Spectroscopy and Analytical Chemistry (CHM2922) - Lab Reports
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This document provides lab reports for the Spectroscopy and Analytical Chemistry course (CHM2922) at Monash University, Malaysia Campus. It includes information on the experiment, instrument used, procedures, results, and calculations. Download now!
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Spectroscopy and Analytical Chemistry (CHM2922) - Lab Reports Chemistry Monash University, Malaysia Campus 65 pag.
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Spectroscopy and Analytical Chemistry (CHM2922) – Lab Reports
Intentional plagiarism or collusion amounts to cheating under Monash UniversityStatute 4.1 –Student Discipline. Plagiarism:Plagiarismmeanstotakeanduseanotherperson’sideasandormannerofexpressingthemandt opasstheseofas one’s own by failing to give appropriate acknowledgement, including the use of material from any source, staf, students ortheinternet, published and unpublishedworks. Collusion: Collusion means unauthorised collaboration on assessable written, oral or practical work with another person. Where there are reasonable grounds for believing that intentional plagiarism or collusion has occurred, this will be reported to the Associate Dean (Education) or nominee, who may disallow the work concerned by prohibiting assessment or refer the matter to the Faculty Discipline Panel for a SCHOOL OF SCIENCE ASSESSMENT COVER SHEET Student’s name(Surname) Amran(Given names) Nuramira Batrisyia ID number27467236Phone Unit nameSpectroscopy and Analytical Chemistry Unit codeCHM2922 t Note: If this is a group assignment, please include the names of all other group members. Title of assignment Experiment 1: Gas Chromatography - Measuring the Alcohol Content of Wine Lecturer/tutorAssoc Prof Dr Lim Yau Yan Is this an authorisedgroup assignment?YesNo Has any part of this assignment been previously submitted as part ofanotherunit/course?YesNo Tutorial/laboratory day & time Tuesday, 2PM Due dateTuesday, 2PMDate submittedT u e s d a y All work must be submitted by the due date. If an extension of work is granted this must be specifed with the signature of the lecturer/tutor. Extension granted until(date)................................Signature of lecturer/tutor................................................. Please note that it is your responsibility to retain copies of your assessments. Student Statement: I have read the university’s Student Academic IntegrityPolicyandProcedures. I understand the consequences of engaging in plagiarism and collusion as described
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RISK ASSESSMENT Name: Nuramira Amran Lab Course details (e.g. CHM 2922) CHM2922Date5/8/2020 Experiment name and number Experiment 1: Gas Chromatography – Measuring the Alcohol Content ofWine Identify the HAZARD (the POTENTIAL to do harm) Determine the RISK (the PROBABILITY that harm mayresult) CONTROL the Risk (PREVENTING an incident) Absolute ethanolHighly flammable. Causes eye irritation. Handle in fumehood. Wear protective gloves and goggles Acetone Highly flammable. Causes eye irritation. May cause drowsiness or dizziness. Handle in fumehood. Wear protective gloves and goggles. GlasswareCuts, stab wound from sharp edges Handle with care, dispose of broken glass using a dustpan & brush. If cut, see demonstrator.
CHM2922Laboratory ReportName:NuramiraAmran EXPERIMENT1: GASCHROMATOGRAPHY–MEASURING THEALCOHOLCONTENT OFWINE AIM: Todeterminethecontentofwinebygaschromatographyusingtwomethodsofquantif cation: by the calibration and internal standardmethods. To determine the chromatographic elution parameters: capacity factor andresolution. DETAILS OF INSTRUMENT USED AND WHY IT IS SELECTED FOR THIS EXPERIMENT: According to Staufer et al. (2008), gas-liquid chromatography is defned as “a specifc type of chromatography that utilizes an inert gaseous mobile phase and a liquid stationary phase”. The instrument would separate mixtures and determine the amount of each component. It is selected for this experiment because it could separate volatile samples such as acetone and ethanol which could easily vaporise. EXPERIMENTALSECTION: (Briefly summarise the procedures < 150 words) The calibration starts with the preparation of standard solutions of ethanol in water with concentrations of 5, 10, 15 and 20 % (v/v) ethanol. The peak areas for ethanol peaks were measured and recorded. The internal standard method starts with the preparation of an acetone standard,which contains 15 % (v/v) of ethanol and acetone. For each wine sample a specifc amount of the acetone standardwasaddedtomake15%(v/ v)anddilutedtothemarkwiththesample.Thesesampleswould be called acetone-spiked samples.Next,1μLinjectionsof15%(v/v)ethanol-15%(v/v)acetone standardandoftheacetone- spikedwinesamplesweremade.Todeterminetheaccuracy,theQCwas provided, with 15 % (v/v) ethanol and 15 % (v/v) acetone. The results obtained from the QC was 4.1
/ tR(acetone) = 1.398 mins t’R(acetone) = 1.238 mins k’ (acetone) = 7.7375 w (ethanol) = 0.1 mins w (acetone) = 0.1 mins R = 4.91 1 of 8
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/ / Ethanol Concentration % (v/v) 2520051015 y = 743.41x - 142.45 R² = 0.9996 16000 14000 12000 10000 8000 6000 4000 2000 0 Calibration Graph of Peak Area vs Diferent Concentration of Ethanol Standard Solution Table 2: Calibration data Ethanol concentrat ion %(v/v) Peak area 1 Peak area 2 Peak area 3 Mean area Standa rd deviati on % RSD 53374.063586.6214504.39354115 0 4. 2 107339.717408.6611224.34727717 3 2. 4 1511426.410766.457081.151113933 8 3. 0 2014492.6214935.073663.251464425 2 1. 7 Calibration Graph Figure1:Calibrationgraphofpeakareasvsethanolindiferentconcentration,5%,10 %,15% and 20% Peak Area 6.1
/ Table 3: Calibration method results Wine Sample run number Peak area (Ethanol)Calculated Ethanol Concentration - % (v/v) 18167.8511.179 28065.7811.041 38095.5711.081 Average concentration - %(v/v) 11.1 Standard deviation0.0706 04 Relative standard deviation (%) 0.6360 5 Table 4: Internal standard method (acetone spiked) results Internal standard number Peak area (Acetone) Peak area (Ethanol) 12470524999 22481925131 32461625131 Average area24713.33101.75 Standard Deviation 2508776.21
/ Average concentrati on (% v/v) 10.838 Standard deviation 0.0731 75 Dilution factor1.18 Ethanol concentration in wine - corrected for dilution (% v/ v) 12.788 Relative standard deviation (%) 0.6752 CALCULATIONS Table 1: Peak Elution Data t’R(ethanol)= tR–tM = 1.889 – 0.16 = 1.729 mins k’ (ethanol)= t’R/ tM= 1.729 / 0.16 = 10.81 mins R =2 (tR(ethanol) – tR(acetone)) / (w (ethanol) + w (acetone)) = 2 (1.889 – 1.398) / (0.1 + 0.1) = 4.91 mins Table 2: Calibration Data For 5% ethanol concentration: Average peak area = (3374.06 + 3586.62 + 3663.25) / 3 = 3541 Standard Deviation = √ ((3374.06 – 3541)2+ (3586.62 – 3541)2+ (3663.25 –
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Peak Area = 8167.85 From the equation obtained by calibration graph: y = 743.41x – 142.45 Ethanol Concentration % (v/v)= (8167.85 + 142.45) / 743.41 = 11.179 % (v/v)
/5 Table 4: Internal Standard Method (acetone spiked) Results Spiked Wine Sample 1: Peak Area (acetone), (ethanol): 24800, 18008 Peak Area (internal, acetone), (internal, ethanol): 24705, 24999 )((((((((((((((( ����(ℎ(ℎ(ℎ(ℎ(ℎ(ℎ(ℎ(ℎ(ℎ(ℎ(ℎ(ℎ(ℎ(ℎ(ℎ ) Concentrationofethanol%(v/ v)=��������(,(,(,(,(,(,(,(,(,(,(,(,(,(,(, ) ���� ����)(,ℎ(,ℎ(,ℎ(,ℎ(,ℎ(,ℎ(,ℎ(,ℎ(,ℎ(,ℎ(,ℎ(,ℎ(,ℎ(,ℎ(,ℎ 2480 0 18008 2470 5 2499 9 x 15= 12.701 % (v/v) Dilution Factor =10 mL of the fnal sample / 8.5 mL of the wine sample = 1.18 Ethanol concentration in wine – corrected for dilution % (v/v) =12.701 x 1.18 = 12.788 % (v/v) DISCUSSION ANDCONCLUSIONS: There are two objectivesto thisexperiment. There are, to determine the content of wine by gas chromatography using two methods of quantifcation, which is by the calibration and internal standard methods; and to determine thechromatographicelutionparameters,suchascapacity factorandresolution.Fromtable1,theretentiontimeofthesolutes,tR,ofethanolwas1.72 9minswhiletheretention time for acetone was 1.238 mins. According to Bushra (2018), retention time is defned as the “time that a solute spends in a column x =
AccordingtoBushra(2018),theretention factorisdefnedas“theratiooftimespentbythesoluteinthestationaryandmobilephase”.A higher value of retention factor would indicate that the solute is much more polar that the other. The resolution (R), is a parameter that is used to measure the degree of peak separation. From table 1, it was determined that the resolution was 4.91.
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Based on the data in table 2, a calibration graph of peak areas against ethanol in diferent concentrations, 5%, 10%, 15% and 20%, was plotted. From the equationthatwasobtainedfromthe calibrationgraph,theconcentrationofethanolwasdetermined.Theaverageconcentra tionofethanol inallthreesamplesofwinewas11.179%(v/v).Thisconcentrationofethanolwasobtaine dfromthe calibration technique. The results that were obtained from the internal standard method is shown in table, whereby the average concentration of ethanol was 12.788 % (v/v), after multiplying with the dilution factor. The diference in the two concentration of ethanol is not big, rather it is a slight diference. The precision of both results that were obtained from the two quantifcation techniques can be determined using the %RSD. The %RSD of the ethanol concentration, 5%, 10%, 15% and 20%, in table 2 were 4.2%, 2.4%, 3.0% and 1.7%,respectively.Sincethe%RSDthatwerecalculatedforthe concentrations were lower than 5%, it would mean that the values are precise. The %RSD for the ethanol concentration determined in the wine samples for the calibration method was 0.63605%, which is lower than 5%, making it precise. The %RSD for the ethanol concentration that was determined using the internal standard method was 0.6752. Since the %RSD for the ethanol concentration determined using calibration method is lower, it would mean that the method is much more precise that the other. Inconclusion,thetwoobjectivesoftheexperimentwereachieved.Theconcentrationof ethanolwasdeterminedusingtwoquantifcationmethods,calibrationand internalstandard.Throughcalibration method,theconcentrationofethanolwasdeterminedtobe11.179%(v/v)whiletheconc entrationof ethanol that was obtained through the internal standard method, was
1Whatefectwouldincreasingtheoventemperaturehavehadontheretentiontimeof ethanoland acetone? (4marks) The retention time would decrease when the oven temperature increases. This isbecausethehigh temperaturewouldexcitethesamplemoleculesanditwouldresultinthemoleculestovapori zefaster. Hence, it would separate faster, but it could lead to poor separation since the components would mainly be in the gas phase, decreasing the accuracy of the result (Zuo, Yang, Huang and Xia,2013).
/ 2Suggest why a column with a BP20 stationary phase was specifed for this analysis? (4 marks) ThecolumnwithaBP20stationaryphaseismadefrompolyethyleneglycolanditiscomm onlyused as a polar stationary phase. This experiment separates ethanol and acetone, and because ethanol is a higher polar component, it would be elutedlast. 3Are the acetone and ethanol peaks sufciently resolved to enable the proper use of theinternalstandardmethod? (3marks) The resolution that was calculated was 4.91 which is higher than the baseline resolution, which is at 1.5. This would indicate that the ethanol and acetone peaks are sufciently resolved to enable the proper use of the internal standard method. 4There have been cases where wine has been mistakenly adulterated with ethyleneglycol(1,2-ethanediol,bp760197.6˚C).Asaforensicchemist, suggest how would you use GLC to proveconclusively that ethylene glycol was actually present? (4 marks) Thestandardsolutionofethyleneglycol1,2-ethanediolandwinethat containsethyleneglycol1,2-ethanediolthatarepreparedwouldbeinjectedinto theGLCanditsretentiontimeandpeakareasaremeasuredandrecorded.The retention time and peak areas are compared, and if the wine contains ethylene glycol 1,2-ethanediol, it would have the same retention time and peak area as the standard solution. 14.1 14.2
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/ REFERENCES: Bushra,R.,2018. FunctionalizedNanomaterialsfor Chromatography.In:C.Hussain, ed.,Nanomaterialsi n C h r o m a t o g r a p h y,1 s t e d . [ o n l i n e ] E l s e v i e r , p p . 4 0 3 - 4 1 4 . A v a i l a b l e a t : <https://www.sciencedirect.com/book/9780128127926/nanomaterials-in- chromatography#book-info> [Accessed 6 August 2020]. Staufer, E., Dolan, J. and Newman, R., 2008.Fire Debris Analysis. Boston, Mass.: Academic Press, pp.235-293. Zuo, H., Yang, F., Huang, W. and Xia, Z., 2013. Preparative Gas Chromatography and Its Applications.Journal of Chromatographic Science, [online] 51(7), pp.704-715. Available at: <https://academic.oup.com/chromsci/article/51/7/704/474245> [Accessed 7 August2020]. Total ReportMark/
Index of comments 4.1what about the unknown wine sample? 6.1error bars missing 12.1you can discuss accuracy by comparing with QC ethanol in calibration method, and you should discuss possible sources of errorfor each method, and you should discuss more on the merits of each method, give your opinions which method is more preferable? 14.1you should describe what kind of interaction of bonding is involved here 14.2you should also describe how to set up your GC to accommodate boiling point of ethylene glycol
SCHOOL OF SCIENCE ASSESSMENT COVER SHEET Student’s name(Surname)(Given names) ID numberPhone Unit nameUnit code t Note: If this is a group assignment, please include the names of all other group members. Title of assignment Lecturer/tutor Is this an authorised group assignment?YesNo Has any part of this assignment been previously submitted as part of another unit/course?YesNo Tutorial/laboratory day & time Due dateDate submitted All work must be submitted by the due date.If an extension of work is granted this must be specified with the signature of the lecturer/tutor. Extension granted until (date) ................................Signature of lecturer/tutor ................................................. Please note that it is your responsibility to retain copies of your assessments. Intentional plagiarism or collusion amounts to cheating under Monash UniversityStatute 4.1–Student Discipline. Plagiarism: Plagiarism means to take and use another person’s ideas and ormanner of expressing them and to pass these off as one’s own by failing to give appropriate acknowledgement, including the use of material from any source, staff, students or the internet, published and unpublished works. Collusion: Collusion means unauthorised collaboration on assessable written, oral or practical work with another person. Where there are reasonable grounds for believing that intentional plagiarism or collusion has occurred, this will be reported to the Associate Dean (Education) or nominee, who may disallow the work concerned by prohibiting assessment or refer the matter to the Faculty Discipline Panel for a hearing. Student Statement: I have read the university’sStudent Academic IntegrityPolicyandProcedures. I understand the consequences of engaging in plagiarism and collusion as described inUniversity Statute 4.1–Student Discipline, Part 2 Misconducthttp://adm.monash.edu/legal/legislation/statutes/statute4-1-student-discipline.pdf. I have taken proper care to safeguard this work and made all reasonable efforts to ensure it could not be copied. No part of this assignment has been previously submitted as part of another unit/course. I acknowledge and agree that the assessor of this assignment may for the purposes of assessment, reproduce the assignment and:
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RISK ASSESSMENT Name: Nuramira Amran Lab Course details (e.g. CHM 2922) CHM2922Date13/8/2020 Experiment name and numberExperiment 3:Measuring Iron in “Concrete Boots” using Atomic Absorption Spectrometry Identify the HAZARD (the POTENTIAL to do harm) Determine the RISK (the PROBABILITY that harm may result) CONTROL the Risk (PREVENTING an incident) Hydrochloric AcidCauses severe skin burns and eye damage. Toxin if inhaled. Handle in fumehood. Wear protective gloves and goggles Aluminium Stock SolutionCauses skin and serious eye irritation. Handle in fumehood. Wear protective gloves and goggles. Calcium Stock SolutionCauses skin and serious eye irritation. Handle in fumehood. Wear protective gloves and goggles. Iron Stock SolutionCauses skin and serious eye irritation. Handle in fumehood. Wear protective gloves and goggles. GlasswareCuts, stab wound from sharp edges Handle with care, dispose of broken glass using a dustpan & brush. If cut, see demonstrator.
CHM2922 Laboratory ReportName:Nuramira Amran ONLINEEXERCISE2: ANALYSIS OFIRON IN“CONCRETE BOOTS”BY ATOMICABSORPTION SPECTROMETRY Aim: •To learn the principles of atomic absorption spectroscopy •To determine the iron content of three cement samples and hence solve a murder case. /2 PRELABQUIZ: Q1:Write a brief account (150–200 words) of the general principles and uses of atomic absorption spectrometry for chemical analysis. The atomic absorption spectrometry (AAS) is a technique that is based on the process called atomic absorption. According to Sanz-Medel and Pereiro (2014), the process occurs when“ a ground-state electron of the analyte absorbs energy, in the form of light of a given frequency. From an external light source and so the electron is excited to an upper-energy-level state of the atom.”The technique is used when analysing copper in food and beverages (Barberá et al., 2003) and used in forensic science to determine the concentration or the presence of gunshot residueon a suspect’s hand(Salles et al., 2012). Q2: A series of five calibration standards 25, 50, 75 and 100 mg/L Fe is required to be made from a 1000mg/L Fe standard solution. If the final volume of the calibration standards is 100 mL, what is the required volume of the 1000 mg/L Fe standard solution? Show your calculation. M1= concentration of standard solution (mg/L) V1= volume of standard solution (mL) M2= concentration of iron solution required (mg/L) V2= volume of standard flask (mL) 25 mg/L calibration solution:M1V1= M2V2 3.1
Table 1: The concentration of calibration solutions required, and the volume of Fe standard solution added. Concentration (mg/L)Volume of the 1000 mg/L Fe standard solution (mL) 252.5 505.0 757.5 10010.0 Q3: Suggest a method to accurately make the above calibration standards Firstly, in order to make sure that the calibration standards were made accurately, the apparatus that is used must be clean and free from any contaminations. Secondly, an accurate amount of standard solution must be pipetted into the volumetric flasks and when adding water for dilution, it should not exceed the mark on the volumetric flask. Lastly, the absorbance readings should be done twice or three times to avoid any errors and ensure that the calibration curve that is plotted would be accurate. /10 /8 EXPERIMENTALSECTION: (brief description; < 150 words) Preparation of Calibration Solutions: A series of five calibration standards of Fe were prepared in 100 mL volumetric flasks. Extraction of Iron from cement by acid digestion 1.The cement sample was weighed onto a piece of filter paper, making sure that all the lumps had been crushed into fine powder. 2.The cement was then carefully poured into a large test tube and the paper was reweighed to determine the exact amount that was poured into the test tube. 3.Ten millilitre of 5.5 M hydrochloric acid was added to the test tube and agitated until the cement is dissolved.
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CHM2922 Laboratory ReportName:Nuramira Amran DISCUSSION ANDCONCLUSIONS: •Comment on the accuracy using both your solid QA and liquid QA. Comment on the reproducibility of your results: Accuracy refers to how close is the measured values that have been obtained during the experiment to the true value. To determine the accuracy the percentage relative error (%RE) was calculated using the QC standard data in both solid and liquid in Table 4. The lower the % RE, the more accurate the measured values are. The expected concentration that was given for liquid QC standard was 85 mg (Fe)/L while the solid QC standard was 18 mg (Fe)/g. Using the concentration that was calculated, the % RE for the QC standard in solid was 160.17 % while the QC standard in liquid is 1.412 %. The high percentage in relative error for QC standard solid could be due to errors that had occurred during the experiment, such as poor calibration of the AAS instrument. The high value would indicate that the measured values are inaccurate. Precision refers to how close are the measured values are to the values obtained when the procedure was triplicated. The precision is determined calculating the relative standard deviation (% RSD) of the samples. When the % RSD is low, this means that the measured values are precise. The percentage value that is acceptable and is still considered precise is 20 %. If the % RSD exceeds 20%, the measured value would be considered precise. The % RSD for the Australian Builders sample was 5.168 % while the % RSD for the Melcann Grey samples was 0.9589. The % RSD for the unknown sample was 9.885 % while the %RSD for the solid QC was 1.750 %. The %RSD for all the samples is below 20 %, meaning reproducibility is high. •Identify the most like sources of error in your experimental procedure: There are many errors that could have occurred during the experiment, which would alter the result. One of the most highly likely errors that could have happened was the cement samples getting stuck on the filter paper that was used to weigh the cement samples. This could have affected the final calculations of the concentration of iron in the sample. Another error that could have occurred, would
•What is the origin of the bright flame colour that is emitted when cement samples are aspirated into the AAS? The cement samples would be aspirated into the AAS through a nebulizer and then sprayed as an aerosol. The cement samples would be mixed with fuel and oxidant gases inside the chamber and then go to the burner head where combustion and atomization would occur. During atomization, ground state atoms, which are in gaseous state, are formed. These atoms would absorb the energy from the light source and become excited. This would make them go to a higher energy level and when they return, they would emit energy in a form of a specific wavelength of light, which would result in the flame having different colors (Viets and O'Leary, 1992). During this experiment, the flame colors that was observed for calcium, aluminium and iron were red-pink, orange and brownish orange, respectively. •How is it possible to measure theabsorbanceof iron in the AAS flame when there is also an emission process occurring? The presence of a rotating chopper would allow the measurement of iron in the AAS and the emission process occurring at the same time. It is found in between the lamp, which is the light source, and the atomizer, which is the flame. The chopper would rotate a half mirror, which, at one moment, would block the light coming from the light source and allowing only the light emitted from the flame to be read. At the next moment, the light emitted from the flame and from the light source would be read. The signal processor would then subtract emission from the flame from the emission from the flame and the light source (Sanz-Medel and Pereiro, 2014). •Can you identify the origin of the“concrete boots” cement from your results? According to the results obtained from the experiment, it could be determined that the cement from the “concrete boots” came from the MelcannGrey building. This is because the mean concentration of iron that came from Melcann Grey building, which was 0.963 %, was close to the mean concentration of iron of the unknown sample, which was 0.962 %. CONCLUSION 9.1 9.2
REFERENCE Barberá, R., Farré, R. and Lagarda, M., 2003. Copper: Properties and Determination. In: B. Caballero, ed.,Encyclopedia of Food Sciences and Nutrition, 2nd ed. [online] Academic Press, pp.1634-1639. Available at: <https://www.sciencedirect.com/science/article/pii/B012227055X002972> [Accessed 14 August 2020]. Salles, M., Naozuka, J. and Bertotti, M., 2012. A forensic study: Lead determination in gunshot residues.MicrochemicalJournal,[online]101,pp.49-53.Availableat: <https://www.sciencedirect.com/science/article/pii/S0026265X11001883>[Accessed14August 2020]. Sanz-Medel, A. and Pereiro, R., 2014.Atomic Absorption Spectrometry: An Introduction. 2nd ed. New York: Momentum Press, LLC, pp.23-24. Viets, J. and O'Leary, R., 1992. The role of atomic absorption spectrometry in geochemical exploration.JournalofGeochemicalExploration,[online]44(1-3),pp.107-138.Availableat: <https://www.sciencedirect.com/science/article/pii/037567429290049E>[Accessed15August 2020]. Total Report Mark/90
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Index of comments 3.1more details on general principles 9.1should mention how to separate emission and absorption wavelength 9.2SD should be referred as well
SCHOOL OF SCIENCE ASSESSMENT COVER SHEET Student’s name(Surname)(Given names) ID numberPhone Unit nameUnit code t Note: If this is a group assignment, please include the names of all other group members. Title of assignment Lecturer/tutor Is this an authorised group assignment?YesNo Has any part of this assignment been previously submitted as part of another unit/course?YesNo Tutorial/laboratory day & time Due dateDate submitted All work must be submitted by the due date.If an extension of work is granted this must be specified with the signature of the lecturer/tutor. Extension granted until (date) ................................Signature of lecturer/tutor ................................................. Please note that it is your responsibility to retain copies of your assessments. Intentional plagiarism or collusion amounts to cheating under Monash UniversityStatute 4.1–Student Discipline. Plagiarism: Plagiarism means to take and use another person’s ideas and ormanner of expressing them and to pass these off as one’s own by failing to give appropriate acknowledgement, including the use of material from any source, staff, students or the internet, published and unpublished works. Collusion: Collusion means unauthorised collaboration on assessable written, oral or practical work with another person. Where there are reasonable grounds for believing that intentional plagiarism or collusion has occurred, this will be reported to the Associate Dean (Education) or nominee, who may disallow the work concerned by prohibiting assessment or refer the matter to the Faculty Discipline Panel for a hearing. Student Statement: I have read the university’sStudent Academic IntegrityPolicyandProcedures. I understand the consequences of engaging in plagiarism and collusion as described inUniversity Statute 4.1–Student Discipline, Part 2 Misconducthttp://adm.monash.edu/legal/legislation/statutes/statute4-1-student-discipline.pdf. I have taken proper care to safeguard this work and made all reasonable efforts to ensure it could not be copied. No part of this assignment has been previously submitted as part of another unit/course. I acknowledge and agree that the assessor of this assignment may for the purposes of assessment, reproduce the assignment and:
RISK ASSESSMENT Name: Nuramira Amran Lab Course details (e.g. CHM 2922) CHM2922Date26/8/2020 Experiment name and numberExperiment 6: Detecting gunshot discharge residues using UV-Vis Spectrophotometry Identify the HAZARD (the POTENTIAL to do harm) Determine the RISK (the PROBABILITY that harm may result) CONTROL the Risk (PREVENTING an incident) Sodium NitrateCauses severe skin burns and eye damage. Handle in fumehood. Wear protective gloves and goggles Sodium NitriteCauses skin and serious eye irritation. Toxic if swallowed. Handle in fumehood. Wear protective gloves and goggles. N(1-naphthyl) ethylenediamine dihydrochloride Causes skin and serious eye irritation. Handle in fumehood. Wear protective gloves and goggles. SulphanilamideCauses serious skin and eye irritation. Harmful if inhaled Handle in fumehood. Wear protective gloves and goggles. Hydrochloric AcidCauses severe skin burns and eye damage. Toxic if inhaled. Handle in fumehood. Wear protective gloves and goggles. GlasswareCuts, stab wound from sharp edges Handle with care, dispose of broken glass using a dustpan & brush. If cut, see demonstrator.
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CHM2922 Laboratory ReportName:Nuramira Amran EXPERIMENT6: DETECTION OFGUNSHOTDISCHARGERESIDUES BYUV-VISSPECTROPHOTOMETRY AIM: •To apply a suitable sampling method for collecting gunshot discharge residue from the hands of a suspect. •To use spectrophotometry for the determination of nitrite in gunshot discharge or explosive residues. •To determine who fired the weapon! DETAILS OF INSTRUMENT USED AND WHY IT IS SELECTED FOR THIS EXPERIMENT: According to Pentassuglia et al. (2018), UV-Vis spectrophotometry “is a type of absorption spectroscopy in which UV-visible light is absorbed by the molecule, which would result in the excitation of the electrons from lower to higher energy levels.”It is the chosen instrument for this experiment because it is very versatile and has a high selectivitythat it could detect every molecule at a specific wavelength for a parameter. /5 EXPERIMENTALSECTION: (Describe briefly with about 150 words) 1.Prepare 100 μM nitrite standard solution by performing a serial dilution from the 10 mM NaNO2stock solution that was provided. From there, a set of five nitrite standards (0, 2.5, 5, 10 and 15 μM) was prepared. 2.Next, to prepare the Quality Control solution, add 1 mL of Diazotizing Reagent to each standard solution and the Quality Control solution. Next, wait 5 minutes and then add 1 mL of Coupling Reagent and then wait for another 10 minutes. 3.Next, add Diazotizing Reagent and Coupling Reagent to each diluted sample extract in the same order and same reaction times as the standards. Wait for 10 minutes and then measure 3.1 3.2
SUMMARY OFRESULTS ANDCALCULATIONS: Table 1: Calibration Data Concentration (μm) Abs 1Abs 2Abs 3Mean Abs Std Deviation% RSD 00.000.000.000.000.000.00 2.50.10210.1020.10280.10234.36 x 10-40.4261 50.22460.21860.21850.22063.493 x 10-31.584 100.42590.42430.42480.4258.19 x 10-40.1926 150.6720.66740.6550.66488.793 x 10-31.323 /5 Calibration Graph: Figure 1: Calibration graph of absorbance at 542 nm against the concentration of nitrite standards (μm) y = 0.0441x - 0.0043 R² = 0.9991 -0.2 -0.1 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 -505101520 Absorbance at 545 nm Concentration of nitrite standards (μm) Calibration graph of absorbance at 542 nm vs. concentration of nitrite standards (μm)
Sample calculations Table 1: Calibration Data For Concentration at 2.5 μm Mean Absorbance: (0.1021 + 0.102 + 0.1028) / 3 = 0.1023 Standard Deviation: = √ ((0.1021 –0.1023)2+ (0.102–0.1023)2+ (0.1028–0.1023)2) / 2 = 4.36 x 10-4 % RSD =(standard deviation / average) x 100 = (4.36 x 10-4/ 0.1023) x 100 = 0.4261% Table 2: Sample Data For Blank 1: Average Absorbance: (-0.0069 + -0.009 + -0.0099) / 3 = -0.0086 Concentration (μm) From the calibration curve: y = 0.0441x–0.0043 -0.0086 = 0.0441x–0.0043 x = (-0.0086 + 0.0043) / 0.0441 = -0.10 /5 5.1
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CHM2922 Laboratory ReportName:Nuramira Amran 4 of 8 Table 2: Sample data SampleAbs1Abs 2Abs 3Mean AbsConc (μM)Mean Conc (μM)Standard Deviation% RSD BLANK 1-0.0069-0.009-0.0099-0.0086-0.10 BLANK 2-0.0088-0.0093-0.0091-0.0091-0.11 BLANK 3-0.009-0.0094-0.0095-0.0093-0.11-0.1060.008082-7.601 QC Standard0.04020.03880.03870.03920.99 SUSPECT 1, LEFT A0.00880.00890.00960.00910.20 SUSPECT 1, LEFT B0.01160.00780.00660.00870.29 SUSPECT 1, LEFT C0.00460.00470.00440.00460.300.2660.0621 SUSPECT 1, RIGHT A-0.0102-0.0093-0.0098-0.0098-0.12 SUSPECT 1, RIGHT B-0.0102-0.01-0.0097-0.0100-0.13 SUSPECT 1, RIGHT C-0.0102-0.0093-0.0093-0.0098-0.12-0.1250.002618-2.087 SUSPECT 2, LEFT A-0.0095-0.0092-0.0091-0.0093-0.11 SUSPECT 2, LEFT B-0.0096-0.0098-0.0099-0.0098-0.12 SUSPECT 2, LEFT C-0.008-0.0087-0.0099-0.0089-0.10-0.1130.010225-9.019 SUSPECT 2, RIGHT A-0.0104-0.0103-0.0092-0.0100-0.13 SUSPECT 2, RIGHT B-0.0096-0.0101-0.0111-0.0103-0.14 SUSPECT 2, RIGHT C-0.0093-0.0095-0.0103-0.0097-0.12-0.1280.006428-4.993 /20 6.1 Document shared on https://www.docsity.com/en/spectroscopy-and-analytical-chemistry-chm2922-lab-reports/8957042/ Downloaded by: dongxiaoma666 (dongxiaoma666@gmail.com)
CHM2922 Laboratory ReportName:Nuramira Amran STATISTICALANALYSIS t-Test: Two-Sample Assuming Unequal Variances Suspect 1, LeftSuspect 2, Left Mean0.266-0.113 Variance0.004320.000208 Observations22 Hypothesized Mean Difference0 df1 t Stat7.59 P(T<=t) one-tail0.0417 t Critical one-tail6.31 P(T<=t) two-tail0.0834 t Critical two-tail12.7 t-Test: Two-Sample Assuming Unequal Variances Suspect 1, RightSuspect 2, Right Mean-0.125-0.128 Variance1.028 x 10-58.256 x 10-5 Observations22 Hypothesized Mean Difference0 df1 t Stat0.3882 P(T<=t) one-tail0.3821 t Critical one-tail6.314 P(T<=t) two-tail0.7642 t Critical two-tail12.71 Test between hands of the apparently guilty suspect t-Test: Two-Sample Assuming Unequal Variances “Guilty Suspect” Right Hand “Guilty Suspect” Left Hand Mean-0.1250.266 Variance1.03 x 10-50.004322 Observations22 7.1 7.2
CONCLUSIONS: Is there any statistically significant difference, at the 95% confidence level for left- and right- hand samples between suspects? The null hypothesis of the t-test is Ho: μ1-μ2= 0, which means that there is no difference between the mean concentrations of nitrite obtained from the two suspects hands while the alternative hypothesis is Ha: μ1-μ2≠0, which means that there is a difference between the mean concentration of nitrite obtained from the two suspects hands. The t-test for the left hand of the two suspects indicate that the t-statistics is 7.59 and p-value is 0.042, which is smaller than the α = 0.05. And hence, the null hypothesis is rejected, indicating that there is a difference between the mean concentration of nitrite from the two suspects hands at 5% level of significance. The t-test for the right hand of the two suspects determined that the t-statistics is 0.39 and the p-value is 0.38, which indicates that there is no difference between the mean concentrations of nitrite from the two suspects. This is because the p-value is larger than the α = 0.05, rejecting the alternative hypothesis. To conclude, at 95% confidence level, there is a statistical difference between the two mean concentrations of nitrite between the left hand of the two suspects but there is no statistical difference between the two mean between the right hands of the two suspects. Which, if any of your suspects should be charged?There should be statistical proof of guilt for a charge to be laid. Suspect 1 should be charged as guilty since the null hypothesis of the t-test for the left hands of the two suspects was rejected, indicating that there is difference between the mean concentrations of nitrite. Furthermore, the mean concentration of nitrite that was calculated using the regression equation that was obtained from the calibration graph also shows that suspect 1’s left hand has the highest amount of nitrite. /15 QUESTIONS 1.Brieflydescribetwocriteriayouusedinselectingtheoptimumwavelengthfor absorbance measurements? 8.1 8.2
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2.Comment on the accuracy of your results. Accuracy is defined as how close the obtained result is to the true result. It can be determined by calculating the %RSD, the lower the value is the more accurate the data that was obtained. For the calibration data, the %RSD for the concentrations, 0, 2.5, 5, 10 and 15, were 0.00%, 0.43%, 1.58%, 0.19% and 1.32% respectively. Since they are lower than 5%, it means that the data for the concentration of the nitrite standard is accurate and close to its true value. Since the calibration data is accurate, the concentration reading for the QC standard which is determined using the regression equation is accurate as well. The concentration reading for the QC standard was calculated to be 0.99 μM. 3.As a forensic scientist, you may be required to present and defend your results in court. Whatadditional(experimental) work could you undertake to ensure that a clever barrister could not demolish your evidence? Fingerprint analysis could be the additional work that would ensure that the clever barrister could not demolish the evidence. This is because according to Hildebrandt et al. (2017), “fingerprint trace is formed by human secretions left by a finger touching a surface”. This would mean it has a part of a person’s DNA and this would determine his/her identity. 4.Julian Cleverdrawers, SC, barrister for the defence, in cross examining you, says "You found nitrite on the defendant's right and left hands, and on those of a number of other suspects. I put it to you that your results are meaningless and cannot be used as evidence that my client fired the pistol". How would you defend the quality your data? According to the t-test that was performed, it was found that the mean concentration of nitrite was the highest on the suspect 1’s left hand. Furthermore, the t-test provided data to prove that the alternative hypothesis, which is that the mean concentration of nitrite between the left hands of the two suspects were different, was accepted. While the t-test that was performed for the right hands of the two suspects, proved that the mean concentrations of nitrite are no different from 9.1 9.2 9.3
REFERENCES: Hildebrandt, M., Dittmann, J. and Vielhauer, C., 2017. Capture and Analysis of Latent Marks. In: M. Tistarelli and C. Champod, ed.,Handbook of Biometrics for Forensic Science. [online] Springer, pp.19-35.Availableat:<https://link.springer.com/book/10.1007%2F978-3-319-50673-9#toc> [Accessed 29 August 2020]. Pentassuglia,S.,Agostino,V.andTommasi,T.,2018.EAB—ElectroactiveBiofilm:A Biotechnological Resource. In: K. Wandelt, ed.,Encyclopedia of Interfacial Chemistry. [online] Elsevier,pp.110-123.Availableat: <https://www.sciencedirect.com/science/article/pii/B9780124095472134614> [Accessed 27 August 2020]. /4 Total Report Mark/90 10.1
Index of comments 3.1more details about UV-vis mention wavelength 3.2past tense passive form 5.1your abs has to deduct from reagent blank to obtain the actual sample reading 6.1calculated conc is wrong as (problem as mentioned) 7.1Incorrect p values 7.25/5 8.10/5 p value mentioned here doesnt correspond to your t-test table your explanation is right but your reported value doesnt correspond to the value reported here 8.2Again, your answer is right but your p value showing p>0.05 8.31/5 -signal to noise ratio? 9.10/5 RE calculation is based on 5uM standard and its absorbance (0.2179) reading obtained from UV and calculated using your cal curve equation 9.22/5 -measure other components of gunshot residues (i.e. antimony) -measure nitrate using another method? 9.30/5 -more statistical components required -sampling population 10.12/4 at least 4 ref
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SCHOOL OF SCIENCE ASSESSMENT COVER SHEET Student’s name(Surname)(Given names) ID numberPhone Unit nameUnit code t Note: If this is a group assignment, please include the names of all other group members. Title of assignment Lecturer/tutor Is this an authorised group assignment?YesNo Has any part of this assignment been previously submitted as part of another unit/course?YesNo Tutorial/laboratory day & time Due dateDate submitted All work must be submitted by the due date.If an extension of work is granted this must be specified with the signature of the lecturer/tutor. Extension granted until (date) ................................Signature of lecturer/tutor ................................................. Please note that it is your responsibility to retain copies of your assessments. Intentional plagiarism or collusion amounts to cheating under Monash UniversityStatute 4.1–Student Discipline. Plagiarism: Plagiarism means to take and use another person’s ideas and ormanner of expressing them and to pass these off as one’s own by failing to give appropriate acknowledgement, including the use of material from any source, staff, students or the internet, published and unpublished works. Collusion: Collusion means unauthorised collaboration on assessable written, oral or practical work with another person. Where there are reasonable grounds for believing that intentional plagiarism or collusion has occurred, this will be reported to the Associate Dean (Education) or nominee, who may disallow the work concerned by prohibiting assessment or refer the matter to the Faculty Discipline Panel for a hearing. Student Statement: I have read the university’sStudent Academic IntegrityPolicyandProcedures. I understand the consequences of engaging in plagiarism and collusion as described inUniversity Statute 4.1–Student Discipline, Part 2 Misconducthttp://adm.monash.edu/legal/legislation/statutes/statute4-1-student-discipline.pdf. I have taken proper care to safeguard this work and made all reasonable efforts to ensure it could not be copied. No part of this assignment has been previously submitted as part of another unit/course. I acknowledge and agree that the assessor of this assignment may for the purposes of assessment, reproduce the assignment and:
RISK ASSESSMENT Name: Nuramira Amran Lab Course details (e.g. CHM 2922) CHM2922Date3/10/2020 Experiment name and numberExperiment7:Fluoride Analysis by Ion Selective Electrode Identify the HAZARD (the POTENTIAL to do harm) Determine the RISK (the PROBABILITY that harm may result) CONTROL the Risk (PREVENTING an incident) Al2(SO4)3Causes eye irrationHandle in fumehood. Wear protective gloves and goggles 1 mg/L Fluoride QC standardCauses skin and eye irritation.Handle in fumehood. Wear protective gloves and goggles. 0.1 M EDTACauses serious eye irritation.Handle in fumehood. Wear protective gloves and goggles. 4 M NaClCauses skin and eye irritation.Handle in fumehood. Wear protective gloves and goggles. 2M NaOHCauses severe skin burns and eye damage. Handle in fumehood. Wear protective gloves and goggles. Total Ionic Strength Buffer (TISAB)Causes eye damage.Handle in fumehood. Wear protective gloves and goggles. GlasswareCuts, stab wound from sharp edges Handle with care, dispose of broken glass using a dustpan & brush. If cut, see demonstrator.
Name: Nuramira Amran Session: 2PM Date: 20/9/2020 Provide explanations for your observations below.Total mark/20 1. Effect of addingAl2(SO4)3, followed by the addition of EDTAMark/5 2. Effect of adding NaClMark/5 3. Effect of adding 2M NaOHMark/5 Initially, the potential of the QC standard was 80 and then after adding the aluminium sulphate, the potential incre seconds after the addition of aluminium sulphate, the potential decreased to 150. It later dropped even more to 90 a of aluminium ions causes an interference for the fluoride determination and EDTA is used to lower the interferenc potential. The potential decreased from 80 to -50 after the addition of NaOH. This is because OH- is a major The potential increased from 79 to 95 after the addition of NaCl. The addition of NaCl is not supposed to have a inte fluoride electrode is from the OH ions. 3.1 3.2 3.3 3.4
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4. TISAB buffer is a solution made up of CDTA (a compound similar to EDTA but with faster kinetics), 4M NaCl, and has a pH of 5 - 5.5. What are the rea measuring Fluoride concentration using an ISE? Mark /5 Reference Švarc-Gajić, J., Stojanović, Z., Vasiljević, I. and Kecojević, I., 2013. Determination of fluorides in pharmaceutical products for o Journal of Food and Drug Analysis, [online] 21(4), pp.384-389. Available at: <https://www.sciencedirect.com/science/article/pii/S1021949813000537> [Accessed 27 September 2020]. Total ionic strength adjustment buffer, also known as TISAB, reduces the interference that are from OH- ions by ad formation between H+ and F- in acidic solutions". It would also be used to reduce the interference that are from po Vasiljević and Kecojević, 2013). 4.1
Name:Mark breakdown: Session:2PMDate: Cal curve R2 Value/4 Calibration - Enter mean values to check calibration%RSD of samples/9 Standard Number [F-] (M)log [F-]Mean E (mV) 11.0E-02-2.00-40.0%RE of QC/9 21.0E-03-3.0016.7ALL POINTS≥1.E-05 M 31.0E-04-4.0075.7Slope =-42.5-56.2Calculation of F in toothpaste/10 41.0E-05-5.00127.7Intercept =-108.1-151.7 51.0E-06-6.00154.0r2=0.9490.999Answer to question/8 61.0E-07-7.00164.7 Samples - Enter sample data to calculate concentrations ALL DATA POINTS SampleMean EMean [F-]mgF-/L QC76.334.57E-050.87Remember to show below how you calculated: Tap Water90.332.14E-050.411. a concentation from an E value Unknown10.001.66E-0331.572. the %error in the standard reference material (QC) Experiment 7 - ISEStudent proforma Parts 2 & 3:Data Analysis. Marked /40 Nuramira Amran y = -42.495x - 108.12 R² = 0.9493 y = -56.201x - 151.7 R² = 0.9994 -100.0 -50.0 0.0 50.0 100.0 150.0 200.0 250.0 -8.00-7.00-6.00-5.00-4.00-3.00-2.00-1.000.00 Potential difference (V) log[F-] Chart Title 5.1 5.2 Document shared on https://www.docsity.com/en/spectroscopy-and-analytical-chemistry-chm2922-lab-reports/8957042/ Downloaded by: dongxiaoma666 (dongxiaoma666@gmail.com)
Seawater10.001.66E-0331.573. the %RSD from your replicates Toothpaste58.671.19E-042.34. the % of F in toothpaste EXCL <1.E-05 SampleMean EMean [F-]mgF-/LRemember to answer the question below QC76.338.76E-051.66 Tap Water90.334.94E-050.94 Unknown10.001.33E-0325.21 Seawater10.001.33E-0325.21undiluted Toothpaste58.671.81E-043.4343.2131964 Your calculations: Standards [F]reading 1reading 2reading 3meanstd 1x10 -2M-39-43-38-402.645751311 1x10 -3M17191416.666666672.516611478 1x10 -4M73757975.666666673.055050463 1x10 -5M130126127127.66666672.081665999 1x10-6M1511521591544.358898944 1x10 -7M166163165164.66666671.527525232 QC75767876.333333331.527525232 Tapwater90928990.333333331.527525232 Toothpaste60556158.66666667 QC1.00E-04 F- 1F- 2F- 3 MeanStandard Deviation%RSD QC4.91773E-054.65838E-054.18E-054.58537E-053.74244E-068.161702472 Tapwater2.18184E-051.95778E-052.30331E-052.14765E-051.75285E-068.161702472 Toothpaste0.0001108420.0001453290.0001049970.000120392.17953E-0518.1039765 F- 1F- 2F- 3 MeanStandard Deviation%RSD% FSRM QC9.25222E-058.88082E-058.18213E-058.77172E-055.43325E-066.194050071.23E+01 Tapwater5.00434E-054.61063E-055.21363E-054.94287E-053.06164E-066.19405007 Toothpaste0.0001710590.0002099480.0001641920.0001817332.4675E-0513.577614170.343213196 Measured electrode potential (mV) All Data Points EXCL < 1.E-0.5 One of them shows the calibration graph that is between the log of the concentration value and the potential differences for the different concentration values of fluoride standard solutions. While the other shows the calibration graph that complies with the Nernst equation by having concentrations of 10-5, 10-6 and 10-7 removed. Answers to question: Why are two calibration curves drawn? 6.1 Document shared on https://www.docsity.com/en/spectroscopy-and-analytical-chemistry-chm2922-lab-reports/8957042/ Downloaded by: dongxiaoma666 (dongxiaoma666@gmail.com)
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Questions to Parts 2 and 3 Question 1Mark Discuss the calibaration curve in terms of the Nernst equation. What is the signifiance of the gradient? List three factors which would contribute to departure from Nernstian behaviour. /10 Question 2 Provide as many error sources in your calibration of the ISE as you can (up to five). /10 The calibration graph does adheres to the Nernst equation because the plot for the concentrations of 10-2 to 10-5 shows linearity while the plot for the concentrations of 10-6 and 10-7 would be away from the trendline. Furthermore, the r2 for the calibration graph is 0.9994. The Nernst equation that was used during this experiment was: E(mv) = k - 59.2log [F-] in the form of y = mx + c. According to the equation, a negative gradient is expected to be observed. This is also observed in the regression equation that is obtained from the calibration graph. The equation that was obtained was y = -56.201x - 151.7. The factor that would contribute to the departure from Nernstian behaviour would be when the electrode potential does not obey the Nernst equation when the concentration changes. This can be detected when the concentration that is plotted is away from the trendline. One possible source of error could be stirring the sample using the electrode, which would affect the ion selective membrane and hence disrupting the reading. 7.1 7.2 Document shared on https://www.docsity.com/en/spectroscopy-and-analytical-chemistry-chm2922-lab-reports/8957042/ Downloaded by: dongxiaoma666 (dongxiaoma666@gmail.com)
Question 3 Compare your determined value of fluoride with the manufacturer's claimed value. Discuss sources of error /10 Total/30 According to the toothpaste manufacturer, the fluoride content is 1000 ppm, which is equivalent to 1000 mg F/L. The amount that was calculated during the experiment was 343.21 mg F/L. This is much lower than the value that was provided from the manufacturer. The difference might not be accurate because the %RE was 12.28%, which would suggest that there might be some discrepancies. Powered by TCPDF (www.tcpdf.org) 8.1 Document shared on https://www.docsity.com/en/spectroscopy-and-analytical-chemistry-chm2922-lab-reports/8957042/ Downloaded by: dongxiaoma666 (dongxiaoma666@gmail.com)
Index of comments 3.110/20 3.23/5 The description of causes an interference is too general. How Al3+ interfere? It binds to which ions? Same goes to EDTA, what does it bind to and lead to what kind of changes? Discuss the kinetics of EDTA reaction as well. 3.30/3 Again, the explanation is too general. Explain about the ionic effect NaCl was added. How does it change the E? 3.43/5 mention the size of OH- and how does it interfere F-? 4.14/5 how about the role of CDTA? 5.117/30 5.2- %RSD of sample should be <5% - %RE? Where is the calculation? - show the calculation for % [F] 6.1So which curve is correct? explain the curvature and detection limit of ISE. 7.1- how about the effect of temperature? 7.2Give 4 more sources of error 8.1discuss what are the possible reasons that caused the error Powered by TCPDF (www.tcpdf.org) Document shared on https://www.docsity.com/en/spectroscopy-and-analytical-chemistry-chm2922-lab-reports/8957042/ Downloaded by: dongxiaoma666 (dongxiaoma666@gmail.com)
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SCHOOL OF SCIENCE ASSESSMENT COVER SHEET Student’s name(Surname)(Given names) ID numberPhone Unit nameUnit code t Note: If this is a group assignment, please include the names of all other group members. Title of assignment Lecturer/tutor Is this an authorised group assignment?YesNo Has any part of this assignment been previously submitted as part of another unit/course?YesNo Tutorial/laboratory day & time Due dateDate submitted All work must be submitted by the due date.If an extension of work is granted this must be specified with the signature of the lecturer/tutor. Extension granted until (date) ................................Signature of lecturer/tutor ................................................. Please note that it is your responsibility to retain copies of your assessments. Intentional plagiarism or collusion amounts to cheating under Monash UniversityStatute 4.1–Student Discipline. Plagiarism: Plagiarism means to take and use another person’s ideas and ormanner of expressing them and to pass these off as one’s own by failing to give appropriate acknowledgement, including the use of material from any source, staff, students or the internet, published and unpublished works. Collusion: Collusion means unauthorised collaboration on assessable written, oral or practical work with another person. Where there are reasonable grounds for believing that intentional plagiarism or collusion has occurred, this will be reported to the Associate Dean (Education) or nominee, who may disallow the work concerned by prohibiting assessment or refer the matter to the Faculty Discipline Panel for a hearing. Student Statement: I have read the university’sStudent Academic IntegrityPolicyandProcedures. I understand the consequences of engaging in plagiarism and collusion as described inUniversity Statute 4.1–Student Discipline, Part 2 Misconducthttp://adm.monash.edu/legal/legislation/statutes/statute4-1-student-discipline.pdf. I have taken proper care to safeguard this work and made all reasonable efforts to ensure it could not be copied. No part of this assignment has been previously submitted as part of another unit/course. I acknowledge and agree that the assessor of this assignment may for the purposes of assessment, reproduce the assignment and:
RISK ASSESSMENT Name: Nuramira Amran Lab Course details (e.g. CHM 2922) CHM2922Date18/10/2020 Experiment name and numberExperiment 4:Measuring Chloride in Marine Water Using Fluorescence Quenching Identify the HAZARD (the POTENTIAL to do harm) Determine the RISK (the PROBABILITY that harm may result) CONTROL the Risk (PREVENTING an incident) Sulfuric AcidCauses severe skin burns and serious eye damage. Handle in fumehood. Wear protective gloves and goggles Quinine Sulphate Causes skin, serious eye irritation and respiratory irritation. Handle in fumehood. Wear protective gloves and goggles. ChlorideHarmful if swallowed or inhaled. Handle in fumehood. Wear protective gloves and goggles. NaClCauses skin irritation and eye damage. Handle in fumehood. Wear protective gloves and goggles. GlasswareCuts, stab wound from sharp edges Handle with care, dispose of broken glass using a dustpan & brush. If cut, see demonstrator.
CHM2922 Laboratory ReportName EXPERIMENT4: PROFORMA FORMEASURINGCHLORIDE INMARINE WATER BY FLUORESCENCE QUENCHING AIM: •To determine the concentration of chloride in a marine water sample using fluorescence quenching of quinine sulphate. •Investigate if pH changes affect the quantitative analysis of quinine sulphate content and if so, how you can improve the accuracy of measurements. /1 OUTLINE OF THE METHOD: To prepare the standard solution, 0.1000 g quinine sulphate was dissolved with water in a 1L volumetric flask and then was sonicated for a few minutes to assist dissolution of the solid. Next, 10mg/L quinine sulphate standard solution was prepared using the correct amount of sulfuric acid, making sure that the solution has a pH of 3. The fluorescence cell was filled not to the brink. In order to measure the chloride in seawater samples, six solutions containing 0, 50, 100, 300, 1000 and 2000 mg/L chloride, 5 mg/L quinine sulphate and the correct amount of 0.05 M sulfuric acid was prepared. Next, 5 mL of unknown chloride solution was pipetted into a 100 mL volumetric flask, also ensuring that the solution also contains 5 mg/L quinine sulphate and the correct amount of 0.05 M sulfuric acid. It is then diluted to the mark with deionized water. This procedure was repeated triplicated. The fluorescence emission spectrum was recorded for one of the triplicates. Once the spectra were measured at each of the [Cl-] conditions, use the point measurement function for the other two replicate solutions. The instrument must be zeroed before each reading or run a control measurement of the fluorescence of a sulfuric acid solution at pH 3 under the same conditions and subtract any 3.1
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ANSWER THE FOLLOWING QUESTIONS:/12 Q1.For a quinine solution (exposed to air)vsthat of the similar solution which has been bubbled with nitrogen gas for several minutes, is there any difference in the fluorescence readings? Why? No, because according to Lakowicz (1999), fluorescence quenching “refers to any process which decreases the fluorescence intensity of a sample”.Bubbling nitrogen through the solution when measuring the fluorescence would avoid the quenching effect of oxygen (Williams and Bridges, 1964). VIDEO:Watch the video on fluorescence and answer the following question. http://www.youtube.com/watch?v=CcssdJf0pKQ(First 5 minutes, but the rest is interesting, too.). Q2. Explain why the UV and green lasers produced fluorescence when shone through the yellow dye but the red laser did not. The fluorescence is produced when the energy of the light that is emitted has a lower energy than the light that is absorbed. The red laser did not shine through the yellow because it needs light of higher energy like violet and green for it to glow. This is because the yellow light has a higher energy when compared to the red light and so it can’t excite the dye. The UV light can shine through the yellow dyebecause it’s the highest easily accessible light and so it could activate most dyes. Q3. How do you measure quinine sulphate concentration using fluorescence method? What is the one important factor that you need to control in order to obtain accurate result? In order to obtain an accurate result, the optimum pH of the solution must be maintained at 3. This is because the fluorescence spectrum for quinine sulphate is pH dependent and if the pH increases, then the lambda max of the spectrum would be lower than when it is pH 3, which is when the fluorescence intensity is the highest. 4.1 4.2 4.3
SUMMARY OFRESULTS ANDCALCULATIONS 1: Attach the spectra of quinine sulphate emission in presence of Cl-(including title and correctly labelled axes) (Choose one without chloride and one with chloride) /2 Figure 1: Spectra of quinine sulphate emission without the presence of Cl- 0 200 400 600 800 1000 1200 300350400450500550600650 Intensity Wavelength (nm) Triplicate runs 0 mg Cl added to 5.0 mg/L Quinine sulphate at pH 3 0 mg rep 20mg rep 10 mg rep 3 300 400 500 600 700 800 Intensity Triplicate runs 50 mg Cl added to 5.0 mg/L Quinine sulphate at pH 3
2: Calibration data pH of the standard solutions: Cl- Conc (mol/L) Cl- Conc (mg/L) Reading 1 Reading 2 Reading 3 Mean FSD%RSDFo/FError in Fo/F 0.0000 0977.9971.9971.7973.83.50.41.00.0 0.0014 50663.4669.2668.6667.13.20.51.59.0 x 10-3 0.0028 100466.3469.2468.0467.81.50.32.10.01 0.0085 300274.6274.8276.8275.41.20.43.50.02 0.0282 1000105.7106.9106.8106.50.70.69.16.6 x 10-2 0.0563 200057.858.357.657.90.70.616.80.1 Sea Water 1107.9105.9107.7107.21.11.09.19.9 x 10-2 Sea Water 2129.9127.8125.8127.82.11.67.60.1 Quality Control51.250.850.951.00.20.419.10.1 /15 3: Stern-Volmer Plot: y = 279.47x + 1.1473 R² = 0.9996 4.000 6.000 8.000 10.000 12.000 14.000 16.000 18.000 Fo/F
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4: Calculation of Stern-Volmer Constant KSV, quenching constant kq, and [Cl-]: Calculate KSVfrom the gradient of your S-V plot. Remember to take care of units! (Hint: Express units as M-1.) Converting concentration of Cl- from mg/L to mol/L: For 50 mg/L of Cl-: 50 mg/L = (0.05 g/ 1L) x (1/35.5 gmol-1) = 0.0014 mol/L Regression equation from plot: y = 279.47x + 1.1473 KSV=279.47 mol/L /8 Calculate kqfrom KSVusing the fluorescence lifetime of quinine. Again, take care of units! KSV= kqt0 KSV= 279.47 mol/L t0= 18.9 x 10-9seconds 279.47 = kqx 18.9 x 10-9 kq= (279.47/18.9 x 10-9) =1.48 x 1010L/mol s-1 /8 Calculate the [Cl-] in seawater sample and the Quality Control sample using the gradient of your S-V plot. Remember to take care of units! Using the regression equation from Figure 1: y = 279.47x + 1.1473 F0/F = 279.47 x (Concentration of chloride in seawater sample) + 1.1473 For Seawater Sample 1: 9.1 = 279.47 x (Concentration of chloride) + 1.1473 Concentration of chloride = (9.1–1.1473) / 279.47 =0.028 mol/L 7.1
What is the %RE of the quenching method? Known concentration of chloride in QC = 2000 mg/L Converting mg/L to molarity = 2 x (1/35.5) = 0.05633 mol/L % RE = ((measured concentration–original concentration) / original concentration) x 100 = = ((0.064–0.056) / 0.056) x 100 =14.29 % The %RE is quite high, which would indicate that the measurement is not very accurate. This might be due to some errors that might have happened during the experiment. /9 References: Lakowicz, J., 1999.Principles Of Fluorescence Spectroscopy. New York, NY: Springer, pp.237-265. Williams, R. T., & Bridges, J. W., 1964. Fluorescence of solutions: a review.Journal of clinical pathology,17(4), 371–394. https://doi.org/10.1136/jcp.17.4.371 /2 Total Mark/90 PLEASE COMPLETE RISK ASSESSMENTS AND ATTACHED A RISK ASSESSMENT FORM AT THE END OF THIS REPORT.3MARKS WILL BE DEDUCTED FOR NOT DOING SO. 8.1
Index of comments 3.1at what wavelength? 4.1O2 has quenching effect thus reducing the reading 4.2UV and green lasers have sufficient energy to excite electronically the dye molecule to excited state(s) which can relax to ground state to give colour of lower energy (yellow light) ( 2 marks) 4.3First a calibration plot is prepared using standard quinine sulphate solutions, andthe fluorescence intensity at 450 nm (or any wavelenght near to it) is measued (using 350 nm as excitation wavelength). The fluorescence of the unknown solution at the same pH is measured which can then be used to dtermine its concentration ( 2 marks). 7.1wrong units 8.1at least 2 refs
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SCHOOL OF SCIENCE ASSESSMENT COVER SHEET Student’s name(Surname)(Given names) ID numberPhone Unit nameUnit code t Note: If this is a group assignment, please include the names of all other group members. Title of assignment Lecturer/tutor Is this an authorised group assignment?YesNo Has any part of this assignment been previously submitted as part of another unit/course?YesNo Tutorial/laboratory day & time Due dateDate submitted All work must be submitted by the due date.If an extension of work is granted this must be specified with the signature of the lecturer/tutor. Extension granted until (date) ................................Signature of lecturer/tutor ................................................. Please note that it is your responsibility to retain copies of your assessments. Intentional plagiarism or collusion amounts to cheating under Monash UniversityStatute 4.1–Student Discipline. Plagiarism: Plagiarism means to take and use another person’s ideas and ormanner of expressing them and to pass these off as one’s own by failing to give appropriate acknowledgement, including the use of material from any source, staff, students or the internet, published and unpublished works. Collusion: Collusion means unauthorised collaboration on assessable written, oral or practical work with another person. Where there are reasonable grounds for believing that intentional plagiarism or collusion has occurred, this will be reported to the Associate Dean (Education) or nominee, who may disallow the work concerned by prohibiting assessment or refer the matter to the Faculty Discipline Panel for a hearing. Student Statement: I have read the university’sStudent Academic IntegrityPolicyandProcedures. I understand the consequences of engaging in plagiarism and collusion as described inUniversity Statute 4.1–Student Discipline, Part 2 Misconducthttp://adm.monash.edu/legal/legislation/statutes/statute4-1-student-discipline.pdf. I have taken proper care to safeguard this work and made all reasonable efforts to ensure it could not be copied. No part of this assignment has been previously submitted as part of another unit/course. I acknowledge and agree that the assessor of this assignment may for the purposes of assessment, reproduce the assignment and:
RISK ASSESSMENT Name: Nuramira Amran Lab Course details (e.g. CHM 2922) CHM2922Date25/10/2020 Experiment name and numberExperiment 5: Identifying Adulterants and Contaminants in Food and Drugs Using FTIR and Raman Spectroscopy Identify the HAZARD (the POTENTIAL to do harm) Determine the RISK (the PROBABILITY that harm may result) CONTROL the Risk (PREVENTING an incident) Salicylic AcidHarmful if swallowed. Causes serious eye damage. Handle in fumehood. Wear protective gloves and goggles ParacetamolHarmful if swallowed. Causes skin and serious eye irritation. Handle in fumehood. Wear protective gloves and goggles. Methyl SalicylateHarmful if swallowed. Causes eye and skin irritation. Handle in fumehood. Wear protective gloves and goggles. CaffeineHarmful if swallowed.Handle in fumehood. Wear protective gloves and goggles. AspirinHarmful if swallowed. Causes skin and serious eye irritation. Handle in fumehood. Wear protective gloves and goggles. GlasswareCuts, stab wound from sharp edges Handle with care, dispose of broken glass using a dustpan & brush. If cut, see demonstrator.
CHM2922 Laboratory ReportName Experiment 5: Identifying Adulterants and Contaminants in Food and Drugs using FTIR and Raman Spectroscopy Aim: •Identify contaminants in aspirin and paracetamol sold in supermarkets. /2 OBJECTIVES: According to Olubiyi et al. (2015),“Raman spectroscopy is a spectroscopic technique used to detect vibrational, rotational and other states in a molecular system, capable of probing the chemical compositions of materials. According to Jadhav et al. (2013), infrared spectroscopy (FTIR) is defined as“chemically specific analysis technique that identifies the chemical bonding or molecular structure of materials, based on absorption in the infrared region of the electromagnetic spectrum.” /2 SUMMARY OFRESULTS Table 1: IR and Raman band assignments of Salicylic acid IR(cm-1)Raman (cm-1)Assignment 3050 (m), 3080(m) 1652 (m) 1030 (m) 757 (s) 3228 (s, br) 3032 (s), 3068 (vs) 1631 (m) 1032 (vs) 772 (vs) 3077 (w) v(CH) v(C=O) (CH) (=C-H) v(O-H) aRelative intensities: v–very; s–strong; m–medium; w–weak; sh–shoulder; br–broad. 3.1
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Table 2:IR and Raman band assignments for Aspirin IR(cm-1)Raman (cm-1)Assignment 1083 (s) 1752 (s) 3281 (m) 755 (m) 1045 (s) 1751 (w) 3096 (m) 784 (m) v(C-O) v(C=O) v(CH) (=C-H) Table 3: IR and Raman band assignments for Paracetamol IR(cm-1)Raman (cm-1)Assignment 3159 (br, m), 3108 (m) 1610 (m) 3321 (m) 1226 (s) 3105 (m), 3065 (m) 1610 (m) 1238 (s) v(C-H) (N-H) v(O-H) v(C-O) Table 4: IR and Raman band assignments for Caffeine IR(cm-1)Raman (cm-1)Assignment 1480 (m) 1239(mw) 744(vs) 1646(s) 1361 (vs) 1329 (s) 740 (m) 1697 (mw) v(-C-H) v(C-N) (=C-H) v(C=O) Table 5: IR and Raman band assignments for Acetyl Salicylate 4.1 4.2 4.3
Table 6: IR and Raman band assignments for Methyl Salicylate IR(cm-1)Raman (cm-1)Assignment 3179 (br) 1674 (vs) 1211 (vs), 1194 (s) 1440 (mw) 2963 (w) 1677 (mw) 1252 (m) 1440 (w) v(O-H) (C=O) v(C-O) v(C=C) /36 Table 7: IR and Raman band for Unknown 1 IR(cm-1)Raman (cm-1)Mode 1681 (m) 1606 (s) 1185 (vs) 916 (vs) 1648 (mw) 1608 (s) 1169 (m) 858 (vs) v v v Table 8: IR and Raman band for Unknown 2: IR(cm-1)Raman (cm-1)Mode 1650 (s) 1185 (vs) 837 (s) 745 (vs) 1607 (s) 1169 (m) 858 (s) 785 (s) v v v Table 9: IR and Raman band assignments for Unknown 3 IR(cm-1)Raman (cm-1)Mode 5.1 5.2 5.3 5.4 5.5
CONTENTS OF THE THREE UNKNOWN MIXTURES (with a brief explanation) /12 Unknown 1 was found to be a mixture of alkyl halide (C-F), alkene (=C-H & C=C) and amide (N-H) that contains carbonyl because the peaks at 1185 cm-1, 916 cm-1, 1606 cm-1and 1681 cm-1, are within the range of characteristic absorptions, matches the type of vibration and the intensity of the mixture of the functional groups. Unknown 2 was found to be a mixture of alkene (=C-H), alkyl halide (C-Cl), ether (C-O) and amide (C=O) that contains carbonyl because the peaks on IR spectrum at 837 cm-1, 745 cm-1, 1185 cm-1and 1650 cm-1, are within the range of characteristic absorptions, matches the type of vibration and the intensity of the mixture of the functional groups. Unknown 3 was found to be a mixture of alkene (=C-H), aromatic ring (C=C), amide (C=O), alkyl halide (C-Cl) and amine (C-N) because the peaks on the IR spectrum at 756 cm-1, 1440 cm-1, 1651 cm-1, 658 cm-1and 1185 cm-1are within the range of characteristic absorptions. It also coincides with the type of vibration and the intensity of the functional groups. QUESTIONS/8 1.Analgesics do not contain just an active ingredient but may contain other materials as well. How will you argue that a particular peak on an IR or Raman spectrum belongs to a suspected contaminant rather than to a legitimate ingredient? There are two regions in an IR spectrum, a functional group region and the fingerprint region. The fingerprint region, which is a range in the IR spectrum (1500–400 cm-1) that represents the characteristic of molecular symmetry or combination bands. The functional group region is a region (4000–1500 cm-1) that is unique to a specific kind of functional group. A legitimate ingredient would have peaks in these regions, which would distinguish them from the contaminants. 2.Besides IR and Raman spectroscopy, briefly describe an analytical method that would 6.1 6.2
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REFERENCE Argenta, D., Martelli, S. and Caon, T., 2019. Dendrimer as a platform for drug delivery in the skin. In: A. Holban and A. Grumezescu, ed.,Materials for Biomedical Engineering. [online] Elsevier, pp.331-367. Jadhav N., Yan M., Vetter C.A., Kasisomayajula S.V., Gelling V.J., 2013. Infrared Spectroscopy (IR). In: Wang Q.J., Chung YW. (eds)Encyclopedia of Tribology. Springer, Boston, MA. https://doi.org/10.1007/978-0-387-92897-5_1226 Olubiyi, O., Lu, F., Calligaris, D., Jolesz, F. and Agar, N., 2015. Advances in Molecular Imaging for Surgery. In: A. Golby, ed.,Image-Guided Neurosurgery. [online] Academic Press, pp.407-439. Availableat:<https://www.sciencedirect.com/science/article/pii/B9780128008706000170> [Accessed 26 October 2020]. Total Mark/90 PLEASE COMPLETE RISK ASSESSMENTS AND ATTACHED A RISK ASSESSMENT FORM AT THE END OF THIS REPORT.3MARKS WILL BE DEDUCTED FOR NOT DOING SO.
Index of comments 3.1IR 1291-1030: v(C-O) 4.11 more IR peak required. 2500-3350: v(OH) 4.2IR 3322: v(NH) 3350-3000: v(OH) 1610: v(C=C) 4.31 more IR peak required. 1480: d(CH3) 1646: v(C=N) 4.41 more IR peak required. 1183: v(C-O) 5.1IR 1439: d(CH) 5.2missing some important bands 5.31562.7 5.4missing some important bands 5.5missing some important bands 5.6missing some important bands 5.7missing some important bands 6.1You should identify the name of compound (e.g. does it contain aspirin? paracetamol? etc.), not the structure that present in the compound. 6.24/4 6.32/4 Before MS analysis, the dissolved drug samples can be separated through LC first.