scholarly journals VALIDATION OF ANALYTICAL METHOD FOR DETERMINATION OF HIGH LEVEL CARBON DIOXIDE (CO2) IN NITROGEN GAS (N2) MATRIX USING GAS CHROMATOGRAPHY THERMAL CONDUCTIVITY DETECTOR

2015 ◽  
Vol 12 (24) ◽  
pp. 7-16
Author(s):  
Harry BUDIMAN ◽  
Oman ZUAS
Keyword(s):  
Carbon Dioxide ◽  
Thermal Conductivity ◽  
Gas Chromatography ◽  
Limit Of Detection ◽  
Good Precision ◽  
Thermal Conductivity Detector ◽  
Limit Of Quantitation ◽  
Carbon Dioxide Co2 ◽  
High Level

High accurate result of carbon dioxide (CO2) measurement is of great importance since the result (data) is used as the foundation for decision making related to regulated monitoring program and law enforcement. In this study, therefore, method for measurement of high level of carbon dioxide (CO2) in nitrogen (N2) matrix using gas chromatography thermal conductivity detector (GC-TCD) was validated to achieve the optimum performance of the method. For this purposes, identity confirmation, selectivity, limit of detection (LoD), limit of quantitation (LoQ), repeatability, reproducibility, accuracy, and linearity of the method were evaluated. The result shows that the GC-TCD method has good precision in term of repeatability and reproducibility having values of 0.07 and 0.37%, respectively. No bias of the method can be found and an excellent linearity of the method was obtained in the range of 2 - 13.97% mol/mol. Thus, based on the result evaluation under given criteria of this study, it can be concluded that the GC-TCD method is reliable and suitable for determination of high level of CO2 in N2 matrix.

Gas Chromatographic Determination of Pentachlorophenol in Gelatin

1984 ◽  
Vol 67 (2) ◽  
pp. 275-277
Author(s):  
Arnold P Borsetti ◽  
Lee S Thurston
Keyword(s):  
Gas Chromatography ◽  
Liquid Phase ◽  
Electron Capture ◽  
Limit Of Detection ◽  
Direct Determination ◽  
Chromatographic Determination ◽  
Gelatin Matrix ◽  
Limit Of Quantitation ◽  
Acetate Derivative

Abstract A method is described for the determination of pentachlorophenol (PCP) in gelatin. The method employs acid and heat to hydrolyze the gelatin matrix, a base partition and wash for separation and cleanup, and a reacidification and extraction with hexane for direct determination of PCP, without preparation of a derivative, using gas chromatography (GC) with a 1% SP-1240DA liquid phase and a 63Ni electron capture detector. Recoveries averaged 106% for fortifications between 0.02 and 1.0 ppm. The limit of quantitation is 20 ppb. The limit of detection is 4-6 ppb. The method, which has undergone a successful intralaboratory trial, is simple and rapid, and requires only general laboratory reagents and equipment. GC of the acetate derivative of PCP is used for confirmation of identity.

scholarly journals Validasi Metode Penentuan Mn Dalam Oli Lubrikan Dengan Metode Pengenceran Langsung Menggunakan Spektrofotometer Serapan Atom

2019 ◽  
Vol 6 (2) ◽  
pp. 94-100
Author(s):  
Rona Maningting Napitupulu ◽  
Dirgarini Julia ◽  
Aman S. Panggabean
Keyword(s):  
Detection Limit ◽  
Limit Of Detection ◽  
Lubricating Oil ◽  
Dilution Method ◽  
Good Precision ◽  
Validation Method ◽  
Limit Of Quantitation ◽  
Environment Control ◽  
Repeatability And Reproducibility

Validation method on the determination of Mn in lubricating oil by direct dilution method using Atomic Absorption Spectrophotometer (AAS) in Laboratory & Environment Control PT. Badak NGL Bontang has been done The validation method was done with research stages such as determination of  optimum solvent, and determination of some important parameters influential for validation method such as parameter of liniearitas (r), Instrument Detection Limit (IDL), Methode Detection Limit (MDL), accuracy, precision, Limit of Detection(LOD) and Limit of Quantitation(LOQ). The result of research obtain is good, showed that the linearity value with R2 ≥ 0,997. The IDL and MDL value was 0.0021 ppm and 0.0092 ppm respectively and has been acceptability requirements of MDL. The accuracy paramater obtained recovery value with range 82.25-88.34%. The measurement of repeatability and reproducibility, the CV Horwitz value smaller than % RSD, indicating the method had a good precision. The measurement of  LOD and LOQ value was 0.095 ppm 0.317 ppm respectively. Based on the result of the research determination method of Mn in lubricating oil by direct dilution method using AAS concluded valid.

scholarly journals Validasi Metode Penentuan Benzena, Toluena dan Xilena pada Sampel Udara dan Tanah Menggunakan Kromatografi Gas

2019 ◽  
Vol 15 (1) ◽  
pp. 177
Author(s):  
Aman Sentosa Panggabean ◽  
Tika Widyastuti ◽  
Noor Hindryawati
Keyword(s):  
Gas Chromatography ◽  
Retention Time ◽  
Limit Of Detection ◽  
Soil Samples ◽  
Analytical Performance ◽  
Air Samples ◽  
Limit Of Quantitation ◽  
Benzene Toluene ◽  
Precision And Accuracy

<p>Penelitian tentang validasi metode penentuan kadar benzena, toluena dan xilena pada sampel udara dan tanah dengan menggunakan kromatografi gas telah dilakukan. Untuk mendapatkan hasil pengukuran yang valid, beberapa parameter penting yang berpengaruh dalam validasi metode telah ditentukan. Beberapa parameter penting yang dilakukan adalah penentuan besaran dasar kromatografi yang meliputi: waktu retensi, kapasitas (k’), faktor selektivitas (α) dan kinerja analitik yang meliputi: penentuan linearitas (r), limit deteksi (LOD), limit kuantitasi (LOQ), presisi dan akurasi. Hasil penelitian penentuan kinerja analitik sangat baik ditunjukkan oleh nilai presisi sebagai % KV &lt; 2/3 nilai KV Horwitz, LOD untuk masing-masing senyawa benzena, toluena dan xilena adalah 0,02 mg/L; 0,59 mg/L dan 0,08 mg/L serta LOQ untuk masing-masing senyawa benzena, toluena dan xilena adalah 0,07 mg/L; 1,99 mg/L dan 0,27 mg/L. Akurasi  metode ini sangat baik ditunjukkan dengan nilai presentase perolehan kembali masing-masing senyawa benzena, toluena dan xilena untuk sampel tanah sebesar 102,61 ± 4,61%; 101,65 ± 7,41%; 102,15 ± 4,15%, dan untuk sampel udara masing-masing senyawa sebesar 101,69 ± 5,77%; 102,08 ± 5,43% dan 98,55 ± 5,11%. Berdasarkan hasil penelitian ini, metode kromatografi gas dapat digunakan dalam penentuan benzena, toluena dan xilena pada sampel udara dan tanah dengan memberikan hasil yang valid.</p><p><strong>Validation Method </strong><strong>o</strong><strong>n The Determination </strong><strong>o</strong><strong>f Benzene, Toluene </strong><strong>a</strong><strong>nd Xylene </strong><strong>i</strong><strong>n Air </strong><strong>a</strong><strong>nd Soil Samples Using Gas Chromatography. </strong>The present study investigated the method for the determination of the content of benzene, toluene, and xylene in air and soil samples using gas chromatography. To obtain a valid measurement result, several important parameters that influence the method validation have been determined. The several important parameters carried out are the determination of the basic chromatographic such as retention time, capacity factor (k'), selectivity (α) and analytical performance measurement includes: the determination of linearity (r), limit of detection (LOD), limit of quantitation (LOQ), precision and accuracy. The result of analytical performance of the research are well verified, in which the value of precision was % CV &lt; 2/3 CV Horwitz value, LOD for benzene, toluene, and xylene compound were 0.02 mg/L, 0.59 mg/L, 0.08 mg/L, respectively, and LOQ for benzene, toluene and xylene compounds was 0.07 mg/L, 1.99 mg/L and 0.27 mg/L respectively. This method achieved high accuration, indicated by a percentage of recovery value of benzene, toluene, and xylene for soil samples of 102.61 ± 4.61%; 101.65 ± 7.41%; 102.15 ± 4.15%, and for air samples was 101.69 ± 5.77%, 102.08 ± 5.43%, and 98.55 ± 5.11% respectively. Based on the results of this research, the method presented in this study can be applied for the determination of benzene, toluene, and xylene using gas chromatography in air and soil samples with valid results.</p>

Automated Thermal Conductivity Determination of Carbon Dioxide in Wine

1981 ◽  
Vol 64 (3) ◽  
pp. 547-549
Author(s):  
J Dale Mitchell ◽  
Christian R Benjamin
Keyword(s):  
Carbon Dioxide ◽  
Thermal Conductivity ◽  
Good Accuracy ◽  
Enzymatic Method ◽  
Average Difference ◽  
Thermal Conductivity Detector ◽  
Co2 Gas ◽  
Automatic Analyzer

Abstract Determination of CO2 in Lambrusco, using an automatic analyzer, has proven to be both fast and precise. The analyzer uses a thermal conductivity detector to measure CO2 gas liberated from the sample. Good accuracy was obtained when the method was compared to the enzymatic method. Ten samples gave an average difference of 1.4% from the accepted method.

scholarly journals Verifikasi Metode Penentuan Residu Pestisida Beta Siflutrin dalam Kentang (Solanum tuberosum L) secara Kromatografi Gas (Verification of Method for Determination of Residual Pesticides Beta Siflutrin in Potato (Solanum tuberosum L) with Gas Chromatography)

1970 ◽  
Vol 3 (1) ◽  
pp. 50-55
Author(s):  
Fahrizal Hazra ◽  
Lisa Rosdiana
Keyword(s):  
Gas Chromatography ◽  
Solanum Tuberosum ◽  
Limit Of Detection ◽  
Solanum Tuberosum L ◽  
Nitrogen Gas ◽  
Verification Method ◽  
A Value ◽  
Relative Standard ◽  
Limit Of Quantitation

The determination of residual pesticides beta siflutrin in potato (Solanum tuberosum L) was conducted by Gas Chromatography (GC). The separation was conducted on a DB-1 (30m×0.25mm×0.25µm) coloum, using a nitrogen gas as mobile phase at flow rate of 25 mL/min. The determination of beta siflutrin in potato with GC was based on the verification method. The detection was ECD detector. Verification parameters tested were linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ). Linearity had a correlation coefficient (r) of 0.9992. Accuracy had a recovery value of 99.49%. Precision had a value of relative standard deviation (% RSD) of 2.48%. The limit of detection (LOD) and limit of quantitation (LOQ) obtained was 0.001305 and 0.00435 mg/kg. The result of this research showed that the method of determination of residual pesticides beta siflutrin in potato with GC can be used as a routine analysis.Key words: verification, beta siflutrin, GC, potato

scholarly journals Determination of Carbon Monoxide in Tuna by Gas Chromatography with Micro-Thermal Conductivity Detector

2008 ◽  
Vol 46 (5) ◽  
pp. 392-394 ◽  
Author(s):  
C. Bernardi ◽  
L. M. Chiesa ◽  
S. Soncin ◽  
E. Passero ◽  
P. A. Biondi
Keyword(s):  
Thermal Conductivity ◽  
Gas Chromatography ◽  
Carbon Monoxide ◽  
Thermal Conductivity Detector

scholarly journals Single-Laboratory Validation of a Method for the Determination of Furan in Foods by Using Static Headspace Sampling and Gas Chromatography/Mass Spectrometry

2006 ◽  
Vol 89 (5) ◽  
pp. 1417-1424 ◽  
Author(s):  
Patricia J Nyman ◽  
Kim M Morehouse ◽  
Timothy P McNeal ◽  
Gracia A Perfetti ◽  
Gregory W Diachenko
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Apple Juice ◽  
Limit Of Detection ◽  
Peanut Butter ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation

Abstract A headspace gas chromatography/mass spectrometry method was developed and validated in-house for the determination of furan in foods. The method of standard additions with d4-furan as the internal standard was used to quantitate furan. The limit of detection and limit of quantitation (LOQ) values ranged from 0.2 and 0.6 ng/g, respectively, in apple juice to 0.9 and 2.9 ng/g, respectively, in peanut butter. Recoveries were obtained at 0.5, 1, 2, and 3 times the LOQ. At 1, 2, and 3 times the LOQ, the recoveries ranged from 89.4 to 108%, and the relative standard deviations ranged from 3.3 to 17.3% for all the matrixes. For apple juice, chicken broth, and infant formula, the averaged coefficients of determination from the linear regression analyses were &gt;0.99 with each food fortified at 0.5, 1, 2, and 3 times the LOQ. The coefficients of determination were &gt;0.99 for green beans and 0.96 for peanut butter with the foods fortified at 1, 2, and 3 times the LOQ. Within-laboratory precision was determined by comparing the amounts of furan found in 18 samples by 2 analysts on different days with different instruments. For most of the foods, the difference between the amounts found by each analyst was &lt;18%. The method was used to conduct a survey of &gt;300 foods. The furan levels found ranged from none detected to 174 ng/g.

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