Experiment 5: Determination of Calcium in Tums

Quantitative Analysis II SCH113 03

March 24, 2015
Kayla Chapman
 Chapman 2

I. TITLE:
Determination of Calcium in Tums®

II. OBJECTIVE:
The goal of this experiment is to determine the amount of calcium in a Tums® tablet

using Atomic Absorption Spectroscopy and Gravimetric Analysis.

III. THEORY:

This experiment uses two different methods to try to determine the amount of

calcium in a tums tablet, the AAS method and the Gravimetric Analysis method. It is

always good to have two different techniques to compare results with at the end of

an experiment.

The first approach for this experiment was the AAS. The quantitative analysis

laboratory is equipped with a tool called the Atomic Absorption Spectroscopy, AAS,

which is used to quantitatively determine the amount of metal elements in aqueous

samples. The Atomic Absorption Spectroscopy calculates the absorbance and

average absorbance of a substance. The tool requires samples to be in solution and

works by measuring the absorbance of light corresponding to specific atoms in a

gaseous state. The light source is called a Hallow Cathode lamp, and is element

specific. In this case, the element is calcium. In order to analyze a substance with the

AAS instrument, it is essential to convert it to an aqueous solution. In this specific

experiment, 𝐶𝑎𝐶𝑂3 solid is the initial substance, and because it is not soluble, HCl

was added to convert it to an aqueous solution, creating the reaction

𝐶𝑎𝐶𝑂3(𝑠) + 2𝐻𝐶𝑙(𝑎𝑞) → 𝐶𝑎𝐶𝑜2(𝑎𝑞) + 𝐻2 𝐶𝑂3(𝑎𝑞) → 𝐻2(𝑙) 𝐶𝑂2(𝑔)

The water is added to dilute the substance to get its volume.

 Chapman 3

The second one is the Gravimetric Analysis method. The gravimetric analysis method

is an analytical technique based on the measurement of mass. It is a very accurate

technique measuring concentration to ppm. Instead of using an instrument, this

method involves isolating an ion in a solution by filtering and washing out all excess

material. However, this method can be tricky because in order to work, it must be

completely precipitated. If all the water is not all out, it can compromise the results.

In order to do that, take the constant weight of the empty crucible to make sure

further results will be accurate, then take it again after the product is entered to

make sure all water is out. The purpose of heating the product to constant weight is

to basically to get rid of any excess water in the product that will ultimately affect its

weight and essentially become a source of error. The methyl red indicator is applied

to ensure visibility of the neutralization of the solution. It also makes sure that the

pH stays below 4. Then further more, the urea is added to precipitate the calcium

back out of the solution by creating the insoluble oxalate compound, which can be

represented by

𝐶𝑎𝐶𝑙2(𝑎𝑞) + (𝑁𝐻4 )2 𝐶2 𝑂4 → 2𝑁𝐻4 𝐶𝑙(𝑎𝑞) + 𝐶𝑎𝐶2 𝑂4 ∙ 𝐻2 𝑂(𝑠)

The urea ensures that the reaction is back in neutral condition.

IV. PROCEDURE:
First weigh a Tums® tablet and record it’s mass to 0.1 mg, then thoroughly crush the

tablet. Transfer the crushed tablet into a weighing bottle and cry it in the oven for

about one hour. After completely cooled, transfer 0.0202 of tablet into a 100mL

beaker. Next add 5.0 mL of 6.0M HCl into the beaker and record. Then add 50 mL of
 Chapman 4

distilled water into the beaker and transfer it into a 500 mL flask. Next, add 0.5g of

KCl to the flask and swirl until dissolved. Finally dilute to the volume with distilled

water. Next weigh 0.3500 g of the tablet into a 250mL beaker and add 100 mL of

distilled water. Then add 6mL or 6 M HCl and swirl until dissolved while recording

observations. Next take the pH to ensure the pH is 1. Then add 5 drops of methyl red

indicator and swirl, then add 25 mL of the ammonium oxalate (𝑁𝐻4 )2 𝐶2 𝑂4 and 15g

of urea. Next heat the solution on a hot plate until the solution turns yellow. Next

use a vacuum to remove all precipitate from the beaker. Rinse the beaker out with

acetone and distilled water. Let the crucible sit for about 30 minutes then bring the

crucible to constant weight again. Finally, put about 250 mL of the calcium

carbonate solution into a 500 mL volumetric flask and use the AAS instrument to

determine the average absorbances.

V. DATA:
TUMS® Tablet Information from Bottle:
Calcium Carbonate Tums® Antacid: Peppermint, Ultra Strength 1000. 400mg
Calcium per Tablet
Mass of Tums® tablet, whole: 2.5307 g
Mass of Tums® tablet, used for AAS solution: 0.0202 g
Mass of Tums® tablet, used for gravimetric analysis solution: 0.3505 g

Table 1. Atomic Absorption Data For Calcium Carbonate Standard Solutions And Tums Solutions
Standard (ppm) Abs. 1 Abs. 2 Abs. 3 Average
Absorbance
0 .003 .002 .004 .003
2.5 .112 .112 .113 .113
5 .215 .211 .210 .212
10 .386 .385 .384 .385
15 .565 .559 .561 .561
Tums® .232 .233 .233 .233
 Chapman 5

Table 2. Constant Weight of Crucible

Empty Crucible Crucible With Product
Reading 1 30.6201 g 30.8325 g
Reading 2 30.6201 g 30.8278 g
Reading 3 30.6197 g 30.8276 g
Reading 4 N/A 30.8263 g
Reading 5 N/A N/A
Reading 6 N/A N/A
*Constant Weight = average of two rdgs within +/- 0.4 mg

VI. CALCULATIONS:
Atomic Absorption Spectroscopy
1. Graph 1. Beer’s Law Plot

AAS Readings
0.6
0.5
Absorbance

0.4
0.3
0.2
0.1
0
0 2 4 6 8 10 12 14 16
y = 0.0367x + 0.016 Concentration(ppm)

i. Adding a trend line will lead to an equation that will assist in helping find

concentration of AAS Tums® solution:

𝑦 = 0.0367𝑥 + 0.016

. 244 = 0.0367𝑥 + 0.016

. 228 = 0.0367𝑥

𝒙 = 𝟔. 𝟐𝟏𝟐𝟓 𝒑𝒑𝒎

ii. Use Volume and 1ppm = 1 mg/L to calculate mg of calcium in the solution.
 Chapman 6

1 𝑚𝑔
1 𝑝𝑝𝑚 =
𝐿

500 𝑚𝐿 = .5 𝐿

. 5𝐿 𝑥 6.2125 𝑝𝑝𝑚 = 𝟑. 𝟏𝟎𝟔𝟐𝟓 𝒎𝒈 𝒐𝒇 𝑪𝒂

iii. The concentration of Ca. in Tums is calculated by dividing by the mass of Tums used

to make solution:

3.10625 𝑚𝑔 𝒎𝒈
= 𝟏𝟓𝟑
0.0202 𝑔 𝑇𝑢𝑚𝑠® 𝒈

iv. With the average grams of Tums to the manufacturer’s claim (400 mg Ca. per

tablet), you are able to calculate it’s percent error:

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑔 𝑜𝑓 𝑇𝑢𝑚𝑠® = 𝟐. 𝟓𝟗𝟓𝟒 𝐠

400 𝑚𝑔
= 𝟏𝟓𝟖. 𝟎𝟔 𝒈
2.5307 𝑔

|𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 − 𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙|
𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝐸𝑟𝑟𝑜𝑟 = 𝑥 100
|𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙|

| 158𝑔 − 158𝑔 |
𝑥 100 = 𝟏. 𝟑%
|158𝑔|

2. Collect values from others and conduct the following test:

156 mg/g 152 mg/g 156 mg/g 153 mg/g

 Chapman 7

a. A Q-Test is conducted to determine if any suspicious result can be omitted.

In this experiment, a Q test was not conducted because all results were

reasonable. Nothing was suspicious.

b. The average is calculated because it will be needed in future equations,

also to get an overall number for the experiment.

∑ 𝑥𝑖
𝑥̅ = 𝑎𝑣𝑒𝑟𝑎𝑔𝑒 =
𝑁

𝑥𝑖 = 𝑖𝑛𝑑𝑖𝑣𝑖𝑑𝑢𝑎𝑙 𝑑𝑎𝑡𝑎 𝑝𝑜𝑖𝑛𝑡𝑠 𝑁 = 𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑑𝑎𝑡𝑎 𝑝𝑜𝑖𝑛𝑡𝑠

𝑚𝑔 𝑚𝑔 𝑚𝑔 𝑚𝑔
∑(156 + 152 + 156 + 153
𝑔 𝑔 𝑔 𝑔 ) 𝒎𝒈
= 𝟏𝟓𝟐 𝑪𝒂
4 𝒈

c. Standard deviation is calculated to see how much the data points deviate

from the average.

∑(𝑥̅ − 𝑥𝑖 )2
𝑠=√
𝑁−1

𝒎𝒈
𝒔 = 𝟏𝟓𝟒 ± 𝟒
𝒈

d. The Coefficient Variation is an indication of the precision of the data.

𝑠
𝐶𝑉 = 𝑥 100
𝑥̅
 Chapman 8

𝒎𝒈
𝟏𝟓𝟒 ± 𝟒 𝒈
𝑪𝑽 = 𝒎𝒈 𝒙 𝟏𝟎𝟎 = 𝟐 . 𝟔𝟑% 𝒐𝒓 𝟑%
𝟏𝟓𝟐 𝒈

3. Compare your result to the manufacturer’s claim from the bottle label using % error

|𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 − 𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙|
𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝐸𝑟𝑟𝑜𝑟 = 𝑥 100
|𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙|

|152𝑔 − 150𝑔|
𝑥 100 = 𝟏. 𝟑%
|150𝑔|

Gravimetric Analysis

1. Calculate the average of the 2 constant weight crucible to get an overall general number

for each, the empty crucible and the one with product.

∑ 30.6201 𝑔 + 30.6201 𝑔
= 𝟑𝟎. 𝟔𝟐𝟎𝟏 𝒈 (𝑬𝒎𝒑𝒕𝒚 𝑪𝒓𝒖𝒄𝒊𝒃𝒍𝒆)
2

∑ 30.8267 𝑔 + 30.8264 𝑔
= 𝟑𝟎. 𝟖𝟐𝟔𝟓 𝒈 (𝑪𝒓𝒖𝒄𝒊𝒃𝒍𝒆 𝒘𝒊𝒕𝒉 𝑷𝒓𝒐𝒅𝒖𝒄𝒕)
2

2. Then subtract the difference to find the mass of the product so the moles of Ca can be

calculates.

30.8265 𝑔 − 30.6201 𝑔 = 𝟎. 𝟐𝟎𝟔𝟓 𝒈

3. Convert the grams 𝐶𝑎𝐶2 𝑂4 ∙ 𝐻2 𝑂 to moles to get the mg of Ca collected, then divide by

the mass of Tums® (0.35 mg) to get experimental yield. Then determine the percent

error:
 Chapman 9

Molecular Weight 𝐶𝑎𝐶2 𝑂4 ∙ 𝐻2 𝑂 = 146.12 gg

Molecular Weight Ca: 40.08 g

1 𝑚𝑜𝑙 0.2065
𝑥 = 𝟎. 𝟎𝟎𝟏𝟒𝟏𝟑 𝒎𝒐𝒍 𝑪𝒂𝑪𝟐 𝑶𝟒 ∙ 𝑯𝟐 𝑶
142.12 𝑔 𝐶𝑎𝐶2 𝑂4 ∙ 𝐻2 𝑂

0.001413 𝑚𝑜𝑙 40.08 𝑔 𝐶𝑎 1 𝑚𝑔

𝑥 = .05663 𝑔 𝐶𝑎 𝑥 = 𝟓𝟔. 𝟔𝟑 𝒎𝒈 𝑪𝒂
1 1 𝑚𝑜𝑙 1000𝑔

56.63 𝑚𝑔 𝐶𝑎 𝒎𝒈
= 𝟏𝟔𝟏. 𝟖
0.35 𝑚𝑔 𝑇𝑢𝑚𝑠 𝒈

|162𝑔 − 150𝑔|
𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝐸𝑟𝑟𝑜𝑟 = 𝑥 100 = 𝟖%
|150𝑔|

4. Collect values from others and conduct the following test:

162 mg/g 167 mg/g 165 mg/g 166 mg/g

a. A Q-Test is conducted to determine if any suspicious result can be omitted.

In this experiment, a Q test was still not conducted because all results were

reasonable. Nothing was suspicious.

 Chapman 10

b. The average is calculated because it will be needed in future equations,

also to get an overall number for the experiment.

∑ 𝑥𝑖
𝑥̅ = 𝑎𝑣𝑒𝑟𝑎𝑔𝑒 =
𝑁

𝑥𝑖 = 𝑖𝑛𝑑𝑖𝑣𝑖𝑑𝑢𝑎𝑙 𝑑𝑎𝑡𝑎 𝑝𝑜𝑖𝑛𝑡𝑠 𝑁 = 𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑑𝑎𝑡𝑎 𝑝𝑜𝑖𝑛𝑡𝑠

𝑚𝑔 𝑚𝑔 𝑚𝑔 𝑚𝑔
∑(162 + 167 + 166 + 165 ) 𝒎𝒈
𝑔 𝑔 𝑔 𝑔
= 𝟏𝟔𝟓 𝑪𝒂
4 𝒈

c. Standard deviation is calculated to see how much the data points deviate

from the average.

∑(𝑥̅ − 𝑥𝑖 )2
𝑠=√
𝑁−1

𝒎𝒈
𝒔 = 𝟏𝟔𝟓 ± 𝟐
𝒈

d. The Coefficient Variation is an indication of the precision of the data.

𝑠
𝐶𝑉 = 𝑥 100
𝑥̅

𝒎𝒈
𝟏𝟔𝟓 ± 𝟐 𝒈
𝑪𝑽 = 𝒎𝒈 𝒙 𝟏𝟎𝟎 = 𝟏. 𝟐𝟏%
𝟏𝟔𝟓 𝒈
 Chapman 11

5. Compare your result to the manufacturer’s claim from the bottle label using % error

|𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 − 𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙|
𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝐸𝑟𝑟𝑜𝑟 = 𝑥 100
|𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙|

|165𝑔 − 150𝑔|
𝑥 100 = 𝟏𝟎%
|150𝑔|

6. Calculate percent difference to see the difference between the two methods.

|𝐴𝐴𝑆 − 𝐺𝑟𝑎𝑣𝑖𝑚𝑒𝑡𝑟𝑖𝑐|
𝑃𝑒𝑟𝑐𝑒𝑛𝑡 𝐷𝑖𝑓𝑓𝑒𝑟𝑒𝑛𝑐𝑒 = 𝑥 100
𝐵𝑖𝑔𝑔𝑒𝑟 𝑁𝑢𝑚𝑏𝑒𝑟

|152𝑔 − 165𝑔|
𝑥 100 = 𝟕. 𝟖𝟕%
165𝑔

VII. DISCUSSION:
All goals were achieved in this goal. Both the AAS and Gravimetric method were

conducted properly. The percent error for the AAS method was 1.3% and 10% for

the gravimetric. This proved that the AAS method was more accurate. However, the

CV% for AAS was 3% while the Gravimetric was only 1.2%, thus proving that the

Gravimetric analysis method is ore precise, proving overall it is the better method.

The percent error for the AAS After getting group results, the percent difference is

only 7.87%. The average for the AAS method is 152 mg/g and 165 mg/g for the

Gravimetric method. The gap in these averages can be a result from the sources of

error for each. Sources of error for AAS include the dilute standards or
 Chapman 12

contamination from the tap water. For the Gravimetric, errors could include that not

all water was removed at constant weight, the crucible not being at room

temperature, or even the product not being rinsed enough during filtration. Overall,

I learned how to extract calcium from a Tums® tablet and conducted a successful

experiment due to the circumstances. I also learned that the Gravimetric Analysis

method is more precise, giving better results, whole the AAS method is more

accurate. Although the other Tums® ingredients were probably mixed in with the

product the amount of calcium was still reasonable. Overall, my omly complaint

about this lab was it took multiple classes to compete it, and that can put the

experiment at a higher risk for even more sources or error. Other then that, I have

no suggestions to improve this lab.

 Chapman 13

Works Cited

Department of Chemistry, Texas A&M University. "GRAVIMETRIC ANALYSIS." Gravimetric

Analysis. Texas A&M University, 2015. Web. 19 Mar. 2015.
<https://www.chem.tamu.edu/class/majors/tutorialnotefiles/gravimetric.h
tm>.

"Task 1. Atomic Absorption Spectroscopy." LTT. Australian Council for Private Education
and Training, 2012. Web. 23 Mar. 2015.
<http://www.ltt.com.au/simulab/5/PMLTEST506/41step01.htm>.