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Concept Map Iuk107

The document discusses analytical techniques for analyzing organic and inorganic samples. It focuses on biomass samples and describes several techniques for characterization including UV-vis spectroscopy, atomic absorption spectroscopy, inductively coupled plasma, infrared spectroscopy, nuclear magnetic resonance spectroscopy, gas chromatography-mass spectrometry, scanning electron microscopy with energy dispersive X-ray analysis. It provides an overview of each technique and guidance on selecting the appropriate technique depending on whether the sample contains organic or inorganic components and whether it is a solid, liquid or gas.

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Anis Keww
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© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
386 views

Concept Map Iuk107

The document discusses analytical techniques for analyzing organic and inorganic samples. It focuses on biomass samples and describes several techniques for characterization including UV-vis spectroscopy, atomic absorption spectroscopy, inductively coupled plasma, infrared spectroscopy, nuclear magnetic resonance spectroscopy, gas chromatography-mass spectrometry, scanning electron microscopy with energy dispersive X-ray analysis. It provides an overview of each technique and guidance on selecting the appropriate technique depending on whether the sample contains organic or inorganic components and whether it is a solid, liquid or gas.

Uploaded by

Anis Keww
Copyright
© Attribution Non-Commercial (BY-NC)
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Other Chem Window

IUK107 Part 2 Other Window of Chemistry for Technologists

1. Materials: synthetic (IUK 107 Part 1) & natural (IUK 107 Part 2) 2. Trendy natural: Biomass 3. Inorganic component is naturally contained in biomass 4. Analysis should include inorganics: Uv-vis, AAS, ICP, EDAX. 5. Previous organic analysis included: IR, NMR, (+GC-MS)
02/12/2013 Concept Map - Part 2 IUK107 - Other Chem Window for Technologists 1

Concept Map
IUK107 Part 2 Other Window of Chemistry for Technologists

5 December 2013

1.Organic & Inorganic Samples: Preparation Concept & Analyses 2Touch up on MS of Halogenated Compounds

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Concept Map - Part 2 IUK107 - Other Chem Window for Technologists

Summary - Inorganics
IUK107 Part 2 Other Window of Chemistry for Technologists

INORGANICS:
Biomass & Materials

New: fungus on keratinised tissue: Touch on sample preparation: matrix + filler Scanning Electron Microscopy with Energy Dispersive Analysis of X-ray Light & Absorption as Materials Response to Radiation
02/12/2013 Concept Map - Part 2 IUK107 - Other Chem Window for Technologists 3

IUK107 Part 2 Other Window of Chemistry for Technologists

Summary
AAS

Towards relevance in intellectual capacity:


Uv-visible Spectroscopy Atomic Absorption Spectroscopy Inductively Coupled Plasma Quiz 1
UV-VIS ICP

Source
Sample Response

Uv-vis light (many effects)


Low E radiation

HCL Atomise

Plasma Ionise

Power

Furnace: <2000oC Furnace: >2000oC

Group Presentation - excellent collaborative work although too detail. <End of Inorganic >
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Sample preparation
IUK107 Part 2 Other Window of Chemistry for Technologists

INORGANIC
Supposedly

Sample can contain mixture of elements Name 1 that experience inteference if in mixture
Normally Quantitative -calibration curve

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Concept Map - Part 2 IUK107 - Other Chem Window for Technologists

IUK107 Part 2 Other Window of Chemistry for Technologists

Summary

ORGANICS:
Infra-red Spectroscopy functional groups only Nuclear Magnetic Resonance Structure proposal Mass spectroscopy structure verification Gas Chromatography-Mass Spectrometry -separation technique interfaced with speciation of fragmented molecule.
02/12/2013 Concept Map - Part 2 IUK107 - Other Chem Window for Technologists 6

Sample preparation
IUK107 Part 2 Other Window of Chemistry for Technologists

ORGANIC
Borrowed pic dont confuse Required due to instrument limitation at handling mixture Name one technique thats capable

Consequence

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Concept Map - Part 2 IUK107 - Other Chem Window for Technologists

Spectral Responses
IUK107 Part 2 Other Window of Chemistry for Technologists

SEM/EDAX: Electron image | EDX: Intensity vs energy (keV) UV-VIS: 200-800 nm; analyte responses: A vs l (nm) AAS: HCL source; atomisation; atoms A; A vs l (nm) ICP: Plasma source and ioniser; ions A; A vs l (nm)
IR: wavelength =0.78-1000 mm: % transmittance vs 1/l (cm-1 : 400-4000) NMR: nucleus resonance; probe dependent; Intensity vs chemical shift (ppm) GC-MS: GC Separation:intensity vs tR | MS Fragment: Abundance vs m/z (speciation)
02/12/2013 Concept Map - Part 2 IUK107 - Other Chem Window for Technologists 8

IUK107 Part 2 Other Window of Chemistry for Technologists

Sample Form

Uv-visible Spectroscopy All - colour Atomic Absorption Spectroscopy Inductively Coupled Plasma SEM/EDX S, organic, inorganic-EDX Infra-red Spectroscopy:L/S/G Nuclear Magnetic Resonance: PROBE - L/S Gas Chromatography-Mass Spectrometry L/G volatile, stable <400oC.
Inorganic

organic

liquid quantitative
9

02/12/2013

Concept Map - Part 2 IUK107 - Other Chem Window for Technologists

Stepwise Analysis - organics


IUK107 Part 2 Other Window of Chemistry for Technologists

Uv-vis where colour is present

IR
Scan the functional group of a molecule Pure or reference/standard/expertise /familliarity required

Functional region: 15004000 cm-1

NMR
structural elucidation Pure or simple mixture

Fingerprint:
500-1500 cm-1
Atlas/Database match

MS
verify/confirm elucidated structure Must pure or need standards
Concept Map - Part 2 IUK107 - Other Chem Window for Technologists 10

Mixture is ridiculous
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Stepwise Analysis Inorganics


IUK107 Part 2 Other Window of Chemistry for Technologists

Uv-vis where colour is present

SEM/EDX
Check types of elements Proceed with quantitative techniques

AAS
Decide on hollow cathode lamp Prepare standards Find sample digestion procedure

ICP
Allows us to skip SEM/EDX and AAS To some extent, ICPMS rules out the need for XRD, XRF, XPS

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Concept Map - Part 2 IUK107 - Other Chem Window for Technologists

11

Stepwise Analysis Totally unknown (s & l)


IUK107 Part 2 Other Window of Chemistry for Technologists

Start off: SEM/EDX

If (l): Start off: IR for Image identify variation (# of forms) functional Semiquantitative via EDX group.
Check the types of elements present Check presence of C
If none check ash % If C present, analysis of inorganics requires ashing procedure Next proceed woth analysis.

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Concept Map - Part 2 IUK107 - Other Chem Window for Technologists

12

Important Examples
CH2Cl2
Calculate MW. This is for M+ Check radioisotopic probability:
M+ and all M+ +2 Abundance: 50:50% (note complexity)

Draw: Indication:
IUK107 - Part 2. Separation and Speciation: GC-MS

13

Mass Spectroscopy
IUK107 Part 2 Other Window of Chemistry for Technologists

1. CH2CCl2

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Concept Map - Part 2 IUK107 - Other Chem Window for Technologists

14

Important Examples
CH2Br2
Calculate MW. This is for M+ Check radioisotopic probability:
M+ and all M+ +2 Abundance: 50:50% (note complexity)

Draw: Indication:
IUK107 - Part 2. Separation and Speciation: GC-MS

15

Mass Spectroscopy
IUK107 Part 2 Other Window of Chemistry for Technologists

1. CH2Br2

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Concept Map - Part 2 IUK107 - Other Chem Window for Technologists

16

Questions
IUK107 Part 2 Other Window of Chemistry for Technologists

1. Quiz 1 2. Quiz 2

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17

Concept Map - together


IUK107 Part 2 Other Window of Chemistry for Technologists

02/12/2013

Concept Map - Part 2 IUK107 - Other Chem Window for Technologists

18

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