CN110320264A - Inductively coupled plasma mass spectrometry measure marine sediment in lead, cadmium, chromium, copper, zinc, nickel content detection method - Google Patents
Inductively coupled plasma mass spectrometry measure marine sediment in lead, cadmium, chromium, copper, zinc, nickel content detection method Download PDFInfo
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Abstract
The present invention provides lead in a kind of inductively coupled plasma mass spectrometry measurement marine sediment, cadmium, chromium, copper, zinc, nickel content detection method, comprising: standard uses the preparation of solution, the preparation of standard solution, the preparation of test solution, blank reagent solution, measurement.This method has the characteristics that spectral line is simple, high sensitivity, speed are fast and interference is few, can be completed at the same time the quantitative determination of this 6 elements in a few minutes.The detection method for the specification that content of beary metal measures in marine sediment can be provided for society; research achievement carries out quality monitoring for government department and provides the technical standard and technical basis of science, has important learning value and application prospect to improvement marine environment, protection marine resources and damage etc. of preventing and remedying pollution is accelerated.
Description
Technical field
The present invention relates to lead in a kind of marine sediment, cadmium, chromium, copper, zinc, nickel content detection method, and in particular to one
Lead in kind of inductively coupled plasma mass spectrometry measurement marine sediment, cadmium, chromium, copper, zinc, nickel content detection method.
Background technique
Influence with the mankind to environment, many heavy metal contaminants are discharged into maritime waters, and heavy in ocean
Product object will affect fractions distribution, Transport And Transformation and home to return to of the heavy metal in ocean to absorption, the release of heavy metal.As pollution
" memory " of object, marine sediment pollutant transport and storing process in all play an important role.In deposit not
The heavy metal and microelement pollutant of disconnected accumulation can generate toxic action to benthon or by the biology of deposit existence,
Thus deposit is being increasingly used for evaluation mankind's activity impact caused by water environment.
In recent years, due to being influenced by factors such as cultivation density height, external contaminants, cause eutrophication problem increasingly tight
Weight, red tide happen occasionally, and cause harm to Fujian Province's marine environment ecology.The safety of aquatic products is influenced simultaneously, and heavy metal is made
At potential food safety hazard more can not be ignored.Therefore heavy metal and microelement pollutant in monitoring marine sediment
Changes of contents is of great significance.
China at present not yet establish and meanwhile measure lead in marine sediment, cadmium, chromium, copper, zinc, nickel content examination criteria,
National standard " the 5th part of GB 17378.5-2007 marine monitoring specification: sediment analysis " prevailing for the time being in force and ocean industry
Standard " iron in HY/T 206-2016 marine sediment and organism, manganese, nickel, potassium, sodium, calcium, magnesium measurement Atomic absorption point
Light photometry ", 5 in metallic element in common heavy metal (totally 6 kinds, respectively lead, cadmium, chromium, copper, zinc, nickel) can only be detected
Kind (lead, cadmium, copper, zinc, nickel), not comprehensively；And be to be detected using atomic absorption spectrography (AAS), each element need one by one into
Row detection, detection time are long.Ocean professional standard " HY/T 132-2010 marine sediment and marine organism prevailing for the time being in force
Middle Analysis of Heavy Metal pre-treatment Microwave Digestion ", before only having standardized 5 kinds of metal class heavy metals (lead, cadmium, chromium, copper, zinc)
Processing method, and not comprising the content of detection method, not comprehensively.Therefore it is badly in need of developing a comprehensive, quick sea
The examination criteria of foreign Heavy Metal In Sediments content.
With the rapid development of instrumental analytical chemistry and greatly improving for social economy's strength, there is high sensitivity, detection
Limit the inductive coupling etc. for the features such as low, spectral line simply, relative to spectral technique interferes less, analysis speed is fast and high degree of automation
Gas ions mass spectrograph has been obtained generally transporting by the favor of government and market in units such as many testing laboratories, scientific research institutions
With.But country, industry and the provincial standard of inductively coupled plasma mass spectrometry detection metallic element class is used not to keep up with section
The skill speed of development carries out follow-up in time and formulates and implement, so that detection unit is not available icp ms
Detection task is rapidly completed, causes that great assets are idle and the wasting of resources, has seriously affected detection efficiency, the industry of relevant unit
Business is promoted and development speed, therefore develops, formulates and implement the standard of inductively coupled plasma mass spectrometry measurement metallic element
It is a very urgent project.
Therefore, this project establish for the first time using inductively coupled plasma mass spectrometry measurement marine sediment in lead, cadmium,
Chromium, copper, zinc, nickel content detection method standard, it is special that this method has that spectral line is simple, high sensitivity, speed are fast and interference is few etc.
Point can be completed at the same time the quantitative determination of this 6 elements in a few minutes.Heavy metal in marine sediment can be provided for society to contain
The detection method of fixed specification is measured, research achievement carries out quality monitoring for government department and provides the technical standard and technology of science
Foundation, to accelerate to improve marine environment, protection marine resources and prevent and remedy pollution damage etc. with important learning value with
Application prospect.
Summary of the invention
The purpose of the present invention is to provide a kind of inductively coupled plasma mass spectrometry measurement marine sediment in lead, cadmium,
Chromium, copper, zinc, nickel content detection method.
To achieve the above object, the present invention adopts the following technical scheme:
Lead in a kind of marine sediment, cadmium, chromium, copper, zinc, nickel content detection method, include the following steps:
(1) standard uses the preparation of solution: taking suitable Standard Stock solutions, is diluted to response step by step with 1wt% nitric acid solution
Concentration, the hybrid standard for being configured to following concentration use solution: lead, cadmium, chromium, nickel are 1.0 μ g/mL, and copper, zinc are 10.0 μ g/mL；
(2) 0mL, 0.05 mL, 0.25 mL, 0.50 mL, 1.00 mL, 2.50 mL standards accurately the preparation of standard solution: are drawn
Using solution, in 6 50mL volumetric flasks, it is settled to scale with nitric acid solution dilution, is mixed, lead, cadmium, chromium, nickel standard series
Concentration are as follows: 0 μ g/L, 1.0 μ g/L, 5.0 μ g/L, 10.0 μ g/L, 20.0 μ g/L, 50.0 μ g/L；Copper, zinc standard series concentration are as follows: 0
μg/L,10.0μg/L,50.0μg/L,100.0μg/L,200.0μg/L,500.0μg/L；
(3) preparation of test solution: learning from else's experience mixes well representational sample and is no less than 1000g, and sample is dried through 65 DEG C
To constant weight, crushes or grind, cross 0.25mm sample sifter, mix to obtain sample, be fitted into closed container, room temperature preservation is spare；Claim
Materials 0.1~0.5g, is accurate to 0.001g, is placed in micro-wave diminishing pot, and accurate addition 6mL nitric acid solution, 2mL hydrofluoric acid are molten
Liquid and 1mL perchloric acid solution, slight wobble infiltrate sample, after tightening bottle cap, heat up under 1600W: initial temperature room temperature, even in 5min
Speed is warming up to 120 DEG C, keeps 3min, and 150 DEG C are then at the uniform velocity warming up in 5min, keeps 3min, then in 5min at the uniform velocity
180 DEG C are warming up to, 3min is kept, 200 DEG C is at the uniform velocity warming up in last 5min, keep 20min；After cooling, by counteracting tank
It is transferred in digesting and catches up with acid to 1mL, after cooling, shift digestion solution in 25mL volumetric flask, rinse counteracting tank with deionized water
And cleaning solution is transferred in volumetric flask, with water constant volume, mix, stand for standby use；
(4) blank reagent solution: according to the method reagent preparation blank solution of step (3)；
(5) it measures: choosing Sc, In, Rh, Ho element is internal standard, and is corrected to the element of measurement；Sequentially determining is each dense
The standard solution of degree, using the average value of 3 survey measurements as ordinate, concentration is abscissa, draws standard curve；It will be for
Test sample solution is introduced into icp ms, and measurement takes the average value of 3 readings, calculates from standard curve
Corresponding concentration is obtained, the concentration of corresponding blank solution is deducted, calculates the content of each element.
The present invention has the advantages that this project is established for the first time measures oceanographic sedimentation using inductively coupled plasma mass spectrometry
Lead in object, cadmium, chromium, copper, zinc, nickel content detection method standard, this method have that spectral line is simple, high sensitivity, speed are fast and
The features such as interference is few, can be completed at the same time the quantitative determination of this 6 elements in a few minutes.Marine sediment can be provided for society
The detection method of the specification of middle content of beary metal measurement, research achievement carry out quality monitoring for government department and provide the technology of science
Standard and technical basis, improve marine environment, protection marine resources to quickening and damage etc. of preventing and remedying pollution is with important
Learning value and application prospect.
Chloroazotic acid (hydrochloric acid ± nitric acid) is usually used to be digested, because of deposit after digestion in existing Microwave Digestion
There is the presence of many element silicons, and chloroazotic acid cannot dissolve silicon, so there is the precipitating of many whites, that is, be not easy to filter, also be easy
It causes to digest the disadvantages of incomplete.Digestion time is very long simultaneously, at least needs 72h.The present invention is using hydrochloric acid ± hydrogen fluorine
Acid ± perchloric acid, digestion time is very short, about 1h, while digestive juice is clarified very much.
Detailed description of the invention
Fig. 1 is lead standard solution curve graph；
Fig. 2 is cadmium standard solution curve graph；
Fig. 3 is chromium standard solution curve graph；
Fig. 4 is copper standard solution curve graph；
Fig. 5 is Zinc standard solution curve graph；
Fig. 6 is nickel standard solution curve graph.
Specific embodiment
1 principle
For sample after micro-wave digestion, test liquid introduces icp ms.For certain mass-to-charge ratio it is to be measured from
Son, mass signal response is directly proportional to the number of ions entered in mass spectrograph, measures sample by measuring mass spectrographic signal-count
The concentration of middle element.Using calibration curve method calculating elements content.
2 reagents and material
Unless otherwise indicated, this method agents useful for same is excellent pure grade.Experimental water meets the rule of level-one water in GB/T 6682
It is fixed.
Warning: various strong acid answer careful operation, dilute and take and carry out in draught cupboard, pay attention to not when using perchloric acid
It dryouies, it is careful to explode.
2.1 hydrofluoric acid solutions, ρ (HF)=1.49g/mL.
2.2 perchloric acid solutions, ρ (HClO4)=1.67g/mL。
2.3 nitric acid solutions, ρ (HNO3)=1.42g/mL。
2.41% nitric acid solution draws 1mL nitric acid, is settled to 100mL with deionized water.
2.5 Standard Stock solutions: directly buy it is commercially available have card the dedicated multielement standard solution of ICP-MS.
2.6 standards use solution: taking suitable Standard Stock solutions, be diluted to the dense of response step by step with 1% nitric acid solution
Degree, the hybrid standard for being configured to following concentration use solution: lead, cadmium, chromium, nickel are 1.0 μ g/mL, and copper, zinc are 10.0 μ g/mL.It is mixed
Standardization uses solution matching while using.
The 2.7 online inner mark solutions of mixing: scandium (45Sc), indium (115In) rhodium (103Rh), holmium (165Ho) concentration is 50.0 μ g/L,
Nitric acid solution medium.
2.8 mass spectrums tune solution: instrument provides tuning solution for oneself.
3 instrument and equipments
Note: container used is boiled using preceding with dust technology.If using dedicated digest tube and glassware, before each use
It does not need to be boiled with nitric acid.
3.1 icp ms (ICP-MS).
3.2 microwave digestion systems are furnished with high temperature high voltage resistant counteracting tank.
3.3 ultrapure water system.
3.4 assay balances: weighing accuracy to 0.0001g.
3.5 high-purity argon gas: purity is not less than 99.99%.
3.6 pipettors: 50 μ of μ L~1000 L of range.
3.7 sample comminution equipment: ball mill, pulverizer, 0.25mm sample sifter etc..
The preparation of 4 samples
It learns from else's experience and mixes well representational sample and be no less than 1000g.Sample is after through 65 DEG C, drying to constant weight, crushes or grinding,
0.25mm sample sifter is crossed, mixing is fitted into closed container, and room temperature preservation is spare.
5 analytical procedures
5.1 resolution
Sample about 0.1~0.5g is weighed, 0.001g is accurate to, is placed in micro-wave diminishing pot, it is accurate that 6mL nitric acid solution, 2mL is added
Hydrofluoric acid solution and 1mL perchloric acid solution, slight wobble infiltrate sample, after tightening bottle cap, heat up under 1600W: initial temperature room temperature,
It is at the uniform velocity warming up to 120 DEG C in 5min, keeps 3min, 150 DEG C are then at the uniform velocity warming up in 5min, keeps 3min, then
It is at the uniform velocity warming up to 180 DEG C in 5min, keeps 3min, 200 DEG C is at the uniform velocity warming up in last 5min, keep 20min.It is cooling
Afterwards, counteracting tank is transferred in digesting and catches up with acid to 1mL, after cooling, shift digestion solution in 25mL volumetric flask.Use deionized water
It rinses counteracting tank and cleaning solution is transferred in volumetric flask, with water constant volume, mix, stand for standby use.In postdigestive sample if any
Insoluble matter will stand overnight or take part centrifugal to clarification.
5.2 instrument reference conditions
Power (RF power): 1200W.
Sampling depth (sampling depth): 5mm.
Flow rate of carrier gas (carrier-gas flow): 0.70L/min.
Carrier gas compensation current speed (make-up-gas flow): 1.10L/min.
Sample promotes rate (sampling rate): 0.30L/min.
The time of integration (intergretion time): 0.2s.
The drafting of 5.3 standard curves
It is accurate to draw 0mL, 0.05 mL, 0.25 mL, 0.50 mL, 1.00 mL, 2.50 mL standard solutions, hold in 6 50mL
In measuring bottle, it is settled to scale with nitric acid solution dilution, is mixed.Lead, cadmium, chromium, nickel standard series concentration are as follows: 0 μ g/L, 1.0 μ g/L,
5.0μg/L,10.0μg/L,20.0μg/L,50.0μg/L；Copper, zinc standard series concentration are as follows: 0 μ g/L, 10.0 μ g/L, 50.0 μ g/
L,100.0μg/L,200.0μg/L,500.0μg/L.It is online to be added internal standard, concentration sample detection from low to high, with signal-count-
Concentration mapping, obtains standard curve regression equation.
5.4 measurement
With indexs such as the tuning sensitivity of solution conditioning instrumentation, oxide and double charge interference, to meet test request.Instrument is steady
After fixed, test liquid is introduced into plasma mass, internal standard is added online, obtains the signal meter of each element to be measured and internal standard element
Number, according to the intensity rate of element to be measured and internal standard element, the signal-count of each element to be measured after being corrected, by standard song
Line checks in the mass concentration of each element in sample.It is analyzed again after then applying nitric acid solution to dilute more than the range of linearity.
5.5 blank test
Duplicate blank test is carried out to be measured in parallel in addition to sample is not added using identical determination step.
6 results calculate
In terms of mass fraction X, unit is indicated the content of each element with milligrams per kilogram (mg/kg) in sample, is calculated by formula (1):
In formula:
The content of each element in X- sample, unit are milligrams per kilogram (mg/kg)；
A1The content of each element in sample liquid is measured, unit is nanograms per milliliter (ng/mL)；
A2The content of each element in blank solution, unit are nanograms per milliliter (ng/mL)；
V- sample constant volume, unit are milliliter (mL).
The quality of m- sample, unit are gram (g).
Each sample takes two Duplicate Samples to be measured, and is as a result, result indicates 0.01mg/ with its arithmetic mean of instantaneous value
kg。
7 precision
When 7.1 constituent contents≤0.5 mg/kg, the absolute difference of the measurement result independent twice obtained under the conditions of repeatability is not
30% more than arithmetic mean of instantaneous value is obtained, premised on being greater than 30% situation of arithmetic mean of instantaneous value of the two measured values and be no more than 5%.
When 7.2 constituent content 0.5 mg/kg of >, the absolute difference of the measurement result independent twice obtained under the conditions of repeatability
Value must not exceed the 20% of arithmetic mean of instantaneous value, before being no more than 5% with 20% situation of the arithmetic mean of instantaneous value greater than the two measured values
It mentions.
Table 1 analyzes substance mass number, corresponding internal standard compound and its mass number
The regression equation and related coefficient of standard curve are shown in Table 2, and related coefficient is both greater than 0.999, illustrates that linear relationship is good.
2 standard curve regression equation of table and related coefficient
Lead in marine sediment, cadmium, chromium, copper, zinc, nickel content measuring method carry out accuracy test, test result is shown in Table 3,3
For the testing result of a standard substance all in the error range of standard value, illustration method accuracy is good.
3 standard substance Comparability test result of table
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with repair
Decorations, are all covered by the present invention.
Claims (1)
1. the detection method of lead in a kind of marine sediment, cadmium, chromium, copper, zinc, nickel content, which is characterized in that including walking as follows
It is rapid:
(1) standard uses the preparation of solution: taking suitable Standard Stock solutions, is diluted to response step by step with 1wt% nitric acid solution
Concentration, the hybrid standard for being configured to following concentration use solution: lead, cadmium, chromium, nickel are 1.0 μ g/mL, and copper, zinc are 10.0 μ g/mL；
(2) 0mL, 0.05 mL, 0.25 mL, 0.50 mL, 1.00 mL, 2.50 mL standards accurately the preparation of standard solution: are drawn
Using solution, in 6 50mL volumetric flasks, it is settled to scale with nitric acid solution dilution, is mixed, lead, cadmium, chromium, nickel standard series
Concentration are as follows: 0 μ g/L, 1.0 μ g/L, 5.0 μ g/L, 10.0 μ g/L, 20.0 μ g/L, 50.0 μ g/L；Copper, zinc standard series concentration are as follows: 0
μg/L,10.0μg/L,50.0μg/L,100.0μg/L,200.0μg/L,500.0μg/L；
(3) preparation of test solution: learning from else's experience mixes well representational sample and is no less than 1000g, and sample is dried through 65 DEG C
To constant weight, crushes or grind, cross 0.25mm sample sifter, mix to obtain sample, be fitted into closed container, room temperature preservation is spare；Claim
Materials 0.1~0.5g, is accurate to 0.001g, is placed in micro-wave diminishing pot, and accurate addition 6mL nitric acid solution, 2mL hydrofluoric acid are molten
Liquid and 1mL perchloric acid solution, slight wobble infiltrate sample, after tightening bottle cap, heat up under 1600W: initial temperature room temperature, even in 5min
Speed is warming up to 120 DEG C, keeps 3min, and 150 DEG C are then at the uniform velocity warming up in 5min, keeps 3min, then in 5min at the uniform velocity
180 DEG C are warming up to, 3min is kept, 200 DEG C is at the uniform velocity warming up in last 5min, keep 20min；After cooling, by counteracting tank
It is transferred in digesting and catches up with acid to 1mL, after cooling, shift digestion solution in 25mL volumetric flask, rinse counteracting tank with deionized water
And cleaning solution is transferred in volumetric flask, with water constant volume, mix, stand for standby use；
(4) blank reagent solution: according to the method reagent preparation blank solution of step (3)；
(5) it measures: choosing Sc, In, Rh, Ho element is internal standard, and is corrected to the element of measurement；Sequentially determining is each dense
The standard solution of degree, using the average value of 3 survey measurements as ordinate, concentration is abscissa, draws standard curve；It will be for
Test sample solution is introduced into icp ms, and measurement takes the average value of 3 readings, calculates from standard curve
Corresponding concentration is obtained, the concentration of corresponding blank solution is deducted, calculates the content of each element.
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| CN111122692A (en) * | 2020-01-15 | 2020-05-08 | 自然资源部第一海洋研究所 | Method for measuring trace elements and rare earth elements in marine sediments and soil |
| CN111122550A (en) * | 2020-01-15 | 2020-05-08 | 自然资源部第一海洋研究所 | Method for measuring trace elements and macro-components in marine sediments |
| CN112630291A (en) * | 2020-11-02 | 2021-04-09 | 河北省药品医疗器械检验研究院 | Method for determining trace elements in silica gel medical instrument |
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| CN111122692A (en) * | 2020-01-15 | 2020-05-08 | 自然资源部第一海洋研究所 | Method for measuring trace elements and rare earth elements in marine sediments and soil |
| CN111122550A (en) * | 2020-01-15 | 2020-05-08 | 自然资源部第一海洋研究所 | Method for measuring trace elements and macro-components in marine sediments |
| CN114076793A (en) * | 2020-08-13 | 2022-02-22 | 深圳市疾病预防控制中心（深圳市卫生检验中心、深圳市预防医学研究所） | Method for determining iodine content in food based on inductively coupled plasma mass spectrometry |
| CN114076793B (en) * | 2020-08-13 | 2023-06-09 | 深圳市疾病预防控制中心（深圳市卫生检验中心、深圳市预防医学研究所） | Method for measuring iodine content in food based on inductively coupled plasma mass spectrometry |
| CN112630291A (en) * | 2020-11-02 | 2021-04-09 | 河北省药品医疗器械检验研究院 | Method for determining trace elements in silica gel medical instrument |
| CN113109323A (en) * | 2021-04-15 | 2021-07-13 | 山东省海洋资源与环境研究院(山东省海洋环境监测中心、山东省水产品质量检验中心) | Method for determining main heavy metal elements in marine sediments |
| CN113109322A (en) * | 2021-04-15 | 2021-07-13 | 山东省海洋资源与环境研究院(山东省海洋环境监测中心、山东省水产品质量检验中心) | Method for determining main heavy metal elements in marine organisms |
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Application publication date: 20191011 |