CN106092720A - A kind of Soil K+adsorption measures the micro-wave digestion pre-treating method of total sodium potassium calcium content - Google Patents
A kind of Soil K+adsorption measures the micro-wave digestion pre-treating method of total sodium potassium calcium content Download PDFInfo
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Abstract
The invention discloses a kind of Soil K+adsorption and measure the micro-wave digestion pre-treating method of total sodium potassium calcium content, for measuring the total sodium of soil, total potassium and the content of total calcium, learn from else's experience pretreated pedotheque in politef digestion tube, add concentrated nitric acid, Fluohydric acid. and hydrogen peroxide to described digestion tube, then carry out micro-wave digestion；Cool down after clearing up, use the sample solution catching up with acid instrument that digestion tube is contained to catch up with acid treatment；After catching up with acid, with the nitric acid of 1%～3% (v/v), the residue in digestion tube is dissolved and constant volume, i.e. obtain the solution after soil pre-treatment, then record the content of total sodium potassium calcium of solution.The present invention increase catch up with acid step, measurement result is made more accurately and to avoid the too high damage to experimental apparatus of acidity, soil digestion is the most thorough simultaneously, the degree of accuracy that constituent content measures is higher, in addition the method measuring soil total sodium potassium calcium relative to existing soil pre-treatment, the present invention is the most simple.
Description
Technical field
The present invention relates to environment measuring field, the microwave particularly to the total sodium potassium calcium content of a kind of Soil K+adsorption-measure disappears
Solve pre-treating method.
Background technology
In the scientific research industry of soil investigation, particularly at alkaline land improving with reparation, usually can relate to measure soil
Total sodium, total potassium and the content of total calcium.The mensuration total sodium of soil, total potassium, the committed step of total calcium are soil pre-treating methods, and before this
Processing method is different from the pre-treating method measuring heavy metal-polluted soil, measures the total sodium of soil, total potassium, the soil pre-treatment side of total calcium
Method, it is more prone to occur clear up not exclusively, and measurement error is big and introduces the shortcomings such as impurity, and operating process is loaded down with trivial details and complicated.
At present, the mensuration total sodium of soil, total potassium, the soil pre-treating method of total calcium mainly have Wet and micro-wave digestion, Wet
Clearing up thoroughly, but also existing to clear up takes time and effort acid, program is complicated, loaded down with trivial details, and the pre-treating method of each element determination is not
The problems such as unification；Micro-wave digestion automatic programming controls, and clears up step simple, fast, and sample contamination is few, but micro-wave digestion exists
And clear up thoroughly, and the problem not catching up with acid after clearing up.Clear up not thorough after micro-wave digestion, testing result can be made on the low side；Micro-
Ripple does not catch up with acid after clearing up, and liquid to be measured can be made cannot to keep consistent with the acidity of mark song mark liquid and cause detection error, can simultaneously yet
Damaging experimental apparatus, during as used ICP to measure, the too high meeting of acidity makes the intensity of spectral line decline；When using graphite furnace to measure, acidity mistake
Height can damage graphite-pipe.
Microwave digestion method such as U.S. EPA soil pre-treatment: take and put into 9mL less than the representational sample of 0.500g
Concentrated nitric acid and 3mL Fluohydric acid. (typically) are cleared up 15 minutes, uses suitable laboratory microwave system to heat.Micro-wave digestion journey
Sequence is: reach 180 ± 5 DEG C within the time about less than 5.5 minutes, and keeps 180 ± 5 DEG C within 9.5 minutes, to make reaction complete.It
Rear cooling, processes (may filter that or be centrifuged), dilution metering.It does not catch up with acid step after micro-wave digestion terminates.
The method measuring soil total sodium potassium calcium method such as some existing GB of China, has following several, and it clears up time-consuming consumption
Power consumption acid, program is complicated, loaded down with trivial details, easily causes bigger error or is easily introduced other impurity:
Measure total potassium, the pre-treatment of total sodium (NY/T 1254-1999) in soil: weigh 0.3g (being accurate to 0.0001g) and lead to
Cross the slight slope sample of 0.149mm sieve aperture, be placed in 30mL platinum crucible (or platinum ware), few drops water-wet sample a little.Add people 5mL dense
Perchloric acid solution, then add the dense hydrofluoric acid solution of people 5mL.Careful shake, is allowed to uniformly mix.Crucible is placed on low temperature on electric furnace add
Heat, makes Fluohydric acid. fully act on sample, and prevents it from volatilizing rapidly or spattering mistake.Treat that perchloric acid emits Bai Yanshi, take off crucible slightly
Cold, then add 5mL Fluohydric acid., continuation heating disappears and boils, and is evaporated near dry, takes off pincers pot and adds 3mL perchloric acid again, continues to be evaporated expeling
Unnecessary Fluohydric acid., and steaming and decocting of slowly heating is to having a small amount of white cigarette to emerge, basic removes unnecessary perchloric acid.With 4mL
2mol/l hydrochloric acid adds people and fills in the crucible boiling residue that disappears, and puts low-temperature heat on electric furnace, makes residue dissolve.The most all wash
In 100mL measuring bottle, constant volume, shake up standby.
The pre-treatment of soil total potassium algoscopy (NY/T 87-1988): weigh the wind desiceted soil by 0.149mm aperture sieve
0.1g, is accurate to 0.0001g, contains in platinum crucible or politef crucible, adds concentrated nitric acid 3mL, perchloric acid 0.5mL, is placed in
Electric heating sand-bath or be covered with on the electric hot plate of asbestos cloth, is heated to nitric acid in ventilating kitchen and is caught up with to the greatest extent, and part perchloric acid decomposes and occurs
Substantial amounts of white cigarette, when sample becomes pasty state, takes off cooling.Add Fluohydric acid. 5mL with plastic suction pipet, then add perchloric acid 0.5mL, be placed in
After heating makes the mineral such as silicate decompose in 200-225 DEG C of sand-bath, continue to be heated to remaining Fluohydric acid. and perchloric acid and caught up with to the greatest extent.
Stop emitting Bai Yanshi, take off cooling.Add 3mol/L hydrochloric acid solution 10mL, continue to be heated to residue and dissolve.Take off cooling, add 2%
Boric acid solution 2mL.Quantitatively proceed in 100mL volumetric flask with deionized water, constant volume, mixing (if residue dissolves not exclusively, should be by molten
Liquid is evaporated, repeated hydrogenation fluoric acid 3.5mL, perchloric acid 0.5mL, continues to clear up).This is soil digested solusion.
Measure total potassium, the pre-treatment of total sodium (GB 7874-1987) in soil: weigh 0.3g (being accurate to 0.0001g) and pass through
The pedotheque of 0.1mm sieve aperture, is placed in 30mL platinum crucible (or platinum ware), few drops water-wet sample a little.Add 5mL perchloric acid
Solution, then add people's 5mL hydrofluoric acid solution.Careful shake, is allowed to uniformly mix.Crucible is placed on low-temperature heat on electric furnace, makes hydrogen
Fluoric acid fully acts on sample, and prevents it from volatilizing rapidly or spattering mistake.Treat that perchloric acid emits Bai Yanshi, take off crucible the coldest, then add
5mL Fluohydric acid., continuation heating disappears and boils, and is evaporated near dry.Take off crucible and add 3mL perchloric acid again, continue to be evaporated the unnecessary hydrogen of expeling
Fluoric acid, and steaming and decocting of slowly heating is to having a small amount of white cigarette to emerge, basic removes unnecessary perchloric acid.With 4mL 2mol/L hydrochloric acid
Adding fills in the crucible boiling residue that disappears, and puts low-temperature heat on electric furnace, makes residue dissolve.The most all wash in 100mL measuring bottle,
Constant volume, shakes up standby.
Measure total calcium, the pre-treatment (NY/T 296-995) of total sodium in soil: weigh by 0.149mm aperture sieve wind desiceted soil
0.5000g, is accurate to 0.0001g, is carefully placed in politef crucible, adds concentrated nitric acid 15mL, perchloric acid 2.5mL, is placed in
Electric heating sand-bath or be covered with on the electric hot plate of asbestos cloth, disappears in fume hood and boils to micro-boiling, treats that nitric acid is caught up with to the greatest extent, part perchloric acid divides
Solve substantial amounts of when cigarette, sample become pasty state, take off cooling.Add Fluohydric acid. 5mL with pipet, then add perchloric acid 0.5mL, be placed in
Heat in 200-225 DEG C of sand-bath, after silicate decomposes, continue to be heated to remaining Fluohydric acid. and perchloric acid and caught up with to the greatest extent, stop
Emit Bai Yanshi and take off cooling.Add 3mol/L hydrochloric acid solution 10mL, continue to be heated to residue dissolving and (as residue dissolves not exclusively, answer
Being evaporated by solution, repeated hydrogenation fluoric acid 3-5mL, perchloric acid 0.5mL continue to clear up), take off cooling, add 20g/L boric acid solution 2mL,
Quantitatively proceeding in 250mL volumetric flask with water, constant volume, this is soil digested solusion.
Summary of the invention
The present invention provides the micro-wave digestion pre-treating method of the total sodium potassium calcium content of a kind of Soil K+adsorption-measure, existing to solve
There is drawbacks described above in technology.
Technical scheme is as follows:
The micro-wave digestion pre-treating method of the total sodium potassium calcium content of a kind of Soil K+adsorption-measure, comprises the following steps:
(1) the pretreated particle diameter of the learning from else's experience pedotheque less than 0.5mm is in politef digestion tube, to described
Digestion tube adds concentrated nitric acid, Fluohydric acid. and hydrogen peroxide, then carries out micro-wave digestion；
(2) cool down after micro-wave digestion terminates, use the sample solution catching up with acid instrument that digestion tube is contained to catch up with acid treatment, catch up with
Acid instrument is set to 200 DEG C, as sample solution residue about 1mL, adds perchloric acid to it, then proceedes to catch up with acid little to solution
In 1mL；
(3), after catching up with acid, with the nitric acid of 1%～3% (v/v), the residue in digestion tube is dissolved and constant volume,
Obtain the solution after soil pre-treatment, then record the content of total sodium potassium calcium of solution after described soil pre-treatment.
The most preferably, the capacity of described digestion tube is 50mL, and the weight of the pedotheque weighed is for being less than
0.5000g, degree of accuracy is 0.0001g, and the weight of described pedotheque is preferably 0.2500g.
The most preferably, the amount of the concentrated nitric acid of addition, Fluohydric acid. and hydrogen peroxide is respectively 9mL, 3mL and 2mL, adds
The consumption of perchloric acid is 2mL.
The most preferably, the step of described micro-wave digestion is followed successively by: 1000w climbs 2 minutes to 100 DEG C time；
1000w climbs 1.5 minutes to 150 DEG C time；1000w climbs 1.5 minutes to 185 DEG C time, keeps 15 minutes.
The most preferably, during described step 2 catches up with acid, the sample solution that described digestion tube contains is the most competent
Dry up.
The most preferably, it is pure that concentrated nitric acid, Fluohydric acid., hydrogen peroxide and perchloric acid used is top grade.
Compared with prior art, beneficial effects of the present invention is as follows:
A kind of micro-wave digestion pre-treating method of the total sodium potassium calcium content of the Soil K+adsorption of the oneth, present invention-measure, compared to
The microwave digestion method of U.S. EPA soil pre-treatment, its advantage has: optimize digestion process, makes clearing up of soil more complete；
After micro-wave digestion terminate, increase by one catch up with acid step so that clear up more completely, measurement result the most accurate, also avoid simultaneously
The acidity too high damage to experimental apparatus；
A kind of micro-wave digestion pre-treating method of the total sodium potassium calcium content of the Soil K+adsorption of the 2nd, present invention-measure, compared to
The existing GB of China measures the method for soil total sodium potassium calcium, which obviates the various shortcomings of GB, takes time and effort acid as cleared up,
Program is complicated, loaded down with trivial details, so that error is big or is easily introduced other impurity, and the pre-treating method disunity etc. of each element determination is asked
Topic, the method for the present invention is simple to operate, fast, and sample contamination is few and more easy.
Certainly, the either method implementing the present invention it is not absolutely required to reach all the above advantage simultaneously.(represent
Do not understand that what does this mean)
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate this
Bright, rather than limit protection scope of the present invention.Those skilled in the art are according to changing that the present invention makes in actual applications
Enter and adjust, still falling within protection scope of the present invention.
The micro-wave digestion pre-treating method of the total sodium potassium calcium content of a kind of Soil K+adsorption of the present invention-measure, including following step
Rapid:
(1) learn from else's experience pretreatment the pedotheque less than 0.5mm of the particle diameter after sieving, in 50mL politef digestion tube
In, weight is less than 0.5000g, and degree of accuracy is 0.0001g, adds 9mL concentrated nitric acid, 3mL Fluohydric acid. and 2mL to described digestion tube
Hydrogen peroxide, when adding above-mentioned acid, is flushed to be stained with the soil clearing up on tube wall at the bottom of pipe with acid simultaneously, then carries out microwave and disappear
Solving, it is pure that concentrated nitric acid, Fluohydric acid., hydrogen peroxide and perchloric acid used is top grade；
(2) step of the micro-wave digestion described in is followed successively by: 1000w climbs 2 minutes to 100 DEG C time；1000w climbs the time
1.5 minutes to 150 DEG C；1000w climbs 1.5 minutes to 185 DEG C time, keeps 15 minutes；
(3) cooling down after micro-wave digestion terminates, digestion solution is not required to transfer to other vessel, only need to continue to carry out in digestion tube
Catch up with acid, use the sample solution catching up with acid instrument that digestion tube is contained to catch up with acid treatment, catch up with acid instrument to be set to 200 DEG C, when sample is molten
During liquid residue about 1mL, add 2mL perchloric acid to it, then proceed to catch up with acid to solution less than 1mL, during catching up with acid, institute
The sample solution that the digestion tube stated contains can not dry up, and otherwise can have a strong impact on measurement result.This catches up with acid process to be equivalent to be similar to
Wet, unlike Wet, this catch up with acid step be to proceed in digestion tube, the most there is not wet method and disappear
Solve complex operation, be easily introduced the problems such as impurity；
(4), after catching up with acid, with the nitric acid of 1%～3% (v/v), the residue in digestion tube is dissolved and constant volume,
Obtain the solution after soil pre-treatment, do suitably process, then record described soil with atomic absorption spectrophotometer TAS-990
The content of total sodium potassium calcium of solution after earth pre-treatment.
In order to better illustrate the micro-wave digestion pre-treating method of the total sodium potassium calcium content of the Soil K+adsorption of the present invention-measure,
Compared to U.S.'s EAP microwave digestion method and China's GB standard determination method, the measuring accuracy of the method for the present invention is high, sample
Product pollute less, simple to operation and to instrument without damage.
Embodiment 1
(1) learn from else's experience pretreatment the pedotheque less than 0.5mm of the particle diameter after sieving, in 50mL politef digestion tube
In, weight is 0.2500g, and degree of accuracy is 0.0001g, adds 9mL concentrated nitric acid, 3mL Fluohydric acid. and 2mL to described digestion tube double
Oxygen water, when adding above-mentioned acid, is flushed to be stained with the soil clearing up on tube wall at the bottom of pipe with acid simultaneously, then carries out micro-wave digestion,
It is pure that concentrated nitric acid, Fluohydric acid., hydrogen peroxide and perchloric acid used is top grade；
(2) step of the micro-wave digestion described in is followed successively by: 1000w climbs 2 minutes to 100 DEG C time；1000w climbs the time
1.5 minutes to 150 DEG C；1000w climbs 1.5 minutes to 185 DEG C time, keeps 15 minutes；
(3) cooling down after micro-wave digestion terminates, digestion solution is not required to transfer to other vessel, only need to continue to carry out in digestion tube
Catch up with acid, use the sample solution catching up with acid instrument that digestion tube is contained to catch up with acid treatment, catch up with acid instrument to be set to 200 DEG C, when sample is molten
During liquid residue about 1mL, add 2mL perchloric acid to it, then proceed to catch up with acid to solution less than 1mL, during catching up with acid, institute
The sample solution that the digestion tube stated contains can not dry up, and otherwise can have a strong impact on measurement result.This catches up with acid process to be equivalent to be similar to
Wet, unlike Wet, this catch up with acid step be to proceed in digestion tube, the most there is not wet method and disappear
Solve complex operation, be easily introduced the problems such as impurity；
(4), after catching up with acid, with the nitric acid of 1%～3% (v/v), the residue in digestion tube is dissolved and constant volume,
Obtain the solution after soil pre-treatment, do suitably process, then record described soil with atomic absorption spectrophotometer TAS-990
The content of total sodium potassium calcium of solution after earth pre-treatment, measurement result is as shown in Table 1.
Embodiment 2
(1) learn from else's experience pretreatment the pedotheque less than 0.5mm of the particle diameter after sieving, in 50mL politef digestion tube
In, weight is 0.3000g, and degree of accuracy is 0.0001g, adds 9mL concentrated nitric acid, 3mL Fluohydric acid. and 2mL to described digestion tube double
Oxygen water, when adding above-mentioned acid, is flushed to be stained with the soil clearing up on tube wall at the bottom of pipe with acid simultaneously, then carries out micro-wave digestion,
It is pure that concentrated nitric acid, Fluohydric acid., hydrogen peroxide and perchloric acid used is top grade；
(2) step of the micro-wave digestion described in is followed successively by: 1000w climbs 2 minutes to 100 DEG C time；1000w climbs the time
1.5 minutes to 150 DEG C；1000w climbs 1.5 minutes to 185 DEG C time, keeps 15 minutes；
(3) cooling down after micro-wave digestion terminates, digestion solution is not required to transfer to other vessel, only need to continue to carry out in digestion tube
Catch up with acid, use the sample solution catching up with acid instrument that digestion tube is contained to catch up with acid treatment, catch up with acid instrument to be set to 200 DEG C, when sample is molten
During liquid residue about 1mL, add 2mL perchloric acid to it, then proceed to catch up with acid to solution less than 1mL, during catching up with acid, institute
The sample solution that the digestion tube stated contains can not dry up, and otherwise can have a strong impact on measurement result.This catches up with acid process to be equivalent to be similar to
Wet, unlike Wet, this catch up with acid step be to proceed in digestion tube, the most there is not wet method and disappear
Solve complex operation, be easily introduced the problems such as impurity；
(4), after catching up with acid, with the nitric acid of 1%～3% (v/v), the residue in digestion tube is dissolved and constant volume,
Obtain the solution after soil pre-treatment, do suitably process, then record total sodium potassium calcium of solution after described soil pre-treatment
Content, measurement result is as shown in Table 1.
Embodiment 3
(1) learn from else's experience pretreatment the pedotheque less than 0.5mm of the particle diameter after sieving, in 50mL politef digestion tube
In, weight is 0.4000g, and degree of accuracy is 0.0001g, adds 9mL concentrated nitric acid, 3mL Fluohydric acid. and 2mL to described digestion tube double
Oxygen water, when adding above-mentioned acid, is flushed to be stained with the soil clearing up on tube wall at the bottom of pipe with acid simultaneously, then carries out micro-wave digestion,
It is pure that concentrated nitric acid, Fluohydric acid., hydrogen peroxide and perchloric acid used is top grade；
(2) step of the micro-wave digestion described in is followed successively by: 1000w climbs 2 minutes to 100 DEG C time；1000w climbs the time
1.5 minutes to 150 DEG C；1000w climbs 1.5 minutes to 185 DEG C time, keeps 15 minutes；
(3) cooling down after micro-wave digestion terminates, digestion solution is not required to transfer to other vessel, only need to continue to carry out in digestion tube
Catch up with acid, use the sample solution catching up with acid instrument that digestion tube is contained to catch up with acid treatment, catch up with acid instrument to be set to 200 DEG C, when sample is molten
During liquid residue about 1mL, add 2mL perchloric acid to it, then proceed to catch up with acid to solution less than 1mL, during catching up with acid, institute
The sample solution that the digestion tube stated contains can not dry up, and otherwise can have a strong impact on measurement result.This catches up with acid process to be equivalent to be similar to
Wet, unlike Wet, this catch up with acid step be to proceed in digestion tube, the most there is not wet method and disappear
Solve complex operation, be easily introduced the problems such as impurity；
(4), after catching up with acid, with the nitric acid of 1%～3% (v/v), the residue in digestion tube is dissolved and constant volume,
Obtain the solution after soil pre-treatment, do suitably process, then record described soil with atomic absorption spectrophotometer TAS-990
The content of total sodium potassium calcium of solution after earth pre-treatment, measurement result is as shown in Table 1.
Embodiment 4
(1) learn from else's experience pretreatment the pedotheque less than 0.5mm of the particle diameter after sieving, in 50mL politef digestion tube
In, weight is 0.3500g, and degree of accuracy is 0.0001g, adds 9mL concentrated nitric acid, 3mL Fluohydric acid. and 2mL to described digestion tube double
Oxygen water, when adding above-mentioned acid, is flushed to be stained with the soil clearing up on tube wall at the bottom of pipe with acid simultaneously, then carries out micro-wave digestion,
It is pure that concentrated nitric acid, Fluohydric acid., hydrogen peroxide and perchloric acid used is top grade；
(2) step of the micro-wave digestion described in is followed successively by: 1000w climbs 2 minutes to 100 DEG C time；1000w climbs the time
1.5 minutes to 150 DEG C；1000w climbs 1.5 minutes to 185 DEG C time, keeps 15 minutes；
(3) cooling down after micro-wave digestion terminates, digestion solution is not required to transfer to other vessel, only need to continue to carry out in digestion tube
Catch up with acid, use the sample solution catching up with acid instrument that digestion tube is contained to catch up with acid treatment, catch up with acid instrument to be set to 200 DEG C, when sample is molten
During liquid residue about 1mL, add 2mL perchloric acid to it, then proceed to catch up with acid to solution less than 1mL, during catching up with acid, institute
The sample solution that the digestion tube stated contains can not dry up, and otherwise can have a strong impact on measurement result.This catches up with acid process to be equivalent to be similar to
Wet, unlike Wet, this catch up with acid step be to proceed in digestion tube, the most there is not wet method and disappear
Solve complex operation, be easily introduced the problems such as impurity；
(4), after catching up with acid, with the nitric acid of 1%～3% (v/v), the residue in digestion tube is dissolved and constant volume,
Obtain the solution after soil pre-treatment, do suitably process, then record described soil with atomic absorption spectrophotometer TAS-990
The content of total sodium potassium calcium of solution after earth pre-treatment, measurement result is as shown in Table 1.
Embodiment 5
(1) learn from else's experience pretreatment the pedotheque less than 0.5mm of the particle diameter after sieving, in 50mL politef digestion tube
In, weight is 0.2000g, and degree of accuracy is 0.0001g, adds 9mL concentrated nitric acid, 3mL Fluohydric acid. and 2mL to described digestion tube double
Oxygen water, when adding above-mentioned acid, is flushed to be stained with the soil clearing up on tube wall at the bottom of pipe with acid simultaneously, then carries out micro-wave digestion,
It is pure that concentrated nitric acid, Fluohydric acid., hydrogen peroxide and perchloric acid used is top grade；
(2) step of the micro-wave digestion described in is followed successively by: 1000w climbs 2 minutes to 100 DEG C time；1000w climbs the time
1.5 minutes to 150 DEG C；1000w climbs 1.5 minutes to 185 DEG C time, keeps 15 minutes；
(3) cooling down after micro-wave digestion terminates, digestion solution is not required to transfer to other vessel, only need to continue to carry out in digestion tube
Catch up with acid, use the sample solution catching up with acid instrument that digestion tube is contained to catch up with acid treatment, catch up with acid instrument to be set to 200 DEG C, when sample is molten
During liquid residue about 1mL, add 2mL perchloric acid to it, then proceed to catch up with acid to solution less than 1mL, during catching up with acid, institute
The sample solution that the digestion tube stated contains can not dry up, and otherwise can have a strong impact on measurement result.This catches up with acid process to be equivalent to be similar to
Wet, unlike Wet, this catch up with acid step be to proceed in digestion tube, the most there is not wet method and disappear
Solve complex operation, be easily introduced the problems such as impurity；
(4), after catching up with acid, with the nitric acid of 1%～3% (v/v), the residue in digestion tube is dissolved and constant volume,
Obtain the solution after soil pre-treatment, do suitably process, then record described soil with atomic absorption spectrophotometer TAS-990
The content of total sodium potassium calcium of solution after earth pre-treatment, measurement result is as shown in Table 1.
Duplicate Samples determination data (unit: g/kg) in table 1 embodiment
Additionally, above-described embodiment 1～5 is also recorded the meansigma methods of total Na, K, Ca and uses U.S. EPA micro-wave digestion by the present invention
The measured value of method and China's standard method is contrasted, and as shown in table 2, result shows, accurate with the method mark of the present invention
Total Na, K, Ca value of soil sample is more near the mark the standard value of soil sample, and fluctuation range is little, and degree of accuracy is high.
Table 2 (unit: g/kg)
The present invention is to increase one and catches up with acid step so that measurement result is more accurately and to avoid acidity too high to experiment instrument
The damage of device, soil digestion is the most thorough simultaneously, and the degree of accuracy that constituent content measures is the highest.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.Preferred embodiment is the most detailed
Describe all of details, be also not intended to the detailed description of the invention that this invention is only described.Obviously, according to the content of this specification,
Can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is to preferably explain the present invention
Principle and actual application so that skilled artisan can be best understood by and utilize the present invention.The present invention is only
Limited by claims and four corner thereof and equivalent.
Claims (6)
1. the micro-wave digestion pre-treating method of the total sodium potassium calcium content of a Soil K+adsorption-measure, it is characterised in that include following step
Rapid:
(1) the pretreated particle diameter of the learning from else's experience pedotheque less than 0.5mm, in politef digestion tube, is cleared up to described
Pipe adds concentrated nitric acid, Fluohydric acid. and hydrogen peroxide, then carries out micro-wave digestion；
(2) cool down after micro-wave digestion terminates, use the sample solution catching up with acid instrument that digestion tube is contained to catch up with acid treatment, catch up with acid instrument
It is set to 200 DEG C, as sample solution residue about 1mL, adds perchloric acid to it, then proceed to catch up with acid to solution to be less than
1mL；
(3), after catching up with acid, with the nitric acid of 1%～3% (v/v), the residue in digestion tube is dissolved and constant volume, obtain
Solution after soil pre-treatment, then records the content of total sodium potassium calcium of solution after described soil pre-treatment.
The micro-wave digestion pre-treating method of the total sodium potassium calcium content of a kind of Soil K+adsorption the most according to claim 1-measure, its
Being characterised by, the capacity of described digestion tube is 50mL, and the weight of the pedotheque weighed is for less than 0.5000g, and degree of accuracy is
0.0001g。
The micro-wave digestion pre-treating method of the total sodium potassium calcium content of a kind of Soil K+adsorption the most according to claim 2-measure, its
Being characterised by, the amount of the concentrated nitric acid of addition, Fluohydric acid. and hydrogen peroxide is respectively 9mL, 3mL and 2mL, adds the consumption of perchloric acid
For 2mL.
The micro-wave digestion pre-treating method of the total sodium potassium calcium content of a kind of Soil K+adsorption the most according to claim 1-measure, its
Being characterised by, the step of described micro-wave digestion is followed successively by: 1000w climbs 2 minutes to 100 DEG C time；1000w climbs the time
1.5 minutes to 150 DEG C；1000w climbs 1.5 minutes to 185 DEG C time, keeps 15 minutes.
The micro-wave digestion pre-treating method of the total sodium potassium calcium content of a kind of Soil K+adsorption the most according to claim 1-measure, its
Being characterised by, during described step 2 catches up with acid, the sample solution that described digestion tube contains can not dry up.
The micro-wave digestion pre-treating method of the total sodium potassium calcium content of a kind of Soil K+adsorption the most according to claim 1-measure, its
Being characterised by, it is pure that concentrated nitric acid, Fluohydric acid., hydrogen peroxide and perchloric acid used is top grade.
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| CN112014174A (en) * | 2020-07-14 | 2020-12-01 | 中国科学院城市环境研究所 | Method for measuring phosphorus content in livestock and poultry manure and biochar thereof |
| CN112649276A (en) * | 2020-12-30 | 2021-04-13 | 中国地质大学（武汉） | Method for digesting geological sample by using ammonium bifluoride or ammonium fluoride |
| CN113588397A (en) * | 2021-07-12 | 2021-11-02 | 江苏久诚检验检测有限公司 | Pretreatment method for digesting soil sample by constant temperature shaking table |
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