X-ray Analysis

This laboratory manual originated from eighteen years of teaching the
class Inorganic Preparations, which follows the Descriptive Inorganic
Chemistry course in the Inorganic Chemistry curriculum of Missouri State University (USA). Both courses are designed for chemistry majors. They represent a logical progression and harmonic combination of theoretical background in the discipline at first, with enhancement and retention of gained knowledge during following experimental laboratory work. This course is designed for lab sessions of four hours each.
The book provides an extensive and necessary introduction for students to typical glassware and lab equipment (labware) which are normally used in the synthetic chemistry laboratory. This introduction is followed by a brief description of the main laboratory procedures and operations that are essential for safe and productive laboratory work. These were limited to: filtration, extraction, distillation and reflux, work with vacuum,
anaerobic/moisture free procedures, flash column and preparative thinlayer chromatography, and products recovery from solutions. In this
context it is very important to note that this laboratory manual is neither
intended to promote or advertise any of the equipment brands and their
manufacturers, nor it is intended to show off, or brag about the laboratory capabilities that exist at the authors’ institutions! In fact, the glassware, apparatuses and equipment used in this book fit very well into the average teaching and research facilities typical of numerous institutions of higher education around the world. Moreover, during the description of laboratory glassware, hardware and laboratory methods at the beginning of this manual, special attention is drawn to inexpensive alternative solutions when building equipment for common procedures, as well as to cost-saving lab techniques.

All preparative experiments are designed for the synthesis of grams’
quantities of compounds. This ensures students’ satisfaction with the
whole process of the synthesis, work-up procedures and post-lab handling of substances, many of which will be further studied. This manual is heavily illustrated with 224 figures, 12 schemes and 20 tables, to aid students in carrying out all experiments and to help them learn laboratory techniques. The main purpose of such an illustrative approach is to go in step with a new and younger generation of visual learners, who, in the digital age of the internet and mobile devises, truly value the old sentiment that ‘a picture is better than a thousand words’. Almost all illustrative material was produced by the authors, taking photographs from actual lab equipment and setups, or making drawings using freely available software.

Before the description of many experiments and characterizations of the
obtained compounds, there are brief and condensed sections of theoretical background information. These allow the reader to get familiar with the topic that follows. Thus, the following physical methods and techniques are presented in these short introductory sections: 1) thermal analysis, 2) X-ray diffraction methods, 3)  molecular weight determination - cryoscopic measurements, 4)
cyclic voltammetry measurements in solutions, 5) solutions electrical conductivity measurements, 6) magnetochemistry in solid state and in solution, 7) spectroscopy (vibrational, electronic, 1H and 13C NMR).

The concept of indirect learning has been used by authors for many years. In our academic settings, that means splitting a class of students into two equal groups, both of which conduct the same kind of experimental preparations, but use different compounds and some alternative work-up and samples handling details. There are laboratory exercises with extensions A, B, or C. Being in the same laboratory for four hours, students, in an indirect way, learn what their peers in the other group are working on. All experiments are presented in clear, step-by-step fashion to help students to carry out particular syntheses, conduct important procedures, and accomplish necessary measurements. All sections in the book are supplied with appropriate literature references for the reader interested in further learning.
During the course of these lab experiments, suitable single crystals of several compounds were grown by students, and subsequently characterized using the X-ray analysis. The main results of this work are
presented and discussed in this manual, with all CIFs for five determined
structures deposited into the Cambridge Crystallographic Data Center
(CCDC).

Therefore, a combination of specially selected series’ of experiments,
with alternative lab work, accompanied with paragraphs of short and
concise theoretical background, and detailed examples of calculations,
make this book truly unique in the modern academic environment. This
book also can be a useful reference for other synthetic chemists not limited to the inorganic/coordination chemistry field, who will be interested in the interpretation of vibrational, electronic, and - more importantly – 1D and 2D NMR spectra.

In summary, according to numerous students' feedback and evaluations, it is engaging, very intense, and yet likeable, and is considered to be a useful class. It has been a popular laboratory course, with 120+ chemistry majors who have enjoyed taking it, thus far.

"Alameda Brown Ware and San Francisco Mountain Gray Ware Technology and Economics" addresses topics related to the production and distribution of Alameda Brown Ware and the consumption of San Francisco Mountain Gray Ware as reflected in archaeological collections from 41 sites that date from about A.D. 400 through the early-to-mid A.D. 1100s and which are located along U.S. 89 north of Flagstaff, Arizona. The chapter represents the most successful application of the petrofacies approach to sand temper provenance determination to date, given that the compositional data are evaluated using oxidation/refiring of clay and sherd samples, inductively coupled plasma-mass spectrometry (ICP-MS) analysis, x-ray analysis, and direct evidence of production collected from project area sites. Building on the work of Dean Arnold (1985), included are four tables that summarize ethnographic/ethnoarchaeological data which should prove useful in reconstructing pottery production and distribution systems elsewhere. Table 5.1 reports 64 new distance to clay resource measurements. Table 5.17 reports annual ceramic production rates in 25 potting communities. Table 5.23 summarizes examples of the goods and services exchanged for ceramics. Table 5.24 summarizes 12 distance traveled by foot  to trade pottery measurements.

We have tested an X-ray diode working in reflection geometry, which uses commercial spark-plugs as plasma cathode. The results of the characterisation work confirm that the spark-plug plasma cathode is a reliable and long-lifetime electron source for X-ray diodes. After more than 10^6 shots, the X-ray dose, uniformity, and ionisation rate values guarantee an effective preionisation of excimer laser discharges. Owing to both the long lifetime and the substantial absence of maintenance, this X-ray diode seems suitable to preionise commercial gas lasers, such as excimer and TEA CO2 lasers.

Particle-Induced X-ray Emission (PIXE) analysis was employed to characterize Hydroxypropyl Methylcellulose (HPMC) polymer film via depth profiling on silicon-based substrates, and compared with Rutherford Backscattering Spectrometry (RBS) results. We utilize the concept that α particle incident energy loss by the polymer film affects the α particle penetration depth into the substrate, and can thus find the areal density of the film by computing the amount of energy loss via comparing the yield of X-ray emitted from a substrate element with and without the polymer film. It is demonstrated in this paper that this method and RBS measurements both yield comparable results for areal densities ranging from 1018 to several 1019 atom/cm2. A collection of techniques including PIXE, RBS, Tapping Mode Atomic Force Microscopy (TMAFM), and Sessile Drop contact angle method were used to compute surface free energy, analyze surface topography and roughness parameters, determine surface composition depth profiling, and to predict the water affinity and condensation behaviors of silicates, phosphosilicates, and other compounds used for high impact resistance vision ware coatings. The visor surface under study is slightly hydrophilic, with root mean square of surface roughness on the order of one nm, and surface wavelength between 200 and 300 nm. Water condensation is manifests itself under sports conditions with raised temperature and humidity. Water condensation can be controlled on such surfaces via polymers adsorption. HPMC polymer surface composition is previously determined via 4.265 MeV 12C(α, α) 12C , 3.045 MeV 16O(α, α)16O nuclear resonance analysis (NRA), and 2.8 MeV elastic recoil detection (ERD) of hydrogen1, and combined with PIXE depth profiling technique as detailed in this work to support the analysis of the surface water affinity and topography and therefore control condensation behavior2. HPMC film between 1018 and 1019 atom/cm2 is found to effectively alter the water condensation pattern and prevents fogging by forming a wetting layer during condensation.