Nama : Crismonia Rinta

NIM : 17035004
Prodi : Pendidikan Kimia B
Tugas Kimia Analitik 2 Bab 4 dan Bab 5
BAB 4
4-1.Substances P and Q have distribution coeficients of 490 and 460, respectively, on
particular column. Which compound will he eluted first in a chromatographic separation?
Diketahui: KD P = 490
KD Q = 460
Ditanya: Senyawa yang pertama mengelusi?
Jawab:
Semakin besar KD suatu senyawa maka waktu retensi (tr) akan semakin besar
karena interaksi dengan fase diam besar semakin lama ia keluar dan migrasinya
semakin lambat, sehingga yang pertama akan mengelusi adalah zat Q karena
memiliki KD yang lebih kecil dari zat P, yaitu interaksinya kecil dengan fase diam
sehingga migrasinya lebih cepat.

4-2.Component Y is eluted in 15.0 min. Component Z requires 25.0 min and a non-retarded
substance X requires 2.0 min.
(a) What is the relative retention time of Z with respect to Y? Ans. 1.77
(b) What is the relative retention time of Y with respect to Z? Ans. 0.57
(c) What is the capacity factor for Y in this column? Ans. 6.5
(d) What fraction of the total time does Y spend in the mobile phase?Ans. 0.133
(e) Of the 25 minutes required to elute Z, how much time does the average Z molecule
spend in the stationary phase?Ans. 23.0 min
Diketahui : Y = 15 menit
Z = 25 menit
X = 2 menit
Jawab:
a. waktu retensi relatif Z terhadap Y = 25 / 15 = 1,77
b. waktu retensi relatif Y terhadap Z = 15 / 25 = 0,6
c. faktor kapasitas untuk Y = (15 – 2) / 2 = 6,5
d. k = 15 / 2 = 7,5 fraction of time spent in mobile phase = 1 / 7,5 = 0,133
e.
4-3. The width of a certain peak (measured in time units) is 50 sec and its retention time is 50
min. How many theoretical plates does the column contain under thesc conditions? Ans.
57.600
Diketahui: W: 50 detik
tr : 50 menit = ( 50 x 60 )detik = 3000 detik
Ditanya: n = ?
Jawab:
n = ( 4tr/W)2 = ((4 x 3000)detik / 50 detik)2
= ( 12000 / 50 )2
= (240)2
= 57600

4-4. Iso-octane and n-octane give retention times of 800 and 815 seconds on a column known
to have 8100 theoretical plates.
(a) What resolution will be obtained if a sample containing both compounds is run on i
this column?Ans. 0.42
(b) Assuming the retention times to be unchanged, how many plates would be required
to achieve a resolution of 1.00?
(c) Assuming the retention times to be unchanged, how many plates would be required
to achieve baseline resolution (R=1.5)?Ans. 103,400
4-5. The retention times of several compounds, measured from sample injection, are: air, 45
sec; propane, 1.5 min; pentane, 235 min; acetone, 2.45 min; butyraldehyde, 3.95 min;
xylene, 15.0 min. What are the relative retention tirnes of the organic compounds using
pentane as the standard?Ans. a for acetone = 1.06
Jawab :

a. 𝜶 𝒖𝒏𝒕𝒖𝒌 𝒂𝒄𝒆𝒕𝒐𝒏𝒆

𝒕𝑹 − 𝒕𝑴
𝜶=
𝒕 ∗ 𝑹 − 𝒕𝑴
𝟐. 𝟒𝟓 𝒎𝒊𝒏 − 𝟐𝟔 𝒎𝒊𝒏
𝜶=
𝟐. 𝟑𝟓 𝒎𝒊𝒏 − 𝟐𝟔 𝒎𝒊𝒏
𝜶 = 𝟏. 𝟎𝟒 𝒎𝒊𝒏
b. 𝜶 𝒖𝒏𝒕𝒖𝒌 𝒃𝒖𝒕𝒚𝒓𝒂𝒍𝒅𝒆𝒉𝒊𝒅
 𝒕𝑹 − 𝒕𝑴
𝜶=
𝒕 ∗ 𝑹 − 𝒕𝑴
𝟑. 𝟗𝟓 𝒎𝒊𝒏 − 𝟐𝟔 𝒎𝒊𝒏
𝜶=
𝟐. 𝟑𝟓 𝒎𝒊𝒏 − 𝟐𝟔 𝒎𝒊𝒏
𝜶 = 𝟏. 𝟔𝟖 𝒎𝒊𝒏

c. α untuk xylene

𝒕𝑹 − 𝒕𝑴
𝜶=
𝒕 ∗ 𝑹 − 𝒕𝑴
𝟏𝟓. 𝟎 𝒎𝒊𝒏 − 𝟐𝟔 𝒎𝒊𝒏
𝜶=
𝟐. 𝟑𝟓 𝒎𝒊𝒏 − 𝟐𝟔 𝒎𝒊𝒏
𝜶 = 𝟔. 𝟑𝟖 𝒎𝒊𝒏

4-6. The constants in the Van Deemter equation (4-10) for a particular column at 150C were
found to be: A 0.08 cm, B =0.15 cm2/sec and C= 0.03 sec. What is the optimum gas
(mobile phase) velocity for this column? What is the corresponding minimum H? Ans.
224 cm/sec, 2.14 mm
Jawab :

𝑩
𝑯=𝑨+ + 𝑪𝑼
𝒖
𝒄𝒎𝟐
𝑯 = 𝟎. 𝟎𝟖 𝒄𝒎 + 𝟎. 𝟏𝟓 /+𝟎. 𝟑𝟓
𝒔𝒆𝒄
𝑯 = 𝟐. 𝟐𝟒 𝒄𝒎/𝒔𝒆𝒄

4-7.Obtain an expression for Hmin and u in terms of A, B, and C by differentiating: Equation

4-10 and setting dH/du =0.
Jawab :
𝒅𝑯
= A + B /U + CU
𝒅𝑼

𝒅𝑯
= A+ BU-1+ CU
𝒅𝑼

𝒅𝑯
= A+2√𝑩𝑪
𝒅𝑼
 𝒅𝑼
= A + B /U + CU
𝒅𝑯

𝒅𝑼
= BU-1+ CU
𝒅𝑯

𝒅𝑼
= √𝑩/𝑪
𝒅𝑯

4-8. State the requirements for ideal chromatography and show why it is impossible to
achieve.
Jawab :
In ideal cromatoghrafi the component zones ( also called bands or peaks ) would
have no tendency to speread and would eluted from the outlet of the coloumn in the
same volume or time interval as they werw introduced at the inlet. Since the zone of
introduction can be very sharp, an ideal cromatogram would appear as a series of
very sharp, completely separated peaks, even for a sample containing many
components.
4-9. Predict the effect on resolution of adding the sample over a long period of time.
Jawab : Semakin tinggi daya kemampuan pemisahan sampel maka waktu retensi
yang dihasilkan semakin lama sehingga resolusi semakin tinggi yang berarti
pemisahan sampel yang dihasilkan kromatogram semakin baik.
4-10. Starting from Equations 4-7,4-8, and 4-11 and the approximations that W1= W2 and
that ta<tg, derive an expression for R in terms of n and a.
Jawab : R = (√𝒏/𝟒)(𝜶 − 𝟏)/𝜶)
4-11. Using the answer given for Problem 4-10, predict the resolution which will be obtained
for a two-component mixture in a 50-m column, if a 20-m column (otherwise identical)
gives a resolution of 0.80 for the same mixture. Ans. 1.27
Jawab :
4-12.What length of column is required to give a resolution of 1.50 for the mixture in
Problem 4-11?Ans. 70.3 m
BAB 5
5-1. If a monolayer of water occupies 2.86 x 103 m2/ml estimate the number of monolayer
of water corresponding to each step on the Brockmann scale for a sample of alumina
with a surface area of 175 m2/g.
Jawab :
Jumlah monolayer sesuai dengan langkah pada skala Brockmann II menyatakan
alumina mengandung air sebanyak 3 %:
3 % x 2,86. 103 m2/ml = 85,8 m2/ml
Karna 1 Kg = 1 Liter ,
maka
m2/ml= m2/gram
𝟖𝟓, 𝟖 𝒎𝟐/𝒈𝒓𝒂𝒎
𝑱𝒖𝒎𝒍𝒂𝒉 𝒎𝒐𝒏𝒐𝒍𝒂𝒚𝒆𝒓 =
𝟏𝟕𝟓 𝒎𝟐/𝒈𝒓𝒂𝒎
𝑱𝒖𝒎𝒍𝒂𝒉 𝒎𝒐𝒏𝒐𝒍𝒂𝒚𝒆𝒓 = 𝟎. 𝟒𝟗 𝒎𝒐𝒏𝒐𝒍𝒂𝒚𝒆𝒓

5-2. A 3.001 sample of sugar and potassium nitrate is dissolved in exactly 100 ml of water
and passed through a cation exchange column in the H-form. The efluent requires 5.30
ml of 0.0100 N sodium hydroxide for titration. Calculate the percentage of KNO3 in
the sample.
Jawab :
NO3-+ C6H12O2+ NaOH===>NaNO3+ KOH + C6H12O2
NaOH 0,0100N maka dalam molar = 0.0100M x e
= 0.0100M x 1
= 0.0100M
NO3-+ C6H12O2+ NaOH===>NaNO3+ KOH + C6H12O2
n NaOH = M x V
=0.0100M x 5,30 .10-3 L
=0.053x10-3 mol
n NO3- =1/1 xmol NaOH
=1/1 x 0.053x10-3 mol
=0.053x10-3 mol
𝒏
M= 𝑽(𝑳)

𝟎. 𝟎𝟓𝟑𝒙𝟏𝟎−𝟑 𝒎𝒐𝒍
𝑴=
𝟎. 𝟏 𝑳
 𝑴 = 𝟎. 𝟓𝟑 𝒙𝟏𝟎−𝟑 𝑴

Gram KNO3 :
0.053x10-3 mol= gram / Mr
0.053x10-3 mol= gram/101 mol gram-1
gram =101 mol gram-1x0.053x10-3 mol
gram =𝟎. 𝟎𝟎𝟓𝟑𝟓𝟑 𝐠𝐫𝐚𝐦

𝐠𝐫𝐚𝐦 𝐳𝐚𝐭 𝐭𝐞𝐫𝐥𝐚𝐫𝐮𝐭

% 𝐰/𝐰 = x 100 %
𝐠𝐫𝐚𝐦 𝐜𝐚𝐦𝐩𝐮𝐫𝐚𝐧
𝟎.𝟎𝟎𝟓𝟑𝟓𝟑 𝐠𝐫𝐚𝐦
% 𝐰/𝐰 = x100 %
𝟑.𝟎𝟎𝐠𝐫𝐚𝐦

%𝐰/𝐰 = 𝟎. 𝟎𝟎𝟏𝟕𝟗x100 %
% 𝐰/𝐰 = 0.179 %
5-3. Desctibc a procedure for analyzing a solution of sodium chloride in hydrochloric acid
using ion exchange resin: and 'Add-base titmtions. Indicate the method of calculating
the concentration of each of the principat ions present.
Jawab :
 Melarutkan resin Na dan resin Cl ke dalam larutan Garam NaCl 0,5N dan 0,4N
lalu membentuk reaksi kesetimbangan.
Reaksi Kation : R-Na+ + NaCl  R-Na+ + NaCl
Reaksi Anion : R+Cl- + NaCl  R+Cl- + NaCl
 Kedua, Resin Na dan Resin Cl di larutkan dalam larutan asam kuat HCl 0,4 N
dan 0,5 N, ini bertujuan untuk mengetahui proses regenerasi pada penukar ion,
di mana resin dari dari percobaan pertama di kembalikan ke keadaan awal
sehingga dapat di manfaatkan kembali. Reaksi kesetimbangan yang terjadi
antara resin dan larutan asam yaitu :
Proses Anion = R+Cl- + HCl  R+Cl- + HCl
Proses Kation = R-Na+ + HCl  R-H+ + NaCl
 Ketiga, penentuan tetapan kesetimbangan pertukaran ion dan daya pisah di
lakukan dengan cara melarutkan resin Na dan resin Cl, kedalam air (H2O) dan
juga larutan campuran dari NaCl dan HCl, sehingga terjadi reaksi
kesetimbangan pertukaran ion.
Proses Kation = R-Na+ + H2O  R-H+ + NaOH
 Proses Anion = R+Cl- + H2O  R+OH- + HCl
Pada Campuran NaCl+HCl L
Proses Anion =R+Cl- + HCl + NaCl R+Cl- + HCl + NaCls
Proses Kation =R-Na+ + HCl + NaCl  R-H+ + NaCl + NaCl’

5-4. One gram 0f dry ation exchange resin has a capacity of 5.0 meq. After swelling and
packing 1“ ! column, the same amount of resin oewpies 7. 5 ml. If the total column
contains 25 ml. how many mg of calcium Ion could it exchange?
Jawab :
𝒎𝒆𝒒
𝟓. 𝟎 𝒈𝒓𝒂𝒎 𝒙 𝟕, 𝟓 𝐦𝐥
𝐂=
𝟐𝟓 𝒎𝒍
𝒎𝒆𝒒
𝐂 = 𝟏, 𝟓
𝒈𝒓𝒂𝒎
𝐤𝐚𝐫𝐧𝐚 𝟓 𝐦𝐞𝐪,
maka massa ion kalsium yang bias ditukar adalah
𝟓 𝒎𝒆𝒒
gram= 𝟏.𝟓 𝒎𝒆𝒒/𝒈𝒓𝒂𝒎

gram= 3.34 gram

= 334 mg

5-5. Commercial ion-cxchange water softener: are commonly regenerated with a

concentrated soiution of rock salt. Why is. it not feasible to regenerate mixed bed water
deionizers?
Jawab :
Pelembut Air Industri dan Domestik adalah unit pertukaran ion
dioperasikan secara manual dirancang khusus untuk keperluan industri. hal ini
mudah dioperasikan, murah untuk mempertahankan dan banyak digunakan
dalam industri. yang terdiri dari Baja pelembut/FRP tekanan pembuluh
mengandung tidur dari resin penukar kation, sebuah sistem regenerasi dan
Multiport katup. A asam kuat resin penukar kation dalam bentuk natrium
digunakan untuk pertukaran ion natrium untuk kekerasan-membentuk ion
kalsium dan magnesium, dan dengan demikian menghasilkan air lembut. Pada
akhir setiap siklus layanan, solusi yang pertukaran ion resin dibuat ulang dengan
natrium klorida, setelah yang yang unit siap untuk layanan siklus berikutnya.
 Tidak layak untuk regenerasi air deionizers campuran karena
menggunakan dapat sesuai dengan persyaratan kualitas air: pertama kelas multi-
media filter, yang dapat menghapus lumpur, karat, koloid dan suspensi dalam air.
kelas dua karbon aktif filter, yang dapat menghapus warna, penciuman, biokimia
organik dalam air dan encrease nilai dan polusi dalam air oksigen yang kiri. kelas
Tiga dilengkapi peralatan pelembut.Kapasitas Limbah air mencapai pasokan air
dari nasional bioler tekanan rendah.

5-6. A common expression for the distribution coefficient in ion exchange studies is K=
amount of ionllof dry resin / amount of ion/mi of solution Calculate K {or Mg" ion for
the following case. A |.000-g portion of dry resin is shaken with 30.0 ml of 0.1000 M
Mg(NO,),. After equilibration. a tO-ml aliquot ot“ the supernatant solution required
2.00 ml of 0.01M F EDTA solution for titration of the magnesium: _ Mg'z-iEDTA :
Mg'EDTA Aus. 1320
Jawab :
- Mg 2+ dan Zn 2+ Sampel (ml) NO 1000 Mg
Mg 2+ Sampel (ml) NaOH (ml) 10 4,3 10 4,3 VI.
Perhitungan
a. Jumlah total mgrek H + dan ion-ion Na +, Mg 2+, Zn 2+
Volume NaOH = 200 ml Volume sampel = 10mL
Konsentrasi NO\ = 0,05 M
N NaOH = M X e = 0,05 X 1 = 0,05 N
Mgrek H + dan ion logam = mgrek Mg(NO) = V X N = 3,2 X 0,05 = 0,16
mgrek
b. Penentuan konsentrasi H + dalam sampel
Volume sampel = 10mL Volume NaOH = 2,8mL
6 N NO = 0,05 N Mgrek H + = mgrek Mg(NO)2 = V NaOH X N NaOH = 2,8 X
0,05 = 0,14 mgrek
c. Penentuan konsentrasi Mg 2+, Zn 2+
Volume Sampel = 10mL Volume EDTA = 10,325 ml
N EDTA = 0,02 N Mgrek Mg 2+ dan Zn 2+ = mgrek EDTA = V EDTA X N
EDTA = 10,325 X 0,02 = 0,2065 mgrek
d. Konsentrasi Mg 2+ Volume sampel = 10mL Volume EDTA = 4,3mL N EDTA
= 0,02 N Mgrek 2+ = mgrek
 EDTA = V EDTA X N EDTA = 4,3 X 0,02 = 0,086 mgrek Mgrek Na + =
mgrek total - mgrek H + - (Mg 2+ + Zn 2+ )
7 = 0,16-0,14-0,2065 = -0,1865 mgrek Mgrek Zn 2+ = (Mg 2+ + Zn 2+ ) Mg 2+
= 0,2065 0,086 = 0,125
5-7. Show that Equation 5-6 is equivaicnt to vo : VM + Kvs where K = Cs/Cu and Vs is. the
volume of resin.
Jawab :
Vr=VM + KVs
Vr=VM + 𝐊Vs
𝐕𝐫−𝐕𝐌
K= 𝐕𝐬
𝐕𝐌(𝟏+ 𝐊’)−𝐕𝐌
K= 𝐕𝐬
𝐂𝐒𝐂𝐕
𝐕𝐌(𝟏+ )−𝐕𝐌
𝐂𝐌𝐕𝐌
K= 𝐕𝐬
𝐕𝐌𝐂𝐒𝐂𝐕
(𝐕𝐌+ )−𝐕𝐌
𝐕𝐌𝐂𝐌𝐕𝐌
K= 𝐕𝐬
𝐂𝐒𝐂𝐕
𝐕𝐌𝐂𝐌
K= 𝐕𝐬
𝐂𝐒
K=𝐂𝐌
𝐂𝐒
Jadi Vr=VM + KVs ≅ K=𝐂𝐌

5-8. The elution volume of Zn' on a certain ion exchange column is 400 ml f or which it is
known that the interstitiat volume is 7.0 _rnl. What Is the value of D (as defined in
Equation 5-5) for Zn" under these conditions?
Jawab :
𝑗𝑢𝑚𝑙𝑎ℎ 𝑠𝑎𝑚𝑝𝑒𝑙 𝑑𝑎𝑙𝑎𝑚 𝑟𝑒𝑠𝑖𝑛 𝑘𝑜𝑙𝑜𝑚
D=
𝑗𝑢𝑚𝑙𝑎ℎ 𝑠𝑎𝑚𝑝𝑒𝑙 𝑑𝑎𝑙𝑎𝑚 𝑙𝑎𝑟𝑢𝑡𝑎𝑛 𝑖𝑛𝑡𝑒𝑟𝑠𝑡𝑖𝑡𝑖𝑎𝑙 𝑑𝑎𝑟𝑖 𝑘𝑜𝑙𝑜𝑚
𝑚𝑜𝑙
400𝑚𝐿
D= 𝑀𝑂𝐿
7 𝑚𝐿
𝑔𝑟
65𝑔𝑟/𝑚𝑜𝑙
400𝑚𝐿
D= 𝑔𝑟
65𝑔𝑟/𝑚𝑜𝑙
7 𝑚𝐿

400 𝑚𝑙
D=
7𝑚𝑙

D=56.1
5-9. In the separation at amino acids shown In Figure 5-6. the pH was held constant at 3.! (or
the first 340 ml of eluent. Would you expect acids with the largest diésociation constants
to elute first or last du'ring this interval? What 5ther factors innuencc the order of etution
of these acids? The last portion of eluent (700 to 350 ml) is at pH 5. ! . Do you expect
that the acids eluted in this interval are stronger or weaker than those eluted tint? Explain
your answers.
Jawab :
 Konstanta disosiasi untuk asam yang kuat lebih besar dari pada asam lemah.
Karena kecendrungan asam kuat untuk memisah atau melepaskan proton (H +)
lebih besar dari pada asam lemah. Maka pada pemisahan asam amino diatas
konstanta disosiasi pada kondisi elusi pertama (Ph 3.1) lebih kecil dari pada
konstanta elusi yang terakhir (Ph 5.1).
 Faktor lain yang mempengaruhi urutan elusi adalah kepolaran pelarut atau
elusi. Kepolaran ini sangat berpengaruh pada proses pemisahan.
 Asam yang dielusi pada kondisi terakhir (Ph 5.1, vol 700Ml-800mL) lebih kuat
dari pada asam pada kondisi pertama (Ph 3.1, vol 340 mL). Hal ini dilihat dari
pH antara keduanya Ph 5.1 lebih bersifat asam kuat dari pH 3.1.

5-10. Sucrose end Blue dextrnn are often used to measure V.. and V; for get columns (sec
Figure 5-8). On a certain gel eoiumn the clution volumes of these two substances are
55.5 and 9.0 ml, respectively.
(a) Predict the elution volume a! a substance with e K value of 0.40. Aus. 27.6 mi
Jawab :
𝑽𝒐
K = 𝑽𝒊

𝒐𝑽
0.40 = 𝟓𝟓.𝟓 𝒎𝑳+𝟗,𝟎 𝒎𝑳

𝑽𝒐 = 𝟎. 𝟒𝟎 𝒙 𝟔𝟒. 𝟓 𝒎𝑳
𝑽𝒐 = 𝟐𝟕. 𝟔 𝒎𝑳
(b) What is the K value for: substance for which the elution volume is 25.0 mi? Ans.
0.344
Jawab :
𝑽𝒐
K = 𝑽𝒊
𝟐𝟓,𝟎 𝐦𝐋
K = 𝟔𝟒.𝟓 𝒎𝑳
K = 0,344