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

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Introduction

1. Literature review

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

1.4 Main components of AES-ICP instruments

1.4.1 Sprayers

1.4.2 Spray booths

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 limit of detection. Correctness 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 AES-ICP 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 various methods for all laboratories of the Institute involved in the creation and study of new catalysts. For these purposes, several groups have been created in the laboratory, into which analysis methods are distributed. The group in which this work was done is called the group of chemical spectral analysis. The task of developing a method for analyzing the Fe-Co-Ni catalyst supported on Al 2 O 3 and MgO for the content of active components (Fe, Co and Ni) and carrier components (Al, Mg) arose in the group for the synthesis of surface compounds, where work is carried out on the use of catalysts in the production of multi-walled carbon nanotubes (MWNTs).

Relevance of the topic.

Fe-Co-Ni-O catalysts are multi-phase solids with high particle size (6 - 23 nm). Used in the synthesis of multilayer carbon nanotubes (MWNTs) with unique physical and chemical properties (high electrical and thermal conductivity, mechanical strength, chemical inertness, etc.). It is known that carbon nanotubes are becoming a key material for developing nanotechnologies, in particular, for the production composite materials wide purpose. The synthesis of nanotubes is carried out by the methods of gas-phase catalytic carbon deposition and significantly depends on chemical composition and structures of the catalysts used. These factors largely determine the quality of the resulting nanotubes - their diameter, length, number of layers. This explains the role of elemental analysis of catalyst substances. The development of a methodology for the analysis of catalysts for active components is an important link in the creation of high-quality catalysts.

Goal of the 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 methodology for the analysis of Fe-Co-Ni-O catalysts for the elements Fe, Co, Ni, Al, Mg by the AES-ICP method with methods for improving the error in determining concentrations of 1-50 wt.d, %.

Stages of solving the problem:

1. Studying 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 AES-ICP method.

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

Scientific novelty.

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

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

The practical significance of the thesis.

To solve practical problems of detection of the main elements in Fe-Co-Ni-O-catalysts, the methodological part of the modern multi-element highly sensitive method of analysis of AES-ICP 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 technique for their detection were transferred to the group for the synthesis of surface compounds of the Institute of Catalysis of the Siberian Branch of the Russian Academy of Sciences 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, the calculations of dilution factors, the choice of analytical lines. Analytical signals were measured on the ORTIMA 4300DV instrument and concentrations were calculated. The author took an active part in testing the developed methodology on other samples, in discussing the results obtained, in preparing slides for the report together with the supervisor.

spectrometry catalyst solution

1 . Literature review

1.1 Known information about the objects of analysis

Fe-Co-Ni-O catalysts are multi-phase solids with high particle size (6-23 nm). Used in the synthesis of multilayer carbon nanotubes (MWNTs) with unique physical and chemical 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 clearly defined crystal lattice. The size of the crystallites 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 (AES-ICP) 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 predominantly solution analysis. The analytical characteristics of the method are considered in this aspect of its application. By dissolving solid samples prior to analysis, many of the interferences associated with the solid state of matter are eliminated. The AES-ICP 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 provided good reproducibility comparable to flame methods (especially atomic absorption analysis). The reproducibility is somewhat 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 test solution required for analysis.

Problems arise in the determination of certain elements at very high concentrations (30% and above), if it is necessary to obtain very accurate results.

Other disadvantages of this method should also be noted: difficulties in determining elements whose atoms have very high energies excitation (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 because of the inability to protect the operator and because of the difficulties associated with standard substances; it is not possible to determine different valence forms of an element from a single solution; high consumption of carrier gas is required; there is some difficulty in developing a sample dissolution technique that allows you to simultaneously and stably keep all the elements of a solid sample in solution. Despite all the shortcomings, the method 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 as a single element analysis. To obtain accurate results with low errors, there are a number of methods: high dilution of the studied solutions, signal measurement from several lines, non-use of analytical lines with spectral noise, sample preparation with several samples.

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

1.3 Theoretical basis AES-ICP 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 in the study of trace concentrations of a wide range of elements. At the same time, flame photometry was already widely used to determine easily excitable 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. The plasma is generated by passing an argon flow through an inductor spiral, through which a high-frequency current passes. Argon is heated to a very high temperature, an electric discharge-spark arises in it, which breaks electrons from argon atoms. The spark starts a chain reaction of knocking out electrons from argon atoms, i.e. starts the process of argon ionization and plasma formation. Such a plasma is called inductively coupled. Plasma formation takes place in a specially designed burner. The sample solution enters the argon flow through a nebulizer. In a plasma, the sample solution is exposed to high temperatures sufficient to dissociate the substance into atoms and to excite the atoms as a result of their collisions. Absorbing the energy of the plasma, the atoms are excited, their electrons jump to more distant energy orbits. Flying away to a colder region of the plasma, 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 contained in the reference books of spectral lines. As a rule, they are of great intensity. Emission polychromatic radiation that has arisen in a plasma with a solution is captured by means of the focusing optics of the spectrometer, then it is divided into separate parts of the spectrum by a dispersing device. In early spectrometers, diffraction gratings were used; in modern instruments, this is an echelle grating. They are able to isolate very narrow parts of the spectrum, almost equal to the length of the analytical line, which has turned the method of emission spectroscopy into a selective multielement method. Knowing from the reference books the lengths of the analytical lines of individual elements, you can configure the device to output a signal of a certain wavelength after the separation of polychromatic light. The light signal obtained in this way from a narrow part of the spectrum then enters the photomultiplier, after converting it into an electrical signal and amplification, it is displayed on the device screen in the form of a digital value of the electrical signal and in the form of a light wave curve in a small part of the spectrum, similar to the curve of the Gaussian function.

Schematically, the AES-ICP method is shown in Scheme 1.

Scheme 1. Schematic representation of the AES-ICP method

1.4 Main components of ICP-AES instruments

Devices 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 or gaseous. Solid and liquid samples require special equipment. We will further consider the introduction of a liquid sample. Liquids are usually sprayed. Atomizers are devices for introducing liquid samples into a spectrometer in the form of a fine aerosol. The nebulizers used with ICP for dispersing liquids into an aerosol are pneumatic (most convenient, but not the most efficient) and ultrasonic.

1.4.2 Spray chambers

Once an aerosol has been generated by the nebulizer, it should be transported to the torch so that it can be injected (sprayed) 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 affects the ionized argon passing through the burner, heating it. Such an interaction of ionized argon and a pulsating magnetic field is called inductive coupling, and the heated plasma is called ICP "flame" with a temperature of 6000-10000 K.

Figure 2. Burner layout

Zones in the plasma jet: 1 - analytical; 2 - primary radiation; 3 - discharge (skin layer); 4 - central channel (preheating zone). Details of the plasma torch: 5 - inductor; 6 - protective tube preventing breakdown on the inductor (installed only on short burners); 7 - outer tube; 8 - intermediate tube; 9 - central tube. Gas flows: 10 - external; 11 - intermediate; 12 - transporting.

1.4.4 Devices for separating light by wavelength

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

1.4.5 Detectors

After the analytical emission line has been identified by the spectrometer, 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 light photons strike it. These knocked out electrons are accelerated towards the dynode, knocking out two to five secondary electrons for every electron that hits its surface. The amount of electricity generated is proportional to the amount of striking light. Quantitative analysis in the ICP-AES method is based on this law of physics.

1.5 Interference in the AES-ICP method

For an analytical chemist, interference is anything that causes an emission signal from an analyte (element) in a sample to differ from an analyte signal of the same concentration in a calibration solution. The presence of interference can negate the accuracy of the determination, so modern instruments are designed to minimize these interferences. 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-NPP need to be detected specifically. The causes of various interferences are complex.

1.5.1 Spectral interference

Spectral interference- overlays (including continuum and background radiation). These disturbances are best understood. Often they are 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 interfering element. The following are examples of spectral overlays.

Figure 3. Types of spectral aliasing found in ICP spectrometry.

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

c - imposition of a continuum or background. Three levels of overlaps are given, corresponding to increasing concentrations of the interfering element. Here you need to look for a line in another region of the spectrum.

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

1.5.2 Matrix interference and stray light

Matrix noise 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 related to the design of the spectrometer, while matrix noise is related to 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 interference can always be detected. So, when the acid concentration changes, the spraying efficiency changes, and, as a result, the sensitivity. Below are examples of such influence on the sensitivity of various mineral acids that are used in sample preparation.

Figure 4. Decrease in signal intensity (in % of the original signal) with the addition of various acids.

In order to apply this information in normal analytical practice, the concentrations of added acids are expressed as 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 percentage). It can be seen from the figures that all acids suppress the signal of aluminum (along the 308.2 nm line) and manganese (along the 257.61 nm line), and the effect of HCl 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 of influence on sensitivity, therefore, when developing methods with varying acid concentrations, it is necessary to carry out such a study and take into account the results. Effective method eliminating such interference from acids - maintaining their adequate levels in the standard. Increasing the temperature of the spray liquid can reduce the matrix effect of acids.

Another type of matrix interference is associated with plasma, i.e. with the excitation process. Thus, it is possible to detect the influence of a changing concentration of a matrix element (K, Na, Mg, Ca) on the excitation process, leading to a decrease in the output signal. As the concentrations of these elements in the solution increase, 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 methodology. It is necessary to keep in mind the ionization interference from the presence of a large excess of easily ionized elements (alkaline). A universal way to avoid matrix interference is to dilute the solutions under study to a fixed (no longer changing upon further dilution) background level. Here, the problem may be only for the determination of low concentrations of elements, when dilution will lead to going beyond the lower limit of detection.

1.5.3 Lower limit of detection. Correctness and reproducibility

The lower limit of detection (LLD) is an important indicator when evaluating an instrument and a method. This is the lowest concentration that can be reliably identified as being above zero radiation and can be easily quantified. The zero level corresponds to the value 3?, where? is the standard deviation of the average value of the drift (noise) of the background, 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 value? is multiplied by 3 and converted to the concentration of this element through the calibration curve for the element. µg/cm3 of the element corresponding to the 3? signal is taken as the detection limit of the element. In modern devices with computer programs concentration corresponding to signal 3? are calculated automatically. In the PERKINELMER OPTIMA 4300DV it is shown as the SD value in µg/cm 3 when the BLANK background solution (usually distilled water) is sprayed. Measurements of concentrations near the limit of detection can only be semi-quantitative. For quantitative measurements with an error of ±10% relative to n.p.o. increase by 5 times, with an error of ±2% relative to n.p.o. should be increased by 100 times. 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, reducing the dilution by 5-100 times or increasing the sample by 5-100 times. Difficulties may arise if there is insufficient amount of the analyzed solution or dry matter. In such cases, it is necessary to find a compromise on accuracy together with the customer.

The ICP-AES method is a method with good reproducibility. Reproducibility can be calculated from simply repeating measurements of the same solution in a short period of time, or doing repeated analyzes covering a large period of time, including sampling and sample dissolution. When approaching n.p.o. reproducibility is greatly reduced. Reproducibility is affected by changes in spray conditions (nozzle clogging, temperature, etc.), as they greatly change the output signal of the emission. Slight fluctuations in pressure in the spray chamber also change the emission, so care must be taken 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 element internal standard to the element being analyzed. But this method is not very suitable for routine analysis because of the 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 overall level of noise in the ICP AES method is different in each case, but in most cases systematic noise 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 interference by dilution, then it is possible to determine the analyte in different (by matrix) samples using the same calibration curves, making several parallel signal measurements to assess reproducibility. Its modern devices also calculate automatically as the RSD value that accompanies each result obtained on the device. It is calculated using the same formulas as SD.

2. Stages of developing a technique for the analysis of solid substances by the AES-ICP method.

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

Figure 5. Scheme of the main stages of methodology development.

Explanations for some stages of the scheme.

Stage 1. The sample must be carefully (100%) crushed in an agate mortar with elimination of large particles and their repeated grinding.

Stage 4. The lower detection limit (LLD) is important to know for 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

Sample (g) \u003d μg / cm 3 * V / 10 4 * C, where

µg/cm 3 - range of concentrations of working standard solutions. The formula uses the concentration of the first and last standard solution, according to which the calibration graph will be built;

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

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

Step 6. The method of transferring a solid sample to a solution can be any known in analytical practice. If there are many ways, you need to choose the fastest, cleanest (in the sense of introducing fewer additional chemical elements during sample preparation) and the most accessible. This is usually an acid solution. For the tasks of analysis by the AES-ICP 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 use it to select a solvent that will ensure the process of dissolution without loss of the elements to be determined in the form of volatile compounds or in the form of secondary precipitation. There are many manuals for sample preparation purposes.

The solvent is selected according to the properties of the elements of the substance being 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 ask about the solubility of this substance. And only after that it is necessary to start the search for a solvent.

Step 13: Dilution is an important procedure for reducing spectral and matrix noise in the ICP-AES method. General rule there may be advice to make several 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 to reduce the concentration in the photometric solution, i.e. keep increasing the dilution rate. If the possibilities of dilution are exhausted (you go beyond the detection limit of the element), you need to look for another, more sensitive line of the spectrum or make measurements on the device using the addition method. In most cases, in the AES-ICP method, it is possible to avoid any interference by dilution.

Stage 14. Additional dissolution of the precipitate is carried out under more severe conditions compared to those selected according to clause 6. Here you can use both microwave heating under pressure and fusion.

Stage 12, 15, 16. Photometry of the studied solutions is carried out along pre-selected 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 a 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 the element and eliminate spectral noise using various methods of concentration (increasing the sample, evaporation, extraction, ion exchange, distillation of volatile compounds of the matrix, etc.)

3. Experimental part

In Chapter 2, we outlined the main steps involved in developing an ICP-AES analysis methodology. In this chapter, we have applied this guideline to develop a specific methodology for performing basic element analysis in a Fe-Co-Ni catalyst supported on Al 2 O 3 . the accuracy of the results, such techniques include:

1) increase in the number of parallel weights;

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 studied solutions;

4) determination of concentrations to carry out on several selective lines;

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

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

The analytical task was as follows: to select a solvent for the catalyst, to find analytical lines for Fe, Co, Ni, Al, and Mg, to select photometry conditions on the OPTIMA 4300DV instrument, to obtain data on analyte concentrations, to check the correctness of determining these concentrations, to 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 Catalyst solvent selection

Having studied the literature on dissolution methods for systems similar to 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, noticeable, they are free from the radiation of other elements from this list, their radiation 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 most selective and sensitive lines for 70 elements of the periodic system, 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, at what concentration, will interfere with the work of the selected analytical line. The interfering influence of accompanying elements is most often manifested when determining low concentrations against the background of high accompanying elements. In our sample, all concentrations are high and there is no particular danger of concomitant influence if a selective line is chosen. You can also verify this using the software of the device, which draws the spectra either in the form of a separate bell, or with their overlays on each other. Acting according to the described principle, we chose three analytical lines for the elements to be determined from those included in the program. (Table 2)

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

3.3 Choosing the optimal conditions for photometry on the OPTIMA 4300 DV instrument

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

3.4 Preparation of standard solutions

To perform concentration measurements in test solutions, it is necessary to calibrate the instrument using standard solutions. Standard solutions are prepared either from purchased state standard samples of the composition (GSO of the composition), or from substances suitable for the standards.

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

The preparation of the spectrometer and the operation of spraying solutions are carried out in accordance with the operating instructions for the device. First spray a joint working standard solution 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 from the mass concentration of the element (Fe, Co, Ni, Mg and Al). It turns out, five calibration graphs for five elements.

Spray the test solution. 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 were used as the studied solutions. The computer calculates the mass concentration of the elements (Fe, Co, Ni, Mg and Al) in µg/cm 3 . The results are shown in table 3.

Table 3. Results of determining the concentration of Fe, Co, and Al from three lines in the samples. No. 1.

The data from the table was used to calculate the results of the analysis in mass fractions, %. Elements were determined from 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 determining the concentrations of Fe, Co, Ni, Al and Mg

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

1) Check for correctness using another method of analysis;

2) Verify the correctness of the standard sample of the same composition of the catalyst;

3) By the method of "guided-found"

We used the "entered - found" method. This is very convenient, because this is a replacement for expensive standards that are not always at hand. The bottom line is that we introduce an additive from the standard solution of the element into the test solution, then we measure the concentration of the element on the device in two solutions - without the additive and with the additive. The result without additive is subtracted from the result with additive. The difference should be the concentration of the additive. Table 6 shows the results of such a test with sample No. 1.

Table 6. The results of checking the results for samples No. 1 and No. 2 using the “found-found” method.

Because the technique should 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 results of such calculations are shown in Table 7.

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

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

where is the standard deviation of a single result;

x i -single result of the analysis;

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

where x cf - the average result of the analysis;

Standard deviation of the mean.

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

where r is the ratio of the systematic component to the random one. 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 the 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 AES-ICP 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 economic efficiency its production. It reflects all aspects economic activity and the results of the use of all production resources are accumulated.

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

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

Calculation of the cost of measuring instruments and laboratory equipment

Table 9. Equipment for analysis

Table 10. Equipment for establishing the calibration dependence

Calculation of the cost of the laboratory

The laboratory involved in the analysis is 35 m 2 .

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

C \u003d 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 ​​\u200b\u200bthe premises, rubles;

S - occupied area, m 2.

For our calculation, the cost of the laboratory is:

40,000 rubles / m 2 * 24m 2 \u003d 96,000 rubles

Depreciation of fixed assets

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

The depreciation included in the cost of analysis was calculated using the following formulas:

H a \u003d (1 / n) * 100%, (6)

where N a - depreciation rate,%;

n - standard service life, years.

A year \u003d F n * N a / 100%, (7)

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

N a - depreciation rate,%;

A year - annual depreciation charges, rubles.

A month \u003d A year / m, (8)

where A year - annual depreciation, rubles;

m is the number of months in a year;

A month - depreciation per month, rubles.

A hour \u003d A month / t months, (9)

where A month - depreciation per month, rubles;

And an hour is depreciation per hour.

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

where A hour - 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 a calibration dependence

Reagent Cost Calculation

Table 13. Calculation of the cost of reagents for analysis

Table 14. Calculation of the cost of reagents to establish the calibration dependence

Calculation of time spent on analysis

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

Conducting the experiment - 1 hour;

Processing and delivery of results - 0.5 hours.

It takes 2 hours to complete the analysis. Operating time of the equipment - 1 hour.

In order to calibrate the analyzer it is necessary to 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 hours;

Processing of measurement results - 0.5 hours.

It takes 2 hours to establish the calibration dependence. The operating time of the equipment is 1 hour.

Calculating the cost of laboratory glassware for analysis

The calculation of the cost of laboratory glassware included in the cost of the analysis was carried out according to the following formulas:

where C is the cost of laboratory glassware;

m is the number of months in a year;

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

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

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

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

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

t analysis - analysis time, hours;

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

Table 15. Cost of laboratory glassware for analysis

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

Table 16. The cost of laboratory glassware to establish the calibration dependence

To establish the 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 wages of a laboratory assistant

Table 19. Calculation of wages of a laboratory assistant for analysis

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

Deductions for social needs

Deductions for social needs is 30%, of which:

We get:

Amount, total * Tariff rate

Total: 200 * 0.3 \u003d 60 rubles. - deductions for social needs for analysis

Total: 200 * 0.3 \u003d 60 rubles. - deductions for social needs to establish a calibration dependence

Overhead calculation

In the project, overhead costs are assumed in the amount of 32% of the salary of a laboratory assistant:

Amount, total * 0.32

200 * 0.32 \u003d 64 rubles. - overhead for analysis

200 * 0.32 \u003d 64 rubles. - overhead costs for establishing the calibration dependence

Calculation of other costs

Other expenses accepted in the amount of 7% of the above expenses:

Crockery + Reagents + Energy + Wages + Social Security Contributions needs + depreciation. fixed assets + overhead = expenses

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

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

Expenses * 0.07 = Other expenses.

408.56 * 0.07 \u003d 28.60 rubles. - other costs attributable to one analysis

403.89 * 0.07 \u003d 28.27 rubles. - other costs incurred to establish the calibration dependence

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

Scheme 2. Cost structure.

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

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

Main conclusions

1. Studied theoretical questions method of atomic emission spectrometry with inductively coupled plasma.

2. The device of the spectrometer OPTIMA 4300DV was studied.

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

4. Methods for performing analysis were used, which make it possible to determine high concentrations of elements by a highly sensitive method, namely:

– increase in the number of parallel weights;

– obligatory 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 studied solutions;

– determination of concentrations by several selective lines.

– a metrological evaluation of the obtained results was carried out: accuracy characteristics were determined - correctness and reproducibility. The error in determining 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 of parallel inductively coupled plasma atomic emission spectrometers, 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).

Management - completely from a PC running under Windows, the Neslab M33PD1 circulating cooler is included in the package.

Instruments of the 720th series really provide the simultaneous measurement of almost all emission lines of the elements, allowing you to determine all the components of the sample after a single aspiration.

Specifications

Typical optical resolution (pm) on respective elements

Design features of Varian 720-ES and 725-ES ICP spectrometers

Optical design - real echelle

Patented VistaChip CCD detector based on I-MAP technology. 70,000 pixels are located exactly according to the two-dimensional image of the eshellogram 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 being determined.

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

Individual pixel overload protection with 3-stage charge dissipation system.

Polychromator - 0.4 m Echelle (creates an Eshellogram of 70th order), thermostated 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 no more than 18 l.

RF generator - air-cooled, with a traveling wave (Free running) 40 MHz with a programmable power setting in the range of 0.7-1.7 kW. Highly efficient plasma generator energy transfer >75% with stability better than 0.1%. Has no consumables.

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

ICP burners in the 720-ES series

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

Radial Plasma View (725-ES) allows you to:

• select a plasma region along the length of the flame and along the radius to optimize sensitivity and minimize interference,
• avoid matrix influences,
• select the viewing position according to the height of the burner,
• 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 in the case of a radial view.

Besides:

• it is possible to carry out the determination of 73 elements in 35 seconds with an accuracy that cannot be achieved on devices with a double view,
• symmetrical water-cooled cone; blowing off the "cold tail" of the plasma is not required,
• the patented axial design allows continuous operation for several hours with solutions with 10% salinity.

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

Hazardous element regulations are becoming more stringent, so food safety requirements are increasing. In addition, in accordance with modern standards, food packaging is required to be labeled with a listing of the content of individual components. Such labeling usually includes information on mineral and other components that support a balanced diet and human health.

When using analytical equipment for food analysis, it is becoming increasingly important to obtain highly reliable elemental composition data over a wide range of concentrations, whether hazardous elements in trace amounts or mineral components in high concentrations.

• Measurements are performed in a wide dynamic range from ppb units to percent due to the dual - radial and axial - view of the plasma. This allows comprehensive analysis to be carried out simultaneously over a wide range of concentrations.
• Simultaneous registration of all wavelengths makes it possible to take into account the influence of the matrix and automatically select the optimal wavelengths. Accurate analysis data can be obtained in a short time.
• Distinctive characteristics spectrometer (eco mode, mini-torch, evacuated spectrometer) can significantly reduce the current consumption of argon.

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

To control objects environment reliable, highly sensitive analysis is required, 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 that analyze more than 100 samples per day, the challenges of increasing productivity and reducing operating costs are relevant.

On inductively coupled plasma spectrometers of the ICPE-9800 series:

• Designed to minimize burner plugging and memory effects, a sample injection system with a vertical burner ensures a high level of reliability. Even when measuring boron, which has a strong memory effect, the wash 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 is 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 is currently being approved International Conference on Harmonization regarding the analysis of mineral impurities in medicinal products. Limits of detection must strictly comply with the allowable daily dose. Method validation is also given great attention to ensure the validity of the resulting analytical data. In addition, the analysis of residual organic solvents, such as dimethylformamide, which is quite 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 of great importance.

On inductively coupled plasma spectrometers of the ICPE-9800 series:

• The highly sensitive one-inch CCD detector provides the required detection limits. In addition to 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 a matrix based on, for example, titanium dioxide.
• The plasma torch is designed to resist carbon adhesion, allowing measurement of organic based samples.
  solvents without the use of oxygen. This allows a stable analysis without additional costs and time.
• Support for users in terms of electronic data management in accordance with Part 11 of Chapter 21 of the FDACFR is implemented
  via ICPEsolution software *

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

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

*Supports the functioning of the laboratory network of analytical equipment using the 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 prescribed in Part 11 of Chapter 21 of the Code of Federal Regulations FDACFR, as well as the requirements stipulated by the Ministry of Health, Labor and Welfare of Japan, is ensured by using the appropriate version of the ICPESolution software (Part 11 full version, optional). In addition, since the software supports the laboratory network, the main server can be used to integrally manage the measurement results obtained
from a variety of analytical instruments including HPLC, GC, GCMS, LCMS, UV, FTIR, balances, TOC, thermal analyzers, particle size analyzers, and third party equipment.

ICP spectrometers are widely used in the chemical and petrochemical industries for the control of hazardous metals in production, the control of additives of components that are key to the functionality of products, and the control of 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 productivity. daily work for quality control.

On inductively coupled plasma spectrometers of the ICPE-9800 series:

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

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

On inductively coupled plasma spectrometers of the ICPE-9800 series:

• Get accurate data even when analyzing complex materials. This is achieved by recording all wavelengths from the sample and an extensive wavelength database including all information about spectral influences (overlaps).
• A high level of reproducibility and long-term stability is achieved thanks to a proprietary high-frequency generator, a memory-free plasma injection system, and a robust optical system.
• The axial view unit can be removed and the system can be used exclusively with radial view.

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

Today, only Agilent has this patented analysis method and a spectrometer that has been mass-produced for more than 2.5 years.

Runs on air, no gas cylinders or lines required.

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

In March 2014, Agilent introduced the next generation of microwave plasma spectrometers
– 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 operating costs- the spectrometer does not consume expensive gases. Nitrogen plasma runs on nitrogen automatically obtained from laboratory air.

Increasing the level of safety in the laboratory- The Agilent 4200 MP-AES does not consume combustible and oxidizing gases, so gas communications for these gases or work with cylinders are not required.

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

Worthy specifications - this fundamentally new method combines the advantages of ICP-OES (high performance and 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 compared to the previous generation of the MP-AES 4100 spectrometer:

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

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

MP Expert v1.2:- intuitive software additional features in the ‘PRO’ package, e.g. data transfer to Excel, ability to eliminate spectral noise for target elements, automatic correction in 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 improved the performance and life of the burner, especially when working with complex matrix samples.

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

For all MP-AES 4100 spectrometers in the Russian Federation, we supply an upgrade kit to work with new burners and higher salinity of the analyzed sample.

• Determination of concentrations of 75 elements (metals / non-metals) in solutions at a speed of 10 sec / element
• Range of measured concentrations - 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 level of AAC, significant savings in operating costs
• Easy to operate, clean and change the injection system
• Software in Russian
• For the analysis of solid and inhomogeneous liquid samples, sample preparation is necessary, the optimal one is express microwave in autoclaves

Other technical features

• Robust magnetically excited plasma source simplifies analysis of complex matrices (soils, geological formations, alloys, fuels and organic mixtures)
Original vertical burner design: greater stability when analyzing complex samples; Direct Axial Viewing of Plasma: Improved Limits of Detection New hydride attachment with MSIS membrane technology offers better performance and allows simultaneous detection of hydride-forming and conventional elements to increase sensitivity
• The relatively low temperature of the Agilent MP-AES 4200 nitrogen plasma (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 analyzing food samples, metals/alloys, geological rocks, oil products, environmental objects. The latter is especially convenient for entry-level users and makes the spectrometer easier to use than AAS. The Agilent MP-AES 4200 outperforms flame AAS in terms of sensitivity, linear range, detection limits and speed.

MP Expert software (in Russian)

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

You can also see the presentation of the Agilent OneNeb nebulizer