COLOYAN, Paulerni G.

CH36 –B 140998
Final Examinations

1. What type of balance has a maximum load of 160-200g, and has a precision of 0.1mg?
- Analytical Balance
2. Define a primary-standard grade reagent
- A primary standard grade reagent is a reagent used in analytical chemistry used
in calibration of amounts of substances to be reacted to it. It will serve as the starting point
of subsequent analytical calculations. It must have an indicated purity (assay) that is very
high so that its amount is very representative of the moles of the substance it will dispense.
Also, a primary standard should possess characteristics such as low hygroscopicity (attract
water molecules from environment), and high stability so that its parameters such as mass
cannot drastically affected by external factors such as the air.
3. Identify three types of error and contrast the three
a.) Personal Error – brought upon by the experimenter’s faulty procedure,
such as misreading a scale by a person
b.) Systematic Error – brought upon by equipment’s defect, such as a faulty
balance
c.) Random Error – brought upon by experimental conditions beyond the
experimenter’s control such as temperature, humidity,
etc.
4. Define RSD and SD
SD or Standard Deviation is the measure of the spread of measurements within a
set of data. In other words, it tells how precise the average is, or how well the
measurements agree with one another. It is expressed in the way the measurements are
labeled.
̅ −𝑿𝒏 )𝟐
(𝑿
s = √∑𝒏𝒊=𝟏 𝒏−𝟏
Relative Standard Deviation on the other hand, is the ratio of the SD of a given set
of data and its mean, and often expressed in percentage. Since it is not expressed as a ratio,
RSD is more convenient when it comes to comparing the precision of sets of data with
different absolute means.
𝒔
RSD = 𝒙̅x1000
5. Define precision and accuracy
Accuracy describes how measurements are close to the real or true value while
precision describes how consistent the measurements are or how they are close to each
other. Accuracy is often measured in %error while precision in standard deviation.
6. What is a sample blank?
A blank is a sample treatment in analytical methods (titrations, spectrometric
analyses, etc.) that is prepared the same manner as the other treatments (same reagents,
dilution factors) but no analyte of interest. It is employed in order to trace contamination of
the sample to be analyzed with a small amount of the analyte of interest. The value
calculated will then be subtracted to all treatments to provide more accurate value of the
property to be determined. An example is a blank containing only deionized water and
indicator in an acid base titration. Since deionized water is slightly acidic, titrating it,
getting its [H+] and subtracting it to the treatments’ derived [H+] will provide the true [H+]
of the analyte, without the H+ contributed by the solvent which can be deemed as a
“contamination”.
7. Why do we calibrate?
Calibration of instruments, i.e. volumetric instruments are essential in analytical
chemistry because it adjusts the value of the volume the glassware can contain or dispense
to warrant more accuracy. This is because the conditions in a chemical laboratory may be
different than the place where the glassware is initially calibration by the manufacturer.
For example, the volume of water a buret can dispense at 283 K is different than at 298 K.
8. In what situations will you use a volumetric pipet over a buret?
A volumetric pipet is more convenient to use when the liquid to be dispensed is
exactly equal to the volume of liquid the volumetric pipet can hold. A buret on the other
hand, can be used to dispense any amount of liquid. A buret is more appropriate to use
when the reaction must be approached in a way that the reactant is to be added dropwise
since tightening the stopcock will enable the dispensing to be at a slower pace. A
volumetric pipet on the other hand is easier to use since it is much smaller than a buret.
9. Why is KHP used as a standard for NaOH titrations?
Potassium hydrogen phthalate (KHP) is used as a primary standard for NaOH
titrations since it is an acid which reacts to NaOH in a 1-1 molar ratio, it has a high purity
assay (more than 99.9%), it is very stable, non-hygroscopic, and has a pH of 8.9 at
equivalence point when used to titrate NaOH which is near the phenolphthalein endpoint,
thus minimizing titration error.
10. Why is the pH important for EDTA titrations?
Ethylenediaminetetraacetic acid (EDTA) can be present as H4Y, H3Y-, H2Y2-,HY3-,
and Y4-. The amounts of each of these forms of EDTA are dependent to the pH of the sol’n,
which makes pH a very important aspect in EDTA titration. For example, Ca2+ can be
chelated with the Y4- form of EDTA. EDTA titration of Ca2+ is most probably be buffered at
pH = 10 since Y4- comprises most of the EDTA added at this pH.
11. Why do we dilute our samples prior to analysis?
Diluting is very essential prior analysis since reagents are purchased in high
concentrations, and for them to be usable in the lab, they must be accurately diluted to a
known, lower concentration. Also, in titrations, diluting either the analyte or titrant will
give the experimenter a larger room to hit the endpoint and not overshoot since smaller
amounts of reagents are added to react.
12. Why do we standardize our reagents?
Standardizing reagents are essential in order to determine their exact
concentration. For example, a 1.00 M NaOH solution prepared at the stockroom may not be
exactly 1.0 M, and the discrepancy may be magnified as calculations are done.
Standardizing solutions against a primary standard will accurately determine their
concentrations.
13. Write out the redox equation of the permanganate-oxalate titration
2MnO4-(aq) + 16H+(aq) + 5C2O42-(aq)⇌10CO2(g) + 2Mn2+(aq) + 8H2O(l)
14. Why must some samples be dried prior to analysis?
Some samples must be dried prior analysis because they may have absorbed water
from the atmosphere, which affects the weight of the sample, which in turn makes the
weight of the sample non-representative of the amount of the target substance it can
dispense.
15. How will CO2 affect titrations? How can this be prevented?
CO2 may react with H2O which is the solvent used in almost all acid-base titrations,
to form carbonic acid H2CO3, which may loose 2 protons, altering the [H+] of the system:
CO2(aq) + H2O(l)⇌H2CO3(aq)
H2CO3 (aq) ⇌ H+ (aq) + HCO3- (aq)
HCO3- (aq) ⇌ H+ (aq) + CO32- (aq)
Boiling the water to bubble out the CO2 present may be done to prevent this.
16. What could cause the formation of a brown precipitate in a permanganate-oxalate
titration?
MnO4- may be reduced to MnO2 which is a brown precipitate when not enough H+ is
present to provide an acidic medium, as well as when the stirring is not vigorous enough
while titrating.
17. Why is urea used in the gravimetric determination of Calcium?
Urea decomposes to ammonia and CO2 given high temperatures, making the
solution basic over time due ammonia being a weak base. Ca2+ is insoluble in basic media,
which will react to C2O42- to precipitate CaC2O4. Since the precipitation must be gradual in
order to prevent the formation of many seeds, the pH must be gradually increased, the
thermal decomposition of urea is preferred.
∆
NH2CONH2(aq) + H2O(l) → 2NH3(aq) + CO2(aq)
Ca2+(aq) + C2O42-(aq) ⇌CaC2O4 •H2O (s)
18. Define Beer’s Law, and explain.
Beer-Lambert’s Law states that the absorbance of a material sample is linearly
proportional to the path length and to the molar concentration of the sample. Given a fixed
path length, the molar absorptivity coefficient (a constant for a specific substance) and the
absorbance from a UVVIS spectrophotometer, the molar concentration of that substance
can be determined:
A = ebc
A = absorbance, e = molar absorptivity coefficient, b = path length (path travelled by light
through the sample), c = molar concentration
19. Why must some samples be treated in HNO3?
Some samples must be treated with HNO3 in order to dissolve them, or to provide an
acid in order for reactions requiring acidic media to proceed.
20. How do you handle a UV-vis cuvette?
The cuvette must be held in its frosted sides so that the sides where the light passes
through will not have any prints or oils whick may cause errors on the absorbance to be
calculated. Also, when loading the cuvette to the spectrophotometer, the arrow must be on
the side where the light passes out of the cuvette.