11/15/2021 Practical 9:

Gravimetric
analysis
Analysis of chloride by gravimetry

Nothando Sharon Mthethwa (220020733)

This study source was downloaded by 100000842939993 from CourseHero.com on 10-14-2022 06:43:51 GMT -05:00

https://www.coursehero.com/file/143506576/prac-9-apch-321pdf/
 AIM

To introduce gravimetric analysis and in order to be able to compare and differentiate the two methods of
analysis.

PROCEDURE

Pipette 20ml of sample into 400ml beakers. In each sample add 50ml of distilled water and 2-3 ml of 6M
HNO3. Add about 20ml of 0.2M AgNO3 to each of the samples and stir well until the AgCl is coagulated and
add 3 to 5 ml. Heat to almost boiling for about 10 mins. Add a few drops of AgNO3 to confirm that
precipitation is complete. If more precipitate forms, add 3 mL of AgNO3, digest, and again test for
completeness of precipitation. Pour any unused AgNO3 into a waste container. Cover each beaker, and
store in a dark place for at least 1 hr. Wash the precipitates several times with a solution consisting of 2 to 5
mL of 6 M HNO3 per litter of distilled water; decant these washings through the filters. Transfer the AgCl
from the beakers to the individual crucibles with fine streams of wash solution; use rubber policemen to
dislodge any particles that adhere to the walls of the beakers. Continue washing until the filtrates are
essentially free of Ag+ ion. Dry the precipitate at 110°C for at least 1 hr. Store the crucibles in a desiccator
while they cool. Find out the mass of the crucibles and their contents. Repeat the cycle of heating, cooling,
and weighing until consecutive weighing agree to within 0.2 mg. Determine the mass of the crucibles and
their contents. Repeat the cycle of heating, cooling, and weighing until consecutive weighing agree to
within 0.2 mg. You will probably allow them to dry overnight and weigh the next day; in this case you will
not have to test to see if the sample is properly dry. Calculate the percentage of chloride in the sample.

RESULTS

1. Personal Mass of the AgCl = 0.2105 g

1.1 Average mass of AgCl = 0.2276 g

Moles of AgCl = 0.2276/143.32

= 1.588x10-3 moles

Moles of Cl = 1.588x10-3 moles

Mass of Cl = 1.588x10-3 ×35.45

= 0.05629 g

% Chloride = 0.0563/0.2276 ×100

= 24.73%

1.2 Average mass of AgCl =0.2454 g

Moles of AgCl = 0.2454/143.32

= 1.712x10-3 moles

Moles of Cl = 1.712x10-3 moles

Mass of Cl = 1.712x10-3 ×35.45

= 0.0607 g

% chloride = 0.0607/0.2454 ×100

This study source was downloaded by 100000842939993 from CourseHero.com on 10-14-2022 06:43:51 GMT -05:00

https://www.coursehero.com/file/143506576/prac-9-apch-321pdf/
 =24.73%

1.3 Average mass of AgCl = 0.2165 g

Moles of AgCl = 0.2165/143.32
= 1.5104x10-3 moles

Moles of Cl = 1.5104x10-3 moles

Mass of Cl= 1.5104x10-3 ×35.45

= 0.0535 g

% Chloride = 0.0535/0.2165×100
= 24.73%

𝐸𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 𝑦𝑖𝑒𝑙𝑑−𝑡ℎ𝑒𝑜𝑟𝑖𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑

1.4 % Error for Thursday group = ×100
𝑇ℎ𝑒𝑜𝑟𝑖𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
= 0.2105 g – 0.2276 g /0.2276 g × 100
= 7.51%

𝐸𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 𝑦𝑖𝑒𝑙𝑑−𝑡ℎ𝑒𝑜𝑟𝑖𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑

% Error for Friday group = 𝑇ℎ𝑒𝑜𝑟𝑖𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
×100
= 0.2105g-0.2454g/0.2454g ×100

= 14.22%
𝐸𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡𝑎𝑙 𝑦𝑖𝑒𝑙𝑑−𝑡ℎ𝑒𝑜𝑟𝑖𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
% Error for combined group= 𝑇ℎ𝑒𝑜𝑟𝑖𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
×100

= 0.2105-0.4730/0.4730×100

= 55.50%

Normal Distribution of Thursday group

14

12

10

0
0 0,05 0,1 0,15 0,2 0,25 0,3 0,35
X

Series1
A.

This study source was downloaded by 100000842939993 from CourseHero.com on 10-14-2022 06:43:51 GMT -05:00

https://www.coursehero.com/file/143506576/prac-9-apch-321pdf/
 Normal Distribution for Friday group
3,5

2,5

2
Y

1,5

0,5

0
-0,2 -0,1 0 0,1 0,2 0,3 0,4 0,5 0,6 0,7
X
B.

Normal Distrubution curve for both groups

4,5

3,5

2,5
Y

1,5

0,5

0
-0,1 0 0,1 0,2 0,3 0,4 0,5 0,6
X

3.1. Population standard deviation of the entire APCH 231 class = 0,1342

3.2. For Thursday Group: Standard deviation = 0,02990

For Friday Group: Standard Deviation = 0,1344

3.3.

Thursday Group Standard Deviation Friday Group Standard Deviation

This study source was downloaded by 100000842939993 from CourseHero.com on 10-14-2022 06:43:51 GMT -05:00

https://www.coursehero.com/file/143506576/prac-9-apch-321pdf/
 Bench A 0,003045 Bench A 0,0009142
Bench B 0,003950 Bench B 0,02928
Bench C 0,07027 Bench C 0,07180
Bench D 0,004006 Bench D 0,1108
Bench E 0,006498 Bench E 0,2432

𝑠𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝑑𝑒𝑣𝑖𝑎𝑡𝑖𝑜𝑛
3.4. % RSD For Thursday = 𝐴𝑣𝑒𝑟𝑎𝑔𝑒
× 100

= 0,0299/0,2275 ×100

= 13.14 %
𝑆𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝑑𝑒𝑣𝑖𝑎𝑡𝑖𝑜𝑛
% RSD For Friday = 𝐴𝑣𝑒𝑟𝑎𝑔𝑒
× 100

= 0,1344/0,2454 × 100

= 54.76 %

3.5. X ± Zs√n
0.473+/_ 1.96×0.1342/ √44

= 0.5127 or 0.4333

3.6. 0.473+/_ 1.96×0.1342

= 0.4135

3.7.

Thursday Group Confidence Limit Friday Group Confidence Limit

Bench A 0,004845 Bench A 0,001455
Bench B 0,006285 Bench B 0,04658
Bench C 0,1118 Bench C 0,1143
Bench D 0,004974 Bench D 0,1377
Bench E 0,008068 Bench E 0,3019

3.8. 95 % Confidence Limit for Thursday Group = 0,01293

3.9. 95 % Confidence Limit for Friday Group = 0,05959

DISCUSSION

The AgCl precipitate produced had high level of standard deviation from the mean. The Thursday standard
deviation is 0,02990 which is lesser than any of the groups. The Friday standard deviation is 0,1344 and the
combined standard deviation is 0,1342. The percentage of RSD were low but the combined measurement
had high percentage of RSD. The RSD for Thursday group was 7.51%, for Friday group was 14.22% and for
combined group is 55.50%. The precipitate was measured by difference and was 0.2105g.

CONCLUSION

The Fridays group data was outside the 95% confidence interval. The results show that more analysis is
needed to obtain an accurate mass.

This study source was downloaded by 100000842939993 from CourseHero.com on 10-14-2022 06:43:51 GMT -05:00

https://www.coursehero.com/file/143506576/prac-9-apch-321pdf/
 REFERENCES

APCH 231 Practical manual chemical analysis Ajay bissessur

This study source was downloaded by 100000842939993 from CourseHero.com on 10-14-2022 06:43:51 GMT -05:00

https://www.coursehero.com/file/143506576/prac-9-apch-321pdf/
Powered by TCPDF (www.tcpdf.org)