Volumetric Determination of KHP (Acid-Base Titration)

(Experiment 6) INTRODU TION The object of this analysis is to determine the amount (mass percentage) of "KHP" in a solid sample by direct acid base titration !ith a standard solution of "a#H$ KHP is actually "potassium hydrogen phthalate" !hich is the mono potassium salt of phthalic acid% a diprotic organic acid$ &s illustrated belo!% KHP is amphoteric it reacts !ith acid to reform the diprotic acid H'P or !ith base (e$g$% "a#H) to produce the salt of its dianion (e$g$% K"aP)$
# ( ( # (*H6#+ ,- . /66$/0 phthalic acid (a diprotic acid) "H'P" #H #H
K#H H)

# ( ( # (*H1K#+ ,- . '2+$'' potassium hydrogenphthalate or potassium biphthalate # K) #H

"a#H H)

# ( ( # (*H+K"a#+ ,- . ''6$'2 potassium sodium phthalate (a salt of dianion P' ) "K"aP" # K) # "a)

"KHP"

Pure KHP meets all of the criteria of a primary standard grade reagent$ &s such% it !ill be used to standardi3e a solution of "a#H 4 2$/ -) that% in turn% !ill ser5e as the titrant in the determination of the KHP un6no!n$ Teamwork. &lthough each student !ill prepare their o!n standard "a#H solution and analy3e their o!n un6no!n (and be graded indi5idually as usual)% this experiment also in5ol5es !or6ing in assigned groups of four to accomplish some common goals$ ,or example% !ithin the group% each person !ill chec6 the standardi3ation of their teammate7s "a#H solutions and !ill also analy3e their teammate7s un6no!n KHP samples$ This !ill allo! us to pool the data and do a meaningful statistical analysis of the results$ There is a lot of !or6 to be done here including many extra !eighings% solution preps% and titrations% etc$ Thus% it is critical that teams coordinate their efforts and plan their work in advance ! 8e !ill spend two weeks on this experiment roughly one for preparation and standardi3ation of solutions and one for the un6no!n KHP determination$ UNKNO"N The un6no!n pro5ided !ill be a !hite po!dery solid containing some amount of KHP (typically% 01 61 9 by mass) and inert impurities$ Each member of a team !ill ha5e a different un6no!n sample that they !ill analy3e themsel5es (+ trials) and that !ill also be analy3ed by each other team member (/ trial each)$ Thus% there !ill be a total of : results generated for each un6no!n$

R#A$#NT% and %TANDARD %O&UTION% Primary standard grade KHP. ;ry 4 * g of KHP at //2 ( for one hour and store in a desiccator$ <ou !ill need four 2$1 2$6 g portions (!eighed to the nearest 2$/ mg) of KHP to standardi3e your o!n "a#H solution$ <ou !ill also need a 1$/ g portion (!eighed to the nearest 2$/ mg) of KHP to prepare a standard KHP solution$ This KHP solution !ill be used to standardi3e the "a#H solutions made by your teammates$ Preparation of 0.1 M KHP standard solution. &ll of the solutions in this experiment must be prepared using (#' free ;= !ater$ Enough (#' is effecti5ely remo5ed by simply boiling the !ater for a fe! minutes prior to use$ >oil about 122 m? of ;= !ater for 1 minutes and allo! to cool$ Pour the !ater into a polyethylene bottle !hich should be tightly capped !hene5er possible to minimi3e re absorption of (#' from the air$ 8eigh 1$/ g of dry KHP to the nearest 2$/ mg$ Transfer the KHP @uantitati5ely to a '12 m? 5olumetric flas6% add some of the pre boiled !ater$ mix thoroughly% and then fill carefully to the mar6$ (alculate the molarity of KHP to + significant figures$ <ou !ill use this solution to chec6 the standardi3ation of your teammates "a#H solution$ Preparation of 50 !a"H stock solution. Each team should prepare (and then share) one batch of "a#H stoc6 solution$ ;issol5e 4 12 g of solid "a#H in 4 12 m? of pre boiled !ater$ This should be done in a hood and the "a#H should be added slo!ly !ith stirring to dissipate the heat generated in the solution process$ #oncentrated $ase solutions are very corrosive and should $e handled carefully. The solution should be allo!ed to stand (o5ernight if possible) since some precipitate of "a'(#0 is normally present$ Atore the stoc6 solution in a tightly sealed container (a polyethylene bottle is best)$ &5oid disturbing the precipitate !hen portions of the supernatant are measured$ Preparation of appro%imately 0.1 M !a"H solution. The density of 12 9 "a#H is about /$1 gBm?$ (alculate the 5olume of this solution that is re@uired to prepare / ?iter of 2$/ "a#H (it should be 4 1$0 m?)$ >oil another liter of ;= !ater for about 1 minutes to remo5e (#' and cool$ Pour the !ater into a polyethylene bottle% !hich should be tightly capped !hene5er possible to minimi3e absorption of (#' from the air$ &dd 4 1$0 m? of 129 "a#H to a / ? 5olumetric flas6 and fill to the mar6 !ith (# ' free !ater$ The exact 5olumes are not critical here since the solution !ill be standardi3ed$ -a6e sure that the base solution is thoroughly mixed and then allo! it to cool to room temperature before performing the standardi3ation$ &tandardi'ation of !a"H solutions. =n the follo!ing procedures% your individual NaOH solution will be standardized in ten separate titrations - 4 done by you and 2 done by each of your 3 teammates. &ll /2 results must be recorded in your noteboo6 and !ill be re@uired for the lab report$ (a) *our own !a"H solution. 8eigh (to the nearest 2$/ mg) four 2$1/ g portions of dry KHP and dissol5e each in 4 '1 m? of pre boiled !ater in either a '12 m? bea6er or conical flas6$ Cinse your buret !ith ' or 0 small portions (4 0 1 m?) of your "a#H

solution$ The buret should ha5e a loosely fitted cap to minimi3e entry of (# '$ &dd + 1 drops of phenolphthalein indicator to each KHP solution$ Titrate each !ith your "a#H solution to the phenolphthalein endpoint !hich is the first appearance of pin6 color that persists for /1 seconds$ (Each sample should re@uire 4 '2 02 m? of 2$/ - "a#H in the titration$) The indicator color !ill slo!ly fade as (# ' from the air dissol5es in the solution$ (alculate the "a#H molarity (to + sig figs) for each trial% the a5erage% and the standard de5iation$ The three closest 5alues should agree to !ithin D 2$'9$ =f necessary% titrate another KHP sample$ ($) Teammate+s !a"H solutions. #btain about :1 m? of standard "a#H solution from each of your teammates$ (They should "#T tell you the concentration of their solutionE) -a6e sure that you obtain each of these solutions in a clean and ,-* flas6 or bottle in order to not alter the "a#H concentration$ ?abel each solution !ith the o!ner7s name and $e very careful to keep track of who+s solution you are working with at all times. <ou !ill then standardi3e each of these solutions by running t!o trials on each one (i$e$% a total of six titrations) using your o!n standard KHP solution prepared abo5e$ /se the following procedure for each titration. Cinse your buret thoroughly !ith ;= !ater to remo5e traces of any other "a#H solution$ Then rinse it !ith ' or 0 small portions (4 0 1 m?) of the "a#H solution that you intend to standardi3e$ Fsing a '1 m? transfer pipet% carefully measure '1$22 m? of your standard KHP solution and transfer it to a conical flas6 or bea6er$ &dd + 1 drops of phenolphthalein indicator and titrate !ith the "a#H solution to the pin6 end point as described abo5e$ (alculate the molarity of the "a#H solution and% in the end% pro5ide each of your teammates the t!o 5alues that you obtained for their solution$

PRO #DUR# -- Anal'sis of KHP Un(no)ns >y means of the follo!ing procedures% your individual KHP unknown will be analyzed in seven separate titrations - 4 done by you and by each of your 3 teammates. &ll : results must be recorded in your noteboo6 and !ill be re@uired for the lab report$ /$ ;ry your KHP un6no!n sample for at least an hour at //2 G($ (ool in desiccator$ '$ 8eigh (to the nearest 2$/ mg) four 4 2$1 2$6 g samples of your KHP un6no!n$ ;issol5e each in 4 '1 m? of pre boiled ;= !ater and add + 1 drops of phenolphthalein indicator to each solution$ Titrate each one !ith your standard "a#H solution to the pin6 endpoint as described abo5e$ 0$ (alculate the moles of KHP in each un6no!n sample by noting that one mole of "a#H neutrali3es one mole of KHP$ (alculate the mass percentage of KHP in your un6no!n for each trial and the a5erage$ The three best 5alues should agree !ithin D 2$'9$ =f necessary% titrate another sample$

+$ #btain a portion of KHP un6no!n from each of your teammates$ 8eigh (to the nearest 2$/ mg) a 4 2$1 2$6 g sample of each un6no!n% ta6ing special care not to mix them up$ (<ou should "#T be told the percent KHP in these samplesE) 1$ ;issol5e each sample in 4 '1 m? of pre boiled !ater and add + 1 drops of phenolphthalein indicator to each solution$ Titrate each one !ith your standard "a#H solution to the pin6 endpoint as described abo5e$ 6$ ,or each sample% calculate the percent KHP and report the results to the teammate !ho pro5ided the sample$

R#PORT% The lab report for this experiment consists of t!o parts that !ill count '1 points each$ (i$e$% e@ui5alent to t!o labs)$ >oth reports !ill be submitted electronically$ Part One =ndi5idual data and KHP un6no!n results$

This includes the data and results that you obtained yourself for your o!n "a#H standardi3ation and KHP un6no!n analysis$ & standard report form !ill be pro5ided$ Part T)o (ombined data and results$

>y combining the team data% each person !ill prepare a report% including an Excel spreadsheet% that summari3es and analy3es the "a#H standardi3ation data and KHP results$ &dditional details and a blan6 spreadsheet template !ill be pro5ided$

NOTE: This entire experiment requires very careful attention to detail and excellent organization, both individually and as a team. or! closely "ith your teammates to insure that no solutions, un!no"ns, etc. get mixed up. #$$ data that you obtain yourself %% regardless of "hether it pertains to your o"n solutions and un!no"n or your teammates %% must be accurately recorded in your lab noteboo!. &ata provided by a teammate must also be recorded along "ith a notation as to "ho provided it. e "ill definitely be chec!ing noteboo!s on this one'