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18 Cards in this Set

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What does Atomic spectroscopy study?

Metals, right hand side of the periodic table.


(Pb,Fe etc)

Why do you need to know metal content in drugs?

Somemetals are good catalysts in degradation reactions. These would decrease theshelflife of drug products.

Where do these metals come from?

1.If these metals arepresent in a sample this is due to contamination from the productionprocess/starting materials.


2. Strong acids/Thiolsused in the production process attack vessels and this could end up in the drugproduct.

Metal limits in drugs?

lessthan 10-20ppm

What are the 4 components in Atomic absorption spectroscopy?

1.Source of light 2. Method of producing gaseous metal atoms (flame) 3.Monochromater to separate light. 4. Photomultiplier (detector)

How hot is the flame in atomic absorption spectroscopy and What gas is used to aid the flame?

1. 2500-3150k


2. N2O since it gave a higher amount of oxygen (33%)

Linear range of atomic absorption spectroscopy?

The liner range is 1-5mg L-1

General Advantages/Disadvantages

1. Wide range of metals can be detected, there is a lamp for almost every element.


2. Process can be automated.


3. Cannot be left overnight due to flame.

Interferences in AAS

1. Chemical (due to insolubility) - Add a realising agent such as 10% lanthium solution/ EDTA


2.Alkaline and earth metals easily ionise , so add a large excess for determination


3.Transport of sample, solutions should have the same viscosity.

Why is Standard addition used in AAS?

Thisis so that matrix effects are overcome however there are errors due to lineextrapolation and errors if the unstrument is not zero-ed. This also assumesline linearity.

Increasing sensitivity in AAS?

1. Use better solvent extraction (less solvent -> higher concentration). Use an organic solvent


2. Generate hydrides using NaBH4


3. Cold vapour generation

Why is absorption used and not emission?

1. Greater stability of spectrometer


2. Fewer interferences


3. Greater sensitivity


4. Different lamp for each experiment.

Advantages of AA?

1. Rapid


2. Easily automated (however cannot be run unattended)


3. Generally free from interferences


4. Known interferences can be overcome.5. Little sample pre-treatment.

What is Flame photometry?

Flame photometry is an atomic emission method for the routine detection of metal salts, principally Na, K, Li, Ca, and Ba

Advantages of flame photometry?

1. Simple equipment, limited number of elements Na, Ca, K, Li, Rb


2. Linear range is 0-10 mgL-1 Na and K


3. Tends to drift over time. Needs to run standard at the same time assamples

What is ICP-OES/MS?

Inductively coupled plasma atomic emission spectroscopy used to detect trace metals using plasma that has a temperature of 6000-10,000K


(OES - Optical emission spec, MS- Mass spec)

Advantages of ICP-OES/MS?

60 elements can betested simultaneously including halogens and non-metalsVery wide dynamicrange, sensitivity is better than flame AA.Can determine tracemetals and high concentrations at the same time.


ICP-MS uses massspec, this is to overcome interference by overlapping emission lines.

Disadvantages of ICP-OES/MS?

ICP-MS uses massspec, this is to overcome interference by overlapping emission lines.