Q1.

a) Qualitative Analysis

What is in the sample. Tell the identity of analytes.

b) Quantitative Analysis
The amount or concentration of analytes in the sample.

c) Sensitivity
The per unit analyte detector responds, i,e slope of the calibration curve.

d) Detection Limit
Smallest amount (concentration) of analytes that generate a detector response significantly different from
that of a blank.

e) Selectivity
The ability of the analysis to differentiate/distinguish the analytes from other chemical species co-exist in
the sample

f) Accuracy
A measure of how close the measured result is to the true amount/concentration

g) Precision
Reproducibility of the result from multiple/replicated measurement

h) Robust
Results unaffected by small changes in experimental conditions

i) Calibration Check
It is by analyzing a standard solution of known conc./formulation regularly to make sure our in

j) Quality Control Sample

Sample of known composition parallel to the analyte as unknown. It is used to check and eliminate bias
introduced by the experiment operator.

k) Recovery
Percentage of analyte recovered/extracted from the sample to the solution for analysis after accounting for
analyte instability/decomposition and recovery loss during the sample preparation.

l) Reagent Blank
A sample containing all components except analyte but not subject to sample preparation procedures.

m) Field Blank
A sample containing all components except analyte, including the sample preparation and exposed to the
site of sampling.
Q2.

a) Mean and Standard Deviation of the Protein Sample Signals

Given Signals:
0.0054, 0.0062, 0.0060, 0.0046, 0.0056, 0.0052, 0.0044

Mean Calculation:
0.0054+0.0062+0.0060+0.0046+0.0056+0.0052+0.00447
Mean= = 0.00534
7

Standard Deviation Calculation:

Apply the formula for standard deviation:

∑(𝑥𝑖 − 𝑚𝑒𝑎𝑛)2
𝑆=
𝑛−1
Calculating each squared deviation:
(0.0054−0.00534)2 = 0.0000000036

(0.0062−0.00534)2 = 0.0000007396

(0.0060−0.00534)2 = 0.0000004356

(0.0046−0.00534)2 = 0.0000005476

(0.0056−0.00534)2 = 0.0000000676

(0.0052−0.00534)2 = 0.0000000196
(0.0044−0.00534)2 = 0.0000008836

Sum the squared deviations:

𝑆 = 0.0000000036 + 0.0000007396 + 0.0000004356 + 0.0000005476 + 0.0000000676

+ 0.0000000196 + 0.0000008836 = 0.0000026964

Standard deviation:

0.00000269646
𝑠=√ ≈ 0.000670
6

• Mean: 0.00534

• Standard Deviation: 0.000670

b) Absolute Uncertainty, Relative Uncertainty, and % Relative Uncertainty

Absolute Uncertainty: This is typically taken as the standard deviation.

Absolute Uncertainty=s=0.000670
Relative Uncertainty:
𝑠 0.000670
Relative Uncertainty = 𝑚𝑒𝑎𝑛 = ≈ 0.1255
0.00534

Percentage Relative Uncertainty:

Percentage Relative Uncertainty=Relative Uncertainty×100=0.1255×100≈12.55

• Absolute Uncertainty: 0.000670

• Relative Uncertainty: 0.1255

• % Relative Uncertainty: 12.55%

c) Signal Detection Limit

To find the signal detection limit, we can use the standard deviation of the blanks.

Given Blanks:
0.0006, 0.0012, 0.0022, 0.0005, 0.0008, 0.0011, 0.0010

Mean of Blanks:
0.0006 + 0.0012 + 0.0022 + 0.0005 + 0.0008 + 0.0011 + 0.00107
𝑀𝑒𝑎𝑛𝑏𝑙𝑎𝑛𝑘𝑠 = ≈ 0.001057
7
Standard Deviation of Blanks:
𝑠=
(0.0006−0.001057)2 +(0.0012−0.001057)2 +(0.0022−0.001057)2 +(0.0005−0.001057)2 +(0.0008−0.001057)2 +(0.0011−0.001057)2 +(0.00107−0.001057)2
√ =
6

0.000565.
Detection Limit:
The detection limit is often calculated as:

Detection Limit=Meanblanks+3×sblanks= 0.001057+3×0.000565 ≈ 0.00275

• Signal Detection Limit: 0.00275

d) Minimum Detection Concentration and Lower Limit of Quantitation

Slope of Calibration Curve: m=2.20×104M−1

Minimum Detection Concentration:

Using the detection limit:
3𝑠 3 ⋅ 0.00275
𝐶𝑚𝑖𝑛 = = 4
= 7.708 × 10−8 𝑀
𝑚 2.2 × 10
Lower Limit of Quantitation (LOQ): Typically defined as 10 times the standard deviation/mean:
10𝑠 10 ⋅ 0.00275
𝐿𝑂𝑄 = = = 2.569 × 10−7 𝑀
𝑚 2.2 × 104
 e) Concentration of the Protein in the Sample

Using the mean signal from the protein sample:

𝑀𝑒𝑎𝑛 𝑠𝑖𝑔𝑛𝑎𝑙 − 𝑁𝑜𝑖𝑠𝑒 0.00534
𝐶= = ≈ 1.95 × 10−7 𝑀
𝑚 2.20 × 104
Q3.

a) Blank Titration

A titration performed without the analyte of interest, but with all other elements. It is used to correct the
difference between the end point and equivalent point.

b) Back Titration
A known excess amount of a standard reagent is added to react with analytes in the solution. The excess
amount of the standard reagent is determined by another(back) titration. From the difference in amount
of the reagent added and that consumed in the back titration, the amount of reagent consumed by
reactivity with the analyte can be determined.

Q4.

a) Weight Percentages of Carbon and Hydrogen

The moles of CO2 and H2O produced:

o Molar mass of CO2=12.01+(2×16.00)=44.01 g/mol

o The molar mass of H2O (H: 1.01 g/mol, O: 16.00 g/mol) = 2×1.01+16.00=18.02 g/mol

The number of moles of CO2 produced:

16.43 𝑚𝑔
𝑀𝑜𝑙𝑒𝑠 𝑜𝑓 𝐶𝑂2 = ≈ 0.000373 𝑚𝑜𝑙
44.01 𝑔/𝑚𝑜𝑙

The number of moles of H2O produced:

2.84 𝑚𝑔
𝑀𝑜𝑙𝑒𝑠 𝑜𝑓 𝐻2𝑂 = ≈ 0.000157 𝑚𝑜𝑙
18.02 𝑔/𝑚𝑜𝑙
The mass of Carbon and Hydrogen in the original compound:
12.01 𝑔
𝑀𝑎𝑠𝑠 𝑜𝑓 𝐶𝑎𝑟𝑏𝑜𝑛 = 𝑀𝑜𝑙𝑒𝑠 𝑜𝑓 𝐶𝑂2 × 𝑀𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑜𝑓 𝐶 = 0.000373 𝑚𝑜𝑙 ×
𝑚𝑜𝑙
≈ 0.00448

𝑀𝑎𝑠𝑠 𝑜𝑓 𝐻𝑦𝑑𝑟𝑜𝑔𝑒𝑛 = 2 × 𝑀𝑜𝑙𝑒𝑠 𝑜𝑓 𝐻2𝑂 × 𝑀𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑜𝑓 𝐻

= 2 × 0.000157 𝑚𝑜𝑙 × 1.01 𝑔/𝑚𝑜𝑙 ≈ 0.000316 𝑔

Weight percentages:

𝑊𝑒𝑖𝑔ℎ𝑡 % 𝐶𝑎𝑟𝑏𝑜𝑛 = (4.48 𝑚𝑔8.73 𝑚𝑔) × 100 ≈ 51.3

𝑊𝑒𝑖𝑔ℎ𝑡 % 𝐻𝑦𝑑𝑟𝑜𝑔𝑒𝑛 = (0.316 𝑚𝑔8.73 𝑚𝑔) × 100 ≈ 3.62

 • Weight % Carbon: 51.3% 51.36

• Weight % Hydrogen: 3.62% 3.639

b) Smallest Reasonable Integer Mole Ratio of C:H

Convert masses to moles:

o Moles of Carbon ≈0.000373 mol

o Moles of Hydrogen ≈ 0.000313 mol

0.000373
𝑇ℎ𝑒 𝑚𝑜𝑙𝑒 𝑟𝑎𝑡𝑖𝑜 = ≈ 1.19 ≈ 1.20 = 6: 5
0.000313
• Smallest Reasonable Integer Mole Ratio of C:H: 6:5, 13:11
Q5.

Amount of Carbon from CO2

Given Data:
Volume of seawater = 6.23 mL

Mass of CO2 produced = 2.38 mg

Molar Mass of CO2:

Molar mass of CO2 = 12.01 (C) + 2 × 16.00 (O) = 44.01 g/mol

Moles of CO2 Produced:

2.38 𝑚𝑔
𝑀𝑜𝑙𝑒𝑠 𝑜𝑓 𝐶𝑂2 = = ≈ 0.0000540 𝑚𝑜𝑙
44.01 𝑔/𝑚𝑜𝑙

Moles of Carbon:
Since each mole of CO2 corresponds to one mole of carbon: Moles of C = 0.0000540 mol

Mass of Carbon:
Mass of C=Moles of C×Molar mass of C=0.0000540 mol×12.01 g/mol≈0.000649 g

Concentration of Carbon in mg/L:

Since 1 L = 1000 mL, the concentration in mg/L is calculated as follows:

0.649 𝑚𝑔
𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 (𝑚𝑔/𝐿) = × 1000 𝑚𝐿/𝐿 ≈ 104.2 𝑚𝑔/𝐿
6.23 𝑚𝐿

Convert to ppm:
Since 1 mg/L = 1 ppm in water:

𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 (𝑝𝑝𝑚) = 104.2 𝑝𝑝𝑚

 Convert to µg/L:

𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 (µ𝑔/𝐿) = 104.2 𝑚𝑔/𝐿 × 1000 µ𝑔/𝑚𝑔 = 104,200 µ𝑔/𝐿

Convert to g/L:
104.2 𝑔/𝐿
𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 (𝑔/𝐿) = = 0.1042 𝑔/𝐿
1000
Volume in Liters:

𝑉𝑜𝑙𝑢𝑚𝑒 (𝐿) = 0.00623 𝐿

Molar Concentration of Carbon:

0.0000540 𝑚𝑜𝑙
𝑀𝑜𝑙𝑎𝑟 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 (𝑚𝑜𝑙/𝐿) = ≈ 0.00866 𝑚𝑜𝑙/𝐿
0.00623 𝐿
• Concentration of Carbon:
o ppm: 104.2 ppm

o µg/L: 104,200 µg/L

o g/L: 0.1042 g/L

• Molar Concentration: 0.00866 mol/L

Q6: All no need to be dry before use:

a) Volumetric Flask

Water/solvent will be added to make the solution eventually.

b) Conical Flask
Water/solvent there will not affect the number of moles of the analyte in the conical flask.

Pipette and Buret

Will be rinsed with the analyte solution before use anyway.

Q7:

Qualitative Analysis

Analyte standard added increases signal with very similar detection response, eg, retention time, as that
of analyte in the sample analysis (original), giving evidence that the signal was originated from the target
analyte.

Standard addition is primarily a quantitative technique. While it doesn't directly identify unknown
substances (qualitative analysis), it can be used in conjunction with qualitative techniques. For
example, if you suspect a particular analyte is present, you could use standard addition to confirm
its presence and determine its quantity. A positive response (increase in signal proportional to the
added standard) would provide further evidence for the presence of the suspected analyte.

Quantitative Analysis
 Known amount of analyte added to the sample containing analyte (at the concentration to be determined),
the amount of signal increase (in the presence of very similar matrix effect) was used to estimate the
amount of analyte in the original sample by correlating the signal in the original sample analysis.

Standard addition is a powerful tool in quantitative analysis because it directly addresses matrix
effects. By adding the standard directly to the sample matrix, the calibration occurs within the
matrix itself, effectively compensating for any interferences. This leads to a more accurate
determination of the analyte concentration.

Q8

Blind sample:
A blind sample is a sample of known concentration given to the analyst who performs the tests as an
unknown value. It is a QC measure to help eliminate bias introduced by the analyst who knows
concentration or composition of the calibration check.

A blind sample is a sample of known concentration (determined independently or by another lab) that's
presented to the analyst as if it were an unknown. The analyst is unaware of the true concentration.

How it helps in quality assessment: Blind samples assess the accuracy and precision of an
analytical method and the proficiency of the analyst. By comparing the analyst's determined
concentration to the known true value, you can evaluate:

Accuracy: How close the measured value is to the true value. A large difference indicates
systematic errors in the method or analyst technique.

Precision: How reproducible the results are. If multiple blind samples are analyzed, the
consistency of the results reflects the method's precision.

Certified Reference Material

A certified reference sample is a sample of known composition, with known/certified analyte

concentration, in the same sample matrix being tested. It is used to demonstrate that a method is fit for its
intended purpose by showing that it can accurately measure the analyte in a relevant matrix.
A CRM is a "matrix-matched" sample with a certified value for one or more analytes. "Matrix-matched"
means the CRM has a similar composition to the samples routinely analyzed in the lab (e.g., soil, blood
serum, steel). The certified values are determined by multiple highly accurate analytical techniques in
different laboratories.

How it helps in quality assessment: CRMs are crucial for:

Method Validation: CRMs are used to demonstrate that a method is fit for its intended purpose by
showing that it can accurately measure the analyte in a relevant matrix.

Instrument Calibration/Verification: CRMs can be used to calibrate instruments or verify the

accuracy of existing calibrations.

Quality Control: Regular analysis of CRMs helps monitor the ongoing performance of a method
and identify any drifts or biases that may develop over time.
 Proficiency Testing: Laboratories often participate in proficiency testing programs where they
analyze CRMs and compare their results to other labs, ensuring comparability and high standards.

Fortification Recovery Test

A fortification recovery test is adding known concentration of analyte to a sample (blank, eg). The amount
found after all experiment steps is calculated as a test of method recovery.

In a fortification recovery test, a known amount of the analyte (the "spike") is added to a sample, and the
sample is then analyzed using the chosen method. The percentage of the added analyte that is recovered
is calculated.

How it helps in quality assessment: This test assesses the method's ability to accurately measure the
analyte in the presence of the sample matrix. It helps to evaluate:

Matrix Effects: A low recovery percentage suggests that the sample matrix is interfering with the
analysis, either by suppressing or enhancing the signal. This helps identify potential issues and
optimize the method to minimize matrix effects.
Method Accuracy and Precision: Consistent and high recovery percentages (ideally close to
100%) indicate that the method is accurate and precise in the specific sample matrix.

Linearity: Performing spike recovery tests at different concentration levels helps assess the
linearity of the method over the desired analytical range.