Analytical Chemistry Laboratory Report 1 PDF

Preview

Summary

Analytical Laboratory Report...

Description

ANALYTICAL CHEMISTRY LABORATORY REPORT SHEET

Laboratory Title: Determination of Total Suspended Solids and Determination of Method Detection Limit Partner A or B: B

Name: Thinh Vo 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) Standard deviation % Relative Standard Deviation (% RSD)

400 mg/L 240.2 mg/L 60%

Sample: CaCO3 Suspension Result (mean) Standard deviation

262 mg/L 37.92 mg/L

% Relative Standard Deviation (% RSD)

14%

1 Thinh Vo - 991519197

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

i Thinh Vo - 991519197

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 1 (Lake Sample) 2 (Lake Sample ) 3 (Lake Sample ) 4 (CaCO3) 5(CaCO3) 6(CaCO3) 7(CaCO3) 8(CaCO3) 9(CaCO3) 10(CaCO3) 11(CaCO3)

Mass of GFF (g) 0.2143 0.2129 0.2188 0.2144 0.2137 0.2157 0.2141 0.2142 0.2150 0.2114 0.2143

Mass of GFFF + residue 0.2400 0.2191 0.2469 0.2290 0.2268 0.2250 0.2287 0.2276 0.2289 0.2227 0.2289

Calculations: 1. Lake Water Sample Total Suspended Solids (TSS): TSS(mg/L) =

( A−B ) x 1000

mL L

V 1st sample of lake water: mL ( A−B ) x 1000 L TSS(mg/L) = V 

TSS(mg/L) =



1000 mg mL x 1000 mg L 1g =514 L 50 .00 ml

( 0.2400 g−0.2143 g ) x 1 g x

2nd sample of lake water:

1 Thinh Vo- 991519197

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



Standard Deviation (S) of lake sample: Mean ´x =

514 +124 + 562 =400 3

Table 2: Calculating Standard Deviation Table of Lake Sample

xi

´x

514 124 562

400 400 400

TSS

1 2 3 x xi−¿´ ¿ ¿2 ¿ ¿ N

∑¿ i =1

x xi−¿´ ¿ ¿2 ¿ S= ¿ N

∑¿

=

√

115416 =240.2 mg/L 2

i =1

¿

√¿

 Standard deviation of lake sample is 240.2 mg/L Percent relative standard deviation: 100 x S 240.2 x 100 =60 % =  %RSD = 400 ´x 2. CaCO3 Suspension: Total Suspended Solids (TSS): TSS(mg/L) =

( A−B ) x 1000 V



4th sample of CaCO3:

2 Thinh Vo- 991519197

mL L

x xi−¿´ ¿ ¿ ¿ 12996 76176 26244

Laboratory 1: Determination of Total Suspended Solids and Determination of Method Detection Limit TSS(mg/L) =

( A−B ) x 1000

mL L

V TSS(mg/L) =       

1000 mg mL x 1000 mg L 1g =292 L 50.00 ml

( 0.2290 g−0.2144 g) x 1 g x

5th sample of CaCO3: mg TSS(mg/L) = 262 L th 6 sample of CaCO3: mg TSS(mg/L) = 186 L th 7 sample of CaCO3: mg TSS(mg/L) = 292 L th 8 sample of CaCO3: mg TSS(mg/L) =268 L th 9 sample of CaCO3 mg TSS(mg/L) = 278 L th 10 sample of CaCO3 mg TSS(mg/L) = 226 L th 11 sample of CaCO3 mg TSS(mg/L) = 292 L

Standard Deviation (S) of CaCO3 : Mean ´x

=

292 + 262 + 186 + 292+ 26 8+ 278 +2 26+ 292 =26 2 mg/L 8

Table 3: Calculating Standard Deviation Table of CaCO3 Suspension

TSS

xi

´x

4 5 6 7 8 9 10 11

292 262 186 292 268 278 226 292

262 262 262 262 262 262 262 262

3 Thinh Vo- 991519197

x xi− ´¿ ¿ ¿ ¿ 900 0 5776 900 36 256 1296 900

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

∑¿ i =1

x xi− ¿´ ¿ 2 ¿ ¿  S= = ¿ N

∑¿

√

100 6 4 =3 7 . 92 mg/L 7

i =1

¿

√¿

Percent relative standard deviation: 100 x S 3 7 . 92 x 100 %=14 % = %RSD = 261.25 ´x  MDL: Table 4: Values for calculating MDL

-

-

Values (mg/L) Mean = 292 262 186 292 268 278 226 292 mg 292 + 262 + 186 + 292 +2 68 + 2 78 +2 26+ 292 =2 6 2 L 8 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

TSS values for 4 Thinh Vo- 991519197

Mean( mg/L)

Standard

Percent relative

Laboratory 1: Determination of Total Suspended Solids and Determination of Method Detection Limit lake samples (mg/L)

GFF number 1: 514 GFF number 2: 124 GFF number 3: 562

deviation of lake samples(mg/L ) 240.2

400

standard deviation (%)

60

Table 6: Summary of CaCO3 Suspension

TSS values of CaCO3 suspension(mg/L ) GFF number 4: 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

Mean( mg/L)

262

Standard deviation of lake samples(mg/L) 3 7 . 92

Percent relative standard deviation (%) 14

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 5 Thinh Vo- 991519197

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.

6 Thinh Vo- 991519197

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

Raw Data

7 Thinh Vo- 991519197

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

8 Thinh Vo- 991519197

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

9 Thinh Vo- 991519197

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

10 Thinh Vo- 991519197...