CN104089917B - Method for testing content of oxygen in villaumite - Google Patents
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Abstract
The invention discloses a method for testing the content of oxygen in villaumite. The method comprises the following steps: carrying out halogen removal on a sample to be tested by adopting an inert gas fusion process, and detecting the oxygen in villaumite, wherein monocrystalline lithium fluoride is used as a standard sample, and the sample to be tested has no contact with air in the preparation and test process of the sample to be tested. The testing method is an absolute oxygen determination method, has the advantages of small amount of the tested sample, low detection limit, wide determination range, high testing precision and low deviation, can prevent the water absorption or oxygen in the sample preparation process of villaumite, and can solve a problem that halogen-containing volatile matters generated in the heating of the sample corrode apparatuses.
Description
Technical field
The present invention relates to the method for testing of oxygen content in a kind of villiaumite.
Background technology
Inorganic salt and melt thereof, because having that thermal capacitance is big, heat transfer is fast, good fluidity, use temperature range width, have relatively material
The advantages such as high solvability, can be widely used as heat transfer and chemical reaction medium.At chemical industry, electrolytic metal, rare valuable gold
Belonging to and smelting, three-protection design, there is special application prospect in the fields such as emerging energy such as solar energy, Hydrogen Energy and nuclear energy.
But, the inorganic salt that purity is the highest is relatively strong to the corrosivity of structural material, and this is the principal element limiting its application
One of.As a example by fluorine fused salt, the oxygen impurities of hundreds of ppm, i.e. can significantly strengthen its corrosivity.Higher oxygen content considerably limit
Villiaumite application in prepared by nuclear energy and low oxygen content metal material, therefore, oxygen content is assessment one-component villiaumite, Yi Jiduo
One of important indicator of unit's fluorine fused salt quality.Find and accurately measure the assay method of low oxygen content in villiaumite, be to be badly in need of at present solving
Problem certainly.
At present, the method measuring villiaumite oxygen content has hydrofluorination method, KBrF4Method, electrochemical process, spectrographic method etc., but, as
Shown in table 1, from factors such as required sample size, measurement lower limit, measurement repeatability and single measurement required times relatively, have only
Inert gas fusion method can meet the test request of villiaumite sample.
Inert gas fusion method, is currently the standard method of the oxygen content measuring metal material (with reference to " GB/T11261-
2006 " mensuration of iron and steel oxygen content, PULSE HEATING inert gas fusion-infrared absorption；Or " YS/T539.13-2009 " is Ni-based
Alloyed powder chemical analysis method, the 13rd part, the mensuration of oxygen amount, PULSE HEATING inert gas fusion-infrared absorption).
Inert gas fusion method is facing generally towards metal sample, but, villiaumite sample is distinct with steel samples:
First, the fusing point of steel samples is about about 1500 DEG C, and the fusing point of villiaumite sample is typically below 1000 DEG C, if
Under the test condition of steel sample, measure villiaumite sample, sample can be caused acutely to volatilize, block exhaust pipe.Secondly, steel samples
Conducting heat, at high temperature can absorb heat and discharge oxygen element equably, and the heat transfer of villiaumite sample is bad, grind into powder is beneficial to it
Absorb heat equably and discharge oxygen element.Again, steel samples is commonly exposed to air, and the water absorption of villiaumite sample is very strong,
Certain oxygen barrier means must be taked during sample preparation.Then, iron and steel volatilization does not affect for device longevity and test result, and villiaumite
Volatilization is then contrary, therefore, must choose certain measured power, and, on the premise of ensureing measurement accuracy, villiaumite usage amount is more
Few the best.
Table 1
Wherein, hydrofluorination method reference literature W.Grimes, " Chemical research and development for
molten-salt breeder reactors,”Oak Ridge National Laboratory,Oak Ridge,
Tennessee,ORNL-TM-1853,1967.KBrF4 oxidizing process reference literature Goldberg, G.；Meyer,A.S.；White,
J.C.,Determination of Oxides in Fluoride Salts by High-Temperature
Fluorination with Potassium Bromotetrafluoride.Analytical Chemistry1960,32
(3),314-317；Eklund,S.E.；Toth,L.M.；Chambers,J.Q.；Mamantov,G.,Determination of
Oxide in Fluoride Salts Using an Yttria-Stabilized-Zirconia Oxygen
Pump.Analytical Chemistry1998,71(3),539-543；Or Q.Pham and R.S, Glass.Oxygen
pumping characteristics of yttria-stabilized-zirconia.Electrochimica Acta,
Vol.43,No.18,pp.2699-2708,1998.Electrochemical process reference literature Manning, D.L.；Mamantov,G.,
Electrochemical Studies Of Oxide Ions And Related Species In Molten
Fluorides.J Electrochem Soc1977,124(4),480-483；White,S.H.Molten Salt
Techniques；Plenum Press:New York,1983；Vol.1,p50；Bjerrum,N.J.；Berg,R.W.；
Chistensen,E.；Kerridge,D.H.；von Barner,J.H.Anal.Chem.1995,67,2129-35；Or Ito,
Y.；Yabe,H.；Nakai,T.；Ema,K.；Oishi,J.Electrochim Acta1986,31,1579-84.Spectrographic method reference
Document Polyakova, L.P.；Polyakov,E.G.；Bjerrum,N.J.Rus.J.Electrochem.1997,33,1339-
42。
Summary of the invention
The technical problem to be solved is to overcome the method for testing of oxygen content in existing villiaumite to detect institute
Need sample size height, measurement lower limit height, bad measurement repeatability, single measurement required time length, sample hygroscopic and instrument corrosion is tight
The defect such as heavily, and provide the method for testing of oxygen content in a kind of villiaumite.The method of testing of the present invention is the absolute measuring of a kind of oxygen
Determine method, the oxygen element total amount of form of ownership in testing sample can be measured；Test sample consumption is few, and detection limit is low, measurement range
Width, measuring accuracy is high, and relative standard deviation is low, and sample preparation is convenient, and can prevent sample in sample preparation and test process well
Affected by moisture in air and oxygen, sample can be solved and add the problem containing halogen volatile matter corrosion instrument hankering producing, behaviour
Work is simple, it is quick to measure.
The invention provides the method for testing of oxygen content in a kind of villiaumite, it comprises the steps: to use noble gas to melt
Melt method, after testing sample is gone halogen operation, detect oxygen content in villiaumite, wherein with lithium fluoride monocrystalline as standard sample,
The preparation of testing sample and test process not ingress of air.
Method of testing of the present invention, specifically includes following step:
(1) sample preparation: by testing sample under inert gas shielding, be ground into powder, then wrap up with soft capsule and seal
Mouthful；
(2) obtain standard curve: use oxygen analyzer, demarcate lithium fluoride monocrystalline standard sample with steel sample, then with lithium fluoride
Standard sample obtains standard curve；
(3) sample test: take testing sample, puts in the oxygen analyzer identical with step (2), carries out oxygen content test,
Obtain determination of oxygen content value；
Wherein, described oxygen analyzer is contained in described oxygen analyzer with halogen catcher, described halogen catcher
Heating chamber and COxBetween detector；Wherein, X is 1 or 2；Step (2) and (3) are carried out under inert gas shielding.
In the present invention, described inert gas fusion method uses the oxygen analyzer with halogen catcher to realize, such as, adopt
Realize by the oxygen analyzer of Laboratory Equipment Corporaton (LECO) company of the U.S., further preferred type
It number it is the oxygen analyzer of RO600 or RO836.Described halogen operation of going is to realize in halogen catcher.Described halogen
Catcher can use the halogen catcher of the various routine in this area, as long as it can absorb halogen-containing gaseous material but not absorb
COx.It with the halogen having severe corrosive produced in absorption measurement flow process and compound thereof, thus can extend making of detector unit
With the life-span, improve the accuracy of test.
Described oxygen analyzer parameter in use typically uses the starting-up method and routine provided in instrument description
Parameter sets.In step (2) and step (3), the heating-up temperature of described oxygen analyzer is set as 1000-1800 DEG C.
In step (1), described sample preparation preferably includes following steps: under inert atmosphere protection, wraps up with soft capsule
The villiaumite 0.1～0.2g of powder also seals, and obtains testing sample.
In step (1), described noble gas is the conventional inert gas of this generic operation in this area, preferably argon, institute
The purity preferred mass percentage ratio of the argon stated is more than or equal to 99.9%, and described mass percent refers to that the quality of argon accounts for
The percentage ratio of argon reagent gross mass.Described soft capsule preferred soft gelatin capsule shape stannum capsule or soft gelatin capsule shape nickel capsule, further preferred glue
Pellet stannum capsule.Described soft gelatin capsule shape stannum capsule preferred mass percentage composition is the stannum capsule more than or equal to 99.99%, described stannum capsule
Preferred 0.7mm～0.8mm of thickness of middle stannum.The soft gelatin capsule shape of the preferred one end open of shape of described soft gelatin capsule shape stannum capsule.Described
Stannum capsule, the soft fold closure that is prone to of matter, oxygen content is more stable, and in stannum capsule, oxygen content value is preferably 20～40ppm.Described is soft
The all operations that matter capsule wraps up and seals, is preferably used clean metallic instrument, is so possible not only to avoid encapsulated metal to pollute,
Oxygen and the water pollution to testing sample in air can also be completely cut off.
In step (1), described testing sample is villiaumite, described villiaumite preferred fluorinated sodium, potassium fluoride, lithium fluoride, fluorine
Change one or more in beryllium, calcium fluoride and Afluon (Asta).The described oxygen content in villiaumite is typically 10～104ppm。
In step (2), it is thus achieved that during standard curve, accepted standard sample the most all volatilizees under steel sample Applicable temperature, and
And, under fused salt Applicable temperature, test result is equal with test result under steel sample Applicable temperature, preferably steel sample and lithium fluoride monocrystalline
Combine.Described standard sample obtains calibration factor for calibration instrument, when measuring testing sample the most every time, and be with this standard
Sample is compared.The Functionality, quality and appealing design of described lithium fluoride elects 0.1g～0.2g as, preferred 70ppm～90ppm of its oxygen content.
In step (3), when carrying out sample test, according to this area routine operation, first carry out background and test again to be measured
Sample is tested.Described background test refers to deduct the background of soft balsam capsule material.Described deduction soft balsam capsule material
Background, refer to deduct impurity oxygen contained in soft balsam capsule material, method is repeatedly to measure same batch material oxygen content, makes even
Average is as background rejection.
In step (3), described test is preferably carried out in pyrographite crucible, and described pyrographite crucible is the highest
The graphite crucible of pure graphite material.Preferred 4000W～5000W of calcination power of described pyrographite crucible.Described high temperature
Graphite crucible preferably employs following step and processes: take graphite crucible, calcination repeatedly under inert gas shielding, removes graphite crucible
The oxygen of surface adsorption.The number of times of described calcination repeatedly preferably three times.
In step (3), power during described test comes really according to the vapour pressure under the fusing point of testing sample and its high temperature
Fixed, power is too low, and the oxygen in fused salt cannot be made fully to volatilize and react with graphite, and temperature is too high, causes fused salt all to volatilize,
Jam detection gas circuit, therefore, preferred 2000W～3500W of measured power during described test, corresponding heating-up temperature is about 1000
～1800 DEG C.
In step (3), described method of testing specifically includes following steps: take testing sample, puts into described oxygen analysis
In the dress sample mouth of instrument, testing sample, under inert gas shielding, automatically falls into described pyrographite crucible.Test merit is set
Rate, instrument produces high temperature after running, and the carbon making oxygen element in testing sample and pyrographite crucible surface escape reacts, generation
COxGas, all gaseous products, through halogen catcher, enter infrared detector with carrier gas；Computer program is to COxDetection
Device signal processes, and after deducting background, draws the oxygen content value of testing sample.
Without prejudice to the field on the basis of common sense, above-mentioned each optimum condition, can combination in any, obtain the present invention each preferably
Example.
Agents useful for same of the present invention and raw material are the most commercially.
The most progressive effect of the present invention is: the method for testing of the present invention can optimize and micro amount of oxygen in villiaumite is transformed into
The technique that can measure oxycarbide, had both guaranteed that in sample, oxygen element is fully converted into measurable gaseous carbon oxide, ensured again
Salt at high temperature will not measuring contamination system:
1, the oxygen content method of testing of the present invention is a kind of absolute determination method of oxygen, can measure institute in testing sample tangible
The oxygen element total amount of formula.
2, the oxygen content method of testing test sample consumption of the present invention is few, it is only necessary to 100mg～200mg.
3, the oxygen content method of testing detection limit of the present invention is low, up to 0.01ppm.
4, the oxygen content method of testing measurement range width of the present invention, 0.05ppm～5%.
5, the oxygen content method of testing measuring accuracy of the present invention is high, and relative standard deviation is less than 10%.
6, the oxygen content method of testing sample preparation of the present invention is convenient, and can prevent sample in sample preparation and test process well
Affected by moisture in air and oxygen.
7, the oxygen content method of testing of the present invention can solve sample add hanker produce containing halogen volatile matter corrode instrument
Problem.
8, the program that the oxygen content method of testing of the present invention provides based on commercialization instrument, simple to operate, measure quickly.
Detailed description of the invention
Further illustrate the present invention below by the mode of embodiment, but the most therefore limit the present invention to described reality
Execute among example scope.The experimental technique of unreceipted actual conditions in the following example, conventionally and condition, or according to business
Product description selects.
Embodiment 1:
1.1 instruments and material
U.S. LECO oxygen analyzer model RO600 or RO836, including halogen catcher, air-channel system, injector, high temperature
Stove, detecting system etc.；Glove box；Electronic balance；Stannum capsule；High purity graphite crucible；Standard sample (steel)；Lithium fluoride monocrystalline；NaF powder
End sample.
1.2 analysis condition
Oxygen analyzer employs nitrogen as power gas, and pressure is 0.28MPa～0.29MPa.Water, oxygen content is used to be below
The high-purity argon gas of 1ppm is carrier gas, and pressure is 0.15MPa.High temperature furnace power is set to 2900W, and the degassing cycle is 3 times.
1.3 operating procedure
Prepared by sample: be placed on electronic balance by soft gelatin capsule shape stannum capsule in glove box, load the NaF of about 0.15g after peeling
Powder sample, weighs soft gelatin capsule shape stannum capsule fold seals after recording；
Start and parameter set: according to instrumentation requirement, regulation power gas and the pressure of carrier gas, open instrument, by height
Pure graphite crucible loads instrument heating cavity；Set heating-up temperature 1650 DEG C (analyzing power 2900W), degassing power 4500W, take off
The gas cycle is 3.
Instrument calibration: select LiF Crystals (oxygen content is 80 ± 10ppm), calibration instrument, draw calibration factor；
Skip test: use stannum capsule as " blank " mensuration three times, it is thus achieved that meansigma methods as background values, it will finally
Result of calculation in deduct；
Sample test: under inert gas shielding, puts into the stannum capsule being encapsulated with sample in the injection port of oxygen analyzer, presses
Lower initiating key, sample, automatically in the graphite crucible in high temperature furnace, is heated to high temperature, in sample according to the intrinsic program of instrument
Oxygen and carbon in crucible react generation COx, COxEntering detector with carrier gas, computer is to COxAfter detector signal integral and calculating
To molten salt sample oxygen content value.
1.4 interpretation of result
As a example by NaF sample, testing three parallel sample under same test condition, its test value is respectively 5986ppm,
5802ppm, 5824ppm, its meansigma methods is 5871ppm, and recording relative standard deviation is 0.017%, it is seen that test accuracy is very
Height, the method can meet the oxygen content test request of one pack system villiaumite well.
1.5 residual oxygen measure
For obtaining optimized analysis power, the oxygen in sample can be made to react with graphite completely, fluoride salt can be made again at this
At a temperature of will not because of the volatilization under high temperature severe contamination sample test system, it is necessary to measure sample heating power carry out excellent
Change.For this in operation, in addition to testing normally, also to the NaF sample tested, reheat test two
Secondary, now do not find CO againxDetection peak, it was demonstrated that the oxygen content recorded for the first time is sample total oxygen content.
Embodiment 2:
2.1 instruments and material
U.S.'s LECO oxygen analyzer, including halogen catcher, air-channel system, injector, high temperature furnace, detecting system etc.；Hands
Casing；Electronic balance；Stannum capsule；High purity graphite crucible；Standard sample (lithium fluoride monocrystalline)；LiF-NaF-KF(46.5-11.5-
42mol%) eutectic salts.
2.2 analysis condition
Oxygen analyzer uses the oxygen content high-purity argon gas less than 1ppm and high pure nitrogen to be carrier gas, and pressure is respectively
0.15MPa and 0.28-0.29MPa, power setting analyzed by high temperature furnace is 2500W, and the degassing cycle is 3 times.
2.3 operating procedure
Prepared by sample: be placed on electronic balance by stannum capsule in glove box, loads the LiF-NaF-KF of about 0.15g after peeling
Powder sample, weighs stannum capsule fold seals after recording；
Start and parameter set: according to instrumentation requirement, regulation power gas and the pressure of carrier gas, open instrument, by height
Pure graphite crucible loads instrument heating cavity；Set heating-up temperature 1460 DEG C (analyzing power 2500W), degassing power 4500W, take off
The gas cycle 3.
Instrument calibration: select LiF Crystals (oxygen content is 80 ± 10ppm), calibration instrument, draw calibration factor；
Skip test: use stannum capsule as " blank " mensuration three times, it is thus achieved that meansigma methods as background values, it will finally
Result of calculation in deduct；
Sample test: under inert gas shielding, puts into the stannum capsule being encapsulated with sample in the injection port of oxygen analyzer, presses
Lower initiating key, sample, automatically in the graphite crucible in high temperature furnace, is heated to high temperature, in sample according to the intrinsic program of instrument
Oxygen and carbon in crucible react generation COx, COxEntering detector with carrier gas, computer is to COxAfter detector signal integral and calculating
To molten salt sample oxygen content value.
2.4 interpretation of result
Test two identical proportionings, but difference prepares the LiF-NaF-KF villiaumite sample of batch, to each sample equally
Arranging three parallel sample under test condition, test result is as follows:
| Fused salt batch | Three test value/ppm | Meansigma methods/ppm | Relative standard deviation/% |
| 1 | 240 | 235 | 237 | 237 | 1.003 |
| 2 | 219 | 203 | 218 | 214 | 4.257 |
It can be seen that test result relative standard deviation is relatively low, test accuracy is the highest, and test repeatability is fine.This surveys
Method for testing is well suited for mixing the oxygen content testing requirement of villiaumite, simple to operate, highly sensitive.
2.5 residual oxygen measure
For obtaining optimized analysis power, the oxygen in sample can be made to react with graphite completely, fluoride salt can be made again at this
At a temperature of will not because of the volatilization under high temperature severe contamination sample test system, it is necessary to measure sample heating power carry out excellent
Change.For this in operation, in addition to testing normally, also to the LiF-NaF-KF sample tested, again add
Thermal test twice, does not now find CO againxDetection peak, it was demonstrated that the oxygen content recorded for the first time is sample total oxygen content.
Claims (11)
1. a method of testing for oxygen content in villiaumite, it comprises the steps: to use inert gas fusion method, to testing sample
Oxygen content in villiaumite is detected, wherein with lithium fluoride monocrystalline as standard sample, the preparation of testing sample after carrying out halogen operation
With test process not ingress of air；
In described villiaumite, the method for testing of oxygen content specifically includes following step:
(1) sample preparation: by testing sample under inert gas shielding, be ground into powder, then wrap up with soft capsule and seal；
(2) standard curve is obtained: use oxygen analyzer, with the standard sample described in the demarcation of steel sample, then with described standard sample
Obtain standard curve；
(3) sample test: take testing sample, puts in the oxygen analyzer identical with step (2), carries out oxygen content test, obtain oxygen
Assay value；
Wherein, described oxygen analyzer is contained in adding of described oxygen analyzer with halogen catcher, described halogen catcher
Hot cell and COxBetween detector；Wherein, X is 1 or 2；Step (2) and (3) are carried out under inert gas shielding；
In step (3), measured power during described test is 2000W～3500W.
2. method of testing as claimed in claim 1, it is characterised in that: in step (2) and (3), adding of described oxygen analyzer
Hot temperature is set as 1000-1800 DEG C.
3. method of testing as claimed in claim 1, it is characterised in that: in step (1), described sample preparation comprises the following steps:
Under inert atmosphere protection, wrap up the villiaumite 0.1～0.2g of powder with soft capsule and seal, obtaining testing sample.
4. the method for testing as described in claim 1 or 3, it is characterised in that: in step (1), described testing sample is villiaumite；
Described villiaumite is one or more in sodium fluoride, potassium fluoride, lithium fluoride, beryllium fluoride, calcium fluoride and Afluon (Asta)；And/or institute
Oxygen content in the villiaumite stated is 10～104ppm。
5. method of testing as claimed in claim 1, it is characterised in that: in step (1), described noble gas is argon；Institute
The soft capsule stated is soft gelatin capsule shape stannum capsule or soft gelatin capsule shape nickel capsule；Described soft gelatin capsule shape stannum capsule is that weight/mass percentage composition is more than or equal to
The stannum capsule of 99.99%, in described stannum capsule, the thickness of stannum is 0.7mm～0.8mm；In described stannum capsule oxygen content value be 20～
40ppm。
6. method of testing as claimed in claim 5, it is characterised in that: described soft gelatin capsule shape stannum capsule be shaped as one end open
Soft gelatin capsule shape.
7. method of testing as claimed in claim 1, it is characterised in that: in step (3), before carrying out sample test, first carry out
Background is tested.
8. method of testing as claimed in claim 1, it is characterised in that: in step (3), described test is at pyrographite crucible
In carry out.
9. method of testing as claimed in claim 8, it is characterised in that: in step (3), the calcination of described pyrographite crucible
Power is 4000W～5000W；Described pyrographite crucible uses following step to process: take graphite crucible, protects at noble gas
Protect down calcination repeatedly, remove the oxygen of graphite crucible surface adsorption.
10. method of testing as claimed in claim 9, it is characterised in that the number of times of described calcination repeatedly is three times.
11. method of testings as claimed in claim 8, it is characterised in that: in step (3), described method of testing specifically includes
Following steps: take testing sample, put in the dress sample mouth of described oxygen analyzer, and testing sample is under inert gas shielding, certainly
Move and fall into described pyrographite crucible；Arranging measured power, instrument produces high temperature after running, and makes the oxygen element in testing sample
React with the carbon of pyrographite crucible surface effusion, generate COxGas, all gaseous products are through halogen catcher, with indifferent gas
Body enters infrared detector together；Computer program is to COxDetector signal processes, and after deducting background, draws and treat
The oxygen content value of test sample product.
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| CN105784530A (en) * | 2014-12-19 | 2016-07-20 | 北京有色金属研究总院 | Method for measuring contents of oxygen and nitrogen in neodymium iron boron (NdFeB) material |
| CN107064045A (en) * | 2016-12-12 | 2017-08-18 | 中核北方核燃料元件有限公司 | The assay method of oxygen content in a kind of composite material of silicon carbide |
| CN113030000B (en) * | 2021-03-01 | 2023-02-21 | 西安奕斯伟材料科技有限公司 | Method and device for measuring interstitial oxygen content of silicon single crystal rod |
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