Analisis penentuan Iodine dengan Potentiometer (Titrino/Titroprocessor)

Peralatan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0431.100 Pt Titrode; input 1

Pereaksi :
c(Na2S2O3) = 0.1 mol/L; D0

Sampel :
3 mL c(KI3) = 0.05 mol/L
5 mL c(H2SO4) = 0.5 mol/L
20 mL dist. Water

Rangkuman
· Reaksi yg terjadi :

I2 + 2 S2O32- → 2 I - + S4O62-

Perhitungan :

c(KI3)=EP1*C01/C02/C00;4;mol/L

c(KI3) = concentration of KI3 solution in mol/L
C01 = concentration of titrating agent (0.1 mol/L)
C02 = factor for “normality“ (2)

· Titrate samples immediately.

Jawaban :

c(KI3)=2.997x0.1/2/3=0.0499 mol/L

EP1=2.997 mL
C00=3 mL

Literatur
Metrohm’s Teachware on CD-ROM

Analisis penentuan Logam dg alt potensiometer (Titrino/Titroprocessor)

Peralatan :

Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0502.140 Cu2+ sensitive indicator electrode; input 1
6.0726.100 Ag/AgCl double junction reference electrode (KNO3 sat.)

Pereaksi :
c(Na2EDTA) = 0.1 mol/L; D0

Sampel :
2 mL c(ZnSO4) = 0.1 mol/L
5 mL buffer pH = 10
1 mL c(CuEDTA) = 0.1 mol/L
40 mL dist. Water

Rangkuman :
· Calculations:

Content=EP1*C01*C02/C00;2;g/l

Content = content of metal in g/L
C01 = concentration of titrating agent (0.1 mol/L)
C02 = molecular mass of metal (65.38 g/mol)

Jawaban :

Content=2.006x0.1x65.38/2=6.56 g/L

EP1=2.006 mL
C00=2.000 mL

· Buffer pH = 10: Dissolve 54 g NH4Cl and 350 mL w(NH3) = 0.25 (25%) in dist. water and fill up to 1 litre.
· Buffer pH = 4.7: Dissolve 123 g Na-acetate and 86 mL acetic acid in dist. water and fill up to 1 liter.
· The following metals can be determined according to this method: buffer solution molar mass Water, total hardness (Ca + Mg) pH = 10… 64.40
Barium Ba pH = 10… 137.36
Cadmium Cd pH = 10… 112.41
Cobalt Co pH = 10… 58.94
Nickel Ni pH = 10… 58.71
Zinc Zn pH = 10…65.38
Lead Pb pH = 4.7…207.21

Literatur :
· Metrohm Application Bulletin No. 101: Complexometric titrations with the Cu ISE

Analisis penentuan Calcium/Magnesium di dalam air dg alat potensiometer (Titrino/Titroprocessor)

Peralatan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0504.100 Ca2+ sensitive indicator electrode; input 1
6.0733.100 Ag/AgCl reference electrode (c(KCl) = 3 mol/L)

Pereaksi :
c(Na2EDTA) = 0.05 mol/L in c(KOH) = 0.1 mol/L; D0

Sampel :
100 mL tap water
15 mL c(Acetylacetone) = 0.1 mol/L in c(Trishydroxymethylaminomethane)= 0.1 mol/L (auxiliary complexing agent, pH app. 8.5)

Rangkuman :
Langkah 1 : Ca2+
Langkah 2 : Mg2+·

Perhitungan :

Ca++=EP1*C01*C02/C00;2;mmol/l
Mg++=(EP2-EP1)*C01*C02/C00;2;mmol/l
Total = EP2*C01*C02/C00;2;mmol/l

Ca++ = calcium hardness in mmol/L
Mg++ = magnesium hardness in mmol/L
Total = total hardness in mmol/L
C01 = concentration of titrating agent (0.05 mol/L)
C02 = factor for the conversion mol Þ mmol (1000).

Jawaban :

Ca++=4.245x0.05x1000/100=2.12 mmol/L
Mg++=(5.535-4.245)x0.05x1000/100=0.64 mmol/L
Total = 5.535 x 0.05 x 1000 / 100 = 2.77 mmol/L

EP1=4.245 mL
EP2=5.535 mL
C00=100 mL

· Electrode preparation:Ca electrodes should be conditioned for 10 min. in c(CaCl2) = 0.01mol/L before use.

· The volume of auxiliary reagent can be optimised for the magnesiumcontent. Rule of thumb: Ratio Mg/Acetylacetone app. 0.05.

Literatur :

Metrohm Application Bulletin No. 125: Complexometric simultaneousdetermination of calcium and magnesium in water samples andbeverages with the aid of an ion-selective calcium electrode

Analisis penentuan Ca2+ dg alat Poensiometer (Titrino/Titroprocessor)

Peralatan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0430.100 Ag Titrode amalgamated; input 1

Pereaksi :
c(Na2EDTA) = 0.1 mol/L; D0

Sampel :
2 mL c(CaCl2) = 0.1 mol/L 10 mL
buffer pH = 10
40 mL dist. Water

Rangkuman :
· Perhitungan :

c(Ca++)=EP1*C01/C00;3;mol/l

Ca++ = concentration of Ca2+ in mol/L
C01 = concentration of titrating agent (0.1 mol/L)

. Jawaban :

c(Ca++) = 2.043 x 0.1/2 = 0.102mol/L

EP1=2.043 mL
C00=2.000 mL

· Coating of Ag Titrode: Clean Ag Titrode first by immersing it in conc. HNO3, then immerse it shortly in Hg.
· Buffer pH = 10: Dissolve 54 g NH4Cl and 350 mL w(NH3) = 0.25 (25%) in dist water and fill up of 1 liter.

· If several metal ions which form EDTA complexes are present, their sum is determined.

· For a greater break, add Hg-EDTA complex.

Literatur :

Metrohm’s Teachware on CD-ROM

Analisis asam oksalat dlm fase organik ( Oxalic Acid non-Aqueous) dengan Potensiometer

Peralatan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0103.100 pH glass electrode; input 1
6.0726.100 Ag/AgCl double junction reference electrode (LiCl sat. in ethanol)

Pereaksi :
c(TBAOH) = 0.1 mol/L; D0
TBAOH = Tetrabutyl ammonium hydroxide

Sampel :
2 mL c(C2H2O4) = 0.1 mol/L; HOOC-COOH
25 mL ethanol

Rangkuman :

Perhitungan:

Oxalic=EP2*C01/C02/C00;3;mol/l

Oxalic = concentration of oxalic acid in mol/L
C01 = concentration of titrating agent (0.1 mol/L)
C02 = factor for “normality“ (2)
· Compare also titration in aqueous medium, application No. 1-4

Answer

Oxalic = 4.221 x 0.1 / 2 / 2 = 0.106 mol/L

EP1 = 2.048 mL
EP2 = 4.221 mL
C00 = 2.00 mL

Literatur:
Metrohm’s Teachware on CD-ROM

Analisis penentuan asam oksalat dengan potensiometer (Titrino/Titroprocessor)

Peralatan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0232.100 combined pH glass electrode; input 1

Pereaksi :
c(NaOH) = 0.1 mol/L; D0

Sampel :
2 mL c(C2H2O4) = 0.1 mol/L; HOOC-COOH pK1 = 1.42, pK2 = 4.31
50 mL dist. water

Rangkuman :

Perhitungan:

Oxalic=EP2*C01*C37/C02/C00;3;mol/L

Oxalic = concentration of oxalic acid in mol/L
C01 = concentration of titrating agent (0.1 mol/L)
C02 = factor for “normality“ (2)
C37 = titer of titrating agent (1.0013 common variable of “Tit.NaOH“)
Compare also titration in non aqueous medium, application No. 1-5
For pK determinations, the electrode should be calibrated.

Jawaban :

Oxalic = 4.098 x 0.1 x 1.0013 / 2 / 2 = 0.103 mol/L

EP1 = 2.110 mL
EP2 = 4.098 mL
C00 = 2 mL

Literatur:
Metrohm’s Teachware on CD-ROM

Analisis penentuan asam kuat dengan potensiometer (Titrino/Titroprocessor)

Parameter:
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0232.100 combined pH glass electrode; input 1

Pereaksi :

c(NaOH) = 0.1 mol/L; D0

Sampel :
2 mL c(HCl) = 0.1 mol/L
50 mL dist. Water

Rangkuman

Perhitungan:

C(acid) = EP1*C01*C37/C00 ; 3 ; mol/L

c(acid) = concentration of acid in mol/L
C01 = concentration of titrating agent (0.1 mol/L)
C37 = titer of titrating agent (1.0013 common variable of “Tit.NaOH“)
Carbonate may be detected separately if present!

Jawaban :

C(acid) = 1.996 x 0.1 x 1.003 / 2.00 = 0.100 mol/L

EP1 = 1.996 mL
C00 = 2.00 mL

Literatur:
Metrohm’s Teachware on CD-ROM

Analisis penentuan Non-ionic Surfactants dengan elektrode NIO

Perhitungan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0507.010 NIO surfactant electrode; input 1
6.0726.100 Ag/AgCl double junction reference electrode
(inner electrolyte c(KCl) = 3 mol/L, outer electrolyte
c(NaCl) = 1 mol/L)

Pereaksi :
c(STPB) = 0.01 mol/L; D0
STPB = sodium tetraphenylborate

Sampel :
5 mL sample solution
3 mL c(BaCl2) = 0.1 mol/L
60 mL dist. water

Rangkuman :
Titrating agent:
Dissolve 3.4223 g sodium tetraphenylborate in 300 mL dist. water. Dissolve separately 10 g polyvinyl alcohol in 300 mL dist. water and heat it slightly. Allow to cool and rinse both solutions in a 1000 mL flask. Add 10 mL buffer pH = 10 and fill up to 1 liter.

BaCl2 solution:
Dissolve 21 g BaCl2 or 25 g BaCl2*2H2O in dist. water, add 1 mL
conc. HCl and fill up to 1 liter.
Buffer pH = 10:
Dissolve 1.24 g H3BO4 in dist. water, add 10 mL c(NaOH) = 1 mol/L and fill up to 100 mL.

Preparasi Sampel :
Dissolve app. 0.5 ... 1 g detergent (Renex 650 ICI; polyoxyethylene-(30)-nonylphenol, molecular mass 1541 g/mol) in 100 mL dist. water.

Perhitungan:

Nonionic=EP1*C01*C02/C00;4;meq/g

Nonionic = concentration of nonionic Tensides in meq/g
C01 = concentration of titrating agent (0.01 mol/L)
C02 = dilution factor for the sample solution, aliquot (20)

Nonionic = 8.795 x 0.01 x 20 / 0.5145 = 3.4189 meq/g

EP1 = 8.795 mL
C00 = 0.5145 g

Literatur :
Metrohm Application Bulletin No. 230: Titrimetric/potentiometric determination of non-ionic tensides (oxyethylates) with the NIO electrode

Analisis penentuan EDTA/NTA di dalam Detergents dengan alat potensiometer (Titrino/Titroprocessor)

Peralatan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0502.140 Cu2+ sensitive indicator electrode; input 1
6.0726.100 Ag/AgCl double junction reference electrode (KNO3 sat.)

Pereaksi :
c(Cu2+) = 0.01 mol/L; D0

Sampel :
10 mL sample solution
10 mL buffer pH = 9.6 [c(NH3/NH4NO3) = 1 mol/L]
2 mL c(Na2EDTA) = 0.01 mol/L
30 mL dist. Water

Rangkuman
Perhitungan :

EDTA=(EP1-C01)*C02*C03/C00;2;%
NTA=(EP1-C01)*C02*C04/C00;2;%

EDTA = content of EDTA in %
NTA = content of NTA in %
C01 = amount of EDTA/NTA added (2 mL)
C02 = factor for % (100)
C03 = 1 mL c(Cu2+) = 0.01 mol/L = 2.9225 mg EDTA
C04 = 1 mL c(Cu2+) = 0.01 mol/L = 1.9114 mg NTA

Jawaban :

EDTA = (3.004-2.00) x 100 x 2.9225 / 82.63 = 3.55 %
NTA = (3.004-2.00) x 100 x 1.9114 / 82.63 = 2.32 %

EP1 = 3.004 mL
C00 = 82.63 mg

Preparasi sampel :
Dissolve 0.5 ... 1 g detergent in 50 mL dist. water at 40 °C. Allow solution to cool and add up to 100 mL. •Select the appropriate formula. The other may be deleted. Na2EDTA is added to get a greater break. Treat the amount of Na2EDTA added like a blank value.

Literatur:
•Metrohm Application Bulletin No. 143: Potentiometric determination of nitrilotriacetic acid (NTA) and/or ethylenediaminetetracetic acid (EDTA) in detergents.

Analisis penentuan EDTA/NTA idi dalam Detergents dengan alat potensiometer (Titrino/Titroprocessor)

Equipment
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrodes = 6.0502.140 Cu2+ sensitive indicator electrode; input 1
6.0726.100 Ag/AgCl double junction reference electrode (KNO3 sat.)

Reagents
c(Cu2+) = 0.01 mol/L; D0

Sample
10 mL sample solution
10 mL buffer pH = 9.6 [c(NH3/NH4NO3) = 1 mol/L]
2 mL c(Na2EDTA) = 0.01 mol/L
30 mL dist. Water

Remarks
Calculations:

EDTA=(EP1-C01)*C02*C03/C00;2;%
NTA=(EP1-C01)*C02*C04/C00;2;%

EDTA = content of EDTA in %
NTA = content of NTA in %
C01 = amount of EDTA/NTA added (2 mL)
C02 = factor for % (100)
C03 = 1 mL c(Cu2+) = 0.01 mol/L = 2.9225 mg EDTA
C04 = 1 mL c(Cu2+) = 0.01 mol/L = 1.9114 mg NTA

Answer

EDTA = (3.004-2.00) x 100 x 2.9225 / 82.63 = 3.55 %
NTA = (3.004-2.00) x 100 x 1.9114 / 82.63 = 2.32 %

EP1 = 3.004 mL
C00 = 82.63 mg

Sample preparation:
Dissolve 0.5 ... 1 g detergent in 50 mL dist. water at 40 °C. Allow solution to cool and add up to 100 mL. Select the appropriate formula. The other may be deleted. Na2EDTA is added to get a greater break. Treat the amount of Na2EDTA added like a blank value.

Literature
Metrohm Application Bulletin No. 143: Potentiometric determination of nitrilotriacetic acid (NTA) and/or ethylenediaminetetracetic acid (EDTA) in detergents.

Analisis penentuan 2-Aminophenol dengan alat potensiometer (Titrino/Titroprocessor)

Peralatan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0431.100 Pt Titrode; input 1

Pereaksi :
c(NaNO2) = 0.2 mol/L; D0

Sampel :
app. 0.3 ... 0.35 g sample (2-aminophenol)
10 mL w(HBr) = 0.20 (20%)
30 mL dist. Water

Rangkuman :
Determination reaction:
H+
R-NH2 + HNO2 + HBr →[R-NN+]Br- + 2 H2O

Calculations:

Content=EP1*C01*C02*C03/C00;2;%

Content = content of 2-aminophenol in %
C01 = molecular mass of 2-aminophenol (109.13 g/mol)
C02 = factor for conversion mL to L, and for % (0.001*100=0.1)
C03 = concentration of titrating agent (0.2 mol/L)
Enter the appropriate molecular mass for other amines (C01).
Instead of the Pt Titrode the 6.0420.100 combined Pt electrode can
be used.

. Jawaban :

Content = 14.396 x 109.13 x 0.1 x 0.2 / 0.3188 = 98.56 %

EP1 = 14.396 mL
C00 = 0.3188 g

Literatur :
•Metrohm Application Bulletin No. 228: Diazotisation titrations

Analisis penentuan Lipase dengan alat potensiomter (Titrino/Titroprocessor)

Peralatan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrodes = 6.0233.100 combined pH glass electrode; input 1
6.1110.100 T sensor

Pereaksi :
c(NaOH) = 0.1 mol/L; D0

Sampel :
29.5 mL substrate emulsion
0.5 mL enzyme solution

Rangkuman :
•Pancreas lipase is determined using a TIP method: The pH is adjusted to 9.20 with a pretitration (LipPre), then the sample is added and the pH kept at 9 during 5 minutes (LipDeter). The determination is carried out in a thermostated titration vessel (e.g. 6.1418.220) at 37 °C.

Perhitungan :

FIP=C70*C31/C00;1;U/mg

LipStd
Factor = calculation factor
FIP = activity of the reference standard in FIP units/mg.
C01 = declared activity of FIP standard (36.2)
C02 = 1000*concentration of titrating agent (100)
C70 = mean rate from LipDeter
LipSmpl1)
FIP = activity of the sample in FIP units/mg.
C30 = calculation factor from LipStd
C70 = mean rate from LipDeter
LipSmpSC2)
FIP = Aativity of the sample in FIP units/mg.
C31 = calculation factor from silo calculation of LipStd
C70 = mean rate from LipDeter
1): Delete the following assignments in method „LipStd“:
. in key , >silo calculations, C24=RS1 and C25=RS2
. in key , >common variables, C31=C26
2): Delete the following assignment in method „LipStd“:
. in key , >common variables, C30=MN1

Solution of Arabic gum:
Dissolve 100 g Arabic gum in 1000 mL dist. water. Centrifuge until the solution is clear (app. 10 minutes with 4000 r/min). This solution can be kept several weeks if frozen in portions.

•Substrate standard solution:
Add 165 mL Arabic gum solution, 20 mL olive oil (BP 73) and 15 mLdist. water and cool it in ice to 5 °C. Homogenize with an electric mixer during 30 minutes. The temperature of the solution should never rise above 30 °C. This solution can be kept up to 14 days in a refrigerator. Always homogenize the emulsion before use.

•Substrate emulsion:
Stir 100 mL substrate standard solution, 80 mL TRIS buffer solution, 20 mL sodium taurocholate and 95 mL dist. water. This solution must be prepared daily.

•TRIS buffer solution:
Dissolve 60.6 mg Tris(hydroxymethyl)-amino methane (C4H11NO3) and 234.0 mg sodium chloride in dist. water and fill up to 100 mL. This solution can be kept up to 3 days in a refrigerator.

•Sodium taurocholate solution:
Dissolve 4.0 g sodium taurocholate (F.I.P. controlled) in dist. Water and fill up to 50 mL.

Enzyme solvent:
Dissolve 10.0 g sodium chloride, 6.06 g Tris(hydroxymethyl)-amino methane and maleic acid anhydride (C4H2O3) in 900 mL dist. water. Adjust pH to 7.0 with 4N NaOH (app. 13 mL) and fill up to 1000 mL. This solution can be kept up to 3 days in a refrigerator.

Sample preparation:
Dissolve the enzyme in the enzyme solvent. The solution should
contain between 8 and 16 FIP Units per mL.

Comments to parameters:
LipDeter Time windows for rate evaluation. Monitoring of rate and temperature is ON: the rate should be kept in the range of 0.08...0.16 mL/min, the temperature in 0.1°C. LipStd, LipSmpl, LipSmpSC T may be measured with .

Literatur :
B. Stellmach, Bestimmungsmethoden Enzyme, Steinkopff Verlag Darmstadt, 1988, p. 263

Analisis penentuan Trypsin dengan alat potensiometer (Titrini/Titroprocessor)

Peralatan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0234.100 combined micro pH glass electrode; input 1
6.1110.100 T sensor

Pereaksi :
c(NaOH) = 0.1 mol/L in a 1 mL exchange unit; D0

Sampel :
10 mL borate buffer solution pH = 8.0
1 mL substrate solution
0.05 mL enzyme solution

Rangkuman :
•Trypsin is an enzyme which is determined using a TIP method: The pH is adjusted to 8.00 with a pretitration (TrypsPre), then the sample is added and the pH kept at 8 during 8 minutes (TrypsDet). The determination is carried out in a thermostated titration vessel (e.g.6.9914.023 with 6.2036.000 holding ring) at 25 °C.

•Perhitungan:
FIP = calculation using the final volume, according to FIP. Result in FIP units/mg.
FIP(reg) = calculation using the mean rate. Result in FIP units/mg. *)
C01 = (factor for mLL) * (concentration of reagent)(100)
C02 = determination time = 8 minutes
C70 = final volume from TrypsDet
C71 = mean rate from TrypsDet
*) The calculation using the mean rate is fundamentally different form the FIP method (final volume / time). The mean rate is calculated by linear regression over all measuring points of the list. If you wish to use only the linear part of the curve for the regression, use a start time of app. 30 s in the method “TrypsDet“. If one of the formulas is not used, you may delete it.

•Sample preparation:
Dissolve the enzyme in c(HCl) = 0.001 mol/L. The solution should not contain more than 50 FIP Units per mL.

•Substrate solution:
Dissolve 171.3 mg N-Benzoyl-L-arginine ethylester hydrochloride in dist. water and fill up to 25 mL.

•Borate buffer solution pH = 8.00:
Dissolve 286.0 mg Disodiumtetraborate-decahydrate and 1.47 g Calciumchloride-dihydrate in 400 mL dist. water, set the pH with c(HCl) = 1 mol/L to 8.00 and fill up with dist. water to 500 mL.

Comments to parameters:
TrypsDet Monitoring of pH and temperature is ON: pH should be kept in the range of 0.1, the temperature in 0.1°C. Trypsin T may be measured with .

Literature
•B. Stellmach, Bestimmungsmethoden Enzyme, Steinkopff Verlag
Darmstadt, 1988, p. 263

Analisis penentuan antacida di dalam tablet

Peralatan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0233.100 combined pH glass electrode; input 1
6.1110.100 T sensor

Pereaksi :
c(HCl) = 1.0 mol/L; D0

Sampel :
25 mL dist. water
1 drop c(NaOH) = 0.1 mol/L
0.268 g Antacid Trigastril (or 0.2-0.4 g)

Rangkuman :
. Method to determine the efficiency of tablets against an excess of acid in the stomach. Use a TIP method for the determination: The pH is adjusted to 3 with a pretitration (AntacPre), then the sample is added and the pH kept at 3 during 30 minutes (AntacDet). The determination is carried out in a thermostated titration vessel (e.g.6.1418.220) at 37 °C. You may have to adjust the control parameters of the submethod “AntacDet“ according to your sample. The given parameters are optimized for products which release their base slowly (rate app. 100 L/min).

. Perhitungan:

Acid cap=C70*C01/C00;3;mmol/g

acid cap = acid capacity in mmol/g
C01 = concentration of titrating agent (1 mol/L)

Jawaban :

Acid cap = 3.218 x 1 /0.268 = 12.008 mmol/g

C00= 0.268
C01= 1
C70= 3.218

Preparasi Sampel:
Pulverize the tablet and weigh it exactly. Rinse the powder with 20 mL of pretitrated solution (pH=3) into the titration vessel during the request “Add smpl & start“ and titrate immediately.

Literatur :
•N.J. Kerkhoff et al., Journal of Pharmaceutical Sciences, 66, 1528-
1535 (1977)

Analisis ion Na+ / Cl- di dalam larutan Isotonic dengan alat Potensiometer (Titrino/Titroprocessor )

Alat yg digunakan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrodes = 6.0430.100 Ag Titrode; input 1

Pereaksi :
c(AgNO3) = 0.1 mol/L; D0

Sampel :
5 mL sample solution (153 mmol/L Na+ / Cl-)
2 mL c(HNO3) = 2 mol/L
30 mL dist. water

Rangkuman :
• Calculations:

Na+Cl-=EP1*C01*C02/C00;2;mmol/l

Na+Cl- = concentration of Na+ / Cl- in isotonic solution in mmol/L
C01 = concentration of titrating agent (0.1 mol/L)
C02 = factor for conversion mol/L Þ mmol/L (1000)

. Jawaban :

Na+Cl- = 7.652 x 0.1 x 1000 / 5.00 = 153.04 mmol/L

EP1 = 7.652 ml
C00 = 5 mL

Literatur :
• Metrohm Application Bulletin No. 130: Chloride titrations with
potentiometric end-point indication.

Analisis ( penentuan ) Vitamin C dengan alat Potensiometer (Titrino/Titroprocessor )

Alat yang digunakan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrodes = 6.0309.100 double Pt sheet electrode; input Pol
polarized Ipol = 1 mA
Voltametric indication

Reagents
c(DPIP) = 0.001 mol/L; D0
2,6-Dichlorophenol indophenol

Sample
5 mL sample solution
Dissolve 1 effervescent vitamin C tablet in 1 L dist. water
15 mL oxalic acid solution 1 g/L
1 mL w(sodium acetate) = 0.10 (10%)
10 mL dist. Water

Remarks
• Calculations:

Vit.C=EP1*C01*C02*C03;0;mg/pc
Vit.C=EP1*C01*C02/C00;4;g/l

Vit.C = content of Vitamin C in mg/pc (tablet)
Vit.C = content of Vitamin C in g/L
C01 = mg Vitamin C / 1 mL titrating agent (0.088)
C02 = factor of titrating agent (1.00)
C03 = dilution factor (200)

. Answer

Vit.C = 15.291 x 0.088 x 1.00 x 200 = 269 mg/pc
Vit.C = 15.291 x 0.088 x 1.00 / 5.00 = 0.2691 g/L

EP1 = 15.291 mL
C00 = 5.00 mL

• Titrating agent:
Dissolve 295 mg 2,6-Dichlorophenol indophenol with vigorous agitation in 1 L dist. water, then filter and mix with 100 mg sodium bicarbonate. This solution can be stored in the refrigerator for about 1 month, the factor should be checked daily with standard ascorbic acid. (As a titrating agent, the more readily soluble sodium salt may be used instead.)

• Standard solution:
r (Vitamin C) = 500 mg/L
Dissolve 50 mg ascorbic acid in oxalic acid solution (1 g/L) and make up to 100 mL. This solution should be freshly prepared daily.

• Sample preparation:
Place dist. water, oxalic acid solution and sodium acetate buffer in the titration vessel and deaerate by passing a stream of nitrogen for 3...5 min. Then add a quantity of sample or standard solution containing about 0.05...0.5 mg vitamin C. Now titrate under nitrogen with titrating agent.
• Store electrode in acidified Na2S2O3 solution.
• Select the appropriate formula. The other may be deleted.
• The 6.0431.100 Pt Titrode may be used together with mode MET U.

Literature
• Metrohm Application Bulletin No. 98: Determination of ascorbic acid
(Vitamin C) and its compounds.

Analisis (penentuan) angka Iod ( Iodine Number ) dengan alat potensiometer (Titrino/Titroprocessor)

Alat yang digunakan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrodes = 6.0431.100 Pt Titrode; input 1

Reagents
c(Na2S2O3) = 0.1 mol/L; D0

Sample
app. 0.5 g sunflower oil
15 mL CCl4
25 mL c(ICl) = 0.1 mol/L (according to Wijs in glacial acetic acid / CCl4,
e.g. Merck No. 9163)
10 mL w(Hg acetate) = 0.025 (2.5%) in glacial acetic acid
15 mL w(KI) = 0.10 (10%)
30-50 mL dist. water

Remarks
• Calculations:

Iod.No=(C01-EP1)*C02/C00;2;g/100g

Iod.No = iodine number in g iodine / 100 g sample
C01 = consumption of blank sample (0 mL)
C02 = molecular mass of I * concentration titrating agent * 100g
sample / factor mL -> L (126.9 * 0.1 *100/1000 = 1.269)

. Answer

Iod.No = (0 – 6.149) x 1.269 / 0.5204 = 104.61 g/100g

EP1 = 6.149 mL
C00 = 0.5204 g

• Sample preparation:
According to the expected iodine number, weigh out 0.10 ... 1.00 g of the sample in an Erlenmeyer flask and add 15 mL CCl4. Add 25 mLiodine monochloride solution and add 10 mL mercuric acetate solution, mix and allow to stand for 5 min. in a dark place. Then add 15 mL KI solution, rinse into a beaker with dist. water and back-titrate the excess iodine with sodium thiosulphate. A blank control sample should be prepared and treated in the same way. Enter the blank value as C01.
• You may add a solution of w(Mg-acetate) = 0.03 (3%) instead of the Hg-acetate solution.
• The sample must be stirred well during the titration, in order to obtain a good emulsion.

Literature
• Metrohm Application Bulletin No. 141: Analysis of edible oils and fats.

Penentuan angka asam dengan alat potensiometer

Alat yang digunakan :

Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0133.100 pH glass electrode; input 1
6.0726.100 Ag/AgCl double junction reference electrode
(LiCl sat. in ethanol)

Pereaksi yg digunakan :

c(NaOH) = 0.1 mol/L; D0

Contoh :
app. 5-10 g minyak bunga matahari
50 mL ethanol / diethylether (1 : 1), neutralized

Rangkuman :
• Perhitungan :

Acid.No=EP1*C01/C00;2;mg/g
FFA=RS1*C02/C03;2;

Acid.No = acid number in mg KOH per g of sample
FFA = free fatty acid
C01 = mg KOH / 1 mL titrating agent (5.61)
C02 = relative molecular mass (282 for oleic acid)
C03 = factor (561)

. Jawaban

Acid.No = 0.150 x 5.61 / 10.3223 = 0.08 mg/g
FFA = 0.08 x 282 / 561 = 0.04

RS1 = 0.08
EP1 = 0.150 mL
C00 = 10.3223 g

Literature
• Metrohm Application Bulletin No. 141: Analysis of edible oils and fats.

Penentuan angka saponifikasi ( Saponification Number ) dengan alat potensiomter ( titrino/titroprocessor )

Alat yg digunakan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrodes = 6.0232.100 combined pH glass electrode; input 1

Pereaksi :
Konsentresi c(HCl) = 1 mol/L; D0

Sampel :
app. 2 g minyak bunga matahari
25 mL c(KOH) = 0.5 mol/L in ethanol
app. 10-20 mL dist. water

Rangkuman
• Perhitungan:

Sapon.No=(C01-EP1)*C02/C00;1;mg/g

Sapon.No = saponification number in mg KOH per g of sample
C01 = consumption of blank sample (12.199 mL)
C02 = mg KOH / 1 mL titrating agent (56.1)

. Jawaban

Sapon.No = (12.199-5.271) x 56.1 / 2.0224 = 192.2 mg/g

EP1 = 5.271 mL
C00 = 2.0224 g

• Preparasi Sampel :
Weigh out approx. 2 g sample in a round-bottomed flask. Add 25 mL alcoholic KOH solution plus a few boiling beads and allow to boil lightly for at least 30 min. Shake from time to time. Finally rinse the content of the round-bottomed flask into a beaker with a small quantity of dist. water and back titrate the excess of potassium hydroxide with HCl. A blank control sample should be prepared and treated identically. Enter the blank value as C01.

Literatur :
• Metrohm Application Bulletin No. 141: Analysis of edible oils and fats.

Penentuan angka peroksid ( Peroxide Number ) dengan alat Potensiometer ( Titrino/Titroprocessor )

Peralatan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrodes = 6.0431.100 Pt Titrode; input 1

Pereaksi :

c(Na2S2O3) = 0.01 mol/L; D0
Prepared daily from c = 0.1 mol/L

Sampel :
app. 5 g sunflower oil
50 mL glacial acetic acid / chloroform (3 : 2)
1 mL KI saturate
100 mL dist. water

Rangkuman :
• Perhitungan :

Perox.No=(EP1-C01)*C02/C00;2;meq/kg

Perox.No = peroxide number in meq.O2/kg
C01 = consumption of blank sample (0 mL)
C02 = factor (10)

. Jawaban :

Perox.No = 0.8874 x 10 / 5.0188 = 1.77 meq/Kg

EP1 = 0.8874 mL
C00 = 5.0188 g

• Preparasi Sampel :
Weigh out accurately 5 g sample in an Erlenmeyer flask and add 50 mL of the glacial acetic acid / chloroform mixture. Then add 1 mL of the KI solution and shake during 5 s. Now allow the mixture to stand for about 1 min. in a dark place. After this, rinse the contents of the Erlenmeyer flask out into a beaker with 100 mL dist. water and immediately back-titrate the iodine thus liberated with sodium thiosulphate. A blank control sample should be prepared and treated in the same way. Enter the blank value as C01.
• The sample must be stirred well during the titration, in order to obtain a good emulsion.

Literatur :
• Metrohm Application Bulletin No. 141: Analysis of edible oils and fats.

Penentuan (analisis) Calcium/Mg di dalam produk susu dengan alat potensiometer (Titrino/Titroprocessor)

Alat yang digunakan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0502.140 Cu2+ sensitive indicator electrode; input 1
6.0726.100 Ag/AgCl double junction reference electrode (KNO3 sat.)

Pereaksi yang digunakan :
c(EGTA) = 0.1 mol/L; D0
c(Cu complex) = 0.100 mol/L; D1
Larutan Buffer pH = 10; D2

Contoh :
app. 10 g milk

Rangkuman
• Perhitungan :

Calcium=C70*C01*C02*C03/C00;3;%

Calcium = Kandungan calcium dalam %
C01 = concentration of titrating agent (0.1 mol/L)
C02 = molecular mass of calcium (40.08 g/mol)
C03 = factor for % (0.1)
C70 = EP1 from submethod Milk-Ca3

. Jawaban :

Calcium = 3.008 x 0.1 x 40.08 x 0.1 / 10.0516 = 0.12%

C70 = 3.008

• Pereaksi :
c(EGTA) = 0.100 mol/L:
38.04 g EGTA - ethylene glycol-0,0’-bis-(2-aminoethyl)-N,N,N’,N’- tetraacetic acid are added to a 1 liter volumetric flask, dissolved in 250 mL c(NaOH) = 1 mol/L and the solution made up to the mark with dist. water.
Cu complex:
EGTA titrant (100 mL) is mixed with 100 mL of a solution containing 0.2 mol/L NH4Cl and exactly 0.100 mol/L Cu(II)nitrate. Titration can used to check that this solution contains no excess of Cu(II) or EGTA.
Buffer solution pH = 10:
54 g NH4Cl is dissolved in ca. 400 mL dist. water in a volumetric flask, 300 mL w(NH3) = 0.25 (25%) added and the solution made up to 1 liter with dist. water.
• The method „Milk-Ca3“ can also be used as work-alone method (without TIP). Add the Cu complex-solution and the buffer solution manually.

Literature
• Metrohm Application Bulletin No. 235: Potentiometric titration of Ca (Mg) in milk products

Penentuan dari Formaldehyde Number di dalam jus buah dengan alat potensiometer

Alat yang digunakan :
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0232.100 combined pH glass electrode; input 1

Pereaksi yang digunakan :
c(NaOH) = 0.1 mol/L; D0
w(HCHO) = 0.35 (35%), diatur sampai pH = 8.5 dengan NaOH; D1

Contoh : Jus jeruk
25 mL contoh

Electrode
6.0232.100 combined pH glass electrode; input 1

Rangkuman :
• Determination reaction:
OH
H2C=O + H2N-R Þ H2C + H+
NHR
Amino groups of amino acid react according to the above reaction.

• Perhitungan :

Formol No = C70*C01;1;

Formol No = formol number as mL NaOH 0.1 mol/L for 100 mLsample solution
C01 = factor for 100 mL sample solution (4)
• Calibrate the electrode for the SET titration.

. Jawaban :

Formol No = 5.634 x 4 = 22.5

C70 = 5.634

Literature :
• Metrohm Application Bulletin No. 180: Automatic determination of the
formol number in fruit and vegetable juices

Penentuan (analisis) NaCl di dalam larutan menggunakan alat Potensiometer

Alat yang digunakan
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrode = 6.0430.100 Ag Titrode amalgamated; input 1

Pereaksi
c(AgNO3) = 0.1 mol/L; D0

Contoh
20 mL larutan contoh
5 mL c(HNO3) = 2 mol/L
30 mL air destilasi


Rangkuman
· Perhitungan

NaCl=EP1*C01*C02*C03/C00;2;%

NaCl = kandungan NaCl di dalam larutan in %
C00 = banyaknya contoh (10 g / 100 = 0.1 g)
C01 = Berat molekul dari NaCl (58.44 g/mol)
C02 = konsentrasi larutan titer (0.1 mol/L)
C03 = faktor konversi mL Þ L dan % (0.001*100 = 0.1)

. Jawaban

NaCl = 8.070 x 58.44 x 0.1 x 0.1 / 0.1 = 47.16 %

EP1 = 8.070 mL
C00 = 0.1 g

· Sample preparation:
Dissolve 10 g (1 cube) conc. broth in 800 mL boiling dist. water. Rinse
this solution in a 2000 mL measuring flask. Allow to cool down and fill
up to the mark. Filter with a folded filter. Take 20 mL aliquots.

Literature
· Metrohm Application Bulletin No. 130: Chloride titrations with
potentiometric end-point indication.

PENENTUAN KADAR Cu, Cd DAN Pb DALAM ABU LIMBAHMEDIS DENGAN SPEKTROFOTOMETER SERAPAN ATOM (AAS)

ABSTRAK
PENENTUAN KADAR Cu, Cd DAN Pb DALAM ABU LIMBAH MEDIS DENGAN SPEKTROFOTOMETER SERAPAN ATOM (AAS). Telah dilakukan preparasi dan penentuan logam-logam berat Cu, Cd dan Pb dalam contoh abu limbah medis dengan metode nyala spektrofotometri serapan atom. Abu limbah medis digerus dan diayak hingga lolos 100 mesh, kemudian didestruksi menggunakan campuran asam nitrat dan asam fluorida pekat dalam teflon bom digester pada suhu 150 0 C selama 3 jam, untuk mendapatkan larutan yang jernih. Hasil pelarutan dijadikan volume tertentu dengan penambahan akuabides. Kadar unsur logam-logam berat Cu, Cd dan Pb dalam contoh ditentukan dengan kurva kalibrasi standar pada kondisi optimum masing-masing unsur. Diperoleh kadar logam-logam berat Cu, Cd dan Pb dalam cuplikan masing-masing 136 ± 0.544 ppm, 4,250 ± 0.068 ppm dan 72,5 ± 1,523 ppm. Kadar ini sudah melebihi ambang batas , oleh karena itu industri terkait harus melakukan pengolahan limbah lebih lanjut.

STUDI TOKSISITAS DEKONTAMINAN PRUSSIAN BLUE PADA KERA EKOR PANJANG MACACA FASCICULARIS

Tur Rahardjo dan Siti Nurhayati
Pusat Teknologi Keselamatan dan Metrologi Radiasi BATAN
ABSTRAK
STUDI TOKSISITAS DEKONTAMINAN PRUSSIAN BLUE PADA KERA EKOR PANJANG MACACA FASCICULARIS. Dekontaminan pada kadar tertentu dalam tubuh korban kontaminasi dapat menimbulkan efek keracunan. Oleh karena itu telah dilakukan pengukuran biokimia darah kera ekor panjang sebagai uji toksisitas akibat diberi dekontaminan Prussian Blue (PB) dengan dosis 600, 900, 1050 mg/berat badan (BB). Pengamatan biokimia darah meliputi ureum, kreatinin, gula darah, protein total, SGOT (serum glutamic oxalic transaminase) dan SGPT (serum glutamic piruvic transaminase) yang dilakukan pada hari-hari ke 0, 1, 2, 3, 7, 14, 21, 28, dan 35 setelah pemberian PB. Hasil pengamatan menunjukan bahwa pemberian dekontaminan PB tidak mempengaruhi kadar ureum, kreatinin, gula dalam darah, protein total, SGOT dan SGPT sebagai fungsi ginjal dan hati sampai hari ke 35 pasca pemberian dekontaminan, tetapi enzim-enzim, ureum dan kreatinin dalam darah sedikit lebih tinggi daripada kontrol dan masih dalam batas-batas normal, tetapi pemberian PB hanya mempengaruhi fungsi hati dan ginjal kera yang bersifat sementara. Perubahan terjadi pada hari pertama dan kembali normal dalam waktu 7- 28 hari pasca pemberian. Dosis PB hingga dosis 1050 mg/BB belum bersifat toksik pada hewan.