Analytical Chemistry Laboratory Report 1

Analytical Chemistry I (Sheridan College)

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 ANALYTICAL CHEMISTRY LABORATORY REPORT SHEET

Laboratory Title: Determination of Total Suspended Solids and Determination of Method

Detection Limit

Partner A
Name: Thinh Vo or B: B

Lab Partner: Ning Zhu

Date Performed: Sep 11 2019

Date Due: Sep 18 2019

Date Submitted: Sep 18 2019

RESULTS:
Sample: Lake water

Result (mean) 400 mg/L

Standard
deviation 240.2 mg/L
% Relative Standard
Deviation (% RSD) 60%

Sample: CaCO3 Suspension

Result (mean) 262 mg/L
37.92
Standard deviation mg/L
% Relative Standard Deviation (% RSD) 14%

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 Laboratory 1: Determination of Total Suspended Solids and Determination of
Method
Detection Limit

Table of Contents
Purpose:.....................................................................................................................................1
Observations..............................................................................................................................1
Numerical Observations............................................................................................................1
Calculations...............................................................................................................................1
Result.........................................................................................................................................4
Conclusion..................................................................................................................................4
Possible Sources Of Error..........................................................................................................5
Reference:..................................................................................................................................5

Table of Tables

Table 1: Data of recorded mass of GFF and residue.................................................................1

Table 2: Calculating Standard Deviation Table of Lake Sample.................................................2
Table 3: Calculating Standard Deviation Table of CaCO3 Suspension........................................3
Table 4: Values for calculating MDL...........................................................................................3
Table 5: Summary of Lake Sample.............................................................................................4
Table 6: Summary of CaCO3 Suspension...................................................................................4

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 Laboratory 1: Determination of Total Suspended Solids and Determination of
Method
Detection Limit

Purpose:
This laboratory 1 let students study how to determine Total Suspended Solids (TSS) by
taking samples of lake water and using vacuum filtration and oven drying to analyze. 8
replicate measurements of CaCO3 suspension were used to find the Method Detection Limit
(MDL).1

Observations:
For the filtering of the lake water, the residue particles we got that were dark-
green color and there are such things floating on top of the sample. One thing for
noticing is the solid settle was fairly fast. If the sample’s solution was not stirred
about 5s, majority of residues and particles could be seen at the bottom of the
beaker.

Numerical Observations:
Table 1: Data of recorded mass of GFF and residue

GFF number Mass of GFF (g) Mass of GFFF + residue

1 (Lake Sample) 0.2143 0.2400
2 (Lake Sample ) 0.2129 0.2191
3 (Lake Sample ) 0.2188 0.2469
4 (CaCO3) 0.2144 0.2290
5(CaCO3) 0.2137 0.2268
6(CaCO3) 0.2157 0.2250
7(CaCO3) 0.2141 0.2287
8(CaCO3) 0.2142 0.2276
9(CaCO3) 0.2150 0.2289
10(CaCO3) 0.2114 0.2227
11(CaCO3) 0.2143 0.2289

Calculations:
1. Lake Water Sample
Total Suspended Solids (TSS):
( mL
A−B) x 1000
TSS(mg/L) = L
V
• 1st sample of lake water:
( mL
A−B) x 1000
TSS(mg/L) = L
V
( 1000 mg mL
0.2400 g−0.2143 g ) x 1 g x x 1000
TSS(mg/L) = 1g L mg
50 .00 ml =514 L

• 2nd sample of lake water:

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 Laboratory 1: Determination of Total Suspended Solids and Determination of
Method
Thinh Vo- 991519197 Detection Limit

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 Laboratory 1: Determination of Total Suspended Solids and Determination of
Method
mg Detection Limit
124
TSS(mg/L)=
rd
L
• 3 sample of lake water:
mg
=562
TSS(mg/L) L

Standard Deviation (S) of lake

sample: 514
Mean ´x =
3
+124+562
=400
Table 2: Calculating Standard Deviation Table of Lake Sample

TSS xi ´x x
xi−
¿´
¿
¿
¿
1 514 400 12996
2 124 400 76176
3 562 400 26244
x
xi−
¿´
¿
2
¿¿
¿
N

∑¿
i =1
x
xi−
¿´
¿
√
115416
2 = =240.2 mg/L
¿¿ 2
S= N
¿
∑
¿
i =1
¿
√¿
• Standard deviation of lake sample is 240.2 mg/L
Percent relative standard deviation:
• 100 x S 240.2 x 100
%RSD = ´x = 400 =60 %

2. CaCO3 Suspension:
Total Suspended Solids (TSS):
( mL
A−B) x 1000
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 Laboratory 1: Determination of Total Suspended Solids and Determination of
Method
TSS(mg/L) = L Detection Limit
V
• 4th sample of CaCO3:

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 Laboratory 1: Determination of Total Suspended Solids and Determination of
Method
Detection Limit
mL
( A−B) x 1000
TSS(mg/L) = L
V
( 1000 mg mL
0.2290 g−0.2144 g) x 1 g x x 1000
TSS(mg/L) = 1g L mg
=292
• 5th sample of CaCO3: 50.00 ml L
mg
= 262
TSS(mg/L)
th
L
• 6 sample of CaCO3:
mg
= 186
TSS(mg/L)
th
L
• 7 sample of CaCO3:
mg
= 292
TSS(mg/L)
th
L
• 8 sample of CaCO3:
mg
=268
TSS(mg/L)
th
L
• 9 sample of CaCO3
mg
= 278
TSS(mg/L)
th
L
• 10 sample of CaCO3
mg
= 226
TSS(mg/L)
th
L
• 11 sample of CaCO3
mg
= 292
TSS(mg/L) L
Standard Deviation (S) of CaCO3 :

292+262+186+ 292+ 268+278+2 26+292

Mean ´x = =26 2 mg/L
8
Table 3: Calculating Standard Deviation Table of CaCO3 Suspension

TSS xi ´x x
xi−
¿´
¿
¿
¿
4 292 262 900
5 262 262 0
6 186 262 5776
7 292 262 900
8 268 262 36
9 278 262 256
10 226 262 1296
11 292 262 900

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 Laboratory 1: Determination of Total Suspended Solids and Determination of
Method
x Detection Limit
xi−
¿´
¿
2
900 x 3+ 0+3 6+5776+256+1296=¿ 10064
¿¿
¿
N

∑
¿
i =1
x
xi−
¿´
¿

√
100 64
⇨ S= ¿¿
2 = =3 7 . 92 mg/L
7
¿
N

∑
¿
i =1
¿
√¿
Percent relative standard deviation:
100 x S 3 7 . 92
%RSD = ´x = 261.25 x 100 %=14 %
• MDL:
Table 4: Values for calculating MDL

Values
(mg/L)
- Mean = 292
262
186
292
268
278
226
292
292+262+186+ 292+2 68+2 78+2 26+292 mg
8 =2 62 L
- Standard Deviation (SD) = 3 7 . 92 mg mg/L
- Students’ t = 2.998, n =8
⇨ MDL = t x SD =2.998 x 37.92 = 114 mg/L

Result
Table 5: Summary of Lake Sample

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 Laboratory 1: Determination of Total Suspended Solids and Determination of
Method
TSS values for Mean( mg/L) Detection Limit
Standard Percent relative

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 Laboratory 1: Determination of Total Suspended Solids and Determination of
Method
Detection Limit
lake samples deviation of standard
(mg/L) lake deviation (%)
samples(mg/L
)
GFF number 1: 400 240.2 60
514
GFF number 2:
124
GFF number 3:
562

Table 6: Summary of CaCO3 Suspension

TSS values of Mean( mg/L) Standard Percent relative

CaCO3 deviation of standard
suspension(mg/L lake deviation (%)
) samples(mg/L)
GFF number 4: 262 3 7 . 92 14
292
GFF number 5:
262
GFF number 6:
186
GFF number 7:
292
GFF number 8:
268
GFF number 9:
278
GFF number 10:
226
GFF number 11:
292

Conclusion
The Conclusion consists of two sentences which state “The lake water sample was found to
have a TSS value of 400 mg/L with a relative standard deviation of 49%. The Method
Detection Limit for TSS was found to be 114mg/L”.

Possible Sources Of Error

1. The first source of error is likely deriving from weighting Glass Fibre Filters (GFF)
if they still remains water. Before putting GFFs on a top loader balance, we
should ensure those are dried and cooled at the appropriate temperature for
sufficient amount of time to let filters are water-free completely. Unless, the
mass would be

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 Laboratory 1: Determination of Total Suspended Solids and Determination of
Method
Detection Limit
heavier than it should be, resulting incorrect calculations of TSS’s both lake water
sample and CaCO3 suspension.
2. When applying the GFFs into the vacuum filter and wetting them, we should do
gently since GFFs can be torn out which would allow some particles go through the
filter and the obtained mass would be lower than expected. As for the GFF number
2 of lake sample, which illustrated the filter I used in the experiment had been torn
out a little bit, showed the TSS with only 124mg/L which was far less than over
500mg/L from the rest of 2 figures of TSS’s lake sample.
3. The GFF number 6 with TSS only 186 mg/L of CaCO3 had been conducted
unsuccessfully since when I did pipette, I noticed I did let the CaCO3 suspension free
fall to the filter in which some of particles were out of the filter’s centre and let
some particles go all the way down to flask. That’s why the figure was less than the
rest which were over 225 mg/L.

Reference:
1. CHEM25770 Analytical Chemistry 1 Laboratory Manual, Sheridan College,
Brampton, ON. Fall 2019, pp 3-12.

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 Laboratory 1: Determination of Total Suspended Solids and Determination of
Method
Detection Limit
Raw Data

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Method
Detection Limit

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Method
Detection Limit

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 Laboratory 1: Determination of Total Suspended Solids and Determination of
Method
Detection Limit

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