CN111257247A - Method for measuring iron content in marine sediments - Google Patents
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Abstract
The invention relates to the technical field of analysis and detection, provides a method for determining the iron content in marine sediments, and aims to solve the problem that the existing method for determining the iron content in marine sediments has poor accuracy of a determination result, and the method comprises the following steps: (1) pretreating a sample; (2) adding nitric acid and hydrofluoric acid, heating for digestion, cooling, adding perchloric acid, evaporating, cooling, adding hydrochloric acid solution, dissolving in warm water, transferring to a pipette, adding distilled water to a constant volume, and shaking up to obtain a sample solution; (3) drawing a standard curve; (4) and (3) measuring the absorbance of the sample solution by using a flame atomic absorption spectrophotometry, and comparing the absorbance with a standard curve to obtain the content of Fe in the marine sediment sample. The detection method provided by the invention is simple to operate and high in accuracy, and the mineral lattices in the marine sediments are destroyed by adopting a hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid full digestion method, so that all the element iron to be detected in the sample enters the solution, and the accuracy is improved.
Description
Technical Field
The invention relates to the technical field of analysis and detection, in particular to a method for measuring the content of iron in marine sediments.
Background
The continuous development of national economy of China continuously pushes the improvement of the living standard of people, environmental problems are more and more concerned by people in a new period, the investment in the field of marine environmental protection is increased along with the increase of the country, the marine environmental protection work is also developed to a higher level, heavy metal pollution is always a key point in the aspect of marine monitoring, the current marine standard mainly aims at preparing a standard method for copper, lead, zinc, cadmium, chromium, mercury and arsenic, but the marine standard in the aspect of trace elements is less developed by referring to other industrial, international and foreign standards and the like.
Mild iron poisoning can cause the harm of retarded development of children, hepatomegaly, liver cirrhosis, myocardial damage and the like, so that the determination of the iron content in the marine sediments has important research significance. The existing method for measuring the iron content mainly comprises a spectrophotometry method, wherein the method is combined with an oxalic acid-ammonium oxalate method for measuring, and part of crystal iron is possibly dissolved in the process of leaching amorphous iron in ocean sediments by an acidic oxalic acid solution, so that the measurement result is higher.
Disclosure of Invention
The invention provides the method for measuring the iron content in the marine sediments, which has high accuracy and simple operation, in order to overcome the problem of poor accuracy of the measurement result of the existing method for measuring the iron content in the marine sediments.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method of determining the iron content of a marine sediment comprising the steps of:
(1) collecting a marine sediment sample for pretreatment, then grinding and pressing, uniformly mixing through a 2mm nylon sieve, grinding through a 100-mesh nylon sieve, and uniformly mixing to obtain a sample to be detected;
(2) weighing 0.2-0.3 g (accurate to 0.0001g) of a sample to be detected, putting the sample to be detected into a digestion tank, sequentially adding nitric acid and hydrofluoric acid, heating and digesting, adding perchloric acid after cooling, evaporating at 150-180 ℃ until the content is viscous, taking down the digestion tank, cooling, adding a hydrochloric acid solution, dissolving soluble residues in warm water, completely transferring the soluble residues into a pipette, adding distilled water to a constant volume, and shaking up to obtain a sample solution; the step is carried out in a microwave digestion tank;
(3) preparing standard solutions of Fe with different set concentrations, sequentially measuring the absorbance of the standard solutions from low concentration to high concentration by using a flame atomic absorption spectrophotometry, and drawing a standard curve;
(4) and (3) measuring the absorbance of the sample solution in the step (2) by using a flame atomic absorption spectrophotometry, and comparing the absorbance with the standard curve drawn in the step (3) to obtain the content of Fe in the marine sediment sample.
The measurement principle of the invention is as follows: the mineral crystal lattices in the marine sediments are destroyed by adopting a hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid full digestion method, so that the element iron to be detected in the sample completely enters the solution, and simultaneously, all iron is oxidized in the digestion process. The digestion liquid is then sprayed into a flame of a flammable air-acetylene flame. At the high temperature of the flame, iron ground state atoms are formed and generate selective absorption to characteristic spectral lines emitted by the iron hollow cathode lamp. Under the selected optimum measurement conditions, the absorbance of iron was measured.
Preferably, in the step (2), the heating digestion temperature is 50-60 ℃, and the heating digestion time is 30-60 min.
Preferably, in the step (2), the volume ratio of the nitric acid to the hydrofluoric acid to the perchloric acid to the hydrochloric acid is (3-5): (2-5): 1: (1-2).
Preferably, in the step (3), the absorbance of the blank is measured by flame atomic absorption spectrophotometry using distilled water as the blank, and the absorbance of the blank is subtracted from the absorbance of the standard solution to draw a standard curve corresponding to the concentration of iron.
Preferably, at least two blank sets are designed for each batch of samples.
Preferably, in the step (1), the pretreatment method comprises the following steps: putting the marine sediment sample into a ball mill for ball milling treatment, and adding grinding beads, wherein the surfaces of the grinding beads are coated with silicon adsorbents.
Preferably, the silicon adsorbent consists of the following components in parts by weight: 10-20 parts of oxalic acid, 40-50 parts of ammonium molybdate and 20-30 parts of hydrogel.
Preferably, in the step (1), the pretreatment method comprises the following steps: before ball milling treatment, the milling beads are soaked in water for 10-30 min.
The main factor influencing the accuracy of the iron atomic absorption method is chemical interference of silicon in a sample, a ball milling method is firstly adopted in the pretreatment process of a marine sediment sample to remove silicon residues in the sample, and a silicon adsorbent coated on the surface of a grinding bead is used for adsorbing silicon in the marine sediment sample in the ball milling process, and the principle is as follows: under the acidic environment provided by oxalic acid, silicon in the sample and ammonium molybdate in the silicon adsorbent are subjected to complexation by the hydrogel which adsorbs water in advance to generate yellow silicon molybdenum yellow, so that the complexation adsorption removal of silicon in the marine sediment sample is completed, the chemical interference is removed, and the accuracy is improved.
Preferably, in the soaking process, ultrasonic oscillation treatment with the frequency of 40-60 KHZ is adopted, and the ultrasonic oscillation treatment is favorable for uniform distribution of ammonium molybdate and oxalic acid in the system.
Preferably, in the step (4), the content of Fe in the sample to be tested is calculated according to the following formula:
in the formula: w is the iron content in the marine sediment sample;
rho is the concentration of iron obtained on the standard curve, and the unit is mg \ L;
v is the volume of the deposit after constant volume, and the unit is mL;
m is the weighed mass of the sample, in g.
Therefore, the invention has the following beneficial effects:
(1) the detection method is simple to operate and high in accuracy, mineral lattices in marine sediments are destroyed by adopting a hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid full digestion method, so that all element iron to be detected in a sample enters a solution, and the accuracy is improved;
(2) in the pretreatment process of the marine sediment sample, the complex adsorption removal of silicon in the sample is completed, the chemical interference is removed, and the accuracy is improved.
Drawings
FIG. 1 is a standard curve of a standard solution of Fe at different set concentrations.
Detailed Description
The technical solution of the present invention is further specifically described below by using specific embodiments and with reference to the accompanying drawings.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
The reagents used in the following examples of the invention were:
hydrochloric acid (HCl): rho is 1.19g/mL, and the product is of high-grade purity;
hydrochloric acid solution, 1+ 1: preparing by using the (3.1);
nitric acid (HNO)3): rho is 1.42g/mL, and the product is high-grade pure;
nitric acid solution (1+ 99): preparing by using the (3.3);
hydrofluoric acid (HF): rho is 1.49 g/mL;
perchloric acid (HClO)4): rho is 1.67g/mL, and the product is super pure;
iron standard stock solution (1000 mg/L).
Example 1
(1) Sample collection
And (3) uniformly mixing the dried marine sediment samples, grinding and pressing the marine sediment samples by using a wood bar, passing through a 2mm nylon sieve, and uniformly mixing. Grinding the sample by using an agate mortar until the sample completely passes through a nylon sieve of 100 meshes, and uniformly mixing for later use;
(2) sample digestion
Accurately weighing 0.2013g of sample, putting the sample into a 50mL polytetrafluoroethylene microwave digestion tank, adding 6mL of nitric acid (3.3) and 4mL of hydrofluoric acid (3.5), and digesting according to a certain temperature-raising program, wherein the heating digestion temperature is 60 ℃, and the heating digestion time is 60 min; after cooling, 2mL perchloric acid (3.6) are added. Placing on an electric heating plate, controlling the temperature at about 160 ℃, driving white smoke and steaming until the content is viscous. Taking down the digestion tank for cooling, adding 4mL of hydrochloric acid solution (3.4), dissolving the soluble residues in warm water, completely transferring to a 25mL pipette, fixing the volume to the marked line by using distilled water, and shaking up; (ii) a
(3) Standard curve
Accurately transferring 0.000 mL, 0.020 mL, 0.040 mL, 0.080 mL and 0.160mL of iron standard stock solution (3.7) into a 50mL volumetric flask, then using distilled water to fix the volume to a marked line, and shaking up, wherein the iron concentrations are 0.00, 0.40, 0.80, 1.60 and 3.20mg \ L respectively. Measuring the absorbance of the standard solution according to the instrument measuring conditions from low concentration to high concentration; subtracting the blank absorbance and the corresponding iron concentration mg \ L to draw a standard curve, as shown in figure 1;
(4) blank test
Using distilled water instead of sample, sampling and preparing the same steps and reagents as those of sample preparation, preparing a blank solution of the whole process, and carrying out the steps
(4) The same conditions were used for the measurements; preparing at least more than 2 blank solutions for each batch of samples;
(5) assay sample
Taking a proper amount of sample solution, and measuring the absorbance of the sample according to the same conditions as the step (4). Checking the iron content from the standard curve (figure 1) in the absorbance;
(6) calculation of results
And calculating the content of iron in the marine sediment dry sample according to the following formula:
in the formula: w is the iron content in the ocean sediment dry sample
Rho is the concentration of iron in mg \ L from the standard curve
V is the final volume of the deposit, in mL
M is the weighed mass of the sample, in g.
Example 2
(1) Sample collection
Putting the dried marine sediment sample into a ball mill for ball milling treatment, and adding grinding beads, wherein the surfaces of the grinding beads are coated with a silicon adsorbent, and the silicon adsorbent consists of the following components: 10g of oxalic acid, 50g of ammonium molybdate and 20g of hydrogel, and before ball milling treatment, firstly soaking grinding beads in water for 10 min; and (3) uniformly mixing the pretreated marine sediments, grinding and pressing the mixture by using a wood bar, and uniformly mixing the mixture through a 2mm nylon sieve. Grinding the sample by using an agate mortar until the sample completely passes through a nylon sieve of 100 meshes, and uniformly mixing for later use;
(2) sample digestion
Accurately weighing 0.2536g of sample, putting the sample into a 50mL polytetrafluoroethylene microwave digestion tank, adding 6mL of nitric acid (3.3) and 4mL of hydrofluoric acid (3.5), and digesting according to a certain temperature-raising program, wherein the heating digestion temperature is 50 ℃, and the heating digestion time is 30 min; after cooling, 2mL perchloric acid (3.6) are added. Placing on an electric heating plate, controlling the temperature at 150 ℃, driving white smoke and steaming until the content is viscous. Taking down the digestion tank for cooling, adding 4mL of hydrochloric acid solution (3.4), dissolving the soluble residues in warm water, completely transferring to a 25mL pipette, fixing the volume to the marked line by using distilled water, and shaking up;
(3) standard curve
Accurately transferring 0.000 mL, 0.020 mL, 0.040 mL, 0.080 mL and 0.160mL of iron standard stock solution (3.7) into a 50mL volumetric flask, then using distilled water to fix the volume to a marked line, and shaking up, wherein the iron concentrations are 0.00, 0.40, 0.80, 1.60 and 3.20mg \ L respectively. Measuring the absorbance of the standard solution according to the instrument measuring conditions from low concentration to high concentration; subtracting the blank absorbance and the corresponding iron concentration mg \ L to draw a standard curve, as shown in figure 1;
(4) blank test
Using distilled water instead of sample, sampling and preparing the same steps and reagents as those of sample preparation, preparing a blank solution of the whole process, and carrying out the steps
(4) The same conditions were used for the measurements; preparing at least more than 2 blank solutions for each batch of samples;
(5) assay sample
Taking a proper amount of sample solution, and measuring the absorbance of the sample according to the same conditions as the step (4). Checking the iron content from the standard curve (figure 1) in the absorbance;
(6) calculation of results
The measured data were used to calculate the iron content of the dry deposit sample according to the following formula:
in the formula: w is the iron content in the ocean sediment dry sample
Rho is the concentration of iron in mg \ L from the standard curve
V is the final volume of the deposit, in mL
M is the weighed mass of the sample, in g.
Example 3
(1) Sample collection and pretreatment
Putting the dried marine sediment sample into a ball mill for ball milling treatment, and adding grinding beads, wherein the surfaces of the grinding beads are coated with a silicon adsorbent, and the silicon adsorbent consists of the following components: 20g of oxalic acid, 50g of ammonium molybdate and 30g of hydrogel, wherein before ball milling treatment, grinding beads are soaked in water for 30min, and ultrasonic oscillation treatment with the frequency of 40KHZ is adopted in the soaking process; and (3) uniformly mixing the pretreated marine sediment sample, grinding and pressing the sample by using a wood bar, and uniformly mixing the sample through a 2mm nylon sieve. Grinding the sample by using an agate mortar until the sample completely passes through a nylon sieve of 100 meshes, and uniformly mixing for later use;
(2) sample digestion
Accurately weighing 0.3003g of sample, putting the sample into a 50mL polytetrafluoroethylene microwave digestion tank, adding 6mL of nitric acid (3.3) and 4mL of hydrofluoric acid (3.5), and digesting according to a certain temperature-raising program, wherein the temperature for heating and digesting is 55 ℃, and the time for heating and digesting is 40 min; after cooling, 2mL perchloric acid (3.6) are added. Placing on an electric heating plate, controlling the temperature at about 180 ℃, driving white smoke and steaming until the content is viscous. Taking down the digestion tank for cooling, adding 4mL of hydrochloric acid solution (3.4), dissolving the soluble residues in warm water, completely transferring to a 25mL pipette, fixing the volume to the marked line by using distilled water, and shaking up; (ii) a
(3) Standard curve
Accurately transferring 0.000 mL, 0.020 mL, 0.040 mL, 0.080 mL and 0.160mL of iron standard stock solution (3.7) into a 50mL volumetric flask, then using distilled water to fix the volume to a marked line, and shaking up, wherein the iron concentrations are 0.00, 0.40, 0.80, 1.60 and 3.20mg \ L respectively. Measuring the absorbance of the standard solution according to the instrument measuring conditions from low concentration to high concentration; subtracting the blank absorbance and the corresponding iron concentration mg \ L to draw a standard curve, as shown in figure 1;
(4) blank test
Using distilled water instead of sample, sampling and preparing the same steps and reagents as those of sample preparation, preparing a blank solution of the whole process, and carrying out the steps
(4) The same conditions were used for the measurements; preparing at least more than 2 blank solutions for each batch of samples;
(5) assay sample
Taking a proper amount of sample solution, and measuring the absorbance of the sample according to the same conditions as the step (4). Checking the iron content from the standard curve (figure 1) in the absorbance;
(6) calculation of results
And calculating the content of iron in the marine sediment dry sample according to the following formula:
in the formula: w is the iron content in the ocean sediment dry sample
Rho is the concentration of iron in mg \ L from the standard curve
V is the final volume of the deposit, in mL
M is the weighed mass of the sample, in g.
The precision and accuracy of the measurement methods of examples 1 to 3 of the present invention were measured, and the results are shown in table 1:
TABLE 1 precision and accuracy
As can be seen from Table 1, the method for determining the content of iron in the marine sediments has high precision and accuracy, wherein the method for determining the content of iron in the marine sediments after the pretreatment of silicon removal completes the complex adsorption removal of silicon in the sample, effectively removes chemical interference and improves the accuracy.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (10)
1. A method for determining the iron content of marine sediments, comprising the steps of:
(1) collecting a marine sediment sample for pretreatment, then grinding and pressing, uniformly mixing through a 2mm nylon sieve, grinding through a 100-mesh nylon sieve, and uniformly mixing to obtain a sample to be detected;
(2) weighing a sample to be detected in a digestion tank, sequentially adding nitric acid and hydrofluoric acid, heating for digestion, cooling, adding perchloric acid, evaporating at 150-180 ℃ until the content is viscous, taking down the digestion tank, cooling, adding a hydrochloric acid solution, dissolving soluble residues in warm water, completely transferring to a pipette, fixing the volume with distilled water, and shaking up to obtain a sample solution;
(3) preparing standard solutions of Fe with different set concentrations, sequentially measuring the absorbance of the standard solutions from low concentration to high concentration by using a flame atomic absorption spectrophotometry, and drawing a standard curve;
(4) and (3) measuring the absorbance of the sample solution in the step (2) by using a flame atomic absorption spectrophotometry, and comparing the absorbance with the standard curve drawn in the step (3) to obtain the content of Fe in the marine sediment sample.
2. The method for determining the iron content in the marine sediments according to claim 1, wherein in the step (2), the heating digestion temperature is 50-60 ℃, and the heating digestion time is 30-60 min.
3. The method for determining the iron content in the marine sediments according to claim 1, wherein in the step (2), the volume ratio of the nitric acid to the hydrofluoric acid to the perchloric acid to the hydrochloric acid is (3-5): (2-5): 1: (1-2).
4. The method for determining the iron content in marine sediments as claimed in claim 1, wherein in the step (3), distilled water is used as a blank test group, the absorbance of the blank test group is measured by flame atomic absorption spectrophotometry, and the absorbance of the blank test group is subtracted from the absorbance of the standard solution, so as to draw a standard curve with the corresponding iron concentration.
5. The method of claim 4, wherein at least two blank test sets are designed for each sample.
6. The method for determining the iron content in the marine sediments as claimed in claim 1, wherein in the step (1), the pretreatment method comprises the following steps: putting the marine sediment sample into a ball mill for ball milling treatment, and adding grinding beads, wherein the surfaces of the grinding beads are coated with silicon adsorbents.
7. The method for determining the iron content in marine sediments as claimed in claim 6, wherein the silicon adsorbent consists of the following components in parts by weight: 10-20 parts of oxalic acid, 40-50 parts of ammonium molybdate and 20-30 parts of hydrogel.
8. The method for determining the iron content in the marine sediments as claimed in claim 7, wherein in the step (1), the pretreatment method comprises the following steps: before ball milling treatment, the milling beads are soaked in water for 10-30 min.
9. The method for determining the iron content in the marine sediments as claimed in claim 8, wherein the soaking process is carried out by ultrasonic oscillation with the frequency of 40-60 KHZ.
10. The method for determining the iron content in the marine sediments as claimed in any of claims 1 to 9, wherein in the step (4), the content of Fe in the sample to be tested is calculated according to the following formula:
in the formula: w is the iron content in the marine sediment sample;
rho is the concentration of iron obtained on the standard curve, and the unit is mg \ L;
v is the volume of the deposit after constant volume, and the unit is mL;
m is the weighed mass of the sample, in g.
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| CN114544531A (en) * | 2022-02-28 | 2022-05-27 | 滨州市海洋发展研究院 | Method for measuring content of organic carbon in marine sediments |
| CN114544531B (en) * | 2022-02-28 | 2024-10-22 | 滨州市海洋发展研究院 | Method for measuring organic carbon content in marine sediment |
| CN117191769A (en) * | 2023-09-14 | 2023-12-08 | 华南理工大学 | Method for detecting total iron content in red mud |
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