Spectroscopy Europe Vol. 33 No. 5 (2021)

The Pyramids of Giza and the Great Sphinx, Egypt

Spectroscopy since 1975

Vol 33 No 5 July August 2021

3 Editorial 4 News 21 Are carbon micro-clusters in the Khufu pyramid blocks of organic origin Guy Demortier 30 Struc

Vol 33 No 5 July August 2021

PIGE and PIXE have been used to reveal that some blocks of the Khufu (Great) Pyramid at Giza were cast in situ: Egypt

Publisher Ian Michael E-mail: ian impopen com Advertising Sales Ian Michael IM Publications Open, 6 Charlton Mill, Ch

ISSN: 2634-2561

Spectroscopy Europe is published by IM Publications Open LLP, 6 Charlton Mill, Charlton, Chichester, West Sussex PO18

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Spectroscopy Europe is a digital magazine, published eight times a year and available free-of-charge to qualifying in

method for the detection of natural, solid TNT John Hammond continues his series of Quality Matters Columns looking

We have a bumper issue with three articles Roman concrete is well known and has lasted well Now, it seems that the

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MS-based alien life detector University of Glasgow researchers have developed a new method called Assembly Theory whi

approaches, however, it is the first to be experimentally measurable The team demonstrated that it was possible to e

ZooMS provides new insights on animals in the African past In order to understand foodways and subsistence strategies

Experimental correlation of mass spectrometry data to MA and MA analysis of mixtures Reproduced from doi org 10 1038

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ambiguous or unidentifiable bone fragments However, the lack of complete reference peptide markers for African anima

Raging Raman Researchers from the Single-Cell Center at the Qingdao Institute of Bioenergy and Bioprocess Technology

Raman-Activated Gravity-driven single-cell Encapsulation and Sequencing, or RAGE sequencing This sequencing techniqu

A yellow backed duiker at the Knoxville Zoo Credit: University of Tennessee, Knoxville

A technique to sort and sequence the genome of bacteria in soil one bacterial cell at a time Credit: Liu Yang

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bacteria with D2O, the general metabolic activity of the cells can be tracked via their Raman spectra The technique

misleading analysis results due to an erroneous assumption during calibration XPS is a standard method in materials

Criticism of the method was raised as early as the 1970s and into the early 1980s After that, however, knowledge abo

Grzegorz Greczynski, senior lecturer in the Department of Physics, Chemistry and Biology at Linköping University Cre

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a quantitative, label-free assay platform integrating nuclear magnetic resonance (NMR) spectroscopy and mass spectrom

patients were statistically more likely to have biochemical abnormalities This is an immensely dangerous disease tha

Bruker has begun validation of this integrated NMR MS clinical research assay set in Europe, with the goal of develop

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Company News Oxford Instruments acquires WITec Oxford Instruments has acquired WITec for a cash-free, debt-free consi

other coronaviruses Results were evident in under five minutes Their research was published in ACS Nano (doi org gk

in its electronic energy , Berry said In this experiment, we modified graphene with an antibody and, in essence, ca

An illustration of the graphene-based COVID-19 spike protein detection process The white rectangle represents the su

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24-year track record of making WITec a prosperous and innovative Raman imaging company Now that we are joining the O

the limitations are in the read-out of the device The study suggests several potentially simple modifications to lat

and the beamline staff, including beamline scientists and technicians as well as the continuing user support from var

WITec s representatives following the official announcement at WITec Headquarters in Ulm, Germany From left to right

WITec will, of course, fulfil its obligations toward existing customers and business partners in the usual manner and

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JEOL and SCiLS sign distribution agreement for MSI software SCiLS Lab is software for mass spectrometry imaging, prov

important after the medication has been removed from its initial packaging and blister and then been placed in unlabe

hampers reliable rapid diagnostic methods in everyday clinical practice In addition to histological typing, the tumo

EinverständniserklärungsNr: 2216a, 2217a, 2218a,  Frederik Großrüschenkamp, Nina Goertzen, Klaus Gerwert  Die Bilder dürfen nur im Kontext der Ruhr-Universität Bochum (RUB) unter Angabe des Copyrights RUB, Marquard verwendet werden, zum Beispiel für Webseiten der RUB sowie für Texte oder Webseiten, die sich speziell mit Ereignissen an der RUB oder Leistungen von RUB-Mitgliedern beschäftigen Die Bilder dürfen nicht in Kontexten verwendet werden, in denen die RUB nur stellvertretend für Hochschulen im Allgemeinen steht

Frederik Großerüschkamp, Nina Goertzen and Klaus Gerwert (from left) are part of the research team RUB, Marquard

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We are thrilled Jeff has joined IonSense as his experience positions him well to lead the company and achieve our st

in everyday clinical practice, which can sometimes take several days, the new procedure only takes around half an hou

an inexhaustible supply of pluripotent stem cells—the most versatile of stem cells—that can become any type of cell,

Raman spectroscopy has been used to train an AI so it can monitor if the reprogramming of ordinary cells into stem ce

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causes a problem of bringing the antibody into the cells , Watanabe said Solution of these problems can accelerate

To measure the progress, they assigned the chemical fingerprint of neuronal cells as the transformation starting po

model In this research, published in the Journal of the American Chemical Society (doi org gkrg2j), using the princi

image description

Schematic diagram of the principle of the general surface enhanced Raman spectroscopy method for actively capturing t

New SERS method actively captures target molecules in small gaps

Professor Yang Liangbao, from the Institute of Health and Medical Technology, Hefei Institutes of Physical Science (H

general surface-enhanced Raman spectroscopy (SERS) method for actively capturing target molecules in small gaps based

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can detect chemical variations at length scales much smaller than a human cell There is no reason to think that ever

their presence in the brain, and in fact it is not yet clear whether such particles are indeed linked to disease The

very presence underlines the importance of the future work now needed to learn about the way in which metals are proc

The experimental team at I08 Diamond left to right: James Everett, Jake Brooks and Frederik Lermyte Credit: Keele Un

X-ray microscope images and X-ray absorption spectra obtained from two AD plaque cores, measured at Diamond Light Sou

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paths for the instrumental performance of the Diamond I08 Scanning X-ray Microscopy Beamline These new findings off

of lithium-ion batteries She has been instrumental in the development of next-generation batteries and cost-effectiv

At the time Grey was still a student, most chemist and physicists used X-rays to determine the internal structure of

Professor Clare Grey Credit: Gabriella Bocchetti; Cambridge University

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optimising the NMR method to design even more powerful, faster-charging and more environmentally friendly batteries

of molecules and chemical bonds in crystalline organic inorganic hybrid thin films deposited on a substrate as small

light, revealing their orientation Any lab with a 3-D printer can make these ATR optical setups This method, which

3D printable optical setup with built-in sample chamber for an FT-IR spectrometer Sample is put on the Si ATR crysta

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Lausanne s Institute of Physics of the School of Basic Sciences The scientists used a compact 100 mm-long device, to

AlInGaN system is a highly robust and mature semiconductor platform that shows strong excitonic optical transitions u

key to the device s success Moreover, an advanced algorithm plays an equally important role in this spectrometer, pa

Schematic of AlInGaN polariton waveguide structure Courtesy of Dr Paul Walker, University of Sheffield

Ultracompact on-chip computational infrared spectrometer With potential applications that range from detecting greenh

An optical micrograph of two typical on-chip spectrometers Scale bar: 8 m

operational at a 2 9 m wavelength range, based on a single tuneable photodetector The material, which is about 10 n

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involved in the IR detection process, and the image, converted to the visible, can be captured by eye or a phone-type

With this idea in mind, researchers from The Australian National University, Nottingham Trent University and collabor

the use of counter-propagating excitation beams, as well as incidence at different angles and, most importantly, mult

Through the sum-frequency generation (SFG) non-linear optical process, two incident photons, one of them in the IR sp

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typically in the XUV region To be able to obtain intense XUV pulses, it is important to generate as much XUV light a

are generated (2) The generated XUV beam is large and has a large divergence and can, therefore, be focused to a sma

and four XUV photons, respectively In spite of the small footprint of this intense XUV source, the obtained XUV inte

Compact intense XUV source An NIR pulse (red) is focused, and high harmonics are generated in a gas jet that is plac

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Are carbon micro-clusters in the Khufu pyramid blocks of organic origin PIXE and PIGE reveal the construction of Giz

Introduction The interdisciplinary approach of the technique of construction of the Big Pyramids of Egypt is a subjec

Hawass, former minister of the Egyptian Antiquities who was initially sceptical about the Morishima s conclusions of

of mixed materials 9 In addition to the already reported elemental analysis of Na, S and Cl associated with natural l

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Rectangle

Guy Demortier has a PhD in nuclear physics, is Emeritus Professor of Physics at University of Namur, Belgium, Co-foun

Rectangle

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They were crushed and pressed to obtain flat circular pellets without any additional binder (Figure 3) The sampling

Figure 1 The PIXE microprobe chamber at Atomki (Debrecen, Hungary)

Figure 2 Micro-PIXE maps of a copper grid on a carbon substrate Left: copper; data collected with the Be windowed d

Figure 3 Pellet samples on their target holder

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Micro-PIXE analysis of Egyptian pyramid blocks The choice of the positions of the SUTW and Be-windowed detectors inst

Figure 4 Information depth for C, O and Ca in CaCO3

Figure 5 PIXE spectra collected by SUTW detector (left) and Be-windowed detector (right) on the homogeneous Corning

characteristic lines of elements from CKa upwards as well as escape and pile-up peaks present in the spectra are fitt

in the SUTW detector could indeed suffer from partial interference with the La line of Fe (705 eV): iron is indeed pr

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(around 15 30 m in diameter) of Al, Si and Fe can also be observed in addition to nearly pure calcium carbonate (C,

Figure 6 PIXE spectra collected by SUTW detector (left) and Be-windowed detector (right) on a limestone sample from

Figure 7 PIXE spectra collected by SUTW detector (left) and Be-windowed detector (right) on a sample of the external

Figure 8 Flatness check of pellet samples by comparison of CaKa maps in both detectors

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Figure 9 Distribution maps of 14 elements in Tura quarry sample (1 mm 1 mm)

Figure 10 Distribution maps of 14 elements in Maadi quarry sample (1 mm 1 mm)

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Figure 11 Distribution maps of 14 elements in FH123 Khufu Great Gallery sample (1 mm 1 mm)

Figure 12 Distribution maps of 14 elements in VT3 outside block of Khufu (1 mm 1 mm)

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Figure 13 Distribution maps of 14 elements in 15a outside block of Khufu (1 mm 1 mm)

Figure 14 Distribution maps of 14 elements in 15b outside block of Khufu (1 mm 1 mm)

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of sodium chloride Nevertheless, the Na signal is always higher than what is needed to form NaCl (as confirmed by me

in both Ca and O maps as shown in the central upper part of maps, indicates that the CKa line is produced deeper than

Conclusion Elemental distribution maps of C, O, Na, S, Cl and Ca clearly indicate that the structure of the samples o

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References 1 K Morishima, M Kuno, A Nishio, N Kitagawa, Y Manabe, M Moto, F Takasaki, H Fujii, K Satoh, H

$5 J Davidovits, X-ray analysis and X-ray diffraction of casing stones from the pyramids of Egypt, and the limeston$

11 G Demortier, G Quarta, K Butalag, M D Elia and L Calcagnile, X-Ray Spectrom 37, 178 (2008) https: doi org

Guy Demortier has a PhD in nuclear physics, is Emeritus Professor of Physics at University of Namur, Belgium, Co-foun

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Structural, dielectric and Raman spectroscopic study of complex electric and magnetic interactions in multiferroic io

Introduction While ordinary materials are usually either magnetically or electrically ordered, a relatively new class

Raman spectroscopy with suitable laser sources One particular interesting system is MnWO4, in which the Mn2+ is the

On the other hand, the variation of non-magnetic ions can help to increase the ion displacements and the spin-induced

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Dr Holger Gibhardt studied physics in Heidelberg and Aachen (Germany) and graduated from Aachen in 1994 with the dip

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final sintering were applied in order to produce well-defined samples of a series of compositions of MnW1 xMoxO4 wi

$Group III (blue): 0 65 x 1: the diffraction pattern consists of the reflections of pure MnMoO4 and the four-fol$

novel solid-state red laser Solo640 (UNIKLASERS), which meets these requirements very well This laser has a waveleng

$Figure 1 X-ray diffraction pattern of sintered MnW1 xMoxO4 samples with different concentrations Different colour$

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et al ,4 there is a saturation near x 0 35 at TC 14 7 K more than 2 K higher than for pure MnWO4 The results of

in multiferroic MnWO4 , Mater Res Express 2, 096103 (2015) https: doi org 10 1088 2053-1591 2 9 096103 2 L Med

3 L Y Chang, Subsolidus phase relations in the system ZnWO4-ZnMoO4-MnWO4-MnMoO4 , Mineral Mag 36(283), 992 996

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Figure 3 Left: temperature dependence of the real part of the dielectric permittivity of MnW1 xMoxO4 for different

Figure 2 Raman spectra of sintered MnW1 xMoxO4 samples with different concentrations The three concentration regi

Dr Holger Gibhardt studied physics in Heidelberg and Aachen (Germany) and graduated from Aachen in 1994 with the dip

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Surface-enhanced Raman spectroscopy for selected energetic material detection Mohamed Mokhtar,* Tamer Wafy and Mahmou

Introduction Nowadays, with terrorism attacks around the World, researchers are looking at ways to reduce both civili

problem as it affects directly both living aquatic species and humans 2 Various analytical techniques have been used

identify the investigated sample 7 10 The mechanism of the Raman spectroscopy detection process is that the incident

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Mohamed Mokhtar had obtained his BSc and MSc (Chemical Engineering) from the Military Technical College, Cairo, Egypt

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Mahmoud Abdelhafiz obtained his BSc and MSc (Chemical Engineering) from the Military Technical College, Cairo, Egypt

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Tamer Z Wafy graduated from the Chemical Engineering branch of the Military Technical College (MTC), Egypt in 1997,

Rectangle

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excitation of these particles When these excited nanoparticles return back to their relaxation mode, the emitted rad

and diglycidyl ether of bis Phenol A (DGEBA) of EEW 500 epoxy and polyamide as a hardener were purchased from ISPAC

Ag-nanoparticles Two of them were then coated: substrate B was coated with a 0 01 mm epoxy layer and substrate C was

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Figure 1 Preparation of SERS substrates

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(EDS) for elemental analysis was conducted to confirm the nature of the Ag-nanoparticles on the substrate SERS for e

the substrate from the analysis of the real samples) 0 01 mg of the explosive powder was put on the membrane substra

Results and discussion UV-vis spectroscopy UV-vis spectra of the prepared Ag-nanoparticles in the spectral range 200

Figure 2 UV-vis spectrum of Ag-nanoparticles sample

Figure 3 Several selected points for Raman analysis of pure Ag-nanoparticles on substrate

Figure 4 Several selected points for Raman analysis of Raman spectrum of TNT + Ag-nanoparticles on substrate at 785 nm

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get a good spectrum for TNT Different peaks were seen in the range between 1700 cm 1 and 100 cm 1 Peaks at 1616 cm

Figure 5 Raman spectrum for TNT sample alone and TNT sample on the prepared substrate A using a laser source at 785

Figure 6 Raman spectrum for TNT sample alone and Raman spectrum for TNT sample on the prepared substrate B using a l

Figure 7 Raman spectrum for TNT sample alone using a laser source of 532 nm and power of 2 5 mW and TNT sample alone

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as 532 nm This is a good verification that substrate A significantly enhances the peak at 2956 cm 1 when we use a Ra

elastomer—gave clear results when the 532 nm laser source with 2 5 mW power was used The decrease in the intensity o

Ag-nanoparticles are in the size range 130 250 nm and are distributed evenly through the substrate From the EDS anal

Figure 8 SEM spectroscopy of substrate A (Ag-nanoparticles on filter paper substrate)

Figure 9 EDS elemental analysis for substrate A

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Author contributions The manuscript was written through contributions of all authors All authors have given approval

References 1 W O Rivera, Standoff Raman Spectroscopy System for Detection of Explosives, Chemical Warfare Agents Si

Techniques (2012) https: doi org 10 5162 IMCS2012 P2 3 11 4 N Zhang, L Tong and J Zhang, Graphene-based enhanc

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Figure 10 EDS elemental distribution pattern of substrate A

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for remotely detecting trace explosives , Lincoln Lab J 17(2), 1 (2008) https: www ll mit edu about lincoln-labor

and J Zhang, Surface enhanced Raman spectroscopy on a flat graphene surface , Proc Natl Acad Sci USA 109(24), 9

of TNT by imprinting molecular recognition using a new type of stable substrate , Chem Eur J 16(42), 12,683 12,693

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VOL 33 NO 5 (2021)

Mohamed Mokhtar had obtained his BSc and MSc (Chemical Engineering) from the Military Technical College, Cairo, Egypt

Tamer Z Wafy graduated from the Chemical Engineering branch of the Military Technical College (MTC), Egypt in 1997,

Mahmoud Abdelhafiz obtained his BSc and MSc (Chemical Engineering) from the Military Technical College, Cairo, Egypt

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QUALITY MATTERS

Metrology (OIML) was held at NBS in Washington, DC Six international organisations and 12 countries were represented

TC 334—Reference Material continues in 2021 and beyond, and the key likely changes are detailed here 1st Generation:

Four generations of quality: measuring up New ISO committee for reference materials committed to excellence in accu

Introduction This article, the fourth in the series, details the ISO technical committee that is responsible for refe

DOI: 10 1255 sew 2021 a24 2021 The Author Published under a Creative Commons BY-NC-ND licence

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John Hammond is an experienced analytical scientist, spectroscopist and technical marketing professional, skilled in

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QUALITY MATTERS

VOL 33 NO 5 (2021)

Oval

Oval

Oval

4) To prepare guidelines for technical committees for making reference to RMs in ISO documents To prepare guidelines

ISO Guide 30 Terms and definitions used in connection with reference materials : harmonises the vocabulary used in c

The 15th meeting of REMCO in May 1991 saw Mr S Rasberry (ANSI, NIST) take the Chair of REMCO A revised work program

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QUALITY MATTERS

for certified reference material , and to this day the vast majority are certified for specific applications within

The 20th meeting of REMCO was strongly focused on draft revised Guide 34 based on the ILAC document The ILAC represe

Figure 1 ISO REMCO Committee structure (2020)

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QUALITY MATTERS

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until its disbandment in 2021, was approved The Executive Committee was renamed the Chairman s Advisory Group an

producers as the basis for the accreditation of RM producers instead of the corresponding ILAC Guide 12, and so bega

Figure 2 ISO REMCO Guides and TRs (2020)

Guide(s) under development ISO Guide 85:202x RMs for qualitative property values ISO Guide 86:202x Purity RMs for

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QUALITY MATTERS

VOL 33 NO 5 (2021)

Guide 34 , Spectrosc Europe 29(4), 11 (2017) https: www spectroscopyeurope com quality future-part-2-changes-iso-1

keep you updated in the Quality Matters column, as these details are released So, on reflection, and given the histo

John Hammond is an experienced analytical scientist, spectroscopist and technical marketing professional, skilled in

task that the new TC 334 has to consider is how to meet this requirement and convert these Guides into the appropriat

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Sampling COLUMN

Sampling vs analytical error: where the money is Pentti Minkkinen Professor emeritus, Lappeenranta Lahti Universi

VOL 33 NO 5 (2021)

Sampling for analysis is a multi-stage operation, from extracting a primary sample (s1) via sub-sampling (s2) (s3)

Along the full lot-to-analysis pathway Analytical measurements comprise at least two error generating steps: delineat

(1) This variance can be reduced (always popular for those who worry about the total sampling-plus-analysis error)

Master example: the effectiveness of replication The following example will help gain insight into where efforts to r

DOI: 10 1255 sew 2021 a25 2021 The Author Published under a Creative Commons BY licence

Pentti Minkkinen received his MSc (eng ) from Helsinki University of Technology in 1969 He then worked as an Associa

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Sampling COLUMN

This example demonstrates that even if the best and most expensive analytical technology available is used in the l

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First, there is no significant difference between them if the process standard deviation is estimated from all nine s

are needed Operators usually can estimate the cost structure, but the variance estimates can seldom be estimated the

Figure 1 A: Random sampling: sampling times or locations are selected randomly B: In stratified (random) sampling t

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Sampling COLUMN

empirical results recommended a new sampling system to be implemented—this was accepted In comparison to the old, th

the payback time of the audit and the panel investigations was about 12 h It does not have to be expensive to invoke

at different EU ports were sampled by collecting 100 primary 0 5-kg samples (each containing approximately 3000 beans

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Sampling COLUMN

number of samples needed to reach a specified quality specification—compared to informed TOS-competent understanding

that something is not right A TOS rationale follows below Involving TOS The mass of aflatoxin in a single mould

of the primary sample size For the two lot averages used here as examples, aL is 0 02 mg kg 1 and 0 005 mg kg 1, and

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Sampling COLUMN

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the target In sample preparation, if the secondary samples are each 10 kg and the analytical sample from which the t

control measurements First, then is it possible to set realistic decision limits so that they can be reached with me

soybean sampling for GMO control , Trends Anal Chem 32, 154 164 (2012) https: doi org 10 1016 j trac 2011 09 008

Pentti Minkkinen received his MSc (eng ) from Helsinki University of Technology in 1969 He then worked as an Associa

sampling at undergraduate and graduate courses at several universities, at professional continuing education courses,

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SurveyIR and cultural heritage Gildings are commonly found highlighting details of ornamental or iconographic value s

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battery QA QC applications, as the well-resolved spectra of the small organic molecules and ions are ideally suited f

Observing and monitoring electrolyte decomposition by benchtop NMR Lithium-ion (Li-ion) batteries have become ubiquit

ATR analysis of the relative concentrations of active pharmaceutical ingredients lnfrared quantitative analyses are a

Compact mass spectrometers: controlled substance detection Controlled substance analysis is changing with compact mas

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risk of exposure to fentanyl and its analogues, there is a need in law enforcement and decontamination services for a

Pulse sequence diagram of the PFGSE experiment Rectangular hard pulses are shown in orange, and pulsed field gradien

Measuring diffusion at different temperatures using NMR with pulsed field gradients Benchtop NMR instruments have bro

temperature capability allows the study of sample thermal behaviour under a range of expected working conditions Fin

Time-resolved spectroscopy of phosphorescent oxygen sensors in a relevant in vitro environment for biomedical applica

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PRODUCT: FLS1000 Photoluminescence Spectrometer APPLICATIONS: Life sciences n Forensic science & security n Environ

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PRODUCT: Certified Fluorescent Reference Materials APPLICATIONS: Instrumental verification and monitoring n Spectra

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Ocean Insight has introduced the Ocean HDX Raman spectrometer, a compact, high-performance spectrometer for 785 nm Ra

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Infrared Greenhouse gas analyser The Gasera One GHG greenhouse gas analyser is based on the Gasera One platform combi

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Richard D Smith at Pacific Northwest National Laboratory It can separate and identify molecular structures that can

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done also with unbiased single cell proteomics, as cells at different stages in the growth cycle have a protein core

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structural information can be extracted and quantified from diverse compound types Compared to previous systems, the

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Maximum (FWHM) resolution and part-per-billion mass accuracy independent of scan speed The MRT technology features a

SELECT SERIES MRT DESI XS right angle beauty

Thermo Scientific Orbitrap IQ-X Tribrid mass spectrometer

Thermo Scientific FAIMS Pro Duo interface with Thermo Scientific Orbitrap Exploris 240 mass spectrometer

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Mass spectrometer for the semiconductor industry Atonarp has announced the launch of Aston, an in situ mass spectrom

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acquisition control, continuous measurements, additional data processing capabilities and viewing options B&W Tek

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the Flow-UV is used to automate reaction product collection in either Collect All , Steady State or Balanced col

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4 7 July, Skagen, Denmark International Association for Spectral Imaging (IASIM) 2020 iasim net, https: 2020 i

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LTB Lasertechnik Berlin GmbH,info ltb-berlin de www ltb-berlin de en homepage , object Rectangle ,Magritek GmbH sales

object Rectangle ,Starna Scientific Limited sales starna com www starna com, object Rectangle ,Wasatch Photonics inf

VOL 33 NO 5 (2021)

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Related Equipment, object Rectangle ,Bruker Optik GmbH info bopt de bruker com www bruker com optics, object Rectangl

Spectroradiometry, object Rectangle ,ABB Measurement & Analytics ftir ca abb com abb com analytical, object Rectangle

VOL 33 NO 5 (2021)

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$object Rectangle ,Starna Scientific Limited sales starna com www starna com,X-ray Diffraction,Bruker AXS GmbH,info B$

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