31 Analysis of Volhards Methods Calculations of the experiment Step 1- Determining the average titre of Potassium Thiocyanate for the

titrations The first step of the calculations will involve calculating the mean titre of the potassium thiocyanate used for every individual cheese titrations. Three concordant titres should be taken within .1cm! of each other during the titration" these three titres will be used to calculate the average titre. #e calculate the average titre by following the formula given below$

% & % & % ' (verage titre n

)#here *%+ is the concordant titre and *n+ is the number of values used., The values are rounded to 1 decimal place in the average titre and are measured in -cm!.. Example- Philadelphia cheese spread /.0 & /./ & /./ ' /./cm! )1ounded to 1 decimal place, 3 Average titres for all the different cheese experimented with in Volhards Method: Philadelphia 2heese spread ' /./ cm! 3lue Stilton ' 4o result" as no precipitation was formed during titration. 1ed 5eicester titrated with original batch of solution ' /./cm! 1ed 5eicester titrated with new batch of solution ' /.1 cm! 5ancashire" sample boiled in 6 minutes ' 7.8 cm! 5ancashire" sample boiled in // minutes ' 9.6 cm! :dam ' 7.0 cm! :dam repeat ' 9.0 cm! Step 6- 2alculating the moles of potassium thiocyanate used The ne;t step is to calculate the moles of potassium thiocyanate we used in the titrations assuming the value we use is the average titre value. The concentration of potassium thiocyanate solution we used to titrate with the cheese solution was .1 mol. Therefore we multiply the average titre value with the concentration of the potassium thiocyanate solution" and then divide the value by 1 as we need to convert the value of cm! to dm!.

(verage titre < .1 ' mole of potassium thiocyanate used 1

Example- Philadelphia cheese spread =ingsley #ong

36 /./ < .1 ' /./ <1 mol )1ounded to 1 decimal place, 1 Moles of potassium thiocyanate used in the different cheeses experimented with: Philadelphia cheese spread ' /./ <1 mol 3lue Stilton ' no results 1ed 5eicester titrated with original batch of solution ' /./ <1 mol 1ed 5eicester titrated with new batch of solution ' /.1 <1 mol 5ancashire" sample boiled in 6 minutes ' 7.8 <1 mol 5ancashire" sample boiled in // minutes ' 9.6 <1 mol :dam ' 7.0 <1 mol :dam repeat ' 9.0 <1 mol Step 3- #orking out the moles of unreacted silver nitrate in the cheese e;tract solution >rom the background information" we have found out the e?uation of the reaction between silver ions and thiocyanate ions are as follows$ (g &)a?, & S24- (aq) (gS24)s, >rom the e?uation" we know the ratio of the reaction between silver ions and thiocyanate ions are 1$1. Therefore" the mole of potassium thiocyanate used in the reaction will be the same as the silver ions reacted in the cheese e;tract solution. Moles of silver ions reacted in the different cheeses experimented with (1 decimal place : Philadelphia cheese spread ' /./ <1 mol 3lue Stilton ' no results 1ed 5eicester titrated with original batch of solution ' /./ <1 mol 1ed 5eicester titrated with new batch of solution ' /.1 <1 mol 5ancashire" sample boiled in 6 minutes ' 7.8 <1 mol 5ancashire" sample boiled in // minutes ' 9.6 <1 mol :dam ' 7.0 <1 mol :dam repeat ' 9.0 <1 mol Step 8- #orking out the moles of unreacted silver nitrate in / solution cm3 of cheese e;tract

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33 @n the method stated" we used 1 cm3 of cheese e;tract solution each time from the total of / cm3 of the solution for the titrations. (s we have worked out the moles of unreacted silver ions in 1 cm3 of cheese e;tract solution in the previous step" we multiple the values by / to work out the total moles of unreacted silver ions. Example- Philadelphia cheese spread /./ <1 < / ' 6.A/<1 3 mol )1ounded to 6 decimal places, Moles of silver ions reacted in the different cheeses experimented with in !"" cm#: Philadelphia cheese spread ' 6.A/ <1 3 mol 3lue Stilton ' no results 1ed 5eicester titrated with original batch of solution ' 6.A/ <1 3 mol 1ed 5eicester titrated with new batch of solution ' 6.// <1 3 mol 5ancashire" sample boiled in 6 minutes ' 8.6 <1 3 mol 5ancashire" sample boiled in // minutes ' 8.0 <1 3 mol :dam ' 8.3 <1 3 mol :dam repeat ' 8.7 <1 3 mol Step /- 2alculate the moles of silver nitrate in the / cm3 of solution added during sample preparation During sample preparation" we added / cm3 of .1 mol silver nitrate solution to the grated cheese. #e now need to work out the mole in which we added to find out total amount used. Thus showing us the moles of silver ions involved in the whole procedure. To work out the mole" we convert the cm3 of the silver nitrate solution used to dm3 by dividing the value by 1 " then multiple it by the concentration which is .1 mol.

/ < .1 ' / <1 3 mol 1 So the mole of silver nitrate in / cm3 of solution is / <1 3 mol.
Step 0- 2alculate the moles of silver nitrate reacted with the salt from the cheese >rom the previous steps we have worked out the silver nitrate added and the e;cess silver nitrate reacted during titrations. So in order to work out the moles of silver nitrate which reacted directly with the salt from the cheese" we subtract the e;cess silver nitrate reacted from the total moles of silver nitrate added. Example$Philadelphia cheese spread / <1 3 mol - 6.A/ <1 3 mol ' 6.6/ <1 3 mol

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38 Moles of silver nitrate reacted with the cheese in the different cheeses experimented with: Philadelphia cheese spread ' 6.6/ <1 3 mol 3lue Stilton ' no results 1ed 5eicester titrated with original batch of solution ' 6.6/ <1 3 mol 1ed 5eicester titrated with new batch of solution ' 6.8/ <1 3 mol 5ancashire" sample boiled in 6 minutes ' .7 <1 3 mol 5ancashire" sample boiled in // minutes ' .8 <1 3 mol :dam ' .A <1 3 mol :dam repeat ' .6 <1 3 mol Step A- #orking out the moles of chloride ion in the sample of cheese >rom the background research" we found the e?uation of the reaction between silver and chloride ions$

(g& )a?, & 2l- )a?, (g2l)s,

This e?uation shows the reaction between silver and chloride ions have a 1$1 ratio. This means the mole of silver ions reacted will be the same as the mole of chloride ions reacted. (s we have worked out the silver ions reacted" therefore we know the mole of chloride ions reacted. Moles of chloride ions reacted with the cheese in the different cheeses experimented with: Philadelphia cheese spread ' 6.6/ <1 3 mol 3lue Stilton ' no results 1ed 5eicester titrated with original batch of solution ' 6.6/ <1 3 mol 1ed 5eicester titrated with new batch of solution ' 6.8/ <1 3 mol 5ancashire" sample boiled in 6 minutes ' .7 <1 3 mol 5ancashire" sample boiled in // minutes ' .8 <1 3 mol :dam ' .A <1 3 mol :dam repeat ' .6 <1 3 mol Step 7- 2onverting the moles of chloride ions to grams #e have found out the moles of chloride ions e;tracted in all the different cheeses we e;perimented with" now we will need to convert the moles to grams in order to make an =ingsley #ong

3/ easier comparison. To convert moles to grams" we must first find out the (tomic Bass of chlorine. >rom the periodic table" we can find out the (tomic Bass of chlorine is 3/./. #e multiply the (tomic mass of chlorine with the moles of chloride ions found to make the conversion. Example- Philadelphia cheese spread 6.6/ <1 3 < 3/./ ' . A97A/g %rams of chloride ion found in the different cheeses experimented with: Philadelphia cheese spread ' . A97A/g 3lue Stilton ' no results 1ed 5eicester titrated with original batch of solution ' . A97A/g 1ed 5eicester titrated with new batch of solution ' . 709A/g 5ancashire" sample boiled in 6 minutes ' . 678g 5ancashire" sample boiled in // minutes ' . 186g :dam ' . 6870g :dam repeat ' . A1g grams of cheese

Step 9- >inding out the mass of chloride ion per 1

4ow that the mass of chloride ions have been worked out the / cm3 of cheese e;tract solution which contains around 0g of cheese in each sample varying due to accuracy difference during weighing. So to work out the gram of chloride ion per type of cheese" we divide it by the mass of cheese added during sample preparation. Then multiple it by 1 to find out the value of chloride ions per 1 g of cheese. Example$ Philadelphia cheese spread Bass of cheese added- 0. 1g . A97A/ < 1 0. 1 ' 1.369g )1ounded to 3 decimal places,

Mass of chloride ion per 1"" grams for the different cheeses experimented with: Philadelphia cheese spread ' 1.369g 3lue Stilton ' no results 1ed 5eicester titrated with original batch of solution ' 1.333g 1ed 5eicester titrated with new batch of solution ' 1.8/ g 5ancashire" sample boiled in 6 minutes ' .8A3g 5ancashire" sample boiled in // minutes ' .63Ag =ingsley #ong

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:dam ' .818g :dam repeat' .117g Comparisons of results gathered from Volhards Method Type of cheese Philadelphia cheese spread 3lue Stilton 5ancashire )>ast boiling, 5ancashire )Slow boiling, 1ed 5eicester ) Dld solution, 1ed 5eicester )4ew solution, 2hloride ion e;pected per 1 g of cheese )g, .01A 4C( .9A6 .9A6 1.111 1.111 2hloride ion found per 1 g of cheese )g, 1&#'( 4C( .8A3 "&'#) 1.333 1.8/ "&*1* "&11+ 2hloride ion differences )g, .A16 more 4C( .899 less .A3/ less .666 more .339 more 1.169 less 1.81 less

:dam 1./83 :dam repeat 1./83 )3old figures represent possible anomalies, Control experiment

@ conducted several control e;periments to prove that Eolhard.s Bethod does work by using Fust salt" in the first trialG @ followed the full procedure of the method using .0/g of salt. 3ut the solution was titrated with" no precipitation was formed. @n the second trial of control e;periment" @ used the same amount of salt but @ missed out the steps involving addition of nitric acid and potassium permanganate as the there were no cheese that was needed to be digested. However" when titrating" no precipitation was formed again. @nstead" there was a strong scent of chlorine from the solution. This led me to believe that e;cess chloride ions from the salt had reacted with the water in chlorination to form chlorine water. This causes a problem as less chloride ion will react with the silver ions. Dr all of the silver ions had reacted with the chloride ions" but there were still an e;cess of it. @n the third trial" @ reduced the silver nitrate concentration to . 6mol and continued to skip the addition of nitric acid and potassium permanganate. Dnce again" no precipitation was formed. Possible reasons were that the salt was lost during filtration" and that the chloride had reacted with water again to form some chlorine water. @n the fourth trial" @ recognised that @ was using far too much salt" as lower amount of salt means less will react with the silver ions" meaning there will be more silver ions available to react with the sodium thiocyanate during titration. @ reduced the salt to .1/g" and continued to use .1mol of silver nitrate. @n the titration" precipitations formed. The results gathered had an average titre of A.9cm. (nd following the methods of calculations" the result was 1. / <1 mol of chloride ions were found. 2onverting it into grams" it was . 3Ag )3 decimal places,. .1/g of salt was added at the start of the control e;periment" to find out the grams of chloride ion present in that. #e simply divide the mass of the salt by the molecular mass of the compound" which is /7./. This finds the mole of sodium chloride present" we then multiple that value with the atomic mass of chlorine which is 3/./ to find the mass of chlorine in .1/g of sodium chloride. The result is . 91g )3decimal places,. The difference in chloride ion was . /8g. This is a big difference" but =ingsley #ong

3A factors such as chlorination of water and lost of solution through filtration all contribute to the inaccuracy. The main thing gathered from the control e;periment was that the method does work" although @ was unable to completely follow the procedure" it was the best possible control e;periment possible. Analysis of the results (fter calculating the chloride ion found in the different types of cheeses e;perimented with" @ have formulated the results to a table for comparisons. @n general" there were no perfect results. @t would have been near impossible to gather a set of perfect measurements of the chloride ion content. The results found out are compared with theoretical chloride ion e;pected" it is not the actual value but of a rough estimation. ,hiladelphia cheese spread- the chloride ion found was the third highest in the list of cheeses tested. @t had the greatest difference compared to the chloride ion e;pected" with .A16g more. This result is e;tremely unusual when @ e;pected Philadelphia cheese to only have around .01Ag of chloride ions" the lowest of all the cheeses tested on. Philadelphia cheese spread was a soft cheese" so @ e;pected easier digestion of the cheese which would therefore release the ma;imum amount of sodium chloride" hence chloride ions. However" the results suggest a much higher amount of chloride ions was present in the cheese. -lue .tilton- there was no results gathered for the 3lue Stilton cheese e;periment. This is because when titrating the solution containing the cheese e;tract" there was no precipitation forming in the addition of potassium thiocyanate. (fter two repeats" @ concluded there was no chloride ion present in the solution. This could be because the cheese was unable to be digested during sample preparation. The silver nitrate solution may be e;posed to the light for too long" causing o;idation of the silver ions. @t could be the reasons to why no precipitation was formed during the titrations. (fter conducting Eolhard.s Bethod using 3lue Stilton cheese and with no results shown" @ thought of possible reasons to why it could have occurred. Dne of the possible reasons to which @ thought might have contributed to the lack of results was the stock solutions. @ ?uestioned the stock solutions accuracy in concentration. So @ made a complete new set of standard solution to conduct with in the ne;t cheese e;periment" along with the original solutions to see if there were going to be difference in results. The ne;t cheese used was 1ed 5eicester" in which two separate set of chemicals were used during sample preparation and titration in two separate e;periments. /ed 0eicester (1riginal solutions $ The chloride ions found was 1.333g per 1 grams of cheese and the e;pected value was around 1.111g. So .666g more of chloride ion content is found" this was another unusual result as @ was not e;pecting the cheese to have more chloride ions than e;pected. /ed 0eicester (2ew solutions - the chloride ions found was 1.8/ g per 1 grams of cheese and the e;pected value was around 1.111g" (round .339g more of chloride ions was found" again" an une;pected result as more chloride ion is found in comparison to around the e;pected value. @n both e;periment" there were still undigested cheese particles remaining during sample preparation. There was most definitely a difference in the results of titration between the same cheeses by using different chemicals. The original solutions proved to give a slightly more accurate result in comparison to the new solutions. (nd both sets of solutions used provided some results" which eliminates the possibility of the stock solution in not gaining any results in the previous e;periment. (s the original set of solution provided a more accurate result" @ assumed that very small variation in the concentration of stock solutions could affect the end result. >rom the e;periment" @ decided to use the original solutions for the remaining cheeses to be tested. 3ut the fact that both cheeses had more chloride ions =ingsley #ong

37 than e;pected raised other ?uestions such as problems in my method in sample preparation. So @ decided to review the method" which could perhaps provide a more accurate salt e;traction. @n the ne;t cheese @ conducted with" 5ancashire" @ carried out two different e;periments using the same stock solutions and same mass of cheese. The difference between the two e;periments was that one would be heated for 6 minutes during sample preparation" and the other would be heated for // minutes. @ chose two e;treme values to observe the effect time under heating has on salt e;traction and efficiency of which the cheeses are dissolved. 0ancashire ('" minutes 3oiling time I .8A3g of chloride ions was found per 1 grams of cheese and the e;pected value was around .9A6g. So there was .899g less chloride ion than e;pected" this result was completely the opposite of the previous results found. The results seemed more reliable as @ e;pected less chloride ions to be found as they are lost through filtration and not all of which are released. 0ancashire (!! minutes 3oiling time I .63Ag of chloride ions was found per 1 grams of cheese and the e;pected value was around .96Ag. There is .A3/g less than the e;pected value. This result is far less accurate than the less boiling time e;periment. @ e;pected this e;periment to be more accurate as @ e;pected longer heating would release more salt from the cheese. However" there were far less chloride ions than e;pected. This set of results from the 5ancashire cheese shows that the longer heating time provided a less accurate result which was opposite to my e;pectations. However" in the longer boiling time e;periment" @ discovered that @ was conducting my method wrong. @ did not allow the reaction between nitric acid and potassium permanganate to be completed fully in the previous e;periments. So in order for the reactions to be complete" a long duration in heating is necessary" but the longer duration heating also made the results less accurate. (t the end of both the e;periments" there were still large amount of cheese particles left undigested. These results helped me to improve my method in conducting the e;perimentsG however" it raised furthermore ?uestions to the problems with the method. Prolonged heating of the solutions without digesting cheese and releasing salt could have promoted chlorination of the solution" forming some chloride water as free chloride ions have increased activation enthalpy in the solution from the heating. >ormation of chlorine water or the release of any chlorine gas would of decreased concentration of chloride ions in solution" meaning less will react with the silver nitrate. Beaning more silver ions are left" thus increasing the titres during titration. The ne;t cheese used to conduct Eolhard.s Bethod with was :dam. @ conducted the e;periment with the original solutions and @ heated it for the longer duration of time in order to try and dissolve more cheese. @ recognised that perhaps the lowered concentration of nitric acid from 0mol to /mol due to health and safety regulation in school could be a reason to why there was always a large amount of cheese particles left undigested. @n order to try and digest more of the cheese" @ increased the amount of nitric acid added from 6 cm to 3 cm and the amount of potassium permanganate added from 8 cm to 0 cm. Edam$ .818g of chloride ions was found per 1 grams of cheese and the e;pected value was around 1./83g. There is a difference of 1.169g. 1.169g of chloride ions less than e;pected was unusual" as @ e;pected :dam cheese to contain the highest amount of chloride ions as it contains the highest salt level. The :dam cheese e;periment.s results show that it contains even less chloride ions than the previous cheeses. @ increased the nitric acid used during this e;periment" but there was still undigested cheese particles left. This meant that the increased amount of nitric acid did not help to digest the :dam cheese. :dam is a very tough cheese with a chewy te;ture" this could be one of the reasons to why so little salt was e;tracted as it was harder to digest. (nother reason why the chloride ion content is calculated to be low is the interpretation of the end point. The end point of the titration was difficult to Fudge" so @ have noted down =ingsley #ong

39 several sets of possible values to which the titre could be in the :dam cheese e;periment. @ took the last set of possible values recorded and used it as my concordant titres. @ repeated the :dam e;periment again for a second set of results. Edam repeat$ .117g of chloride ions were found per 1 grams of cheese and the e;pected value is around 1./83g. There is a massive difference of 1.81 g. The repeat of the e;periment seemed to have provided even less accurate results. The trends of the data found suggest several reasons to why the results values were unusual. The softer cheeses provided more chloride ions" as the type of cheese changed" to harder cheeses" the values of chloride ion content were smaller. This suggest that the softer cheese such as Philadelphia was digested more" providing better salt e;traction in comparison to the harder cheeses such as :dam and 5ancashire. The almost rubbery nature of :dam perhaps made it harder for the cheese to be digested and the reaction rate becomes slower. (nother possible reason to the unusual trend of the data could be because additional salt is added to cheese after the manufacturing stage for better taste and prolonged preservation. This may not be included in the nutritional information provided" which therefore leads to inaccuracy when comparing the data. There was no trend suggesting that as the salt content of the cheese is higher there is a higher amount of chloride ion concentration" which would have been the logical e;pectation. @ have highlighted several values that seem to be anomalies due to the e;treme nature of the result. @ have highlighted Philadelphia cheese spread result" one of the 5ancashire result and both of the :dam results. Philadelphia showed a much higher chloride ion value and the other three results showed much lower chloride ion values" this could have arisen from all the reasons @ suggested previously. The trend showed the opposite of what @ e;pected the results to beG the logical e;pectation would be that the cheese with the highest salt content would contain the highest concentration of chloride ions. However" my e;periment shows that the cheese with the least salt contained the highest concentration of chloride ions. This trend clearly highlights some form of mistake" as the chloride ion concentration in the Philadelphia cheese spread is almost at an impossible value. This led me to review my formatted data and my raw data again. (fter carefully analysing my rough notes and raw data again" @ recognised a simple but maFor flaw in the e;periment data which could be the reason to why the trend of the date is unusual. (s stated earlier" the end point was down to interpretation and was hard to Fudge. >or some of the e;periments such as the :dam cheese e;periments" @ noted down more than 1 set of possible titre values. @ took the highest set of values as concordant titres" which was a mistake. @ used the values 7./ cm!" 7.0 cm! and 7.//cm! which made the average titre 7.0cm. However" @ also noted down A.9 cm!" A.7 cm! and A.A cm!. @f @ took these 3 titres" the average titre would be A.7 cm!. >ollowing the calculations procedures stated earlier with that starting value will provide me with .0/ g of chloride ion concentration per 1 g of :dam cheese. @n comparison to the value .818g in the original data" there is a notable difference. (lthough it would still make the value found around .793g less than the e;pected value" it proves to be more accurate. Therefore @ can conclude that the data collected are less reliable than e;pected because of the Fudgement of the end points" it is hard to rely on human eyes to decide on the titres. This clearly highlights how human error is a maFor limitation and effect on the accuracy of the e;periment from the analysis of the results. (lthough the values of e;pected chloride ion concentration for each type of cheese are estimations" it most certainly would have been impossible to get 1 percent accuracy in determining the chloride ion concentration. The data does show the method works" but it does not prove the reliability of the method.

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