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QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

Rania Fardyani 08.54.06287 SMK SMAK Bogor

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

Institution Profile

Phthalate

Gas Chromatography

Mass Spectrometer

Control Chart

Analytical Method

Result Discussion

Conclusion

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

INSTITUTION PROFILE PT SUCOFINDO (Persero) Values The Company Scopes Laboratories

Instrument Laboratory

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

PHTHALATE

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

GAS CHROMATOGRAPHY
History

1910
Mikhail S. Tswett

1930
Schuftan and Eucken

1941
Martin and Synge

1952
Gas Chromatography

1955
PerkinElmer

1959
GOW-MAC

1973
HawlettPackard (HP)

2007
Agilent Technologies

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

GAS CHROMATOGRAPHY
Main Definition
Gas Chromatography is a separating method by using Sample for GC liquid as stationary phase and gas as mobile pha of This method can analyze gases, of Good Factorsse. Separating Process and Indicationvolatile compounds, or easy to be volatilized.

Separation

The Advantages of GC
The Disadvantages of GC

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

GAS CHROMATOGRAPHY
Basic Principal

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

GAS CHROMATOGRAPHY
Instrumentation

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

GAS CHROMATOGRAPHY
Carrier Gas

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

GAS CHROMATOGRAPHY
Sample Injection

Direct Injection

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

GAS CHROMATOGRAPHY
Sample Injection

Split Injection

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

GAS CHROMATOGRAPHY
Sample Injection

Splitless Injection

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

GAS CHROMATOGRAPHY
Sample Injection

On Column Injection

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

GAS CHROMATOGRAPHY
Oven

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

GAS CHROMATOGRAPHY
Oven
Isothermal Temperature Programming

Low Temp.

High Temp.

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

GAS CHROMATOGRAPHY
Column

Packed Column

Capillary Column

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

GAS CHROMATOGRAPHY
Detector
An electronic sensor to convert the signal of carrier gas and the components within it into electronic signals.

MASS SPECTROMETER

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

MASS SPECTROMETER

-- - Ion Source

sample

+ + + ++ + ++

Quadropole Mass Analyzer

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

CONTROL CHART
Statistical Process Control
A powerful problem-solving tools and useful in achieving process stability and improving capability through the reduction of variability. Histogram Check Sheet Pareto Chart Cause and Effect Diagram Defect Concentration Diagram Scatter Diagram

Control Chart

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

CONTROL CHART
Control Chart
A graphical design of a quality characteristic that has been measured from a sample versus the sample number or time.

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

CONTROL CHART
The Function of Control Chart IMPROVE THE PROCESS
Input

Process Measurement System


Verify and follow up

Output

Detect assignable cause

Implement corrective action

Identify root cause of problem

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

ANALYTICAL METHOD

A1 A2 A3 A4 (BBP, DBP, DEHP, DIBP, DINP)

Vial 2 mL

GC/MS

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

RESULT | DISCUSSION
Phthalate Standards : 1. Diisobutyl Phthalate 2. Dibutyl Phthalate 3. Benzyl Butyl Phthalate 4. Di (2-ethylhexyl) Phthalate 5. Diisononyl Phthalate Start Date : January 2, 2012 End Date : January 12, 2012

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

RESULT | DISCUSSION
PARAMETER CASNUMBER STANDARD A-1 A-2 A-3 A-4 A-1 A-2 A-3 A-4 A-1 A-2 A-3 A-4 A-1 A-2 A-3 A-4 A-1 A-2 A-3 A-4 CONCENTRATION (ppm) 2.394 4.787 11.968 23.936 1.998 3.996 9.990 19.976 2.319 4.639 11.600 23.194 2.308 4.617 11.540 23.084 20.056 40.112 100.280 200.560 AVERAGE A STD/A ISTD 0.6518 1.4317 4.0382 8.4110 0.0564 0.1039 0.2853 0.6179 0.3115 0.7478 2.1429 4.8262 0.3382 0.8291 0.3726 5.5787 2.1688 5.3151 15.6758 40.1682 UCL 0.6978 1.5325 4.2832 8.9353 0.0700 0.1167 0.3120 0.6504 0.4140 0.8294 2.5221 5.3746 0.3984 0.9126 2.4775 6.1701 2.9409 6.6765 16.6987 43.6265 LCL 0.6058 1.3309 3.7932 7.8867 0.0428 0.0912 0.2587 0.5854 0.2089 0.6662 1.7639 4.2779 0.2780 0.7456 2.2677 4.9873 1.3967 3.9536 14.6530 36.7098 MAX 0.6737 1.4850 4.1099 8.5794 0.0623 0.1087 0.2964 0.6366 0.3744 0.7916 2.4189 5.1656 0.3672 0.8632 2.4204 5.8061 2.4684 5.9787 16.2198 41.2930 MIN 0.6384 1.3918 3.9064 8.1178 0.0490 0.0970 0.2695 0.6053 0.2720 0.7140 2.0403 4.5749 0.3112 0.7954 2.3099 5.1803 1.7021 4.7935 15.3427 37.9405 %RSD 2.35% 2.35% 2.02% 2.08% 8.02% 4.09% 3.11% 1.75% 10.98% 3.64% 5.90% 3.79% 5.94% 3.36% 1.47% 3.53% 11.87% 8.54% 2.17% 2.87%

Diisobutyl Phthalate

84-69-5

Dibutyl Phthalate

84-74-2

Benzyl Butyl Phthalate

85-68-7

Di (2-ethylhexyl) Phthalate

117-81-7

Diisononyl Phthalate

28553-12-0

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

RESULT | DISCUSSION
Parameter Inject 1 Inject 2 Inject 3 Inject 4 Inject 5 Inject 6 Inject 7 DIBP 0.9999 0.9999 0.9997 0.9998 0.9999 0.9989 0.9999 DBP 1.0000 0.9999 0.9999 0.9998 0.9987 0.9991 1.0000 BBP 0.9999 0.9997 1.0000 0.9999 0.9997 0.9999 0.9999 DEHP 1.0000 0.9998 0.9998 0.9994 0.9999 0.9972 0.9997 DNIP 1.0000 1.0000 0.9994 0.9996 1.0000 0.9996 0.9996 Parameter Inject 1 DIBP 0.9927 0.9893 0.9934 0.9876 0.9817 0.9777 0.9753 DBP 0.9899 0.9861 0.9895 0.9811 0.9772 0.9731 0.9691 BBP 0.9905 0.9856 0.9906 0.9843 0.9843 0.9746 0.9707 DEHP 0.9897 0.9841 0.9891 0.9829 0.9818 0.9725 0.9690 DNIP 0.9881 0.9816 0.9858 0.9818 0.9753 0.9697 0.9645

The Correlation of Standard Concentration to A STD/A ISTD

The Correlation of Standard Concentration to A STD

Inject 2 Inject 3 Inject 4 Inject 5 Inject 6 Inject 7

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

CONCLUSION
Based on the calculation, it can be concluded that the performance of GC/MS Agilent 5975 Series is still in good condition and the addition of internal standards is important in phthalate analysis by the method of GC / MS.

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

SUGGESTION
The maintenance needs to be done regularly to achieve the optimum conditions, such as cleaning the ion source, checking the vacuum pressure, interface, and column. Limit of Quantitation (LoQ) and Limit of Detection (LoD) of the instrument needs to be verified again so that the reading process of the analyte is stable and under control.

QUALITY CONTROL PERFORMANCE FOR PHTHALATE ANALYSIS BY GAS CHROMATOGRAPHY MASS SPECTRA

THANK YOU

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