Acetonitrile test

Eor the selective pre-concentration of deactivated phenols a new silica-based material with the grafted 2,3,5-triphenyltetrazole was proposed. This method is based on the formation of molecular chai ge-transfer comlexes of 2,3,5-triphenyltetrazole (7t-acceptor) with picric acid (7t-donor) in the phase of the sorbent. Proposed SPE is suitable for HPEC analysis of nitrophenols after their desorption by acetonitrile. Test-system for visual monitoring of polynitrophenols under their maximum concentration limits was developed using the proposed adsorbent. 

The dienaminonitrile derived from the azulene-5-acetonitrile involving two possibilities of direction of ring-closure should preferentially cyclize, according to the MO theory, to give the benz(e)azulenes. But all attempts to synthesize the azulene-5-acetonitrile testing these predictions have hitherto been unsuccessful. 

Pesticides. Chlorinated hydrocarbon pesticides (qv) are often found in feed or water consumed by cows (19,20) subsequently, they may appear in the milk, where they are not permitted. Tests for pesticides are seldom carried out in the dairy plant, but are most often done in regulatory or private specialized laboratories. Examining milk for insecticide residues involves extraction of fat, because the insecticide is contained in the fat, partitioning with acetonitrile, cleanup (FlorisH [26686-77-1] column) and concentration, saponification if necessary, and determination by means of paper, thin-layer, microcoulometric gas, or electron capture gas chromatography (see Trace and residue analysis). 

Equation (16) was tested against some data obtained for (R) 4-phenyl-2-oxazolidinone using a range of mixtures of ethanol, acetonitrile and -hexane as the mobile phase. The column chosen was similar to that previously used for the separation of the 4-phenyl-2-oxazolidinone which was 25 cm long, 4.6 mm I.D. packed with 5 mm silica particles bonded with the stationary phase Vancomycin. The results obtained are shown in Table 1 and this is the data used in subsequent computer calculations. 

Generally, Ultrahydrogel columns are compatible with aqueous mobile phases from pH 2 to pH 12. The addition of organic modifiers such as acetonitrile is recommended up to 50%, but most common applications do not require such a high concentration of organic modifier. These columns have been tested in applications from 10 to 80°C using aqueous mobile phases. 

Some groups of pollutants also have specific problems. For instance, PAHs tend to adsorb on the walls of the system with which they come into contact and so an organic solvent or surfactant must be added to the sample. Several solvents have been tested (66, 67) isopropanol or acetonitrile are the most often used solvents, while Brij is the most recommended surfactant (66). A very critical parameter in these cases is their concentration. 

All analytical and test samples were recrystd from either acet-n-hexane mixts or acetonitrile and dried in an Abderhalden drying app over refluxing nitrobenzene for at least 4 hours. The product was identified as 2,2,2,f,4,4/,4, 6,6,6w-nonanitroter-phenyl by elemental analysis and X-ray molecular wt detn ... 

In the context of their new synthetic route to arenediazo phenyl ethers (see Sec. 6.2), Tezuka et al. (1987 a, 1989) investigated the reaction products of phenyldi-azo 1-naphthyl ether (12.10) under various conditions. When an acetonitrile solution of the diazo ether 12.10 was kept standing at room temperature for one week in the dark, the 4- and 2-phenylazo-l-naphthol isomers (12.11 and 12.12) were formed in 48% (20%) and 9% (8%) yields respectively. In the presence of acid (aqueous HC1 or H2S04) or of various bases (aqueous NaOH, pyridine, aniline, or sodium acetate) the yields of the azo products are much lower, but higher proportions of biphenyl, 1-naphthol, and phenol are formed. The crosscoupling product l-phenylazo-2-naphthol was not detected when the reaction was carried out in the presence of 2-naphthol. As this mechanistic test reaction gave rather low yields of the two azo compounds 12.11 and 12.12 in the presence and absence of 2-naphthol,... 

The role of Lewis acids in the formation of oxazoles from diazocarbonyl compounds and nitriles has primarily been studied independently by two groups. Doyle et al. first reported the use of aluminium(III) chloride as a catalyst for the decomposition of diazoketones.<78TL2247> In a more detailed study, a range of Lewis acids was screened for catalytic activity, using diazoacetophenone la and acetonitrile as the test reaction.<80JOC3657> Of the catalysts employed, boron trifluoride etherate was found to be the catalyst of choice, due to the low yield of the 1-halogenated side-product 17 (X = Cl or F) compared to 2-methyI-5-phenyloxazole 18. Unfortunately, it was found that in the case of boron trifluoride etherate, the nitrile had to be used in a ten-fold excess, however the use of antimony(V) fluoride allowed the use of the nitrile in only a three fold excess (Table 1). 

Various extraction methods for phenolic compounds in plant material have been published (Ayres and Loike, 1990 Arts and Hollman, 1998 Andreasen et ah, 2000 Fernandez et al., 2000). In this case phenolic compounds were an important part of the plant material and all the published methods were optimised to remove those analytes from the matrix. Our interest was to find the solvents to modily the taste, but not to extract the phenolic compounds of interest. In each test the technical treatment of the sample was similar. Extraction was carried out at room temperature (approximately 23 °C) for 30 minutes in a horizontal shaker with 200 rpm. Samples were weighed into extraction vials and solvent was added. The vials were closed with caps to minimise the evaporation of the extraction solvent. After 30 minutes the samples were filtered to separate the solvent from the solid. Filter papers were placed on aluminium foil and, after the solvent evaporahon, were removed. Extracted samples were dried at 100°C for 30 minutes to evaporate all the solvent traces. The solvents tested were chloroform, ethanol, diethylether, butanol, ethylacetate, heptane, n-hexane and cyclohexane and they were tested with different solvent/solid ratios. Methanol (MeOH) and acetonitrile (ACN) were not considered because of the high solubility of catechins and lignans to MeOH and ACN. The extracted phloem samples were tasted in the same way as the heated ones. Detailed results from each extraction experiment are presented in Table 14.2. 

To test the quality of some synthetic dyes according to standardized procedures, a screening is recommended based on TLC analysis on silica plates 60 F 254 using elutions with an ethyl acetate pyridine water 25 25 20 (v v v) mixture. To determine purity and secondary dyes (components or by-products of a dye that are not allowed to be present), successive TLC separations are recommended or, for more accurate answers, HPLC-DAD using RP-18 columns and eluents like acetonitrile and phosphate buffer."... 

GL 1] [R 1] [R 3] [P le] The performance of a typical laboratory bubble column was tested and benchmarked against the micro reactors (Figure 5.17). Using acetonitrile as solvent, the conversion of the laboratory bubble column ranged from 6 to 34% at selectivities of 17-50% [3, 38]. This corresponds to yields of 2-8%. Hence the yields of the laboratory tool are lower than those of the micro reactors, mainly as a consequence of lower selectivities. 

The testing of impnrities in active pharmacentical ingredients has become an important initiative on the part of both federal and private organizations. Franolic and coworkers [113] describe the utilization of PLC (stationary phase — silica gel and mobile phase — dichloromethane-acetonitrile-acetone (4 1 1, v/v)) for the isolation and characterization of impurities in hydrochlorothiazide (diuretic drug). This drug is utilized individually or in combination with other dmgs for the treatment of hypertension. The unknown impurity band was scraped off the plate and extracted in acetonitrile. The solution was filtered and used for LC/MS and NMR analysis. The proposed procedure enabled the identification of a new, previonsly nnknown impurity. It was characterized as a 2 1 hydrochlorothiazide-formaldehyde adduct of the parent drug substance. 

For multi-analyte and/or multi-matrix methods, it is not possible to validate a method for all combinations of analyte, concentration and type of sample matrix that may be encountered in subsequent use of the method. On the other hand, the standards EN1528 andEN 12393 consist of a range of old multi-residue methods. The working principles of these methods are accepted not only in Europe, but all over the world. Most often these methods are based on extractions with acetone, acetonitrile, ethyl acetate or n-hexane. Subsequent cleanup steps are based on solvent partition steps and size exclusion or adsorption chromatography on Florisil, silica gel or alumina. Each solvent and each cleanup step has been successfully applied to hundreds of pesticides and tested in countless method validation studies. The selectivity and sensitivity of GC combined with electron capture, nitrogen-phosphorus, flame photometric or mass spectrometric detectors for a large number of pesticides are acceptable. 

Prohexadione-calcium standard solutions Dissolve 10 mg of prohexadione-calcium in 100mL of water to prepare a lOOmgL" solution. Transfer 100 p.L of this solution into a 30-mL test-tube, evaporate water to dryness under reduced pressure and to methylate prohexadione-calcium according to Section 6.3. Dissolve the product in acetonitrile to prepare the 0.05,0.2,0.4,0.6 and 0.8 mgL acetonitrile solutions. 

Adjust to pH 2 by addition of concentrated HCl to 500 mL of water sample. Apply this acidic water to the Bond Elut LRC Cig (500-mg) cartridge column. Pass the elution solvent (2 mL of acetonitrile) through the cartridge and collect in a test-tube. Concentrate the eluate under an N2 gas flow at about 40 °C. 

Transfer an aliquot of the sample extract equivalent to 0.5-g of crop (5 mL) into a disposable test-tube (10-mL) and evaporate the sample in a heating block at 50 °C under a stream of dry air to < 1 mL. Add 5 mL of acetonitrile-water (3 7, v/v) to the sample and ultrasonicate the solution to ensure that the sample is fully dissolved. 

To make 1, [CpRu(CH3CN)3]3 F6 in acetone was allowed to react with 4, forming a mixture of 3d and chelate 1 (10). This mixture could be used but for purposes of catalyst characterization and further testing was converted to > 90% pure 1 by repeated coevaporation of added acetone with the acetonitrile liberated. Complex 1 showed diagnostie NMR data consistent with a chiral stracture and foin unique, diastereotopic methyl groups. 

Figure 4.10 Typical routine column test chromatogram for a 30 cm X 4.6 mm I. D. column pacXed with an octadecylsiloxane bonded silica packing of lO micrometers particle diameter. The test mixture consisted of resorcinol (0.55 mg/ml), acetophenone (0.025 mg/ml), naphthalene (0.20 mg/ml) and anthracene (0.01 mg/ml) in acetonitrile, 10 microliters injected. The separation was performed isocratically at 23 C with acetonitrile-water (55 45) as the mobile phase at a flow rate of 1.5 ml/min. Detection was by UV at 254 nm (0.1 AUFS).

Sander and wise have proposed a test method to determine the bonding chemistry used to prepare octadecylsiloxane column packings based on the relative retention of three polycyclic aromatic hydrocarbons, benzo[a]pyrene (BaP), phenanthro-phenanthrene (PhPh), and l,2 3,4 5,6 7,8-tetrabenzonaphthalene (TBN) eluted with the mobile phase acetonitrile-water (85 15) [52,67,199,210]. On monomeric phases the test solutes elute in the... 

Figure 7.13 Separation of a test eixture using automated multiple development with a universal mobile phase gradient from acetonitrile through dlchloromethane to carbon disulfide on a silica gel HPTLC plate. The chromatogram was scanned at different wavelengths to enhance the chromatographic information.

Figure 1.15 Fast analysis of a test mixture on a 10 cm x 4.6 mm I.D. column packed with 3 micrometer octa< ecylsilanized silica with a mobile phase flow rate of 3.4 mi. i.n (acetonitrile-water 7 3) and operating pressure of ca. 340 atmospheres. Peaks 1 uracil, 2 phenol, 3 - nitrobenzene, 4 - toluene, 5 -ethylbenzene, 6 - isopropylbenzene, and 7 - tert.-butylbenzene. (Reproduced with permission from ref. 222. Copyright Friedr. Vieweg 6 Sohn).

To test this hypothesis, the picolinamide 22 was prepared using in situ activated picolinic acid (Scheme 8.12). The in situ activation of picohnic acid was used because picolinyl chloride (available commercially as the HC1 salt) is relatively expensive. The coupling reaction was not straightforward, and the best results were obtained by adding 1.4equiv of thionyl chloride to a solution of 1.4equiv of picolinic acid in acetonitrile, followed by addition of triethylamine. As soon as the addition of triethylamine was complete, aniline 5 was introduced immediately because the activated picolinic acid was unstable in the presence of triethylamine. 

Surface Modification. A polydiene film (supported on a microscope slide) was immersed in a stirred, room temperature, RTD-acetonitrile solution of known concentration contained in a large glass-stoppered test tube. After a specific reaction time, the film was removed from the solution, washed with acetonitrile, water, and acetonitrile again, and dried under vacuum (Step 1). Films subsequently treated with base were immersed in aqueous solutions for 5-15 min. They were then washed with water and CH3CN, and vacuum dried (Step 2). Some films were aged in air at room temperature. 

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