CN105921191A - Crucible for measuring contents of fluorine and chloride in biomass - Google Patents
Crucible for measuring contents of fluorine and chloride in biomass Download PDFInfo
- Publication number
- CN105921191A CN105921191A CN201610464173.8A CN201610464173A CN105921191A CN 105921191 A CN105921191 A CN 105921191A CN 201610464173 A CN201610464173 A CN 201610464173A CN 105921191 A CN105921191 A CN 105921191A
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- China
- Prior art keywords
- crucible
- sample stage
- sample
- crucible body
- support bar
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/04—Crucibles
Abstract
The invention provides a crucible for measuring contents of fluorine and chloride in biomass. The crucible comprises a crucible body, a support rod and a sample table, wherein the crucible body is provided with a bottom part, a side wall and an opening; the support rod is positioned in the crucible body and is vertical to the bottom part of the crucible body; the bottom part of the support rod is connected with the bottom part of the crucible body; the sample table is connected with the support rod, and is parallel with the bottom part of the crucible body; the sample table is of a hole-shaped structure. Compared with the prior art, the crucible has the advantages that the sample table with the hole-shaped structure is arranged in the crucible; under the condition of high-temperature reaction, the air can form air flow from bottom to top in the crucible, the high-temperature reaction is sufficient, and the condition of insufficient high-temperature reaction of the sample is solved.
Description
Technical field
The invention belongs to chemical devices technical field, particularly relate to a kind of fluorine, chlorinity in biomass
The crucible measured.
Background technology
Biomass energy is the form of energy that solar energy is stored in biomass with chemical energy form, is that one can
The renewable sources of energy, are also unique reproducible carbon sources simultaneously.Biomass energy has environmental friendliness and reproducible
Double attribute is it is considered to be maximum in the world potential Renewable Energy Resources.Along with countries in the world more
Pay attention to the problem such as environmental conservation, climate change and energy shortage, actively formulate new energy development strategy,
Regulation and policy, Renewable Energy Development has become the inexorable trend of world development.So, biomass energy
Exploitation oneself is extremely urgent, its irreplaceable advantage is by the common concern of society.China issues
Cloth " People's Republic of China's Renewable Energy Law ", and implement the preferential rate for incorporation into the power network of biomass power generation
Etc. relevant supporting policy, existing 87 of biomass scale power generation project, total installation of generating capacity is 2,200,000 kilowatts,
" planning of regenerative resource Long-and Medium-term Development " announced determines the year two thousand twenty biomass power plant installed capacity 3000
The developing goal of ten thousand kW, it follows that biomass are as a kind of renewable sources of energy, the value in its future
It is widely recognized, to the accurate detection of harmful components in biomass, is that following rational exploitation and utilization is raw
The basis of material and guarantee.
Both at home and abroad certain research is all carried out in chlorine, fluorine content measurement in biomass, it is determined that some are surveyed
Determine method, such as high-temperature combustion hydrolytic-potentiometric titration, sulfur hydracid potassium titrimetry, colorimetry, liquid phase color
Spectrometry, gas chromatography, the chromatography of ions etc..Wherein, the chromatography of ions is due to measurement accuracy Gao Erguang
General employing, as external European Union has promulgated " solid biomass fuel-solubilized C1, Na, K content measuring side
Method (BS EN 15105:2011) ".The mensuration key of chlorine, Oil repellent in ion-chromatographic determination biomass
Being that sample early stage is decomposed, will chlorine in sample, fluorine extracting to detect with chromatography of ions, wherein
A kind of method that early stage is decomposed is that sample is cleared up process, chemical drugs and biomass will be put in earthenware
High temperature sintering in crucible so that it is pyroreaction, thus the chlorine in biology, fluorine are converted into water-soluble salt,
Detecting with chromatography of ions, therefore crucible is that High-temperature Digestion is for containing the vitals of sample again.Commonly use
Crucible capacity is 50ml, often occurs Specimen eliminating thorough in using, and detonation, splash phenomena are serious,
This can have extreme influence to chlorine, the accuracy of fluorine detection in biology.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide one to be conducive to pyroreaction abundant
The crucible of fluorine, chloride content determination in biomass.
The invention provides a kind of crucible, including:
Crucible body, described crucible body includes bottom, sidewall and opening；
It is positioned at described crucible body, is perpendicular to the support bar bottom crucible body, and described support bar
Bottom is connected with the bottom of described crucible body；
It is connected on described support bar, and the sample stage parallel with the bottom of crucible body, described sample stage
There is cavernous structure.
Preferably, the base diameter of described crucible body is more than the diameter of crucible body opening.
Preferably, described sample stage is made up of metal gauze.
Preferably, the aperture of the cavernous structure of described sample stage is 0.1～1mm.
Preferably, described sample stage includes the fan-shaped sample stage of 2 or more than 2.
Preferably, the central angle of described fan-shaped sample stage is 20 °～160 °.
Preferably, the connected mode of described sample stage and support bar, for being flexibly connected, makes the described sample stage can
Rotate around support bar.
Preferably, described crucible includes 1～5 layer of sample stage.
Preferably, described crucible includes 2～3 layers of sample stage.
The invention provides a kind of crucible of fluorine, chloride content determination in biomass, including crucible body,
Described crucible body includes bottom, sidewall and opening；It is positioned at described crucible body, is perpendicular to crucible originally
Support bar bottom body, and the bottom of described support bar is connected with the bottom of described crucible body；Connect
On described support bar, and the sample stage parallel with the bottom of crucible body, described sample stage has poroid
Structure.Compared with prior art, in the crucible that the present invention provides, it is provided with the sample stage with cavernous structure,
During pyroreaction, air can form air stream in crucible from bottom to up, so that pyroreaction is abundant,
Solve high-temperature sample and react halfway situation.
Accompanying drawing explanation
The front elevation of the Fig. 1 nickel crucible for providing in the embodiment of the present invention 1；
The normal cross-section schematic diagram of the Fig. 2 nickel crucible for providing in the embodiment of the present invention 1；
The normal cross-section image figure of the Fig. 3 nickel crucible for providing in the embodiment of the present invention 1；
The side generalized section of the Fig. 4 nickel crucible for providing in the embodiment of the present invention 1；
The side section image figure of the Fig. 5 nickel crucible for providing in the embodiment of the present invention 1；
The schematic top plan view of the Fig. 6 nickel crucible for providing in the embodiment of the present invention 1；
The aerial view of the Fig. 7 nickel crucible for providing in the embodiment of the present invention 1；
Fig. 8 is the plan structure schematic diagram of the umbrella-type sample stage of the nickel crucible of offer in the embodiment of the present invention 1；
The structural representation of the Fig. 9 commercially available ship type crucible for providing in comparative example 1 of the present invention；
The structural representation of the Figure 10 commercially available bowl-type crucible for providing in comparative example 2 of the present invention；
The photo of the Figure 11 commercially available bowl-type crucible for providing in comparative example 2 of the present invention.
Detailed description of the invention
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Describe, it is clear that described embodiment is only a part of embodiment of the present invention rather than all wholely
Embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creativeness
The every other embodiment obtained under work premise, broadly falls into the scope of protection of the invention.
The invention provides a kind of crucible of fluorine, chloride content determination in biomass, including: crucible is originally
Body, described crucible body includes bottom, sidewall and opening；It is positioned at described crucible body, is perpendicular to earthenware
The support bar of crucible body bottom portion, and the bottom of described support bar is connected with the bottom of described crucible body；
It is connected on described support bar, and the sample stage parallel with the bottom of crucible body, described sample stage has
Cavernous structure.
It is provided with the sample stage with cavernous structure, during pyroreaction, air in the crucible that the present invention provides
Air stream can be formed in crucible from bottom to up, so that pyroreaction is abundant, solve high-temperature sample
React halfway situation.
The crucible structure that heretofore described crucible body is well known to those skilled in the art, there is no spy
Different restriction, including bottom, sidewall and opening；The material of described crucible body is those skilled in the art
Known to crucible material, there is no special restriction, owing to the crucible of the present invention mainly uses alkali fusion side
Method carries out pre-treatment to sample, therefore can not use irony, porcelain, corundum, platinum, can use graphite,
The material such as nickel, gold, preferably nickel crucible, graphite crucible or gold crucible；In the present invention, described crucible
The base diameter of body is preferably greater than the diameter of crucible body opening, and the most whole crucible body is base diameter
Flat bowl-type structure more than opening diameter.Using this structure that sample can be made when pyroreaction, air can
Form air stream with ecto-entad so that chemical reaction is abundant, simultaneously bottom can facilitate crucible for plane
It is positioned in table top or high temperature furnace.
Described support bar is positioned at crucible body, is perpendicular to bottom crucible body, and the end of described support bar
Portion is connected with the bottom of described crucible body, at the bottom of the bottom of the most described support bar and described crucible body
The middle position in portion is connected；The material that the material of described support bar is well known to those skilled in the art,
There is no particular restriction, the present invention is preferably metal bar.
According to the present invention, described support bar connects and has sample stage, and described sample stage is with described crucible originally
The bottom of body is parallel, and described sample stage has cavernous structure；The aperture of described cavernous structure is 0.1～1mm,
More preferably 0.2～0.8mm, it is further preferably 0.3～0.7mm, is further preferably 0.4～0.6mm, most preferably
For 0.5mm；The material that the material of described sample stage is well known to those skilled in the art, it is special to there is no
Restriction, the present invention is preferably made up of metal gauze.
Described sample stage preferably includes the fan-shaped sample stage of 2 or more than 2, more preferably includes 2～6
Fan-shaped sample stage, further preferably includes 3～5 fan-shaped sample stages, most preferably includes 4；Described sector
The central angle of sample stage is preferably 20 °～160 °, more preferably 30 °～150 °, is further preferably 30 °～100 °,
It is further preferably 30 °～80 °, most preferably 40 °～60 °；In the present invention, can between described fan-shaped sample stage
Contact with each other, it is possible to do not contact, there is no special restriction, do not contact between the most described fan-shaped sample stage；
Placing sample for convenience, described sample stage is preferably with the connected mode of support bar and is flexibly connected, and makes institute
State sample stage to rotate around support bar, receive together so that described fan-shaped sample stage can merge, work as sample
Multiple fan-shaped sample stage can be opened time many, can only open 1～2 fan-shaped sample stage therein when sample is few；
For making the sample on sample stage be heated evenly, the most described sample stage does not contacts with the sidewall of crucible body,
Leave gap.
In the present invention, in order to make full use of the inner space of crucible, and also to avoid the heap of sample
Long-pending problem, described crucible preferably includes 1～5 layer of sample stage, more preferably includes 2～4 layers of sample stage, more excellent
Choosing includes 2～3 layers of sample stage, most preferably includes 3 layers of sample stage；Every layer of sample stage includes 2 or 2
Above fan-shaped sample stage, described fan-shaped sample stage is same as above, does not repeats them here.Multilamellar in crucible
Sample stage collectively forms the structure of multi-layer umbrella style sample platform, solves sample stacking together, and air is difficult to
Enter sample interior thus the unfavorable phenomenon such as detonation, splashing easily occurs, it is ensured that high-temperature sample course of reaction is suitable
Profit, improves the accuracy of late detection.
In order to further illustrate the present invention, a kind of crucible provided the present invention below in conjunction with embodiment is carried out
Describe in detail.
Reagent used in following example is commercially available.
Embodiment 1
1.1 provide nickel crucible, and described crucible body is flat bowl-type, and base diameter is more than top diameter,
Crucible body is Ni substrate crucible, is inside provided with multi-layer rotating umbrella-type sample stage, uses metal gauze establishment,
Aperture about 0.5mm.There is a metal bar crucible inner bottom part middle position as support bar, multi-layer umbrella style product
Platform is connected on metal bar, and multi-layer umbrella style sample platform is divided into three layers, is positioned at the internal position, upper, middle and lower of crucible
Put, between multi-layer umbrella style sample platform and crucible internal walls, leave gap.Every layer of umbrella-type sample stage is symmetrical four
Block curved metal silk screen, its central angle is 45 °, and four pieces of curved metal silk screens can rotate with intermetallic metal rod,
And can reclaim and combine.The front elevation of described crucible is as shown in Figure 1；The normal cross-section of described crucible
Schematic diagram is as shown in Figure 2；The normal cross-section image figure of described crucible is as shown in Figure 3；The side of described crucible is cutd open
As shown in Figure 4, wherein 1 is the sidewall of crucible body to face schematic diagram, and 2 is support bar, and 3～5 is fan-shaped sample
Sample platform；The side section image figure of described crucible is as shown in Figure 5；The schematic top plan view of described crucible such as Fig. 6
Shown in, wherein 1 is the sidewall of crucible body, and 3～5 is fan-shaped sample stage；The aerial view of described crucible such as figure
Shown in 7；The plan structure schematic diagram of described umbrella-type sample stage is as shown in Figure 8.
1.2 weigh a certain amount of biomass standard substance sample (GBW07603), are placed on 1.1 offers
Nickel crucible in.Sample is placed KOH or the NAOH medicine of 1g；Then crucible is put into high temperature
Carrying out high-temp combustion in stove, crucible is taken out after terminating by reaction, lets cool.20mL water is added in crucible,
Dissolved samples, is transferred to this solution in 100mL volumetric flask, washs crucible for several times with 20mL moisture,
It is incorporated in volumetric flask, is settled to scale with water, mixing, detect chlorine, Oil repellent in sample with chromatography of ions,
Obtain the results are shown in Table 1.
Comparative example 1
The form of 1.1 commercially available crucibles is generally divided into ship type and bowl-type, and wherein the structural representation of ship type crucible is such as
Shown in Fig. 9.
1.2 weigh a certain amount of biomass standard substance sample (GBW07603), are placed on 1.1 offers
Nickel crucible in.Sample is placed KOH or the NAOH medicine of 1g；Then crucible is put into high temperature
Carrying out high-temp combustion in stove, crucible is taken out after terminating by reaction, lets cool.20mL water is added in crucible,
Dissolved samples, is transferred to this solution in 100mL volumetric flask, washs crucible for several times with 20mL moisture,
It is incorporated in volumetric flask, is settled to scale with water, mixing, detect chlorine, Oil repellent in sample with chromatography of ions,
Obtain the results are shown in Table 1.
Comparative example 2
The form of 2.1 commercially available crucibles is generally divided into ship type and bowl-type, and wherein the structural representation of ship type crucible is such as
Shown in Figure 10, photo is as shown in figure 11.
2.2 weigh a certain amount of biomass standard substance sample (GBW07603), are placed on 2.1 offers
Nickel crucible in.Sample is placed KOH or the NAOH medicine of 1g；Then crucible is put into high temperature
Carrying out high-temp combustion in stove, crucible is taken out after terminating by reaction, lets cool.20mL water is added in crucible,
Dissolved samples, is transferred to this solution in 100mL volumetric flask, washs crucible for several times with 20mL moisture,
It is incorporated in volumetric flask, is settled to scale with water, mixing, detect chlorine, Oil repellent in sample with chromatography of ions,
Obtain the results are shown in Table 1.
Chlorine, Oil repellent testing result in table 1 sample
Biomass standard substance sample (GBW07603) fluorine standard value is 23ug/g ± 4ug/g, chlorine standard
Value is 1.92%.
As can be seen from the table, use crucible of the present invention that biomass standard substance carries out pyroreaction thorough,
Completely, relative deviation is minimum, and the Oil repellent of mensuration is in standard value range of uncertainty, and other crucibles
Endogenous substance standard substance pyroreaction is incomplete, so that the Oil repellent relative deviation measured is relatively big, and
Measured value is well below standard value lower limit.The sample chloride content determination result phase that the application present invention measures simultaneously
Minimum (0.52%), well below other crucible sample determination relative deviations to deviation.
Above example and comparative example have absolutely proved and present invention can ensure that high-temperature sample chemical reaction fills
Point, solve the not thorough situation of high-temperature sample reaction；Solve high-temperature sample reaction time be susceptible to detonation,
The unfavorable phenomenons such as splashing, it is ensured that sample pretreatment process is smooth, improve chlorine in biology, fluorine detection accurate
Property.
Claims (9)
1. fluorine, the crucible of chloride content determination in biomass, it is characterised in that including:
Crucible body, described crucible body includes bottom, sidewall and opening；
It is positioned at described crucible body, is perpendicular to the support bar bottom crucible body, and described support bar
Bottom is connected with the bottom of described crucible body；
It is connected on described support bar, and the sample stage parallel with the bottom of crucible body, described sample stage
There is cavernous structure.
Crucible the most according to claim 1, it is characterised in that the base diameter of described crucible body
Diameter more than crucible body opening.
Crucible the most according to claim 1, it is characterised in that described sample stage is by metal gauze system
Become.
Crucible the most according to claim 1, it is characterised in that the cavernous structure of described sample stage
Aperture is 0.1～1mm.
Crucible the most according to claim 1, it is characterised in that described sample stage includes 2 or 2
Individual above fan-shaped sample stage.
Crucible the most according to claim 5, it is characterised in that the central angle of described fan-shaped sample stage
It it is 20 °～160 °.
Crucible the most according to claim 1, it is characterised in that described sample stage and the company of support bar
The mode that connects, for being flexibly connected, makes described sample stage can rotate around support bar.
Crucible the most according to claim 1, it is characterised in that described crucible includes 1～5 layer of sample
Platform.
Crucible the most according to claim 1, it is characterised in that described crucible includes 2～3 layers of sample
Platform.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610464173.8A CN105921191A (en) | 2016-06-21 | 2016-06-21 | Crucible for measuring contents of fluorine and chloride in biomass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610464173.8A CN105921191A (en) | 2016-06-21 | 2016-06-21 | Crucible for measuring contents of fluorine and chloride in biomass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105921191A true CN105921191A (en) | 2016-09-07 |
Family
ID=56831137
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610464173.8A Pending CN105921191A (en) | 2016-06-21 | 2016-06-21 | Crucible for measuring contents of fluorine and chloride in biomass |
Country Status (1)
| Country | Link |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201959808U (en) * | 2011-01-10 | 2011-09-07 | 刘瑄 | Small-size crucible for combustion test |
| CN202803270U (en) * | 2012-10-21 | 2013-03-20 | 刘婵娟 | Crucible |
| JP3188484U (en) * | 2013-11-08 | 2014-01-23 | 東京科学株式会社 | Adapter for small sample processing for high frequency equipment |
| CN203615736U (en) * | 2013-11-14 | 2014-05-28 | 长沙理工大学 | Novel multifunctional crucible |
| CN103938160A (en) * | 2014-03-06 | 2014-07-23 | 京东方科技集团股份有限公司 | Crucible |
| CN203764975U (en) * | 2014-03-07 | 2014-08-13 | 贵州中航聚电科技有限公司 | Hole-type multi-layer tantalum crucible |
| CN104959175A (en) * | 2015-05-20 | 2015-10-07 | 哈尔滨工程大学 | Crucible suitable for preparation of materials with hierarchical porous structures |
| CN205269698U (en) * | 2015-12-22 | 2016-06-01 | 江苏国测检测技术有限公司 | Polytetrafluoroethylene crucible |
-
2016
- 2016-06-21 CN CN201610464173.8A patent/CN105921191A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201959808U (en) * | 2011-01-10 | 2011-09-07 | 刘瑄 | Small-size crucible for combustion test |
| CN202803270U (en) * | 2012-10-21 | 2013-03-20 | 刘婵娟 | Crucible |
| JP3188484U (en) * | 2013-11-08 | 2014-01-23 | 東京科学株式会社 | Adapter for small sample processing for high frequency equipment |
| CN203615736U (en) * | 2013-11-14 | 2014-05-28 | 长沙理工大学 | Novel multifunctional crucible |
| CN103938160A (en) * | 2014-03-06 | 2014-07-23 | 京东方科技集团股份有限公司 | Crucible |
| CN203764975U (en) * | 2014-03-07 | 2014-08-13 | 贵州中航聚电科技有限公司 | Hole-type multi-layer tantalum crucible |
| CN104959175A (en) * | 2015-05-20 | 2015-10-07 | 哈尔滨工程大学 | Crucible suitable for preparation of materials with hierarchical porous structures |
| CN205269698U (en) * | 2015-12-22 | 2016-06-01 | 江苏国测检测技术有限公司 | Polytetrafluoroethylene crucible |
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Application publication date: 20160907 |
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