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Chemicals Identification Related To The Chemical Weapons Convention During The 15th Interlabory Proficiency Test Sri Sumartini; Harry Budiman; Nuryatini Nuryatini; Puspa Dewi
Jurnal ILMU DASAR Vol 9 No 1 (2008)
Publisher : Fakultas Matematika dan Ilmu Pengetahuan Alam Universitas Jember

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (436.476 KB)

Abstract

Identification of some chemical weapons in the water and organic sample has been carried out during 15th proficiency testing hold by OPCW (Organisation Prohibition of Chemical Weapon). Sample preparation method was adopted from Recommended Operational Procedure (ROP) from OPCW and Helsinki University, Finlandia. Prepared sample was identified by gas chromatography (FID and FPD), gas chromatography mass spectrometry (EI and CI mode) and Liquid chromatography mass spectrometry method.. From 7 spiking chemical weapons introduced to water and organic sample, 3 spiking chemicals could be identified (propylphosphonic acid, isoprophylphosphonic acid and 1,4 Bis 2-chloroethyl (thio) butane). One chemical was reported as Butyl S-2-diisopropylaminoethyl propylphosphonothiolate but obviously this is not a spiking chemical (category false positive identification).
SIMULTANEOUS MEASUREMENT OF SYN-GAS COMPONENT (H2, CO2, CH4, AND CO) AS PRODUCT OF BIOMASS GASIFICATION BY USING VALIDATED GC-TCD METHOD Muhammad Rizky Mulyana; Oman Zuas; Harry Budiman; Sabar Simanungkalit; Nino Rinaldi
Scientific Contributions Oil and Gas Vol. 41 No. 1 (2018): SCOG
Publisher : Testing Center for Oil and Gas LEMIGAS

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.29017/scog.41.1.298

Abstract

Biomass gasification has been widely known method to produce syn-gases, which can be considered as great alternative substitution for fossil fuels. However, accurate verification of the syn-gas composition requires a reliable and validated method for simultaneous measurement of H2, CO2, CH4, and CO. In order to fulfill the aforementioned requirements, which is the objective of this study; a GC-TCD method for simultaneous measurement of H2, CO2, CH4, and CO component in syn-gas has been validated in accordance to ISO/IEC 17025 and its application for real samples. For the method validation purpose, all of the performance parameters were evaluated and discussed in detail in this study. Intraday precision and interday precision were found to be acceptable having the %RSD below 0.67xCV Horwitz and below 1.0xCV Horwitz, respectively. The bias value falls within +2? for entire components, indicating that the method accuracy can be accepted. Coefficient correlation for all components was higher than 0.99, which means that the method has suffi cient linearity. LoD and LoQ for each component were found to be lower than typical syn-gas concentration range. The method roughness was also found in an acceptable level (the p-values was higher than 0.05 for allctarget components. Application of the validated method for the measurement of a real syn-gas samples indicated that the method is quite reliable to produce an accurate data and the validated methid can be used in a routine analysis. The innovation of this study, as shown by experiment results, is to evaluate the validated methods performance for simultaneous determination of syn-gas components concentration in one channel, compared to common method in which the syn-gas components were measured separatedly in a different channel. Biomass gasifi cation has been widely known method to produce syn-gases, which can be consideredas great alternative substitution for fossil fuels. However, accurate verifi cation of the syn-gas compositionrequires a reliable and validated method for simultaneous measurement of H2, CO2, CH4, and CO. Inorder to fulfi ll the aforementioned requirements, which is the objective of this study; a GC-TCD methodfor simultaneous measurement of H2, CO2, CH4, and CO component in syn-gas has been validated inaccordance to ISO/IEC 17025 and its application for real samples. For the method validation purpose,all of the performance parameters were evaluated and discussed in detail in this study. Intraday precisionand interday precision were found to be acceptable having the %RSD below 0.67xCV Horwitz and below1.0xCV Horwitz, respectively. The bias value falls within +2? for entire components, indicating that themethod accuracy can be accepted. Coeffi cient correlation for all components was higher than 0.99, whichmeans that the method has suffi cient linearity. LoD and LoQ for each component were found to be lowerthan typical syn-gas concentration range. The method roughness was also found in an acceptable level(the p-values was higher than 0.05 for allctarget components. Application of the validated method for themeasurement of a real syn-gas samples indicated that the method is quite reliable to produce an accuratedata and the validated methid can be used in a routine analysis. The innovation of this study, as shown byexperiment results, is to evaluate the validated methods performance for simultaneous determination ofsyn-gas components concentration in one channel, compared to common method in which the syn-gascomponents were measured separatedly in a different channel.Keywords: syn-gas, GC-TCD, method validation.
Analisis senjata kimia melalui uji profisiensi organisation prohibition of chemical weapon (OPCW) Evita Boes; Dyah Styarini; Nuryatini Nuryatini; Harry Budiman
JURNAL STANDARDISASI Vol 11, No 1 (2009): Vol. 11(1) 2009
Publisher : Badan Standardisasi Nasional

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.31153/js.v11i1.12

Abstract

Identification of some chemicals weapons in the water and organic sample has been carried out during 21th proficiency testing conducted by OPCW (Organisation Prohibition of Chemical Weapon). The samples were prepared and analysed in accordance with the principles describe in the work instructions for the preparation of test samples for OPCW proficiency test. The extract of samples were analysed and identified by GC-EI-MS, GCCI-MS, GC-FPD, GC-NPD and LC-MS. From 7 spiking chemical weapons introduced to water and organic sample, 3 spiking chemicals could be identified such as Bis(2,4,4 trimethylpentyl)methylphosphonate, 2-(N-Ethyl-N-isoprophylamino)etanol and Bis(2-diisoprophylaminoethyl)disulfide.
KETIDAKPASTIAN PENGUKURAN: EVALUASI, SUMBER-SUMBER DAN KONTRIBUSINYA DALAM PEMBUATAN BAHAN ACUAN CAMPURAN GAS (N2O DALAM MATRIKS N2) SECARA GRAVIMETRI Muhammad Rizky Mulyana; Harry Budiman; Oman Zuas; Nur Tjahyo Eka Darmayanti
JURNAL STANDARDISASI Vol 20, No 1 (2018)
Publisher : Badan Standardisasi Nasional

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.31153/js.v20i1.599

Abstract

Gas dinitrogen monoksida (N2O) merupakan salah satu komponen gas rumah kaca dengan konsentrasi atmosferik yang terus meningkat setiap tahun, sehingga dibutuhkan upaya mitigasi yang didukung dengan metode pengukuran yang tervalidasi. Berdasarkan ISO/IEC 17025, metode pengukuran harus divalidasi unjuk kerjanya menggunakan bahan acuan yang memenuhi persyaratan, salah satunya yaitu memiliki nilai konsentrasi yang tersertifikasi beserta ketidakpastiannya. Di Indonesia, beberapa perusahaan gas specialty telah memulai upaya memproduksi bahan acuan gas sendiri untuk memenuhi kebutuhan dalam negeri. Untuk mendukung upaya tersebut, dalam studi ini akan dibahas secara rinci sumber-sumber ketidakpastian bahan acuan gas N2O dan kontribusi dari masing-masing sumber, hingga diperoleh nilai ketidakpastian akhir melalui prosedur estimasi yang akurat dan dapat diterima secara internasional berdasarkan ISO 6142. Nilai ketidakpastian diestimasi berdasarkan eksperimen aktual pembuatan 5 buah bahan acuan gas N2O dengan konsentrasi yang berbeda secara gravimetrik. Hasil ketidakpastian akhir untuk bahan acuan gas AH06018, AH06023, AH06021, AH06010, AH06020 berturut – turut adalah 2.528%, 3.490%, 4.215%, 4.785%, 5.292%. Adapun sumber ketidakpastian terbesar berasal dari fraksi mol komponen dalam parent gas, yang kontribusinya meningkat seiring bertambahnya pengenceran. Sementara itu, kontribusi ketidakpastian dari massa gas yang ditransfer mengalami penurunan dengan semakin rendahnya konsentrasi N2O. Berdasarkan hasil tersebut, disimpulkan bahwa nilai ketidakpastian konsentrasi bahan acuan meningkat seiring bertambahnya pengenceran, dan sumber ketidakpastian yang memberikan kontribusi terbesar adalah fraksi mol komponen dalam parent gas. Diharapkan hasil studi ini dapat menjadi acuan bagi produsen bahan acuan gas lokal dalam mengestimasi ketidakpastian secara tepat, serta meminimalkan kontribusi sumber-sumber ketidakpastian yang telah dibahas secara rinci.