Analytical characteristics of the method of atomic emission spectrometry with inductively coupled plasma. The main units of the AES-ICP instruments. Development of a method for the analysis of solids. The choice of solvent for the catalyst. Determination of concentrations in solutions.

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Introduction

1. Literary review

1.2 Analytical characteristics of the method of atomic emission spectrometry with inductively coupled plasma (AES-ICP)

1.4 Main units of AES-ICP instruments

1.4.1 Sprayers

1.4.2 Spray chambers

1.4.3 Plasma and torches

1.4.4 Wavelength separation devices

1.4.5 Detectors

1.4.6 Dynamic range in the ICP-AES method

1.5 Interference in the ICP-AES method

1.5.1 Spectral interference

1.5.3 Lower detection limit. Accuracy and reproducibility

1.5.4 Dynamic range of concentrations in the ICP-AES method

2. Stages of developing a methodology for the analysis of solids by the ICP-AES method

3. Experimental part

3.2 Finding Analytical Lines

3.6 Checking the correctness of determining the concentrations of Co, Fe, Ni, Al and Mg according to the developed method

3.7 Checking the reproducibility of determining the concentrations of Co, Fe, Ni, Al and Mg according to the developed method

The main results and conclusions of the thesis

Bibliography

Introduction

The tasks of the analytical laboratory of the Institute of Catalysis include conducting analytical control by various methods for all laboratories of the Institute engaged in the creation and study of new catalysts. For these purposes, several groups have been created in the laboratory, into which the methods of analysis are distributed. The group in which this work was done is called the chemical spectral analysis group. The task of developing a technique for analyzing a Fe-Co-Ni catalyst deposited on Al 2 O 3 and MgO for the content of active components (Fe, Co and Ni) and support components (Al, Mg) arose in the group of synthesis of surface compounds, where the work is being carried out on the use of catalysts in the production of multiwalled carbon nanotubes (MCNT).

Relevance of the topic.

Fe-Co-Ni-O-catalysts are multiphase solids with high particle dispersion (6 - 23 nm). They are used in the synthesis of multilayer carbon nanotubes (MCNTs) with unique physicochemical properties (high electrical and thermal conductivity, mechanical strength, chemical inertness, etc.). It is known that carbon nanotubes are becoming a key material for developing nanotechnology, in particular, for the production of composite materials for a wide range of applications. The synthesis of nanotubes is carried out by the methods of gas-phase catalytic carbon deposition and significantly depends on the chemical composition and structure of the catalysts used. The quality of the resulting nanotubes - their diameter, length, and the number of layers - largely depends on these factors. Hence, the role of elemental analysis of catalyst substances is clear. The development of a method for analyzing catalysts for active components is an important link in the creation of high-quality catalysts.

Purpose of work.

Achieve the smallest error in determining high concentrations of elements (1-50 wt.d.,%) by inductively coupled plasma atomic emission spectrometry (ICP-AES).

Scientific task

Development of a unified technique for analyzing Fe-Co-Ni-O-catalysts for elements Fe, Co, Ni, Al, Mg by the ICP-AES method with methods for improving the error in determining concentrations of 1-50 wt.d,%.

Stages of solving the task:

1. Study of the problems of analysis of Fe-Co-Ni-O-catalysts for the main elements Fe, Co, Ni, Al and Mg with a concentration from 1 to 50 wt.d,%

2. Study of the theoretical foundations of the AES-ICP method.

3. Development of a methodology for performing analysis by the ICP AES method.

4. Performing analysis for a series of samples of Fe-Co-Ni-O-catalysts

Scientific novelty.

1. A technique has been developed for the detection of basic elements in Fe-Co-Ni-O-catalysts supported on Al 2 O 3 and MgO. The technique is unified: it allows quickly, from one sample, to detect the following basic elements: Co, Ni, Fe, Al and Mg with a concentration of 1 to 50%.

2. The technique makes it possible to achieve the magnitude of the error before its permissible values ​​in the methods of atomic absorption spectrometry: the accuracy of the analysis should ensure that the sum of the sample elements is obtained within 99.5-100.5%.

The practical significance of the thesis.

To solve practical problems of detecting basic elements in Fe-Co-Ni-O-catalysts, the methodological part of the modern multi-element highly sensitive method of analysis of ICP-AES has been developed. Experiments have shown that the developed technique significantly reduces the error in determining the main elements.

Approbation of work.

The results of the study of the composition of impurity elements and the method for their detection were transferred to the group for the synthesis of surface compounds of the Institute of Catalysis of the SB RAS and were used in scientific reports.

All theoretical and experimental studies were carried out by the author personally. An analysis of the literature data on the topic of the work was carried out, the planning of the experiment was carried out, namely: the selection of a solvent for the objects of analysis, calculations of the dilution coefficients, the choice of analytical lines. Measurement of analytical signals on the ORTIMA 4300DV device was carried out and concentration calculations were made. The author took an active part in approbation of the developed methodology on other tests, in discussing the results obtained, in preparing slides for the report together with the scientific supervisor.

spectrometry solution catalyst

1 ... Literature review

1.1 Known information about the objects of analysis

Fe-Co-Ni-O-catalysts are multiphase solids with high particle dispersion (6-23 nm). They are used in the synthesis of multilayer carbon nanotubes (MCNTs) with unique physicochemical properties (high electrical and thermal conductivity, mechanical strength, chemical inertness, etc.). Multicomponent catalysts for the synthesis of MWCNTs consist of round or cubic particles with a distinct crystal lattice. The crystallite size changes significantly with the use of various carriers, and also partially changes with varying the content of the active component - it decreases with a decrease in the proportion of active metals (Fe, Ni, Co).

1.2 Analytical characteristics of the method of atomic emission spectrometry with inductively coupled plasma

Atomic emission spectroscopy with inductively coupled plasma (ICP-AES) is a method of elemental analysis based on the optical emission spectra of atoms of the analyzed sample in the excitation source - in plasma.

ICP analysis is primarily a solution analysis. The analytical characteristics of the method are considered in this aspect of its application. Dissolving solid samples before analysis removes many solid state interferences. The ICP-AES method achieves unusually low detection limits. Detection range 1-100 μg / L. All elements have different detection limits: some elements have extremely low detection limits; a wide range of elements have “good” detection limits. Modern equipment has provided good reproducibility comparable to flame methods (especially atomic absorption analysis). The reproducibility is slightly worse than for some other analytical methods, but it is acceptable for most analytical tasks. The method can give very accurate results, especially when detecting low concentrations (up to 1%). An important advantage in the ICP-AES method is the small volume of the test solution required for analysis.

Problems arise in the determination of some elements at their very high contents (30% and more), if very accurate results are to be obtained.

Other disadvantages of this method should be noted: difficulties in determining elements whose atoms have very high excitation energies (P, Pb, Pt, Re, S, Se, Sn, Ta, Te, Cl, Br, J), or high ionization energies (alkali metals), as well as weak analytical lines (Pb, Pt, Os, Nb, Ge, P, S, Se, Sn, Ta, Th, U), leading to low sensitivity; it is not possible to determine H, N, O and C due to their presence in the environment or solvent; radioactive elements cannot be identified due to the impossibility of ensuring the protection of the operator and due to the difficulties associated with standard substances; there is no way to determine different valence forms of an element from one solution; high carrier gas consumption is required; There is some difficulty in developing a method for dissolving a sample, which allows simultaneously and stably keeping all elements of a solid sample in solution. Despite all the shortcomings of the method, it is widely used to detect up to 72 elements of the periodic system in the concentration range from 0.001 to 100%. One of the fundamental advantages of ICP is the ability to simultaneously determine 20 - 40 elements in the same time during which a single-element analysis is performed. To obtain accurate results with low errors, there are a number of techniques: large dilution of the test solutions, measurement of the signal along several lines, non-use of analytical lines with spectral interference, sample preparation with several weighed portions.

So, the analytical characteristics of the AES-ICP method allow using this method to achieve the goal set in the thesis - to obtain results of high concentrations (1-50%) with the smallest errors for this method. But for this it is necessary to use all possible methods of increasing the accuracy.

1.3 Theoretical foundations of the ICP-AES method

Atomic emission spectroscopy began to develop in the early twentieth century. By the middle of the century, arc and spark spectrometry had become the best tool for analysts to study trace concentrations of a wide range of elements. At the same time, flame photometry was already widely used to determine easily excited elements. A new impetus for the development of the method was a series of publications on the use of inductively coupled plasma as a high-temperature source of excitation of sample atoms. Plasma is generated by passing an argon flow through a coil-inductor, through which a high-frequency current flows. Argon is heated to a very high temperature, an electric discharge-spark arises in it, which strips electrons from argon atoms. The spark starts a chain reaction of electrons knocking out of argon atoms, i.e. starts the process of argon ionization and plasma formation. This plasma is called inductively coupled. Plasma is generated in a specially designed burner. The sample solution enters the argon flow through a nebulizer. In plasma, the sample solution is exposed to high temperatures sufficient to dissociate the substance into atoms and to excite atoms as a result of their collisions. By absorbing the energy of the plasma, the atoms are excited, their electrons jump to more distant energy orbits. Escaping into a colder plasma region, the excited atoms return to their normal state with the emission of polychromatic light (emission), which contains the unique characteristic radiation of each element of the injected solution with a strictly defined wavelength. These wavelengths are called analytical lines. There may be several of them, in different parts of the spectrum. They have been known for a long time, well measured, and are contained in spectral line handbooks. As a rule, they are very intense. Emission polychromatic radiation generated in the plasma with the solution is captured by the focusing optics of the spectrometer, and then it is divided into separate parts of the spectrum by a dispersing device. In early spectrometers, diffraction gratings were used; in modern instruments, these are echelle gratings. They are able to distinguish very narrow spectral regions, almost equal to the length of the analytical line, which turned the method of emission spectroscopy into a selective multielement method. Knowing the lengths of the analytical lines of individual elements from the reference books, you can configure the device to output a signal of a certain wavelength after separating the polychromatic light. The light signal obtained in this way from a narrow part of the spectrum then enters the photomultiplier tube, after converting it into an electrical signal and amplification, it is displayed on the device screen in the form of a digital value of an electrical signal and in the form of a light wave curve in a small part of the spectrum, similar to the Gaussian function curve.

The ICP-AES method is shown schematically in Scheme 1.

Scheme 1: Schematic representation of the ICP-AES method

1.4 Main components of ICP-AES instruments

Instruments of the AES-ICP method are complex modern devices that require special theoretical training to work on them. Therefore, below are descriptions of the main components of these devices.

1.4.1 Sprayers

The first step in analyzing any sample using the ICP-AES method is introducing it into the burner. The sample can be solid, liquid and gaseous. Special tools are required for solid and liquid samples. We will further consider the introduction of a liquid sample. Liquids are usually sprayed. Nebulizers are devices for introducing liquid samples into the spectrometer in the form of a fine aerosol. The nebulizers used with ICP for dispersing liquids into aerosols are pneumatic (most convenient, but not the most effective) and ultrasonic.

1.4.2 Spray chambers

Once the aerosol is generated by the nebulizer, it should be transported to the burner so that it can be injected (injected) into the plasma. To obtain more stable injection conditions, a spray chamber is placed between the atomizer and the burner. The main function of the spray chamber is to remove large droplets from the aerosol and smooth out the pulsation that occurs during spraying.

1.4.3 Plasma and torches

The plasma, into which the analyzed solution is injected, is a gas in which the atoms are in an ionized state. It occurs in burners placed in the inductor of a high-frequency generator. When high-frequency currents flow through the inductor coil, an alternating (pulsating) magnetic field arises inside the coil, which acts on the ionized argon passing through the burner, heating it. This interaction of ionized argon and a pulsating magnetic field is called inductive coupling, and the heated plasma is called an ICP "flame" with a temperature of 6000-10000 K.

Figure 2. Burner diagram

Plasma torch zones: 1 - analytical; 2 - primary radiation; 3 - discharge (skin layer); 4 -central channel (preheating zone). Plasmatron details: 5 - inductor; 6 - protective tube preventing breakdown to the inductor (installed only on short burners); 7 - outer tube; 8 - intermediate tube; 9 - central tube. Gas streams: 10 - external; 11 - intermediate; 12 - transporting.

1.4.4 Wavelength separation devices

When the analyzed solution enters the plasma region, called the normal analytical zone, the molecules of the analyte disintegrate into atoms, their excitation and the subsequent emission of polychromatic light by the atoms of the analyte. This light emission carries in itself the qualitative and quantitative characteristics of the atoms of the elements, therefore it is selected for spectrometric measurement. First, it is collected by the focusing optics, then it is fed to the entrance slit of the dispersing device (or spectrometer). The next step of the ICP-AES is to distinguish the emissions of one element from the emissions of other elements. It can be implemented in a variety of ways. Most often it is the physical dispersion of different wavelengths by diffraction gratings. Prisms, filters and interferometers can be used for these purposes. In modern devices, echelle gratings are most often used to separate polychromatic light by wavelength.

1.4.5 Detectors

After the spectrometer has selected the analytical emission line, a detector is used to measure its intensity. Until now, the most widely used detector in ICP AES is the photomultiplier tube (PMT), which is a vacuum tube that contains a light-sensitive material that ejects electrons when photons of light strike it. These knocked-out electrons are accelerated towards the dynode, knocking out two to five secondary electrons for each electron striking its surface. The amount of electricity generated is proportional to the amount of light striking. Quantitative analysis in the ICP-AES method is based on this law of physics.

1.5 Interference in the ICP-AES method

For the analytical chemist, interference is everything that leads to a difference between the emission signal from the analyte (element) in the sample from the signal of the analyte of the same concentration in the calibration solution. The presence of interference can negate the accuracy of the determination, so modern instruments are designed to minimize this interference. Interference can be of spectral and matrix origin. There are serious influences, but in almost all cases they can be easily eliminated. Influences in ICP AES need to be detected on purpose. The reasons for the various interference are complex.

1.5.1 Spectral interference

Spectral interference- overlays (including continuum and background radiation). These interferences are best understood. They are often eliminated simply by increasing the resolution of the spectrometer or by changing the spectral line. The signal recorded by the measuring electronics is the total radiation intensity of the analyte and the interfering element. Below are examples of spectral overlays.

Figure 3: Types of spectral overlays found in ICP spectrometry.

a - direct overlap of the analytical (1) and interfering (2) lines. The wavelengths are too close to be resolved. You need to make a strong dilution or find another line without such an overlay;

b - overlapping of wings or partial overlap of analytical and interfering lines. You can reduce the noise by increasing the resolution;

в - superposition of a continuum or background. Three levels of overlap are given, corresponding to increasing concentrations of the interfering element. Here you need to look for a line in a different region of the spectrum.

There are atlases of excitation spectra in ICP. They contain almost complete information on the most suitable lines in ICP and experimental data on many possible interference. Difficulties arise when an element has few analytical lines. Particular attention should be paid to samples with a high aluminum content. in the region of 190-220 nm, it emits a recombination continuum (Figure 3c).

1.5.2 Matrix Interference and Scattered Light

Matrix interferences and stray light are often the result of high concentrations of certain elements or compounds in the sample matrix. The effect of scattered light is associated with the design of the spectrometer, and matrix noises are associated with the method of introducing the sample into the plasma and the operation of the excitation source, i.e. plasma. In modern designs of spectrometers, the level of scattered light is significantly reduced.

Matrix interferences can always be detected. So, when the acid concentration changes, the spray efficiency changes, and, as a result, the sensitivity. Below are examples of such an effect on the sensitivity of various mineral acids that are used in sample preparation.

Figure 4. Decrease in signal intensity (in% of the original signal) when adding different acids.

In order for this information to be applied in normal analytical practice, the concentrations of added acids are expressed in volume percent of commonly used concentrated acids, namely, 37% HCl, 60% HClO 4, 85% H 3 PO 4, 70% HNO 3, 96 % H 2 SO 4 (mass percent). It can be seen from the above figures that all acids suppress the signal of aluminum (along the 308.2nm line) and manganese (along the 257.61nm line), and the effect of НCl and HClO 4 is much weaker than that of H 2 SO 4. It can also be seen from the figures that all acids and all elements have their own dependences on the effect on sensitivity, therefore, when developing methods with varying concentrations of acids, it is necessary to carry out such a study and take the results into account. An effective way to eliminate such acid interference is to maintain adequate levels in the standard. Increasing the temperature of the spray liquid can reduce the matrix effect of acids.

Another type of matrix noise is associated with plasma, i.e. with the process of excitement. Thus, it is possible to detect the influence of the varying concentration of the matrix element (K, Na, Mg, Ca) on the excitation process, leading to a decrease in the output signal. With an increase in the concentration of these elements in solution, the analytical signal decreases, and the background increases. It can be assumed that the list of such elements can be replenished with new elements, i.e. it is necessary to check the presence of such a matrix effect when developing a method. It is also necessary to bear in mind the ionization interference from the presence of a large excess of easily ionizable elements (alkaline). A universal way to avoid matrix interferences is to dilute the test solutions to a fixed (no longer changing with further dilution) background level. Here, the problem can only be for the determination of low concentrations of elements, when dilution will lead to a drift beyond the lower detection limit.

1.5.3 Lower detection limit. Accuracy and reproducibility

The lower detection limit (LOD) is an important metric when evaluating an instrument and method. This is the lowest concentration that can be reliably identified as above zero radiation and can be easily quantified. The zero level corresponds to the value 3?, Where? is the standard deviation of the mean value of the background drift (noise), which is the sum of the emission (noise) of the plasma, distilled water, photomultipliers and electronics. To obtain the lower detection limit (μg / cm 3), the signal corresponding to the β value is multiplied by 3 and, through the calibration curve for the element, is converted into the concentration of this element. Μg / cm 3 of the element, corresponding to the signal 3?, Is taken as the detection limit of the element. In modern devices with computer programs, the concentration corresponding to the signal 3? are calculated automatically. In the PERKINELMER OPTIMA 4300DV it is shown as SD value in µg / cm 3 when sprayed with a background BLANK solution (usually distilled water). Concentration measurements near the detection limit can only be semi-quantitative. For quantitative measurements with an error of ± 10% relative n.o. increase by 5 times, with an error of ± 2% relative to n.o. need to be increased by a factor of 100. In practice, this means that if you took a sample and / or dilution and determined a concentration in them close to the SD value, then you need to redo the analysis by reducing the dilution by 5-100 times or increasing the sample by 5-100 times. Difficulties can arise if there is an insufficient amount of the analyzed solution or dry matter. In such cases, a compromise on accuracy must be found with the customer.

The ICP-AES method is a method with good reproducibility. Reproducibility can be calculated as simply repeating measurements of the same solution over a short period of time, or repeated analyzes spanning a long period of time, including sampling and sample dissolution. When approaching n.p. reproducibility is severely impaired. Reproducibility is influenced by changes in spray conditions (nozzle clogging, temperature, etc.) they greatly change the emission output. Slight pressure fluctuations in the spray chamber also change the emission, therefore, care must be taken to ensure that no gas from the test solution and from the drain tank (hydrogen sulfide, nitrogen oxides, SiF 4, etc.) enters the chamber. To improve reproducibility, an internal standard can be used by fitting the internal standard element to the analyzed element. But this method is not very suitable for routine analysis due to its laboriousness.

The correctness of a method is partly determined by its reproducibility. But to a greater extent by its systematic influences (the influence of matrices and other interferences). The general level of interference in the ICP-AES method is different in each specific case, but in most cases, systematic interference can be eliminated, and then the correctness (accuracy) of the analysis is limited only by reproducibility. So, if it is possible to achieve the elimination of matrix noise by dilution, then it is possible to determine the analyte in different (according to the matrix) samples using the same calibration curves, making several parallel measurements of the signal to assess reproducibility. Its modern devices also automatically calculate the RSD value, which accompanies each result obtained on the device. It is calculated using the same formulas as SD.

2. Stages of development of a methodology for the analysis of solids by the ICP-AES method.

In this chapter, we provide a schematic diagram of the development of a methodology for performing elemental analysis in solids by the ICP-AES method. We have identified 17 main stages in the development of the methodology.

Figure 5. Diagram of the main stages of method development.

Explanations for some stages of the diagram.

Stage 1. The sample should be thoroughly (100%) crushed in an agate mortar, screening out large particles and grinding them again.

Stage 4. The lower limit of detection (n.o.) is important to know for the tasks of determining concentrations below 1%, in order to correctly calculate the sample and decide on the need for concentration.

Stage 5. The calculation of the sample is carried out according to the formula

Weighed portion (g) = μg / cm 3 * V / 10 4 * C, where

μg / cm 3 is the concentration range of working standard solutions. The formula uses the concentration of the first and last standard solution, which will be used to build a calibration graph;

V-volume of the volumetric flask, where the sample solution is transferred, ml;

C is the estimated concentration of the element, in mass fraction,%. If such a concentration is unknown, then the maximum possible weight for the ICP-AES method should be taken. This is 1g per 100ml of stock solution. Large weights can cause matrix effects, but not always, so it is necessary to check and, if necessary, the weighed amount can be increased. This can be done when very low concentrations are required (below the lower detection limit). This technique is called analyte concentration.

Step 6. The method of transferring a solid sample into solution can be any method known in analytical practice. With the existence of many methods, it is necessary to choose the fastest, the cleanest (in the sense of adding less additional chemical elements during sample preparation) and the most accessible. This is usually an acidic dissolution. For the tasks of analysis by the ICP-AES method, acid dissolution is the most preferable for us. Which acid to take depends on the properties of the sample elements. Here you need to work with the literature and select with its help such a solvent that will ensure the dissolution process without loss of the determined elements in the form of volatile compounds or in the form of secondary precipitates. There are many tutorials for sample preparation purposes.

The solvent is selected according to the properties of the elements of the substance, which is analyzed, even if some elements from the composition of the substance are not determined. In order to find a solvent for the catalyst, you need to find out from the customer what was brought to you for analysis. As a rule, the customer knows this. You can also ask about the solubility of this substance. And only after that it is necessary to start searching for a solvent.

Step 13. Dilution is an important procedure for reducing spectral and matrix interference in the ICP-AES method. A general rule of thumb here is to advise you to do a few dilutions and compare the results of photometry. If they turn out to be the same (in terms of the original solution) for at least the last two dilutions, this indicates the absence of any interference in these two solutions. If there are no such identical results, it is necessary to continue decreasing the concentration in the photometric solution, i.e. continue to increase the dilution rate. If the possibilities of dilution are exhausted (you go beyond the detection limit of an element), you need to look for another, more sensitive, spectrum line or carry out measurements on the device by the addition method. In most cases, in the ICP-AES method, dilution avoids any interference.

Stage 14. Dissolution of the sediment is carried out under more stringent conditions than those selected in paragraph 6. Here you can use both microwave heating under pressure and fusion.

Stage 12, 15, 16. Photometry of the test solutions is carried out according to preselected analytical lines, which should be as selective as possible, without spectral interference. As a rule, there are several analytical lines, they are located in different parts of the visible part of the spectrum, which makes it possible to select a selective line. When replacing the line, a problem arises in its sensitivity, it may not be high and will be unsuitable for detecting low concentrations of elements. It is possible to increase the concentration of an element and eliminate spectral interference using various concentration methods (increasing the sample, evaporation, extraction, ion exchange, distillation of volatile matrix compounds, etc.)

3. Experimental part

In Chapter 2, we outlined the main stages of developing an analysis methodology using the ICP-AES method. In this chapter, we used this guideline to develop a specific method for performing basic elemental analysis on a Fe-Co-Ni catalyst supported on Al 2 O 3. accuracy of results such techniques include:

1) an increase in the number of parallel samples;

2) mandatory dilution of the initial test solutions with the addition of a sufficient amount of acid to suppress the hydrolysis of salts;

3) preparation of standard solutions in one flask for all elements with the same amount of acid as in the test solutions;

4) carry out the determination of concentrations along several selective lines;

Table 1. The sought concentrations of the main elements of the sample and the admissibility of their determinations

We adopted the limits of permissible errors (achieved accuracy) according to the recommendations of the All-Union Scientific Research Institute of Mineral Raw Materials (VIMS). The instructions of the Scientific Council for Analytical Chemistry for spectral methods indicate that the accuracy of the analysis should ensure that the sum of the sample elements is obtained in the range of 99.5-100.5 mass fraction,%. For the rest of the concentrations, we calculated these error tolerances based on the following logic - the lower the absolute%, the greater the relative error can be.

The analytical task was as follows: select a solvent for the catalyst, find analytical lines for Fe, Co, Ni, Al and Mg, select the conditions for photometry on the OPTIMA 4300DV instrument, obtain data on analyte concentrations, check the correctness of determination of these concentrations, evaluate the reproducibility of the results by standard deviation , calculate and write the text of the methodology according to the rules of GOST

3.1 Choice of catalyst solvent

Having studied the literature on dissolution methods for systems like Fe-Co-Ni-O-catalyst supported on Al 2 O 3 and MgO, we chose the necessary solvent - H 2 SO 4 (1: 1) and heating until the sample was completely dissolved.

3.2 Finding Analytical Lines

For the determined elements Fe, Co, Ni, Al and Mg, we found analytical lines. Each of the listed elements has at least one analytical line in the visible part of the spectrum, more often there are several of them. These lines are bright, conspicuous, free of emissions from other elements on this list, and their emission can be measured well. The search for such lines in the OPTIMA device is carried out according to the instructions for the device. The program of the device contains 5-7 of the most selective and sensitive lines for 70 elements of the periodic table, which greatly facilitates the search for the desired line. The same program contains information about the close environment of the analytical line from the list of sample elements. It also helps to quickly figure out which element, with what concentration, will interfere with the work of the chosen analytical line. The interfering effect of accompanying elements is most often manifested when determining low concentrations against the background of high accompanying ones. In our sample, all concentrations are high and there is no particular danger of a concomitant effect if a selective line is selected. You can also verify this with the help of the software of the device, which draws spectra either in the form of a separate bell, or with their overlays. Acting according to the described principle, we have chosen three analytical lines for the elements to be determined from those laid down in the program. (Table 2)

Table 2. Analytical lines of the determined elements (included in the program).

3.3 Selecting the optimal photometry conditions on the OPTIMA 4300 DV device

The conditions for performing measurements on the OPTIMA 4300DV spectrometer can be selected for each sample, but if a unified technique is being made, then it is necessary to choose the averaged parameters that provide good results for all elements. We have chosen such conditions.

3.4 Preparation of standard solutions

To perform measurements of concentrations in the test solutions, it is necessary to calibrate the device using standard solutions. Standard solutions are prepared either from commercially available state reference materials of the composition (GSO composition), or from substances suitable for standards.

3.5 Calibration of the spectrometer and determination of concentrations in the test solutions

The preparation of the spectrometer and the operation of spraying solutions are carried out in accordance with the instructions for use of the device. First, a joint working standard solution is sprayed with a mass concentration of the elements Fe, Co, Ni, Mg and Al 10 μg / cm 3. The computer calculates the calibration dependences of the radiation intensity of each element (Fe, Co, Ni, Mg and Al) in arbitrary units on the mass concentration of the element (Fe, Co, Ni, Mg and Al). It turns out that there are five calibration curves for five elements.

Spray the test solution. The test solutions were sample No. 1 of the composition (Fe-Co-O / Al 2 O 3) and sample No. 2 of the composition Fe-Ni-Co-O / Al 2 O 3 + MgO. The computer calculates the mass concentration of elements (Fe, Co, Ni, Mg and Al) in μg / cm 3. The results are shown in Table 3.

Table 3. The results of determining the concentration of Fe, Co and Al by three lines in the samples. # 1.

The data from the table were used to calculate the analysis results in mass fractions,%. Elements were determined along three analytical lines. The results are shown in the table.

Table 4. Results in% for sample No. 1 (Fe-Co-O / Al 2 O 3)

Table 5. Results in% for sample No. 2 (Ni-Co-O / Al 2 O 3 + MgO)

3.6 Checking the correctness of the determination of the concentrations of Fe, Co, Ni, Al and Mg

To prove the correctness of the results obtained, we can use three ways:

1) Check the correctness using another method of analysis;

2) Check the correctness using a standard sample of the same catalyst composition;

3) By the "entered-found" method

We used the "entered - found" method. This is very convenient because it is a replacement for expensive standards that are not always at hand. The bottom line is that we introduce an additive from a standard solution of an element into the test solution, then we measure the concentration of the element on the device in two solutions - without an additive and with an additive. Subtract the result without the addition from the result with the addition. The difference should be the concentration of the additive. Table 6 shows the results of such a test with sample # 1.

Table 6. Results of checking the results for samples No. 1 and No. 2 by the "entered-found" method.

Because the technique must be provided with errors in determining the desired concentrations of each element, we calculated this error according to the calculation algorithm given in GOST 8.207. All the results of such calculations are shown in Table 7.

Table 7. Summation of the components of the error: correctness and reproducibility for samples No. 1 and No. 2.

The results in the table are obtained using the following formulas:

where is the standard deviation of a single result;

x i is a single analysis result;

n is the number of parallel definitions (we have 6).

where x cf is the average result of the analysis;

Standard deviation of the mean.

where is the correctness of the analysis result, or the total systematic error, μg / cm 3 or wt.d.,%

where r is the ratio of the systematic component to the random one. A criterion for comparing random and systematic errors.

If r? 0.8, then the error = ± 2 * with a probability of 95%, i.e. the error is due only to the random component.

If r? 8, then =, i.e. the error is due to a random component

If r is from 0.8 to 8 then =, i.e. the error is a component of two components.

So, we have developed a method for determining high concentrations of elements (1-50%) in the Fe-Co-Ni-O / Al 2 O 3 + MgO catalyst by the ICP-AES method with acceptable errors. The text of the methodology is compiled in accordance with GOST R8.563-96.

4. Settlement and economic part

4.1 Calculation of the cost of determining Fe, Co, Al, Ni, Mg by the ICP AES method

The cost of analysis is the most important indicator of the economic efficiency of its production. It reflects all aspects of economic activity and accumulates the results of the use of all production resources.

Calculation of the cost of fixed assets for the analysis and establishment of the calibration dependence

Calibration dependence for determination of iron, cobalt, aluminum, nickel, magnesium in ICP-AES.

Calculation of the cost of measuring instruments and laboratory equipment

Table 9. Equipment for analysis

Table 10. Equipment for establishing the calibration dependence

Laboratory cost calculation

The laboratory involved in the analysis is 35 m 2.

The calculation of the cost of the laboratory is determined by the formula:

C = C 1 m 2 * S, (5)

where C is the cost of the premises, rubles;

From 1 m 2 - the cost of 1 m 2 of the area of ​​the premises, rubles;

S - occupied area, m 2.

For our calculation, the cost of the laboratory is:

40,000 rubles / m2 * 24m 2 = 96,000 rubles

Depreciation of fixed assets

Depreciation is a gradual transfer of the cost of fixed assets to the cost of finished goods.

The calculation of depreciation included in the cost of the analysis was carried out using the following formulas:

H a = (1 / n) * 100%, (6)

where H and - depreciation rate,%;

n - standard service life, years.

A year = F n * H a / 100%, (7)

where F n - the initial cost of fixed assets, rubles;

H a - depreciation rate,%;

And year - annual depreciation deductions, rubles.

A month = A year / m, (8)

where A year is the annual depreciation, rubles;

m is the number of months in a year;

A month - depreciation per month, rubles.

A hour = A month / t month, (9)

where A month is depreciation per month, rubles;

And an hour is depreciation per hour.

And for analysis = A hour * t analysis, (10)

where A hour is depreciation per hour;

And for analysis - depreciation included in the cost of analysis.

Table 11. Calculation of depreciation of fixed assets for analysis

Table 12. Calculation of depreciation of fixed assets to establish the calibration dependence

Calculating the cost of reagents

Table 13. Calculation of costs for reagents for analysis

Table 14. Calculation of costs for reagents to establish a calibration dependence

Calculation of time spent on analysis

In order to determine the content of iron, cobalt, aluminum, nickel, magnesium by atomic emission spectrometry with inductively coupled plasma, it is necessary to perform the following operations:

Experiment - 1 hour;

Processing and delivery of results - 0.5 hours.

To carry out the analysis, you need to spend 2 hours. Equipment operation time - 1 hour.

In order to calibrate the analyzer, you must perform the following operations:

Preparation for the experiment - 0.5 hours;

Preparation of calibration solutions - 0.5 hour;

Establishment of the calibration dependence - 0.5 hour;

Processing of measurement results - 0.5 hour.

To establish the calibration dependence, it is necessary to spend 2 hours. The equipment operating time is 1 hour.

Calculation of costs for laboratory glassware for analysis

The calculation of the costs for laboratory glassware included in the cost of analysis was made according to the following formulas:

where C is the cost of laboratory glassware;

m is the number of months in a year;

3 month - costs for laboratory glassware per month, rubles.

where 3 month - the cost of laboratory glassware per month, rubles;

t month - the number of working hours in a month;

3 hour - the cost of laboratory glassware per hour, rubles.

where Z hour is the cost of laboratory glassware per hour, rubles;

t analysis - analysis time, hours;

Z for analysis - the cost of laboratory glassware per analysis.

Table 15. Costs for laboratory glassware for analysis

For one analysis, it is required to spend 0.5 rubles on laboratory glassware.

Table 16. Costs for laboratory glassware to establish the calibration dependence

To establish a calibration dependence on laboratory glassware, you need to spend 0.5 rubles.

Energy cost calculation

The calculation of energy costs is based on the power consumption of the equipment involved, the operating time of the equipment and the price per kWh of energy.

Table 17. Calculation of energy costs for analysis

Table 18. Calculation of energy costs to establish the calibration dependence

Calculation of the salary of a laboratory assistant

Table 19. Calculation of the salary of a laboratory assistant for the analysis

Table 20. Calculation of the salary of a laboratory assistant for establishing the calibration dependence

Social contributions

Social contributions is 30%, of which:

We get:

Amount, total * Tariff rate

Total: 200 * 0.3 = 60 rubles. - social contributions for analysis

Total: 200 * 0.3 = 60 rubles. - deductions for social needs to establish the calibration dependence

Overhead calculation

In the project, overhead costs are taken at the rate of 32% of the salary of a laboratory assistant:

Amount, total * 0.32

200 * 0.32 = 64 rubles. - overhead for analysis

200 * 0.32 = 64 rubles. - overhead costs for establishing the calibration dependence

Calculation of other costs

Other expenses assumed at the rate of 7% of the amount of the above expenses:

Crockery + Reagents + Energy + Salary + Deductions for social needs + Amorth. fixed assets + Overhead = Expenses

0.5 + 4.14 + 28.52 + 200 + 60 + 51.4 + 64 = 408.56 - costs spent for the analysis

0.5 + 4.14 + 28.05 + 200 + 60 + 47.2 + 64 = 403.89 - costs spent to establish the calibration dependence

Costs * 0.07 = Other costs.

408.56 * 0.07 = 28.60 rubles. - other costs attributable to one analysis

403.89 * 0.07 = 28.27 rubles. - other costs incurred to establish the calibration dependence

Table 21. Percentage structure of costs for the analysis, taking into account the establishment of the calibration dependence

Scheme 2. Cost structure.

Conclusion: The cost of the analysis, taking into account the costs of the calibration dependence, was 861.72 rubles.

The largest share in the structure of costs is occupied by the costs of the salary of a laboratory assistant (46.41%), depreciation of fixed assets (10.55), the share of other costs is insignificant.

Main conclusions

1. The theoretical questions of the method of atomic emission spectrometry with inductively coupled plasma have been studied.

2. The structure of the OPTIMA 4300DV spectrometer has been studied.

3. A unified method has been developed for the analysis of Fe-Co-Ni-O-catalyst deposited on Al 2 O 3 and MgO, for elements Fe, Co, Ni, Al and Mg with concentrations from 1 to 50% by ICP AES using a spectrometer OPTIMA 4300DV.

4. The methods of performing the analysis were used, which make it possible to carry out the determination of high concentrations of elements by a highly sensitive method, namely:

- an increase in the number of parallel samples;

- mandatory dilution of the initial test solutions with the addition of a sufficient amount of acid to suppress the hydrolysis of salts;

- preparation of standard solutions in one flask for all elements with the same amount of acid as in the test solutions;

- determination of concentrations for several selective lines.

- a metrological assessment of the results obtained was carried out: the accuracy characteristics were determined - correctness and reproducibility. The error in the determination of different concentrations of analytes (1-50%) was calculated. It is shown that the error component of the developed technique is only a random component.

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The flagship among parallel atomic emission spectrometers with inductively coupled plasma, the Varian 720-series ICP spectrometers are designed for the simultaneous precision rapid determination of up to 73 elements of the periodic table in liquid and solid samples (in solid samples, complete with Cetac laser ablation attachments or after microwave dissolution in Milestone Ethos systems).

Control - completely from a PC running under Windows, the delivery set includes a Neslab M33PD1 recirculating cooler.

The 720 Series instruments do indeed measure virtually all emission lines of an element simultaneously, allowing all sample components to be determined after a single aspiration.

Specifications

Typical optical resolution (pm) at corresponding elements

Design Features of Varian 720-ES and 725-ES ICP Spectrometers

Optical design - real Echelle

Patented VistaChip CCD based on I-MAP technology. 70,000 pixels are located exactly in the two-dimensional image of the echelogram in the optical range of 167-785 nm, thermostated at -35 ° C (three-stage Peltier thermoelement), pixels are located only in those areas of the optical range where there are lines of the elements to be detected.

The maximum pixel readout speed is 1 MHz. The total readout time with full illumination of all pixels is 0.8 sec.

Individual pixel overload protection with a three-stage charge drain system.

Polychromator - 0.4 m Echelle (creates an Echelle 70 order), thermostatted at 35 ° C. The total consumption of argon at the flow into the plasma (Plasma gas flow) is 15 l / min, the total operating consumption of argon is not more than 18 l.

RF generator - air-cooled, with a free running wave of 40 MHz with a programmable power setting in the range of 0.7-1.7 kW. High efficiency energy transfer of generator to plasma> 75% with stability better than 0.1%. Has no consumable parts.

A wide range of attachments expands the analytical capabilities of the 720/725-ES spectrometers.

720-ES series ICP torches

Axial OR radial design only. Taking into account the well-known fact that a dual view ICP spectrometer is an unsuccessful version of an axial view instrument, Varian spectrometers are principally produced only in specialized versions - only with axial (720-ES) or only radial (725-ES) plasma view; Expansion of the range of determined concentrations is possible due to simultaneous measurements of several lines of one element of different intensities with automatic selection of the integration time: the unique Vista Chip CCD allows simultaneous determination of one element along 20-30 lines (with differences in intensity by hundreds of thousands of times).

Radial Plasma View (725-ES) enables:

• select a plasma section along the torch length and radius to optimize sensitivity and minimize interference,
• avoid matrix influences,
• select the viewing position along the torch height,
• determine elements in solutions with 30% salinity for 8 hours without cleaning the burner.

Axial view (720-ES) (horizontal plasma) Ideal for trace analysis, detection limits are on average 5-10 times lower than radial coverage.

Besides:

• it is possible to determine 73 elements in 35 seconds with an accuracy that cannot be achieved on instruments with a double view,
• symmetrical water-cooled cone; no need to blow off the "cold tail" of the plasma,
• patented axial design allows continuous operation for several hours with solutions with 10% salinity.

Some features of the analysis on ICP spectrometers Varian 720-ES / 725-ES.

The regulation of the content of hazardous elements is becoming more and more stringent, so the requirements for food safety are increasing. In addition, in accordance with modern standards, labeling with a listing of the content of individual components is mandatory on food packaging. Such labeling usually includes information on minerals and other ingredients that support a balanced diet and human health.

When using analytical equipment for the analysis of food, it becomes more and more important to obtain highly reliable data on the elemental composition in a wide range of concentrations, whether it is hazardous elements in trace amounts or minerals in high concentrations.

• Measurements are made over a wide dynamic range from ppb to percent with dual radial and axial plasma views. This allows a comprehensive analysis to be carried out simultaneously over a wide concentration range.
• Simultaneous registration of all wavelengths allows you to take into account the effect of the matrix and automatically select the optimal wavelengths. Accurate analysis data can be obtained in a short time.
• Distinctive features of the spectrometer (eco-mode, mini-burner, evacuated spectrometer) can significantly reduce the current consumption of argon.

Simultaneous multi-element analysis of drinking water and solution containing mineral decomposition products of cheese:

Environmental monitoring requires reliable, highly sensitive analysis, always performed in accordance with regulations designed to ensure the safety of the water supply and the protection of the environment. In addition, in laboratories analyzing more than 100 samples per day, the challenges of increasing productivity and reducing operating costs are urgent.

On ICPE-9800 series inductively coupled plasma spectrometers:

• Designed to minimize burner plugging and reduce memory effects, a vertical torch sample injection system provides a high level of reliability. Even when measuring boron, which has a strong memory effect, the flushing time between measurements is short, which reduces the overall analysis time.
• The axial view of the plasma has been optimized for maximum sensitivity.
• An even higher level of sensitivity has been achieved through the use of an additional ultrasonic nebulizer and hydride generator.

Blank measurement results after
analysis of a sample with a boron concentration of 100 mg / l for 2 minutes

An updated version of the ICH Q3D guidance document of the International Conference on Harmonization regarding the analysis of mineral impurities in pharmaceuticals is currently being approved. The detection limits must strictly comply with the allowable daily dose. Method validation is also given a great deal of attention to ensure the validity of the analytical data obtained. In addition, the analysis of residual organic solvents, such as dimethylformamide, which is often used to dissolve samples, should be simple, and its results should be stable. User support for electronic data management in accordance with Part 11 of Chapter 21 of the FDACFR is also important.

On ICPE-9800 series inductively coupled plasma spectrometers:

• The highly sensitive one-inch CCD detector provides the required detection limits. In addition to its high sensitivity, the spectrometer is capable of recording all wavelengths simultaneously. This allows you to quickly and easily take into account spectral influences when analyzing tablets and capsules with matrix based, for example, titanium dioxide.
• The plasma torch is designed to inhibit carbon adhesion, allowing organic samples to be measured.
  solvents without the use of oxygen. This allows for stable analysis without additional costs and time.
• User support for electronic data management in accordance with Part 11 Chapter 21 of the FDACFR is implemented by
  via ICPEsolution software *

Analysis of elemental impurities in pharmaceuticals in accordance with the ICH Q3D document using an ICP spectrometer

PDE (Permissible Daily Dose) from ICH draft document Q3D version step4
The results of the analysis with data for 24 elements are given in the methodological materials on the use of ICP-OES (Application News No. J99).

* Support for the laboratory network of analytical equipment using ICPEsolution software in accordance with the requirements of Part 11 of Chapter 21CFR

Full compliance with the requirements for electronic records and electronic signatures, which are spelled out in Part 11 of Chapter 21 of the FDACFR, as well as the requirements of the Ministry of Health, Labor and Welfare of Japan, is ensured by using the appropriate version of the ICPESolution software (part 11 of the full version, optional). In addition, since the software supports the laboratory network, the main server can be used for integrated management of the measurement results obtained
from a variety of analytical instruments including HPLC, GC, GCMS, LCMS, UV, FTIR, balance, TOC, thermal analyzers, particle size analyzers, and third party equipment.

ICP spectrometers are widely used in the chemical and petrochemical industries to monitor hazardous metals in production, monitor additives of components that are key to product functionality, monitor the environment throughout the plant. It is desirable to have reliable and highly stable equipment for this, capable of analyzing a variety of samples, regardless of the type of solvent (aqueous / organic), or in the presence of a matrix. It is also important to simplify the analysis process and reduce its cost, which will increase the productivity of your daily quality control work.

On ICPE-9800 series inductively coupled plasma spectrometers:

• The vertical torch orientation, which reduces memory effects, ensures stable analytical results even when testing samples with high concentrations of acids and salts, as well as organic solvents.
• The latest version of the powerful ICPEsolution software makes day-to-day analysis simple and easy.
• Distinctive features of the spectrometer (eco mode, mini-burner, evacuated spectrometer) can significantly reduce the current consumption of argon.

In metallurgy, mining, electronics, ICP spectrometers are mainly used to control the quality of materials. Therefore, the main demand is for high-precision analysis and long-term stability. In addition, some minerals and electronic waste are complex matrix samples. In these cases, it is important to avoid matrix spectral influences to obtain reliable results.

On ICPE-9800 series inductively coupled plasma spectrometers:

• Get accurate data even when analyzing complex materials. This is achieved by capturing all wavelengths from the sample and an extensive wavelength database that includes all spectral aliasing information.
• A high level of reproducibility and long-term stability is achieved thanks to a proprietary high-frequency generator, a plasma sample introduction system that eliminates memory effects, and a reliable optical system.
• The axial view unit can be removed and the system can only be used with radial view.

A fundamentally new method that combines the advantages of ICP-OES (high productivity and a wide range of linearity of the determined concentrations) and flame AAS (simplicity, high selectivity, low cost of equipment).

Today, only Agilent has this patented method of analysis and a spectrometer that has been commercially available for more than 2.5 years.

Powered by air, no gas cylinders or lines required.

Agilent 4200 MP-AES- a unique solution both for routine analysis of remote laboratories and as a new tool for research centers.

Agilent introduced the next generation of microwave plasma spectrometers in March 2014
– Agilent 4200 MP-AES.
Main advantages Agilent MP-AES 4200 MP-AES:

LOW OPERATING COSTS.

SAFE AND ECONOMIC ELEMENTAL ANALYSIS.

WITHOUT EXPENSIVE AND COMBUSTIBLE GASES - WORKS ON AIR!

Low running costs- the spectrometer does not consume expensive gases. Nitrogen plasma works on nitrogen automatically obtained from laboratory air.

Improving laboratory safety- The Agilent 4200 MP-AES does not consume flammable and oxidizing gases, so there is no need for gas service for these gases or work with cylinders.

Ease of operation- the software in Russian has built-in ready-made methods for working with different types of samples (for example, food, soil, geochemistry, etc.)

Decent technical characteristics- This fundamentally new method combines the advantages of ICP-OES (high productivity and a wide range of linearity of determined concentrations) and flame AAS (simplicity, high selectivity, low cost of equipment).

High efficiency- a plasma source with magnetic excitation, a new design of sampling systems, an optimized signal path in the optical scheme, provide detection limits at the level of radial ICP-OES.

The main innovations in the MP-AES 4200 model in comparison with the previous generation of the MP-AES 4100 spectrometer:

Optimized second generation microwave generator and new burner: improved analytical characteristics, burner life and its resistance to high-salt samples, expanded analysis capabilities of complex matrix samples, improved reproducibility.

New nebulizer gas flow controller and efficient sampling system- better reproducibility and long-term stability for "heavy" samples.

MP Expert v1.2:- intuitive software, with additional features in the ‘PRO’ package, for example, data transfer to Excel, the ability to eliminate spectral interference for target elements, automatic correction in the internal standard mode

Optimized waveguide design- now the plasma is formed farther from the injector, the plasma is more symmetrical, the capture of aerosol into the plasma is better. This has improved performance and burner life, especially when handling difficult matrix samples.

New monochromator drive- Better wavelength reproducibility, which improves background modeling and enhances long-term stability

For all MP-AES 4100 spectrometers on the territory of the Russian Federation, we supply an upgrade kit for working with new burners and higher salinity of the analyzed sample.

• Determination of concentrations of 75 elements (metals / non-metals) in solutions at a rate of 10 sec / element
• Measured concentration range - from tenths of ppb (μg / l) to tens of%
• Relative standard deviation (RSD) 1-3%
• Linear range of determined concentrations up to 5 orders of magnitude
• Excellent long term stability
• Flammable gases and argon are not required for operation: low operating costs and safety
• The cost of a set of equipment at the AAS level, significant savings in operating costs
• Easy to operate, clean and change the sample inlet system
• Software in Russian
• For the analysis of solid and inhomogeneous liquid samples, sample preparation is required, optimal - express microwave in autoclaves

Other technical features

• Robust magnetically excited plasma source simplifies analysis of complex matrices (soils, geologic rocks, alloys, fuels and organic mixtures)
Original vertical burner design: great stability when analyzing complex samples; direct axial plasma observation: improved detection limits The new hydride attachment with MSIS membrane technology has better efficiency and allows the simultaneous determination of hydride-forming and conventional elements. Automatic optimization of all parameters of the new technique when working with the selected line, incl. to increase sensitivity
• The relatively low temperature of the nitrogen plasma of the Agilent MP-AES 4200 (6000 0C versus 8000 oC for ICP-OES) gives a simpler emission spectrum, which allowed the manufacturer to offer ready-made solutions in the spectrometer software for the analysis of food samples, metals / alloys, geological rocks, petroleum products, environmental objects. The latter is especially convenient for entry-level users and makes the spectrometer easier to use than the AAS. At the same time, the Agilent MP-AES 4200 outperforms flame AAS in sensitivity, linear range, detection limits and speed.

MP Expert software (in Russian)

The software works under Windows 7 (8)
Convenient intuitive interface for data management and processing
Help system and pop-up tips
Automated systems for optimizing and eliminating interference
Preset methods for different types of samples
The MultiCal function is the ability to analyze both high and low content elements in one sample at the same time.
The ability to work on multiple spectral lines for each element to expand the dynamic range.

Also view the Agilent OneNeb Nebulizer Presentation