CN111122550A - Method for measuring trace elements and macro-components in marine sediments - Google Patents
Method for measuring trace elements and macro-components in marine sediments Download PDFInfo
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- CN111122550A CN111122550A CN202010034964.3A CN202010034964A CN111122550A CN 111122550 A CN111122550 A CN 111122550A CN 202010034964 A CN202010034964 A CN 202010034964A CN 111122550 A CN111122550 A CN 111122550A
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- 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
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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Abstract
The invention discloses a method for measuring trace elements and macro components in marine sediments, which comprises the following steps: drying the marine sediments, and grinding the marine sediments to 200 meshes to obtain a sample; placing a sample in a polytetrafluoroethylene inner container, sequentially adding redistilled hydrofluoric acid and redistilled nitric acid, sealing, heating for dissolving, cooling, adding redistilled nitric acid and ultrapure water, sealing, heating for extracting, cooling to room temperature, and adding redistilled nitric acid for constant volume; and measuring the trace elements and the constant components in the sample solution by using an inductively coupled plasma emission spectrometer. The invention selects high-temperature high-pressure closed digestion samples in the reaction kettle, has complete digestion, less acid consumption and low process blank value, is clear and transparent liquid after digestion, avoids the centrifugation step before the sample is measured on a machine, and is very suitable for the digestion of marine sediments and soil samples. The method fully considers the error introduced by the sample in the pretreatment process to prepare the working curve solution, thereby improving the accuracy of the method.
Description
Technical Field
The invention belongs to the field of chemical detection, and particularly relates to a method for determining trace elements and macro-components in marine sediments.
Background
Various sediments deposited on the water bottom, such as bottom mud and the like. The sources are: (1) suspended matters such as silt carried in water bodies of rivers, lakes and seas; (2) remains of aquatic organisms and their decomposition products; (3) water pollutants, in particular to heavy metals such as mercury, cadmium, lead, zinc, nickel and the like and organic matters with strong adsorbability. Through the analysis of the physical, chemical, biological and other characteristics of the sediment at the water bottom and the research of the sediment environment, the types of the pollutants in a plurality of past times can be found out, the pollution degree is judged, and the position of the pollution source is determined.
Disclosure of Invention
The invention aims to provide a method for measuring trace elements and macro-components in marine sediments, so as to improve the accuracy of measuring the trace elements and the macro-components in the marine sediments and simplify the operation steps.
In order to realize the purpose of the invention, the invention adopts the following technical scheme to realize:
a method for determining trace elements and macro-components in marine sediments, comprising the steps of:
s1: drying the marine sediments, and grinding the marine sediments to 200 meshes to obtain a sample;
s2: placing a sample in a polytetrafluoroethylene closed tank inner container, sequentially adding redistilled hydrofluoric acid and redistilled nitric acid, heating and dissolving after sealing, adding redistilled nitric acid and ultrapure water after cooling, heating and extracting in a sealing way, cooling to room temperature, and adding redistilled nitric acid to a constant volume to obtain a sample solution;
s3: analyzing standard substances by using a standard stock solution and a water system component to draw a working curve, measuring trace elements and major components in a sample solution and a blank solution by using an inductively coupled plasma emission spectrometer under the same condition, and calculating the contents of aluminum oxide, ferric oxide, manganese oxide, titanium dioxide, phosphorus pentoxide, calcium oxide, magnesium oxide, potassium oxide, sodium oxide and barium according to the formula (1); calculating the contents of strontium, vanadium, chromium, copper, zinc and zirconium according to the formula (2);
in the formula:
ρi-the values of the mass concentration of the elements in the sample solution in micrograms per gram;
ρ0-the values of the mass concentration of each element in the blank solution in units of micrograms per gram;
mi is the value of the mass of the sample solution in grams;
m is the value of the mass of the sample in grams.
Further, the drying temperature in the S1 is 100-110 ℃.
Further, the step S2 includes heating for dissolution, uncovering the cover, heating to be in a wet salt shape, adding redistilled nitric acid to drive hydrofluoric acid to be evaporated to be nearly dry, and cooling.
Further, the heating and dissolving in the S2 are carried out at the temperature of 180-200 ℃ for 45-50 h.
Further, the heating temperature of the opened cover in S2 is 140-160 ℃.
Further, the indoor operating conditions of S2 are: the indoor temperature is 20-25 ℃, and the relative humidity is 50-65%.
Further, the volume ratio of the redistilled nitric acid to the ultrapure water in the S2 is 1-1.2: 1.
Further, the heating and extraction temperature in S2 is 141-170 ℃, and the time is 7-10 hours.
Further, the drawing method of the S3 working curve includes: weighing four parts of water system component analysis standard substances in parallel, taking one part of the water system component analysis standard substances to prepare standard solution STD1, taking the other three parts as substrates, respectively adding the three parts into three groups of mixed standard solutions prepared by diluting standard stock solutions according to the proportion of 1: 1 to prepare standard solutions STD2, STD3 and STD4, and keeping the nitric acid acidity with the volume fraction of 2%; nitric acid with a volume fraction of 2% was used as a blank standard solution STD0, and a working curve was drawn in proportion to the concentration of the standard sample solution.
Further, in the step S3, at least 1 time of the standard substance sample solution is measured for each 10 sample solutions, and the cleaning time of each sample injection is not less than 1 min.
Compared with the prior art, the invention has the advantages and the technical effects that: the invention provides a method for measuring trace elements and major components in marine sediments, which is used for measuring 15 components of aluminum oxide, ferric oxide (total iron), manganese oxide, titanium dioxide, phosphorus pentoxide, calcium oxide, magnesium oxide, potassium oxide, sodium oxide, barium, strontium, vanadium, chromium, copper and zinc in the marine sediments.
The method selects a high-temperature high-pressure closed digestion sample in the reaction kettle, has the advantages of complete digestion, less acid consumption, low process blank value and the like, is clear and transparent liquid after digestion, avoids the centrifugation step before the sample is measured on a machine, does not need to worry about the blockage problem of subsequent instrument detection, and is very suitable for the digestion of marine sediments and soil samples.
The method fully considers the error introduced by the sample in the pretreatment process, so that a national primary standard substance similar to an unknown sample component is used for preparing the sample according to the same pretreatment step, and then the sample is uniformly mixed with a multi-element standard solution with a concentration gradient to prepare a working curve solution, thereby improving the accuracy of the method.
Drawings
FIG. 1 is a schematic view of a polytetrafluoroethylene inner container of a stuffy can;
figure 2 is a schematic representation of a teflon-containing closed can placed in an oven containing the sample.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the following examples.
Example 1
The method disclosed by the invention is suitable for measuring 15 components of aluminum oxide, ferric oxide (total iron), manganese oxide, titanium dioxide, phosphorus pentoxide, calcium oxide, magnesium oxide, potassium oxide, sodium oxide, barium, strontium, vanadium, chromium, copper and zinc in the marine sediments.
The principle of the method is as follows: the sample is decomposed by redistilled hydrofluoric acid and redistilled nitric acid under high temperature and high pressure, the hydrofluoric acid is evaporated and removed in an open system, salts are heated and dissolved by nitric acid, and finally the salts are converted into a 2% nitric acid solution medium, and 15 elements are measured by an inductively coupled plasma emission spectrometer.
Reagent and preparation
Hydrofluoric acid (. rho.1.15 g/mL);
re-steaming hydrofluoric acid: distilling hydrofluoric acid (rho is 1.15g/mL) by a sub-boiling distiller;
nitric acid (. rho.1.42 g/mL);
redistilling nitric acid: nitric acid (. rho.1.42 g/mL) was distilled via a sub-boiling still.
Nitric acid (2+ 98): preparing nitric acid (rho is 1.42g/mL) according to the volume fraction of 2: 98;
standard stock solutions: preparing standard stock solution of each component by using spectrally pure metal, metal oxide or salts thereof, or using a commercially available certified single element standard solution.
Second, instrument and equipment
A full-spectrum direct-reading inductively coupled plasma emission spectrometer;
automatic temperature control electric heating plate: the highest temperature is 250 ℃, the temperature error is less than +/-5 ℃, and the surface of the composite material is protected by a polytetrafluoroethylene coating;
a polytetrafluoroethylene closed sample dissolving tank: the volume is 10mL, and the sealing cover and the overpressure protection function are realized;
balance: the sensory dose is 0.01 mg.
Automatic temperature control oven: the maximum temperature is 250 ℃, and the temperature error is less than +/-5 ℃.
Method for measuring micro and macro components in marine sediments
The method comprises the following specific steps:
1. sample preparation
Drying the marine sediments at 105 ℃, and grinding the marine sediments to 200 meshes in a clean environment by using an agate mortar for later use.
2. Sample digestion
50mg of sample is accurately weighed to the nearest 0.01 mg. Putting a sample in a polytetrafluoroethylene sealed tank inner container (figure 1), wetting by using a plurality of drops of deionized water, sequentially adding 1.5mL of redistilled hydrofluoric acid and 1.5mL of redistilled nitric acid, covering and putting in a sealed steel sleeve, heating and dissolving for 48h at 190 ℃ in an oven (figure 2), taking out a cover, putting on an electric heating plate, heating to a wet salt state at 150 ℃, adding 1mL of redistilled nitric acid to drive out hydrofluoric acid, drying by distillation, taking down and cooling, adding 1.5mL of redistilled nitric acid and 1.5mL of ultrapure water, covering and putting in a sealed steel sleeve, fully extracting for 8h at 150 ℃ in the oven, obtaining a clear and transparent solution, and cooling to room temperature. And (5) accurately metering the volume to 50g by redistilled nitric acid, shaking up, and preparing for measurement.
The preparation process of the sample is completed in a clean laboratory, and the experimental conditions are that the temperature is 22 ℃ and the relative humidity is 60%.
3. Sample assay
1) Preparation of working curve
The standard stock solutions were removed separately and diluted to three sets of mixed standard solutions (S1, S2, S3) according to table 1, keeping the nitric acid acidity at a volume fraction of 2%.
TABLE 1 concentration of each component of the mixed standard solution/(μ g/g)
Weighing four parts of national first-class standard substance-water system component analysis standard substance GBW07311 in parallel as unknown samples, decomposing the samples according to the steps, taking one part to prepare standard solution (STD1), taking the other three parts as substrates, adding the three parts into S1, S2 and S3 respectively according to the proportion of 1: 1 to prepare standard solutions (STD2, STD3 and STD4), and keeping the acidity of nitric acid with the volume fraction of 2%; the blank standard solution (STD0) was 2% nitric acid by volume fraction (see table 2).
TABLE 2 Standard series of solutions 15 elements concentration/. mu.g/g
2) Sample assay
And drawing a working curve according to the working condition set by the instrument, wherein the measurement peak area is in direct proportion to the concentration of the standard sample solution. Under the same conditions, the concentration or content of unknown sample solution (including blank and monitoring substance) is directly printed.
At least 1 time of measuring the standard substance sample solution every 10 sample solutions, and the cleaning time of each sample injection is not less than 1 min.
4. Recording and calculating
The calculated results of the contents of aluminum oxide, ferric oxide (total iron), manganese oxide, titanium dioxide, phosphorus pentoxide, calcium oxide, magnesium oxide, potassium oxide and sodium oxide are calculated according to the mass fraction WbIn terms of percentage (%), calculated according to formula (1); the calculated results of the contents of barium, strontium, vanadium, chromium, copper, zinc and zirconium are calculated by mass fraction WbIn terms of micrograms per gram (. mu.g/g), the values are calculated according to equation (2).
In the formula:
ρi-the values of the mass concentration of the elements in the sample solution are given in micrograms per gram (μ g/g);
ρ0-the values of the mass concentrations of the elements in the blank solution are given in micrograms per gram (μ g/g);
mi-the mass of the sample solution in grams (g);
m is a value of the mass of the sample in grams (g).
The calculation results of the contents of aluminum oxide, ferric oxide (total iron), manganese oxide, titanium dioxide, phosphorus pentoxide, calcium oxide, magnesium oxide, potassium oxide, sodium oxide and barium are retained to two decimal places. The calculation result of the contents of strontium, vanadium, chromium, copper and zinc is less than 100 mug/g, and three effective digits are reserved; greater than or equal to 100 mug/g, with integer digits retained.
(1) Precision and accuracy
The precision and accuracy of 15 elements of aluminum oxide, ferric oxide (total iron), manganese oxide, titanium dioxide, phosphorus pentoxide, calcium oxide, magnesium oxide, potassium oxide, sodium oxide, barium, strontium, vanadium, chromium, copper and zinc in the marine sediment sample are shown in table 3.
Precision and accuracy measurements of the 315 elements in Table
(2) Quality control
1) Analytical blank test
The remaining steps are exactly equivalent to sample digestion except that no marine sediment sample is added. The solution thus prepared was used as an analysis blank.
2) Method detection limit
The detection limits of 15 components of aluminum oxide, ferric oxide (total iron), manganese oxide, titanium dioxide, phosphorus pentoxide, calcium oxide, magnesium oxide, potassium oxide, sodium oxide, barium, strontium, vanadium, chromium, copper and zinc in the marine sediment sample are shown in table 4.
TABLE 415 measurement results of detection limits of the components
Remarking: the solution in this example was diluted 1000 times before testing on the machine
3) Parallel sample and quality control sample
10% of the samples were randomly sampled for each analysis batch as replicates, while 1-2 standards were inserted for each analysis batch as quality control samples.
4) Matters of attention
(1) The sample collection, storage and transportation shall meet the requirements of the sample collection, storage and transportation part in GB17378.2 ocean monitoring Specification.
(2) The data processing and analysis quality control should meet the requirements of the data processing and analysis quality control part in GB17378.3 ocean monitoring Specification.
(3) The blank of the whole process is strictly controlled to be less than 3 times of the lower limit of the measurement in the experimental process, which is the key for ensuring the lower limit of the measurement of the standard. Otherwise, the lower limit of measurement should be re-determined according to the blank value of the whole process.
(4) The content of silicon, aluminum, iron, calcium and titanium in the marine sediments is high, the interference on the analysis spectral lines of other elements is easy to generate, spectral lines with high spectral line intensity, good peak shape and less interference are selected as analysis lines, and the interference possibly generated by interference elements on other elements is corrected by adopting an interference coefficient method.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (10)
1. A method for measuring trace elements and macro-components in marine sediments is characterized in that: the method comprises the following steps:
s1: drying the marine sediments, and grinding the marine sediments to 200 meshes to obtain a sample;
s2: placing a sample in a polytetrafluoroethylene closed tank inner container, sequentially adding redistilled hydrofluoric acid and redistilled nitric acid, heating and dissolving after sealing, adding redistilled nitric acid and ultrapure water after cooling, heating and extracting in a sealing way, cooling to room temperature, and adding redistilled nitric acid to a constant volume to obtain a sample solution;
s3: analyzing standard substances by using a standard stock solution and a water system component to draw a working curve, measuring trace elements and major components in a sample solution and a blank solution by using an inductively coupled plasma emission spectrometer under the same condition, and calculating the contents of aluminum oxide, ferric oxide, manganese oxide, titanium dioxide, phosphorus pentoxide, calcium oxide, magnesium oxide, potassium oxide, sodium oxide and barium according to the formula (1); calculating the contents of strontium, vanadium, chromium, copper, zinc and zirconium according to the formula (2);
in the formula:
ρi-the values of the mass concentration of the elements in the sample solution in micrograms per gram;
ρ0-the values of the mass concentration of each element in the blank solution in units of micrograms per gram;
mi is the value of the mass of the sample solution in grams;
m is the value of the mass of the sample in grams.
2. The method of claim 1 for determining trace elements and macro-components in marine sediments, comprising: and the drying temperature in the S1 is 100-110 ℃.
3. The method of claim 1 for determining trace elements and macro-components in marine sediments, comprising: and S2, heating and dissolving, opening the cover, heating to a wet salt state, adding redistilled nitric acid to drive hydrofluoric acid to evaporate till the hydrofluoric acid is nearly dry, and cooling.
4. The method of claim 1 for determining trace elements and macro-components in marine sediments, comprising: and the heating and dissolving in the S2 are carried out at the temperature of 180-200 ℃ for 45-50 h.
5. The method of claim 3 for determining trace elements and macro-components in marine sediments, comprising: and the heating temperature of the middle opening cover of S2 is 140-160 ℃.
6. The method of claim 1 for determining trace elements and macro-components in marine sediments, comprising: the indoor operating conditions of S2 are: the indoor temperature is 20-25 ℃, and the relative humidity is 50-65%.
7. The method of claim 1 for determining trace elements and macro-components in marine sediments, comprising: the volume ratio of the redistilled nitric acid to the ultrapure water in the S2 is 1-1.2: 1.
8. The method of claim 1 for determining trace elements and macro-components in marine sediments, comprising: and heating and extracting at 141-170 ℃ in S2 for 7-10 hours.
9. The method of claim 1 for determining trace elements and macro-components in marine sediments, comprising: the drawing method of the S3 working curve comprises the following steps: weighing four parts of water system component analysis standard substances in parallel, taking one part of the water system component analysis standard substances to prepare standard solution STD1, taking the other three parts as substrates, respectively adding the three parts into three groups of mixed standard solutions prepared by diluting standard stock solutions according to the proportion of 1: 1 to prepare standard solutions STD2, STD3 and STD4, and keeping the nitric acid acidity with the volume fraction of 2%; nitric acid with a volume fraction of 2% was used as a blank standard solution STD0, and a working curve was drawn in proportion to the concentration of the standard sample solution.
10. The method of claim 1 for determining trace elements and macro-components in marine sediments, comprising: and in the S3, the standard substance sample solution is measured at least 1 time every 10 sample solutions are measured, and the cleaning time of each sample injection is not less than 1 min.
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Application publication date: 20200508 |