FINAL 01 - Chromatography and Test Procedures Flashcards
(146 cards)
1
Q
Relationship is determined by chemical stoichiometry (Types of analytical methods)
A
Classical method
2
Q
Physical or chemical properties of the analyte, but with instrument (Types of analytical methods)
A
Instrumental method
3
Q
More suitable for analysis of major constituents (Types of analytical methods)
A
Classical method
4
Q
Used to certify analytical standards (Types of analytical methods)
A
Classical method
5
Q
Is generally cheaper; only uses buret and reagent (Types of analytical methods)
A
Classical method
6
Q
More accurate and precise (Types of analytical methods)
A
Classical method
7
Q
More robust and susceptible to environmental fluctuations (Types of analytical methods)
A
Classical method
8
Q
Ability to perform trace analysis (Types of analytical methods)
A
Instrumental method
9
Q
Most are multi-channel techniques (Types of analytical methods)
A
Instrumental method
10
Q
Shorter analysis time (Types of analytical methods)
A
Instrumental method
11
Q
Amenable to automation (Types of analytical methods)
A
Instrumental method
12
Q
Larger number of samples may be analyzed quickly (Types of analytical methods)
A
Instrumental method
13
Q
Less skill and training required (Types of analytical methods)
A
Instrumental method
14
Q
Refers to the separation of mixtures due to differences in equilibrium distribution affecting the rate which components of a mixture are carried through a stationary phase by a mobile phase
A
Chromatography
15
Q
Phase that is fixed in place either in a column or on planar surfaces (Phases of chromagraphy)
A
Stationary phase
16
Q
Phase that moves over or through the stationary phase carrying with it the analyte mixture maybe a gas, a liquid, or a superficial fluid (Phases of chromatography)
A
Mobile phase
17
Q
SP: Liquid solvent system, MP: Adsorbed water on the surface of the paper, Examples: Paper, HPLC (General types of chromatography)
A
Liquid-liquid chromatography
18
Q
SP: Adsorbent material (silica gel), MP: Liquid solvent system, Examples: Column, TLC (General types of chromatography)
A
Liquid-solid chromatography
19
Q
SP: Gas, MP: High boiling point liquid, Example: Inert gas (General types of chromatography)
A
Gas-liquid chromatography
20
Q
Common technique used in synthetic chemistry for identifying compounds, determining their purity, and following the progress of a reaction (Types of chromatography)
A
Thin layer chromatography (TLC)
21
Q
Stationary phase (Thin layer chromatography) (TP)
A
TLC plate, paper
22
Q
Mobile phase (Thin layer chromatography)
A
Solvent
23
Q
Solid or liquid supported on solid which stays fixed on the layer (Phases of TLC)
A
Stationary phase
24
Q
Flows through the stationary phase and carries the components of the mixture (Phases of TLC)
A
Mobile phase
25
Compounds will have different affinities for the mobile and stationary phases, and this affects the speed at which it migrates (Types of chromatography)
Thin layer chromatography (TLC)
26
↑ component absorbed onto stationary phase, ↓ time spent in mobile phase, ↓ time to migrate up in the plate (Types of chromatography)
Thin layer chromatography (TLC)
27
↑ similarity of compound to mobile phase, ↑ time spent in mobile phase , ↑ time to migrate up in the plate (Types of chromatography)
Thin layer chromatography (TLC)
28
The mobile phase will carry the most ___________ compounds the furthest up the TLC plate
Soluble
29
A sheet of glass, metal, or plastic which is coated with a thin layer of a solid adsorbent (Components of TLC)
TLC plates
30
This maintains a stable environment inside for proper development of spots, prevents the evaporation of solvents, and keeps the process dust-free (Components of TLC)
TLC chamber
31
This comprises of a solvent or solvent mixture (Components of TLC)
Mobile phase
32
Helps develop a uniform rise in mobile phase over the length of the stationary phase (Components of TLC)
Filter paper
33
Being a ____________ technique, TLC is used more for rapid qualitative measurements than for quantitative purposes
Semi-quantitative
34
The sample is applied as a concentrated spot with small dimension (Steps in TLC)
Step 1 (Sample loading/application)
35
Solvent rises by capillary action up through the adsorbent and partitioning occurs (Steps in TLC)
Step 2 (Development of chromatogram)
36
Refers to the pattern formed by substances that have been separated by chromatography
Chromatogram
37
Visualization techniques are applied (Steps in TLC)
Step 3 (Visualization)
38
Destructive; leaves charred blots behind (Examples of TLC visualization techniques)
Sulfuric acid/heat
39
Destructive; leaves dark blue blot behind for polar compound (Examples of TLC visualization techniques)
Ceric stain
40
Semi-destructive; iodine absorbs onto the spots, not permanent (Examples of TLC visualization techniques)
Iodine
41
Non-destructive; short wavelength (background-green, spots-dark), long wavelength (plates-dark, compounds-glow) (Examples of TLC visualization techniques)
UV light
42
Documentation and evaluation is performed (Steps in TLC)
Step 4 (Documentation and evaluation)
43
RF value depends on the following parameters: ___________, __________, __________, and __________ (SAAT)
Solvent system, Adsorbent, Amount of material spotted, Temperature
44
Describes how much longer an analyte is retained by stationary phase compared to non-retained compound (Formulas used in TLC)
Retention factor/Capacity factor
45
Measures the relative retention of two analytes and indicates the column's ability to selectively retain one analyte more than other (Formulas used in TLC)
Separation factor/Selectivity factor
46
Indicates the band broadening that occurs as an analyte passes through column (Formulas used in TLC)
Column efficiency (N)/Number of theoretical plates (N)
47
A __________ N value means less band and more efficient column
Higher
48
Measure of column efficiency in terms of length per theoretical plate (Formulas used in TLC)
Height equivalent to a theoretical plate
49
Quantifies the degree of separation between two adjacent peaks (Formulas used in TLC)
Resolution
50
A __________ resolution means better separation
Higher
51
One of the most useful methods for the separation and purification of solids and liquids when purifying small quantities of material (Types of chromatography)
Column chromatography (CC)
52
Stationary phase (Column chromatography)
Powdered adsorbent packed into a column
53
Mobile phase (Column chromatography)
Solvent/Solvent mixture
54
The higher the adsorption to the stationary phase, the ___________ the molecule will move through the column (Column chromatography)
Slower
55
The higher the solubility in the mobile phase, the ___________ the molecule will move through the column (Column chromatography)
Faster
56
Solvent moving through the column (Terms in CC)
Mobile phase/Carrier
57
Substance that stays fixed inside the column (Terms in CC)
Stationary phase/Adsorbent
58
Fluid entering the column (Terms in CC)
Eluent
59
Fluid exiting the column (Terms in CC)
Eluate
60
Process of washing out a compound through a column using a suitable solvent (Terms in CC)
Elution
61
Mixture whose individual components have to be separated and analyzed (Terms in CC)
Analyte
62
Property of how well a component of the mixture stick to the stationary phase (Terms in CC)
Adsorption
63
Property of how well a component of the mixture dissolves in the mobile phase (Terms in CC)
Solubility
64
2 types of HPLC (NR)
Normal phase, Reverse phase
65
Stationary phase (Normal phase HPLC)
Silica gel
66
Mobile phase (Normal phase HPLC)
Nonpolar solvent
67
A typical column has an internal diameter of 4.6 nm (or less) and has a length of 150-250 nm (Types of HPLC)
Normal phase HPLC
68
Most commonly used form of HPLC
Reverse phase HPLC
69
Stationary phase (Reverse phase HPLC)
Octadecylsilyl (ODS) - a coated silica gel modified to make it nonpolar
70
Mobile phase (Reverse phase HPLC)
Polar solvent
71
Nonpolar compounds will pass more quickly through the column (Types of HPLC)
Normal phase HPLC
72
Polar molecules will travel through the column more quickly (Types of HPLC)
Reverse phase HPLC
73
In HPLC, a pump forces a solvent through a column under high pressure of up to __________ atm
400
74
Used in combination with UV/Vis detector to provide accurate and robust method for quantitative analysis of pharmaceutical products (Types of chromatography)
High performance liquid chromatography (HPLC)
75
Is a technique of separation in which the components of the mixture are adsorbed on the surface of the adsorbent (Types of CC)
Adsorption CC
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Stationary phase (Adsorption CC)
Finely divided alumina or silica
77
Mobile phase (Adsorption CC)
Solvent
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The stationary phase as well as the mobile phase are liquid partition chromatography; separation is based on differences between solubility (Types of CC)
Partition CC
79
2 types of partition CC (NR)
Normal phase chromatography, Reversed phase chromatography
80
Stationary phase (Normal phase partition CC)
Polar
81
Mobile phase (Normal phase partition CC)
Nonpolar
82
Stationary phase (Reverse phase partition CC)
Nonpolar
83
Mobile phase (Reverse phase partition CC)
Polar
84
The separation takes place through a column packed with gel; separation is based on molecular size (Types of CC)
Gel CC
85
Gel column chromatography is also known as ___________
Size exclusion chromatography
86
Stationary phase (Gel CC)
Small silica or polymer particles
87
Mobile phase (Gel CC)
Solvent
88
A chromatography technique in which the stationary phase is always ion exchange resin (Types of CC)
Ion exchange CC
89
Stationary phase (Ion exchange CC)
Ion exchange resin
90
Mobile phase (Ion exchange CC)
Aqueous buffer, Solvent with mixture of salt
91
Refers to the time taken for a particular compound to travel through the column to the detector
Retention time
92
In the early 1900s, gas chromatography was discovered by __________
Mikhail Semenovich Tsvett
93
This technique uses inert gas as the mobile phase through the column containing liquid stationary phase (Types of CC)
Gas chromatography
94
Gas chromatography is also known as ___________
Gas-liquid chromatography
95
In gas chromatography, the sample solution injected into the instruments enter a gas stream which transport the sample into a separation tube known as the __________
Column
96
The sample is injected using a micro syringe (Parts of gas chromatography)
Injector
97
The heart of gas chromatogram is the ___________ (Parts of gas chromatography)
Column
98
Lower boiling point compounds move __________ (Principles of gas chromatography)
Faster
99
Higher column temperature allow the compound to move ____________ (Principles of gas chromatography)
Faster
100
__________ stationary phase tend not to discriminate compounds that give separation dependent on boiling point (Principles of gas chromatography)
Nonpolar
101
__________ stationary phase tend to bind more strongly with polar compound which retard the movement through the column (Principles of gas chromatography)
Polar
102
The ___________ which is 0.05-0.1 cm in diameter and 1.5-3 meters long is coiled in order to fit into the oven
Gas chromatograph
103
2 types of columns in gas chromatography (PC)
Packed, Capillary
104
Contains granular inert solid support coated with silicone rubber or carbowax (Types of columns in gas chromatography)
Packed column
105
Made up of fused silica (Types of columns in gas chromatography)
Capillary column
106
Compares the temperature of the sample filaments and reference filament which is heated using an electric current (Types of detectors in gas chromatography)
Thermal conductivity detector (TCD)
107
Burns the effluent that is coming off the column (Types of detectors in gas chromatography)
Flame ionization detector (FID)
108
Used for halogenated hydrocarbon (Types of detectors in gas chromatography)
Electron capture detector (ECD)
109
This part computes the area of the peaks of the gas (Parts of gas chromatography)
Integrator
110
Shorter retention times means __________ movements of compounds
Faster
111
Longer retention time means __________ movement of sample
Slower
112
Short column length (Shorter or longer RT)
Shorter RT
113
Long column length (Shorter or longer RT)
Longer RT
114
Higher column temperature (Shorter or longer RT)
Shorter
115
Lower column temperature (Shorter or longer RT)
Longer
116
High helium flow rate (Shorter or longer RT)
Shorter RT
117
Low helium flow rate (Shorter or longer RT)
Longer RT
118
High volatility of compound (Shorter or longer RT)
Shorter RT
119
Low volatility of compound (Shorter or longer RT)
Longer RT
120
Nonpolar affinity to column (Shorter or longer RT)
Shorter RT
121
Polar affinity to column (Shorter or longer RT)
Longer RT
122
In gas chromatography, __________ area is proportional to mass of compound injected
Peak
123
Each peak of a gas chromatogram becomes a ____________ of the compound
Fingerprint
124
Peaks that appear too small or too large may be corrected by changing the __________ settings, which may increase or decrease the peak display
Attenuation
125
Used for determining alcohols, aromatics, hydrocarbons, etc. (Types of chromatography)
Gas chromatography
126
Is defined as a list of tests, references to analytical procedures, and appropriate acceptance criteria which are numerical limits, ranges, or other criteria for the tests described
Specification
127
Means that the drug substance and/or drug product, when tested according to the listed analytical procedures, will meet the listed acceptance criteria
"Conformance to specifications"
128
4 universal tests/criteria for new drug products (DIAI)
Description, Identification, Assay, Impurities
129
A qualitative description of the dosage form should be provided (Universal tests/criteria for new drug products)
Description
130
Should establish the identity of the new drug substances in the new drug product (Universal tests/criteria for new drug products)
Identification
131
Used to determine strength (content); it should be included for all new drug products (Universal tests/criteria for new drug products)
Assay
132
Organic and inorganic impurities (degradation products) and residual solvents are included in this category (Universal tests/criteria for new drug products)
Impurities
133
The specification for solid oral dosage forms normally includes a test to measure release of drug substance from the drug product (Specific tests/criteria for new drug products)
Dissolution
134
Single-point measurements are normally considered to be suitable for __________ release dosage forms
Immediate
135
In dissolution test, the permitted variability in mean release rate at any given time point should not exceed a total numerical difference of __________ of the labeled content of drug substance
±10%
136
Apparatus 1 is the __________ apparatus which is a cylindrical vessel (Dissolution apparatus)
Basket
137
Apparatus 2 is the __________ apparatus that is formed from a blade and a shaft (Dissolution apparatus)
Paddle
138
Units tested is 6; Each unit is not less than Q +5% (Stages of dissolution)
Stage 1
139
Units tested is 6; Average of 12 units (S1 + S2) is equal to or greater than Q, and no unit is less than Q15% (Stages of dissolution)
Stage 2
140
Units tested is 12; Average of 24 units (S1 + S2 + S3) is equal to or greater than Q, not more than 2 units are less than Q – 15%, and no unit is less than Q – 25% (Stages of dissolution)
Stage 3
141
For rapidly dissolving products containing drugs which are highly soluble through the physiological range (Specific tests/criteria for new drug products)
Disintegration
142
An in-process control; it is normally not necessary to include these attributes in the specification (Specific tests/criteria for new drug products) (HF)
Hardness, Friability
143
Includes both the mass of the dosage form and the content of the active substance in the dosage form (Specific tests/criteria for new drug products)
Uniformity of dosage units
144
Should be included when appropriate; the acceptance criteria may be justified with data on the effects of hydration or water absorption on the drug product (Specific tests/criteria for new drug products)
Water content
145
A detection procedure which is specific for water, like the __________ titration is preferred
Karl Fischer
146
Is seen as an attribute of GMP as well as of quality assurance; acceptance criteria should be set for the total count of aerobic microorganisms, the total count of yeasts and molds, and the absence of specific objectionable bacteria (Specific tests/criteria for new drug products)
Microbial limits
