CN106680358A - Inductively coupled plasma mass spectrometry method for determining content of chrome, arsenic, cadmium and lead in soil - Google Patents
Inductively coupled plasma mass spectrometry method for determining content of chrome, arsenic, cadmium and lead in soil Download PDFInfo
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- 239000002689 soil Substances 0.000 title claims abstract description 37
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 title claims abstract description 19
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 10
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 title abstract description 14
- 229910052785 arsenic Inorganic materials 0.000 title abstract description 6
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 title abstract description 6
- 238000001514 detection method Methods 0.000 claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 25
- 230000029087 digestion Effects 0.000 claims description 21
- 239000012224 working solution Substances 0.000 claims description 14
- 229910052804 chromium Inorganic materials 0.000 claims description 9
- 239000011651 chromium Substances 0.000 claims description 9
- VTXYFVHXMBFNNN-UHFFFAOYSA-N [As].[Cd].[Pb] Chemical compound [As].[Cd].[Pb] VTXYFVHXMBFNNN-UHFFFAOYSA-N 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 6
- 239000012895 dilution Substances 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- WURBVZBTWMNKQT-UHFFFAOYSA-N 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)butan-2-one Chemical compound C1=NC=NN1C(C(=O)C(C)(C)C)OC1=CC=C(Cl)C=C1 WURBVZBTWMNKQT-UHFFFAOYSA-N 0.000 claims description 5
- 238000005485 electric heating Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- VNSXTVUGRJMVDK-UHFFFAOYSA-N [Pb].[Cr].[As] Chemical compound [Pb].[Cr].[As] VNSXTVUGRJMVDK-UHFFFAOYSA-N 0.000 claims description 3
- 229920002301 cellulose acetate Polymers 0.000 claims description 3
- 239000000112 cooling gas Substances 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 230000002000 scavenging effect Effects 0.000 claims description 3
- 239000012086 standard solution Substances 0.000 claims description 3
- 239000011550 stock solution Substances 0.000 claims description 3
- OTJXRUHUGBSPCL-UHFFFAOYSA-N arsanylidynechromium Chemical compound [As]#[Cr] OTJXRUHUGBSPCL-UHFFFAOYSA-N 0.000 claims description 2
- 239000000523 sample Substances 0.000 claims 5
- 239000003595 mist Substances 0.000 claims 1
- 239000004033 plastic Substances 0.000 claims 1
- 229920003023 plastic Polymers 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 239000012488 sample solution Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 6
- 238000009616 inductively coupled plasma Methods 0.000 abstract description 2
- 238000007865 diluting Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 5
- 230000003595 spectral effect Effects 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000002795 fluorescence method Methods 0.000 description 2
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000006199 nebulizer Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- MTJGVAJYTOXFJH-UHFFFAOYSA-N 3-aminonaphthalene-1,5-disulfonic acid Chemical compound C1=CC=C(S(O)(=O)=O)C2=CC(N)=CC(S(O)(=O)=O)=C21 MTJGVAJYTOXFJH-UHFFFAOYSA-N 0.000 description 1
- QHPJZVWTEPPOMN-UHFFFAOYSA-N [Cr].[As].[Cd].[Pb] Chemical compound [Cr].[As].[Cd].[Pb] QHPJZVWTEPPOMN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ZIXVIWRPMFITIT-UHFFFAOYSA-N cadmium lead Chemical compound [Cd].[Pb] ZIXVIWRPMFITIT-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses an inductively coupled plasma mass spectrometry method for determining the content of chrome, arsenic, cadmium and lead in soil. The method mainly comprises the following steps: 1) decomposing a soil sample; 2) diluting a decomposed solution, achieving a constant volume and filtering; 3) using an inductively coupled plasma mass spectrometer for detecting; and 4) analyzing a result: calculating the content of chrome, arsenic, cadmium and lead in soil according to the weighed soil sample weight and the detected concentration of the decomposed solution. The determining method disclosed by the invention is simple, fast, high in analysis speed and low in detection limit; the detection limit of chrome is 0.0127mg/kg; the detection limit of arsenic is 0.0147mg/kg; the detection limit of cadmium is 0.0048mg/kg; the detection limit of lead is 0.0039mg/kg; the added recovery is 89%-113%; the relative standard deviation is below 4.5%; the measuring dynamic linear scope is wide; and various metal elements in soil can be detected simultaneously, so that the working efficiency is greatly increased.
Description
Technical field
The present invention relates to soil environment protection detection technique field, is specifically related to inductively coupled plasma mass spectrometry survey
Determine the content of Chromium in Soil arsenic cadmium lead.
Background technology
At present the detection method of tenor has atomic absorption method, atomic fluorescence method, ICP-AES methods and ICP-MS in soil
Method.Atomic Absorption Spectrometer is the light that elemental characteristic spectral line to be measured is provided from radiation of light source, by during sample steam by steam
In element ground state atom to be measured absorbed, the degree that is weakened by radiation feature spectral line light to determine sample in element to be measured contain
Amount.Atomic absorption method detection sensitivity is low, and the Element sensitivity that atomic fluorescence method is tested improves 2-3 than Atomic Absorption flame method
The individual order of magnitude, but homoatomic absorption process equally can not simultaneously detect multiple elements, and detection efficiency is relatively low.
ICP has made one of inorganic Analytical Methods of Trace with fastest developing speed since the ionization source of MS is the nineties in 20th century, its
Detection limit up to ng/ml levels, especially for some heavy metals, detection limit 2~3 orders of magnitude lower than common ICP-AES；
It is suitable for Simultaneous multi element analysis；Compared with the pay streak atomic emission spectrum of heavy element, mass spectrographic spectral line wants much less, therefore composes
Comparatively line interference is not a major issue；Isotope analyses can be carried out.ICP-MS is metal in present different medium
The study hotspot of analysis, it is clear that also can be an important directions of future development.
In soil, particularly ambient soil, the content of contamination metal elements is typically relatively low, and in this regard ICP-MS methods are especially
Can show that simultaneously ICP-MS methods greatly expand detectable element species in soil to its superiority, realize the multielement same time-division
Analysis, improves work efficiency.
The content of the invention
The present invention can not simultaneously detect multiple elements for the detection method of tenor in soil in prior art, detect
Less efficient problem, there is provided a kind of easy, quick, analyze speed is fast, and detection limit is low, measures dynamic linear response range width, can be same
When detect soil in Determination of multiple metal elements detection method.
The technical scheme is that：Inductively coupled plasma mass spectrometry determines the content of Chromium in Soil arsenic cadmium lead, main
Comprise the following steps：
1) soil sample is cleared up：Claim the air-dried soil sample that 0.05g or so crosses 200 mesh sieves in 50ml polytetrafluoroethylene beakers, add
8ml nitric acid and 1ml Fluohydric acid .s, shake up, and clear up 150 DEG C of instrument in electric heating and clear up 20~24 hours, and then electric heating is cleared up instrument and is warming up to
180 DEG C are caught up with acid to digestion solution residue 1ml or so；
2) the dilution constant volume of digestion solution is filtered：The digestion solution in polytetrafluoroethylene beaker is washed out to 15ml modelings with ultra-pure water
In material centrifuge tube, 14.0ml is settled to, with 0.45 μm of cellulose acetate film filter resolution liquid, takes the digestion solution 2.0ml after filtering,
10.0ml is settled to ultra-pure water；
3) detected using Inductively coupled plasma mass spectrometry instrument：
A) preparation of standard solution：Hybrid standard stock solution is taken, with 0.5% salpeter solution stepwise dilution to concentration point
Not Wei 0.1,0.2,0.5,1.0,10.0,20.0,50.0,100.0ppb standard working solution；
B) it is molten using icp mses examination criteria working solution and the sample Jing after clearing up constant volume and filter
Liquid；
4) interpretation of result：Chromium arsenic in pedotheque is calculated according to the soil sample weight for weighing and the concentration for detecting digestion solution
The content of cadmium lead；
W be soil sample tenor, mg/kg；
C is metal concentration in digestion solution, μ g/kg；
V be digestion solution constant volume, mL；
M is the quality for weighing soil, g.
Further, in such scheme, described step 3) Plays working solution preparation：Select during detection chromium arsenic lead
Standard working solution concentration be 1.0,10.0,20.0,50.0,100.0ppb；Detect that the standard working solution concentration selected during cadmium is
0.1,0.2,0.5,1.0,10.0ppb.
Further, in such scheme, the step 3) in Inductively coupled plasma mass spectrometry instrument main working parameters be：
Wriggling pump speed：40rpm, scanning times：50 times, repeated measure number of times：2 times, sample lifts the time：50s, scavenging period：10s,
Fog chamber's temperature：2.7 DEG C, nebulizer flow 1.03l/min, plasma torch power：1548.6W, cooling gas flow：14l/min,
Cooling water flow：3.5l/min.
Compared with prior art, the invention has the beneficial effects as follows：The detection method of the present invention is easy, quick, analyze speed
Hurry up, detection limit is low, the detection of chromium is limited to 0.0127mg/kg, and the detection of arsenic is limited to 0.0147mg/kg, the detection of cadmium is limited to
0.0048mg/kg, the detection of lead is limited to 0.0039mg/kg, and TIANZHU XINGNAO Capsul is 89%~113%, and relative standard deviation is less than
4.5%；Measurement dynamic linear response range width, can simultaneously detect Determination of multiple metal elements in soil, substantially increase work efficiency.
Specific embodiment
Take certain field soil cross 200 mesh sieves air-dry after, claim 1g, be divided into 20 parts, be designated as respectively A1, A2, A3,
A4...A20, determines the content of Chromium in Soil arsenic cadmium lead, mainly with the inductively coupled plasma mass spectrometry of the present invention respectively
Comprise the following steps：
1) soil sample is cleared up：Claim the air-dried soil sample that 0.05g or so crosses 200 mesh sieves in 50ml polytetrafluoroethylene beakers, add
8ml nitric acid and 1ml Fluohydric acid .s, shake up, and clear up 150 DEG C of instrument in electric heating and clear up 20 hours, and then electric heating clears up instrument and is warming up to 180 DEG C
Acid is caught up with to digestion solution residue 1ml or so；
2) the dilution constant volume of digestion solution is filtered：The digestion solution in polytetrafluoroethylene beaker is washed out to 15ml modelings with ultra-pure water
In material centrifuge tube, 14.0ml is settled to, with 0.45 μm of cellulose acetate film filter resolution liquid, takes the digestion solution 2.0ml after filtering,
10.0ml is settled to ultra-pure water；
3) detected using Inductively coupled plasma mass spectrometry instrument：
A) preparation of standard solution：Hybrid standard stock solution is taken, with 0.5% salpeter solution stepwise dilution to concentration point
Not Wei 0.1,0.2,0.5,1.0,10.0,20.0,50.0,100.0ppb standard working solution；
The standard working solution concentration selected during detection chromium arsenic lead is 1.0,10.0,20.0,50.0,100.0ppb；Detection cadmium
The standard working solution concentration of Shi Xuanyong is 0.1,0.2,0.5,1.0,10.0ppb；
B) it is molten using icp mses examination criteria working solution and the sample Jing after clearing up constant volume and filter
Liquid；
Inductively coupled plasma mass spectrometry instrument main working parameters are：Wriggling pump speed：40rpm, scanning times：50 times, repeat
Pendulous frequency：2 times, sample lifts the time：50s, scavenging period：10s, fog chamber's temperature：2.7 DEG C, nebulizer flow 1.03l/
Min, plasma torch power：1548.6W, cooling gas flow：14l/min, cooling water flow：3.5l/min；
4) interpretation of result：According to the soil sample weight for weighing and the concentration for detecting digestion solution, calculate by formula below and be unearthed
The content of chromium arsenic cadmium lead in earth sample；
W be soil sample tenor, mg/kg；C is metal concentration in digestion solution, μ g/kg；V be digestion solution constant volume, mL；
M is the quality for weighing soil, g.
As a result it is as shown in table 1：
Table 1 uses testing result of the inventive method to 20 parts of pedotheques
The metallic element actual content of the pedotheque the results are shown in Table 2：
The metallic element actual content of table 2 pedotheque
| Each group metal species | Chromium (mg/kg) | Arsenic (mg/kg) | Cadmium (mg/kg) | Lead (mg/kg) |
| Content | 0.01674 | 0.02867 | 0.0095 | 0.00840 |
From the Comparative result of above Tables 1 and 2, the method for the present invention is detected between the data and actual value for obtaining
Deviation is especially little, and accuracy rate is up to more than 99.88%.
Finally it should be noted that：Above example only to illustrate technical scheme, rather than a limitation；Although
The present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those within the art that：It still may be used
To modify to the technical scheme described in previous embodiment, or equivalent is carried out to which part technical characteristic；And
These modifications are replaced, and do not make the spirit and model of the essence disengaging embodiment of the present invention technical scheme of appropriate technical solution
Enclose.
Claims (3)
1. inductively coupled plasma mass spectrometry determines the content of Chromium in Soil arsenic cadmium lead, it is characterised in that mainly including following
Step：
1) soil sample is cleared up：Claim the air-dried soil sample that 0.05g or so crosses 200 mesh sieves in 50ml polytetrafluoroethylene beakers, add 8ml nitre
Acid and 1ml Fluohydric acid .s, shake up, and clear up instrument in electric heating and clear up, catch up with acid to digestion solution residue 1ml or so.
2) the dilution constant volume of digestion solution is filtered：With ultra-pure water by the digestion solution in polytetrafluoroethylene beaker wash out to 15ml plastics from
In heart pipe, 14.0ml is settled to, with 0.45 μm of cellulose acetate film filter resolution liquid, takes the digestion solution 2.0ml after filtering, use super
Pure water is settled to 10.0ml.
3) detected using Inductively coupled plasma mass spectrometry instrument：
A) preparation of standard solution：Hybrid standard stock solution is taken, is respectively to concentration with 0.5% salpeter solution stepwise dilution
0.1,0.2,0.5,1.0,10.0,20.0,50.0,100.0ppb standard working solution；
B) using icp mses examination criteria working solution and the sample solution Jing after clearing up constant volume and filter；
4) interpretation of result：Chromium arsenic cadmium lead in pedotheque is calculated according to the soil sample weight for weighing and the concentration for detecting digestion solution
Content；
W be soil sample tenor, mg/kg；
C is metal concentration in digestion solution, μ g/kg；
V be digestion solution constant volume, mL；
M is the quality for weighing soil, g.
2. inductively coupled plasma mass spectrometry as described in claim 1 determines the content of Chromium in Soil arsenic cadmium lead, and it is special
Levy and be, described step 3) Plays working solution preparation：The standard working solution concentration selected during detection chromium arsenic lead is 1.0,
10.0,20.0,50.0,100.0ppb；The standard working solution concentration selected during detection cadmium is 0.1,0.2,0.5,1.0,
10.0ppb。
3. inductively coupled plasma mass spectrometry as described in claim 1 determines the content of Chromium in Soil arsenic cadmium lead, and it is special
Levy and be, the step 3) in Inductively coupled plasma mass spectrometry instrument main working parameters be：Wriggling pump speed：40rpm, scanning time
Number：50 times, repeated measure number of times：2 times, sample lifts the time：50s, scavenging period：10s, fog chamber's temperature：2.7 DEG C or so, mist
Change device flow 1.03l/min, plasma torch power：1548.6W, cooling gas flow：14l/min, cooling water flow：3.5l/
min。
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| CN107167361A (en) * | 2017-07-07 | 2017-09-15 | 苏州汉宣检测科技有限公司 | A kind of heavy metal in soil content analysis method |
| CN107389781A (en) * | 2017-08-25 | 2017-11-24 | 金川集团股份有限公司 | Silver-colored rapid assay methods in a kind of cobaltosic oxide, cobalt acid lithium |
| CN108120785A (en) * | 2018-01-03 | 2018-06-05 | 江苏中宜金大分析检测有限公司 | The method of abio-arsenic residues and resolution centrifugal device in a kind of measure rice flour |
| CN108181373A (en) * | 2018-01-02 | 2018-06-19 | 江苏中宜金大分析检测有限公司 | A kind of method of 12 kinds of metallic elements in measure soils and sediments |
| CN108181445A (en) * | 2018-01-02 | 2018-06-19 | 江苏中宜金大分析检测有限公司 | A kind of method for measuring mercury in soils content |
| CN108362545A (en) * | 2018-03-21 | 2018-08-03 | 江苏实朴检测服务有限公司 | The method for measuring soil available arsenic |
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| 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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| CN107167361A (en) * | 2017-07-07 | 2017-09-15 | 苏州汉宣检测科技有限公司 | A kind of heavy metal in soil content analysis method |
| CN107389781A (en) * | 2017-08-25 | 2017-11-24 | 金川集团股份有限公司 | Silver-colored rapid assay methods in a kind of cobaltosic oxide, cobalt acid lithium |
| CN108181373B (en) * | 2018-01-02 | 2020-07-03 | 江苏中宜金大分析检测有限公司 | Method for measuring 12 metal elements in soil and sediment |
| CN108181373A (en) * | 2018-01-02 | 2018-06-19 | 江苏中宜金大分析检测有限公司 | A kind of method of 12 kinds of metallic elements in measure soils and sediments |
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