CN109163958A - A kind of Methods of Soil Digestion and a kind of detection method for measuring various heavy in soil simultaneously - Google Patents
A kind of Methods of Soil Digestion and a kind of detection method for measuring various heavy in soil simultaneously Download PDFInfo
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- CN109163958A CN109163958A CN201811216143.0A CN201811216143A CN109163958A CN 109163958 A CN109163958 A CN 109163958A CN 201811216143 A CN201811216143 A CN 201811216143A CN 109163958 A CN109163958 A CN 109163958A
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
- G01N2021/3114—Multi-element AAS arrangements
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Abstract
The present invention provides a kind of digestion procedures of soil, belong to technical field of analytical chemistry.Method provided by the invention is added to after nitric acid and mixed in hydrochloric acid in pedotheque, enhances the oxidisability of mixed acid, obtained digestion solution can satisfy testing requirements；Meanwhile mixture of hydrochloric acid and nitric acid is mixed with pedotheque, is once cleared up the digestion solution for just obtaining meeting testing requirements, compared to " nitric acid, hydrofluoric acid, perchloric acid, hydrochloric acid " that existing national standard is added, step is easy, reduces the dosage of reagent.In addition, the digestion solution that digestion procedure of the invention obtains is for when detecting, testing result to be accurate.From embodiment it can be seen that method provided by the invention is easy to operate, environmentally friendly；Can be used in detect pedotheque in lead, cadmium, copper, zinc and manganese content, as a result accurately.
Description
Technical field
The present invention relates to technical field of analytical chemistry more particularly to a kind of Methods of Soil Digestion and one kind to measure soil simultaneously
The detection method of middle various heavy.
Background technique
In recent years, with the development of economy, the arable land of national farmland sum 1/6 is accounted for by different degrees of heavy metal-polluted
It contaminates, the heavy metal in Accurate Determining soil will play positive effect to the heavy metal reparation for instructing soil.Resolution is to influence soil
The committed step of middle heavy metal element determination result accuracy, different digestion procedures, operation difficulty is different, clears up effect also not
Together.
At present for heavy metals in soil content detection digestion procedure mainly according to existing national standards such as
" GB/T 17141-1997 soil quality lead, Cadmium detrmination graphite furnace atomic absorption spectrometry ", " GB/T 17138-1997
Soil quality copper, Direct spectrophotometry atomic absorption spectrophotometry " etc. carry out, generally use tetracid (nitric acid, hydrofluoric acid, height
Chloric acid, hydrochloric acid) resolution method carries out resolution processing in polytetrafluoroethylene (PTFE) crucible, and these standard method processes are cumbersome, reagent dosage
Greatly, the hydrofluoric acid and perchloric acid used has strong corrosiveness to skin.Contact hydrofluoric acid vapor, can occur bronchitis,
Pneumonia etc., to experimental implementation person, laboratory environment, there are larger harm, it is therefore necessary to grasp under the good closed environment of ventilation effect
Make.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of Methods of Soil Digestion and one kind while measuring more in soil
The detection method of heavy metal species.Digestion procedure provided by the invention does not use the hydrofluoric acid and perchloric acid of deep-etching, only need by
Nitric acid and hydrochloric acid are added to which in Digestion of Some Soil Samples, resolution effect is good after being mixed in a certain ratio；And method is simple and environmentally-friendly；
Obtained digestion solution can be used in detecting lead, cadmium, copper, zinc and manganese content in pedotheque.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of Methods of Soil Digestion, comprising the following steps:
After pedotheque is mixed with mixed acid, is cleared up through heat, obtain digestion solution；
The mixed acid is nitric acid and the hydrochloric acid mixed preparing of 1:2.5~3.5 by volume；The mass concentration of the nitric acid is
65~68%, the mass concentration of the hydrochloric acid is 36~38%.
Preferably, the amount ratio of the pedotheque and mixed acid is 0.3~0.8g:5~15mL.
Preferably, average grain diameter≤0.149mm of the pedotheque.
Preferably, the temperature of the heat resolution is 98~100 DEG C, and the time is 2~3h.
Preferably, further include that the product of the heat resolution is evaporated to 0.8~1.2mL, be cooled to 20~30 DEG C, will evaporate
Residue is settled to 25~50mL with water afterwards, obtains digestion solution.
Preferably, the temperature of the evaporation is 98~100 DEG C.
The present invention also provides a kind of detection methods for measuring various heavy in soil simultaneously, include the following steps:
The various heavy in digestion solution obtained using digestion procedure described in atomic absorption method detection above-mentioned technical proposal.
Preferably, the heavy metal includes lead, cadmium, copper, zinc and manganese.
Preferably, the atomic absorption method includes flame atomic absorption method and graphite oven atomic absorption.
The present invention provides a kind of Methods of Soil Digestion, comprising the following steps: after pedotheque is mixed with mixed acid, warp
Heat resolution, obtains digestion solution；The mixed acid is nitric acid and the hydrochloric acid mixed preparing of 1:2.5~3.5 by volume；The nitric acid
Mass concentration is 65~68%, and the mass concentration of the hydrochloric acid is 36~38%.The present invention is by after nitric acid and mixed in hydrochloric acid, simultaneously
It is added in pedotheque, enhances the oxidisability of mixed acid, obtained digestion solution can satisfy testing requirements；Meanwhile it mixing
Acid is mixed with pedotheque, is once cleared up the digestion solution for just obtaining meeting testing requirements, " the nitre being added compared to existing national standard
Acid, hydrofluoric acid, perchloric acid, hydrochloric acid ", step is easy, reduces the type of reagent, environmentally protective.In addition, resolution side of the invention
The digestion solution that method obtains is for when detecting, testing result to be accurate.From embodiment it can be seen that method provided by the invention operation letter
Single, environmental protection；And can be used in detecting the content of the lead in pedotheque, cadmium, copper, zinc and manganese, as a result accurately.
Specific embodiment
The present invention provides a kind of Methods of Soil Digestion, comprising the following steps:
After pedotheque is mixed with mixed acid, is cleared up through heat, obtain digestion solution；
The mixed acid is nitric acid and the hydrochloric acid mixed preparing of 1:2.5~3.5 by volume；The mass concentration of the nitric acid is
65~68%, the mass concentration of the hydrochloric acid is 36~38%.
In the present invention, the mixed acid is nitric acid and the hydrochloric acid mixed preparing of 1:2.5~3.5, preferably 1 by volume:
2.75~3.25, more preferably 1:3；The mass concentration of the nitric acid is 65~68%, preferably 66~67%；The hydrochloric acid
Mass concentration is 36~38%, preferably 37%.The present invention does not have special restriction to the preparation method of the mixed acid, uses
Preparation method of mixture well known to those skilled in the art.In an embodiment of the present invention, the preparation step of the mixed acid
It is rapid preferred are as follows: after mixing nitric acid by volume with hydrochloric acid, to be placed at room temperature for 20~30min, obtain mixed acid.
In the present invention, the amount ratio of the pedotheque and mixed acid is preferably 0.3~0.8g:5~15mL, more preferably
For 0.4~0.7g:6~13mL, most preferably 0.5~0.6g:8~10mL.Mixing of the present invention to pedotheque and mixed acid
Mode does not have special restriction, using hybrid mode well known to those skilled in the art.
In the present invention, the pedotheque average grain diameter preferably≤0.149mm.
The present invention does not have special restriction to the source of pedotheque, using pedotheque well known to those skilled in the art
, specifically, the country such as marked as GSS-13 (GBW07427), GSS-14 (GBW07428), GSS-15 (GBW07429)
Standard soil；Normal soil is either removed into impurity, air-dries, be ground up, sieved, obtained pedotheque.
The present invention goes deimpurity method not have special restriction normal soil, and use is well known to those skilled in the art
Soil goes deimpurity method, specifically, such as crushing normal soil, sieving, by stone, gravel, the branch in soil
Equal impurity removal.In the present invention, the sieve mesh number being ground up, sieved is preferably 100 mesh.
In the present invention, the temperature of the heat resolution is preferably 98~100 DEG C, more preferably 98.5~99.5 DEG C, optimal
It is selected as 99 DEG C；The time of the heat resolution is preferably 2~3h, more preferably 2.2~2.8h, most preferably 2.4~2.6h.This hair
It is bright there is no special restriction to hot digestion instrument, using heating device well known to those skilled in the art, of the invention
In embodiment, the process of heat resolution specifically: pedotheque and mixed acid are placed in high-boron-silicon glass digestion tube, by high borosilicate
Glass digestion tube, which is placed in water bath, carries out hot resolution.
After heat resolution, product of the present invention preferably by heat resolution is evaporated to 0.8~1.2mL, is cooled to 20~30 DEG C,
Remaining after evaporation object is settled to 25~50mL with water, obtains digestion solution.
In the present invention, the temperature of the evaporation is preferably 98~100 DEG C, and more preferably 98.5~99.5 DEG C, most preferably
It is 99 DEG C.The present invention does not have special restriction to the time of the evaporation, if the product for clearing up heat be evaporated to 0.8~
1.2mL.
In the present invention, nitric acid and mixed in hydrochloric acid are enhanced into the oxidisability of mixed acid；Mixed acid is added at one time soil
In earth sample, the digestion solution for meeting testing requirements need to only can be obtained through primary heat resolution, step is simple, and saves a large amount of
Solvent；Compared to " nitric acid, hydrofluoric acid, perchloric acid, hydrochloric acid " that existing national standard is added, step is simple, and environmental protection.
The present invention also provides a kind of detection methods for measuring various heavy in soil simultaneously, include the following steps:
The various heavy in digestion solution obtained using digestion procedure described in atomic absorption method detection above-mentioned technical proposal.
In the present invention, the heavy metal includes lead, cadmium, copper, zinc and manganese.In the present invention, the atomic absorption method packet
Include flame atomic absorption method and graphite furnace absorption process.
In the present invention, when detecting the lead and cadmium content in digestion solution, it is preferred to use graphite oven atomic absorption.In this hair
In bright, when detecting lead content in digestion solution using graphite oven atomic absorption, the work of the graphite oven atomic absorption instrument
Parameter is preferred are as follows: wavelength 217nm, slit 0.7nm, lamp current 5mA, drying temperature are 110~130 DEG C, ashing temperature
It is 500 DEG C, atomization temperature is 1600 DEG C, and residual temperature is 2450 DEG C.In the present invention, it is examined using graphite oven atomic absorption
When surveying cadmium content in digestion solution, the running parameter of the graphite oven atomic absorption instrument is preferred are as follows: wavelength 228nm, slit
For 0.7nm, lamp current 4mA, drying temperature is 110~130 DEG C, and ashing temperature is 300 DEG C, and atomization temperature is 1500 DEG C,
Residual temperature is 2450 DEG C.
In the present invention, when detecting copper, zinc and manganese content in digestion solution, it is preferred to use flame atomic absorption method.In this hair
In bright, when detecting copper content in digestion solution using flame atomic absorption method, the running parameter of the flame atomic absorption method instrument
It is preferred that are as follows: wavelength 324.8nm, slit 0.2nm, lamp current 3mA, secondary air amount 2.0L/min, nebulizer flow
For 5.0L/min, acetylene flow is 1.5L/min.In the present invention, using Zn content in flame atomic absorption method detection digestion solution
When, the running parameter of the flame atomic absorption method instrument is preferred are as follows: wavelength 213.9nm, slit 0.2nm, lamp current are
3mA, secondary air amount 2.0L/min, nebulizer flow 5.0L/min, acetylene flow are 1.5L/min.In the present invention,
Using when manganese content, the running parameter of the flame atomic absorption method instrument is preferred in flame atomic absorption method detection digestion solution
Are as follows: wavelength 279.5nm, slit 0.2nm, lamp current 3mA, secondary air amount 2.0L/min, nebulizer flow are
5.0L/min, acetylene flow are 1.5L/min.
An a variety of huge sum of moneys in soil are measured simultaneously to Methods of Soil Digestion provided by the invention and one kind below with reference to embodiment
The detection method of category is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Pedotheque source: number is GSS-13 (GBW07427), GSS-14 (GBW07428) and GSS-15
(GBW07429) national standard soil；
(1) digestion procedure of above-mentioned pedotheque:
Accurately weigh respectively 0.2g (being accurate to 0.0002g) GSS-13 (GBW07427), GSS-14 (GBW07428) and
GSS-15 (GBW07429) pedotheque is placed in 50mL high-boron-silicon glass digestion tube, is separately added into 6mL mixed acid；In 100 DEG C
Water-bath on carry out heat resolution 2h；Heat resolution after, by heat resolution product be evaporated to 1.0mL, be cooled to room temperature, add from
Sub- water is settled to 25mL, obtains digestion solution；It stands overnight, it is to be measured；Blank control is done with the solution that pedotheque is not added simultaneously；Institute
The hydrochloric acid that nitric acid and mass concentration that mixed acid is 65~68% by mass concentration are 36~38% is stated to mix according to volume ratio 1:3
It obtains.
(2) in digestion solution metallic element detection
Using graphite oven atomic absorption in obtained digestion solution lead and cadmium content detect；The graphite furnace is former
The running parameter of sub- absorption process instrument detection lead and cadmium is as shown in table 1.
1 graphite oven atomic absorption instrument of table detects the operating condition of lead and cadmium in digestion solution
Copper, zinc and the manganese content in obtained digestion solution are detected using flame atomic absorption method；The flame is former
The running parameter of sub- absorption process instrument detection copper, zinc and manganese is as shown in table 2.
2 flame atomic absorption method instrument of table detects copper, zinc and manganese operating condition in digestion solution
The results are shown in Table 3 for metal element content in the digestion solution of the three kinds of pedotheques measured using the above method.
The assay result of 5 Heavy Metallic Elements in 3 three kinds of pedotheques of table
From table 3 it can be seen that 5 Heavy Metallic Elements in tri- kinds of standard soil samples of GSS-13, GSS-14 and GSS-15
Substantially all within critical field, relative standard deviation RSD is below 5% for accuracy, illustrates that the digestion procedure obtains digestion solution
With good accuracy and precision, meet testing requirements.
Embodiment 2
Pedotheque source: number is GSS-13 (GBW07427), GSS-14 (GBW07428) and GSS-15
(GBW07429) national standard soil.
(1) digestion procedure of above-mentioned pedotheque
Accurately weigh respectively 0.5g (being accurate to 0.0002g) GSS-13 (GBW07427), GSS-14 (GBW07428) and
GSS-15 (GBW07429) pedotheque is placed in 50mL high-boron-silicon glass digestion tube, 10mL mixed acid is separately added into, in 100 DEG C
Water-bath on carry out heat resolution 3h；Heat resolution after, by heat resolution product be evaporated to 0.8mL, be cooled to room temperature, add from
Sub- water is settled to 50mL, obtains digestion solution；It stands overnight, it is to be measured；Blank control is done with the solution that pedotheque is not added simultaneously；Institute
The hydrochloric acid that nitric acid and mass concentration that mixed acid is 65~68% by mass concentration are 36~38% is stated to mix according to volume ratio 1:3
It obtains.
(2) in digestion solution metallic element detection
Using lead, cadmium, copper, zinc in digestion solution obtained by detecting instrument same as Example 1 and parameter detecting the present embodiment
With the content of manganese；The results are shown in Table 4.
The assay result of 5 Heavy Metallic Elements in 4 three kinds of pedotheques of table
From table 4, it can be seen that 5 Heavy Metallic Elements in tri- kinds of standard soil samples of GSS-13, GSS-14 and GSS-15
Substantially all within the scope of standard substance guarantee value, relative standard deviation RSD is below 5%, illustrates the digestion procedure for accuracy
Obtained digestion solution has good accuracy and precision, meets testing requirements.
Embodiment 3
Soil sources: picking up from paddy soil, and number is respectively S01 and S02.
The preparation of pedotheque: paddy soil removal impurity, air-dried, grinding are sieved with 100 mesh sieve, screenings is soil-like
Product；
(1) digestion procedure of above-mentioned pedotheque
S01 the and S02 pedotheque for accurately weighing 0.5g (being accurate to 0.0002g) respectively is placed in 50mL high-boron-silicon glass and disappears
Xie Guanzhong is separately added into 10mL mixed acid, clears up 3h in carrying out heat on 100 DEG C of water-bath；After heat resolution, heat is cleared up
Product is evaporated to 1.2mL, is cooled to room temperature, and deionized water is added to be settled to 50mL, obtains digestion solution；It stands overnight, it is to be measured；Simultaneously
Blank control is done so that the solution of pedotheque is not added；Nitric acid and mass concentration of the mixed acid by mass concentration for 65~68%
It is mixed to get for 36~38% hydrochloric acid according to volume ratio 1:3.Each pedotheque heat is cleared up 6 times.
(2) in digestion solution metallic element detection
Using lead, cadmium, copper, zinc in digestion solution obtained by detecting instrument same as Example 1 and parameter detecting the present embodiment
With the content of manganese；The results are shown in Table 5.
The assay result of 5 Heavy Metallic Elements in 5 two kinds of pedotheques of table
As can be seen from Table 5, the relative standard deviation RSD of 5 Heavy Metallic Elements is below in S01 and S02 pedotheque
5%, illustrate that the precision for the digestion solution that the digestion procedure obtains meets testing requirements.
The inspection of accuracy: the standard that certain density respective metal element is added in S01 and S02 pedotheque is molten
Liquid, the digestion procedure through the present embodiment clear up sample；By the rate of recovery of each element in measurement digestion solution, to examine this
The accuracy of the digestion procedure provided is provided；The results are shown in Table 6.
The rate of recovery of 6 two kinds of pedotheques of table
As can be seen from Table 6, in S01 and S02 pedotheque the rate of recovery of each heavy metal element in 91.2~107% ranges
It is interior, illustrate that the accuracy of the digestion procedure meets testing requirements.
During metal elements in soil content detection, pre-treatment, that is, digestion process of sample is most important.Existing country
Standard method process is cumbersome, reagent dosage is big, corrosivity is strong, risk is high, big to the harm of human body and environment.The application is by nitre
Acid and hydrochloric acid are added in pedotheque after being mixed in a certain proportion, and mixed acid has stronger oxidisability, promote soil
The resolution of sample；Meanwhile after hydrochloric acid and nitric acid mixing, is mixed with pedotheque, once cleared up and just obtain meeting testing requirements
Digestion solution, compared to " nitric acid, hydrofluoric acid, perchloric acid, hydrochloric acid " that existing national standard is added, step is easy, reduces the use of reagent
Amount.In addition, by bringing quality-control sample into and doing recovery of standard addition, it was demonstrated that the digestion solution energy that digestion procedure provided by the invention obtains
Lead, cadmium, copper, zinc and the manganese content being enough in detection pedotheque, and result is accurate.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of Methods of Soil Digestion, comprising the following steps:
After pedotheque is mixed with mixed acid, is cleared up through heat, obtain digestion solution；
The mixed acid is nitric acid and the hydrochloric acid mixed preparing of 1:2.5~3.5 by volume；The mass concentration of the nitric acid be 65~
68%, the mass concentration of the hydrochloric acid is 36~38%.
2. Methods of Soil Digestion according to claim 1, which is characterized in that the amount ratio of the pedotheque and mixed acid
For 0.3~0.8g:5~15mL.
3. Methods of Soil Digestion according to claim 1 or 2, which is characterized in that the average grain diameter of the pedotheque≤
0.149mm。
4. Methods of Soil Digestion according to claim 1, which is characterized in that the temperature of the heat resolution is 98~100 DEG C,
Time is 2~3h.
5. Methods of Soil Digestion according to claim 1, which is characterized in that further include by the product evaporation of the heat resolution
To 0.8~1.2mL, 20~30 DEG C are cooled to, remaining after evaporation object is settled to 25~50mL with water, obtains digestion solution.
6. Methods of Soil Digestion according to claim 5, which is characterized in that the temperature of the evaporation is 98~100 DEG C.
7. a kind of detection method for measuring various heavy in soil simultaneously, includes the following steps:
It is a variety of heavy in the digestion solution obtained using digestion procedure described in atomic absorption method detection claim 1~6 any one
Metal.
8. detection method according to claim 7, which is characterized in that the heavy metal includes lead, cadmium, copper, zinc and manganese.
9. detection method according to claim 7, which is characterized in that the atomic absorption method includes flame atomic absorption method
And graphite oven atomic absorption.
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| CN111189690A (en) * | 2020-03-04 | 2020-05-22 | 重庆中科检测技术服务有限公司 | Method for detecting heavy metal in soil |
| CN111855645A (en) * | 2020-08-06 | 2020-10-30 | 黄麟杰 | Method for jointly measuring phosphorus in soil by high-pressure digestion-inductively coupled plasma spectrometer |
| CN114414509A (en) * | 2021-12-30 | 2022-04-29 | 通标标准技术服务（天津）有限公司 | Method for detecting heavy metal chromium in food |
| CN114414509B (en) * | 2021-12-30 | 2023-12-12 | 通标标准技术服务（天津）有限公司 | Method for detecting heavy metal chromium in food |
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Application publication date: 20190108 |