CN104849113B - The sample treatment of microwave igniting Oxygen bottle combustion - Google Patents
The sample treatment of microwave igniting Oxygen bottle combustion Download PDFInfo
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- CN104849113B CN104849113B CN201510240510.0A CN201510240510A CN104849113B CN 104849113 B CN104849113 B CN 104849113B CN 201510240510 A CN201510240510 A CN 201510240510A CN 104849113 B CN104849113 B CN 104849113B
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Abstract
The present invention provides the sample treatment that a kind of microwave lights a fire Oxygen bottle combustion, belongs to sample treatment field.Solve existing processing method and need to use filter paper, and Cl chromatography of ions backgrounds it is higher the problem of.This method is that testing sample and microwave absorbing material are placed on combustion carrier, and then combustion carrier is put into Molotov cocktail；Molotov cocktail is oxygenated and closed, Molotov cocktail is then put into progress microwave igniting in microwave oven cavity；After Molotov cocktail all burnt and cooling, injection alkaline absorption solution is absorbed in Molotov cocktail, and then transfer absorbed liquid is to be measured into ultra-clean bottle.The processing method of the present invention replaces filter paper with high-purity microwave absorbing material so that halogen, the background of chlorine especially is lower；Using high purity carbon material as ripple and ignition media is inhaled in sparking mode, so as to realize physics ionization igniting；Meanwhile, microwave power needed for method of the invention is lower, quantity of sample handling increase, sample adaptability are wider.
Description
Technical field
The invention belongs to sample treatment field, and in particular to a kind of sample treatment side of microwave igniting Oxygen bottle combustion
Method.
Background technology
The analysis principle of anion chromatographic technology is：By injecting the desired anion of analysis system in anion-exchange column
Continuous dispensing is carried out between alkaline mobile phase, causes differentiation because of reserve capability difference of the different ions in stationary phase
Migration rate, ultimately forms respective Characteristic chromatographic peak, and is caught with Conductivity detection system, so as to realize qualitative elementary and quantitative
Analysis.Wherein, all samples must be in aqueous solution state before sample introduction analysis, therefore for solid sample, it is necessary to by conjunction
Suitable sample pre-treatments means, the now complexity of sample pre-treatments and its success or failure turn into the whole sample analysis of restriction can be real
The key of existing property and analysis result accuracy.However, due to characteristic and ion chromatography the office in itself of nonmetalloid
It is sex-limited, compared to the metallic element analysis based on ICP-OES/MS technologies, when for organic solid sample analysis, to locating before sample
The limitation of reason is more strict：
Firstly, since the effumability of non-metal kind element, therefore burnt for the most frequently used open high temperature of organic matter decomposition
Burning method is difficult to be applicable.
Secondly, it is widely used based on the Strong oxdiative such as nitric acid, the concentrated sulfuric acid, perchloric acid reagent at high operating temperatures to organic matter
Carrying out the Wet of strong destruction can not equally be applicable in ion chromatography, on the one hand, the risk of vaporization at high temperature loss
Equally exist；On the other hand, there is serious reagent acid ion pollution, cause reagent acid radical anion in itself and adjacent colour
Spectrum anion is difficult to detect.
Compared to developing rapidly for chromatography of ions instrument technology, the development of ion chromatography sample treatment technology has seemed
It is serious delayed, and as the Pinch technology for influenceing it to apply.Up to the present, it is directed to the chromatography of ions in organic solid sample
The sample treatment technology of nonmetalloid analysis has and only a kind of selection：Closed burning/alkali liquor absorption under aerobic conditions, letter
Claim Oxygen bottle combustion technology.
The operating process of conventional Oxygen bottle combustion technology is：SOLID ORGANIC sample is wrapped up with filter paper, and is fixed on and bottle cap phase
On platinum filament combustion head even, light, and be put at once in the closed Molotov cocktail of oxygenation immediately, now target analytes Elemental combustion
It is decomposed into corresponding hydride such as HCl or oxide such as SO2, and C, H, O in Matrix Composition are converted into and do not influence chromatogram to detect
CO2And H2O, the alkaline absorption solution that bottom of bottle layer is burned together with analyte absorbs.
Conventional Oxygen bottle combustion technology is widely used because simple to operate, economical, but simultaneously because is difficult to the Technical Board overcome
It is sex-limited, analyze application effect critical constraints：
1st, poor air-tightness, causes the accuracy and precision of quantitative analysis results out of control；
2nd, quantity of sample handling is low；
3rd, from the seriously polluted of combustion carrier, chromatogram background is high, is not suitable for micro-example or super low loading sample point
Analysis；
4th, the complete artificial operation of single sample processing can only be carried out every time, be not suitable for batch samples analysis.
For problem above, domestic and international researcher has carried out substantial amounts of have tried to.It has studied based on internal contact formula
Spark ignition replaces the outer naked light of bottle to ignite, this method sample that ignites using metallic resistance silk circuit fusing generation electric spark,
Sample combustion carrier is usual inertia silica dish.This method compares conventional Oxygen bottle combustion technology and solves closed problem, while right
Specific sample, has given up the use of filter paper.It is disadvantageous in that electrode ignition header structure is complicated, is not easy to clean and be easily caused
Cross pollution；The metal ion pollution from electrode material and resistance wire is easily produced, is unfavorable for subsequent ion chromatography；And
And because electric discharge belongs to the electric discharge of moment (Millisecond) office point, when sample contact point is not more fire retardant in striking point, or sample,
Loss of ignition rate is than larger, it is often necessary to repeat.
Contactless based on light radiation that Jia Lian companies of the U.S. are proposed a set of commercialization lights Oxygen bottle combustion device, its
Strong light is produced using high-power tungsten lamp, and the platinum basket of carrying sample is radiated at after line focus and sample is lighted.The ignition method is big
Big to improve ignition success rate, igniter is simple, is difficult by outside contamination.Shortcoming is the expensive (country's quotation of instrument price
100000 RMB), and the expensive high-power tungsten lamp of core can be because using and rapid deterioration for a long time；Firing temperature relatively low (300
Below degree), the duration of ignition is longer, is especially difficult to be applied to high-flash sample analysis；In addition, the device can only once carry out it is single
The processing of sample.
With the appearance of microwave technology, someone has developed a kind of noncontact igniting Oxygen bottle combustion based on microwave technology newly side
Method, the microwave burning technology of the thought source of its core in inorganic solid phase synthesis：Micro high concentration NH4NO3Solution is added dropwise suitable
Measure on filter paper, sample is in close contact with filter paper.Under microwave irradiation, electrolyte solution causes because absorbing microwave and steep temperature rise
NH4NO3Decompose and produce microexplosion, and then ignite filter paper and sample.The technology is because of novelty, suitable instrumentation operation and Multi-example
Processing simultaneously and receive highests attention, statistics shows that the analysis application report over nearly 5 years on the technology amounts to 29, and
And there are 5 to be published on Anal.Chem. [1-5].But the newest paper being published according to 2013 on Anal.Chem. is shown
[1], the technology is developed so far does not significantly improve in the sparking mode of core, and still need use filter paper, it is higher
Cl chromatography of ions backgrounds are inevitable.
The content of the invention
The invention aims to solve existing processing method to need to use filter paper, and Cl chromatography of ions backgrounds are higher
The problem of, and the sample treatment that a kind of microwave lights a fire Oxygen bottle combustion is provided.
The present invention provides the sample treatment that a kind of microwave lights a fire Oxygen bottle combustion, and this method includes：
Step one：Testing sample and microwave absorbing material are placed on combustion carrier, combustion carrier is then put into burning
In bottle；
Step 2：Molotov cocktail is oxygenated and closed, Molotov cocktail is then put into progress microwave igniting in microwave oven cavity；
Step 3：After Molotov cocktail all burnt and cooling, injection alkaline absorption solution is absorbed in Molotov cocktail, Ran Houzhuan
Move absorbing liquid to be measured into ultra-clean bottle.
Preferably, described microwave absorbing material is absorbent charcoal powder body, graphite composite powder, graphene powder, carbon filament, graphite
Silk, carbon cloth, Graphite cloth, carbon fiber, the thin rod of carbon or graphite spine.
Preferably, a diameter of 0.1 μm of -2mm of described microwave absorbing material.
Preferably, described combustion carrier is inorfil cloth.
Preferably, described inorfil cloth is quartz fabric.
Preferably, the microwave power of described step two is 300~800W, and the duration of ignition is 5~20 seconds.
Preferably, described alkaline absorption solution is sodium hydroxide solution.
Preferably, described soak time is 1~2h.
Beneficial effects of the present invention
The present invention provides the sample treatment that a kind of microwave lights a fire Oxygen bottle combustion, and this method is by testing sample and microwave
Absorbing material is placed on combustion carrier, and then combustion carrier is put into Molotov cocktail；Molotov cocktail is oxygenated and closed, then will combustion
Flask is put into progress microwave igniting in microwave oven cavity；After Molotov cocktail all burnt and cooling, alkalescence suction is injected in Molotov cocktail
Receive liquid to be absorbed, then transfer absorbed liquid is to be measured into ultra-clean bottle.Compared with prior art, processing method of the invention with
High-purity microwave absorbing material replaces filter paper so that halogen, and the background of chlorine especially is lower；With high-purity carbon in sparking mode
Material is inhales ripple and ignition media, so as to realize physics ionization igniting；Meanwhile, the microwave power needed for method of the invention is more
Low, quantity of sample handling increase, sample adaptability are wider.
Brief description of the drawings
Fig. 1 is the structural representation of microwave of the present invention igniting Oxygen bottle combustion device.
In figure, 1, microwave oven cavity, 2, microwave control switch, 3, Molotov cocktail, 4, closure, 5, quartz hook, 6, treat test sample
Product, 7, microwave absorbing material, 8, combustion carrier, 9, absorbing liquid.
Embodiment
The present invention provides the sample treatment that a kind of microwave lights a fire Oxygen bottle combustion, as shown in figure 1, this method includes：
Step one：Testing sample 6 and microwave absorbing material 7 are placed on combustion carrier 8, then combustion carrier 8 is hung
On quartz hook 5 in Molotov cocktail 3；
Step 2：Molotov cocktail 3 is oxygenated and closed with closure 4, then Molotov cocktail 3 is put into microwave oven cavity 1, beaten
Open microwave control switch 2 and carry out microwave igniting；
Step 3：After all burnt of Molotov cocktail 3 and cooling, injection alkaline absorption solution 9 is absorbed in Molotov cocktail 3, so
Transfer absorbed liquid is to be measured into ultra-clean bottle afterwards.
According to the present invention, described testing sample is organic solid sample, preferably high-purity polyether-ether-ketone, corn or wheat；
The present invention processing method be directed to organic solid sample in nonmetalloid measure, preferably nonmetalloid be sulphur, phosphorus or
Chlorine；Described microwave absorbing material selects high-purity low resistance microwave absorbing material to obtain more preferable microwave energy transformation efficiency,
Preferably absorbent charcoal powder body, graphite composite powder, graphene powder, carbon filament, carbon fiber, graphite silk, carbon cloth, Graphite cloth, the thin rod of carbon or
Graphite spine, the size of described microwave absorbing material is generally avoided micro- in millimeter and micron order with avoiding the occurrence of microwave reflection
Ripple short circuit phenomenon, the diameter of described microwave absorbing material is preferably 0.1 μm of -2mm.Described combustion carrier is preferably inorganic fibre
Wei Bu.Described inorfil cloth is preferably quartz fabric.Described testing sample and the mass ratio of microwave absorbing material are
(0.01-0.5)：(0.01~0.1)
According to the present invention, described Molotov cocktail should select pressure-resistant material, such as hard glass or quartz glass, and its safety is resistance to
Press scope should be in the range of 3-25MPa, bottle cap selects low microwave absorption material and supporting low microwave absorption sealing ring realizes band
Effective air-tightness under pressure and the condition of high temperature, and with preferable thermal deformation and stability, preferably glass or quartzy ground,
PEEK materials, PFA materials, PTFE materials etc..Bottle cap should be connected in order to Sample introduction with sample bearing device simultaneously.Sample
Bogey can be the inorganic non-metallic drum or basket-like device hung with higher oxygen transmitance, or use coupling type,
Combustion carrier is coordinated to wrap up testing sample and microwave absorbing material.
According to the present invention, the microwave power of described step two is preferably 300~800W, and the duration of ignition is preferably 5~20
Second.
According to the present invention, described alkaline absorption solution is preferably sodium hydroxide solution, and described sodium hydroxide volume is preferred
For 10-20 milliliters；Described soak time is preferably 1~2h.
Further detailed description is done to the present invention with reference to embodiment.
Embodiment 1
The ion-chromatographic determination of trace amounts of chlorine in high-purity polyether-ether-ketone (PEEK) sample
It is accurate to weigh PEEK sample 0.10g, 0.01g graphite composite powders are added, PEEK and graphite powder are wrapped up with inorfil cloth
Body is simultaneously hung on the quartz hook in Molotov cocktail, by Molotov cocktail oxygenation and it is closed after be transferred to microwave oven cavity, in 600W power
After down-firing 15 seconds, bottle all burnt and cooling, after 10 milliliters of 60mmoL sodium hydroxides absorbing liquids of injection absorb 2 hours, uncap,
Transfer absorbed liquid is to be measured into ultra-clean bottle.
Test result indicates that：The processing method of the present invention, quantity of sample handling compares conventional oxygen flask combustion method and improves a number
Magnitude, Cl contents (29.7 ± 3.0) μ g/g, (chlorion being added without in PEEK samples, blank solution contains blank background values
Amount) two orders of magnitude are reduced, chlorine element method Monitoring lower-cut reaches 1.7 μ g/g, parallel determination precision (n=6) RSD=
4.26%, and can once carry out the ignition simultaneously of 4 samples.
Embodiment 2
Trace Cl Accurate Determining in corn solids organic standard sample
It is accurate to weigh corn solids organic standard sample 0.15g, 0.03g carbon fibers are added, wrap up beautiful with inorfil cloth
Rice SOLID ORGANIC standard sample and carbon fiber are simultaneously hung on the quartz hook in Molotov cocktail, by Molotov cocktail oxygenation and closed rear transfer
To microwave oven cavity, in 300W power down-firing 20 seconds, bottle all burnt and after cooling down injected 15 milliliters of 60mmoL sodium hydroxides
After absorbing liquid absorbs 1.5 hours, uncap, transfer absorbed liquid is to be measured into ultra-clean bottle.Testing result is as shown in table 1：
Table 1
Embodiment 3
Trace Cl Accurate Determining in wheat solids organic standard sample
It is accurate to weigh wheat solids organic standard sample 0.2g, 0.1g graphene powders are added, are wrapped up with inorfil cloth
Wheat solids organic standard sample and graphene powder are simultaneously hung on the quartz hook in Molotov cocktail, and Molotov cocktail is oxygenated and closed
After be transferred to microwave oven cavity, in 800W power down-firing 5 seconds, bottle all burnt and after cooling down injected 20 milliliters of 60mmoL hydrogen
After sodium oxide molybdena absorbing liquid absorbs 1 hour, uncap, transfer absorbed liquid is to be measured into ultra-clean bottle.Testing result is as shown in table 2：
Table 2
Claims (6)
- The sample treatment of Oxygen bottle combustion 1. a kind of microwave is lighted a fire, it is characterised in that this method includes：Step one：Testing sample and microwave absorbing material are placed on combustion carrier, then combustion carrier is put into Molotov cocktail；Step 2：Molotov cocktail is oxygenated and closed, Molotov cocktail is then put into progress microwave igniting in microwave oven cavity；Step 3：After Molotov cocktail all burnt and cooling, injection alkaline absorption solution is absorbed in Molotov cocktail, and then transfer is inhaled Receive liquid to be measured into ultra-clean bottle；Described microwave absorbing material is absorbent charcoal powder body, graphite composite powder, graphene powder, carbon filament, graphite silk, carbon cloth, graphite The thin rod of cloth, carbon fiber, carbon or graphite spine；A diameter of 0.1 μm of -2mm of described microwave absorbing material.
- The sample treatment of Oxygen bottle combustion 2. a kind of microwave according to claim 1 is lighted a fire, it is characterised in that described Combustion carrier is inorfil cloth.
- The sample treatment of Oxygen bottle combustion 3. a kind of microwave according to claim 2 is lighted a fire, it is characterised in that described Inorfil cloth is quartz fabric.
- The sample treatment of Oxygen bottle combustion 4. a kind of microwave according to claim 1 is lighted a fire, it is characterised in that described The microwave power of step 2 is 300~800W, and the duration of ignition is 5~20 seconds.
- The sample treatment of Oxygen bottle combustion 5. a kind of microwave according to claim 1 is lighted a fire, it is characterised in that described Alkaline absorption solution is sodium hydroxide solution.
- The sample treatment of Oxygen bottle combustion 6. a kind of microwave according to claim 1 is lighted a fire, it is characterised in that described Soak time is 1~2h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109970447B (en) * | 2019-02-28 | 2021-08-13 | 昆明理工大学 | Ignition method for microwave self-propagating sintering of weak absorption type MAX binding agent |
| CN110672778B (en) * | 2019-10-31 | 2022-03-01 | 上海屹尧仪器科技发展有限公司 | Oxygen combustion reaction kettle capable of being ignited by microwave |
| CN114280034A (en) * | 2021-12-24 | 2022-04-05 | 浙江微通催化新材料有限公司 | Application of oxygen bomb combustion method in determination of waste palladium-carbon-palladium content and determination method |
| CN114652012A (en) * | 2022-03-23 | 2022-06-24 | 深圳麦时科技有限公司 | Microwave type carbon heating ignition method, ignition appliance and heating system |
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|---|---|---|---|---|
| CN202710525U (en) * | 2012-07-19 | 2013-01-30 | 广东省生态环境与土壤研究所 | Simple oxygen flask combustion unit |
| CN104614416A (en) * | 2013-11-01 | 2015-05-13 | 深圳职业技术学院 | Detecting method of fluoride in soldering paste |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202710525U (en) * | 2012-07-19 | 2013-01-30 | 广东省生态环境与土壤研究所 | Simple oxygen flask combustion unit |
| CN104614416A (en) * | 2013-11-01 | 2015-05-13 | 深圳职业技术学院 | Detecting method of fluoride in soldering paste |
Non-Patent Citations (2)
| Title |
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| Microwave-Assisted Sample Combustion: A Technique for Sample Preparation in Trace Element Determination;Erico Marlon de Moraes Flores等;《Anal. Chem.》;20040511;第76卷(第13期);全文 * |
| 介绍两种氧瓶燃烧装置;高敏四;《药学通报》;19871231;第22卷(第1期);全文 * |
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