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PREPARASI CONTOH UJI PROFISIENSI UNTUK IDENTIFIKASI SENYAWA KIMIA BERBAHAYA Evita Boes
Jurnal Kimia Terapan Indonesia Vol 17, No 1 (2015)
Publisher : Research Center for Chemistry - LIPI

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (620.877 KB) | DOI: 10.14203/jkti.v17i1.23

Abstract

The sample of proficiency test for hazard chemical compounds in organic and water sample has been made to identify hazard chemical compounds. Here, various matrix was added to these hazard chemical compound. The organic sample derived from organic waste added with dichloromethane as the solvent, undecane 100 µl/mL, 1,2-dimethylbenzene 12 µl/mL, diesel  100 µl/mL and tributhyl phosphate 10,02 µg/mL, whereas water sample derived from  water waste added with magnesium sulfate heptahydrate 120 µg/mL, sodium carbonate anhydrous 106 µg/mL, sodium sulfate anhydrous 284 µg/mL, calsium chloride  dyhidrate 222 µg/mL, dikhloromethane 2,5 µl/mL, polyethylene glycol 505,4 µg/mL, 3,5 dihydroxytoluene 10,05 µg/mL and α methyl-α-propyl succinimide 10,01 µg/mL. Hazard chemical compounds  that being added are Bis (3-methylbutyl) ethylphosphonate 10,04±0,31 µg/mL, Bis (2-chloroethyl) methylamine  20,59±0,14 µg/mL for organic sample and Pinacolyl methylphosphonate 9,80±0,18 µg/mL and Triethanolamine 14,84±0,10 µg/mL for water sample.  Homogeneity and stability are determined quantitatively using  GC-FPD (P-mode) and GC-FID with calibration curve using internal standard dibuty butylphosphonate, 2,6-dimethylphenol, dibutylphosphate and Bis (2-hydroxypropyl) aminoethanol with Relative Standard Deviation (RSD)  8,10 % and 12,40 µg/mL for Bis (3-methylbutyl) ethylphosphonate and 3,46 % and 14,19 µg/mL for Bis (2-chloroethyl) methylamine and 2,22 % and 11,28 µg/mL for Pinacolyl methylphosphonate and 2,70 % and 11,47 µg/mL for Triethanolamine.  Relative Standard Deviation is a homogeneity value with requirements below 20 % and stability is a degradation result which value is less than 30 %.Keywords: hazard chemical compounds, proficiency test, homogeneity, stability, relative standard deviation
PENGGUNAAN EKSTRAKSI FASA PADAT UNTUK ANALISIS TETRASIKLIN DALAM CONTOH UDANG Evita Boes; Julia Kantasubrata; A. T. Karossi
Jurnal Kimia Terapan Indonesia Vol 3, No 2 (1993)
Publisher : Research Center for Chemistry - LIPI

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (3628.598 KB) | DOI: 10.14203/jkti.v3i2.275

Abstract

A great quantity of Indonesian frozen prawns were exported to Japan and America. Unfortunately these products have often been rejected due to their content of tetracycline derivative residues. Qualitative analysis of frozen prawn samples being exported by means of HPLC, indicated that they are contaminated by oxytetracycline and tetracycline residues. A problem of quantitative analysis of such residues could be due to several peaks of the matrix being eluted closely to the peaks of the tetracycline derivatives. An experiment was carried out to eliminate the peaks of the matrix origin using SPE (Solid Phase Extraction) in order to quantify the derivatives more accurately. Application of SPE in the sample pretreatment is useful not only for separating the solute being analyzed from the matrixs, but also for concentrating the tetracycline derivatives of the extract. The recovery of SPE column elution process was about 90% and the SPE octadecyl (1 ml) column capacity for oxytetracycline, tetracycline, demeclocycline and doxycycline i.e. 2.4-7.9 ug; 3.5-11.8 ug; 3.4-11.2 ug and 17.3-57.5 ug respectively.
ANALISIS, IDENTIFIKASI PRECURSOR DAN HASIL DEGRADASI SENYAWA SENJATA KIMIA MENGGUNAKAN TEKNIK GAS CHROMATOGRAPHY MASS SPECTROMETRY– ELECTRON IONISASI (GCMS-EI) Evita Boes
Jurnal Kimia Terapan Indonesia Vol 16, No 1 (2014)
Publisher : Research Center for Chemistry - LIPI

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (2375.902 KB) | DOI: 10.14203/jkti.v16i1.8

Abstract

Telah dilakukan analisis, identifikasi precursor dan hasil degradasi senyawa senjata kimia  diethyl methylphosphonat (DEMP), methyl phosphonic acid (MPA) dalam sampel air dan  dimethyl methyl phosphonat (DMMP), ethyl phosphonic acid (EPA) dalam sampel tanah. Contoh yang dianalisa merupakan contoh senyawa tributilphosphat  (TBP)  40 ug/mL dan poliethilene glycol  56,24 ug/mL ditambahkan sebagai background dan sampel tanah kering yang berpasir. Identifikasi dilakukan dengan  metode  kromatografi gas spektrometri massa - elektron ionisani (GCMS-EI). Ekstraksi fasa organik  pada pH netral, sililasi dari fasa air yang diuapkan,  di mana triethylamine/methanol-sililasi dan  kation exchange-sililasi digunakan untuk ekstraksi senyawa - senyawa precursor dan hasil degradasi sebelum diinjeksikan ke GCMS. Dari hasil analisis diperoleh  waktu retensi  8,9 dan 10,97  menit  masing - masing untuk  diethyl methylphosphonat dan bis(trimethylsilyl) methylphosphonate dalam sampel air sedangkan dalam sampel tanah  6,62 dan 12,06 menit untuk dimethyl methylphosphonat  dan bis(trimethylsilyl) ethylphosphonate. Total Ion Chromatography (TIC) yang dihasilkan dari GCMS dievaluasi dengan menggunakan    Library Data Base NIST (National Institute of Standards and Technology), dan AMDIS (Automated Mass Spectral Deconvolution and Identification System). Spektrum yang dihasilkan memberikan nilai base peak pada m/z = 97  untuk  diethyl methylphosphonate , m/z = 225 untuk  bis(trimethylsilyl) methylphosphonate, m/z = 94 untukdimethyl methylphosphonate dan m/z = 239 untuk bis(trimethylsilyl) ethylphosphonate sedangkan  retention index (RI) yang dihitung digunakan untuk  mengonfirmasi masing-masing senyawa precursorKata kunci : precursor, degradsi senyawa senjata kimia, base peak , waktu retensi,  Total Ion KromatografiAnalysis, precursoridentification have been done and  degradation compoundsof chemical weapon diethyl methylphosphonat , methyl phosphonic acid in water matrices, dimethyl methylphosphonat and ethyl phosphonic acidin soil samples. Water used for extracting those  compounds was an example of simulation that contain tributilphosphat  (TBP)  40 ug/mL and poliethylene glycol  56,24 ug/mL which added as a background and  dry sandy soil samples. Identification was done  by using Gas Chromatographic Mass Spectrometry – Electron Ionization (GCMS-EI) method. Neutral organic extraction, evaporated water - silylation, triethylamine/methanol-silylation and cation exchanged-silylation were performed to extract the precursor’s compounds from the samples, before being analyzed by gas chromatography mass spectrometry .The result of the analysis by  Gas Chromatographic  Mass Spectrometry  method showed that the retention time (in min) was 8,9 and 10,97 for diethyl methylphosphonat and bis(trimethylsilyl) methylphosphonate in the water sample , while the retention time in soil sample was 6,62 and  12,06 for dimethyl methylphosphonat and bis(trimethylsilyl) ethylphosphonate . The result of Total Ion Chromatography (TIC) from GCMS was evaluated using NIST (National Institute of Standards and Technology) database library and AMDIS (Automated Mass Spectral Deconvolution and Identification System). The spectrum’s result gave the value of base peak, which are m/z = 97for diethyl methylphosphonat, m/z= 225 for bis(trimethylsilyl) methylphosphonate , m/z = 94 for dimethyl methylphosphonat and m/z = 239 for bis(trimethylsilyl) ethylphosphonate. On the other hand, the retention indice (RI) calculation was used to get the confirmation of each compounds of precursors. Key word : precursor, degradation of chemical weapon,  base peak, retention time, totalion chromatography.
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.