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1.5 moleq. of the alkyltriphenylphosphonium bromide are in THF1) (10 ml / mmol) dissolved at -78 with 1.5 moleq. one 1.6 M. n-BuLi / hexane solution deprotonated and warmed to room temperature within one hour. Then leave it at 0 1 moleq. the carbonyl compound dissolved in THF (2 ml / mmol) is added dropwise and the solution is stirred for three hours at room temperature. The reaction is quenched with an ice bath by neutralization with 2 N canceled, the crude product isolated by extraction with cold diethyl ether and that largely separated by crystallization. (More quantities can through a rough flashPSC2) be separated from the product.) Drying of the organic phase with Removal of the solvent in vacuo and final PSC deliver the pure product.
Wittig Reaction Mechanism
Wittig Reaction Mechanism Let's now discuss the mechanism of the Wittig reaction. It is a nucleophilic addition-elimination reaction and, in that sense, is still somewhat like the other reactions of aldehydes and ketones such as the ones with cyanides, alcohols or amines Mechanism of the Wittig reaction 1) Nucleophillic attack on the carbonyl 2) Formation of a 4 membered ring 3) Formation of the alken The Wittig Reaction allows the preparation of an alkene by the reaction of an aldehyde or ketone with the ylide generated from a phosphonium salt. The geometry of the resulting alkene depends on the reactivity of the ylide. If R is an electron withdrawing group, then the ylide is stabilized and is not as reactive as when R is alkyl MECHANISM OF WITTIG REACTION The mechanism of Wittig reaction is not fully established. However a simplified picture is given below. The initial step is the nucleophilic addition of negatively charged carbon of ylide onto the carbonyl carbon to give a betaine, which can cyclize to give an oxaphosphetane as an intermediate The Mechanism of the Wittig Reaction. If you look above to the bonds that form and break in the Wittig reaction, you'll see that it essentially swaps C = P and C = O bonds for C = C and O = P bonds. So how does it work? The version of events described in most introductory textbooks follows below. [In this footnote, I describe a slightly modified account of the mechanism that is generally more.
The Wittig Reaction - Chemistry LibreText
- Mechanism of the Wittig reaction For the mechanism of the Wittig reaction, a [2 + 2] cycloaddition of ylene to oxaphosphetane is proposed, which opens to the olefin and phosphine oxide
- In the Wittig reaction, a double bond is formed between an aldehyde or ketone and a phosphorus ylide. This reaction can therefore be used to link two organic molecules with a double bond to form an alkene. You can find everything important about the Wittig reaction here
- In the presence of lithium ions, the Wittig reaction leads to mixtures of (E / Z) olefins in its absence one achieves (Z) selectivity (salt-free) - the Schlosser variant is produced with an excess of lithium salts and a sequence of deprotonation Protonation reactions improved (E) selectivity
- In the Wittig reaction, a new stereogenic unit is created - a double bond. The reactions proceed with a pronounced stereoselectivity. This depends on the substituent of the carbon atom on the ylide (Figure 94). Figure 94 Examples of a Z-selective and an E-selective Wittig reaction
Wittig Reaction - Organic Chemistr
The Wittig reaction or Wittig olefination is a chemical reaction of an aldehyde or ketone with a triphenyl phosphonium ylide called a Wittig reagent. Wittig reactions are most commonly used to convert aldehydes and ketones to alkenes What is Wittig Reaction? Wittig reaction is an organic chemical reaction wherein an aldehyde or a ketone is reacted with a Wittig Reagent (a triphenyl phosphonium ylide) to yield an alkene along with triphenylphosphine oxide. This reaction is named after its discoverer, the German chemist Georg Wittig
The Wittig reaction or Wittig olefination is a chemical reaction of an aldehyde or ketone with a triphenyl phosphonium ylide (often called a Wittig reagent) to give an alkene and triphenylphosphine oxide. The Wittig reaction was discovered in 1954 by Georg Wittig, for which he was awarded the Nobel Prize in Chemistry in 1979 Wittig Reaction Mechanism - YouTube. Write Quickly and Confidently | Grammarly. Watch later. Share. Copy link. Info. Shopping. Tap to unmute. If playback doesn't begin shortly, try restarting your. Wittig Reaction 53 The Wittig Reaction: Synthesis of Alkenes Intro The Wittig Reaction is one of the premier methods for the synthesis of alkenes. It uses a carbonyl compound as an electrophile, which is attacked by a phosphorus ylide (the Wittig reagent.) While many other routes to alkenes can proceed via elimination reactions (E1 or E The mechanism of the Wittig reaction has long been a contentious issue in organic chemistry. Even now, more than 50 years after its announcement, its presentation in many modern undergraduate textbooks is either overly simplified or entirely inaccurate. In this review, we gather together the huge body of evidence that has been amassed to show that the Li salt-free Wittig reactions of non.
. As you can see phosphonium ylide has a nucleophilic carbon. This carbon attacks on the carbon of the carbonyl group and initiates the reaction. Mechanism of Wittig Reaction Wittig reaction starts with the preparation of phosphonium ylide. Although ylides look like a difficult species, but their. The Wittig reaction is a chemical reaction of an aldehyde or ketone with a triphenyl phosphonium ylide (often called a Wittig reagent) to give an alkene and triphenylphosphine oxide. The Wittig reaction was discovered in 1954 by Georg Wittig, for which he was awarded the Nobel Prize in Chemistry in 1979 Unequivocal Experimental Evidence for a Unified Lithium Salt-Free Wittig Reaction Mechanism for All Phosphonium Ylide Types: Reactions with β-Heteroatom-Substituted Aldehydes Are Consistently Selective for cis-Oxaphosphetane-Derived Products. Journal of the American Chemical Society 2012, 134 (22), 9225-9239 The Wittig reaction is an organic reaction used to convert a primary or secondary alkyl halide and an aldehyde or ketone to an olefin using triphenylphosphine and base. The mechanism beings with attack of the PPH 3 on the alkyl halide which releases the halide anion and forms a phosphonium ion. The base then deprotonates at the alpha position to afford a phosphonium ylide. The ylide. It's time for the Wittig Reaction Mechanism to be made easy! Follow me in my walk-through video and we can do the mechanism together. I also provide some use ..
The primary mechanism of the Wittig reaction involves the reaction of the benzalde- hyde (1) with the methyl (triphenylphosphoranylidene) acetate ylide (2) to form a 4- membered ring intermediate (5) Mechanism of the Wittig-Horner Reaction The reaction mechanism is similar to the mechanism of the Wittig Reaction. The stereochemistry is set by steric approach control, where the antiperiplanar approach of the carbanion to the carbon of the carbonyl group is favored when the smaller aldehydic hydrogen eclipses the bulky phosphoranyl moiety Wittig Reaction 1. The Wittig Reaction Below is a useful reaction called the Wittig reaction that achieves this transformation. It won. 2. The Mechanism of the Wittig Reaction If you look above to the bonds that form and break in the Wittig reaction. 3. How are Ylides Made? A quick. . 1997, 1-85. https://doi.org/10.1016/S1068-7394(96)80002-9 Giuseppe Bellucci, Cinzia Chiappe, Giacomo Lo Moro. Crown ether catalyzed stereospecific synthesis of Z- and E-stilbenes by wittig reaction in a solid-liquid two-phases system
Reaction Mechanism of Wittig Reaction The reaction probably proceeds by the nucleophilic attack of the ylide on the carbonyl carbon. The dipolar complex (betain) so formed decomposes to olefin and triphenyphosphine oxide via a four centered transition state Stereochemistry and Mechanism in the Wittig Reaction. 2007, 1-157. https://doi.org/10.1002/9780470147306.ch1 Eoin C Dunne, Éamonn J Coyne, Peter B Crowley, Declan G Gilheany. Co-operative ortho-effects on the Wittig reaction. Interpretation of stereoselectivity in the reaction of ortho-halo-substituted benzaldehydes and benzylidenetriphenylphosphoranes The mechanism of the Wittig reaction has long been a contentious issue in organic chemistry. Even now, more than 50 years after its announcement, its presentation in many modern undergraduate textbooks is either overly simplified or entirely inaccurate In addition to the fast evolution of the emerging CC bond, very early in the reaction, a long range, weak interaction between a lone pair in the oxygen atom of the carbonyl group and an empty p orbital in the phosphorous atom, resulting from the polarization of the P═C bond in the ylide (nO → πP═C *), clamps the P═C and C O bonds to the positions required for the subsequent formation of oxaphosphetanes, thus explaining the formation of cyclic intermediates rather than betaines
1 Wittig Reaction, the Most Important Reaction in Alkene Synthesis 1.1 Alkenes Can Be Synthesized from Ketones and Aldehydes 1.2 The Reaction Mechanism is Nucleophilic Addition of Phosphorus Ylides 1.1 Alkenes Can Be Synthesized from Ketones and Aldehydes 1.2 The Reaction Mechanism is Nucleophilic. Wittig reactions The Wittig reaction, or olefination, is named after Georg Wittig who was awarded the Nobel Prize in 1979 in recognition for his fundamental contributions to organic chemistry. During the Wittig olefination, an anion is formed which then adds into either an aldehyde or ketone to form a betaine In we report an experimental effect that is common to the Wittig reactions of all of the three major phosphonium ylide classes (non-stabilized, semi-stabilized, and stabilized): there is consistently increased selectivity for cis-oxaphosphetane and its derived products (Z-alkene and erythro-β-hydroxyphosphonium salt) in reactions involving aldehydes bearing heteroatom substituents in the β-position • With stabilized ylids the Wittig reaction is E-selective (R = CO 2 R, SO 2 R) • With semi-stabilized ylides one obtains E- / Z-mixtures Z-selective Wittig reaction. Slide No. 3 [2,2] Cycloadditions (Concerted) Slide No. 4 E-Selective Wittig Reaction Two explanations are discussed: 1. Orthogonal approximation. Slide No. 5 M. Vedejs, J. Am. Chem. Soc. 1988, 110, 3948-3958. 2. In the previous post, we discussed the principle and mechanism of the Wittig reaction. Go over those if you need to and in the following practice problem, we will work on proposing a synthesis for Wittig reagents as well as preparing alkenes using the Wittig reagent and alternative methods. First, let's make a plan for solving these problems. Wittig Reaction - Solving Problems by.
for the mechanism of the Wittig reaction see: Bestmann, H. J .: Pure Appl. Chem. 52, 771 (1980) Giese, B., Schoch, J., Rüchardt, Ch .: Chem. Ber. 111, 1395 (1978) Google Scholar 12. BASF AG (Inventors G. Wittig, H. Pommer) Germ. Pat. 950,552 (1954) Google Schola Ylide Reactions with Ketones. Wittig Reactions in Multifunctional Systems. Mechanistic Considerations. Probes for electron transfer. Probes for Betaine Intermediates. Theoretical Considerations. Transition State Characteristics. Interpretation of Stereochemistry. Transition State Geometries of Stabilized Ylides. Miscellaneous reactions
The Wittig reaction involving the reaction of phosphorus ylides with carbonyl compounds is an excellent tool for the formation of carbon-carbon double bonds, and simple phosphazenes, nitrogen isosteres of phosphorus ylides, are the starting materials widely used for the construction of imine (CN) compounds through the aza-Wittig process (Scheme 4) Wittig reaction allows to obtain alkenes in which the localization of the double bond leaves no room for ambiguity. It's also free from typical problems related to alkene synthesis, for examples rearrangements in synthesis by elimination reactions
Wittig Reaction Mechanism Adichemistr
Wittig Reaction - Phosphorous Ylides ORH + Ph 3PCHCH3 H3C R ylide ¥ Stereoselectivity increases as the size of R increases ¥ cis-olefin is derived from non-stabilized ylides Mechanism: Irreversible [2 + 2] cycloaddition ORH Ph 3 3C H + P H3C H Ph 3 ORHR group of aldehydes far away from ylide CH 3 !! 2! A + 2! S cycloaddition 3 H 3C R H3C R + Ph 3PO PPh3 NaHMDS O O H OMe O OMe Chem Ber. 1976. The classic Wittig reaction. 2.1) General. 2.2) Definition of ylids. 2.3) Stability of Ylids. 2.4) Representation of ylids. 2.5) Mechanism of the Wittig reaction. 2.6) stereochemistry. 2.6.1) Labile Ylide, salt-free Wittig and without stereoselectivity. 2.6.2) Semi-stable ylids
Wittig Reaction - Examples and Mechanism - Master Organic
The key step of the mechanism is the formation of the oxaphosphetane, the cyclic intermediate. Wittig reactions can give either the E or Z isomer of the alkene depending on the nature of the phosphonium reagent. In this reaction, we expect primarily the E isomer. Mechanism: PART I. Synthesis of trans-9- (2-phenylethenyl) anthracene Wittig reaction. Mechanism of the salt-free Wittig reaction. Quantum chemical calculation of the reaction of the ylid Me 3PCH 2 with formaldehyde. Via the contact complex TS1, the intermediate oxaphosphetane OP1 is formed in a concerted reaction with trigonal-bipyramidal coordinated phosphorus, the oxygen in the apical and the ylid carbon in the equatorial position. It follows. Some attempts to produce alkynes directly using Wittig-like reactions have failed, which speaks against this mechanism. However, one could argue that the formation of the alkynes is very rapid, but this possibility can be ruled out by comparison with similar structures
The Wittig reaction or Wittig olefination is a chemical reaction of an aldehyde or ketone with a triphenyl phosphonium ylide (often called a Wittig reagent) to give an alkene and triphenylphosphine oxide. It is widely used in organic synthesis to make alkenes. It should not be confused with the Wittig rearrangement The Wittig reaction is a venerable transformation for converting the carbon-oxygen double bond of an aldehyde or a ketone into a carbon-carbon double bond of an alkene group (Scheme 1). Since its introduction over half a century ago [1,2], it has been widely employed in organic synthesis due to its versatility and reliability
Wittig reaction - Chemgapedi
- • Transition state controls Wittig stereochemistry (cis) • Ring closure controls Wadsworth-Emmons stereochemistry (trans) • cis-trans photoisomerization with iodine. Part A (p. 606) (p.590 4th ed.) - Wittig reaction for the synthesis of stilbene. Part B (p. 610) (p.594 4th th. Ed.) - Wadsworth-Emmons reaction for the synthesis of stilbene
- 1. Steric control of the Wittig reaction can be effected by changing the reaction conditions and the structures of the starting compounds. 2. Stereoselective synthesis of cis olefins from alkylideneor benzylidene-triphenylphosphoranes and aldehydes can be effected in the presence of Lewis bases. The maximum relative yield of cis olefins is attained by carrying out the reaction in N, N.
- e formation compounds related to i
Wittig reaction • Mechanism simply explained, reagent
- The Wittig reaction or Wittig olefination is a chemical reaction of an aldehyde or ketone with a triphenyl phosphonium ylide (often called a Wittig reagent) to give an alkene and triphenylphosphine oxide
- Therefore, the Wittig reaction must involve a mechanism other than the betaine pathway. An asynchronous cycloaddition process is consistent with the available evidence. View. Show abstract.
- An aza-Wittig rearrangement is known that involves nitrogen ylids (sec. 8.8.C). 498 The rearrangement is fundamentally similar to the other Wittig rearrangements just discussed. Amides are the most common precursor because the ylid derived from amide are somewhat more stable
- Mechanism of the Wittig Reaction. COPYRIGHT: Vollhardt and Schore, Organic Chemistry: Structure and Function, Fourth Edition, published by W. H. Freeman & Co. © 2002.
- Mechanism of the Wittig reaction. Following the initial carbon-carbon bond formation, two intermediates have been identified for the Wittig reaction, a dipolar charge-separated species called a betaine and a four-membered heterocyclic structure referred to as an oxaphosphatane. Cleavage of the oxaphosphatane to alkene and phosphine oxide products is exothermic and irreversible. 1.
- Wittig Reaction Summary: The Wittig reaction is a classic reaction for converting a carbonyl compound to an olefin through a four-centered intermediate. This reaction traditionally proceeds using a hazardous solvent, such as dichloromethane or dimethyl formamide. Reference: Synthesis of trans-9- (2-phenylethenyl) anthracene (microscale), Macroscale and Microscale Organic Experiments, 6e Brooks.
Video: Wittig Reaction - Organic Chemi
The Wittig Reaction - Formal Report By: Alexander Davies Introduction Alkenes are important initial building blocks in many organic synthesis routes, as shown by Scheme 1.1 It is paramount, therefore, that we have the ability to synthesize alkenes from other readily available, cheap material.Scheme 1: Examples of one-step reactions from an alkene starting material The Classic Wittig Reaction Mechanism and Stereoselectivity. Nature of the Ylide and Carbonyl Compound. Reagents and Reaction Conditions. Horner-Wadsworth-Emmons Reaction Mechanism and Stereochemistry. Reagents and Reaction Conditions. Horner-Wittig (HW) Reaction Mechanism for Wittig-Horner reaction (1) In the Wittig reaction, an organic phosphorus compound with a formal double bond between phosphorus and carbon is reacted with a carbonyl compound. The oxygen of the carbonyl compound is exchanged for carbon, forming a product known as an olefin (2). The method for making olefins has opened up new possibilities, especially for the synthesis of.
I wanted to make a contribution to maybe make it easier for everyone to prepare for the laboratory.
I would be happy if others also post what was asked by them on the day of the laboratory.
The first time I had statistics, they asked:
The questions that should be answered in the protocol, i.e.
-what the density function has to do with the histogram
-what distribution is there
-How is expected value or variance calculated
-Formula density function and what it means
Re: laboratory questions- & quotTests & quot
Contribution by tubuster & raquo 04/20/2016, 11:50 am
Re: laboratory questions- & quotTests & quot
Contribution by StefanPrt & raquo 04/25/2016, 6:31 pm
Maybe it will help who.
last week lock-in
was actually pretty easy again and we finished pretty quickly and could leave earlier.
At the end he only asked briefly how a lock is built in an amplifier, and what happens in it, i.e. how vibrations are superimposed and how
that looks arithmetically.
The second question was what a superconductor is and what happens when a material becomes superconducting.
Re: laboratory questions- & quotTests & quot
(which I can still remember each time)
Optical spectroscopy: structure and function of the laser, line widths / broadening, resolution of the measuring device
Muons: Formation of muons in the atmosphere (exact reactions), structure and functionality of the photomultiplier, why fewer muons with horizontal measurements than with vertical ones?
Statistics: All questions listed in the instructions (how do the expected value and variance behave when adding / multiplying constants, how are the histogram and density function related, has the distribution passed the chi-square test, etc.), explanation of the written protocol
Frank-Hertz: detailed description of the experiment (+ setup, including drawing in the respective potentials) and the physical meaning. Explanation of the difference between the measured wavelength and the predicted wavelength for helium
Login amplifier: Explanation of the principle and structure of the login amplifier, types of magnetism (explanation of susceptibility), superconductivity (definition, connection to the other types of magnetism), function of the thermocouple
Ultrasound: Principle of ultrasonic material testing, advantages & disadvantages, Schnellius' law of refraction (relationship between refractive index and speed), transverse and longitudinal waves, wave equation
Qualitative inorganic analysis
1 Safety in the laboratory - 1.1 General information - 1.2 Special information on qualitative analysis - 1.2.1 Preparation of the analysis - 1.2.2 Dangers of individual preliminary samples and evidence - 1.3 What to do in emergencies - 1.4 First aid measures. - 1.4.1 Cuts - 1.4.2 Poisoning - 1.4.3 Burns / scalds - 1.4.4 Chemical burns - 1.4.5 Accidents with electrical power - 1.5 Disposal - 2 First steps - 2.1 General information - 2.2 Dissolving the analysis substance - 2.3 Preliminary samples - 2.3.1 General preliminary samples - 2.3.2 Flame color - 2.3.3 Annealing with Co (NO3) 2 solution - 2.3.4 Oxidation melt - 2.3.5 Phosphorus salt and borax pearl - 2.4 Soda extract - 2.4.1 Important information on the soda extract - 2.5 Detection of standard anions - 3 cation analyzes - 3.1 HCl group - 3.1.1 Separation process in the absence of S2? and Cl? - 3.1.2 Separation process in the presence of S2? and Cl? - silver, Ag.- lead, Pb.- mercury, Hg.- 3.2 H2S group - 3.2.1 Separation process of the H2S group - 3.2.2 Separation of the arsenic group - 3.2.3 Separation of the Cu -Group.- Bismuth, Bi.- Copper, Cu.- Cadmium, Cd.- 3.2.4 Separation of the arsenic group.- Arsenic, As.- Antimony, Sb.- Tin, Sn.- 3.3 Urotropin- and (NH4) 2S -Group.- 3.3.1 Hydrolysis separation.- 3.3.2 The (NH4) 2S group.- Iron, Fe.- Aluminum, Al.- Chromium, Cr.- Nickel, Ni.- Cobalt, Co.- Manganese, Mn .- Zinc, Zn.- 3.4 (NH4) 2CO3 group.- 3.4.1 Inclined relation in the PSE.- 3.4.2 Separation path of the (NH4) 2CO3 group.- Calcium, Ca.- Strontium, Sr.- Barium, Ba .- 3.5 Soluble group.- Sodium, Na.- Potassium, K.- Ammonium, NH4 + .- Magnesium, Mg.- 4 anion analyzes - 4.1 Preliminary tests for anion groups - 4.2 Separation of anions mixtures - 4.2.1 Separation of the halogen-containing anions .- 4.2.2 Separation of the sulfur-containing anions.- 4.3 7th main group, halogens.- 4.3.1 Hydrogen halides and halides.- Fluoride, F? .- Chloride, Cl? .- Bromide, Br? .- Iodide, I ?. - 4.3.2 p Oxygen acids of halogens and their salts.- Hypochlorite, ClO? .- chlorate, ClO3? .- perchlorate, ClO4? .- bromate, BrO3? .- iodate, IO3? .- 4.4 6th main group, chalcogens.- peroxide, O22? .- 4.4.1 Hydrogen compounds of sulfur (sulphanes) .- Sulphide, S2? .- 4.4.2 Oxygenic acids of sulfur.- Sulphite, SO32? .- Thiosulphate, S2O32? .- Sulphate, SO42? .- Peroxodisulphate, S2O82 ?. - 4.5 5th main group, nitrogen group - 4.5.1 Oxygen acids of nitrogen - Nitrite, NO2? - Nitrate, NO3? - 4.5.2 Oxygen acids of phosphorus - Phosphate, PO43? - 4.6 4th main group, carbon group. - Carbonate, CO33? .- Cyanide, CN? .- Thiocyanate, SCN? .- Silicate, SiO32? .- 4.7 3rd main group, boron group.- Borate, B4O72? .- 5 Dissolving and digesting.- 5.1 General.- 5.2 The digestion process - 5.2.1 Oxidation melt - 5.2.2 Acid digestion with KHSO4 - 5.2.3 Soda / potash digestion - 5.2.4 Freiberg digestion - 5.3 Reactions in molten salts - 5.3.1 Reactions without electron transfer - 5.3.2 Reactions with electro transfer.- 6 Separation with rare elements.- Lithium, Li.- Rubidium, Rb.- Cesium, Cs.- Beryllium, Be.- 6.1 Rare earth metals.- Lanthanum, La.- Cer, Ce.- Titanium, Ti.- Zirconium , Zr.- 6.2 Isopolyacids.- 6.3 Heteropolyacids.- Vanadium, V.- Molybdenum, Mo.- Tungsten, W.- Thallium, Tl.- Selenium, Se.- Tellurium, Te.- 6.4 Separation process with rare elements.- Appendix .- Subject index.
Chemiluminescence of oxalic acid esters with special consideration of substituted condensed benzoid aromatics and their effect as luminophores
2.1 Requirements for luminophores and choice of substance class
So that sufficient electronic excitation of the luminophore can take place, it should be designed in such a way that the electrons of the substance in question are easily »accessible«, distributed over a large area and present in large numbers. The π-electron system of aromatics is excellently suited for this. Especially when we have a complex system made up of several individual π systems. We would have had such a situation with the condensed benzoid aromatics. The linearly condensed representatives, especially anthracene and naphthacene, as well as the angularly condensed ones, such as phenanthrene or benz [b] anthracene. Further possibilities of variation arise if chromophores, such as e.g. B. nitro groups, halogen atoms and the like., Are introduced. What such a thing can look like in the »extreme case« is shown by BASF with the luminophore »KF 856« it has developed:
In order to achieve decent chemiluminescence, you certainly don't have to go that far. The light yields are not to be despised even "on a small scale". The basic structure that I have chosen is that of anthracene. Less because of chemical aspects, there are definitely more efficient substances, but more because, in my opinion, it has the best "price-performance ratio". It is available in large quantities quite cheaply (Lancaster, 250 g 10.70 euros) and it offers many possible variations for syntheses.
Starting from anthracene or from simple derivatives, the 9,10-dibromanthracene has proven to be particularly diverse, many substances can be synthesized that are used as luminophores or. could be of interest as potential luminophores.
Anthracene derivatives with good luminescence properties are z. B. the following:
trans-9- (2-phenylethenyl) anthracene, C22H16
For example, I have tried:
2.2 Considerations for the Synthesis of Selected (Potential) Luminophores
In order to obtain satisfactory results, i.e. yields, in a synthesis, it is necessary to choose synthesis routes that provide a defined product and that can also be implemented with relatively little effort. This is particularly important if you do not have the resources that professional laboratories, for example, can use. I am mainly talking about modern chemical analysis equipment, such as gas chromatography or HPLC. The use of IR or NMR would also be of interest in some cases. But that really exceeds all my possibilities.
In following the progress of my syntheses, I limit myself to thin-layer chromatography, which in most cases gives me sufficient certainty about the success or failure of my practical work.
As mentioned at the beginning, I chose anthracene as the basic structure. However, with anthracene as the starting material, it is not possible to meet the requirements placed on the reaction at the outset. The anthracene itself is due to the lack of "real" functional groups if one looks at the
π-electron system refrains from being too undifferentiated. If you want a certain product, for example an alkylated or arylated anthracene, you can definitely carry out a corresponding reaction on the unsubstituted aromatic. However, the likelihood of an accumulation of by-products is relatively high.
For this reason I only use the anthracene directly for the planned syntheses in the rarest of cases. Rather, I use simple anthracene derivatives, such as anthracene-9-carbaldehyde or 9,10-dibromoanthracene. The latter is, so to speak, the linchpin in my syntheses. It is easy to prepare, inexpensive and with a high degree of purity, and the substituents make it attractive for further reactions.
To produce 9,10-diphenylanthracene by starting with anthracene and, for example, carrying out a Friedel – Crafts reaction using chlorobenzene and aluminum (III) chloride, would be feasible and easy to understand. However, there would be two problems in particular. On the one hand, there is the difficulty of arylating the aromatic at the selected position. It will be
9,10 derivative is preferentially formed due to mesomerism stabilization, but it is more than likely that some other derivatives will also be obtained which are undesirable. These are not only derivatives that are substituted in the wrong position, but also derivatives that have been substituted more often than intended. This is related to the second problem. The substitution with a phenyl radical activates the anthracene structure, which simplifies multiple substitutions. In order to be able to substitute specifically at positions 9 and 10, I start from an educt that is already substituted with reactive groups at these points.
Namely from 9,10-dibromoanthracene. The 9,10-dibromoanthracene is obtained simply by brominating anthracene. It could be said that problems similar to those with arylation could arise here. It is not so. This substitution deactivates the nucleus, making further substitutions more difficult. The main product can also be obtained in pure form by recrystallization.
Elemental bromine can be used directly as a brominating agent. Such brominations are normally carried out in polyhalogenated hydrocarbons, preferably chloroform or carbon tetrachloride .
However, carbon tetrachloride in particular is not very good for health, so it is better to switch to other solvents. Trimethyl phosphate is ideally suited for this purpose . Although it is also labeled as »toxic«, it cannot be compared with the dangers of carbon tetrachloride. This solvent can be handled without problems under a hood. The advantage of trimethyl phosphate lies in another, very decisive property. Trimethyl phosphate has good dissolving power for hydrogen bromide. The hydrogen bromide produced in the reaction to a not inconsiderable extent would have to be diverted or absorbed, which would cause further problems. It is also extremely uncomfortable to be exposed to hydrogen bromide vapors while processing the residue in the flask. Nothing like this is noticed when using trimethyl phosphate. The hydrogen bromide dissolves in it excellently and cannot get into the environment.
In terms of yield, it is in no way inferior to the approach with carbon tetrachloride. Finally, there is another completely non-toxic variant of the solvent - acetic acid. Unfortunately, the yields here are not quite as excellent and recrystallization also causes some difficulties. You have to clean the crystals obtained a second time or dry them for a long time in a vacuum in order to rid them of the pungent, pungent odor of acetic acid that adheres to them.
But now to the actual synthesis:
Starting from 9,10-dibromanthracene, 9,10-diphenylanthracene can be obtained very quickly by reacting it in a Kumada coupling with a suitable Grignard compound . Phenylmagnesium bromide comes into question here. The implementation takes place according to the following formula scheme:
In this scheme, the coupling process is only shown in a greatly simplified and summarized form. The actual characteristic of the Kumada coupling, the so-called Kumada catalyst and its role in the reaction are not shown.
The catalyst is a palladium or nickel complex.
The Kumada coupling is the first coupling ever to use a Pd or Ni catalyst! Triphenylphosphine is often used as a ligand. But it is also possible to work with acetylacetonate. The complexes would be [Pd (PPh3)2], [Ni (PPh3)2] and [Ni (acac)2].
Catalysis can be broken down into four sub-steps:
- oxidative addition
- reductive elimination
In the first step, the aryl halide is added to the nickel or palladium. This creates a square-planar σ-complex in which the metal is no longer in the oxidation state 0, but in the oxidation state + II.
In the subsequent transmetalation, the nickel or palladium organyl becomes diorganyl through the Grignard compound. The metal is released from the organometallic reagent as a corresponding metal halide.
Now find one cis/trans-Isomerization takes place, which means that the two ligands on the one hand and the two organic radicals on the other hand are on the same side.
The catalysis ends with the actual coupling. It is also called reductive elimination, since the catalyst was regenerated after the two organic residues that were now coupled had escaped, which means that the catalyst metal was reduced from + II to 0 again.
In addition to the good yields, the advantage here is that the practical processes during the synthesis are simplified. The magnesium bromide formed is insoluble in the organic solvents used in these reactions, such as diethyl ether, and therefore precipitates. In principle, you only need to filter off the residue after the reaction and you have the desired product in solution.
The product can then be isolated simply by spinning off the solvent. As always with syntheses in which organometallic reagents play a role, one must bear in mind that such substances are very sensitive to moisture or air. The danger of the decomposition of the organometallic compounds can be avoided in different ways: The organometallic compound and even the Kumada catalyst can be generated in situ, so that one can work in a practically closed system, similar to a Barbier reaction.
Unfortunately, this process is associated with a reduced yield. Another possibility is not only to rely on the "ether cushion" present in the apparatus, but also to work under an inert gas atmosphere. This should already be done during the preparations for the synthesis, i.e. when the substances are weighed in, since the catalyst, especially the nickel catalyst, is very sensitive to oxidation by oxygen.
While the Kumada coupling was developed as early as 1972, a "regulation" in the form of a patent (US 6566572B2)  for the synthesis of 9,10-diphenylanthracene was only made available in 2003, which was made by a Japanese developer group around Kuniaki Okamoto was submitted. I mainly used this patent as a guide when carrying out the synthesis. Unfortunately, the patent has a serious flaw: the solvent used (tetrahydrofuran) is completely unsuitable.
It is usually the case that you first prepare the Grignard reagent and then the substance or the like to be converted. This was also intended here, in that the 9,10-dibromanthracene dissolved in tetrahydrofuran is added dropwise to the Grignard reagent. It still is
9,10-dibromoanthracene is not at all soluble in tetrahydrofuran.Since a suspension is difficult to drip in, especially when the finely crystallized needles are used, I initially tried to follow the patent in such a way that I leave the solvent and thus the suspension unchanged, but instead the suspension of 9,10-dibromoanthracene directly to the site of the reaction.
Unfortunately, the yield was much lower than expected. Just under 16%. In order to find out whether it is due to the in situ generation of the Grignard reagent, I prepared the Grignard reagent separately and transferred it to the place of conversion under protective gas via septa.
Interestingly, the yield remained unchanged. Thus, the Grignard reagent or the in situ generation is ruled out. The catalytic converter, even if it is quite sensitive, cannot actually have been damaged, as I have always handled it under protective gas. The only source of error could now only be the suspension of 9,10-dibromoanthracene, which therefore could not be converted sufficiently. The lack of conversion is particularly easy to understand because after the 9,10-diphenylanthracene has been separated from the reaction mixture by shaking it out with toluene, there is always plenty of 9,10-dibromoanthracene left over. The solution to this problem is that you need a solvent that on the one hand dissolves the 9,10-dibromanthracene well and on the other hand is compatible with the Grignard reagent. This is not very easy as some solvents for 9,10-dibromanthracene react with Grignard reagents. Furthermore, the solubility of the catalyst must not be adversely affected by the solvent. In the end, I decided on three solvent variants that seemed suitable to me:
Namely a mixture of toluene and tetrahydrofuran, triethylamine and tetrahydrofuran and finally toluene alone. A toluene-tetrahydrofuran mixture in a ratio of 1: 1 has proven to be the most suitable solvent. The yields have improved significantly: 65% on average. After the fundamental problem of synthesis had been solved, I was able to continue working in other areas. The catalyst offers a further possibility of variation. Palladium catalysts and generally the catalysts with triphenylphosphine ligands are expensive. Nickel acetylacetonate is a much cheaper but equally effective catalyst. Nickel acetylacetonate can easily be produced from nickel (II) nitrate and acetylacetone. However, it must be ensured that the nickel catalysts are significantly more sensitive to oxidation than the palladium catalysts are already. Working with protective gas is definitely recommended here. Here too, the yield is more than satisfactory.
It moves in the area around 70%.
A somewhat different and admittedly more complex synthesis route is that via anthraquinone instead of 9,10-dibromoanthracene. This is the path I actually wanted to go when I was initially unable to get any information on synthetic routes for 9,10-diphenylanthracene and was therefore forced to develop a synthetic route myself. I therefore took the anthraquinone as a starting material because it seemed to me to be suitable in terms of reactivity and I also had it in sufficient quantities, which was not the case with the 9,10-dibromoanthracene or the anthracene itself.
This synthetic route is also based on a Grignard synthesis. However, with further subsequent steps, some of which are also somewhat problematic, but in principle should lead to success.
First, the anthraquinone is reacted with phenyl magnesium bromide and then hydrolyzed. This gives the first intermediate, 9,10-diphenyl-9,10-dihydroxyanthracene. Then the two hydroxyl groups are reduced and one arrives at
The problem that now arises is that, on the one hand, the reducing agent must be so strong that the hydroxyl groups are completely reduced. On the other hand, the anthracene structure must not be endangered.
The solution to this problem was found after a long period of experimentation:
Iron in glacial acetic acid. Unfortunately, cleaning the product is a bit difficult. Later I was also thankfully informed that this path had already been mentioned in French literature . Unfortunately, there was another crucial problem that emerged before the actual synthesis began.
The anthraquinone was practically insoluble in the solvents commonly used for Grignard syntheses, such as diethyl ether or tetrahydrofuran. Anthraquinone is sparingly soluble in warm benzene. However, as has been shown, the solubility is not really noteworthy, so that it would be inexpedient and negligent to accept a risk to the Grignard compound from constant heating. What is possible, however, is to use a suspension of the educt, even if it is not as convenient for further processing as a solution. A variant of the route via anthraquinone became known to me through a chance find. In a 2000 edition of the Chemical Educator , a Chinese team published a very similar approach.
Only phenyllithium was used instead of the Grignard reagent and the hydroxyl groups were reduced with iodide / hypophosphite instead of iron / acetic acid.
This synthesis route would be a case in which IR spectroscopy could be used particularly well to follow the progress of the synthesis. Since everything takes place in a suspension, it is difficult to pay attention to the failure of an intermediate product or to other indicative changes in the system. Regular sampling and evaluation of the IR spectrograms would make it fairly easy to determine whether the planned conversions have actually occurred. A quantitative statement about the progress of the reaction would be e.g. B. possible via gas chromatography. Despite the lack of control, I was able to achieve a satisfactory yield. The literature speaks of 60%. By working in an inert gas atmosphere and changing the reaction times, I was able to increase the yield by more than 5%. A purity control is particularly easy here via the melting point, but also by thin-layer chromatography, since only the desired end product can be sufficiently excited by UV light. The 9,10-dibromanthracene can be recognized by its own color (canary yellow). The method using anthraquinone is particularly recommended because it is of a rather low degree of difficulty, also in terms of the equipment required. Furthermore, the synthesis itself is extremely profitable. The starting materials, i.e. anthraquinone, lithium and bromobenzene, are very inexpensive. The product, on the other hand, is very expensive. 5 g of 9,10-diphenylanthracene cost well over 100 euros! You certainly have to invest less than 10 euros in the synthesis for this amount of product!
The 9.10 DinI synthesize -butylanthracene exactly like 9,10-diphenylanthracene. I'm just replacing phenyllithium with n-Butyllithium.
That n-Butyllithium, however, I did not produce, as it is already in the form of a 10 molar solution in n-Hexane is available from Aldrich.
I chose this synthesis for the following reason:
It struck me that when you vary luminophores you usually only expand the π system with the substituents.
Substituents with a pronounced + I or –I effect are not always mentioned.
The bromanthracenes used as intermediates, ie aromatics with substituents that exert an –I effect, are not conducive to chemiluminescence. 9.10-Di-n-butylanthracene would be an example of an anthracene with electron-donating substituents. I was able to determine that the + I effect is unfortunately not suitable for chemiluminescence either. Apparently the suitability for chemiluminescence is mainly due to the expansion of the π-electron system. It probably also makes sense to experiment with the inductive effect only after expanding the π-electron system.
The 9,9'-bianthryl can be prepared in various ways. The most practicable method will probably be the Ullmann reaction . Coupling takes place via the halogenated aryl derivative under the action of copper. It is comparable to the Wurtz synthesis. So from z. B. 9-bromoanthracene would arise in the first step anthryl copper, which would be coupled with further 9-bromoanthracene, with the release of copper bromide, to 9,9'-bianthryl. If this reaction was carried out with 9,10-dibromoanthracene, theoretically almost infinite condensed anthracene chains could be produced. But I think that from a certain number of "monomers" the stability becomes less and less, similar to the case of the linear condensation of benzoid aromatics.
Not so long ago it was claimed to have produced a heptacene, but this is now again heavily doubted (Bendikov, M., Wudl, F., Perepichka, D. F., Chem. Rev. 2004, 104, P. 4891).
I decided on a reductive coupling of anthraquinone .
How exactly the mechanism works could not be sufficiently clarified on my part.
I take intermediate levels based on radicals.
Unfortunately, there is a risk that the desired coupling will not occur, but that the anthraquinone will only be reduced to anthracene. Unfortunately, this has also occurred to a significant extent, as can be seen from the thin-layer chromatogram and shown in the very low yield (25%). The increased occurrence of side reactions and the low yield could be an indication of the already suspected radical process.
The procedure for the synthesis of 10,10'-diphenyl-9,9'-bianthryl is the same as for the synthesis of 9,10-diphenylanthracene. This means that 10,10'-dibromo-9,9'-bianthryl is first synthesized by bromination with elemental bromine and then reacted with phenylmagnesium bromide in a Kumada coupling:
2.2.5 trans-9- (2-phenylethenyl) anthracene
For the synthesis of trans-9- (2-phenylethenyl) -anthracene I use the Wittig olefination.
It is easy to implement in terms of preparative requirements and has achieved good yields.
First of all, the process of the Wittig synthesis :
The Wittig synthesis is an addition-elimination reaction.
In order to be able to carry out a Wittig synthesis, the so-called Wittig reagent is required. It can be prepared by reacting a triphenylphosphonium salt with a strong base, where sodium hydride or phenyllithium is usually used. Deprotonation produces the Wittig reagent that can be described by two limit formulas. The first form is based on the carbanion that is formed, a zwitterion (positive charge on phosphorus). In the second form, the lone pair of electrons on the carbon became one
C-P double bond formed. The first mesomer is called ylide because of its salt-like structure, the second mesomer is called ylene because of the double bond.
Now the further reaction between the Wittig reagent (ylid) and a carbonyl compound (aldehyde or ketone) takes place. The ylide can attack with its strongly nucleophilic center, the lone pair of electrons on carbon, but also with the electrophilic center, the positively charged phosphorus. In fact, the reaction takes place in two stages. First, the C-C bond is made through a nucleophilic addition on the positively charged carbonyl carbon. This gives us a zwitterionic intermediate (negative charge in carbonyl oxygen, positive charge still in phosphorus), which is known as betaine. Now an O-P bond takes place, which leads to a heterocyclic four-ring compound, the oxaphosphetane. The bonds in the oxaphosphetane are then cyclically shifted, whereby the target molecule (the alkene) and triphenylphosphine oxide are obtained.
That is the elimination. The reaction scheme using the example of the synthesis to be considered here:
In order to be able to carry out the synthesis successfully, one has to work under anhydrous and ideally also oxygen-free conditions, because the Wittig reagent is quite sensitive to these possible influences.
This must also be taken into account when choosing the solvent. Polar aprotic solvents, such as
N,N-Dimethylformamide (DMF) or dimethyl sulfoxide (DMSO). If these solvents should not suffice, which is a very rare case, one could also resort to hexamethylphosphoric acid triamide (HMPT), which is a really excellent representative of this class. Only the carcinogenicity of the HMPT would stand in the way of its use. As already mentioned at the beginning, the Wittig reagent is produced by deprotonating the phosphonium salt with a strong base. Sodium hydride or phenyllithium are normally used for this purpose . In the case of the particularly well stabilized triphenylphosphonium salts, however, it is also possible to fall back on far less dangerous and therefore easier to handle bases. In this example, the use of concentrated sodium hydroxide solution (50%) was already successful.
The problem with Wittig olefination is that the cis- or that trans-Isomer of the alkene is formed alone, but a mixture of these two is always formed. Although you can choose suitable substituents in the phosphonium z. B. or through the use of lithium salts influence the proportions in a certain way, but this turns out to be quite difficult and cannot be used universally.
How the synthesis under discussion takes place cannot be unequivocally clarified by checking using thin-layer chromatography. To determine whether both isomers are formed, one must use NMR spectroscopy or perhaps X-ray structure analysis. If both forms are detected here, the proportions can possibly be determined directly on the NMR spectrogram or otherwise by gas chromatography.
2.2.6 9,10-bis (phenylethynyl) anthracene
In order to produce the 9,10-bis (phenylethynyl) -anthracene (BPEA), I use the so-called Sonogashira – Hagihara coupling. Here, an aryl halide is coupled with an acetylene derivative using a palladium-copper catalyst and an amine.
The mechanism is very similar to that of the Kumada clutch. The palladium catalyst used also performs exactly the same function. But what role do the copper catalyst and the amine play? These two aids are actually what is special about the Sonogashira – Hagihara coupling. It virtually enables a »Kumada coupling«, but without using sensitive Grignard reagents. The organometallic reagent, in this case a copper arylate, is made available for the duration of the coupling through the catalysis.
To prepare the product considered here, 9,10-dibromoanthracene is coupled with phenylacetylene by means of bis (triphenylphosphine) palladium (II) chloride and copper (I) iodide in triethylamine.
First, the palladium (II) is inserted between the carbon-halogen bond of the 9,10-dibromanthracene (oxidative addition). Then follows copper catalysis.
Since the H atom on the triple bond is acidic, the phenylacetylene can easily be deprotonated by triethylamine. The resulting carbanion attacks the copper (I) iodide in a nucleophilic attack (pN2). You should therefore definitely use the iodide of copper, because iodide is a good nucleofug and the rate-determining step can therefore be positively influenced.
The nucleophilic substitution gives the organometallic reagent necessary for the coupling. The copper phenylacetylide is not particularly stable. During the transmetalation, a cyclic transition state is entered with the palladium and the bromine which is also bound to it.
Here, copper (I) bromide is split off. The iodide present in the solution is in equilibrium with the bromide. Since the iodide is more stable, the bromide is displaced, so that copper (I) iodide is obtained and the copper catalyst is regenerated, making it available to the cycle again. The last two steps are the same as those for the Kumada clutch. So it follows the
cis/trans-Isomerization and ultimately the actual coupling by reductive elimination. Now the palladium catalyst has also been regenerated.
2.2.7 5,6,11,12-tetraphenylnaphthacene (rubrene)
Interesting ways of representing 5,6,11,12-tetraphenylnaphthacene can be found in "Fieser and Fieser" :
1. Moureau et al. published in 1929 that rubrene can be prepared by cyclizing 2 moles of 1-chloro-1,1,3-triphenyl-2-propyne:
The cyclization is brought about by simple heating, which makes the reaction particularly interesting. Unfortunately, due to the lack of original literature, more precise information regarding the reaction conditions could not yet be found.
Furthermore, the production of the educt could cause difficulties. I consider two synthesis routes to be most suitable:
The first possibility would be the conversion of dichlorodiphenylmethane, which is prepared from carbon tetrachloride and benzene by means of Friedel – Crafts alkylation, with phenylacetylene in a Sonogashira – Hagihara coupling analogous to the processes involved in the synthesis of
9,10-bis (phenylethynyl) anthracene:
Production of dichlorodiphenylmethane:
A second possibility, which is equally conceivable and should lead to success, would be the reaction of benzophenone with phenylethynyl magnesium bromide.
The necessary chlorination is then carried out with thionyl chloride:
A completely different synthesis route is based on that of 9,10-diphenylanthracene. One begins with a reaction of naphthacenquinone with phenylmagnesium bromide. It is normally assumed that the Grignard reagent attacks the two carbonyl functions that are present. However, this is not the case with naphthacenequinone.Instead, a so-called Grignard addition takes place at positions 1 and 4.
In general, 1,2-addition is also conceivable, but it is ruled out here because steric effects prevent addition at these positions.
After the obligatory hydrolysis, it is oxidized with oxygen in alcoholic potassium hydroxide solution. The first two phenyl residues at positions 6 and 11 are now integrated. The other two necessary substitutions at C5 and C12, i.e. at the locations of the carbonyl groups, are made with phenyllithium. That is to say in the same way as for the preparation of 9,10-diphenylanthracene.
After hydrolysis, the hydroxyl groups formed are reduced with sodium phosphinate / potassium iodide in glacial acetic acid.
The difficulty with this process lies in the procurement of the starting material (naphthacenequinone). It is commercially available, but quite expensive (2.5 g € 45 from Acros Organics). The production of the same is recommended.
According to an Asian chemistry forum, this is achieved from phthalic anhydride and naphthalene, which initially react to form α-naphthoylbenzoic acid, which is then rearranged into β-naphthoylbenzoic acid.
Finally, the ring closes with condensation to form naphthacenquinone:
Sodium chloride and aluminum (III) chloride are said to serve as catalysts.
If this reaction really proceeds in the desired direction and with a correspondingly good yield, this would be an extremely interesting possibility of subsequently synthesizing rubren, which is also expensive, on a larger scale at a tolerable price.Details Christopher Lebeau Published: September 10th, 2016 Last updated: November 6th, 2016 Created: September 10th, 2016 Hits: 2844
2016 ETP1-2 i - laboratory
Minutes (surname, first name): Oesten, Lili Exercise day: 29.04.
Other participants in the exercise: Beyerstedt, Philip Nussbaum, Finn Ole Professor: Prof. Dr. Haase
In the first part of this laboratory exercise, the non-linear I-U characteristic curve of an incandescent lamp should be examined
calculated and measured. The second part deals with one
Bridge circuit and its adjustment characteristic. The characteristics are point-by-point theoretical
and to be determined by measurement and represented graphically.
- Components with non-linear I-U characteristics
- DC resistance, differential resistance
- Representation of measurement results in linear and logarithmic scaling
- linear two-pole equivalent circuit of a non-linear component theory of the
Bridge circuit, bridge equation
I-U characteristics of an incandescent lamp. 3
1.1 calculation. 3
1.1.1 Calculated values. 3
1.1.2 Characteristic curve diagram f (U) = I. 3
1.1.3 Determination of parameters. 4th
1.2 measurements. 5
1.2.1 Measured values. 5
1.2.1 Characteristic diagram. 6th
1.2.2 DC resistance and differential resistance. 6th
1.2.3 Comparison of the measured and calculated values in a double logarithmic diagram. 7th
1.2.4 Determining the best-fit straight line. 8th
1.3 Evaluation. 8th
Bridge circuit. 9
2.1 Calculating the bridge voltage as a function of R1. 9
2.1.2 Determination of the value of 푅 1 at which the bridge voltage 푈 푎푏 = 0 V.
2.2 measurements. 11
2.2.1 Measuring the resistance 푅 1 at 푈 푎푏 = 0 푉. 11
2.2.2 Measuring the bridge voltage as a function of R1. 12th
1.1.3 Determination of parameters
If the characteristic curve calculated / measured above is set on a double-logarithmic scale
represents a straight line. From this, parameters a and b can be calculated using the following calculation
By taking the logarithm of the original formula +, * = 훼 ∗ / 0
1, the formula results
This formula corresponds to the general straight line equation (y = c + m * x).
In the above formula:
It follows that the parameter b (the original formula) is the slope of the characteristic in the
corresponds to double logarithmic representation. The slope can be set using a slope triangle
to be determined. The parameter c corresponds to the value at the point U = 1V:
log 56 +, * = log 56 푎 + 푏 ∗ log 56500
1. 2 measurements
In order to display the characteristic curve by means of a measurement, a simultaneous current and
Voltage measurement carried out in order to determine the characteristic curve point by point. The following
Structure is to be used:
The correct voltage is measured, so the current measurements are subject to larger ones
1.2.1 Measured values
The measured voltages and currents are shown in Table 1.1.1:
U in V 0.01 0.03 0.05 0.07 0.09 0.5
I in mA 1.9259 5.324 8.474 11.153 13.303 26, U in V 1.0 1.5 2.0 2.5 3.0 3.5
I in mA 37.29 46.13 54.01 61.01 67.55 73, U in V 4.0 4.5 5.0 5.5 6.0
I in mA 79.32 84.63 89.76 94.62 99, table 1.1.1
To determine the differential resistance, the U-I characteristic curve is the tangent
the respective voltage values. On the slope of the tangent, the
Read differential resistance. (Tangents see appendix on page 14)
DC resistance 18.82 Ω 37.04 Ω 55.70 Ω
Differential resistance 45.83 Ω 57.14 Ω 100 Ω
1.2.3 Comparison of the measured and calculated values in a double
It is also noticeable in this illustration that larger currents and voltages are used for small currents and voltages
There are deviations. This is correct in larger voltage / current ranges
theoretical formula relatively good.
1.2.4 Determining the best-fit straight line
In a double-logarithmic representation, the following best-fit straight line for the
create measured values:
From this, as described in Exercise 1.2.3, the parameters a and b can be determined
(For graphical determination, see Appendix on page 15): a = 39 and b = 0.41 / 0.71 = 0.58.
The evaluation refers to the question: “From which currents upwards does the
Incandescent lamp approximately linear? ".
From a current of 60 mA, the characteristic curve is almost a straight line. Thus behaves the
Incandescent lamp from 60 mA almost linear.
To determine the equivalent voltage source, the linear part is represented by a straight line
approached. The resistance results from the slope of this straight line (diagram see
Appendix p. 15).
The values from Table 2.1.1 are plotted in Figure 2.1.1:
2.1.2 Determination of the value of 푅 5 at which the bridge voltage 푈 K1 = 0 V
From the calibration condition of a Wheatstone measuring bridge follows:
If you insert the given values, you get:
It follows that the bridge is balanced when 푅 5 is one kiloohm.
2.2.1 Measuring the resistance 푅 5 at 푈 K1 = 0 푉
Now the calculated values are compared via a measurement. Resistor R1 becomes
Represented over a decade resistance and changed until the bridge voltage equals zero
will. The measurement setup corresponds to the circuit diagram from “2. Bridge circuit ".
If the bridge voltage is zero, remove the decade resistor from the circuit
and measures its resistance with an ohmmeter.
The measured and calculated value are now compared:
The measured value and the theoretical value hardly differ from each other, the small one
Deviation can be determined with the tolerances of the resistors and the measurement inaccuracies
Metrahit 18s place
Metrahit 15s 3rd place
2 resistor 10k place 3
100/1000 Ohm resistance 3rd place
2016 ETP1-1 ii - laboratory
Due to the voltage divider rule, the internal resistance and the potentiometer resistance are then the same:
푅퐿 + 푅푖 ∗ 푈푞 푚 푖푡 푅퐿 = 푅푖 → 푈퐿 =
2 ∗ 푅퐿 ∗ 푈푞 =
The internal resistance of the multimeter does not have to be taken into account, as this is very high when measuring the voltage and these are connected in parallel:
Thus the voltage drop across this parallel connection is identical to the voltage drop across RL. Table 1.2 shows the measured resistance values and the possible deviations:
Measuring device resistance in Ω nominal deviation absolute deviation in Ω
Tenma 104.9 ± 2% + 3 D 2,
MetraHit 15S 105.5 ± 0.5% + 3 D 0,
MetraHit 18S 105.52 ± 0.1% + 30 D 0,
2 voltage dividers
At the following circuit, 8 V terminal voltage may be applied to A and B:
First, the partial voltages are calculated theoretically with the help of the voltage divider rule, where the following applies:
푈 퐶푛 - 퐶푚 =
푅 퐶푛 - 퐶푚
푅푔 푒푠 ∗ 푈 푚 푖푡 푛 = 1,2,3,4,5 푢 푛푑 푚 = 2,3,4,5,
푅푔 푒푠 = 푅 1 + 푅 2 + 푅 3 + 푅 4 + 푅 5 = 100 Ω + 100 Ω + 200 Ω + 200 Ω + 400 Ω = 1 푘 Ω
The calculated values and the theoretically possible measured values are given in table 2:
C1-C2 C2-C3 C3-C4 C4-C5 C5-C calculated 0.8000 V 0.8000 V 1.6000 V 1.6000 V 3.200 V nom. Deviation 0.05% + 3D 0.05% + 3D 0.05% + 3D 0.05% + 3D 0.05% + 3D abs. Deviation 0.0007 V 0.0007 V 0.0011 V 0.0011 V 0.005 V measured 0.8041 V 0.8008 V 1.5969 V 1.6011 V 3.195 V actual. Deviation 0.0041 V 0.0008 V -0.0031 V 0.0011 V -0.005 V C1-C3 C2-C4 C3-C5 C4-C calculated 1.6000 V 2.4000 V 3.200 V 4.800 V nominal. Deviation 0.05% + 3D 0.05% + 3D 0.05% + 3D 0.05% + 3D abs. Deviation 0.00 11 V 0.0015 V 0.005 V 0.005 V measured 1.6050 V 2.3975 V 3.197 V 4.796 V actual. Deviation 0.0050 V -0.0025 V -0.003 V -0.004 V C1-C4 C2-C5 C3-C calculated 3.200 V 4.000 V 6.400 V nominal. Deviation 0.05% + 3D 0.05% + 3D 0.05% + 3D abs. Deviation 0.005 V 0.005 V 0.006 V measured 3.201 V 3.998 V 6.393 V actual. Deviation 0.001 V -0.002 V -0.007 V C1-C5 C2-C calculated 4.800 V 7.200 V nominal. Deviation 0.05% + 3D 0.05% + 3D absolute Deviation 0.005 V 0.007 V measured 4.802 V 7.192 V actual. Deviation 0.002 V -0.008 V Table 2
8.0 V is applied to input terminals A and B using the HM7042-5 power supply unit. The voltage values measured with the MetraHit 18S are entered in table 2.
Using the data in Table 2, it can be determined that half of the measured values are in the range of the measuring tolerance of the measuring devices (marked in green). The other half of the values are outside the tolerance range (marked in red).
The internal resistances calculated in this way are listed in Table 3.2:
Internal resistance meter calculated
Tenma 6.6 Ω
MetraHit 15S 15.9 Ω
MetraHit 18S 1.15 Ω Table 3.
The clear deviations in the accuracy of the three measuring devices can be explained by the different internal resistances. An ideal ammeter has an internal resistance of R = 0 Ω. The greater the actual internal resistance, the greater the deviation of the measured values.
It can be seen that the MetraHit 15S is only conditionally suitable for exact current measurement due to an internal resistance of approximately 16Ω. The Tenma is more suitable, but it also leads to inaccurate measurement results. The MetraHit 18S has the lowest internal resistance of the available measuring devices and is therefore best suited for current measurement.
4 flow dividers
With the HM7042-5 power supply unit, 5.0 V is applied to input terminals A and B of the following experiment:
Theoretically, the currents between the individual terminal pairs result from the current divider rule:
Laboratory primer. Biology internship. Chemistry internship. for that. and that
2 Table of contents: General section: Safety in the laboratory: Page 2 What to do in the event of fire and accidents: Page 2 Handling chemicals: Page 3 Laboratory equipment: Page 4 Working technology: Page 6 Frequently used equipment: Page 8 Units of measurement: Page 11 Biology: Rules in biology internship: Page 12 Internship preparation: Page 13 Internship reports Biology: Page 14 Periodic table and hazard symbols Middle sheet Correct information on literature sources Page 16 Correct labeling of tables and images Page 17 Procedure for microscopy: Page 18 Pipetting with micropipettes: Page 19 Project work / Matura work: Page 21 Chemistry: Rules in the chemistry internship: page 22 Evaluation of the laboratory: page 23 Experiments and test execution: page 24 What is a poison? Page 25
3 Dear pupil In the 3rd semester (2nd year, 1st semester) and in the 6th semester (3rd year, 2nd semester) the internships take place in biology and chemistry. They take place alternately every two weeks in half-classes during a double lesson in the laboratories and are part of the compulsory lessons. In this laboratory guide you will find useful tips and information on working in the internship rooms. Further information supplements the primer in a small reference booklet that you should have with you in every internship. Before the first internship you should have read through the following pages: Biology: Pages 2/12/13/14/15 Chemistry: Pages 2/3/22/23 /
4 Safety in the laboratory: There are dangers lurking in the laboratory. Experience has shown that these are mainly everyday dangers, such as the risk of getting burned or cut. But there are also very special dangers that only exist in the laboratory. In the course of time, some rules of conduct have therefore turned out to be useful. For safety and order while working in the laboratory you will find: Rules for the biology internship: page 12 Rules for the chemistry internship: page 22 What to do in the event of fire and accidents: 1. Report a fire to the internship manager immediately and follow his instructions. 2. If a fire breaks out, all flammable chemicals must be removed quickly and the main supply lines for gas, electricity and water must be interrupted. Make a note of the locations of the fire extinguishers. Important: Never extinguish with water in the chemistry laboratory. 3. Injuries of any kind are to be reported to the internship manager immediately. 4. Rinse eye injuries immediately with plenty of water (eye shower). 5. In the event of burns, immediately immerse the relevant part of the body in ice-cold water for at least 30 minutes. 6. Treat minor accidents (e.g. cuts, etc.) with the first aid kit. Emergency numbers: Fire brigade: Sanitary:
5 Handling chemicals: 1. There are poisonous and dangerous substances in the laboratory. These are marked. The substances are provided with hazard symbols. In addition, hazard warnings (R-phrases) and safety warnings (S-phrases) can appear on the packaging. R and S sentences are usually not on our small, filled bottles for reasons of space. There is also a safety data sheet with detailed safety instructions for every substance used. 2. Always hold the supply bottles with the label against the palm. Put the clasp upside down in front of you. Never twist the ground-joint stoppers! Never point container openings at people. (Not even against yourself!) Close the bottles immediately. 3. Remove solids from the bottles with the spatula. Pour liquids directly into the measuring cylinder or use a small funnel. 4. Strictly adhere to the specified quantities. Only take the required amount. Never pour chemical residues back into the storage bottle. 5. Never pipette by mouth, always use a suction ball or a pipetting aid. 6. Store chemicals only in clearly labeled containers! Always write on vessels, even if it is only for a few minutes. 7. Never taste chemicals! The smell can only be determined by shuffling your hand! But only if this is expressly requested. 8. Flammable chemicals (e.g. organic solvents) must not be stored near open flames. 9. Wash off chemical splashes on skin immediately with plenty of water and call the teacher or assistant. Do not wipe up spilled chemicals unless instructed to do so. 10. Work with smelling and / or poisonous substances under the fume cupboard (chapel) is only allowed following the instructions of the teacher (switch on the ventilation !!). This also applies if toxic fumes are produced during the experiment. 11. Working with explosive compounds is strictly forbidden
8 Reading a liquid volume: Working technique: Liquids form either a downward (concave) or upward (convex) curved surface. This is known as the meniscus. The volume is read off at the deepest point of the liquid surface for the concave meniscus and at the highest point for the convex meniscus. Measuring cylinder concave convex When reading, the following must be observed: Hold the vessel vertically. The liquid surface must be at eye level.The smaller the cross-section of the vessel, the greater the reading accuracy. Pipetting: Liquids are either removed with the pipette or poured directly into the measuring cylinder. Never pipette by mouth (risk of contamination !!). Always use a peleus ball or pipette aid. There are different types of pipettes: Pasteur pipette (dropper pipette): Volume: 20 drops correspond to approx. 1 ml. Graduated pipette (rod pipette): Graduated pipette for measuring variable amounts of liquid. Letting the liquid run off drop by drop is also easily feasible. Volumetric pipette: Pipette for measuring a certain, fixed amount of liquid. Greater accuracy than with a pipette! Automatic micropipettes are described in detail in the biology section on page 20
9 Pipetting procedure: 1. The peleus ball is placed on the upper end of the pipette. Make sure that the pipette does not break off when you put it on! 2. To push air out of Peleusball, the top valve is pressed at the same time. 3. Immerse the pipette in the withdrawal vessel. Immerse as deeply as possible so that air is not suddenly drawn up. 4. Suck in the liquid by pressing the middle ball valve. The liquid level must be sucked about 2 cm above the calibration mark. Caution: never suck liquid into the peleus ball! 5. Use the side ball valve to drain the liquid up to the mark. 6. Drain the liquid into the target vessel, keeping it at a 45 - angle. The pipette tip and the wall of the target vessel must touch each other. 7. The pipette must never be immersed in the liquid. 8. When the liquid has run out, wait about 15 seconds so that residues can run on the pipette wall. 9. There is usually some liquid left inside the pipette. This has to be the case, since pipettes are calibrated for the outlet. The remainder must under no circumstances be blown into the target vessel. Heating liquids in the test tube / delayed boiling Liquids can be heated above the boiling point without starting to boil. When shaken, the boiling starts abruptly, a large part of the liquid evaporates in one fell swoop and increases its volume by a factor of approx. 1000! This leads to a real explosion, the liquid can splash around dangerously or the glass vessel can shatter. One speaks of a boiling delay. Accidents caused by delayed boiling can be avoided if the following points are observed: Test tubes (RG) no more than a third full. Add a boiling stone Reduce or stop the supply of heat from boiling (keep RG out of the gas burner flame). Always avoid opening RG with boiling or just heated liquids from people! - 7 -
10 Frequently used equipment: The Bunsen burner: In many chemical experiments a heat source is required. For this purpose, a gas burner (Bunsen burner) is usually used, in which natural gas (mainly contains ethane CH 4) is burned. Working with the Bunsen burner is not entirely safe, because unburned gas that escapes can form an explosive mixture with air. It is therefore important to understand the structure and use of a Bunsen burner. Igniting the Bunsen burner: 1. Connect the Bunsen burner to the gas tap on the laboratory bench with the air and gas supply closed. 2. Open the gas tap on the table. 3. Light a match, open the gas supply on the burner and insert the match from below into the gas flow. 4. The burner now shows a yellow, glowing flame. Luminous Bunsen burner flame (yellow): When the air supply is closed, the gas does not burn completely to form water and carbon dioxide. Soot particles form, which glow yellow when glowing. 5. Now regulate the air supply until a bluish, rustling flame arises. Noisy Bunsen burner flame (blue): When the air supply is open, the gas burns practically completely. In the inner flame cone temperatures up to approx. 500 C, in the outer flame cone up to approx
11 Scales: Analytical scales The analytical scales in the weighing room cost several thousand francs each. They are suitable for weighing up small and very small amounts of material. The accuracy of the devices is ± 0.1 mg. They should only be used in experiments where this level of accuracy is required. Analytical scales are very sensitive to vibrations and are therefore mounted on special weighing tables. Pound scales Scales, which are commonly referred to as pound scales in chemists' slang, have an accuracy of ± 10 mg. They are suitable for weighing larger amounts of substance. The following always applies to all scales: Chemicals must never be placed on the weighing pan without a container or weighing paper
12 Vernier LabPro-Interface: The Vernier LabPro-Interface is a versatile data conversion device that enables data to be collected with various sensors and displayed and evaluated on the computer (or TI computer). Components: Interface device, transformer, power connection cable, LabPro USB cable Connect and set up: 1. Plug the power connection cable into the transformer. 2. Connect the transformer to the Interface AC adapter port. 3. Connect sensors to channels 1-4. 4. When all components (without the laptop) are connected to one another, the power connection cable can be connected to the mains plug. The interface does a self-test (ringtone). 5. Start the laptop. 6. Connect the interface with the USB cable to the operational laptop (upper slot). The slot for the USB cable is on the right side of the device and is marked with the USB symbol. The serial slot next to it is sealed. 7. Double-click the LoggerPro program icon on the computer screen. The program recognizes the connected sensors and creates graphic and numerical evaluation tables with basic settings for the X and Y axes. 8. Depending on the sensors used, continue working according to the teacher's instructions
13 units of measure: The following units of measure are used in the laboratories: kg kilogram 10 3 gg gram mg milligram 10-3 g & microg microgram 10-6 g ng nanogram 10-9 gl liter ml milliliter & microl microliter bp basepairs (base pairs) kb kilobase pairs D Daltons definition : The dalton is another name for the atomic mass unit, thus exactly equal to 1/12 of the mass of an atom of 12 C and roughly corresponds to the mass of a hydrogen atom (1. kg). m Meter Definition: The meter is defined as the distance that light travels in a vacuum in a time of 1 / second. & Aring Angstr & oumlm Definition: The & Aringngstr & oumlm is a unit of length named after the Swedish physicist Anders Jonas & Aringngstr & oumlm. 1 & Aring = 100 pm = 10-1 nm = 10-4 & mum = 10-7 mm = m% -Dilutions / concentrations: g / 100mlg / v (weight in volume) ml / 100ml V / V (volume in volume) g / 100g G / G (weight in weight) ppm mol parts per million gram molecular mass 1mol is the amount of substance in a portion that contains 6 x particles Molar mol / l Grammol in 1 liter solution Molal mol / kg 1 mol in 1000g solvent
14 rules in the biology internship: Every student works during the entire semester at the same workplace assigned to him at the beginning. Coats and jackets are to be hung outside in the cloakroom. School gaps are to be deposited under the work desks, not in the aisles between the desks. Eating and drinking are prohibited in the internship room. Sitting on the workbench is prohibited. Portable music players are switched off and removed. Cell phones are turned off. The dishes used in the internship are washed clean and dried by the dishwashers themselves. The workplace is to be left as tidy and clean as you found it. Wash your hands often. Access to the adjoining rooms through the intermediate doors is only permitted with the permission of the teacher. The material box must be checked for completeness at the beginning of the internship. If something is missing, report to the teacher or assistant. At the end of the internship, the material box is checked again and confirmed with the signature on the yellow card
15 Internship preparation: In preparation for the internship, you should work on the internship instructions at home. The processing should be done in such a way that you can see it. Therefore you have to underline it completely with pencil when reading. At the same time, you mark the most important facts with a light pen. During the internship, the instructions are checked and approved by the teacher. If you do not have a completed internship manual, a grade will be deducted from the respective report grading. The internship preparation should enable a positive learning experience in the biology internship
16 Internship reports Biology: a) Structure Title Date, authors, school, class 1. Theory 2. Aims I. II. III. The goals can be taken directly from the internship instructions. Additional goals can be formulated. Cut out and glue in is also allowed. 3. Material Material lists are to be added. 4. Work orders / test execution The work orders can also be taken from the instructions. Exceptions are deviations, these must also be written down. 5. Results (work log) The tables from the work orders can be glued in for the work log. Additional prepared tables must be added. Drawings, figures and tables are individually labeled (tables above, figures below, see laboratory manual on page 17). In the case of self-made illustrations (drawings), the date, place, author and, if necessary, the enlargement factor are added to the declaration. Drawings must be glued in, even with computer-generated reports. In the results, the results obtained are factually presented without explanations
17 6. Evaluation of results Averages, diagrams, graphics, simplified representations of the results, without attempting to explain. 7. Interpretations This is where the explanations come into play. How can the results be justified? 8. Summary / Conclusion 9. For references, see laboratory primer: page 16. b) Management of the internship reports - entry structure is always the same - no diary! - Work steps must be comprehensible - Findings should be noted - Objective, not emotional - By hand or with a computer c) Examination of an internship report It is worked in groups of two. The first three internship reports are corrected by the teacher. In the 5th internship, the creation of a report is checked and graded during the double lesson. d) The content of the internship is part of the examination material. e) Internship instructions and sample report All internship instructions can be found on the school network at: from the teacher / biology / internship instructions or on the bio homepage. You can use the documents if you are writing the report on the computer. You can also find a sample report on the school network: from the teacher / biology / internship instructions / sample report
18 Correct references to literature sources: References are given consecutively as they appear in the document, numbered with small, superscripted numbers. Example: 3) Books: are given in the following order: Author / s: Last name, first name abbreviated to the first letter. If there are several authors, they are all mentioned and separated by /. If there are more than 3 authors, only the main author is mentioned with the addition among others (= and others, Latin: et al.) Year of publication: Year in brackets () Book title: printed in italics Publisher: Abbreviations e.g. dtv are not permitted. Place of publication: Name of the city without information about the country. In the case of original quotes, the edition and the exact page number of the book are also given here. Example: source for a book content 1) M & uumlller, B./Hofer, M. (2005) The storm in a glass of water. Goldmann, M & uumlnchen Example: citation of source for an original quotation 2) Rieder, T. (2007) The spider on the Christmas tree. Thieme, Hanover. 2nd edition S Journals: Instead of the book title, the title of the article appears in italics, followed by the name of the journal with the issue number and page numbers. The publisher is usually not mentioned here. Example: 3) Muralt, S. (2008) The dynamic of forgetting. Psychologie heute no. 287, S Internet sources: Just mentioning the homepage is not enough. The entire link to the page from which information was taken is required. Example: inadequate. 4) correct example: 4) -
19 Correct labeling of tables and images: Graphics, drawings and photos are summarized under the term "images". They are labeled below the picture and numbered consecutively, whereby the word figure is abbreviated. Fig. 2. In the case of microscopic drawings and photos, the date, place, author and magnification factor are also given. Tables are always labeled and numbered at the top, whereby the word table can also be abbreviated to tab. Correct examples: Fig. 17: Two chicken eggs Fig. 18: Change in weight of the eggs in different solutions Table 5: Results of the egg weights, measured after specified times: Fig. 19: Onion cells, microscopic pencil drawing by S. M & uumlller Wil, X
20 Procedure for microscopy: 1. Put the dust cover in the table drawer. Switch on the lighting, adjust the eyepieces to the interpupillary distance. Check the diopter adjustment. 2. Clamp the specimen slide on the specimen table. 3. With the smallest (4x) lens, raise the table with the coarse drive until the object appears in the field of view. 4. Set as sharp as possible with the fine adjustment, regulate light intensity, regulate light scattering (depth of field) with the condenser diaphragm. 5. Search the object for a suitable location and position it in the center of the field of view. 6. Turn the revolver to the next (10x) objective, only correct the sharpness with the fine adjustment. 7. Same step for the 40x objective, focus may only be adjusted with the fine adjustment, DANGER OF BREAKAGE. 8. The 100x objective (& Oumll) must NOT be used! (The teacher will give precise instructions on the occasion) - Change the slide only with the smallest lens. - The 40x objective must not be used for special microscope slides, RISK OF BREAKAGE. - Slides with a bevel (for amberbites) are twice as thick as normal microscope slides and scratch the lens of the 40x objective, examine amphibians only with 4x and 10x objectives. After using the microscope: 1. Set the weakest objective. 2. Screw the specimen down completely. 3. Remove the specimen slide with the specimen from the specimen table. 4. Switch off the lighting. 5. Cover the microscope with the hood
21 Pipetting with micropipettes: General remarks Never immerse the pipette in a solution without the pipette tips! Never use the same pipette tip for different solutions! INITIAL OPERATION Working position of the pipette Place the finger supports (D) on the third phalanx of the index finger. With a slight movement of the thumb, the push button (B) and tip ejection (C) can be activated. Setting the volume The volume setting for variable models is carried out by turning the push button (B) until the required volume appears in the digital display (E) (turning clockwise reduces the volume and vice versa). Sensitive click stops on the micrometer screw and the freely rotating smartie push-button cap (A) prevent unwanted adjustments during pipetting processes. Note: When the letter E lights up next to the numbers in the display, the selected volume is no longer in the working range of the pipette. Overturning the micrometer screw can damage the mechanism. Socorexpipettes: & mul orange pipettes (like Fig. 1 left) & mul blue pipettes (like Fig. 1 left) ml red pipettes (like Fig. 1 right) 2 20 µm green Bio-Rad pipettes, slightly different shape, same principle and same function Pipetting: Aliquoting: Transferring a certain volume from a larger volume into a new vessel. Dividing a volume into a certain number of smaller volumes
22 Normal pipetting process The precisely set volume is sucked in and then dispensed. Phase 1 Press the control head to the first stop (end of the calibrated working stroke). Phase 2 Dip the tip vertically approx. 2-3 mm deep and slowly release the button. Wait 2 seconds, remove the pipette and briefly wipe the filled tip vertically on the container wall. Phase 3 Place the tip on the wall of the second container, slowly press the actuation button as far as the first stop to expel the liquid. Phase 4 Press the confirmation button to the second stop. The air volume conveyed by the overstroke blows the last remaining debris out of the tip. Tip ejection: Eject the used tip by pressing the ejection button (C). Put on a new tip if necessary. Reverse pipetting process Excess volume is sucked in, but only the set volume is dispensed. Phase 1 Press the control button up to the overstroke (second stop). Phase 2 Dip the tip vertically approx. 2-3 mm deep and slowly release the button. Wait 2 seconds, remove the pipette and briefly wipe the filled tip vertically on the container wall. Phase 3 Place the tip on the wall of the second container and only press the button as far as the first stop to dispense the exact amount of liquid that has been set.Remove phase 4 pipette from the second container and repeat phase 2. Blow out remaining material by pressing the button as far as the second stop (overstroke). Tip ejection: Eject the used tip by pressing the ejection button (C). Put on a new tip if necessary
23 Project work / Matura work: If students or groups of pupils need to carry out their experiments in school in connection with project or Matura work, various services can be offered within the scope of the possibilities of the student body. Conditions: The planned experiments with a brief description, schedule and material order list must be reported to the assistant at least 14 days (for project work at least 2 working days) before the start of the experiment. The same rules of conduct and safety must be observed in the laboratories and group rooms as they apply to the regular internship. The pupils are assigned a workplace in a group room, where the material and possibly equipment are provided and where the experiments have to be carried out. Access to these workplaces is only possible after consultation with the assistant. The material order list must be set up as completely as possible, divided into three areas: see form! 1. Chemicals and reagents: with quantities - reagents with concentration, e.g. 500 ml ethanol 70%, - chem. Substances with formula + purity e.g. 7g calcium chloride CaCl 2 pure - biological material e.g. 200g plantain leaves, dried 2. Glassware and laboratory utensils: with information on size and number of pieces, e.g. 2 Erlenmeyer flasks 200ml, 5 graduated pipettes 10ml, 2 powder spatulas 3. Apparatus and devices: e.g. Magnetic teachers, centrifuges, thermostats, etc. The list of materials is approved by the supervising teacher. According to the list, all material is to be returned to the assistant in its entirety and cleaned at the agreed time. The students are only relieved when the assistant has approved the return
24 rules for the chemistry internship: 1. Only enter the chemistry laboratory in the presence of the teacher. Coats, jackets, folders, rucksacks and similar stumbling blocks are deposited outside the laboratory. 2. Food (including chewing gum) and drinks do not belong in the laboratory. 3. Know the locations of fire extinguishers, fire blankets, emergency showers and eye showers. 4. The chemical assistant provides all required glassware and chemicals in special boxes. 5. Always wear protective goggles when someone is working with chemicals in the room. 6. Protect clothes with a laboratory coat or an old shirt made of cotton. 7. Please tie up long hair at the back. 8. Keep order and cleanliness. 9. After completion of the experiments: Dispose of chemical residues correctly. Wash all glassware with tap water and place in the box provided. Clean the workplace. 10. Schoolchildren have no access to the material and chemical store. 11. Wash hands before leaving the laboratory. 12. The laboratory is not a playground: please no water fights and races!
25 Evaluation of the laboratories: The chemistry laboratory is part of the chemistry class. Two school weeks in front of the laboratory laboratory instructions are available. The instructions must be read through until the internship. The laboratory material is a supplement to the theoretical material. The head of the laboratory instructions indicates in which chapter of the theory the laboratory material is to be classified. The laboratory instructions sometimes contain their own theoretical part. This is to be worked through to the laboratory lesson. The laboratory instructions usually contain preparatory questions. These are to be worked out and answered at the laboratory lesson (fill in the pre-printed boxes): The laboratory instructions contain practical tasks. These are to be carried out in the laboratory lesson. Test arrangements, implementation, observations and interpretations are to be entered in the measurement protocols or laboratory journals provided for this purpose
26 Experiments and implementation of the experiment: Study the instructions carefully before starting the experiment. Experimentation may only be started when the entire workflow is clear and the purpose of the experiment has been understood. If anything is unclear, be sure to ask and never act on your own. Experiments may only be carried out on experiment tables, as other surfaces can be damaged by chemicals. Before the actual experimentation, all the necessary equipment, chemicals and aids are made available at the laboratory. Work with clean and dry equipment. Set up devices with sufficient distance from the edge of the table. Always handle chemicals, glassware and equipment carefully and in an upright position. Never bring your face or hair too close to the gas burner flame. Work carefully and deliberately. Think not only of yourself, but also of your classmates! Improperly damaged material will be invoiced. Utensils that are no longer required are pre-rinsed and collected in a special tub or cleaned at the end of a lesson as instructed by the internship leader. Experiment tables and scales must always be kept clean. Spilled substances are to be picked up immediately. Only wipe up dangerous substances under the guidance of the internship leader. Please deposit spatulas and pipettes belonging to a specific bottle directly next to the bottle. Burning Bunsen burners, switched on heating plates, reactive mixtures etc. must not be left unattended for a second. At the end of the hour, close all the gas cocks
Commented sample protocol for the experiment. g-determination with the help of free fall and Atwood's falling machine
1 Physics Basics Laboratory Annotated sample protocol for the experiment of g-determination with the help of free fall and the Atwood drop machine Sophie Kr & oumlger and Andreas Bartelt summer semester 2017 lecturer. Course of study. Group. Weekday. Trial carried out on:
Comment 2: Deliberately falsifying data or copying data from other laboratory groups violates the Code of Good Scientific Practice. This is a fraud. In the event of a violation, the laboratory must be repeated. 1. Objective In this experiment, the gravitational acceleration g is to be determined with two different fall experiments, an experimental setup for free fall and an Atwood's falling machine, and the measurement accuracy of the two experiments is to be compared. 2. Measurements 2.1. Free fall In the experiment, a steel ball was dropped. An electromagnet triggered the falling movement. At the end of the adjustable fall distance there was a detector that registered the impact of the steel ball 1. The fall time 2 t of the steel ball was measured as a function of the fall distance s covered. In doing so, it was not the total distance s but the displacement & Deltax that was set 3: s = s 0 + & Deltax (1) The initial position s 0 (offset) corresponds to & Deltax = 0 and was initially not known. Measuring equipment: The value of the displacement & Deltax was read off using a steel ruler. The time was measured with an electronic stop watch. The electromagnet provided the start signal and the detector the stop signal. Systematic errors and random errors in position and time measurement are neglected in the case of linear regression analysis. No lengthy treatises or repetitions of what was presented in the laboratory instructions. Comment 2: All physical sizes and symbols must be defined in the text and used consistently. Physical symbols are written in italics and their units are not written in italics. 3 Comment: All equations referred to in the text must be numbered consecutively. 4 Comment: For many evaluations, the random and systematic errors of the location and time measurement must be determined. If the measured value goes directly into an evaluation, the accidental error would be u z = 1 mm as reading error of the steel rule u z = 1 mm and as reading error of the stopwatch u z = 1 ms. If the analysis is carried out by averaging, the random errors result from the standard deviations. The systematic error of the position measurement is u s = 0.05 mm L (L: measured length). The systematic error of the time measurement is u s = 1 ms. 2
3 of the displacements & Deltax i and the associated time spans ti between the start and stop signal are listed in Table 1. 5. Table 1: Fall duration t as a function of the displacement & Deltax in free fall x / cc 0.0 5.0 10.0 15, 0 20.0 25.0 30.0 35.0 40.0 45.0 50.0 55, t / mm Atwood's falling machine In Atwood's falling machine, the masses m 1 + m 2 are on a cord and rollers with the mass m 3 connected 6. The masses m 1 and m 2 are the same. As in the free fall attempt, the running time was measured as a function of the adjustable distance with a stop watch. The electromagnet and the positionable light barrier provided the start and stop signals. The total distance covered s can be set by shifting the position of the light barrier by & Deltax: s = s 0 + & Deltax The initial position s 0 (offset) corresponds to & Deltax = 0 and was initially not known. Measuring equipment: The displacements & Deltax i were set using a steel rule. The measurement of the time spans t i, which the masses need to cover the various distances, was carried out with an electronic stop watch. The masses m 1 and m 2 were measured with a precision balance. The following variables were measured: Large masses m 1 = m 3 = 750.0 g reading error uz = 0.1 g systematic error us = 0.1 g total error ug (m 1) = uz + us = 0.2 g measurement result m 1 = (750.0 & plusmn 0.2) g small mass m 2 = 120.5 g reading error uz = 0.1 g systematic error us = 0.1 g total error ug (m 2) = uz + us = 0.2 g Measurement result m 2 = (120.5 & plusmn 0.2) g 5 Comment: Each table should have a table heading and reference should be made to each table in the text. The data in the table should also be presented as a graph. In the case of longer series of measurements, the measurement data should not be listed in the log for reasons of better readability. Then a graphic representation of the measured values and a reference to the measurement protocol or the attached Excel data sheet are sufficient. 6 Comment: If necessary, a sketch can replace or supplement this text. 3
4 The positions of the light barrier & Deltax i and the associated time spans t i between the start and stop signal are listed in Table 2. Systematic errors and reading errors (random errors) of the position and time measurement are neglected in the case of the linear regression analysis 7. Table 2: Measurement series of fall duration t as a function of the displacement & deltax in Atwood's fall machine. 8 x / cc 97.0 92.0 87.0 82.0 77.0 72.0 67.0 62.0 57.0 52.0 47.0 42.0 t / s 2.321 2.293 2.265 2.228 2.204 2.170 2.127 2.096 2.063 2.026 1.989 1, evaluation 3.1. Free fall The relationship between the time of fall and the height of fall is described by the equation (s 0 + x) = 1 2 g t2 It follows that t 2 = 2 gx + 2 s 0 g This relationship between t 2 and x has the form of the straight line equation f ( x) = bx + a, where b is the slope and a is the y-axis segment. If we plot t 2 as a function of x in a diagram, the slope and axis intercept can be graphically visualized from the regression line. With the help of a linear regression analysis , the slope b = 2 g and the axis intercept a = 2 s 0 g as well as their inaccuracies (random errors) u a and u b can be determined quantitatively. 9 The linear regression analysis of the measurement data was carried out with Excel (see attached Excel sheet). The systematic errors of the sizes a and b are neglected in the case of the linear regression analysis. The measurement data including the best-fit line are shown in Figure 1 Comment: see footnote 4. 8 See footnote 1. 9 Comment: a = 1 (x D i 2 y 2 ixixiyi), ua = x2 sy, b = 1 (nx D iy ixiyi) , ub = n D sy, D = nxi 2 (xi) 2, sy = (yif (xi)) 2 (n 2) laboratory protocol should not be repeated) 10 Comment: The symbols and text in the figures should be large enough. Make sure that you only display the relevant section. 4 D (for formulas see  these formulas must be in
5 t 2 in s 2 x in m Figure 1: Squared duration of the fall as a function of the displacement during free fall. The best-fit line was determined using linear regression. The results of the regression analysis can be found in Table 3. Large value Absolute error Relative error Slope b 0, s 2 / mub = 0.000309 s 2 / mub = 0.15% Axis intercept a 0, s 2 ua = 0, mua = 8.39% Table 3: Results of the linear regression analysis for the free fall acceleration due to gravity g The acceleration due to gravity g can be calculated from the gradient b = 2 g: g = 2 b = 9, ms 2 Since the calculation of g involves simply dividing by the error-prone variable b, the relative error of g is equal to the relative error of b: 11 ug = ub = 0.15% ug = gug = 0, ms 2 0.015 ms 2 11 Comment: the 2 is an exact number and has none Failure. 5
6 Final result 12: acceleration due to gravity g = (9.803 & plusmn 0.015) ms 2 = 9.803 ms 2 & plusmn 0.15% starting position s 0 The initial position s 0 = ab = 0, m the relative error result from the axis intercept a and the slope b 13 u s0 = ua + ub = 8.54% 9% of the absolute error u s0 = s 0 u s0 = 0. m 0.0854 = 0. m 0.0007 m Final result: starting position s 0 = (8.5 & plusmn 0.7) mm = 8.5 mm & plusmn 9% 3.2. Atwood's falling machine In Atwood's falling machine the height of the masses changes according to (s 0 + x) = 1 2 a t2. From this follows t 2 = 2 ax + 2 s 0 a The equation of motion for Atwood's fall machine (2 m 1 + m 2) a = m 2 g is solved after the acceleration a and inserted into the equation above: t 2 = 2 g ( 2m 1 + m 2 m 2) x + 2 g (2m 1 + m 2 m 2) s 0 where m 1 is the large mass and m 2 is the small additional mass. Again there is a straight line equation with the slope b = 2 g (2m 1 + m 2) and the m 2 intercept a = 2 g (2m 1 + m 2) sm 0 (caution: not to be confused with the 2 acceleration a) which can be determined from the measurement data using linear regression. 12 Comment: Reasonably rounded according to the significance determined by the error. 13 Since the starting position s 0 is the quotient of the two error-prone variables a and b, the relative error of the starting position u s0 is calculated as the sum of the relative errors of a and b. 6th
7 The data are evaluated again with Excel. The result of the linear regression is shown graphically in Figure 2: t 2 in s x in cm Figure 2: Squared fall duration as a function of the change in the fall height x in Atwood's fall machine. The best-fit line was determined using linear regression. The results of the linear regression analysis can be found in Table 4. Large value Absolute error Relative error Slope b 2, s & sup2 / mub = 0.0259 s & sup2 / mub = 0.90% Axis intercept a 2, s & sup2 ua = 0.0185 mua = 0, 71% Table 4: Slope and axis intercept for the Atwood falling machine as results of the linear regression analysis Gravitational acceleration g With the help of the slope the gravitational acceleration g is calculated as follows: g = 2 b 2m 1 + m 2 m 2 = 9.33884 ms 2 Da g is the product of the three error-prone quantities is b, m 1 and m 2, the absolute error of g is determined by applying the error propagation: ug = ub + m 1 u m1 + m 2 u m2 = 2 b 2 2m 1 + m 2 m 2 4 ub + ubm m1 + 4 mbmum 2 2 = 0, ms 2 + 0, ms 2 + 0, ms 2 = 0.10 ms 2 where ub = 0.0259 s 2 / m, u m1 = 0.2 g and u m2 = 0.2 g. 7th
8 The relative error is ug = ugg = 1.08% Final result: g = (9.34 & plusmn 0.10) ms 2 = 9.34 ms 2 & plusmn 1.1% starting position s 0 From the axis intercept a and the slope b the initial position s 0 = from = 0.90699 m the relative error 14 u s0 = ua + ub = 0.9% + 0.71% = 1.61% 1.6% the absolute error u s0 = s 0 u s0 = 0.9069 m 0.0161 = 0.01460 m 0.015 m Final result: s 0 = (90.7 & plusmn 1.5) cm = 90.7 cm & plusmn 1.6% 4.Summary of results, free fall acceleration due to gravity g = (9.803 & plusmn 0.015) m = 9.803 m & plusmn 0.15% s 2 s 2 starting position s 0 = (8.5 & plusmn 0.7) mm = 8.5 mm & plusmn 9% Atwood's gravity machine acceleration of gravity g = (9.34 & plusmn 0.10) ms 2 = 9.34 ms 2 & plusmn 1.1% starting position s 0 = (90.7 & plusmn 1.5) cm = 90.7 cm & plusmn 1.6% 14 Since the starting position s 0 is the quotient of the two error-prone quantities a and b, the relative error of the initial position u s0 is calculated as the sum of the relative errors ler of a and b. 8th
9 5. Evaluation of the results The result of the acceleration due to gravity g from the experiment on free fall agrees within the error limits with the literature value of (9, m / s 2 ± 0.000000x) m / s 2 . In contrast, the result of the acceleration due to gravity g using the Atwood drop machine deviates significantly from the literature value. A comparison of the error limits shows that the error limit when determining g with Atwood's falling machine is significantly larger than that in the free fall experiment. Despite the larger error limits, the literature value does not lie within the confidence range of the measurement with the Atwood case machine. At 9.81 m 9.34 m = 0.47 m, the deviation from the literature value is almost s 2 s 2 s 2 five times greater than the error limits. The reason for the deviation can be assumed that in Atwood's fall machine the friction of the line and the moment of inertia of the rotating pulleys have significant influences that were not taken into account in the model.The large error limits of the experiment with Atwood's fall machine result from the fact that, in contrast to free fall, not only the inaccuracy of the slope, but also the inaccuracies of the mass determination are taken into account. Furthermore, the slope in this experiment with 0.9% has a larger relative error than with free fall with 0.15%. 15 The high time resolutions of today's time measurements make it possible that the experiment on free fall delivers the better results. At the time when the Adwood drop machine was invented, such a precise time measurement using fast detectors and electronic stopwatches was not possible. The Atwood drop machine was therefore a good method of measuring the acceleration due to gravity at that time. 16 The values for the initial positions s 0 appear realistic in both cases and match the respective measurement setup. 6. Sources and Bibliography 17  Worksheets for calculating errors (Version 1/03)  Kohlrausch - Practical Physics, Volume 3, Tables and Diagrams, edited by D. Hahn and S. Wagner, BG Teubner Stuttgart, 23. Edition, comment: The level of knowledge of this paragraph does not necessarily have to be achieved. This paragraph represents the K & uumlr. 16 Comment: The level of knowledge of this paragraph does not necessarily have to be achieved. This paragraph represents the K & uumlr. 17 Comment: In the case of external text and image material, the reference source must be quoted. 9
10 7. Appendix: Measurement protocol Comment 1: A protocol of the measurements must be added as an attachment, which contains the original data and all recordings made during the experiment. Under no circumstances should the measurement results be deleted before the end of the laboratory. Comment 2: If the evaluation was carried out using Excel or Calc, the corresponding Excel or Calc file should also be submitted. 10
The metallocenylide Cp2Zr (Ph) (CHPPh3) (1a) reacts with carbon monoxide (room temperature, 40 bar) with insertion into the Zr C (ylid) bond. The product Cp is obtained2Zr (Ph) [η 2 -C (CHPPh3) O] (3a). According to the X-ray structure analysis, the η 2 -acyl ligand of 3a in “O-in” orientation. The connection 3a crystallizes in the space group P.212121 with the cell constants a 11.111(2),b 15.353(3),c 17,428 (2) Å,Z = 4. Carbonylation of Cp2M (C2H5) (CHPPh3) (M = Zr, 1b Hf, 1c) analogously provides the metal-containing stabilized ylides Cp2M (C2H5) [η 2 -C (CHPPh3) O] (3b and 3c). X-ray structure analysis of the hafnium bond 3c: Space group P.22/n,a 10.521(1),b 15.431(2),c 16,863 (1) Å, β 94.28 (1) °,Z = 4.
Differential and integral calculus of one and more variables
1 module overview: Applied computer science Higher mathematics Basic knowledge of: differential and integral calculus of one and more variables vector calculus, complex numbers, Fourier series, linear algebra lecture You have in-depth theoretical and empirical knowledge about the purpose and limits of higher mathematics can select suitable numerical procedures 60 h 90 h 5 CP ECTS 5.0 Prerequisites Written examination K120 Module manager. Prof. Dr. Christoph Nachtigall 150 h every year (SS) Applicability for the EIM and EI-BB Higher Mathematics course no - and surface and volume integrals in space - The integrals (Green, Gau & szlig, Stokes) - Maxwell's equations and their physical meaning - Solutions of Maxwell's equations Lecture script Hoffmann, A., Marx, B., Vogt, W., Mathematics for engineers , Vol. 2. Pearson, / 27
2 Papula, L., Mathematics for Engineers and Natural Scientists, Vol. 2. Vieweg, 2001 Papula, L., Mathematics for Engineers and Natural Scientists, Vol. 3. Vieweg, 2008Weltner, K., Wiesner, H., et al., Mathematik für Physiker, Volume 2. Springer, 2006 Numerical Methods No. E + I2202 Course Content 1 Basic Terms and Principle Procedure 2 Numerical Differentiation and Integration 2.1 Numerical Differentiation 2.2 Numerical Integration 3 Nonlinear Equations with an Independent Variable 3.1 Task 3.2 Bisection Method 3.3 Newton's Method 3.4 Secant method 3.5 Extension of the convergence area of locally convergent methods Damped Newton method Combination of methods 3.6 Determination of roots of real polynomials 4 Nonlinear equations with several independent variables 4.1 Task 4.2 Newton method 4.3 Quasi-Newton method 5 Minimum search for functions with one independent variable 5.1 Task Position and basic procedure 5.2 Bisection procedure 5.3 Newton procedure 6 Minimum search for functions with several independent variables 6.1 Task and basic procedure 6.2 Gau & szlig-Seidel procedure 6.3 Rosenbrock procedure 6.4 Search in negative gradient direction 6.5 Newton procedure 6.6 Fletcher-Reeves procedure 6.7 Quasi -Newton method 6.8 Minimum search with constraints Use of Lagrange factors Use of penalty functions 6.9 Least squares method as a special case of a multidimensional minimum search Direct solution Update equations 7 Eigenvalues and eigenvectors of a matrix 7.1 Exercise 7.2 Basic relationships between a square matrix and its eigenvalues and Eigenvectors 7.3 Eigenvector Calculation Direct Method 2/27
3 7.3.2 Power method Inverse power method Deflation technique 8 Common differential equations 8.1 Task 8.2 Explicit numerical integration method Euler method Modified Euler method Runge-Kutta method Step size control Multi-step method 8.3 Numerical stability of one-step method Engeln-M & uumlllges, G., Niederdrenk, K., Wodicka, Wodicka R., Numerik-Algorithmen, Springer, 10th edition, 2011 Theoretical electrical engineering - Differential calculus - Integral calculus - Vector analysis - Complex number space - Fundamentals of the field concept Lecture You will gain a deeper understanding of electrical and magnetic phenomena and the variables that describe them Understand and explain inherent electrotechnical relationships You have mastered the mathematical description of electromagnetic fields You can calculate basic field types 60 h 90 h 5 CP 150 h ECTS 5.0 Prerequisites M Final exam M (3/5) + RE (2/5) module responsible Prof. Dr.-Ing. Lothar Sch & uumlssele every year (SS) Can be used for the EIM and EI-BB Theoretical Electrical Engineering Master’s course No. E + I2203 3/27
4 Course content Fundamentals of the concept of the field - Static and stationary fields - The Maxwell equations - Solving the Maxwell equations - Treatment of special problems Balanis, CA, Advanced Engineering Electromagnetics, John Wiley & ampSons, New York, 1989 Leuchtmann, P., Introduction to electromagnetic field theory, Pearson, 2006 Henke, H., Electromagnetic Fields - Theory and Application, Springer, 2007 Ulaby, F., T., Fundamentals of Applied Electromagnetics, Prentice Hall, 1999 Strassacker, G., S & uuml & szlige, R., Rotation, divergence and everything around it, Teubner , 2006 Seminar Mathematical Methods Art Seminar No. E + I2204 Contents Selected topics on higher mathematics and numerics are worked on by the students, a handout is created and the topic is presented. Will be announced at the beginning of the semester. Embedded and industrial networks Basic knowledge of communication protocols Lecture / Laboratory The students gain in-depth insight into the internal structure of communication protocols. In this way, they also get to know the most important design paradigms and are thus able not only to select and use the optimal communication protocol for the application, but also to design appropriate adaptations and extensions themselves. 60 h 90 h 150 h 5 CP. The module grade corresponds to the grade of the exam K60. The laboratory is ungraded, but has to be passed. ECTS 5.0 Prerequisites for written examination K60 and successful participation in the laboratory. Prof. Dr.-Ing. Axel Sikora every year (SS) Can be used for the EIM 4/27 Master’s course
5 Embedded and industrial networks No. E + I2205 Course content 1) Introduction 1.1) Overview, requirements 1.2) Architectures & amp; classifications 2) Algorithms 2.1) & transfer mechanisms 2.2) Channel access protocols 2.3) Routing algorithms 2.4) Application protocols 2.5) Network synchronization (time synchronization, power saving algorithms ) 2.6) Network management (planning, simulation, monitoring) 3) Protocol examples 3.1) CAN & amp LIN 3.2) Ethernet & amp Industrial Ethernet 3.3) Profibus & amp Profinet 3.4) HART & amp Wireless HART 3.5) Embedded TCP / IP 3.6) Embedded web applications Schnell, G. , Wiedemann, B., Bus systems in automation and process technology: Basics, systems and trends in industrial communication, Vieweg + Teubner Verlag, 2008 Bender, K., Profibus - The fieldbus for automation, Carl Hanser Verlag, 1992 Pfeiffer, O ., Ayre, A., Keydel, C., Embedded Networking with Can and Canopen, Copperhill Media Corporation, 2008 Shelby, Z., Bormann, C., 6LoWPA N: The Wireless Embedded Internet, John Wiley & amp Sons, 2009 Sikora, A., Technical Basics of Computer Communication: Internet Protocols and Applications, Carl Hanser Verlag, 2003 Laboratory Embedded and Industrial Networks Art Labor / Studio No. E + I2206 Contents Practical Use of interfaces on embedded systems based on the ARM Cortex-M3 platform through parameterization, programming and analysis of network communication Measurement of communication parameters in industrial network protocols PROFINET and Real Time Ethernet Use of application protocol HTTP & uumlber TCP / IP using an embedded web server Laboratory tests: Part 1: Embedded networks 1. Serial Peripheral Interface (SPI) 2. Local Interconnect Network (LIN) 3. Controller Area Network (CAN) 4. Embedded socket communication with TCP / IP 5. Embedded web server programming for using HTTP over TCP / IP 5/27
6 Part 2: Industrial networks 1. PROFINET 2. Real Time Ethernet Zimmermann, W., Schmidgall, R., Bus systems in vehicle technology - protocols, standards and software architecture, 5th edition, Springer Vieweg, 2014 Lawrenz, W., Controller area network: CAN basics, design, applications, test technology, VDE-Verlag, 2011 Bormann, A., Hilgenkamp, I., Industrial networks: Ethernet communication for automation applications, H & uumlthig, 2006 Sikora, A., Technical basics of computer communication: Internet Protocols and applications, Fachbuchverlag Leipzig in Carl Hanser Verlag as well as relevant data sheets, which are provided on the development server. Management for engineers - practical experience in the industrial environment is helpful Lecture / seminar In this module, the participants deepen their general qualifications, motivated by their own experience in the practical semester of the bachelor's degree program and by possible practical experience between the bachelor’s and master’s degree. Emphasis is placed on the areas required of engineers who take on leadership positions. Your personality development will be promoted through these seminars. 2 semesters 60 h 90 h 5 CP 150 h ECTS 5.0 Prerequisites Seminar Management: Referat RE (graded) Management and organizational teaching: Referat RE (ungraded) Module manager. Prof. Dr.-Ing. Tobias Felhauer Semester 1-2 every semester Applicability of the EIM Master’s course Compulsory module Seminar Management / Seminar 6/27
7 No. E + I2207 Course content Company and management Tasks and goals of management Company cultures Communication Intercultural management Practical management know-how do s and don ts in professional life Professional behavior Fisher, R., Ury, W., Getting to Yes: Negotiating an agreement without giving in, Cornerstone Digital, Kindle Edition, 2012 Hoffmann, H.-E., Schoper, Y.-G., Fitzsimons, CJ, Internationales Projektmanagement, Deutscher Taschenbuch Verlag, 2004 Blogs from ZEIT ONLINE on the subject of career and professional leadership - and organizational theory / seminar no. E + I2208 Learning content Practical know-how on employee management do s and don ts of leadership styles Company organization Structural and process organization Matrix organization Primary and secondary organizations Project management Meetings Conversation, conflict management, training, training, training, conflict management, training, conflict management, training, negotiation, protection against manipulation ur conflict solution, Stark Verlagsgesellschaft, 2012 Vahs, D., Organization - A text and management book, 8th edition, Sch & aumlffer- Poeschel, 2012 Gorecki, P., Pautsch, P., Lean Management, 3rd edition, Carl Hanser Verlag, 2013 Verzuh, E., The Fast Forward MBA in Project Management, 4th Edition, John Wiley & amp Sons, 2011 Marketing for Engineers None Necessary Lecture / Seminar 7/27
8 You will learn the basic aspects of successful marketing in the engineering field. You will get to know the most important marketing analyzes, strategies and instruments. In a marketing project, you will learn to apply the marketing knowledge you have acquired. 30 h 120 h CP h ECTS 5.0 Prerequisites Presentation RE (1/2) + oral exam M (1/2) module manager Diplom Kaufmann Achim Labusch every year (WS) Applicability of the Master’s course EIM Seminar Marketing Art Seminar No. E + I2209 Course content Conceptual basics and characteristics of marketing Basics for creating a marketing concept Marketing analysis Marketing strategy Marketing planning and implementation Lecture script Kotler, Armstrong, Saunders, Wong, Basics of Marketing, Pearson Studium, 4th edition, 2006 Werner Gustav Alex, Das Marketing Konzept, Books on Demand GmbH, 2007 Master's thesis The master's thesis is issued at the earliest when 85% of the achievable credits are reached were acquired in this course (without taking into account the master's thesis). Scientific Work / semester The students demonstrate the ability to work on a problem from the subject of the EIM master’s course independently using scientific methods within a specified period of time. To this end, the following competencies are acquired in connection with the academic work and publishing seminar: Formulation of a scientific procedure for processing the selected task Collecting, analyzing and evaluating information from relevant information sources (publications, books, etc.) and presenting the state of the art in the context of the Task Structure of the topic Clear presentation of the results, conclusions and further recommendations. 8/27
9 Creation of a scientific publication according to IEEE guidelines. Preparation of a final presentation of the results obtained 30 h 870 h CP h ECTS 30.0 Prerequisites Scientific work (WA) and successful seminar participation (KO) Responsible for the module. Prof. Dr.-Ing. Tobias Felhauer every semester usability of the Master’s course EIM seminar scientific work and publishing type seminar no of the topic - Targeted research and processing Barley, Stephen R., When I write my Masterpiece: Thoughts on What Makes a Paper Interesting, Academy of Management Journal, Vol. 49, No. 1, 16-20, 2006 Master Thesis Art Scientific Work / seminar no. E + I2210 learning content Individual topics are scientifically processed and documented in a given time and wind turbines as well as when feeding renewable energy into the grid. The participants are then able to design feed-in systems and ensure that they comply with the grid connection conditions. The material learned is consolidated and illustrated in practical exercises. 9/27
10 60 h 90 h 150 h 5 CP. The module grade corresponds to the grade of the exam K60. The laboratory is ungraded, but has to be passed. ECTS 5.0 Prerequisites for written examination K60 and successful participation in the laboratory. Prof. Dr. Michael Schmidt every year (SS) Applicability of the EIM master’s course, focus on energy and automation technology Laboratory, Regenerative Energy Systems Type Laboratory / Studio No. Simulation of the stationary and dynamic behavior of wind turbines Simulation of the grid feed-in behavior during Fault Ride Through Quaschning, V., Regenerative Energy Systems. Technologies - Calculation - Simulation, 7th edition, Hanser-Verlag, 2011 Mertens, K., Photovoltaics: textbook on basics, technology and practice, Hanser-Verlag, 2011 Kaltschmitt, M., Streicher, W., Wiese, A., Renewable energies: System technology, economic efficiency, environmental aspects, 4th edition, Springer-Verlag, 2005 Renewable energy systems No. E + I2212 Learning content Structure and function of PV modules Structure and function of PV inverters Control of grid-connected and stand-alone PV inverters MPP -Tracking Structure and Functionality of Wind Turbines Structure and Functionality of Generators and Inverters in Wind Turbines Control Strategies for Wind Turbines Grid Codes and Fault Ride Through Grid Stability and Grid Expansion Quaschning, V .: Regenerative Energiesysteme. Technologies - calculation - simulation. 7th edition, Hanser-Verlag, 2011 Mertens, K .: Photovoltaics: textbook on basics, technology and practice. Hanser-Verlag, / 27
11 Kaltschmitt, M. Streicher, W.Wiese, A .: Renewable energies: system technology, economic efficiency, environmental aspects. 4th edition, Springer-Verlag, 2005 Mobile and stationary electric drives Basic knowledge of power electronics and control engineering Lecture The participants get to know the most important control engineering models and the specific behavior of the most widespread three-phase machines. You will also gain an overview of the interlocking of the various components in highly dynamic drives and the ability to design controllers for this. This knowledge and skills are rounded off in the field of electromobile applications by the specific features there. The participants are then able to understand the current developments in the field of electromobility and, if necessary, to advance them themselves. 60 h 90 h 150 h 5 CP. Module grade corresponds to the grade of the joint oral exam M ECTS 5.0 Prerequisites Oral exam (M) Responsible for the module. Prof. Dr.-Ing. habil. Uwe Nu & szlig every year (WS) Applicability of the EIM master’s course with a focus on energy and automation technology, electromobility No. Safety mechanisms in vehicles with electric drive & economic considerations Wallentowitz, H., Freialdenhoven, A., Strategies for the electrification of the drive train Technologies, markets and implications, 2nd edition, Vieweg + Teubner-Verlag, 2011 Hofmann, P., Hybrid vehicles - an alternative drive concept for the future, Springer-Verlag, 2010 Naunin, D., Bartz, W., Wippler, E., Hybrid, battery and fuel cell electric vehicles technology, structures and development, Expert-Verlag, / 27
12 Control of electric drives No. E + I2215 Course content Introduction of space vectors and space vector differential equations Transformation of space vectors and space vector differential equations between stationary and rotating coordinate systems Description of the dynamic behavior of permanent magnet synchronous machines Magnetic wheel-oriented control of permanent magnet synchronous current machines Description of the dynamic behavior of asynchronous machines and speed controller design for three-phase drives Nu & szlig, U., Highly dynamic control of electrical drives, Berlin, Offenbach, VDE- Verlag, 2010 Quang, NP, Dittrich, J.-A., Vector Control of Three-Phase AC Machines, Berlin, Heidelberg, Springer- Verlag, 2008 Schr & oumlder, D., Electrical drives - control of drive systems, 2nd edition, Berlin, Heidelberg, Springer-Verlag, 2001 control systems I basics of signal and system control engineering Theory lecture on modeling and simulation: - Getting to know the practical decomposition of real technical processes into physical systems. - Learn to process the given physics in mathematical equations, whereby neglect must be made. - Creation of informative simulation models and simulation with variable representation of the results. to adaptive control systems: - Introduction of the adaptation structure as a second return. - Getting to know the advantages and disadvantages of this second return with regard to the stability of the regulation. - Identification based on aperiodic and periodic test signals. - Application and implementation of adaptive control algorithms. 60 h 120 h 180 h 6 CP. The module grade corresponds to the grade of the joint oral examination M. ECTS 6.0 Prerequisites Oral examination (M) Module responsibility. Prof. Dr.-Ing. Peter Hildenbrand every year (SS) 12/27
13 Applicability for the EIM Master’s course with a focus on energy and automation technology Adaptive control systems No. E + I2217 Learning content Adaptive control systems, definitions, introduction and examples Structures of adaptive control systems Identification, decision-making processes and modification Basic structures: Process of controlled adaptation Process of controlled adaptation with and without comparison model Example : Adaptive speed control of a DC motor Identification methods: direct, indirect identification methods, experimental identification methods, determination of the parameters of time-discrete transfer functions in the quadratic mean Control systems, B & oumlcker, among others (Springer) Control Engineering III, Unbehauen (Vieweg) Simulation and I Implementation of Self-Tuning Controllers, Roffel et al. (Prentice Hall Advanced Reference Series Engineering) Modeling and simulation No. E + I2216 Learning content Purpose of modeling, overview Principal possibilities of modeling Terms: process, system, model Dynamic systems, state variables Principal ways in the Modeling Procedure for theoretical analysis Physical laws, balance equations, phenomenological equations, neural networks Modeling and simulation in technical processes Practical approach to setting the simulation model and simulation Control of systems with deceleration behavior and systems with integral behavior Multi-variable control systems and practical decoupling methods Design of an adaptive controller On the basis of a parallel comparison model, optimization of the tractive power of modern three-phase locomotives by simulating the drive train using the example of Adhesion control Analysis and synthesis of continuous control systems, Reinisch (H & uumlthig) Small manual of technical control processes, Oppelt (Verlag Chemie) Modeling and simulation, Bossel (Vieweg) Control systems II Knowledge from module "Mathematical system description" Knowledge from lecture "Control technology II" Lecture 13/27
14 You will learn and understand state space methods as a tool for designing control systems You will be able to use methods for the analysis and synthesis of discrete-time control systems You will acquire the ability to transfer known continuous-time control design methods to discrete-time control systems 60 h 90 h 150 h 5 CP. The module grade corresponds to the grade of the joint written examination K120. ECTS 5.0 Prerequisites Written Exam (K120) Module Responsible. Prof. Dr.-Ing. habil. Uwe Nu & szlig every year (WS) Applicability of the EIM master’s course with a focus on energy and automation technology State space methods No. E + I2218 Course content Introduction to the state space representation of dynamic systems: Normal forms of state equations General solution of the time-continuous state equations of a linear, time-invariant system Controllability State regulators Design of time-continuous state observers Design of time-discrete state regulators and observers F & oumlllinger, O., Control Engineering, 10th Edition, Berlin, H & uumlthig Buch Verlag, 2008 Lunze, J., Control Engineering 2, 5th Edition, Berlin, Heidelberg, Springer-Verlag, 2008 F & oumlllinger, O., Linear scanning systems, 4th edition, M & uumlnchen, Vienna, Oldenbourg Verlag, 1990 Discrete-time regulations No. E + I2219 Learning content Characteristics of discrete-time control loops Mathematical tools for describing dynamic behavior discrete-time he control loops Assessment of the behavior of time-discrete control loops by analyzing the poles and zeros of the z- transfer function Time-discrete controller design processes in the z-range Algebraic stability criteria Structural measures to improve the control behavior of time-discrete control loops, measures, line limits, size limits for setting variables , Vienna, Oldenbourg Verlag, / 27
15 Lunze, J., Regelstechnik 2, 5th edition, Berlin, Heidelberg, Springer-Verlag, 2008 High-frequency technology Basic knowledge of high-frequency technology (HF I) Lecture / laboratory SWS 6.0 Examples for high-frequency systems such as receivers, transmitters, spectrum analyzer, radar Understanding the radiation of electromagnetic waves. Learn how to calculate the noise behavior of high-frequency systems. Getting to know and designing high-frequency circuits such as mixers, oscillators, power amplifiers and couplers. 90 h 120 h 210 h 7 CP. The module grade corresponds to the grade of the oral exam. The laboratory is ungraded, but has to be passed. ECTS 7.0 Prerequisites Oral examination (M) and successful participation in the laboratory. Prof. Dr.-Ing. Lothar Sch & uumlssele every year (WS) Applicability of the EIM master’s course, focus on communication technology, high-frequency laboratory, II Type of laboratory / studio no 4. Determination of the noise parameters of microwave components 5. Rectangular waveguides in microwave technology 6. EMC measurements (interference voltages and radiation) Hoffmann, M., Hochfrequenztechnik, Heidelberg, Springer Verlag, 1997 Heuermann, H., Hochfrequenztechnik, Wiesbaden, Vieweg Verlag, 2009 Hochfrequenztechnik II 15/27
16 Art No. Lecture E + I2220 Course content 1. Antennas 2. Stability of two ports 3. Noise sources and their description 4. Noise from linear two ports 5. HF oscillators 6. Mischer Hoffmann, M., Hochfrequenztechnik, Berlin, Heidelberg [among others], Springer Verlag, 1997 Heuermann, H., Hochfrequenztechnik, Wiesbaden, Vieweg Verlag, 2005 Microwave technology Basic knowledge of: SWS 6.0 Differential Equations Integral Calculus Vector Analysis Static Electric and Magnetic Fields Lecture / Laboratory You understand the core statements of Maxwell's equations and can apply them to simple electrodynamic problems use. You know the properties of plane waves. You can apply the description of guided waves with the mode concept to any waveguide and know the properties of important waveguide structures. You will learn how to calculate the properties of passive microwave systems 90 h 120 h 210 h 7 CP. The module grade corresponds to the grade of the written examination K60. The laboratory is ungraded, but has to be passed. ECTS 7.0 Prerequisites Written exam (K90) and successful participation in the laboratory. Prof. Dr.-Ing. Andreas Christ every year (SS) Applicability of the EIM Master’s course with a focus on communication technology Guided Wave Theory No. E + I411 Course content Maxwell s equations: general forms, cause-effect-relations, continuity relation, time harmonic fields Wave concept: uniform plane waves, propagation and energy flux, skin effect 16/27
17 Boundary conditions Transmission lines: - Modes: concept and classification, orthogonality - Properties of rectangular waveguides, other waveguide types and coaxial lines Circuit theory for waveguide systems: - Scattering matrix formulation - Equivalent circuits - Examples of passive devices Balanis, CA, Advanced Engineering Electromagnetics, John Wiley & ampSons, New York Ulaby, FT, Fundamentals of Applied Electromagnetics, Prentice Hall Fleisch, D., A Student's Guide to Maxwell's Equations, Cambridge University Press Laboratory Simulation of Electrodynamic Fields Art Laboratory / Studio No. E + I2223 Course content Three-dimensional field numerical simulation passive microwave structures and interpretation of the results (propagation coefficients, scattering parameters, three-dimensional electromagnetic fields): * modes in rectangular waveguide * microstrip line * pin in waveguide * aperture * & transition from microstrip line - waveguide * directional coupler (password will be known in the lecture given or on request). Guest login possible Script for the lecture Guided Wave Theory Theory background waveguide: e.g. Balanis, C. A., Advanced Engineering Electromagnetics, Wiley, 1998, S Funkkommunikation Basic knowledge of digital and transmission technology 17/27
18 Basic knowledge of radio transmission Basic knowledge of matrix calculation Lecture / seminar / laboratory SWS 6.0 You will receive in-depth knowledge of the system-theoretical approach in the analysis and design of modern wireless communication systems You will have in-depth knowledge of the use of modern methods for radio communication You will receive practical experience in metrological analysis of wireless communication links and systems. 90 h 120 h 210 h 7 CP. The module grade is calculated from the mean value of the grades from the oral examination (M, & frac12) and the graded presentation (RE, & frac12). The laboratory is ungraded, but has to be passed. ECTS 7.0 Prerequisites Oral examination (M, & frac12), graded presentation (RE, & frac12) and successful laboratory participation. Prof. Dr.-Ing. Tobias Felhauer every year (WS) usability of the EIM master’s course, focus on communication technology wireless communication / seminar no. E + I2224 Course content 1. Introduction to history spec. technical challenges and problems with wireless communication. 2. Characterization of the radio channel Important properties and parameters of radio channels Propagation models Link budget calculations Stochastic modeling, simulation and measurement of radio channels. 3. Techniques in wireless communication systems Digital modulation techniques and detection techniques Diversity techniques Equalization techniques Multiple access and duplex techniques MIMO architectures Spatial Multiplexing and Space-Time Coding (STC) Molisch, A., Wireless Communications, John Wiley & ampSons Ltd., IEEE Press Rohling, H., OFDM: Concepts for Future Communication Systems, Springer Verlag, Berlin Larsson, E., Stoica, P., Space-Time Block Coding for Wireless Communications, Cambridge University Press 18/27
19 Paulraj, A, Nabar, R., Gore, D., Introduction to Space-Time Wireless Communications, Cambridge University Press Stepping, C., Wireless Networks, Schlembach Fachverlag, Proakis, JG, Digital Communications, McGraw-Hill International Labor Wireless Communication Art Laboratory / Studio No. E + I2225 Learning content Laboratory exercises: Experiment 1: Short-range communication according to the Bluetooth standard Experiment 2: Analysis of a communication link according to the ZigBee standard Experiment 3: Supply and protocol analysis in the fho-publicnet campus WLAN of the Offenburg University of Applied Sciences Experiment 4 : Metrological analysis of digital carrier modulation methods Experiment 5: Real-time location with ultra-wideband (UWB) radio signals Tse, D., Fundamentals of Wireless Communication, Cambridge, Cambridge University Press, 2005 Bensky, A., Short-Range Wireless Communication: Fundamentals of RF System Design and Application, Heinemann Verlag, 2004 Rech, J., Wirelss LANs, Heise-Verlag, M & uumlnchen, 2004 Computer science knowledge from d In the areas of modeling (UML, ERM) and object-oriented programming, lecture / laboratory understand the principles of model-driven software development and apply them to specific problems. Understand the limits of model-driven software development. Analyze existing problems and develop efficient model-based solutions from them Test models can be derived from textual and graphic specifications 60 h 150 h 7 CP 210 h ECTS 7.0 Prerequisites Written examination (K60) and successful participation in the laboratory 19/27
20 module manager Prof. Dr.-Ing. Daniel Fischer every year (WS) Applicability of the EIM Master’s course, advanced module Model-Driven Software Development No. Independent Model (CIM) 3.2 Platform Independent Model (PIM) 3.3 Platform Specific Model (PSM) 4. Domain-specific modeling using the example of embedded systems 4.1 Modeling static behavior 4.2 Modeling dynamic behavior 4.3 Model-based connection of operating systems and HAL 5. Domain-specific modeling using the example of Client-server applications 5.1 Modeling business classes 5.2 Generation of the persistence layer 6. Model-based testing 6.1 Aims, principles and variants of the MBT 6.2 UML Testing Profile (UTP) 6.3 Creation of test models 6.4 Transformation of test models into test languages using the example of TTCN-3 Stahl, T ., V & o umllter, M., Efftinge, S., Haase, A., Model-driven software development, dpunkt.verlag, 2nd edition, 2007 Gruhn, V., Pieper, D., R & oumlttgers, C., MDA: Effective software engineering with UML2 and Eclipse , Springer, 1st Edition, 2006 Kecher, C., UML 2: The Comprehensive Manual, Galileo Computing, 4th Edition, 2011 Tenny, L., Zeeshan Hirani, Entity Framework 4.0 Recipes: A Problem-Solution Approach, Apress, 1 Edition, 2010 Laboratory Model-Driven Software Development Art Laboratory / Studio No. E + I2228 Learning content Part 1: Model-driven software development with IBM Rational Rhapsody Modeling an interrupt-controlled stop clock for the target platform Cortex-M3 using a real-time operating system Part 2: Model-driven software development with Microsoft Visual Studio implementation of a graphical front end. Modeling of the analysis classes. Generation of the persistence layer with the Entity Framework 20/27
21 Part 3: Model Based Testing Extension of an existing distributed system (TCP / IP, C #) Modeling of test models Generation of test cases based on the test models with Conformiq Testsuite Execution of the tests with the test execution framework Elvior TestCast Stahl, T., V & oumllter, M., Efftinge, S., Haase, A., model-driven software development, dpunkt.verlag, 2nd edition, 2007 Gruhn, V., Pieper, D., R & oumlttgers, C., MDA: Effective software engineering with UML2 and Eclipse, Springer, 1. Edition, 2006 Kecher, C., UML 2: The Comprehensive Manual, Galileo Computing, 4th Edition, 2011 Tenny, L., Zeeshan Hirani, Entity Framework 4.0 Recipes: A Problem-Solution Approach, Apress, 1.Edition, 2010 Image processing Knowledge from the courses "Signals and Systems" and "Object-oriented software development" Lecture / Laboratory SWS 6.0 Getting to know newer concepts of digital image processing 90 h 120 h 7 CP 210 h ECTS 7.0 Prerequisites Digital image processing: written examination (K60), weight: 0.5 Three-dimensional image processing: written examination (K60), weight: 0.5 - Admission requirements for written examination: ungraded presentation Laboratory: successful participation in the laboratory (ungraded ) Module manager Prof. Dr. Hensel every year (SS) 21/27
22 Applicability of the EIM Master’s course, advanced module, three-dimensional image processing No. E + I2230 Course content Analytical geometry for describing three-dimensional space, especially rigid transformations and homogeneous coordinates Quaternions OpenGL transformations Stereoscopy and photogrammetry: camera calibration, epipolar geometry, rectification of landmarks, surface and voxel-based Algorithms for the registration of three-dimensional image data & aumltze pixel-, voxel- and edge-based segmentation algorithms Application of Voronoi diagrams and Delaunay triangulation in the three-dimensional surface reconstruction Surface and volume rendering Hough transformation, distance transformation Wavelets Splines processing of the three-dimensional algorithms and others) Handels, H., Medical Image Processing - Image Analysis, Pattern Recognition and Visualization for the Computer Assisted Iche diagnostics and therapy, Vieweg + Teubner Verlag, 2nd revised and expanded edition, 2009 Schreer, O., stereo analysis and image synthesis, Springer, 2005 J & aumlhne, B., digital image processing, Springer, 7th revised edition, 2012 Gonzalez, RC , Woods, RE, Digital Image Processing, Addison Wesley, 3rd International edition, 2008 Dougherty, G., Digital Image Processing for Medical Applications, Springer, 2011 Demant, C., Streicher-Abel, B., Springhoff, A., Industrielle Image processing, Springer, 3rd edition, 2011 Digital image processing No. E + I2229 SWS 3.0 Course content The lecture covers the following topics: 1. Image acquisition The optical system Image sensors, CCD and CMOS digitization and quantization Aliasing effects Color spaces 2. Image preprocessing The histogram 2D- Fourier transform linear filters, ranking filters 3. Feature extraction 22/27
23 Edges Corners 4. Parametric image alignment and connection Detectors and descriptors Model-based image transformation RANSAC Sch & aumltzverfahren Szeliski, R., Computer Vision: Algorithms and Applications, Springer, 2010 J & aumlhne, B., Digital image processing and extraction, Springer 2012 Forsyth, D., COmputer Vision: A Modern Approach, Addison Wesley, 2012 Hartley, R., Zisserman, A., Multiple View Geometry in Computer Vision, 2nd Edition, Cambridge University Press, 2004 Burger, W., Burge, M., J., Digitale Image processing: An introduction with Java and ImageJ, Springer, 2004 Laboratory Digital Image Processing Art Laboratory / Studio No. E + I2231 SWS 1.0 Course content Programming algorithms and operations on images with Matlab exercises from the areas: Image types and image types, color and multi-channel images, linear filters Morphological operators Hough transformation Feature extraction Szeliski, R., Computer Vision: Algorithms and Applications, Springer, 2010 J & aumlhne, B., Digital e image processing and extraction, Springer, 2012 Erhardt, A., introduction to digital image processing, Vieweg + Teubner, 2008 Gonzalez, digital image processing using Matlab, Addison Wesley, 2004 signal processing SWS 6.0 knowledge of courses in the field of signals and systems & quot, in particular Mastery of the Fourier and the z transformation Basic knowledge of digital signal processing, such as from the lecture `` Digital Signal Processing I '' in Bachelor courses of the Faculty E + I Elementary programming knowledge Lecture Safe mastery of the design and the implementation of digital filters Ability to adapt the design to the structure or architecture of the hardware to be used and / or the integrated DSP provided for it A sense of the possibilities for using multi-rate filters and the associated reduction in required resources and their computing load. Understanding of the background and possible uses of the known source coding methods. 23/27
24 90 h 120 h 210 h 7 CP. The module grade results from the weighted mean of the grades from the Digital Signal Processing II exam (K90, weight: 5/7) and the oral examination of source coding (M, weight: 2/7). ECTS 7.0 Requirements Digital Signal Processing II: Exam (K90) Source Coding: Oral Exam (M) Module Responsible. Prof. Dr.-Ing. Werner Reich every year (SS) Applicability for the EIM master’s course, specialization module, source coding No. For audio signals: - PCM, irrelevance reduction (ISO MPEG) - Language (A-Law) Codes for texts Optimal codes: - Information theory: entropy, redundancy - Codes of variable word length: Shannon, Fano, Huffman - Realization aspects, digital transmission and analog message transmission, length coding, message length coding , Pehl (H & uumlthig) Information and Coding, Hamming (VCH) Information Theory and Coding, Mildenberger, O. (Vieweg) Digital Signal Processing II No. E + I2232 Course content DESIGN AND REALIZATION OF RECURSIVE (IIR) FILTERS Filter design: - pulse-invariant, jump-invariant, bilinear Transformation filter structures: - non-canonical, canonical and transposed direct form - cascade enform, parallel form DFT / FFT ALGORITHMS Definition, application to simple sequences Possible ways of interpreting the results: - sampled version of the FT for time-limited signals 24/27
25 - Fourier series for periodic signals - Complex mixer and filter bank FFT algorithms - Circular convolution, segmentation, overlap methods MULTI-RATE PROCESSING Ideal time-continuous sampling rate converter Decimation: - Description in time and frequency domains - Aliasing, controlled aliasing - Multi-level decimation - & Oumeconomic implementation of decimation filters - cascaded MTAs. Interpolation: - Description in time and frequency domains - Suppression of mirror components - Economic implementation of interpolation filters - Constant and linear interpolation as a special case ADAPTIVE FILTER - Vector description Areas of application: - Pre-dictator, system identification - Equalization, compensation, MQA, LMS algorithm in the sense of minimizing the LMS algorithm : - Stochastic approximation - WAVELETS AND FILTERB & AumlNKE convergence condition - Haar wavelets, Daubechies wavelets - Perfect reconstruction - Polyphase filter - Applications Kammeyer, KD, Kroschel, K., digital signal processing, filtering and spectral analysis with MATLAB & Uumlbungen, Vieweg + Teubner, 8th edition 2012 Oppenheim, AV, Schafer, RW, Discrete-Time Signal Processing, Pearson Prentice Hall, 3rd edition, 2009 Microelectronics Lecture The participants understand the structure, manufacture, function and design of microelectronic integrated circuits (VLSI-Scha ltkkreis) with modern IC design systems. They have the ability to assess the integrability of digital and analog circuits, as well as the ability to deal with complex programs for simulation and the design of integrated circuits, and they master the terms and processes in connection with application-specific integrated circuits (ASIC). After completing the lecture: Qualification for the profession of ASIC designer 25/27
26 SWS h 120 h 210 h ECTS 7.0 Module manager Prof. Dr.-Ing. Elke Mackensen every year (SS) Applicability of the advanced module in the EIM Master’s course Laboratory VLSI-Design Art Labor No. E + I2235 Course content The VLSI-Design laboratory supplements the VLSI-Design lecture with the practical application of what has been learned in relation to the design process. In the laboratory, you run through a complete ASIC design flow using professional ASIC design software, i.e. you will design a small mixed signal chip. A software from Cadence, Mentor Graphics and Synopsis, which is widely used in the industry, is used. As part of the laboratory, you will learn how to use such professional software and, in particular, how to handle and interpret the resulting data, e.g. Simulation data. Laboratory Instructions for the VLSI Design Laboratory Documents for the VLSI Design Lecture Cordes, K.-H., Waag, A., Heuck, N., Integrated Circuits, Basics - Processes - Design - Layout, M & uumlnchen, Pearson Studium, 2011 Albers, J ., Basics of integrated circuits, components and microstructuring, 2nd edition. M & uumlnchen, Carl Hanser Verlag, 2010 Hoffmann, K., System integration, From transistor to large-scale integrated circuit, 3rd edition. M & uumlnchen, Oldenbourg Wissenschaftsverlag GmbH, 2011 Jansen, D., Handbook of Electronic Design Automation, M & uumlnchen, Vienna, Carl Hanser Verlag, 2001 VLSI-Design No. E + I2234 Course content Introduction to microelectronics and the VLSI-Design Design process of VLSI circuits Pasture recreation Physical basics Semiconductor technology Manufacturing technologies of integrated circuits Standard processes of IC manufacturing using the example of the LOCOS process Design of integrated CMOS circuits (analog and digital) Cordes, K.-H., Waag, A., Heuck, N., Integrated circuits, Basics - Processes - Design - Layout, M & uumlnchen, Pearson Studium, 2011 Albers, J., Basics of integrated circuits, components and microstructuring, 2nd edition, M & uumlnchen, Carl Hanser Verlag, 2010 Hoffmann, K., System integration, From transistor to large-scale integrated circuit , 3rd edition, M & uumlnchen, Oldenbourg Wissenschaftsverlag GmbH, 2011 Jansen, D., Handbook of Electronic Design Automation, M & uumlnchen, Vienna, Carl Hanser Verlag, / 27
27 Applied Research Laboratory / Studio 1 to 2 semesters 60 h 150 h 210 h ECTS 7.0 Prerequisites Graded practical laboratory work Module respons. Prof. Dr. Tobias Felhauer Max. Participants 1 semester EIM1 and / or EIM2 every year (SS) Applicability of the EIM Master’s course, advanced module Laboratory Applied Research Type Laboratory no. During this time you will be instructed and supervised by the laboratory manager. Finally, a project report must be drawn up and graded. may be specified by the project supervisor on a project-specific basis 27/27