DETERMINATION OF COMBUSTION HEAT (CALORIMETRIC BOMB)

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1 ILEIA UIVERITY F TELGY FAULTY F EMITRY DEPARTMET F PYIAL EMITRY AD TELGY F PLYMER DETERMIATI F MBUTI EAT ALRIMETRI BMB Exris suprvisor: Krzysztof Kroń Pl of xris: room 10 LABRATRY F PYIAL EMITRY

2 DETERMIATI F ELETRLYTE MLAR DUTIVITY AT IFIITE DILUTI I. TE AIM F TE EXERIE Th im of th xris is to msur th ht of omustion of th orni sustn in lorimtri om to lult th stnr nthlpy of tion f II. ITRDUTI AD TE TERETIAL BAKGRUD Evry hmil pross ours with ht xhn, thus, trmintion of ht volv or sor urin rtion llows to follow th xtn of tht rtion. Prosss n trnsitions n nothrmi whn systm sors th ht from th surrounin, Q > 0 or xothrmi whn systm rlss th ht to th surrounin, Q < 0: Th mount of th ht xhn with surrounin pns on onitions of ivn pross.. w istinuish th ht of prosss ourrin t onstnt volum onitions Qv or ht of prosss ourrin t onstnt prssur Qp. t of rtion unr onstnt volum Qv is fin s th mount of ht xhn with surrounin whn: pross ours t isohori v=onst onitions, th ht is th only nry xhn n th systm os not xhn with surrounin ny othr of nry, th pross is rri out xtly for stoihiomtri mounts of rtnts n th pross strts from pur sustrts to iv pur prouts. t of rtion unr onstnt prssur Qp is th mount of ht xhn with surrounin whn: pross is rri out t isori p=onst onitions, th systm xhns with surrounin nry s ht or/n s work th pross is rri out xtly for stoihiomtri mounts of rtnts n th pross strts from pur sustrts to iv pur prouts. Qp is quivlnt to nthlpy or n Qv is quivlnt to intrnl nry U or U. Th rltionship twn th ht of pross t onstnt volum Qv, n th ht of rtion unr onstnt prssur Qp rsults from th rltionship twn nthlpy n intrnl nry U n is s follows: Qp = Qv pv Assumin tht nonsous rnts volum is nliil omprin to sous rnts n tht s prouts n sustrts hv lik prft s, th followin rltionships r otin:

3 DETERMIATI F ELETRLYTE MLAR DUTIVITY AT IFIITE DILUTI 3 pv = RTn, n = U RTn whr n nots hn of sous rnts n n= Σnprouts Σnsustrts. For prtil rsons in thrmoynmi onsirtions n/or lultions r us rfrn vlus whih r th nthlpis of tion or somtims nthlpis of omustion om. Th omustion pross is fin s rtion of on mol of ivn sustn with oxyn in rsult of whih r only simpl, stl prouts suh s liqui, s, s, t. omustion of th orni sustn with th ul ours thn orin to qution: V liqui Q 4 Th tion pross on th othr hn is fin s tion of 1 mol of ivn sustn from pur lmnts inlu in its omposition s thy ppr in ntur. p Q Th nthlpy of tion of ivn sustn n lult from its nthlpis of omustion orin th ss lw. For tht rson r lso n vlus of tion nthlpis of ll prouts of tst ompoun omustion: s l rfit s om s l = om D s rfit s =

4 DETERMIATI F ELETRLYTE MLAR DUTIVITY AT IFIITE DILUTI 4 Th ht of omustion of non-xplosiv, flmml orni sustns is msur in ithrml lorimtr lorimtri om. Burnin ours in oxyn tmosphr t prssur of 0-30 r. Durin th msurmnt, th om is immrs in wtr, whih tks ll th ht rls in th omustion of th tst sustn; wtr tmprtur is msur with ury of t lst 0.01 K. Th onstrution of th lorimtri om is shown in Fiur 1. All th ps n vlvs in th om shoul los with th r hns, without th us of ny tools. mnifyin lss quipp with kliht To ontrol pnl tirrr motor Virtor tirrr Plsti ovr Trmomtr lorimtri vssl with wtr lorimtri om To inition unit Rur skt Inlt vlv xyn supply tl slf-slin p xyn -3 MP Inition wir lmps Prss smpl pllt with th inition wir ruil lorimtri om Fiur 1 lorimtri om shm

5 DETERMIATI F ELETRLYTE MLAR DUTIVITY AT IFIITE DILUTI 5 III. PREDURE Aprtus: lorimtri om, thrmomtr, wihtin ish. Rnts: phtli i 6 4, suini i - -, nzoi i 6 5, istill wtr, PREPARATI F PELLET F RGAI UBTAE A mnul prss is us for th prprtion of pills. 1. In wihin ish wih pproximtly 0.8 of th tst sustn m0.. From oil of rsistn wir ut pi with lnth of out 10 m n wiht it on n nlytil ln m1. 3. In th mil of th wir, spirl out 4-5 turns y winin it on ro with imtr of mm. 4. Pl th spirl in th prss, lin out th ns of th wir outsi throuh spil roovs. 5. Insrt th wih tst sustn into th prss hmr n thn omprss th ontnts to th pllt. 6. Losn th prss piston, rmov th mol s n thn ntly rmov th tlt y srwin th prss plunr into th mol. Th wir shoul prss into th ntr of pill. 7. Wiht stl ruil whih is prt of th lorimtri om m. 8. Wiht th tlt with th wir on n nlytil ln in m3, wihin shoul rri out irtly in stl ruil of known wiht. PREPARATI F TE BMB FR MEAUREMET 1. Unsrw th slf-slin p from th oy of th lorimtr om, rmov th h out of th oy n pl it in stn.. Pl stl ruil in th holr, insrt th pllt into it n thn ntly fix th ns of th inition wir in th lmps on th ltros. 3. t th oy of th om on holr prmnntly tth to th int n pour 3 ml of istill wtr into th oy. Put th wrh on th om oy, hk if th skt fits proprly to th oy n thn los th om tihtly. 4. Trnsfr th om to th stn nxt to th oxyn supply. Unsrw th spil srw ovrin th s inlt in th om n tth thr th onntion from n oxyn supply.

6 DETERMIATI F ELETRLYTE MLAR DUTIVITY AT IFIITE DILUTI 6 5. pn th om outlt vlv 7 y srwin th knurl hnl in lokwis irtion. 6. Ajust th rultor on th oxyn supply to th output prssur of MP, flush th om with oxyn thr tims n thn los th om inlt vlv y unsrwin th knurl hnl in n nti-lokwis irtion to th stop n fill th om with oxyn. 7. los th oxyn supply vlv, isonnt th oxyn supply from th om n rw k th spil srw of th inlt vlv. WARIG! o prt of th lorimtri om or oxyn supply my rs. Th ontmintion with fts rts th nr of xplosion. 8. onnt th ltril wirs to th ontt pins of th om n thn mov it in vrtil position to th lorimtri vssl. Th om shoul sumr in wtr up to 1/3 of th hiht of th outlt vlv. If s uls mr from th om, th om is lkin. In this s, rmov th om from th lorimtri vssl, ry it with loth n rls oxyn from it. Unsrw th slf-slin p n rmov th lk unr th ssistnt's y. MEAUREMET r ll instrutions for strtin th msurmnt! 1. onnt th inition l to th ontrol pnl.. Insrt mhnil stirrr into th lorimtr vssl, ovr on hlf of th lorimtri vssl with plsti ovr. 3. Insrt th thrmomtr into th lorimtr vssl n mount it in its holr with rur prssr. Th thrmomtr mrury tnk shoul rh hlf th hiht of th om. Th ittor n thrmomtr must not touh th lorimtri om. 4. los th othr hlf of th lorimtri vssl with plsti ovr. 5. onnt th lorimtr to th powr sokt. 6. Turn on th powr, mhnil ittor, n virtor. Th virtor striks th thrmomtr in qul 60 sons intrvls. 7. Wit 5-10 minuts to quliz th tmprtur in th lorimtr. 8. Turn on th thrmomtr kliht n th msurmnt momnt inition t th tim of tmprtur rin th inition will us th uzzr to soun, n r liht to flsh. trt tmprtur rins of th initil prio n rpt it vry 60 sons for 5 minuts. Th tmprtur rins must rri out with n ury of 0.01 K, if nssry wth th thrmomtr trouh mnifyin lss quipp with kliht. Whn usin th

7 DETERMIATI F ELETRLYTE MLAR DUTIVITY AT IFIITE DILUTI 7 mnifyin lss you shoul kp movin it ll th tim with mrury lvl hnin o not los th mrury lvl. 9. Aftr th 6th tmprtur rin, i.. ftr th n of th initil prio, immitly prss th inition utton. WARIG! At th momnt of inition n immitly ftr it, o not ln ovr th lorimtr. If th smpl urns orrtly, th r initor liht will om on n o off ftr frtion of son. nly thn shoul you rls th inition utton. If th liht stys on ll th tim with th utton prss, th msurmnt shoul intrrupt, s this inits tht th rsistn wir hs not n lit. Th min prio ins ftr propr omustion pross in om n is hrtriz y quit rpi inrs in tmprtur in its initil phs. 10. ot th tmprtur of th min prio vry 30 sons. In th momnt whn th nxt tmprtur r is lowr or th sm s th prvious on th min prio ns n th nin prio ins. Th nin prio lsts 5 minuts n th tmprtur rin is m in vry 60 sons 5 tmprtur rins. 11. Aftr th lst tmprtur rin, turn off th stirrr, thrmomtr kliht, uzzr n min powr swith. Rmov th lorimtr ovrs, rmov n sur th thrmomtr, pull out th mhnil stirrr. 1. Disonnt th inition wir plu, rmov th om from th lorimtri vssl n pl it on th stn; ry th om with loth. 13. Rls th xhust ss from th om y opnin th outlt vlv. Th vlv is opn y srwin th knurl vlv in lokwis irtion. 14. Unsrw th slf-slin p, rmov th h n st it in th tripo. 15. hk in th ruil n th om if th smpl ws ompltly urnt. nly prtils of sh n unurn prts of th wir shoul rmin in th ruil. 16. Rmov th rmins of th unurn rsistn wir from th lmpin slvs n wih thm on nlityl ln m Wih th ruil m5 n thn ln it. 18. Rins th insi of th om with istill wtr n wip it ry or lft it isssml to ir ry.

8 DETERMIATI F ELETRLYTE MLAR DUTIVITY AT IFIITE DILUTI 8 Durin th xriss you n to ristr: Amint tmprtur Wtr tmprtur in th lorimtri vssl TW Th mss of orni mttr m0 Mss of inition wir m1 Mss of mpty ruil m Th mss of th ruil with pllt of orni mttr n prss wir m3 Mss of unurn wir m4 Mss of th ruil with unurn smpl m5 Mss of unurn smpl m6=m5-m Mss of urn wir m7=m1-m4 Mss of urn smpl m8= m3-m1-m-m6 Tmprtur hns ovr tim T=ft in your lortory notook Aftr finishin th xprimnt mk rquir lultions n fill th xprimntl sht Initil prio T 0' T n' T [...] umr of hlf minut prios n' T' T v [.] Min prio n T Enin prio T 0'' T n'' n'' T'' ummry T= T 0''-T n' =... Σν=. T orr= T Σν =... m 8 [] m 1 [] m 4 [] m 7 [] t of omustion t of tion K [J/K] T= T 0''-T n' [..] Σv [..] T orr= T Σν [..].. =...[...].. =...[...]

9 DETERMIATI F ELETRLYTE MLAR DUTIVITY AT IFIITE DILUTI 9 IV. AFETY AD WATE UTILIZATI RULE TE: Bfor strtin ny work r in nnx th risks n sfty prutions ssoit with th sustns list in th xriss sujt. In s of unwnt ontt with nrous sustn, in th thr immitly. ustn lssifition Risks Prutions suini i - - phtli i 6 4 rious y m tory kin irrittion tory 315, Ey irrittion tory 319, pifi trt orn toxiity - sinl xposur tory 3 335, Xi Irritnt 318 uss srious y m. 315 uss skin irrittion. 319 uss y irrittion. 335 My us rspirtory irrittion. P80 Wr prottiv lovs/ y prottion/ f prottion. P305 P351 P338 IF I EYE: Rins utiously with wtr for svrl minuts. Rmov ontt lnss, if prsnt n sy to o. ontinu rinsin. P61 Avoi rthin ust. P305 P351 P338 P310 IF I EYE: Rins utiously with wtr for svrl minuts. Rmov ontt lnss, if prsnt n sy to o. ontinu rinsin. Wst trtmnt o wst it is urn urin th xprimnt. o wst it is urn urin th xprimnt. nzoi i 6 5 R36/37/38 kin irrittion tory 315, rious y m tory 1 318, pifi trt orn toxiity -rpt xposur, Inhltion tory 1, Luns, 37, 315 uss skin irrittion. 318 uss srious y m. 37 uss m to orns Luns throuh prolon or rpt xposur if inhl. P60 Do not rth ust/ fum/ s/ mist/ vpours/ spry. P80 Wr y prottion/ f prottion. P305 P351 P338 P310 IF I EYE: Rins utiously with wtr for svrl minuts. Rmov ontt lnss, if prsnt n sy to o. ontinu rinsin. Immitly ll PI ETER/otor. o wst it is urn urin th xprimnt.

10 DETERMIATI F ELETRLYTE MLAR DUTIVITY AT IFIITE DILUTI 10 V. ALULATI 1. Mk rph of tmprtur pnn from th tim of msurmnt.. Dtrmin th tmprtur hn usin th pproprit mtho. 3. lult th ht loss orrtion, from th xtn Rnult-Pfunlr ul, rrlss of th urtion of th min prio n thn lult th orrt tmprtur hns Torr: v in T T / / // 0 n 0 = n v / n = // n T T n // n whr: T0 / - wtr tmprtur t innin of initil prio T0 // - wtr tmprtur t innin of nin prio Tn / - wtr tmprtur t th n of initil prio Tn // - wtr tmprtur t th n of nin prio n / - numr of hlf minut prios in initil prio n // - numr of hlf minut prios in nin prio n - numr of hlf minut prios in min prio n 1 vn vin υ = n vin T T 1 whr: T / - wtr mn tmprtur in initil prio, T // - wtr mn tmprtur in nin prio, T0, Tn, - wtr tmprtur t innin n th n of min prio T T 0 n T nt Rin from th rph th hn in th tmprtur of wtr in th ht rivr T s th iffrn twn th first tmprtur of th finl prio T0 // n th finl tmprtur of th initil prio Tn /, n tkin into ount th orrtion for thrml losss ΣV, w t orrt rl hn in th tmprtur of th wtr in th rivr: T orr. = T υ 4. lult th ht of omustion of orni mttr s follows: - Form th nry ln of th prosss tht took pl in th om. Assumin itiity of th lorimtr th sum of ll ht xhn shoul qul to 0. whr: K T qv - ht of orni mttr omustion qwir. - ht of inition wir omustion = kj/ m7 - Mss of urn wir m8 - Mss of urn orni mttr K - thrml pity of th lorimtr with wtr in m q m orr. 7. wir. 8 v = q 0

11 DETERMIATI F ELETRLYTE MLAR DUTIVITY AT IFIITE DILUTI 11 - onvrt th ov ln ul n lult th ht of omustion of 1 mol of th tst sustn: whr: Mi - molulr mss of tst orni mttr Q v = K T orr. m7. qwir. M m i 8 - lult th omustion nthlpy om usin followin pnnis: = U n RT V, T n n = n n prouts r tn ts In lultion us th mn tmprtur of th min prio with th ury of 1 K. 5. lult th nthlpy of tion usin th rltionship prsnt in th thortil prt: D = om in lultions ssum tht your omustion nthlpy rouhly quls to omustion nthlpy in 85 K om om 98 n us th followin tion nthlpis = kJ mol = kJ mol = kJ mol VI. REVIEW QUETI EXAMPLE 1. Giv th finitions of th ht of omustion/tion?. Wht is th ht pity of lorimtr n wht os it onsist of? 3. Disuss th ss lw. 4. Wht typs of lorimtri msurmnts o you know? VII. LITERATURE 1. P. W. Atkins, Physil hmistry, xfor Univrsity Prss. Mtiu ori, Physil hmistry, Tylor & Frnis In, Donl A. MQurri, John D. imon, John hoi, Physil hmistry, Univrsity in Books Pr ziorow; hmi fizyzn; PW Wrszw 1965

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