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WorksheetsM6-M9 Part 1 QC2 Laboratory (Finals)
Total questions: 126
Worksheet time: 4hrs 12mins
➢ A method of analysis based on the measurement of current resulting from the electrolysis of an electroactive species at a given electrode potential under controlled conditions.
➢ Can be used quantitatively and qualitatively.
Chromatography
Polarography
Polarimetry
Refractometry
Polarography is a branch of voltammetry which uses a working electrode ________ or _________.
Dropping Mercury Electrode
Static Mercury Drop Electrode
Voltaic Mercury Drop Electrode
Polarography Mercury Drop Electrode
In polarography, DME means
(a)
In polarography, SME means
(a)
Polarography is invented by a Czech chemist
MIKHAIL SEMYONOVICH TSVET
KARL FISCHER
JAROSLAV HEYROVSKY
CARL ZEISS
an electrochemical method in which information about the analyte is obtained by current
Voltammetry
Voltimetry
Voltagemetry
Formula for % Moisture Content
➢ when a pair of electrode is placed in a sample solution, it shows the potential difference by the addition of the titrant or changing the concentration of the ions.
➢ also used for the quantitative analysis
➢ it has an endpoint determined by a change in potential of an electrode immerse in solution
Polarimetry
Potentiometry
Refractometry
Chromatography
➢ Iodine (Titrant) is generated electrochemically in the titration cell
➢ Water is quantified on the basis of the total charge passed, as measured by the current and time.
➢ It can be determined by measuring the quantity of electricity required to electrolyze the susbstance
➢ This does not need standard solution
Coulometric KFT
Volumetric KFT
All statements about coulometric kft are true except
1. This measures water level much lower than the volumetric method.
2. Detects the endpoint of the titration using the double platinum pin indicator electrode.
3. Sensitive because it can measure even the lowest or small portion of water.
1
2
3
1 and 2
2 and 3
which statement is/are true about volumetric kft
1. This measures water level much lower than the volumetric method.
2. Detects the endpoint of the titration using the double platinum pin indicator electrode.
3. Sensitive because it can measure even the lowest or small portion of water.
1
2
3
1 and 2
2 and 3
Volumetric KFT is also known as
Direct Titration
Indirect Titration
➢ Also known as the DIRECT TITRATION (because the analyst approaches the endpoint directly).
➢ Dispenses the titrating reagent (containing iodine) into the cell, using the burette.
➢ Calculates the end result based on the volume of the KF reagent dispensed, using the on-board microprocessor.
Coulometric KFT
Volumetric KFT
Karl Fischer Titration (water %) formula
In Karl Fischer Titration (water %) formula, F means
water equivalence factor
volume of reagent used (mL)
weight in mg
In Karl Fischer Titration (water %) formula, V means
water equivalence factor
volume of reagent used (mL)
weight in mg
In Karl Fischer Titration (water %) formula, Wt means
water equivalence factor
volume of reagent used (mL)
weight in mg
➢ It deals with the study of the rotary power (optical rotation or specific rotation) of substances.
➢ Rotation of linearly polarized light as it travels through certain materials.
Chromatography
Polarography
Polarimetry
Refractometry
In polarimetry, only chiral can be used.
True
False
It is stereoisomers that differ in spatial arrangement of atoms. Asymmetric in such a way that the structure and the mirror image are not super imposable.
Chiral
Achiral
Chiral are ___________.
Nonsuperimposable
Superimposable
Achiral are ___________.
Nonsuperimposable
Superimposable
In polarimetry, common samples are
Sugars
Peptides
Acids
Glucose
➢ Also known as the “OPTICAL ACTIVITY”
➢ It is the power of rotating plane polarized light when light
passed through solutions of organic substances.
optical power
rotary power
rotatory power
chiral power
when the direction of the rotation is toward the right [+] = CLOCKWISE (S-ENANTIOMER)
DEXTROROTATORY
LEVOROTATORY
when the direction of the rotation is toward the left [-] = COUNTER CLOCKWISE (R-ENANTIOMER)
DEXTROROTATORY
LEVOROTATORY
Common example is fructose
DEXTROROTATORY
LEVOROTATORY
Common example is glucose
DEXTROROTATORY
LEVOROTATORY
Importance of polarimetry includes
1) Assessment of the PURITY of a liquid compound, in comparison with a known / standard
2) Establish identity of substances (can identify if a substance is a dextro or a levo)
3) Establish purity and concentration of samples
4) Indication of its therapeutic value
1 2 3 4
1 3 4
1 2 4
2 3 4
Example: measures syrup
Clinical Application: can easily determine the sugar level in diabetic patients
Establish identity of substances
Establish purity and concentration of samples
Indication of its therapeutic value
• can be computed to manipulate the polarization
• If the ___________ of a sample did not meet the ones in the monograph, there is a possible presence of impurities
Purity value
Concentration value
Therapeutic value
the conditions that involved the malformation of arms and legs of babies
Thalassemia
Huntington's Disease
Phocomelia
Down Syndrome
root cause of phocomelia
Use of Thalidomide
Use of Valdecoxib
Use of Levamisole
Use of Rofecoxib
Thalidomide occurs in two mirror images
R-THALIDOMIDE
S-THALIDOMIDE
D-THALIDOMIDE
L-THALIDOMIDE
contains sedative substance
R-THALIDOMIDE
S-THALIDOMIDE
teratogenic that has effect on the baby
R-THALIDOMIDE
S-THALIDOMIDE
a racemate that has an equal amount of left and right handed enantiomers
Racemate mixture
Racetate mixture
Racemix mixture
Racemic mixture
o used for nausea or morning sickness
o The separation between R and S enantiomer is ineffective and no use.
Thalidomide
Valdecoxib
Levamisole
Rofecoxib
Which of the two is the formula for specific rotation that has a concentration of g/100ml
Which of the two is the formula for specific rotation that has a concentration of g/ml
In the formula of specific rotation, the image means
specific rotation of the substance
relative optical rotation
length of observation tube (in dm)
concentration of optically active substance in a sample [in g/100 mL]
In the formula of specific rotation, a means
specific rotation of the substance
relative optical rotation
length of observation tube (in dm)
concentration of optically active substance in a sample [in g/100 mL]
In the formula of specific rotation, l means
specific rotation of the substance
relative optical rotation
length of observation tube (in dm)
concentration of optically active substance in a sample [in g/100 mL]
In the formula of specific rotation, c means
specific rotation of the substance
relative optical rotation
length of observation tube (in dm)
concentration of optically active substance in a sample [in g/100 mL]
In specific rotation, units are actually cm2 g-1, but usually just given as degrees.
True
False
➢ It deals with the study and measurement of index of refraction of substances in order to assess their composition of purity
➢ commonly uses volatile oils as a sample
Chromatography
Polarography
Polarimetry
Refractometry
Principle of Refractometry
The ratio of the angle of refraction in a vacuum (air) versus the angle of refraction of the sample materials is the INDEX OF REFRACTION.
The ratio of the angle of refraction in a vacuum (liquid) versus the angle of refraction of the sample materials is the INDEX OF REFRACTION.
In the specific rotation of the substance determined at temperature of ________ using the D-line of sodium [wavelength of 589 n, it is the light source of all polarimetric measurements]
37C
25C
39C
29C
In the specific rotation of the substance determined at temperature of 25C using the D-line of sodium [wavelength of ________, it is the light source of all polarimetric measurements]
585 nm
586 nm
587 nm
588 nm
589 nm
Reporting of Refractive Index
The N (Italicized) means
denotes refractive index
D-line of 589 nm
Temperature (20C)
Reporting of Refractive Index
The D means
denotes refractive index
D-line of 589 nm
Temperature (20C)
Reporting of Refractive Index
The 20 means
denotes refractive index
D-line of 589 nm
Temperature (20C)
REFRACTIVE INDEX CHARACTERISTICS INCLUDES
It usually ranges between 1.3000 to 1.7000 for most compounds
Normally determined up to a 5-digit precision
It is a temperature-dependent physical constant
It is a physical property characteristic of a pure compound (can
also be used for qualitative analysis)
Refractive index number or values are unitless
Refractive index normally determined up to a
4-digit precision
5-digit precision
6-digit precision
7-digit precision
REFRACTIVE INDEX SIGNIFICANCE EXCEPT
Confirmation of the IDENTITY of an unknown liquid compound
Assessment of the PURITY of a liquid compound, in comparison with a known / standard
Determination of the CONCENTRATION of a solute in a
solution, by comparison of the refractive index of the sample solution with a standard curve.
Establish identity of substances (can identify if a substance is a dextro or a levo)
Indication of its therapeutic value
An instrument that measured the extent to which the light is bent or refracted, when it moves from the air or vacuum into the sample
Polarimeter
Potentiometer
Chromatograph
Refractometer
Most common refractometer and a bench top instrument that offers the highest precision.
ABBE REFRACTOMETER
TRADITIONAL HANDHELD REFRACTOMETER
DIGITAL HANDHELD REFRACTOMETER
INCLINE PROCESS REFRACTOMETER
An abbe refractometer that has the circulating water bath.
TRADITIONAL ABBE REFRACTOMETER
DIGITAL ABBE REFRACTOMETER
MULTIWAVELENGTH ABBE REFRACTOMETER
MODERN DIGITAL ABBE REFRACTOMETER
An abbe refractometer that has the circulating water bath and has the instant reading of n.
TRADITIONAL ABBE REFRACTOMETER
DIGITAL ABBE REFRACTOMETER
MULTIWAVELENGTH ABBE REFRACTOMETER
MODERN DIGITAL ABBE REFRACTOMETER
An abbe refractometer which wavelength is equal to 589 nm. Allows the measurement of n at different wavelength.
TRADITIONAL ABBE REFRACTOMETER
DIGITAL ABBE REFRACTOMETER
MULTIWAVELENGTH ABBE REFRACTOMETER
MODERN DIGITAL ABBE REFRACTOMETER
An abbe refractometer which circulating water bath is no longer required.
TRADITIONAL ABBE REFRACTOMETER
DIGITAL ABBE REFRACTOMETER
MULTIWAVELENGTH ABBE REFRACTOMETER
MODERN DIGITAL ABBE REFRACTOMETER
Refractometer part no. 1
Eyepiece
Thermometer
Compensator dial
Measuring prism
Illuminating prism
Refractometer part no. 2
Eyepiece
Thermometer
Compensator dial
Measuring prism
Illuminating prism
Refractometer part no. 3
Eyepiece
Thermometer
Compensator dial
Measuring prism
Illuminating prism
Refractometer part no. 4
Eyepiece
Thermometer
Compensator dial
Measuring prism
Illuminating prism
Refractometer part no. 5
Eyepiece
Thermometer
Compensator dial
Measuring prism
Illuminating prism
Refractometer part no. 6
Lamp
Adjustment Handwheel
Compensator dial
Measuring prism
Illuminating prism
Refractometer part no. 7
Lamp
Adjustment Handwheel
Compensator dial
Measuring prism
Illuminating prism
Its function is to fix the place at the center of the cross or to adjust the reflection borderline at the center of the cross mark.
ADJUSTMENT HANDWHEEL
COMPENSATOR DIAL
MEASURING PRISM
ILLUMINATING PRISM
Its function is to adjust the sharpness.
ADJUSTMENT HANDWHEEL
COMPENSATOR DIAL
MEASURING PRISM
ILLUMINATING PRISM
It is where the volatile oil will be placed, and it is made of glass. When sample is placed it is required to use a plastic dropper or else it can create scratches in the glass.
ADJUSTMENT HANDWHEEL
COMPENSATOR DIAL
MEASURING PRISM
ILLUMINATING PRISM
Once the volatile oil is scattered, it is used as cover
ADJUSTMENT HANDWHEEL
COMPENSATOR DIAL
MEASURING PRISM
ILLUMINATING PRISM
The box part is known as ___________ which means that it is the concentration of sugar. It can be used in wine to determine the percent of sugar in grape wine. Uses refractometer to check degrees Bx.
Brix Concentration
Bix Concentration
Brex Concentration
THE FORMULA FOR ADJUSTING THE RAW REFRACTIVE INDEX VALUE IS:
Refractive Index Reading
Reporting Index Reading
Refraction Index Reading
The box part of the formula means that
it is in absolute value
It is not in absolute value
In calculating the refractive index, the equation automatically adjusts the correction factor up or down from 20 ̊C.
True
False
The formula for pH is/are
pH = - log [H+]
pH = - log [OH+]
pH = 14 - pOH
The formula for pOH is/are
pOH = - log [H+]
pOH = - log [OH+]
pOH = 14 - pH
It is based on the reaction of water with an anhydrous solution of sulfur dioxide and iodine in the presence of a buffer that reacts with hydrogen ions.
Residual
Direct
Coulometric
The excess reagent is added to the test specimen, sufficient time is allowed for the reaction to reach completion, and the unconsumed reagent is titrated with a standard solution of water in a solvent.
Residual
Direct
Coulometric
The Iodine is not added in the form of a volumetric solution but is produced in an iodide-containing solution by usually anodic oxidation.
Residual
Direct
Coulometric
Oven drying is classified as:
spectroscopic
Other methods
Chemical
Thermogravimetric
Ca carbide method is classified as:
spectroscopic
Other methods
Chemical
Thermogravimetric
This method has specificity in determining the water content.
spectroscopic
Other methods
Chemical
Thermogravimetric
Azeotropic-toluene distillation is classified under:
spectroscopic
Other methods
Chemical
Thermogravimetric
This method is applied to most systems with a moisture content of >0.1%.
spectroscopic
Other methods
Chemical
Thermogravimetric
Clumping and surface crust formation will lead to erroneous results.
True
False
Pans should be dried in an oven and stored in a desiccator prior to use.
True
False
It is the study of the measurement and interpretation of the polarization of transverse waves.
(a)
An instrument used to measure angle of rotation cause by passing of polarized light through and optically active substance.
(a)
When the direction of the rotation of optically active substance in polarimeter is towards the right, it is known as (a) .
pH meter is used for measuring fluid concentrations such as the sugar content.
True
False
It is a bench-top device for the high-precision measurement of an index of refraction.
(a)
A refracting prism that contains illuminating prism.
Lower prism case
Prism field lamp
Upper prism case
Hinged lightshield
A refracting prism that contains the measuring prism and acts as sample compartment.
Lower prism case
Prism field lamp
Upper prism case
Hinged lightshield
An internal measurement scale is used to observe both the total reflection borderline and the instrument’s internal measurement.
Eyepiece
Measurement scale
Hinged lightshield
Prism field lamp
A refracting prism that prevents stray light from entering the front of the measuring prism.
Eyepiece
Measurement scale
Hinged lightshield
Prism field lamp
➢ It measures the mass of a sample, as it is heated, cooled, or held at constant temperature in a defined atmosphere.
➢ Limitation: do not distinguish weight loss due to vaporization of water from other volatile compounds.
Spectroscopic
Other methods
Chemical
Thermogravimetric
The methods under thermogravimetric includes
Oven Drying
Infrared Drying
Air Drying
Halogen Drying
Microwave Drying
The measurement is based on _______ reaction. _________ reaction occurs where the water is separated chemically from the remainder of the sample.
Spectroscopic
Other methods
Chemical
Thermogravimetric
Advantages of chemical in moisture determination
= specificity for water
high accuracy and precision
selectivity for water
small sample quantities required
rapid determination of water content
Advantages of chemical in moisture determination except
easy sample preparation
short analysis duration
mixture’s composition cannot be changeby simple distillation
nearly unlimited measuring range (1ppm to 100%)
independence of presence of other volatiles
• In moisture determination under chemical it is a method wherein rapid determination of water content from gas pressure uses calcium carbide.
• Usually used to determine the water content in the soil (calcium carbide +water) producing gas.
Calcium carbide method
Azeotropic method
a mixture of two or more liquids (chemicals) in such a ratio that its composition cannot be change by simple distillation
Carbide
Azeotrope
In moisture determination under spectroscopic it includes
Infrared spectroscopy
Microwave spectroscopy
UV-Vis spectroscopy
NMR spectroscopy
The most successful of water content determination in foods. Rapid, accurate, non destructive to the sample.
Infrared spectroscopy
Microwave spectroscopy
UV-Vis spectroscopy
NMR spectroscopy
Instrument used for measuring the moisture content in the atmosphere.
Electrolytic hygrometer
Dew point method
The measurement of relatively low concentrations of water in vapor state in a gas. Water forms a fog or mist when suddenly cooled.
Electrolytic hygrometer
Dew point method
• reaction of water with anhydrous Sulfur dioxide and iodine
• you add a standard titrant to the analyte until you reached the endpoint
IA : Direct Titration
IB: Residual Titration
IC: Coulometric Titration
• Excess reagent is added to the test specimen, the unconsumed reagent is titrated with standard
solution of water in a solvent such as methanol.
• You add an excess of standard titrant to the analyte, and then you titrate the excess titrant to determine how much is in excess.
IA : Direct Titration
IB: Residual Titration
IC: Coulometric Titration
KF reaction is used, however, iodine is not added in the form of vol.sol. but is produced in an iodine- containing solution by usually anodic oxidation.
IA : Direct Titration
IB: Residual Titration
IC: Coulometric Titration
Infrared drying is faster and more reliable than conventional oven drying.
True
False
Moisture or water content determination is an important parameter in the following aspects of drug manufacture;
monitoring of tablet granulations, prior to compression and encapsulation procedures
Water / moisture content of certain drugs, such as antibiotic drugs for suspension (Amoxicillin, Erythromycin and the likes) should be kept between the range of 0.5% to 1.0%, to prevent bacterial growth. This will help enhance product stability.
as a basis for the computation of purity of drugs during quantitative analysis
NOTA
USP SPECIFICATION FOR MOISTURE CONTENT: CORNSTARCH AND WHEAT STARCH
NMT 15%
NMT 18%
NMT 21%
USP SPECIFICATION FOR MOISTURE CONTENT: TAPIOCA STARCH
NMT 15%
NMT 18%
NMT 21%
USP SPECIFICATION FOR MOISTURE CONTENT: POTATO STARCH
NMT 15%
NMT 18%
NMT 21%
USP SPECIFICATION FOR MOISTURE CONTENT: ACACIA, USP
NMT 15% (WATER METHOD)
NMT 18%
NMT 21%
USP SPECIFICATION FOR MOISTURE CONTENT: LACTOSE, USP
NMT 0.2%
NMT 0.3%
NMT 0.4%
NMT 0.5%
USP SPECIFICATION FOR MOISTURE CONTENT: REFINED WHITE SUGAR
0.22% - 2.0%
0.23% - 4.0%
0.24% - 3.0%
0.25% - 1.0%
USP SPECIFICATION FOR MOISTURE CONTENT: TALC, USP
NMT 6.2%
NMT 6.3%
NMT 6.4%
NMT 6.5%
USP SPECIFICATION FOR MOISTURE CONTENT: METHYLCELLULOSE
NMT 6%
NMT 5%
NMT 4%
NMT 3%
In IR analyzer, the greater the surface area of material exposed to the environment, the faster the rate of moisture removal.
True
False
An type of pan in IR that is used because they are relatively cheap and have a high thermal conductivity.
Carbide pan
Calcium pan
Aluminum pan
What type of IR analyzer is available in CEU-Manila?
IR Moisture analyzer 35
IR Moisture analyzer 34
WARNING AND SAFETY IN USING IR ANALYZER
Always use forceps or the tongs to remove the sample pan upon completion of the test. Caution: the pan is hot!
During the operation of the instrument, do not touch the metal surfaces and the external exhaust dome to prevent injuries.
Do not test flammable or toxic materials.
Touch the device while it is working.
