Petroleum chlorophenols

Schnaak et al. [4] Polychlorinated terphenyls, naphthalenes, chloropesticides, halogenated hydrocarbon solvents, aromatic hydrocarbon solvents (BTEX), chlorobenzenes, poly aromatic hydrocarbons (EPA 610), phenols, chlorophenols, phthalates, petroleum hydrocarbons, LAS and nonylphenol (NP), organotin compounds and 2,4-dichloroaniline 1 pg/kg to 10 mg/kg for chlorine-contained compounds 10 pg/kg to 1 g/kg for solvent and phenols 1 mg/kg to 10 g/kg for EPA610, DEHP, LAS, and mineral oils Sewage sludge... 

Lee [42] determined pentachlorophenol and 19 other chlorinated phenols in sediments. Acidified sediment samples were Soxhlet extracted (acetone-hexane), back extracted into potassium bicarbonate, acetylated with acetic anhydride and re-extracted into petroleum ether for gas chromatographic analysis using an electron capture or a mass spectrometric detector. Procedures were validated with spiked sediment samples at 100,10 and lng chlorophenols per g. Recoveries of monochlorophenols and polychlorophenols (including dichlorophenols) were 65-85% and 80-95%, respectively. However, chloromethyl phenols were less than 50% recovered and results for phenol itself were very variable. The estimated lower detection limit was about 0.2ng per g. 

For analyses of PCDEs in chlorophenol formulations, the sample has been dissolved in 1 N NaOH before extraction with petroleum ether or hexane [37-43]. Firestone et al. [37] warmed the sample with water and 1 N NaOH before extraction with petroleum ether. The extract was washed first with water until neutral and then with 0.1 N NaOH. Paasivirta et al. [42] mixed the sample with methanol and NaOH aqueous solution before extraction with petroleum ether. Nilsson and Renberg [39] dissolved the samples in 1 mol l1 KOH and extracted with hexane diethyl ether (1 1) mixture. The extract was washed with 1 mol 1 1 KOH and then with water. Koistinen et al. [33] dissolved the sample in acetone, added hexane, and 0.1 mol 1 1 K2CO,. After shaking the organic layer was separated for analyses. 

Activated alumina (260 °C) column has been used for isolation of PCDEs, PCDDs, and PCDFs from chlorophenol extracts [37,38]. Four fractions were collected from an alumina column (50 g) petroleum ether (400 ml), 5% ethyl ether in petroleum ether (200 ml), 25% ethyl ether in petroleum ether (400 ml), and ethyl ether (400 ml). PCDEs, PCDDs, and PCDFs were determined in the third and fourth fractions after sulfuric acid cleanup. 

Phosphorylation. Chambers et al. found the reagent useful for the preparation of nucleoside diphosphoric acids (3, R —adenine, uracil, etc.). A nucleotide (I) is converted into the 5 -phosphoramidate (2) by reaction with ammonia and dicyclo-hexylcarbodiimide (DCC), and the amidate (2) is treated with dioxane diphosphate in o-chlorophenol (3 hrs..0 ). The diphosphoric acid (3) is precipitated with petroleum ether and purified as the ammonium salt. Yields are around 90%, whereas when 8.5% phosphoric add was used yields were in the order of 50-60%. However, anhydrous... 

Table 8.2 Recoveries of some organic compounds in a clay and peat soil using a screening procedure. Extraction after wetting with ammonium chloride solution and extraction at pH 1 and pH 10 using acetone followed by petroleum ether/dichloromethane. Extracts are dried with anhydrous sodium sulfate, concentrated and injected in a GC-MS. Herbicides and chlorophenols are methylated using trimethylsulfoniumhydroxide (Traag etal. 1997)...

Chlorophenol [108-43-0] M 128.6, m 33°, b 44.2 /lmm,214°/760mm, pK 9.13. It could not be obtained solid by ciystallisation from petroleum ether. It is best purified by distillation under reduced pressure. [Beilstein 6 IV 810.]... 

Chlorophenol [106-48-9] M 128.6, m 43°, 100-101°/10mm, pK 9.38. Distil the phenol, then crystallise it from petroleum ether (b 40-60°) or hexane, and dry it under vacuum over P2O5 at room temperature. [Bemasconi Paschalis J Am Chem Soc 108 2969 1986, Beilstein 6 IV 820.]... 

PCNB. See Pentachloronitrobenzene PCON PCONA. See 4-Chloro-2-nitroaniline PCP. See 4-Chlorophenol Pentachlorophenol PCPI. See 4-Chlorophenyl isocyanate PCPL Solvent, PCP Solvent. See Petroleum... 

Preparation by reaction of acetyl chloride on 4-chlorophenol with aluminium chloride in refluxing petroleum ether, and saponification of the obtained keto ester, the 2-acetoxy-5-chloroacetophenone (90%) [1871]. 

Trifluoroacetic, acid/ chloroform( 10 90)eluent o-Chlorophenol Trifluoroacetic acid chloroform(20 80) solvent Phenol-tetrachloroethane/n-heptane m-Cresol/petroleum ether... 

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