CN105547802B - A kind of chemical reagent for the molten sample methods of Carius and the molten sample methods of Carius using the chemical reagent - Google Patents
A kind of chemical reagent for the molten sample methods of Carius and the molten sample methods of Carius using the chemical reagent Download PDFInfo
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- CN105547802B CN105547802B CN201610031842.2A CN201610031842A CN105547802B CN 105547802 B CN105547802 B CN 105547802B CN 201610031842 A CN201610031842 A CN 201610031842A CN 105547802 B CN105547802 B CN 105547802B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The present invention relates to the molten sample methods of Carius of a kind of chemical reagent for the molten sample methods of Carius and the use reagent.The chemical reagent includes following component：HCl、HNO3And HClO4, using the molten sample methods of the Carius of the chemical reagent, molten sample amount can reach 4g, be existing 2~3 times, meanwhile, method provided by the invention has advantage easy to operate, easy to spread.
Description
Technical field
Present invention relates particularly to the Carius of a kind of chemical reagent for the molten sample methods of Carius and the use chemical reagent
Molten sample method.
Background technology
Carius pipes are a kind of high-temperature and high-presure resistent heavy wall high boron glass pipe or quartz ampoule.Use the Carius pipes
Re-Os (rhenium-osmium) determines year and the method for isotope tracer technique is known as the molten sample method of Carius pipes, is also the molten sample methods of Carius.
The molten sample methods of Carius are that sample, Re, Os mixed diluent are added in Carius pipes, and HCl and HNO is added after freezing3, then will
Through high-temperature heating after the Carius seals of tube, takes out the solution in Carius pipes and carry out Re, Os element sepatation and collect, measure respectively
After the content of Re elements and Os elements, by calculating to obtain the Formed age of sample.
In recent years, Re-Os (rhenium-osmium) determines year with isotope tracer technique by more and more extensive attention, and molybdenite is fixed
Year is one of important application approach of Re-Os isotopic systems.The molten sample methods of Carius are most widely used in Re-Os Isotope Research
A kind of general sample dissolving method.
The molten sample methods of Carius have many good qualities, such as：1, applicable sample type is more, either pyrolite, igneous rock, deposition
Object or PGEs mineral, metal alloy and various sulfide the molten sample methods of Carius can be used to be detected；2, due to
Sample is closed in Carius pipes, the more other methods of this method can prevent the loss of Os to the maximum extent, to ensure the accurate of experiment
Property；3, the isotopic exchange equilibrium of Re and Os is more abundant in sample and diluent, reagent easy purification, the whole process blank of Re and Os
It is relatively low；4, Carius pipes are disposable experimental article, no cross contamination.
But the present inventor is carrying out Re-Os using the molten sample methods of existing Carius to metal sulfide sample
It is found when Isotope Dating, for the higher molybdenite of Re, Os content, the molten sample methods of Carius have and can obtain preferable experiment knot
Fruit, still, for metal sulfides such as pyrite, chalcopyrites since Re, Os content are relatively low, to ensure to have when the instrument is measured
Relatively stable signal, the existing molten sample methods of Carius need to improve molten sample amount.Currently, existing for low content sulfide sample
The molten sample methods of Carius be using the inverse aqua regia dissolution 1g samples more than 20ml, but due to metal sulfides such as samples of pyrite and
Inverse chloroazotic acid reacts very violent, and a large amount of consumption oxidants of matrix element reaction reduce oxidisability to hinder OsO4Generation.
It is larger so as to cause the error of measurement result.H is added in system in this regard, bending text person of outstanding talent etc. and using2O2Method (bend text person of outstanding talent etc., mistake
Hydrogen oxide is in the course of dissolution of pyrite to rhenium-osmium signal strength and the influence at age, analytical chemistry, 36 (2008), 223-
226), to enhance the oxidisability of system, OsO can be promoted4Generation, but be the largest molten sample amount and can only achieve 1.2g.
To solve the problems, such as that molten sample amount is small, Qi etc. decomposes sulfide (L Qi with HNO3 in advance using the device of designed, designed
et al.An improved Carius tube technique for determination of low
Concentrations ofRe and Os in pyrites.Journal ofAnalytical Atomic
Spectrometry, 25 (2010), 585-589) generate gas absorbed with HCl after, by this HCl solution suck-back return Carius pipe
In, then tube sealing close dissolving is carried out, the method can dissolve 3g samples of pyrite, increase molten sample amount, but complicated for operation, unfavorable
In large-scale promotion.
In conclusion the molten sample amount of the existing molten sample methods of Carius generally can only achieve 1.2g, and oxidizer is larger；Qi
Although molten sample amount can reach 3g to the solution that is pre-dissolved of equal foundation, but complicated for operation, be not suitable for promoting.
Invention content
In order to solve the above problem of the existing technology, the present invention provides a kind of chemistry for the molten sample methods of Carius
Reagent and the molten sample methods of Carius for using the chemical reagent, after the chemical reagent, molten sample amount can reach 4g, be existing
2~3 times, meanwhile, method provided by the invention have advantage easy to operate, easy to spread.
The technical solution adopted in the present invention is：A kind of chemical reagent for the molten sample methods of Carius, including following component：
HCl、HNO3And HClO4。
In the present invention, creatively by HClO4(perchloric acid) is added, with HCl, HNO3And HClO4Combination replace tradition
HCl and HNO3Combination, HClO4It is the strongest acid of oxidisability, the HClO of addition in six big inorganic acids4Foot can not only be provided
Enough acidic environments and oxidisability significantly improve molten sample amount so more samples can be handled, and molten sample amount can reach
4g；In addition, after perchloric acid is reduced, chlorion is generated, new anion will not be introduced in system, therefore will not be to subsequentization
It learns separation process and causes harmful effect.
To ensure the effectiveness of the chemical reagent, preferred technical solution is every 1~4 part of quality in the chemical reagent
The mass parts of part sample tie element are：2~4 parts of HCl, HNO38~14 parts and HClO41~6 part.
According to the dosage of the chemical reagent, the sample of 4g is dissolved, heretofore described chemical reagent is at most only used
24g compares dissolving 1g samples in the molten sample methods of existing Carius and needs 20g or more；Heretofore described chemical reagent tool
While having easy to operate, cost is greatly reduced.
As the specific choice implemented under laboratory or other environment, further, the HCl be mass fraction be 30~
35% HCl solution, HNO3The HNO for being 50~60% for mass fraction3Solution, HClO4It is 70~72% for mass fraction
HClO4Solution.
The present invention also provides a kind of molten sample methods of Carius using the chemical reagent, include the following steps：
A, 1~4g samples are weighed, and sample is put into Carius pipes, and Carius pipes are placed in -50~-80 DEG C of ring
In border；
B, mixed diluent is added in the Carius pipes, sequentially adds HCl, HNO3And HClO4；
C, it seals the Carius using hot melt to manage, and the Carius pipes is heated to 200~220 DEG C, keep 18
~30h；
D, after the completion of heating, after the Carius pipes are cooled to room temperature, liquid therein is taken out, and analyze detection.
It should be noted that the present invention uses185Re and190The mixed diluent of Os for example,185Re and190Os's is mixed
Close the height that diluent addition depends on Re, Os content in sample；Certainly, according to the difference of sample type and quantity, ability
Field technique personnel can make the selection of different mixed diluent type and quantity according to the prior art, just no longer superfluous herein
It states.
More samples can be handled using the molten sample methods of Carius provided by the invention, significantly improve molten sample amount, it is molten
Sample amount can reach 4g.In addition, because having used than existing HCl and HNO3The stronger combination of oxidisability only needs in step c
200~220 DEG C are heated to, 18~30h (temperature I d median is 210 DEG C, and heating duration I d median is for 24 hours), comparison are kept
- 48h for 24 hours is heated under conditions of 220 DEG C or more in the existing molten sample methods of Carius, be greatly reduced energy consumption.
To improve the accuracy of experiment, preferred technical solution is, in step a and b, the sample is weighed using assay balance
The sample and the mixed diluent are moved to the Carius using the same long neck funnel and managed by product and mixed diluent
In.
Assay balance can be accurate to 0.0001g, ensure that the accuracy of experiment, in addition, using the same long neck funnel,
It can will remain in the micro-example on long neck funnel to rinse into the Carius pipes using the mixed diluent, reduce
Error.
Further, during three kinds of ingredients that the chemical reagent is sequentially added in step b, when former ingredient freezes
Latter ingredient is added after knot.The purpose so done is in order to avoid Os or oxygen in oxidant and example reaction oxidation sample
Change Os in diluent to result in volatility OsO4, determine year so as to cause sample and deviate actual value.
Further, in step c, after the solution fully charge in the Carius pipes, coal gas-oxygen flame is used
The venturi portion of the Carius pipes is sealed, the Carius pipes are put into stainless steel sleeve pipe after sealing, it will be described
Carius pipes are put into together with stainless steel sleeve pipe in baking oven, and room temperature, the substance in the Carius pipes is kept all to become liquid
Afterwards, it begins to warm up.200~220 DEG C are gradually warming up to, 18~30h is kept.
It is sealed again after the solution fully charge in the Carius pipes, reduces the volatilization of Os in diluent, meanwhile, by institute
It states Carius pipes to be put into stainless steel sleeve pipe, avoid in high-temperature heating, the Carius pipe explosions are hurted sb.'s feelings.
As for heating time and temperature, it is not required to because the stronger chemical reagent of oxidisability is employed herein
Dissolving can be completed in the heating time and temperature reached in the molten sample methods of existing Carius.
Further, the both ends of the stainless steel sleeve pipe are equipped with relief hole.The acting as of the relief hole works as Carius
After pipe explodes in stainless steel sleeve pipe, acid gas can be discharged from relief hole, avoid steel bushing by acid gas corrosion.
Further, the liquid in the Carius pipes is taken out for convenience, while reducing sample loss, in step d, by institute
It states after Carius pipes are cooled to room temperature, the Carius pipes is put into -50~-80 DEG C of environment, solution freezes completely wherein
After knot, in the venturi portion trepanning pressure release of the Carius pipes, in the venturi portion cut of the Carius pipes after pressure release, after put
It is preserved in refrigerator-freezer；When needing, the Carius pipes are placed in ice-water bath, wait for that substance all becomes liquid in the Carius pipes
After body, tapping the venturi portion of the Carius pipes makes it after fracture at cut, takes out liquid therein.
Since sample and acid reaction will produce bulk gas, the air pressure in the Carius pipes can be bigger, pressure release
It is in order to improve safety, in addition, in the venturi portion cut of the Carius pipes, convenient for opening the Carius pipes while protecting
The complete of the Carius pipes main body is held, it will not there is a situation where leakages.
According to one embodiment of present invention, in step a and step d, -50~-80 DEG C of the cooling of environment temperature is obtained and are situated between
Matter is the mixture of ethyl alcohol and liquid nitrogen, if this is because merely with liquid nitrogen cooling due to its boiling temperature it is too low (- 210 DEG C), one
As equipment be difficult to bear.The melting temperature of ethyl alcohol is -114 DEG C, is mixed with liquid nitrogen and is generally obtained -50~-80 DEG C of environment
Temperature can not only ensure all to freeze sour under the range, but also in the tolerance range of most of vessel.
Beneficial effects of the present invention are：
1, the chemical reagent for the molten sample methods of Carius in the present invention, because wherein adding HClO4, it is capable of providing foot
Enough acidic environments and oxidisability significantly improve molten sample amount so more samples can be handled, and molten sample amount can reach
4g；In addition, after perchloric acid is reduced, chlorion is generated, new anion will not be introduced in system, therefore will not be to subsequentization
It learns separation process and causes harmful effect.
2, the chemical reagent for the molten sample methods of Carius in the present invention, dissolves the sample of 4g, the chemical reagent is most
24g is only used, dissolving 1g samples in the molten sample methods of existing Carius is compared and needs 20g or more；Heretofore described chemistry examination
While agent has easy to operate, cost is greatly reduced.
3, the molten sample methods of Carius provided by the invention are because used than existing HCl and HNO3Stronger group of oxidisability
It closes, 200~220 DEG C need to be only heated in step c, keeping 18~30h, (temperature I d median is 210 DEG C, heats position in duration
Numerical value is for 24 hours), -48h for 24 hours will be heated under conditions of 220 DEG C or more by comparing in the molten sample methods of existing Carius, greatly be subtracted
Small energy consumption.
Description of the drawings
Fig. 1 is perchloric acid addition and molten sample magnitude relation figure；
Fig. 2 is different proportion oxidant combination oxidisability schematic diagram.
Specific implementation mode
With reference to embodiment, present disclosure is further illustrated.It should be appreciated that the implementation of the present invention is not limited to
In the following examples, the accommodation in any form and/or change made to the present invention fall within the scope of the present invention.
In the present invention, if not refering in particular to, all parts, percentage are unit of weight, and all equipment and raw material etc. are equal
It is commercially available or the industry is common.Method in following embodiments is unless otherwise instructed the routine of this field
Method.
Embodiment 1
A kind of chemical reagent for the molten sample methods of Carius, including following component：The HNO of HCl, 14g of 2g3With 1g's
HClO4。
A kind of molten sample methods of Carius using above-mentioned chemical reagent, include the following steps：
A, 1g samples are weighed using assay balance, long neck funnel is used in combination that sample is put into Carius pipes, and by Carius
Pipe is placed in -80 DEG C of environment；
B, it is weighed using assay balance185Re and190The mixed diluent of Os, and will be mixed using the long neck funnel in step a
It closes diluent to be added in the Carius pipes, it is 60% to sequentially add HCl, mass fraction that mass fraction is 30%
HNO3The HClO for being 70% with mass fraction4；During three kinds of ingredients for sequentially adding the chemical reagent, when former at
Divide after freezing and adds latter ingredient；
C, after the solution fully charge in the Carius pipes, using coal gas-oxygen flame by the Carius pipes
Venturi portion seals, and the Carius pipes is put into stainless steel sleeve pipe after sealing, the both ends of the stainless steel sleeve pipe are equipped with
Relief hole；The Carius pipes are put into together with stainless steel sleeve pipe in baking oven, room temperature, the substance in the Carius pipes are kept
After all becoming liquid, begin to warm up.220 DEG C are gradually warming up to, 30h is kept；
D, after the completion of heating, after the Carius pipes are cooled to room temperature, the Carius pipes are put into -50 DEG C of environment
In, wherein after solution fully charge, in the venturi portion trepanning pressure release of the Carius pipes, managed in the Carius after pressure release
Venturi portion cut, after be put in refrigerator-freezer and preserve；When needing, the Carius pipes are placed in ice-water bath, are waited for described
After substance all becomes liquid in Carius pipes, tapping the venturi portion of the Carius pipes makes it after fracture at cut, takes
Go out liquid therein, and analyzes detection.
It should be noted that in step a and step d, the cooling medium that obtains -50~-80 DEG C of environment temperatures be ethyl alcohol and
The mixture of liquid nitrogen.
Embodiment 2
A kind of chemical reagent for the molten sample methods of Carius, including following component：The HNO of HCl, 8g of 4g3With 6g's
HClO4。
A kind of molten sample methods of Carius using above-mentioned chemical reagent, include the following steps：
A, 4g samples are weighed using assay balance, long neck funnel is used in combination that sample is put into Carius pipes, and by Carius
Pipe is placed in -50 DEG C of environment；
B, it is weighed using assay balance185Re and190The mixed diluent of Os, and will be mixed using the long neck funnel in step a
It closes diluent to be added in the Carius pipes, it is 50% to sequentially add HCl, mass fraction that mass fraction is 35%
HNO3The HClO for being 72% with mass fraction4；During three kinds of ingredients for sequentially adding the chemical reagent, when former at
Divide after freezing and adds latter ingredient；
C, after the solution fully charge in the Carius pipes, using coal gas-oxygen flame by the Carius pipes
Venturi portion seals, and the Carius pipes is put into stainless steel sleeve pipe after sealing, the both ends of the stainless steel sleeve pipe are equipped with
Relief hole；The Carius pipes are put into together with stainless steel sleeve pipe in baking oven, room temperature, the substance in the Carius pipes are kept
After all becoming liquid, begin to warm up.200 DEG C are gradually warming up to, 18h is kept；
D, after the completion of heating, after the Carius pipes are cooled to room temperature, the Carius pipes are put into -80 DEG C of environment
In, wherein after solution fully charge, in the venturi portion trepanning pressure release of the Carius pipes, managed in the Carius after pressure release
Venturi portion cut, after be put in refrigerator-freezer and preserve；When needing, the Carius pipes are placed in ice-water bath, are waited for described
After substance all becomes liquid in Carius pipes, tapping the venturi portion of the Carius pipes makes it after fracture at cut, takes
Go out liquid therein, and analyzes detection.
It should be noted that in step a and step d, the cooling medium that obtains -50~-80 DEG C of environment temperatures be ethyl alcohol and
The mixture of liquid nitrogen.
Embodiment 3
A kind of chemical reagent for the molten sample methods of Carius, including following component：The HNO of HCl, 11g of 3g3With 3g's
HClO4
A, 2.5g samples are weighed using assay balance, long neck funnel is used in combination that sample is put into Carius pipes, and will
Carius pipes are placed in -65 DEG C of environment；
B, it is weighed using assay balance185Re and190The mixed diluent of Os, and will be mixed using the long neck funnel in step a
It closes diluent to be added in the Carius pipes, it is 55% to sequentially add HCl, mass fraction that mass fraction is 32%
HNO3The HClO for being 71% with mass fraction4；During three kinds of ingredients for sequentially adding the chemical reagent, when former at
Divide after freezing and adds latter ingredient；
C, after the solution fully charge in the Carius pipes, using coal gas-oxygen flame by the Carius pipes
Venturi portion seals, and the Carius pipes is put into stainless steel sleeve pipe after sealing, the both ends of the stainless steel sleeve pipe are equipped with
Relief hole；The Carius pipes are put into together with stainless steel sleeve pipe in baking oven, room temperature, the substance in the Carius pipes are kept
After all becoming liquid, begin to warm up.210 DEG C are gradually warming up to, is kept for 24 hours；
D, after the completion of heating, after the Carius pipes are cooled to room temperature, the Carius pipes are put into -65 DEG C of environment
In, wherein after solution fully charge, in the venturi portion trepanning pressure release of the Carius pipes, managed in the Carius after pressure release
Venturi portion cut, after be put in refrigerator-freezer and preserve；When needing, the Carius pipes are placed in ice-water bath, are waited for described
After substance all becomes liquid in Carius pipes, tapping the venturi portion of the Carius pipes makes it after fracture at cut, takes
Go out liquid therein, and analyzes detection.
It should be noted that in step a and step d, the cooling medium that obtains -50~-80 DEG C of environment temperatures be ethyl alcohol and
The mixture of liquid nitrogen.
For the experiment effect of the detection present invention, spy does experimental example, specific as follows：
Experimental example 1
Fig. 1 is perchloric acid addition and molten sample magnitude relation figure, this experiment is by taking chalcopyrite as an example, for the ease of data comparison,
In 4ml HCl and 16ml HNO3Under conditions of, use 1.5ml 10ppb Ir solution as Os absorbing liquids, Ir is internal standard to data
It is normalized.Therefore it can be calculated by following formula190Os/193Ir relative count rates indicate OsO4Oxidation
Situation, relative count rate is higher, and sour oxidisability is stronger.
Formula is：
It can be derived that from Fig. 1, as sample weighting amount increases when being added without perchloric acid, sample oxidation rate declines obviously, simultaneously
Solution in the Carius pipes from light green color becomes blackish green and with yellow mercury oxide.1ml HClO are added4Later, oxygenation efficiency
It is significantly improved, with the increase of perchloric acid addition, the oxidisability of sample is also continuously improved therewith, and sample size is also gradual
Increase, sample weighting amount is more than that later blasted pipe phenomenon occurs for 5g, does not obtain any data, but sample size is in 4g or less, Bu Huiyin
The excessive generation bombing of sample size.It is believed that the maximum sample weighting amount of this method chalcopyrite is 4g.
The principle of way of distillation Os element sepatation flows is exactly to utilize OsO4Volatility, if the oxidisability of oxidant is not
By force, Os can not be oxidized to highest valence state (+8 valence), then Os concentration of element will be very low in recovered liquid, when this results in measuring
Higher signal strength can not be obtained.It can be derived that from Fig. 1, when only using inverse chloroazotic acid as oxidant, as sample weighting amount increases
Greatly, sour oxygenation efficiency declines apparent, when sample size is 1g, the oxidisability highest of solution, it means that most of Os is by oxygen
Change to highest price；When sample size is 2g, oxygenation efficiency has dropped one times, it means that even if sample size increases to 2g, due to oxygen
The oxidisability of agent is insufficient, and Os elements therein is made not entirely reach highest price, when signal strength when measurement is with dissolving 1g
The signal strength of acquisition is not much different, rather than twice in imagining.When sample size is 3g, the oxidisability of oxidant reaches most
It is low, illustrate that most of Os is not oxidized to highest price, data above proves, in item of the inverse chloroazotic acid medium as oxidant
Part, simple cannot achieve the purpose that improve signal strength by increasing sample meltage not only, instead can be due to oxidisability not
Foot reduces signal strength.As the addition 1ml HClO in inverse chloroazotic acid medium4Later, oxygenation efficiency is significantly improved, with height
The oxidisability of the increase of chloric acid addition, sample is also continuously improved therewith, and sample size also gradually increases, after sample weighting amount is more than 5g
Blasted pipe phenomenon occurs, does not obtain any data, it is believed that the maximum sample weighting amount of this method chalcopyrite is 4g.
Experimental example 2
Fig. 2 be different proportion oxidant combination oxidisability schematic diagram, shown in a test example as above, excessive sample size with
The gas formed when oxidant reaction can make overpressure excessive and lead to blasted pipe phenomenon, cause sample loss, therefore oxidant
Volume controls within 20ml under normal circumstances.Hydrochloric acid is remained as reproducibility acid, in this experimental example constancy of volume
4ml.It has been investigated that when perchloric acid addition is 4ml, it is not special that nitric acid volume rises to the variation of 8ml oxygenation efficiency by 12ml
It is unapparent, but oxygenation efficiency is less than 4ml HCl, 16ml HNO3、3ml HClO4Combination；When perchloric acid addition rises to 5ml
When, oxygenation efficiency significantly improves；When perchloric acid volume reaches 6ml, oxygenation efficiency reaches highest.However, nitric acid volume be less than 8ml it
Afterwards, oxygenation efficiency declines apparent.It can be seen that perchloric acid addition is to oxygenation efficiency decisive action.Nitric acid addition is in 8ml or more oxygen
Rate variation is little, but declines obviously less than 8ml oxygenation efficiency, even if 6ml HClO are added4Also oxygenation efficiency can not be improved.4ml
HCl、8ml HNO3、6ml HClO4Combination has higher oxygen rate, and oxidant combination is finally determined as 4ml to reduce bombing rate
HCl、8ml HNO3、5ml HClO4, not only reduced oxidizer but also can ensure higher oxygenation efficiency.
Experimental example 3
Table 1 is the flow blank in above-mentioned detection
1 flow blank of table
Table 1 is flow blank, is pg ranks, and lower flow blank is suitable for most of sample.
For the metal sulfide of low Re, Os content, flow blank crosses height and directly affects data result, if blank mistake
Height can not thus react sample for certain low Re, Os content samples it is possible that blank value is higher than the possibility of sample size
Product are really data.Flow blank is lower, and shared ratio is smaller in unknown sample, obtains unknown sample data reliability meeting
It improves.
Experimental example 4
This experimental example is verified for standard sample, and concrete outcome is as shown in table 2
2 standard sample of table is verified
CV is recommendation；AV is average value.
This experimental example is mixed into metal sulfide with molybdenite standard sample JDC (GBW 04435) and HLP (GBW 04436)
Low content sample is simulated, the chalcopyrite of the HLP and 3.8g of the JDC and 0.008g of 0.08g mix, due to molybdenite standard
Sample introduction is smaller, can be ignored for entire oxidation process.Re, Os data uncertainty of standard sample come from
It error caused by the weighing of sample and diluent, the measurement error of ICP-MS and measurement accuracy and 1.02% comes from187Re's
Decay coefficient 1.666 × 10-11a-1Error.By data result as can be seen that the molten sample methods of Carius provided by the invention obtain
The result of normal data is coincide with recommendation, it was demonstrated that the molten sample methods of Carius are feasible.
It should be noted last that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although ginseng
It is described the invention in detail according to preferred embodiment, it should be understood that the foregoing is merely the specific implementations of the present invention
Mode is not intended to limit the scope of protection of the present invention, and all within the spirits and principles of the present invention, that is done any repaiies
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of chemical reagent for the molten sample methods of Carius, which is characterized in that the matter of every 1~4 mass parts sample tie element
Measuring part is：2~4 parts of HCl, HNO38~14 parts and HClO41~6 part.
2. chemical reagent according to claim 1, which is characterized in that the HCl is the HCl that mass fraction is 30~35%
Solution, HNO3The HNO for being 50~60% for mass fraction3Solution, HClO4The HClO for being 70~72% for mass fraction4Solution.
3. a kind of molten sample methods of Carius using chemical reagent described in claims 1 or 22, which is characterized in that include the following steps：
A, 1~4g samples are weighed, and sample is put into Carius pipes, and Carius pipes are placed in -50~-80 DEG C of environment
In；
B, mixed diluent is added in the Carius pipes, sequentially adds HCl, HNO3And HClO4；
C, it seals the Carius using hot melt to manage, and the Carius pipes is heated to 200~220 DEG C, keep 18~
30h；
D, after the completion of heating, after the Carius pipes are cooled to room temperature, liquid therein is taken out, and analyze detection.
4. the molten sample methods of Carius according to claim 3, which is characterized in that in step a and b, weighed using assay balance
The sample and mixed diluent are moved to the sample and the mixed diluent using the same long neck funnel described
In Carius pipes.
5. the molten sample methods of Carius according to claim 3, which is characterized in that sequentially add the chemical reagent in step b
Three kinds of ingredients during, add latter ingredient after former ingredient freezes.
6. the molten sample methods of Carius according to claim 3, which is characterized in that in step c, wait for molten in the Carius pipes
After liquid fully charge, the venturi portion of the Carius pipes is sealed using coal gas-oxygen flame, it will be described after sealing
Carius pipes are put into stainless steel sleeve pipe, and the Carius pipes are put into together with stainless steel sleeve pipe in baking oven, room temperature are kept, in institute
It after stating the substance in Carius pipes and all becoming liquid, begins to warm up, is gradually warming up to 200~220 DEG C, keep 18~30h.
7. the molten sample methods of Carius according to claim 6, which is characterized in that the both ends of the stainless steel sleeve pipe, which are equipped with, lets out
Press hole.
8. the molten sample methods of Carius according to claim 3, which is characterized in that in step d, the Carius pipes are cooled to
After room temperature, the Carius pipes are put into -50~-80 DEG C of environment, wherein after solution fully charge, in the Carius
The venturi portion trepanning pressure release of pipe, in venturi portion cut after pressure release, after be put in refrigerator-freezer and preserve；It, will be described when needing
Carius pipes are placed in ice-water bath, after substance all becomes liquid in Carius pipes, tap the thin of the Carius pipes
After neck portion makes it be broken at cut, liquid therein is taken out.
9. the molten sample methods of Carius according to claim 8, which is characterized in that in step a and step d, obtain -50~-80
The cooling medium of DEG C environment temperature is the mixture of ethyl alcohol and liquid nitrogen.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610031842.2A CN105547802B (en) | 2016-01-18 | 2016-01-18 | A kind of chemical reagent for the molten sample methods of Carius and the molten sample methods of Carius using the chemical reagent |
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| CN201610031842.2A CN105547802B (en) | 2016-01-18 | 2016-01-18 | A kind of chemical reagent for the molten sample methods of Carius and the molten sample methods of Carius using the chemical reagent |
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| CN105547802B true CN105547802B (en) | 2018-09-25 |
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| 汽车尾气净化催化剂中铂、钯和铑的测定;方卫等;《稀有金属材料与工程》;20121231;第41卷(第12期);2254-2260 * |
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