Perkin Elmer gas chromatograph

The analysis of the extracts was made in a Perkin Elmer Gas Chromatograph model 8700 with an detector NPD. The analysis conditions were 423 K for 1 minute followed by ramp of 15.0 K/min until 523 K and another ramp with 30.0 K/min until 553 K. Injector and detector were setted at 533 K and 543 K, respectively. It was used a capillar column BP5 (cross-linked 5 % biphenyl, 95 % dimethylssiloxane) with 50 m long and 0.25 pm of diameter from SGE. Carrier gas used was He at 2 ml 7 min. 

The feedstocks (straight-mn naphtha (SRN) and a blend of SRN and hydrocracked naphtha) and hydrotreated products were analysed by ASTM methods for density, carbon, hydrogen, hydrocarbon and boiling point distribution. Total sulfur was determined by ASTM D-4045 method, mercaptan sulfur by the potentiometric method (ASTM D-3227 and UOP-212), disulfides by the UOP-202 method, polysulfides by polarography [1], and elemental sulfur by the UOP-286 method. The Perkin-Elmer gas chromatograph (Model 8700), equipped with a flame photometric detector (GC/FPD) and a DB-1 fused silica capillary column (30 m x 0.53 mm), was used for identification of individual sulfur compounds [2-6]. The sensitivity of the GC/FPD technique was maximized by optimizing the gas flow rates and temperature programming as presented elsewhere [1]. 

Analysis of C3Hg, O2, CO, H2, CO2 and CH4 in gas mixture in the inlet as well as in the outlet of the reactor was performed using a Perkin Elmer gas chromatograph (columns 4 m x 3 mm I.D. 60/80 Poropak Q, and a 2 m x 3 mm I.D. 60/80 Molecular Sieve 5A, both at 150°C). A calibration mixture (Messer-Griesheim) was used as the reference in quantitative analysis of the product samples. The water content in the reaction products was determined by on-line connected Prolabo-hygrometer. 

Inlet and effluent gas streams were analyzed periodically using an on-line Sigma I (Perkin Elmer) gas chromatograph. 

The carbon number distribution of the condensed products was obtained with a Perkin-Elmer 900 chromatograph, using a flame ionization detector and a 3-m column containing 10% SP 2100 on 80-100 mesh Supelcoport. The column was temperature programmed from 60° to 350°C at 8°C/min and held at 350°C. Helium, flowing at 30 cmVmin, was used as the carrier gas. 

TABLE 2.1 Perkin-Elmer Gas-Liquid Chromatographic Columns for the Model 154 Vapor Fractometer... 

After adequate analitical prepai ation according to standai d EPA method 608 samples were analysed gas chromatographic on a gas chromatograph 8500 Perkin Elmer, in glass and capilar columns using a capture electron detector and mass spectrometry, temperature program. 

SORPTOMETER (PERKIN-ELMER). This method is essentially a gas-chromatographic technique with the sample powder in place of the normal chromatographic column. A mixt of He and N2 is passed thru the sample and the concn of N2 in the exit gas is measured by thermal conductivity or gas-density methods,... 

Activities of the catalysts were measured on a microreactor. About 3 g of catalyst was charged into a reactor and heat-treated in nitrogen at reaction temperature. Acetic acid was added to the process and the reaction was initiated by switching nitrogen to ethylene. Reaction product analyses were performed by an online gas chromatograph equipped with a flame ionization detector (Perkin Elmer Auto System II). 

At the end of the experiment the hydrocarbons were removed from the cold trap and analyzed. The cyclohexane content of the sample was determined by gas chromatography on a Perkin-Elmer Fll gas chromatograph. The remainder of the sample was separated into a benzene and a cyclohexane fraction on a preparative gas chromatograph (Varian Auto-prep). 

The CGC analysis of the volatile degradation products were performed using a Perkin-Elmer Sigma 2000 capillary gas chromatograph. The column used was either a fused silica 0.25 micron, bonded methyl silicone (10 m, 0.25 mm I.D.) or a methyl/5% phenyl silicone (15 m 0.25 mm I.D.) bonded phase. The carrier gas was helium and the capillary column head pressure was maintained at 20 psi. The make-up gas for the pulsed electron capture detector (ECD) was 95% Ar/5% methane supplied at a flow rate of 60 ml/min. 

Fig. 9.9 which was obtained using a Perkin Elmer 452 gas chromatograph shows the separation of 0.5ng amounts of four derivatised herbicides A, monoLinuron B, Fenuron C, Linuron and D, chlorobromuron. 

Fig. 9.9 Gas-chromatographic response of a standard mixture of brominated anilines derived from A monoLinuron B Fenuron C, Linuron and D, chlorobromuron (R=14min). Amount applied, 0.5ng. Perkin-Elmer, Model 452, gas chromatograph Sdurce Reproduced with permission of the Royal Society of Chemistry [138]...

The system used by these workers consisted of a Microtek 220 gas chromatograph and a Perkin-Elmer 403 atomic absorption spectrophotometer. These instruments were connected by means of a stainless steel tubing (2mm o.d.) connected from the column outlet of the gas chromatograph to the silica furnace of the atomic absorption spectrometer. The silica furnace was set at 1000°C. The gas chromatographic column was packed with 3% OV-1 supported on Chromosorb W. The column was temperature programmed at 15°C h to 150°C. 

Flame ionisation. Flame Photometric and Thermionic Detection use a Perkin—Elmer Sigma 1 gas chromatograph, equipped with an S.G.E on-column injector. The column used was a 25 metrex0.31mm I.D. fused silica WCOT capillary coated with BP-1 (S.G.E), a methyl silicone. 

Equipment. All melting points were determined with a Mel-Temp apparatus from Laboratory Devices and are uncorrected. Gas chromatography was carried out on either a Varian Aerograph 700 or Hewlett-Packard 5880 chromatograph. Beckman IR-9 and Perkin Elmer FT-1800 spectrophotometers were used for the determination of mid-IR spectra. All NMR spectra were obtained using an IBM NR-80 FT spectrometer. Elemental analyses were determined for all new monomers and polymers by Micro-Tech Laboratories, Inc. of Skokie,... 

Instrumentation. Preliminary gas chromatographic analyses were carried out on a Perkin-Elmer 900 gas chromatograph equipped with a flame ionization detector and on a Hewlett-Packard 5730A gas chromatograph equipped with flame ionization and electron-capture detectors. The columns used were 180 cm x 2 mm ID glass columns packed with 3% SL-2100 (a methyl silicone fluid) on 80/100 mesh Supelcoport we also used 25 m X 0.25 mm ID glass capillary columns statically coated (7) with SE-52. 

A Nester-Faust Model NFT-50 annular spinning-band distillation unit was used to obtain the reported product yields in >99% chemical purity by gas chromatographic analysis (Perkin-Elmer Model Sigma IB Instrument using a 6 x 1/8" 5% SE-30 on silylated Chromosorb W column). Lower product yields (84-86%) of similar chemical purity were obtained using a 200-mm column packed with glass helices. 

Total nitrogen was determined using standard mlcrokjeldahl digestion, and terpenes were analyzed using a Perkin Elmer 3920 gas chromatograph equipped with a Perkin Elmer 0.10 In x 150 ft capillary column packed with 85% OS-138, 14% CO-880, and 1%... 

A calibration standard was prepared by concentrating the solution containing 60 mg oil, 0.2 mg ethyl heptanoate and 160 ml pentane to the equivalent volume (ca. 0.2 ml). A Perkin - Elmer Sigma 2B gas chromatograph equipped with a flame ionization detector was used for analysis. The gas chromatographic conditions were as follows ... 

Standards with a poor UV chromophore (4-methyl-2-pentanone, 1-chlorododecane, and stearic acid) were analyzed on a Perkin-Elmer 3920 gas chromatograph with a flame ionization detector and a 30-m SE-54 wall-coated open tubular (WCOT) fused-silica capillary column (J W Scientific). The injector temperature was 200 °C the detector interface temperature was 280 °C. The carrier gas was He at 16.5 lb/in.2, and the makeup gas was nitrogen at a flow of 40 cm3/min. Splitless l-/zL injections of the 25,000 1 concentrates were made by starting with an oven temperature of 45 °C and the oven door open after 2.75 min, the oven door was closed and the temperature was programmed at 4 °C/min to 280 °C, which was held for 8 min. The syringe was kept in the injection port for 15 s after injection. 

Infrared spectra were determined using Perkin-Elmer infrared spectrophotometers models 137-B and 21. NMR spectra were run using Varian T-60 and A-60 spectrometers. Gas chromatographic analyses were done on a Hewlett-Packard model 5750B instrument. Fractional distillations were performed on a Nester-Faust 18-inch semimicro spinning band column equipped with a stainless steel band. 

Molecular weight determinations were carried out osmometrically on a Hitachi Perkin Elmer model 115 molecular weight apparatus with the complex dissolved in benzene and at 38°C (the lowest possible temperature). The isomerization was followed by GLC analysis (Perkin Elmer model 11, Squalane column). The desired amount of the complex was placed in a reaction flask which was then flushed with N2. Benzene and 1-hexene which had been degassed by refluxing over sodium in an N2-atmosphere, were injected through a membrane attached to the flask. Samples were removed through the membrane and injected immediately into the gas chromatograph. 

Materials. The gases used had a purity >99% the carbon monoxide contained <1% hydrogen by GLC silica gel, 4 m X 1/8 inch, 70 °C, Perkin-Elmer F 11 hot wire gas chromatograph and argon as carrier gas. All hydroformylation experiments were performed with a 1 1 mixture of carbon monoxide and hydrogen. The olefinic substrates were Fluka AG pure or very pure grade. a-Ethylstyrene, prepared according to Ref. 21, was > 98% pure by GLC. 

NMR spectra were taken in deuteriochloroform solution, using a Varian HA100 spectrometer. Thermal measurements were made with a Perkin-Elmer DSC IB differential scanning calorimeter at 40°C/min. Near-infrared spectra were measured in carbon disulfide solution with a Beckman DK 2A spectrophotometer. Gas-chromatographic analyses of reaction mixtures were carried out after conversion of the phenols to trimethylsilyl ethers by reaction with bis (trimethylsilyl) acetamide. 

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