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
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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.
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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)
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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
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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
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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

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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

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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

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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

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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

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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

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Questions
IUK107 Part 2 Other Window of Chemistry for Technologists

1. Quiz 1 2. Quiz 2

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

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Concept Map - together

IUK107 Part 2 Other Window of Chemistry for Technologists

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

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