hydrogenation .ppt; basestock and process control

Copyright M HUSNI RIZAL WTDP 2008 1

Hydrogenation ; Base stock and Process Control

Solidification, Consistency, and Composition Analysis


• Palmitic basedThe major content of oil is palmitic acid which derived from Crude Palm Oil eg. RBDPO, RBDST, RBDOL, Soft ST, COL, CPS, PMF, PFAD, etc

• Lauric basedThe major content of oil is lauric acid which derived from Crude Coconut Oil and Crude Palm Kernel Oil eg. CKS, CKL, RKS, RKL, RCNO, PKFAD, etc

Oil Type


• Crude eg. CPO, CPKO, CCNO, CKS, CKL, etc.

• Refinedeg. RPO, RST, RBDOL, RKS, RKO, RKL, RCNO, etc.

• Hydrogenatedeg. HPO, HKL, HKS, HKO, HCNO, etc.

• Refined Hydrogenatedeg. RHPO, RHPKO, RHCNO, RHKS, RHKL, etc.

• Fatty Acid Distillateeg. PFAD, PKFAD.

Oil Classification


• Free Fatty Acid (%)• Lovibon Color (R/Y)• Iodine Value (Wijs)• Moisture & Impurities (%)• Solid Fat Content (%)• Fatty Acid Composition (as FAMEs) • Cold Test (hrs)• Melting Point & Cloud Point (deg C)• Peroxide Value (meq/kg)• Odor (Organoleptic Test)

Oil Quality Analysis


Hydrogenation

R – CH = CH – CH3 R – H2 – CH2 – CH2 - COOH

H2

Pt / Ni

1. decreasing degree of unsaturated, where poly unsaturated turns to mono unsaturated whilst mono unsaturated becomes saturated

2. tends to solid forming

Breaking double bond replaced by hydrogen, in consequences ;


Types of Hydrogenation ;• fully hydrogenation ( IV ≤ 1 )• partial hydrogenation ( IV ≥ 1)

Hydrogenation cont.

Hydrogenation role in process of ;• Cocoa Butter Substitute• Cocoa Butter Replacer


SFC (%) = number of protons in solid state x 100

number of protons in solid & liquid state

Solid Fat Content

using NMR Spectrometer represent amount of fat on variable temperatures

PurposeDetermining on what temperatures oil solidify or liquidify


Solid Fat Content cont.

Methods

• TemperingApplied for cocoa butter equivalent, or exotic oil blend such as illipe butter and salstearin

• Non TemperingApplied for palm oil, palm kernel oil, fraction derived oil and oil blended product



Tempering procedures

1.apply sample in SFC vial at about 3-4 cm,2.heated to 70 deg C for 30 minutes,3.cooled to 0 deg C for 90 minutes,4.temper at 26 deg C for 40 hours,5.cooled to 0 deg C for 90 minutes,6.distribute to variable temperatures

10 ; 20 ; 25 ; 30 ; 35 ; 40 deg C, for 30 minutes,7.read the SFC using NMR.



Non Tempering procedures

1.apply sample in SFC vial at about 3-4 cm,2.heated to 70 deg C for 30 minutes,3.cooled to 0 deg C for 90 minutes,4.distribute to variable temperatures

10 ; 20 ; 25 ; 30 ; 35 ; 40 deg C for 30 minutes,5.read the SFC using NMR.


Fatty Acid Composition

using Gas Chromatography analysis, FAC of oil analyzed as Fatty Acid Methyl Ester (FAME) resulting peak perform with specific number, order, and intensity. These data is specific for each palmitic or lauric based oil which differentiate on the amount of each specific dominant fatty acids C16 and C12 respectively.

PurposeDetermining the composition of each fatty acids content on specific oil.


Procedures1. weigh sample 0.05 gram onto GC vial2. add 1 ml NaOH-methanolic 0.5 N3. add 1 ml BF3-methanolic (for crude only)4. heated on 70 deg C water bath for 10 minutes5. cooled in room temperature6. add saturated NaCl 0.5 ml7. add 2 ml n-hexane8. apply to GC with syringe

Fatty Acid Composition cont.


Variables contribute in resulting chromatogram;• instrument• column• gas flows• injection technique• recorderThings to concern about the chromatogram;• right number of the peaks• right order of the peaks• right relative sizes

Fatty Acid Composition cont.


Based on hypothesis that every oil & fat properties connected each other while palm kernel oil derivate is an essential part in edible oil industry, so the research undergo with kernel oil (which is lauric based) and it’s hydrogenated derivatives as objects;

Research

Refined RKO RKL RKS

# 1105 # 1104 # 1205

IV 17.61 IV 23.15 IV 6.24

Hydrogenated HRKO HRKL HRKS

# 1302 # 1306 # 1401

IV 0.44 IV 8.69 IV 0.05

Refined Hydrogenated RHKO RHKL RHKS

# 1604 # 1609 # 1601

IV 0.41 IV 8.39 IV 0.09


Chromatogram of RKO IV 17.61


Chromatogram of RKL IV 23.15


Chromatogram of RKS IV 6.24


Chromatogram of HRKO IV 0.44


Chromatogram of HRKL IV 8.69


Chromatogram of HRKS IV 0.05


Chromatogram of RHKO IV 0.41


Chromatogram of RHKL IV 8.39


Chromatogram of RHKS IV 0.09


Solid Fat Content (%) SFC RKO SFC RKL SFC RKS SFC HRKO SFC HRKL SFC HRKS SFC RHKO SFC RHKL SFC RHKS

Source 1105 1104 1205 1302 1306 1401 1604 1609 1601

IV 17,61 23,15 6,24 0,44 8,69 0,05 0,41 8,39 0,09

N 10 72,72 58,43 94,66 96,23 91,53 96,96 96,04 93,14 97,07

N 20 40,74 16,94 86,64 89,64 67,47 95,54 88,34 66,41 95,55

N 25 17,63 0,41 71,26 65,52 37,36 89,11 65,16 38,02 88,39

N 30 0,03 - 33,92 34,29 14,78 47,3 33,22 14,71 48,03

N 35 - - 0,21 12,45 5,68 2,4 12,23 5,44 2,19

N 40 - - - 5,71 0,4 - 5,54 0,96 0,23

Fatty Acid Comp (%) FAME RKO FAME RKL FAME RKS FAME HRKO FAME HRKL FAME HRKS FAME RHKO FAME RHKL FAME RHKS

C6:0 0,30 0,31 0,08 0,22 0,24 0,08 0,21 0,24 0,06

C8:0 3,50 4,29 1,85 3,42 3,85 1,86 3,25 3,93 1,80

C10:0 3,33 3,62 2,82 3,32 3,42 2,79 3,18 3,45 2,77

C12:0 46,59 43,08 55,62 46,77 41,82 55,18 46,39 41,95 55,26

C14:0 15,73 12,75 22,06 15,78 12,66 21,89 15,97 12,67 22,03

C16:0 8,81 8,33 8,68 8,59 8,75 8,80 8,67 8,78 8,75

C16:1 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00

C17:0 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00

C18:0 2,46 2,52 2,07 21,58 18,73 9,26 21,89 18,54 9,15

C18:1 tr 0,11 0,00 0,00 0,05 6,20 0,00 0,10 6,14 0,00

C18:1 cis 16,41 21,42 5,89 0,00 4,06 0,01 0,07 4,04 0,04

C18:2 tr 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00 0,00

C18:2 cis 2,52 3,37 0,81 0,00 0,00 0,00 0,00 0,00 0,00

C18:3 0,11 0,14 0,05 0,00 0,00 0,00 0,00 0,00 0,00

C20:0 0,12 0,13 0,07 0,23 0,23 0,13 0,24 0,22 0,13

C22:0 0,03 0,04 0,00 0,03 0,04 0,00 0,03 0,04 0,00

10 degC 96,21 95,39 98,07 96,36 95,91 98,06 96,54 95,84 98,14

% deviation 24,41439806 38,74839132 3,479293483 0,132776061 4,57003741 1,122486364 0,521266427 2,812767846 1,089297601


Lauric Palmitic

FAC RKO RKL RKS RPO ROL RPS

C 6:0 0.1 - 0.5 0.2 - 0.4 0 - 0.1

C 8:0 3.4 - 5.9 3.6 - 5.0 1.5 - 2.3

C 10:0 3.3 - 4.4 3.2 - 4.5 2.5 - 2.9

C 12:0 46.3 - 51.1 42.1 - 46.3 54.8 - 58.2 0.1 - 0.3 0.2 - 0.4 0.1 - 0.3

C 14:0 14.3 - 16.8 12.3 - 15.5 21.1 - 24.1 1.0 - 1.4 0.9 - 1.2 1.1 - 1.7

C 16:0 6.5 - 8.9 7.4 - 10.6 7.2 - 8.6 40.9 - 47.5 36.6 - 43.2 49.8 - 68.1

C 18:0 1.6 - 2.6 1.8 - 2.7 1.3 - 2.2 3.8 - 4.8 3.7 - 4.8 3.9 - 5.6

C 18:1 13.2 - 16.4 14.6 - 21.3 4.6 - 6.8 36.4 - 41.2 39.8 - 44.6 20.4 - 34.4

C 18:2 2.2 - 3.4 2.6 - 3.8 0.6 - 1.1 9.2 - 11.6 10.4 - 12.9 5.0 - 8.9

C 18:3 ND ND ND 0.1 - 0.6 0.1 - 0.5 0 - 0.5

C 20:0 ND 0 - 0.2 ND 0.2 - 0.7 0.3 - 0.5 0 - 0.5

FAC Ring Specification

SFC Control Limit for CKS Derivatives

Product Target N30 SFC

CKS 30 min

RKS 30 min

HKS 45 min

RHKS 46 min


SFC and FAC of Kernel Oil and Its Hydrogenated Derivatives

0

10

20

30

40

50

60

70

80

90

100

N 10 N 20 N 25 N 30 N 35 N 40

%

0.00

10.00

20.00

30.00

40.00

50.00

60.00

70.00

80.00

90.00

100.00

C6

:0

C8

:0

C1

0:0

C1

2:0

C1

4:0

C1

6:0

C1

6:1

C1

7:0

C1

8:0

C1

8:1tr

C1

8:1cis

C1

8:2tr

C1

8:2cis

C1

8:3

C2

0:0

C2

2:0

%

SFC RKO

SFC HRKO

SFC RHKO

FAME RKO

FAME HRKO

FAME RHKO


SFC and FAC of Kernel Olein and Its Hydrogenated Derivatives

0

10

20

30

40

50

60

70

80

90

100

N 10 N 20 N 25 N 30 N 35 N 40

%

0.00

10.00

20.00

30.00

40.00

50.00

60.00

70.00

80.00

90.00

100.00

C6

:0

C8

:0

C1

0:0

C1

2:0

C1

4:0

C1

6:0

C1

6:1

C1

7:0

C1

8:0

C1

8:1tr

C1

8:1cis

C1

8:2tr

C1

8:2cis

C1

8:3

C2

0:0

C2

2:0

%

SFC RKL

SFC HRKL

SFC RHKL

FAME RKL

FAME HRKL

FAME RHKL


SFC and FAC of Kernel Stearin and Its Hydrogenated Derivatives


Conclusion

In determining correlation between SFC and FAC data of oil and fat using lauric based oil as experiment object end up with unsatisfactorily unfinished complete conclusion. Yet still there’s a patron model that for oil with low IV value perform slight deviation compared both N10 value with sum of fatty acid content with melting point above 10 deg C.


Further Tasks

1. completing oil and fat properties data as a useful catalogue for production or product development purposes,

2. dig more insight to each oil and fat properties that contributes to or influence other, since that every analysis is numerous and routine so whether for efficiency and practical reason, it is beneficial.

In order to get a complete information of oil and fat properties which is very important when dealing with customer specification and the capabilities of production, so we need to do;

hydrogenation .ppt; basestock and process control

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