CN109425602A - Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion method - Google Patents
Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion method Download PDFInfo
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- CN109425602A CN109425602A CN201710737808.1A CN201710737808A CN109425602A CN 109425602 A CN109425602 A CN 109425602A CN 201710737808 A CN201710737808 A CN 201710737808A CN 109425602 A CN109425602 A CN 109425602A
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- beryllium
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- G—PHYSICS
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- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/72—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using flame burners
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Abstract
The present invention relates to chemical analysis technology field, a kind of Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion method are particularly related to；Nature is weighed including a) polytetrafluoroethylene (PTFE) crucible to dry in the shade 100 0.1~0.5g of mesh soil；B) it is added in polytetrafluoroethylene (PTFE) crucible and newly configures chloroazotic acid 6ml, 2ml hydrofluoric acid, High-temperature Digestion 60 minutes；C) temperature is promoted to 180 DEG C of package metals kept in 60 minutes resolution clay lattices；D) continuously add 2ml perchloric acid, kept for 180~230 DEG C continue 60-120 minutes, uncap rush to emit white cigarette rush to it is thick and 1% nitric acid constant volume, to be measured；E) it uses Atomic absorption flame or graphite furnace detects respective element respectively or inductive coupling plasma emission spectrograph directly measures.Resolution multielement coexists in this method, has saved analysis time, reduces the resolution step of different elemental analyses, realizes multielement, high-volume, high efficiency, high accuracy processing analysis.
Description
Technical field
The present invention relates to chemical analysis technology field, it is quick to particularly relate to a kind of Soil Copper, zinc, lead, cadmium, nickel, beryllium
Digestion procedure.
Background technique
Copper, zinc, lead, cadmium, nickel, beryllium be the important meals data target in soil, when a large amount of huge sum of money of remaining in human body
Anxious easily to cause to bear to the intracorporal internal organs of body after category, especially liver and gallbladder maintain people after both organs go wrong
Intracorporal metabolism will get muddled, cirrhosis, and liver ascites is even even more serious, and metallic beryllium and its salt compounds exist
Gastrointestinal tract uptake ratio is no more than 0.2%, can absorb through damaged skin, causes local patholoic change, sucks human body, can seriously hurt to lung
Evil.
Copper, zinc, lead, cadmium, nickel, beryllium not only with metal form, are more deposited in the form of myriad of compounds extensively in nature
In either air, soil or even drinking water all cupric, zinc, lead, cadmium, nickel, beryllium.The production activity of the mankind to copper, zinc, lead, cadmium,
Nickel, beryllium significantly affect；Pesticide, the chemical fertilizer of industrial exhaust gas, waste water, waste residue, waste material and vehicle exhaust, agricultural；Chemistry examination
Agent, additive, house refuse, waste water, sewage, excreta, medical waste, virus, bacterium, putrefaction etc. all can to copper, zinc,
Lead, cadmium, nickel, beryllium content distribution have an important influence, this constitutes a serious threat to human health, therefore to have become the world each for its prevention and treatment
The problem of state's facing.
Environmental pollution is made in order to prevent, so it is aobvious to detect copper, zinc, lead, cadmium, nickel, beryllium in environment using certain technological means
It obtains particularly significant；Great influence is brought to environment Metal Distribution due to the work production activity of the mankind in modern society, therefore copper,
Zinc, lead, cadmium, nickel, beryllium analysis detection means seem more it is necessary to.
Copper, zinc, lead, cadmium, nickel, the measuring method of beryllium content are more in soil, and there are commonly atomic absorption spectrography (AAS)s, inductance
Coupled plasma mass, inductively coupled plasma emission spectrography etc..Concerned countries standard has GB/T 17141-
1997, GB/T 17138-1997, HJ737-2015, national standard difference element are handled respectively, and individual element digestion time is tediously long,
Hydrolytic acid amount is big, and experimenter's operation brings inconvenience.
Summary of the invention
The present invention provides a kind of Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion method in view of above-mentioned technical problem, should
Resolution multielement coexists in method, has saved analysis time, reduces the resolution step of different elemental analyses, realizes polynary
Element, high-volume, high efficiency, high accuracy processing analysis.
This method solves technical solution used by above-mentioned technical problem are as follows:
A kind of Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion method, wherein the described method comprises the following steps:
A) polytetrafluoroethylene (PTFE) crucible weighs nature and dried in the shade 100 0.1~0.5g of mesh soil；
B) it is added in polytetrafluoroethylene (PTFE) crucible and newly configures chloroazotic acid 6ml, 2ml hydrofluoric acid, High-temperature Digestion 60 minutes；
C) temperature is promoted to 180 DEG C of package metals kept in 60 minutes resolution clay lattices；
D) continuously add 2ml perchloric acid, kept for 180~230 DEG C continue 60-120 minutes, uncap rush to emit white cigarette rush to it is viscous
Thick shape, and it is 1% nitric acid constant volume, to be measured；
E) respective element or inductively coupled plasma atomic emission are detected respectively using Atomic absorption flame or graphite furnace
Instrument directly measures.
Above-mentioned Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion method, wherein chloroazotic acid includes the mixing of hydrochloric acid and nitric acid
Object, wherein hydrochloric acid and nitric acid proportion are 3:1 or 1:3.
Above-mentioned Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion method, wherein in step b), 40~100 DEG C of high temperature disappear
Solution 60 minutes.
Above-mentioned Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion method, wherein
Soil Copper, zinc and nickel use Flame Atomic Absorption, and spectral line is respectively copper 324.75nm, zinc 213.86nm, nickel
232.00nm；
Pb in Soil, cadmium and beryllium are measured using sampling Graphite Furnace Atomic Absorption, and general line spectrum line is respectively lead 283.31nm, cadmium
228.80nm, beryllium 234.86nm are directly analyzed using inductive coupling plasma emission spectrograph.
Above-mentioned technical proposal have the following advantages that or the utility model has the advantages that
The present invention provides a kind of Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion methods, can simple strong operability
Mode realize copper in soil, zinc, lead, cadmium, nickel, beryllium analysis processing, reduce the usage amount of acid, this technical costs is low, can
Realize the analysis of one step of high/low temperature element, this technical costs is low, and energy consumption is small, and accuracy is high, and it is high-efficient, it has a extensive future.
Specific embodiment
Below with reference to specific embodiment, the present invention is further illustrated, but not as the limitation of the invention.
The reagent used in the embodiment of the present invention is to analyze pure or analyze more than pure, and water is distilled water or deionization
Water；The glassware of use uses volume fraction 50%HNO3Impregnate 24 hours more than again with distilled water flushing completely and dry,
In following embodiment unless otherwise specified, reagent and instrument are all made of commercial product and operate to specifications.
Specifically, Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion method the following steps are included:
A) polytetrafluoroethylene (PTFE) crucible weighs nature and dried in the shade 100 0.1~0.5g of mesh soil；
B) it is added in polytetrafluoroethylene (PTFE) crucible and newly configures chloroazotic acid 6ml, 2ml hydrofluoric acid, High-temperature Digestion 60 minutes；
C) temperature is promoted to 180 DEG C of package metals kept in 60 minutes resolution clay lattices；
D) continuously add 2ml perchloric acid, kept for 180~230 DEG C continue 60-120 minutes, uncap rush to emit white cigarette rush to it is viscous
Thick shape, and it is 1% nitric acid constant volume, to be measured；
E) respective element or inductively coupled plasma atomic emission are detected respectively using Atomic absorption flame or graphite furnace
Instrument directly measures.
In an embodiment of the present invention, it is 3:1 that chloroazotic acid, which includes the mixture of hydrochloric acid and nitric acid, wherein hydrochloric acid and nitric acid proportion,
Or 1:3.
Preferably, in step b), 40~100 DEG C High-temperature Digestion 60 minutes；In an optional but unrestricted reality of the invention
It applies in example, in which:
Soil Copper, zinc and nickel use Flame Atomic Absorption, and spectral line is respectively copper 324.75nm, zinc 213.86nm, nickel
232.00nm；
Pb in Soil, cadmium and beryllium are measured using sampling Graphite Furnace Atomic Absorption, and general line spectrum line is respectively lead 283.31nm, cadmium
228.80nm, beryllium 234.86nm are directly analyzed using inductive coupling plasma emission spectrograph.
Concrete operations details is as follows:
1, the preparation of soil
1.1 material
Distilled water or deionized water, concentrated nitric acid ρ (HNO3)=1.42g/ml；Excellent pure grade, hydrofluoric acid ρ (HF)=1.49g/
ml；100 mesh nylon mesh, agate mortar, Glass capacity bottle or associated vessel；
1.2 soil processing
Acquisition sample according to country sampling specification is sampled, into laboratory after dry in the shade naturally.
Sample pass through quartering, finally acquire about 500g sample carry out agate mortar grinding, cross 100 mesh nylon mesh obtain to
Survey pedotheque；
It weighs 10~50g sample and carries out drying calculating moisture content in 105 DEG C or so baking ovens, weight must not surpass after cooling down twice
Cross 1%.
2, the resolution of sample
It takes 0.1~0.5g (being accurate to 0.0001g) in polytetrafluoroethylene (PTFE) crucible, new configuration chloroazotic acid (1:3HNO3/ is added
Hcl 180 DEG C of) 6ml, 2ml hydrofluoric acid are cleared up 1 hour, and uncapping to rush to emits white cigarette (if any black precipitate, lid lid to black precipitate
Nothing), rush to thick, 1% nitric acid is added, and to be settled to scale to be measured.
3, contained with copper, zinc, lead, cadmium, nickel, beryllium in the methods of inductively coupled plasma emission spectrography measurement soil
Amount:
3.1 instruments and material
Inductive coupling plasma emission spectrograph Optima8300,7 clean, 50ml Glass capacity bottle, 1000mg/L
The mixed mark of multielement containing each element in soil.
3.2 experimental procedure
3.2.1 the drafting of curve
Mother liquor is drawn: being pipetted multielement standard liquid (1000mg/L) 2ml into 50ml Glass capacity bottle, is pipetted with liquid-transfering gun
0.5ml GR rank nitric acid is settled to scale, obtains the mixed mark 50mg/L of multielement.
Standard point-rendering pipettes 0ml, 1ml, 0.5ml, 1.0ml, 1.5ml, 2.0ml to 50ml Glass capacity from mother liquor
Bottle in, with liquid-transfering gun pipette 0.5ml GR rank nitric acid be settled to scale obtain 0mg/L, 0.1mg/L, 0.5mg/L, 1.0mg/L,
The mixed mark standard liquid of 1.5mg/L, 2.0mg/L copper, zinc, lead, cadmium, nickel, beryllium.
3.3 measurement
It opens plasma emission spectrometer and preheats 30min, after plasma stability, RF power regulation to 1300W,
Cooling gas flow 15L/min, frequency 27.1MHz carrier gas flux 0.55L/min, secondary air amount 0.2min/L；
The measurement formula of the constituent content are as follows:
In formula: concentration of element (mg/L) in ρ-liquid sample
The volume ml of V- reagent constant volume；
M- weighs the weight g of sample；
The content % of moisture in f- sample
In an embodiment of the present invention, quality control assurances are as technical research core:
1) blank test, every batch of sample at least do 1 laboratory blank, and the blank value of surveyed element must not exceed method survey
Fix limit.Reason must be looked for if exceeding, is reanalysed until sample could be analyzed after qualified.
2) every batch of sample point is permitted must to draw calibration curve, and the related coefficient of calibration curve should be greater than or every equal to 0.995.
Calibration check must be carried out with the intermediate point concentration standard solution of a calibration curve by analyzing 50 samples.Its measurement result and recently
The relative deviation of primary calibration curve concentration should be less than or be equal to 10%.Otherwise curve is repainted.
3) accuracy controlling, every batch of sample needs band certified reference material, measurement knot when carrying out full dose measurement to sample
Fruit should provide in range of uncertainty, carry out mark-on control accuracy to sample, recovery of standard addition range should 80%~
Between 120%.
It, can simple strong operability in conclusion Soil Copper of the present invention, zinc, lead, cadmium, nickel, beryllium rapid-digestion method
Mode realizes copper, zinc, lead, cadmium, nickel, beryllium analysis processing in soil, reduces the usage amount of acid, this technical costs is low, can be real
Existing one step of high/low temperature element analysis, this technical costs is low, and energy consumption is small, and accuracy is high, high-efficient, has a extensive future.
It should be appreciated by those skilled in the art that those skilled in the art are combining the prior art and above-described embodiment can be with
Realize the change case, this will not be repeated here.Such change case does not affect the essence of the present invention, not superfluous herein
It states.
Presently preferred embodiments of the present invention is described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, devices and structures not described in detail herein should be understood as gives reality with the common mode in this field
It applies；Anyone skilled in the art, without departing from the scope of the technical proposal of the invention, all using the disclosure above
Methods and technical content many possible changes and modifications are made to technical solution of the present invention, or be revised as equivalent variations etc.
Embodiment is imitated, this is not affected the essence of the present invention.Therefore, anything that does not depart from the technical scheme of the invention, foundation
Technical spirit of the invention any simple modifications, equivalents, and modifications made to the above embodiment, still fall within the present invention
In the range of technical solution protection.
Claims (4)
1. a kind of Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion method, which is characterized in that the described method comprises the following steps:
A) polytetrafluoroethylene (PTFE) crucible weighs nature and dried in the shade 100 0.1~0.5g of mesh soil；
B) it is added in polytetrafluoroethylene (PTFE) crucible and newly configures chloroazotic acid 6ml, 2ml hydrofluoric acid, High-temperature Digestion 60 minutes；
C) temperature is promoted to 180 DEG C of package metals kept in 60 minutes resolution clay lattices；
D) continuously add 2ml perchloric acid, kept for 180~230 DEG C continue 60-120 minutes, uncap rush to emit white cigarette rush to it is sticky
Shape, and it is 1% nitric acid constant volume, to be measured；
E) it uses Atomic absorption flame or graphite furnace detects respective element respectively or inductive coupling plasma emission spectrograph is straight
Connect measurement.
2. Soil Copper according to claim 1, zinc, lead, cadmium, nickel, beryllium rapid-digestion method, which is characterized in that chloroazotic acid packet
The mixture of hydrochloric acid and nitric acid is included, wherein hydrochloric acid and nitric acid proportion are 3:1 or 1:3.
3. Soil Copper according to claim 1, zinc, lead, cadmium, nickel, beryllium rapid-digestion method, which is characterized in that step b)
In, 40~100 DEG C High-temperature Digestion 60 minutes.
4. Soil Copper according to claim 1, zinc, lead, cadmium, nickel, beryllium rapid-digestion method, which is characterized in that
Soil Copper, zinc and nickel use Flame Atomic Absorption, and spectral line is respectively copper 324.75nm, zinc 213.86nm, nickel
232.00nm；
Pb in Soil, cadmium and beryllium are measured using sampling Graphite Furnace Atomic Absorption, general line spectrum line be respectively lead 283.31nm, cadmium 228.80nm,
Beryllium 234.86nm is directly analyzed using inductive coupling plasma emission spectrograph.
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| CN201710737808.1A CN109425602A (en) | 2017-08-24 | 2017-08-24 | Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion method |
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| CN201710737808.1A CN109425602A (en) | 2017-08-24 | 2017-08-24 | Soil Copper, zinc, lead, cadmium, nickel, beryllium rapid-digestion method |
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Cited By (3)
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| CN110618020A (en) * | 2019-09-12 | 2019-12-27 | 广西博世科环保科技股份有限公司 | Method for rapidly digesting heavy metal soil sample |
| CN111398399A (en) * | 2020-03-31 | 2020-07-10 | 广西壮族自治区地质矿产测试研究中心 | Method for determining silver by inductively coupled plasma mass spectrometry |
| CN111650185A (en) * | 2020-04-16 | 2020-09-11 | 苏州昆环检测技术有限公司 | Method for measuring copper, cadmium, lead, nickel, chromium, zinc, cobalt and vanadium in soil |
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Application publication date: 20190305 |