completes; Take off the molten sampling device of hydrofluoric acid resistant, cooling, take out the product processed.
Described molten sample acid 12 is the potpourri of hydrofluorite and nitric acid.
Described absorbing liquid 13 is water.
embodiment 2
A kind of molten sampling device of hydrofluoric acid resistant and using method.Except following technical parameter, all the other are with embodiment 1:
The diameter d of described air hole 9 1for described vertical valve road diameter d 22.5 ~ 3 times.
Gap between described valve body 5 and spool 6 is 0.1 ~ 1.2mm.
The volume of described absorption cell 2 is 5 ~ 60mL.
In molten sample container 3, add the molten sample acid 12 of 1 ~ 30ml, cover the absorption cell 2 that non-return blowdown valve 1 is housed, then add the absorbing liquid 13 of 1 ~ 30ml to absorption cell 2.
To be hydrofluorite mix with more than one in following acid in described molten sample acid 12, and described following acid is hydrochloric acid, perchloric acid and sulfuric acid.
Described absorbing liquid 13 is the one in lime water and sodium hydroxide solution.
This embodiment compared with prior art, has following good effect:
1, this device is only made up of non-return blowdown valve 1, absorption cell 2 and molten sample container 3, and structure is simple; In addition, the annular boss internal diameter of absorption cell 2 is identical with the external diameter of molten sample container 3, and the synergy of tension force when relying on the gravity of absorption cell, non-return blowdown valve and absorbing liquid and molten sample container 3 to be heated reaches sealing, and pressure limiting is vented, without the need to seal.
2, this device is when course of dissolution completes or molten sample container 3 stops heating, pressure drop in molten sample container 3, absorbing liquid liquid level in absorption cell 2 declines, the buoyancy that spool 6 is subject to reduces, spool 6 falls automatically, closes exhaust vent 7, is communicated by vertical valve road with air, pressure release, thus easy to operate.
3, this device is under the effect of non-return blowdown valve 1, and acid vapor is subject to the pressure of absorbing liquid 13, and molten sample acid 12 can reflux in molten sample container 3, and sour velocity of evaporation is slow, therefore can reduce sour consumption, reduces costs.
4, when the molten sample container 3 of this device is by heating, spool 6 upwards holds out against by acid vapor, and steam enters absorption cell 2 from exhaust vent 7, therefore can collect waste gas and be conducive to environmental protection.
Therefore, this embodiment has the advantages that simple, easy to operate, the sour consumption of structure reduces, cost is low, can collect spent acid and environmental protection.

Claims (8)

1. a molten sampling device for hydrofluoric acid resistant, is characterized in that described molten sampling device is made up of non-return blowdown valve (1), absorption cell (2) and molten sample container (3); The upper end of molten sample container (3) is mutually embedding with the annular boss of absorption cell (2) bottom, the lower end of non-return blowdown valve (1) is inserted in the ring groove (10) of absorption cell (2) bottom, and the center line of the center line of non-return blowdown valve (1), the center line of absorption cell (2) and molten sample container (3) is same straight line;
Molten sample container (3) is short cylinder shape container, and described short cylinder shape container refers to that described cylinder heights is less than the container of drum diameter;
Absorption cell (2) is made up of bottom land and cell body; Bottom land is in the form of annular discs, the outer rim of bottom land lower plane is annular boss, the internal diameter of annular boss is identical with the nominal size of molten sample container (3) external diameter, and the center position of bottom land is provided with air hole (9), and the upper plane of bottom land is provided with ring groove (10) concentrically; Cell body is identical with the shape of molten sample container (3), and the openend of cell body and the upper plane of bottom land are linked as entirety, and upward, the end face of blind end has mounting hole (8) to the blind end of cell body; Non-return blowdown valve (1) is inserted in absorption cell (2) from described mounting hole (8);
Non-return blowdown valve (1) is made up of valve body (5) and spool (6), inserts in valve body (5) spool (6) concentricity line; Valve body (5) cylindrically, cylinder nozzle down, the edge of nozzle has " U " shape or square exhaust vent (7) symmetrically, center position at the bottom of cylinder cylinder is provided with spool bore (4), and the valve rod of spool (6) passes from described spool bore (4); The entirety that spool (6) forms for right cylinder and valve rod, be provided with valve rod cylindrical upper surface is concentricity line, horizontal valve road is diametrically being had near cylindrical upper end surface, cylindrical lower surface centrally alignment have vertical valve road, and described vertical valve road communicates with horizontal valve road.
2. the molten sampling device of hydrofluoric acid resistant according to claim 1, is characterized in that the diameter d of described air hole (9) 1for described vertical valve road diameter d 22 ~ 3 times.
3. the molten sampling device of hydrofluoric acid resistant according to claim 1, is characterized in that the gap between described valve body (5) and spool (6) is 0.1 ~ 2mm.
4. the molten sampling device of hydrofluoric acid resistant according to claim 1, is characterized in that the material of described absorption cell (2) and molten sample container (3) is teflon.
5. the molten sampling device of hydrofluoric acid resistant according to claim 1, is characterized in that the volume of described absorption cell (2) is 5 ~ 100mL.
6. the using method of the molten sampling device of a hydrofluoric acid resistant, it is characterized in that described using method is: sample (11) is put into molten sample container (3), the molten sample acid (12) of 1 ~ 50ml is added in molten sample container (3), cover the absorption cell (2) that non-return blowdown valve (1) is housed, then add the absorbing liquid (13) of 1 ~ 50ml to absorption cell (2); Then move on well heater by the molten sampling device of hydrofluoric acid resistant, heating, until course of dissolution completes; Take off the molten sampling device of hydrofluoric acid resistant, cooling, take out the product processed.
7. the using method of the molten sampling device of hydrofluoric acid resistant according to claim 6, it is characterized in that described molten sample acid (12) mixes with more than one in following acid for hydrofluorite, described following acid is nitric acid, hydrochloric acid, perchloric acid and sulfuric acid.
8. the using method of the molten sampling device of hydrofluoric acid resistant according to claim 6, is characterized in that described absorbing liquid (13) is water, one in lime water and sodium hydroxide solution.
CN201510743705.7A 2015-11-05 2015-11-05 The molten sampling device and application method of a kind of hydrofluoric acid resistant Expired - Fee Related CN105203385B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107768274A (en) * 2016-08-22 2018-03-06 盛美半导体设备(上海)有限公司 A kind of mixed liquid bath

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CN202330139U (en) * 2011-11-29 2012-07-11 孙文军 Efficient sample-dissolving equipment
CN103245553A (en) * 2013-05-24 2013-08-14 中国热带农业科学院分析测试中心 Environment-friendly high-efficiency acid reflux collection-type element analysis sample digestion method
CN205091180U (en) * 2015-11-05 2016-03-16 中船重工特种设备有限责任公司 A device of nai hydrofluoric acid for dissolving sample

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Publication number Priority date Publication date Assignee Title
SU1652214A1 (en) * 1989-06-19 1991-05-30 Куйбышевский политехнический институт им.В.В.Куйбышева Breather of tank for volatile liquids
US5345066A (en) * 1991-03-18 1994-09-06 Knapp Guenter Device for heating substances under the development of high pressures in a microwave field
US20040163726A1 (en) * 2002-06-21 2004-08-26 Nanaji Seifollah S. Underground storage tank vapor pressure equalizer
CN201023797Y (en) * 2007-01-18 2008-02-20 广东西陇化工有限公司 Closing device of container for loading decomposable or volatile matter
CN201148262Y (en) * 2008-01-29 2008-11-12 冀州市中意复合材料有限公司 Acid container respirator
CN201464272U (en) * 2009-06-23 2010-05-12 郑啟光 High-temperature and high-pressure resistant anti-leak digestion sample dissolver
CN201795268U (en) * 2010-03-24 2011-04-13 孔令石 Piston type leak-proof gas valve for gas liquor discharge
CN202107249U (en) * 2011-06-21 2012-01-11 李世强 Liquid division type hydraulic relief valve
CN202330139U (en) * 2011-11-29 2012-07-11 孙文军 Efficient sample-dissolving equipment
CN103245553A (en) * 2013-05-24 2013-08-14 中国热带农业科学院分析测试中心 Environment-friendly high-efficiency acid reflux collection-type element analysis sample digestion method
CN205091180U (en) * 2015-11-05 2016-03-16 中船重工特种设备有限责任公司 A device of nai hydrofluoric acid for dissolving sample

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107768274A (en) * 2016-08-22 2018-03-06 盛美半导体设备(上海)有限公司 A kind of mixed liquid bath

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