CN109682662A - A kind of soil alkali fusion pre-treating method - Google Patents
A kind of soil alkali fusion pre-treating method Download PDFInfo
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Abstract
The invention belongs to technical field of analytical chemistry, more particularly to a kind of soil alkali fusion pre-treating method, the pre-treating method includes sample treatment, pre- resolution, it clears up again, post-treating and other steps, pre-treating method is simple and easy, it is most of to be automatically controlled via system, manually-operated error degree can be greatly reduced, and in actual process, it can be according to the difference of metallic element, selectively operated, such as metallic element manganese, barium etc. can directly omit pre- resolution step and directly carry out alkali fusion processing, and metallic element tin etc. is needed according to above-mentioned steps strict implement, expand the actually detected range of the above method.It is incorporated in specific apparatus by the step of simplifying pre-treatment, and by simplified step, greatly improves the efficiency of sample pre-treatments.
Description
Technical field
The invention belongs to technical field of analytical chemistry, and in particular to a kind of soil alkali fusion pre-treating method.
Background technique
In metallic element, heavy metal element cannot be decomposed by the microorganisms in soils and sediments, can constantly be accumulated, and be
Biology is enriched with, and is transmitted by food chain, is threatened to the mankind or even some heavy metals can be by micro- life in soil and bed mud
Object is converted into the bigger compound of toxicity.
Most of measurement of metal is using sour Acid system in many environmental monitorings at present, using sulfuric acid, perchloric acid, nitric acid
Soil is carried out to totally disappeared solution with the mode of hydrofluoric acid etc., finally uses inductively coupled plasma atomic emission spectrometer or atom
The instruments such as luminoscope are measured.But some elements such as metallic tin, potassium, sodium, calcium, magnesium, iron, aluminium, silicon is molten under the conditions of acid is molten
Efficiency is not fully, also and unstable out, therefore the proposition of soil alkali fusion is the supplement and improvement to acid extracting.Due to soil
The pretreatment mode whole process of alkali fusion needs manual operations, and analysis time is long, and operation is not easy enough, and individual metal element needs
Hydrofluoric acid is added to clear up, there are health risks to operator, before soil digestion device on the market is not suitable for alkali fusion at present
Manage device, it is therefore desirable to develop a kind of safe, automatic and easy soil alkali fusion pretreating device.The soil handled by alkali fusion
The monitoring data of the elements such as tin, iron, calcium, magnesium, aluminium all there is good accuracy and the rate of recovery.
For the detection accuracy of heavy metals in soil, publication number 107167361A discloses a huge sum of money in a kind of soil
Belong to content analysis method, by alkaline hydrolysis, acidolysis, concentration, measurement and etc. be measured, but its essence is alkaline solution treatments
With acid solution processing, the detection of Partial Elements can not be well adapted to, and risk is larger.
Summary of the invention
In view of the above problems, the present invention provides that a kind of accuracy height, high degree of automation, applicability be wide, detection
Fast, the highly-safe soil alkali fusion pre-treating method of speed.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of soil alkali fusion pre-treating method, includes the following steps:
(1) sample treatment: re-sieving after pedotheque is air-dried, is ground, is mixed measures moisture content；
(2) pre- resolution: the sample for weighing known aqueous rate is placed in crucible, and crucible is placed on alkali fusion meausring apparatus,
After acid digestion solution is added dropwise into crucible, transfer crucible is heated into temperature controllable heating digestion instrument and cools down pre-
Clear up sample；
(3) it clears up again: pre- resolution sample is transferred on alkali fusion meausring apparatus, the prefabricated mixing examination of alkali fusion is added into crucible
Agent, then crucible is transferred in temperature controllable heating digestion instrument and carries out reheating processing and so cooling that clear up sample again；
(4) it post-processes: sample will be cleared up again and be transferred on alkali fusion meausring apparatus, distilled water is first added into crucible, then add
Acid reagent obtains soil digested solusion.
Pedotheque pre-treating method of the invention is simple and easy, most of to automatically control via system, can substantially drop
Low manually-operated error degree, and in actual process, it can selectively be grasped according to the difference of metallic element
Make, such as metallic element manganese, barium can directly omit pre- resolution step and directly carry out alkali fusion processing, and metallic element tin etc. needs
According to above-mentioned steps strict implement, the actually detected range of the above method is expanded.By the step of simplifying pre-treatment, and will be simple
Step after change incorporates in specific apparatus, greatly improves the efficiency of sample pre-treatments.And moisture content is detection soil
Arbitrary element contained by earth kind requires the amount of measured in advance, aqueous to carry out when calculating elements content after subsequent instrumentation measured value
The deduction of rate.
Preferably, the mesh number of step (1) described sieve is 80-120 mesh.
Preferably, the material of step (2) described crucible includes one or both of platinum, corundum.
Preferably, the alkali fusion meausring apparatus includes that induction claims the solid reagent device added and the liquid quantitatively added examination
Agent device.
Further preferably, alkali fusion meausring apparatus bottom is equipped with vortex homogenous unit and induction weighing device, the vortex
Homogenous unit is for producing soil digested solusion.
Further preferably, the vortex homogenous unit is equipped with transparent safety shield.
Further preferably, the liquid reagent device includes distilled water bottle, sulfuric acid solution bottle, acid of hydrochloric acid and nitric acid mixed solution
Bottle, acid bottle, eight ways valve and pipeline.
Further preferably, the eight ways valve includes valve body and spool, and the valve body is equipped with eight liquid in-out mouths.
Further preferably, the solid reagent device includes solid reagent bottle and adds basic solvent pipe, and described plus alkalinity is molten
Agent pipe and the pipeline are arranged above the vortex homogenous unit.
Preferably, shifting crucible using three-dimensional machinery arm.
Further preferably, the three-dimensional machinery arm passes through support frame as described above activity.
Preferably, step (2) the acid digestion solution is hydrofluoric acid, dripping quantity is quantitative 10ml.As needed for sample
Quality be not very big, so being excessively added in fact, it is intended to sufficiently molten after quantitatively adding the hydrofluoric acid of 10ml in crucible
Pedotheque is solved, the metallic element part for avoiding the need for detection remains in sample, and testing result is caused to have the error of increasing.
Preferably, temperature controllable heating digestion instrument include temperature automatically controlled timing heated case, acid mist absorbing device with
And vacuum pump.
Further preferably, the temperature automatically controlled timing heated case top is equipped with porous venting plate and retractable door.
Further preferably, the acid mist absorbing device setting is in the retractable door side, the vacuum pump and the acid
Mist absorption plant connects.
The present invention by by the pre-treating method of soil all/be partially transferred in specific apparatus and carry out, due to
In the treatment process of pedotheque, it is understood that there may be stronger caustic acid, and the acid of sample is dissolved in closed environment and is carried out,
And hydrofluoric acid is added using dropper, alkali fusion agent is added using reagent bottle, crucible transfer is carried out using mechanical arm, is before ensure that
Safety in treatment process, and then artificial mode is replaced by most of machinery, efficiency is improved, so that in the same time
Manageable sample size is significantly promoted, and is laid the foundation for fast and accurately test sample.
Simultaneously, it is contemplated that the volatilization of hydrofluoric acid is corroded, and wraps up high temperature resistant and anti-acid etching materials in heater box pars intramuralis, and
It installs purification system additional, is taken away absorption in time convenient for acid mist.
Preferably, the temperature of step (2) described heating is 95-105 DEG C, the time of heating is 18-22min.
Preferably, the time of step (2) described cooling is 18-22min, it is cooled to 20-30 DEG C.
Preferably, the prefabricated mix reagent of step (3) alkali fusion includes sodium carbonate, lithium tetraborate, lithium metaborate, peroxide
Change one of sodium or a variety of.
Further preferably, in the prefabricated mix reagent of addition alkali fusion, sodium carbonate first should be placed in crucible bottom, then add it
His reagent.
Preferably, the temperature of step (3) described reheating is 950-1050 DEG C, time 25-35min.
Preferably, step (3) is described to be cooled to 250-350 DEG C.After being cooled to 300 DEG C or so and capable of guaranteeing soil alkali fusion
Convenient for being extracted, because if being room temperature, part alkali fusion agent includes that soil can be adsorbed on sidewall of crucible, is not easy to be extracted by solution,
It in turn results in and causes certain loss.
Preferably, step (4) described acid reagent includes one of acid of hydrochloric acid and nitric acid mixed solution, sulfuric acid solution or two
Kind.
Preferably, being to pass through eight ways valve during above-mentioned addition acidity digestion solution, distilled water, acid reagent
It is converted.Reagent switching is carried out using valve, to save the time for cleaning dropper when conventional reagent addition, improves effect
Rate.
Compared with prior art, the present invention has the advantage that
(1) present invention use based on alkali fusion, and it is first sufficiently to extract metal from sample for the main resolution means supplemented by acid is molten
Element guarantees the accuracy of testing result.
(2) pre-treatment step part of the invention carries out in apparatus, enormously simplifies manpower, and can significantly mention
Rise the safety of pre-treatment.
(3) pre-treating method of the invention can be adjusted according to actually detected element, wide adaptation range.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of soil alkali fusion pretreating device of the present invention.
In figure, 100, crucible；200, alkali fusion meausring apparatus；210, solid reagent device；211, solid reagent bottle；212, add
Basic solvent pipe；220, liquid reagent device；221, distilled water bottle；222, sulfuric acid solution bottle；223, acid of hydrochloric acid and nitric acid mixed solution
Bottle；224, acid bottle；225, pipeline；226, eight ways valve；230, vortex homogenous unit；240, incude weighing device；250, transparent
Safty shield；300, temperature controllable heats digestion instrument；310, temperature automatically controlled timing heated case；311, porous venting plate；312,
Retractable door；320, acid mist absorbing device；330, vacuum pump；400, three-dimensional machinery arm；500, support frame.
Specific embodiment
The following is specific embodiments of the present invention, and technical scheme of the present invention will be further described, but the present invention is simultaneously
It is not limited to these embodiments.
As shown in Figure 1, being soil alkali fusion pretreating device of the present invention, comprising:
Crucible 100, for holding pedotheque.
Alkali fusion meausring apparatus 200, alkali fusion meausring apparatus 200 include that induction claims the solid reagent device 210 added and quantitatively adds
The liquid reagent device 220 added can provide the weighed alkaline digestion agent of sensibility reciprocal but also provide quantitative digestion solution.
Temperature controllable heat digestion instrument 300, temperature controllable heat digestion instrument 300 include temperature automatically controlled timing heated case 310,
Acid mist absorbing device 320 and vacuum pump 330, pedotheque can be put into temperature automatically controlled timing heated case after Hydrolytic acid is added
In 310, the regular hour is set and temperature heats it, openable vacuum pump 330 makes in heating soil sample thereafter
The acid gas of volatilization enters in acid mist absorbing device 320.
Three-dimensional machinery arm 400, three-dimensional machinery arm 400 are used to shift the position of crucible 100, can claim crucible 100 from alkali fusion
It measures and realizes transfer between device 200 and temperature automatically controlled timing heated case 310, realize full automatic treatment.
Preferably, as shown in Figure 1, temperature automatically controlled 310 top of timing heated case is equipped with porous venting plate 311 and retractable door
312, in the work of temperature automatically controlled timing heated case 310, heater box integral sealing need to be can be only achieved heating effect, so setting
Retractable door 312 is set to block ventilation hole, meanwhile, it needs for acid mist to be discharged after heating is completed, therefore porous venting plate is arranged
311 acid mist is discharged.
Preferably, as shown in Figure 1, acid mist absorbing device 320 is arranged in retractable 312 side of door, vacuum pump 330 and acid mist
Absorption plant 320 connects, and when vacuum pump 330 is run, drives acid mist absorbing device 320 to generate suction, while retractable door 312 is beaten
It opens, comes out the acid gas in temperature automatically controlled timing heated case 310 from porous venting plate 311 and absorbed by acid mist absorbing device 320.
Preferably, as shown in Figure 1,200 bottom of alkali fusion meausring apparatus is equipped with vortex homogenous unit 230 and induction weighing device
240, vortex homogenous unit 230 is the use when weighing alkalinity disappears flux for producing soil digested solusion, induction weighing device 240.
Preferably, as shown in Figure 1, liquid reagent device 220 includes distilled water bottle 221, sulfuric acid solution bottle 222, hydrochloric acid nitre
Acid-mixed closes solution bottle 223, acid bottle 224 and pipeline 225, is respectively provided with different solution reagents.
It is further preferred that eight ways valve 226 includes valve body and spool (being not marked in figure), valve body is equipped with eight liquid in-outs
Mouthful, spool is equipped with four arced flow paths, and the both ends of four arced flow paths are corresponding with liquid in-out mouth respectively, forms four and leads to
Road is equipped with quantity tube (being not marked in figure) in channel, when rotational valve core, so that import is separately connected before and after exchanging with outlet
Different quantity tubes forms four kinds of different logical liquid status.
Preferably, pipeline 225 is telescopic tube, connects with pipeline and (is not marked in figure) equipped with gripper through gripper control
The residence time above each crucible 100 of pipeline 225 is arranged in chip in system processed, then drives pipeline by gripper
225 flexible a certain distance realize that each crucible 100 can quantitatively automatic liquid-feeding.
It is further preferred that as shown in Figure 1, vortex homogenous unit 230 is equipped with transparent safety shield 250, transparent peace
Full protection cover 250 can be automatically turned on or be closed, while be guaranteed after adding Hydrolytic acid, and gas will not evaporate into air,
Simultaneously convenient for observation.
Preferably, as shown in Figure 1, solid reagent device 210 includes solid reagent bottle 211 and adds basic solvent pipe 212, add
Basic solvent pipe 212 and pipeline 225 are arranged above vortex homogenous unit 230, when crucible 100 is transferred to addition basic solvent
It, can be respectively by adding basic solvent pipe 212 and pipeline 225 to be added distintegrant and decompose when solid area or liquid regions
Liquid.
Preferably, as shown in Figure 1, further including support frame 500, three-dimensional machinery arm 400 passes through 500 activity of support frame.
The present invention using three-dimensional machinery armband move crucible the region of the addition region of solid reagent, adding liquid reagent with
And position transfer is carried out between temperature automatically controlled timing heated case, the automation of realization device is operated without employee, guarantees employee's peace
Entirely, it improves efficiency simultaneously.
Embodiment 1
(1) sample treatment: standard soil GBW07405 (GSS-5), standard soil GBW07453 (GSS-24), standard is heavy
Re-sieving after 4 kinds of product object GBW07311 (GSD-11), practical soil samples are air-dried respectively, ground, mixing, measures aqueous respectively
Rate；
(2) clear up: 4 kinds of samples for weighing 0.5g known aqueous rate respectively are placed in corundum crucible, respectively place crucible
It is respectively placed in crucible bottom on alkali fusion meausring apparatus, first weighing 1.0g sodium carbonate, then adds 0.1g lithium tetraborate, 0.4g respectively
Crucible is transferred in the heater box of temperature controllable heating digestion instrument one by one using mechanical arm, is added at 1000 DEG C by lithium metaborate
Hot 30min, and be cooled to 300 DEG C and obtain 4 kinds of resolution samples；
(4) it post-processes: 4 kinds of resolution samples is transferred to one by one on alkali fusion meausring apparatus using mechanical arm, respectively into crucible
Distilled water is first added, then adds nitric acid hydrochloric acid mixed solution and obtains 4 kinds of soil digested solusions.
4 kinds of soil digested solusions that embodiment 1 obtains are measured respectively by plasma emission spectrometer, as a result such as table 1-
Shown in 4:
Table 1: the testing result of standard soil GBW07405 (GSS-5)
Table 2: the testing result of standard soil GBW07453 (GSS-24)
Table 3: the testing result of standard deposition object GBW07311 (GSD-11)
Table 4: the testing result of practical soil
After the device, the accuracy of soils and sediments is able to satisfy the deviation requirement of standard sample, and it is opposite
For standard deviation in 0.29-3.0%, precision is good, and practical pedotheque recovery of standard addition is in 98.3%-99.8%.
Embodiment 2
(1) sample treatment: standard soil GBW07405 (GSS-5), standard soil GBW07453 (GSS-24), standard is heavy
Re-sieving after 4 kinds of product object GBW07312 (GSD-12), practical soil samples are air-dried respectively, ground, mixing, measures aqueous respectively
Rate；
(2) pre- resolution: 4 kinds of samples for weighing 0.5g known aqueous rate respectively are placed in corundum crucible, and crucible is placed in
On alkali fusion meausring apparatus, after 10ml hydrofluoric acid is added dropwise into crucible, shifts crucible to temperature controllable heating one by one using mechanical arm and disappear
In the heater box for solving device, 20min is heated at 100 DEG C, and cooling 20min obtains pre- resolution sample to room temperature；
(3) it clears up again: pre- resolution sample being transferred on alkali fusion meausring apparatus respectively, 5g sodium peroxide is added into crucible,
Crucible is transferred in the heater box of temperature controllable heating digestion instrument one by one again, the reheating 15min at 700 DEG C, and cooling
4 kinds of resolution samples are obtained to 300 DEG C；
(4) it post-processes: 4 kinds of resolution samples is transferred to one by one on alkali fusion meausring apparatus using mechanical arm, respectively into crucible
Distilled water is first added, then adds sulfuric acid solution and obtains 4 kinds of soil digested solusions.
4 kinds of soil digested solusions that embodiment 2 obtains are measured into Theil indices by atomic fluorescence detector respectively, as a result such as 5 institute of table
Show:
The Theil indices measurement result of table 5:4 kind pedotheque
After the device, the accuracy of measurement of tin is able to satisfy the deviation requirement of standard sample in soils and sediments, and
And its relative standard deviation, in 1.5-4.2%, precision is good, practical pedotheque recovery of standard addition has 99%.
It is skilled to this field although present invention has been described in detail and some specific embodiments have been cited
For technical staff, as long as it is obvious for can making various changes or correct without departing from the spirit and scope of the present invention.
Claims (10)
1. a kind of soil alkali fusion pre-treating method, which is characterized in that described method includes following steps:
(1) sample treatment: re-sieving after pedotheque is air-dried, is ground, is mixed measures moisture content；
(2) pre- resolution: the sample for weighing known aqueous rate is placed in crucible, and crucible is placed on alkali fusion meausring apparatus, to earthenware
After acid digestion solution is added dropwise in crucible, transfer crucible is heated into temperature controllable heating digestion instrument and cools down to obtain pre- resolution
Sample；
(3) it clears up again: pre- resolution sample being transferred on alkali fusion meausring apparatus, the prefabricated mix reagent of alkali fusion is added into crucible, then
Crucible is transferred in temperature controllable heating digestion instrument and carries out reheating processing and so cooling that clear up sample again；
(4) it post-processes: sample will be cleared up again and be transferred on alkali fusion meausring apparatus, distilled water is first added into crucible, then add acidity
Reagent obtains soil digested solusion.
2. a kind of soil alkali fusion pre-treating method according to claim 1, which is characterized in that the alkali fusion meausring apparatus packet
It includes induction and claims the solid reagent device added and the liquid reagent device quantitatively added.
3. a kind of soil alkali fusion pre-treating method according to claim 1 or 2, which is characterized in that the alkali fusion weighs dress
Bottom set portion is equipped with vortex homogenous unit and induction weighing device, and the vortex homogenous unit is for producing soil digested solusion.
4. a kind of soil alkali fusion pre-treating method according to claim 1, which is characterized in that step (2) described acidity disappears
Solution liquid is hydrofluoric acid, and dripping quantity is quantitative 10ml.
5. a kind of soil alkali fusion pre-treating method according to claim 1, which is characterized in that the temperature controllable heating resolution
Device includes temperature automatically controlled timing heated case, acid mist absorbing device and vacuum pump.
6. a kind of soil alkali fusion pre-treating method according to claim 1, which is characterized in that step (2) described heating
Temperature is 95-105 DEG C, and the time of heating is 18-22min.
7. a kind of soil alkali fusion pre-treating method according to claim 1, which is characterized in that step (2) described cooling
Time is 18-22min, is cooled to 20-30 DEG C.
8. a kind of soil alkali fusion pre-treating method according to claim 1, which is characterized in that step (3) described alkali fusion is pre-
Mix reagent processed includes one of sodium carbonate, lithium tetraborate, lithium metaborate, sodium peroxide or a variety of.
9. a kind of soil alkali fusion pre-treating method according to claim 1, which is characterized in that step (3) it is described it is secondary plus
The temperature of heat is 950-1050 DEG C, time 25-35min.
10. a kind of soil alkali fusion pre-treating method according to claim 1, which is characterized in that step (3) is described to be cooled to
250-350℃。
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Cited By (1)
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| CN110186745A (en) * | 2019-06-18 | 2019-08-30 | 许昌学院 | Se from Soil content measuring system |
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