c180-e062 simulated distillation gc analysis system

7/27/2019 C180-E062 Simulated Distillation GC Analysis System

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C180-E0

Shimadzu Simulated DistillationGC Analysis System



¡¡Total area method and internal standard method

are available.¡¡The distillation curve can be displayed as a graph

and printed.¡¡Baseline correction.¡¡Automatic calibration correction.

By setting the identification retention time range,

the identification table is automatically updated, so

long as the retention time is within that range.¡¡The fraction at a specific temperature range can

be calculated.

The fraction ratio for a certain range can be easily

obtained since the elution amount (%) at a specific

temperature range that has been designated can

be calculated.

¡¡Convert into ASTM D-86, D-1160.

D-86 is applied to kerosene and light oil, while D-

1160 is applied to samples which require reduced-

pressure distillation, such as lubricating oil.¡¡Automatic end-point detection

Automatic end-point detection is useful for the

samples containing components with high boiling

points.¡¡Typical batch templates have been prepared.¡¡Typical method files have been prepared.¡¡Analysis and post run analysis employ the same

operations used in the GCsolution. Since the

batch table option is used, analysis and post run

analysis can be operated using the same

operations employed in the GCsolution.

Features of the Simulated Distillation GC Software

2

Shimadzu Simulated Distillation GC Analysis System



This is a method of measuring the boiling point distributionof oil fractions using gas chromatography.

This technique is commonly called Simulated DistillationGas Chromatography, as the measurement resultsobtained are similar to those obtained with the conven-tional distillation method.

(1) Measurement of Boiling Point Distribution using theTotal Area Method

When a linear temperature programming method is applied tothe analysis using a gas chromatograph with a non-polar liquidphase column, the hydrocarbons will be eluted in the order of boiling point. Since the elution time is more or less directlyproportional to the boiling point, a calibration curve of theretention time and boiling point can be created, as shown inFig.1.1. In other words, the retention time can be converted into

the boiling point.Therefore, by working out the relationship between the retentiontime and the boiling point beforehand through the analysis of ahydrocarbon mixture with a known boiling point (with the gaschromatograph analysis conditions kept constant), it becomespossible to convert the retention time of an unknown sampleinto the boiling point.Furthermore, the total area of the gas chromatogram obtained isdivided into fixed time intervals, and the smaller areascomprised by each time period are calculated. Since the timeinterval can be converted into the boiling point interval, this ineffect calculates the gas chromatogram area for the fraction of aparticular boiling point.In addition, by obtaining the cumulative area through theaddition of all the small areas from the start point onwards, andexpressing it as a ratio of the area of the entire gaschromatogram, the elution amount up to that time will have beencalculated. In Fig.1.2 for example, the cumulative area up to ‘n’consists of ‘S1’, ‘S2’, ‘Sn-1’, ‘Sn’. By figuring out the ratio withrespect to the total area ‘St’, the elution amount at ‘tn’ isobtained. The data in Fig.1.3 is an example of the elutionamount (corresponds to the amount of distillate).This method is applied to samples where all the components of the sample are eluted from the column during high temperatureanalysis using GC, such as the oil fractions of gasoline,kerosene, and light oil.

(2) Measurement of Boiling Point Distribution using theInternal Standard Method

When analyzing samples containing components with boiling

points higher than 1000°F (538°C), such as lubricating oil andcrude oil, all of the components will not be eluted from thecolumn during high temperature analysis. Therefore, the totalamount of components cannot be obtained and the elutionamount cannot be calculated.To overcome this, a known quantity of an internal standardsubstance is added. Using the fact that it will be equivalent tothe ratio of this internal standard substance to the sampleamount, the area for all components, including those which arenot eluted from the column, can be obtained by calculation.From this, the relationship between the amount of sample elutedand the boiling point is sought out in the same way as (1).

Fig.1.1 Calibration Curve

Total area

Fig.1.2 Calculating the elution amount

E l u t i o n t e m p e r a t u r e

Elution amount

Fig.1.3 Distillation characteristics curve

Simulated Distillation GC Analysis System

B o i l i n g p o i n t

Retention time

Overview of SimulatedDistillation GC Analysis



Samples with boiling points below 538°C are measuredusing the total area method. The chromatogram is divided

into fixed time intervals, and the distillation characteristicsare calculated based on this data. The maximum numberof data that can be collected is 5000. The scale on thetemperature axis of the graph changes automaticallywithin a range of 0 to 900°C. The printing sections(distillate amount %) within the table can be set from 1 to99. Up to 10 sections of specific temperature rangefractions can be calculated.

Single Method

When a sample containing components which do not elute areanalyzed using the gas chromatograph, a known component isadded to correct for the area of the component which is noteluted. By multiplying the area/ component amount ratio withthe sample amount, the total area of the sample is calculated.The difference between this value and the area that was actuallyobtained is taken to be the area of the components which did notelute.In the single method, the unknown area is calculated by addingthe standard sample (known sample) to the unknown sample.

The boiling point range of the internal standard component canbe set freely.

Double Method

Unlike the single method described on the left, a sample towhich the known component (internal standard) is added and asample without the known component is analyzed in succession.The area of the components of this difference between the two iscalculated.The boiling point range of the internal standard component canbe set freely.

There are two internal standard methods: the single method and the double method.

The single method is used in cases where the standard sample and the unknown sample do not overlap, whereas the

double method is used when samples which overlap with the standard sample are analyzed.

T = B + B' = (AIS XA —

AIS

BIS) XB — BIS S

T : Theoretical total areaA : Area of the part below 538°C for the sample to which

the internal standard has been addedB : Area of the part below 538°C for the sample without the

internal standardAIS : Area of the internal standard substance distillate section

for the sample to which the internal standard has beenadded

BIS : Area of the section corresponding to the internalstandard substance distillate for the sample without theinternal standard

S : Sample amountI : Amount of internal standard addedA’, B’ : Area corresponding to the components which are not

distilled from within the sample

Chromatogram for a sample to whichthe internal standard has been added

Chromatogram of the sample only

1000ßF(538°C)

A'

1000ßF(538°C)

B'

AIS

S

A

S

B

BIS

I - IBP I - FBPMAX - BP

I —

Estimation of the surface area using the internal standard method

Internal Standard Method


4

Total Area Method



Simulated Distillation GC Software

Initial Settings

Since the screens have been made to match the GCsolution,settings can be made using the same operations.The initial settings are comprised of settings for calibration,parameters, and reports.

Analysis/Post run analysis

As it uses the batch processing of GCsolution, the operation isthe same as the GCsolution.

Distillation Characteristics Calculation Results

After analysis/ Post run analysis, a report on the distillationcharacteristics calculation results is printed out automatically.The results can be checked on the screen as well.

Printout Example

Refer to the application examples on the next page.

Simulated Distillation GCSoftware



Simulated Distillation GC Software

A n a l y s i s D a t e & T i m e : 3 / 8 / 2 0 0 1 6 : 3 1 : 3 8 P M

U s e r N a m e : w a d a

V i a l # : 1

S a m p l e N a m e : U n k n o w n S a m p l e

S a m p l e I D :

S a m p l e T y p e : U n k n o w n

I n j e c t i o n V o l u m e : 0 . 3

I S T D A m o u n t :

D a t a N a m e : F : \ E _ D G C \ D e m o F i l e \ T o t a l A r e a \ D i e s e l \ D i e s e l 1 . g c d

M e t h o d N a m e : F : \ E _ D G C \ D e m o F i l e \ T o t a l A r e a \ D i e s e l \ D i e s e l 1 . g c m

m in

I n t e n s i t y

1 0

5 0 0 0 0 0 0

1 0 0 0 0 0 0 0

1 5 0 0 0 0 0 0

/

7

.

3

4

1

P e a k # R e t . T i m e A r e a H e i g h t C o n c . U n i t M a r k I D # C m p d N a m e

1 7 . 3 4 1 5 4 4 0 4 9 6 0 8 2 8 4 2 9 7 1 2 1 0 0 . 0 0 0

T o t a l 5 4 4 0 4 9 6 0 8 2 T o t a l 8 4 2 9 7 1 2

* * * * B O I L I N G R A N G E D I S T R I B U T I O N * * * *

S A M P L E N A M E : U n k n o w n S a m p l e

S A M P L E I D :

S A M P L E T Y P E : U N K N O W N

A N A L Y S I S T I M E : 2 0 0 1 / 0 3 / 0 8 1 8 : 3 1 : 3 8

T O T A L A R E A : T O T A L A R E A

O U T P U T F I L E : F : \ G C s o lu t i o n \ d g c 1 \ d a t a \ D i e s e l 1 . d a t

C A L I B R A T I O N F I L E : F : \ G C s o l u t i o n \ d g c 1 \ C a l i b \ D i e s e l 1 . c l b

P A R A M E T E R D A T A F I L E : F : \ G C s o l u t i o n \ d g c 1 \ P A R M \ D i e s e l 1 . p a r

R E P O R T D A T A F I L E : F : \ G C s o l u t i o n \ d g c 1 \ P A R M \ D i e s e l 1 . r e p

A S T M D - 8 6

% O F F B P B P

( % ) ( C ) ( F )

I B P 1 7 6 . 0 3 4 8 . 8

1 0 2 0 9 . 2 4 0 8 . 6

2 0 2 3 8 . 3 4 6 0 . 9

3 0 2 5 8 . 9 4 9 8 . 0

5 0 2 9 3 . 0 5 5 9 . 4

7 0 3 1 5 . 1 5 9 9 . 2

8 0 3 2 9 . 4 6 2 4 . 9

9 0 3 4 6 . 2 6 5 5 . 1

F B P 3 6 9 . 8 6 9 7 . 6

V A B P - - - - - 5 4 4 .0 5 1 ( F )

A n a l y s i s D a t e & T i m e : 3 / 1 5 / 2 0 0 1 1 1 : 4 1 : 0 1 P M

U s e r N a m e : A d m i n

V i a l # : 1

S a m p l e N a m e : S a m p l e + I S

S a m p l e I D : U l t r a A L L O Y - S I M

S a m p l e T y p e : U n k n o w n

I n j e c t i o n V o l u m e : 1 .0

I S T D A m o u n t :

D a t a N a m e : F : \ E _ D G C \ D e m o F i l e \ I S \ S g l \ E n g i n e O i l + I S . g c d

M e t h o d N a m e : F : \ E _ D G C \ D e m o F i l e \ I S \ S g l \ E n g i n e O i l . g c m

m in

I n t e n s i t y

1 0 2 0 3 0

5 0 0 0 0

1 0 0 0 0 0

1 5 0 0 0 0

2 0 0 0 0 0

2 5 0 0 0 0

3 0 0 0 0 0

3 5 0 0 0 0

4 0 0 0 0 0

4 5 0 0 0 0

5 0 0 0 0 0

5 5 0 0 0 0

6 0 0 0 0 0

6 5 0 0 0 0

7 0 0 0 0 0

7 5 0 0 0 0

8 0 0 0 0 0

8 5 0 0 0 0

9 0 0 0 0 0

9 5 0 0 0 0

1 0 0 0 0 0 0

1 0 5 0 0 0 0

1 1 0 0 0 0 0

1 1 5 0 0 0 0

1 2 0 0 0 0 0

1 2 5 0 0 0 0

1 3 0 0 0 0 0

1 3 5 0 0 0 0

1 4 0 0 0 0 0

1 4 5 0 0 0 0

1 5 0 0 0 0 0

1 5 5 0 0 0 0

1 6 0 0 0 0 0

1 6 5 0 0 0 0

1 7 0 0 0 0 0

1 7 5 0 0 0 0

1 8 0 0 0 0 0

1 8 5 0 0 0 0

1 9 0 0 0 0 0

1 9 5 0 0 0 0

/

1

5

.

0

0

0

* * * * B O I L I N G R A N G E D I S T R I B U T I O N * * * *

S A M P L E N A M E : S a m p l e + I S

S A M P L E I D : U l t r a A L L O Y - S I M

S A M P L E T Y P E : U N K N O W N

A N A L Y S I S T I M E : 0 2 0 0 / 0 3 / 1 5 1 1 1 : 4 1 : 0 1 P M

T O T A L A R E A : I N T E R N A L S T A N D A R D ( S I N G L E )

S A M P L E W E I G H T : 1 0

I S W E I G H T : 1

O U T P U T F I L E : F : \ G C s o l u t i o n \ d g c 1 \ d a t a \ E n g i n e O i l + I S . d a t

C A L I B R A T I O N F I L E : f : \ G C s o l u t i o n \ d g c 1 \ C a l i b \ E n g i n e O i l . C L B

P A R A M E T E R D A T A F I L E : f : \ G C s o l u t i o n \ d g c 1 \ P A R M \ E n g i n e O i l _ S . P A R

R E P O R T D A T A F I L E : f : \ G C s o l u t i o n \ d g c 1 \ P A R M \ E n g i n e O i l . R E P

D i s t i l l a t i o n D a t a i n S p e c i f i e d T e m p e r a t u r e R a n g e

I B P F B P %

( C ) ( C )

2 0 0 . 0 3 0 0 . 0 0 . 0

3 0 0 . 0 3 5 0 . 0 1 . 8

3 5 0 . 0 4 0 0 . 0 1 7 . 8

4 0 0 . 0 4 8 0 . 0 6 5 . 4

Engine oil sample

Initial Settings

6

Application Examples




System Configuration Example (for 1ch)

• Automatic modification of the retention time – boilingpoint calibration curve through standard sampleanalysis.

• Re-calculation upon changing the boiling pointcalibration curve is possible.

• 5 graphs of the distillation characteristics curve and theboiling point calibration curve can be created.

• Conversion into ASTM D-86, D-1160

• Automatic end-point detection (for the total area methodonly)

Initial Settings

Specifications

No. of input channels 2

Data collection interval Depends on each GC

No. of data collectedMax. 5000

Baseline correction Uses the function of the GCsolution

Retention time – boiling point conversion Multi-linear calibration

Area – volume % conversion Available

Internal standard method The boiling point range can be set as desired

Specific temperature range fraction 10 sections

Gas chromatograph Shimadzu GC-14BPF Gas Chromatograph P/N 221-41674-**CRG-15 Cryogenic option P/N 221-25347-94

(required when an initial column temperature is10°C less than room temperature as)

Solenoid valve unit for the L-CO2 (required when using the CRG)P/N 221-25347-94 P/N 221-43846-**Data processor CBM-102 P/N 223-04860-**

Optical link transmission unit for the GC-14B P/N 221-42171-91

GCsolution workstation P/N 223-05430-92

GCsolution reference manual P/N 223-00568

Software (GCsolution Ver2.0 or higher)

Simulated Distillation GC software P/N 221-57807-92

Column 0V-1 5% Chromosorb W60/80 1m (2 columns 1 set)

For the Capillary Column

Gas chromatograph GC-2010AF Gas Chromatograph P/N 221-47700-**Wide bore injection unit WBI-2010 or P/N 221-47726-**OCI/PTV-2010 P/N 221-49213-**CRG-2010 CO2 100V Cryogenic option P/N 221-48703-**(required when an initial column temperature is less than room temperature +10°C)

Solenoid valve unit for the L-CO2 (required when using the CRG) P/N 221-43846-**Data processor GCsolution workstation P/N 223-05430-92

GCsolution reference manual P/N 223-00568

Software (GCsolution Ver2.0 or higher)

Simulated Distillation GC software P/N 221-57807-92

Example of columns For kerosene: CBP1-W12-500 (Non polar, 0.53mmI.D., 12m, 5mm)

For light oil: CBP1-W12-100 (Non polar, 0.53mmI.D., 12m, 5mm)

Note 1) The column type, size and film thickness are important performance factors.Note 2) When the separation characteristics etc. of the capillary column and packed column differ, different

measurement results may be obtained.

Standard sample For kerosene: n-C6, 7, 8, 9, 10, 12, 14, 16, 18 in CS2 P/N 221-44247-17

For light oil: n-C6, 7, 8, 10, 12, 14, 16, 18, 20, 22, 24 in CS2 P/N 221-44247-18

Mixed samples: n-C8, 10, 12, 16, 20, 24, 28, 30, 32, 36, 40, 44 in C6 P/N 221-44247-19



SHIMADZU CORPORATION. International Marketing Division

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Cable Add.:SHIMADZU TOKYO

SHIMADZU SCIENTIFIC INSTRUMENTS, INC.

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Phone: 1(410)381-1227 Fax. 1(410)381-1222 Toll Free: 1(800)477-1227

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Phone: 61(2)9684-4200 Fax. 61(2)9684-4055

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Phone: (55)11-3611-1688 Fax. (55)11-3611-2209

SHIMADZU (HONG KONG) LIMITED

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Overseas Offices

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URL http://www.shimadzu.com

The contents of this brochure are subject to change without notice.Printed in Japan 3295-11211-10ATD

c180-e062 simulated distillation gc analysis system

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