EXPERIMENT 1

USE OF ANALYTICAL BALANCE AND CALIBRATION OF VOLUMETRIC GLASSWARE

Results and Discussion

I. ANALYTICAL WEIGHING

Table 1.1. Effect of fingerprints in weighing.

Condition Mass (g)

Mass of beaker using crucible tongs 29.068 g

Mass of beaker handled with bare hands 29.069 g

Kent (2016) states that fingerprints average to weight about 0.00004 grams,
containing fats, salts, and at most 20% water. Therefore, handling samples with bare hands
may result in the transfer of fingerprints on the sample, making the sample weigh heavier
than its true value. Moisture, grease, and dirt on fingers will also affect the weight of the
objects. The use of glove is a recommended means to prevent the transfer of fingerprints
while weighing without the use of crucible tongs.

Analytical balances are very sensitive. Therefore, they are heavily affected by the
environment in which they are installed and the way measuring personnel handles them.
Analytical balances have a draft shield or weighing chamber to prevent the very small
samples from being affected by air currents and the balance doors must be closed while
weighing as slightest vibrations or air current can change the results (Hill, 2015).
Temperature is another factor that can affect the accuracy of analytical balances. When the
sample's temperature is higher than the room temperature, a layer of warmer air is created
around the sample, and slight upward air current is created. That air current has the effect
of pushing the weighing sample up, and the weighing measurement will be lighter at first.
When the sample later reaches room temperature, the original weight will be displayed
(Izumo, 2012).
Analytical balance scales weigh the materials under the pretense that the load is
applied parallel to the force of gravity and perpendicular to the weighing platform (Hill,
2015). Thus, it is important to check the bubble level, and if bubble is not well-centered, turn
the adjustable feet so the bubble moves to the center and the balance is properly leveled
ensuring that the balance is leveled to be parallel to the direction of acceleration due to
gravity and be perpendicular to the weighing system (Titmas, 2015). Leaning on the table
where the balance is situated should also be avoided. Leaning on the table may cause
vibrations which are transmitted to the balance. Any vibrations can cause problems with the
accuracy of the balance, even if using a weighing table (Morse & Baer, 2004)
Table 1.2. Comparison of methods of weighing.
Conditions Mass/ Volume

2.1. Mass of crucible cover, g 15.844 g

2.2. Mass of crucible and cover, g 45.696 g

2.3. Mass of crucible, g 29.855 g

2.4. Mass crucible and cover – Mass crucible only, g 15.841 g

2.5.a. Mass of bottle with NaCl, g 4.323 g

2.5.b. Mass of wash bottle, g 157.716 g

2.5.c. Mass of dry beaker, g 29.068 g

2.6. Mass of bottle – NaCl, g 3.023 g

2.7. Mass of beaker + NaCl, g 30.362 g

2.8. Mass of beaker + NaCl + water, g 42.290 g

2.9. Mass wash bottle – water, g 145.783 g

1.294 g
2.10 Mass salt (by addition) (2.7. – 2.5.c.), g
Mass salt (by difference) (2.5.a – 2.6.), g 1.3 g

11.928 g
2.11. Mass water (by addition) (2.8. – 2.7.), g
Mass water (by difference) (2.5.b – 2.9.), g 11.933 g

Direct weighing means that an object is placed directly on a balance and record the mass
displayed. Weighing directly requires that the balance be zeroed (reads zero with nothing
on the balance pan) to obtain accurate results.

Weighing by addition involves weighing of a weighing bottle and then reweighing the
weighing bottle after placing the sample. The difference in the mass of the weighing bottle
containing the sample and the mass of the weighing bottle represents the mass of the sample
transferred to the weighing bottle.

Weighing by difference involves the repetitive weighing of a weighing bottle containing

a sample. As the sample is moved to another vessel, the mass of the weighing bottle contents
decreases. Upon reweighing, a lower mass is found. The difference between the two masses
represents the mass of solid reagent transferred to the vessel. Hence, the phrase "weighing
by difference".
 The difference between the crucible masses obtained in 2.1 and 2.4 is 0.003g. This could
be due to temperature and humidity fluctuations, air currents, vibration, and operator
errors.

II. STATISTICAL EVALUATION OF MEASUREMENTS

Table 1.3. Mass of individual coin and statistical analysis.

Coin
Coin Mass, g (in increasing Mass, g
mass) *
1st coin 5.366 g 1 5.241 g

2nd coin 5.318 g 2 5.294 g

3rd coin 5.440 g 3 5.318 g

4th coin 5.393 g 4 5.328 g

5th coin 5.241 g 5 5.344 g

6th coin 5.328 g 6 5.351 g

7th coin 5.294 g 7 5.366 g

8th coin 5.412 g 8 5.393 g

9th coin 5.344 g 9 5.412 g

10th coin 5.351 g 10 5.440 g

Q - test no outliers

Mean 5.349 g

Average deviation 0.044 g

Range 0.199 g

Standard Deviation 0.058 g

Coefficient of variation 1.09 %

Confidence limits of the μ = 5.349 g ± 0.0338 g
mean (90% level)
 Accuracy cannot be measured since the true value of a 1-peso coin is not known or given.
It is deduced that the machines are relatively precise when manufacturing 1-peso coins, as
the range, standard deviation, coefficient of variation, the width of the confidence interval is
relatively low. A relatively high precision could be due to how the coins are made by the same
machine. By using the same machine for production, the effect of varying machine accuracy
and machine discrepancies when producing the coins is removed, consequently producing
coins with relatively high precision.

III. GLASSWARE AND SAMPLE PREPARATION

Table 1.4. The water temperature.

Container Temperature (°C)

250 mL beaker 21°C

Distilled water bottle 22°C

IV. CALIBRATION OF 50 mL BURET

Table 1.5. Calibration of 50 mL buret.

Conditions Trial 1

Mass of Erlenmeyer flask, g 113.723 g

10-mL delivery (1st)

Final Volume, mL 10.03 mL

Initial Volume, mL 0.00 mL

Volume used, mL 10.03 mL

Mass of flask + 10 mL water, g 123.980 g

Mass of water, g 10.257g

10-mL delivery (2nd)

Final Volume, mL 20.05 mL

Initial Volume, mL 10.03 mL

Volume used, mL 10.02 mL

Mass of flask + 10 mL water, g 133.989 g

continuation of table 1.5.
Mass of water, g 10.009 g

10-mL delivery (3rd)

Final Volume, mL 30.06 mL

Initial Volume, mL 20.05 mL

Volume used, mL 10.01 mL

Mass of flask + 10 mL water, g 143.833 g

Mass of water, g 9.844 g

10-mL delivery (4th)

Final Volume, mL 40.08 mL

Initial Volume, mL 30.06 mL

Volume used, mL 10.02 mL

Mass of flask + 10 mL water, g 153.981 g

Mass of water, g 10.148 g

10-mL delivery (5th)

Final Volume, mL 50.08 mL

Initial Volume, mL 40.08 mL

Volume used, mL 10.00 mL

Mass of flask + 10 mL water, g 163.977 g

Mass of water, g 9.996 g

Mass of Erlenmeyer flask, g 113.814 g

20-mL delivery (1st)

Final Volume, mL 20.03 mL

Initial Volume, mL 0.00 mL

Volume used, mL 20.03 mL

continuation of table 1.5.
Mass of flask + 20 mL water, g 133.435 g

Mass of water, g 19.624 g

20-mL delivery (2nd)

Final Volume, mL 40.05 mL

Initial Volume, mL 20.03 mL

Volume used, mL 20.02 mL

Mass of flask + 20 mL water, g 153.455 g

Mass of water, g 20.02 g

Mass of Erlenmeyer flask, g 113.681 g

30-mL delivery (1st)

Final Volume, mL 30.04 mL

Initial Volume, mL 0.00 mL

Volume used, mL 30.04 mL

Mass of flask + 30 mL water, g 143.493 g

Mass of water, g 29.812 g

Mass of Erlenmeyer flask, g 113.735 g

40-mL delivery (1st)

Final Volume, mL 40.08 mL

Initial Volume, mL 0.00 mL

Volume used, mL 40.08 mL

Mass of flask + 40 mL water, g 153.774 g

Mass of water, g 40.039 g

Mass of Erlenmeyer flask, g 113.878 g

50-mL delivery (1st)

continuation of table 1.5.
Final Volume, mL 50.03 mL

Initial Volume, mL 0.00 mL

Volume used, mL 50.03 mL

Mass of flask + 50 mL water, g 163.527 g

Mass of water, g 49.747 g

Table 1.6. Volumes for the 50 mL buret.

Conditions Trial 1

10-mL delivery (1st)

Apparent volume, mL 10.03 mL

Mass of water, g 10.257 g

Corrected mass, g 10.2728 g

True volume, mL 10.2959 mL

Correction value, mL 0.2659 mL

10-mL delivery (2nd)

Apparent volume, mL 10.02mL

Mass of water, g 10.009g

Corrected mass, g 10.0244 g

True volume, mL 10.0468 mL

Correction value, mL 0.0268 mL

10-mL delivery (3rd)

Apparent volume, mL 10.01 mL

Mass of water, g 9.844 g

Corrected mass, g 9.8592 g

continuation of table 1.6.
True volume, mL 9.8812 mL

Correction value, mL -0.1288 mL

10-mL delivery (4th)

Apparent volume, mL 10.02 mL

Mass of water, g 10.148 g

Corrected mass, g 10.1636 g

True volume, mL 10.1863 mL

Correction value, mL 0.1663 mL

10-mL delivery (5th)

Apparent volume, mL 10.00 mL

Mass of water, g 9.996 g

Corrected mass, g 10.0114 g

True volume, mL 10.0337 mL

Correction value, mL 0.0532 mL

20-mL delivery (1st)

Apparent volume, mL 20.03 mL

Mass of water, g 19.624 g

Corrected mass, g 19.6542 g

True volume, mL 19.6981 mL

Correction value, mL -0.3319 mL

20-mL delivery (2nd)

Apparent volume, mL 20.02 mL

Mass of water, g 20.02 g

Corrected mass, g 20.2311 g

continuation of table 1.6.
True volume, mL 20.0956 mL

Correction value, mL 0.0756 mL

30-mL delivery (1st)

Apparent volume, mL 30.04 mL

Mass of water, g 29.812 g

Corrected mass, g 29.8579 g

True volume, mL 29.9245 mL

Correction value, mL -0.1155 mL

40-mL delivery (1st)

Apparent volume, mL 40.08 mL

Mass of water, g 40.039 g

Corrected mass, g 40.1007 g

True volume, mL 40.1901 mL

Correction value, mL 0.1101 mL

50-mL delivery (1st)

Apparent volume, mL 50.03 mL

Mass of water, g 49.747 g

Corrected mass, 49.8236 g

True volume, mL 49.9348 mL

Correction value, mL -0.0956 mL

 Correction values vs Apparent volume
0.3

0.2

0.1
Correction value, mL

0
0 10 20 30 40 50 60
-0.1

-0.2

-0.3

-0.4
Apparent volume, mL

Correction value, mL

Figure 1. Correction values vs apparent volume

V. CALIBRATION OF 10 mL VOLUMETRIC PIPET

Table 1.7. Calibration of 10 mL measuring pipet.

Conditions Trial 1 Trial 2

Mass of beaker, g 27.846 g 27.895 g

10-mL delivery (1st trial)

Volume delivered, mL 10.03 mL 10.05 mL

Mass of beaker + 10 mL
37.142 g 37.744 g
water, g
Mass of water, g 9.296 g 9.849 g

Corrected mass, g 9.3102 g 9.8641 g

True volume, mL 9.3289 mL 9.8839 mL

10-mL delivery (2nd trial)

Volume delivered, mL 10.05 mL 10.08 mL

Mass of beaker + 10 mL
47.128 g 47.882 g
water, g
continuation of table 1.7.
Mass of water, g 9.986 g 10.138 mL

Corrected mass, g 10.0013 g 10.1535 g

True volume, mL 10.0214 mL 10.1739 mL

10-mL delivery (3rd trial)

Volume delivered, mL 10.03 mL 10.03 mL

Mass of beaker + 10 mL
57.104 g 57.808 g
water, g
Mass of water, g 9.976 g 9.926 g

Corrected mass, g 9.9913 g 9.9412 g

True volume, mL 10.0113 mL 9.9611 mL

Statistical Analysis

Average volume 9.7872 mL 10.0063 mL

Standard deviation 0.39692 mL 0.150193 mL

Relative standard
0.0405547 0.0150098
deviation
95% confidence interval μ = 9.7872 mL ± 0.9861 mL μ = 10.0063 mL ± 0.3731 mL

% relative error -2.1279 % 0.06313 %

Proper use of calibrated volumetric glassware requires that the user be informed
whether the ware is a “to contain” or “to deliver” vessel. Most of the calibrated volumetric
glassware is marked either “TC” or “TD”. When the graduation line denotes the volume
contained in the calibrated vessel, the glassware is marked “TC”. When the graduation line
indicates the volume delivered from the vessel, the glassware is marked “TD”. When a vessel
is calibrated “TD”, it differs from a “TC” calibrated vessel because of a drainage holdback
error, the amount of water required to wet the inner surface of the vessel in contact with the
water, is added to the contained volume. The “TD” vessel then delivers the same volume as
contained in a “TC” vessel (HACH, 2018).

The meniscus is the curve seen at the top of a liquid in response to its container. The
meniscus can be either concave or convex, depending on the surface tension of the liquid and
its adhesion to the wall of the container. A concave meniscus occurs when the molecules of
the liquid are more strongly attracted to the container than to each other. The liquid appears
to "stick" to the edge of the container. Most liquids, including water, present a concave
meniscus. More likely than not, the bottom of the meniscus is lightened by random
reflections in the laboratory. Such variability can produce errors of several hundredths of a
milliliter. A buret card or meniscus reader offers the student a constant dark reflection
against a white background for higher precision in determining relative titrant volumes
(Seely, 2019).

Changes in the environment that interfere with the measurement process and
sometimes imperfect methods of observation such as parallax errors and offset errors are
the errors that could have occurred causing the error to exceed the tolerance volumes for
class A glassware.

Summary and Conclusion

The experiment showed the different methods that can be used to measure a sample's
mass and the factors that can cause variance or errors to be observed. However, certain
factors can affect the accuracy and precision of data gathered, such as temperature and
humidity fluctuations, air currents, vibration, and operator errors. Errors made by the
observer and other systemic errors, such as environmental and instrumental errors, cannot
be avoided but can be minimized.

By rehearsing the convention off right weighing, accuracy in measuring mass can be
achieved. Many errors can be reduced by ensuring that the factors that can affect
measurement accuracy and precision are monitored or prevented. Also, the analysis of
statistical data parameters increases the identification and assessment of acceptable or
unacceptable data.

The experiment verified the concept of how to calibrate glassware, such as burets and
pipets. The glasswares should have already been tested by the manufacturer, but it would be
essential to calibrate the instruments to ensure that possible errors could be reduced. As
random errors can always occur even in a controlled laboratory setting.

Certain factors that can affect the precision and accuracy of measurements of
glasswares are quite a few. A difference in temperature can affect the density of the liquid
being contained or transferred. Density is the mass to volume ratio of a substance such that
the liquid, which is significant since, for every degree of change, there would be a notable
difference in the density. This is because the mass of the water is affected by buoyancy.
Changes due to a difference in temperature, plus other environmental factors, will cause a
significant change between the volume obtained, and the true volume.
Sample Calculations

I. ANALYTICAL WEIGHING

Mass crucible and cover – Mass crucible only = 45.696 g − 29.855 g = 15.841g
Mass salt (by addition) = 30.362 g − 29.068 g = 1.294 g
Mass salt (by difference) = 4.323 g − 3.023 g = 1.3 g
Mass water (by addition) = 42.290 g − 30.362 g = 11.928 g
Mass water (by difference) = 157.716 g − 145.783 g = 11.933 g

II. STATISTICAL EVALUATION OF MEASUREMENTS

|x𝑎 − xb |
Q-test =
R
Qcritical value = 0.412
|5.440 g − 5.412 g|
Q𝑒𝑥𝑝 = = 0.1407
0.199 g
Since 0.1407 < 0.412, therefore 5.440 g is not an outlier
|5.294 g − 5.241 g|
Q𝑒𝑥𝑝 = = 0.2663
0.199 g
Since 0.2663 < 0.412, therefore 5.241 g is not an outlier

Σx
x̅ =
n
x̅ = (5.241 g + 5.294 g + 5.318 g + 5.328 g + 5.344 g + 5.351 g
+ 5.351 g + 5.393 g + 5.412 g + 5.440 g)/(10 )
x̅ = 5.349 g

Σ di
d̅ =
n
d̅ = (1/10) (∣ 5.3487 − 5.241 ∣ + ∣ 5.3487 − 5.294 ∣ + ∣ 5.3487 − 5.318 ∣ +
∣ 5.3487 − 5.328 ∣
+ ∣ 5.3487 − 5.344 ∣ + ∣ 5.3487 − 5.351 ∣ + ∣ 5.3487 − 5.366 ∣ + ∣ 5.3487 − 5.393 ∣
+ ∣ 5.3487 − 5.412 ∣ + ∣ 5.3487 − 5.440 ∣)
̅d = (1/10)(0.1077 + 0.0547 + 0.0307 + 0.0207 + 0.0047 + 0.0023 +
0.0173 + 0.0443 + 0.0633 + 0.0913)
d̅ = 0.0437g

Range = w = 𝑥largest − 𝑥smallest

Range = 5.440 g − 5.241g = 0.199 g
 Σ (xi − x̅)2
s= √
n−1
s = 0.058 g

s
CV = x 100
x̅
0.058 g
CV = 𝑥 100
5.349 g
CV = 1.09%

𝑠
Confidence limits of the mean (90% level) = x̅ ± t ( )
√𝑛
0.058𝑔
Confidence limits of the mean (90% level) = 5.349 g ± 1.833 ( )
√10
Confidence limits of the mean (90% level) = 5.349g ± 0.0338g

III. CALIBRATION OF 50 mL BURET

Volume used = Final Volume − Initial Volume

Volume used = 10.03mL − 0.00mL = 10.03mL

Mass of water = (Mass of flask + 10 mL water) − Mass of Erlenmeyer flask

Mass of water = 123.980 g − 113.723 g = 10.257 g

mass of H2 O with buoyancy effects = mass of H2 O ∙ buoyancy correction

mass of H2 O with buoyancy effects = 10.257 g ∙ 1.00154
mass of H2 O with buoyancy effects = 10.2728 g

corrected mass of H2 O
true volume =
density of H2 O at specified temperature
10.2728g
true volume = g
0.9977735 3
m
true volume = 10.2959 mL

correction value = true volume − apparent volume

correction value = 10.2959 mL − 10.03mL
correction value = 0.2659 mL
IV. CALIBRATION OF 10 mL VOLUMETRIC PIPET

Mass of water = (Mass of beaker + 10 mL water) − Mass of beaker

Mass of water = 37.744 g − 27.895 g = 9.849g

mass of H2 O with buoyancy effects = mass of H2 O ∙ buoyancy correction

mass of H2 O with buoyancy effects = 9.849 g ∙ 1.00153
mass of H2 O with buoyancy effects = 9.8641 g

corrected mass of H2 O
true volume =
density of H2 O at specified temperature
9.8641 g
true volume = g
0.9979955 3
m
true volume = 9.8839 mL

Σx
x̅ =
n
x̅ = (9.88388121 mL + 10.17390473 mL + 9.961153913 mL)/(3)
x̅ = 10.0063 mL

Σ (xi − x̅)2
s= √
n−1
s = 0.1502 mL

s
RSD =
x̅
0.1502 mL
RSD =
10.0063 mL
RSD = 0.015098

𝑠
95% confidence interval = x̅ ± t ( )
√𝑛
0.1502 mL
95% confidence interval = 10.0063 mL ± 4.303 ( )
√3
95% confidence interval = μ = 10.0063 mL ± 0.3731 mL

measured − actual
% relative error = x 100
actual value
10.0063 mL − 10 mL
% relative error = x 100
10 mL
% relative error = 0.06313%
References

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the-difference-between-to-contain-and-to-deliver-glassware?-.
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