Prospective study to assess the clinical efficacy of bone scintigraphy--some analyses of clinical data

The value of preoperative bone scans in patients with primary breast and prostate cancer was evaluated prospectively. Of 414 patients with breast cancer, clinical stage I is 14, II is 219, IIIA is 59, IIIB is 39 and IV is 14. Of 88 patients with prostate cancer, clinical stage I is 14, II is 15, III is 18 and IV is 41. 11 percent of patients with breast cancer and 54 percent of patients with prostate cancer had bone metastases. Clavicle, ribs, thoracic spine, lumbar spine and pelvis metastasized most frequently. The incidences of bone metastases were 18.4% with Scirrhous carcinoma, 15.4% with Medullary tubular carcinoma and 3.8% with Papillotubular carcinoma. The methodology and results of ROC analysis were described in our other papers. Some results of data analysis were described in this paper.     

Determination of paraquat in marijuana by reversed-phase paired-ion high performance liquid chromatography.

A sensitive and selective method is described for the quantitative determination of paraquat in marijuana. Paraquat is extracted from finely ground plant material with hydrochloric acid with sonification, and the resulting acidic solution is extracted with chloroform:isopropanol (9:1) and evaporated to dryness. The residue is reconstituted with aqueous phosphate buffer pH 7.0; the solution is passed through a C-18 SEP-PAK TM and is analyzed with high performance liquid chromatography, using a reversed-phase column and an "ion pairing" reagent in the mobile phase. The recovery of paraquat in laboratory-spiked material varied from 90-97%. Results obtained with confiscated, field-sprayed marijuana by the procedure described were in excellent agreement with those obtained with a well-established ultraviolet procedure. The calculated limit of detection with this method is 2 ng of paraquat.     

Time dependent solution of the chemical kinetic boltzmann equation: two component isothermal system

A two component reactive systems is studied with the chemical kinetic Boltzmann equation. One components is taken to be in large excess and is unperturbed by reaction. The explicit time dependence of the velocity distribution function of the other component is calculated with a moment method. Comparison is made with the solutions calculated with the Chapman-Enskog procedure and with the method introduced by Kapral, Hudson and Ross. The region of validity of the Chapman-Enskog and/or Kapral, Hudson and Ross solutions is for the elastic collisions rate approximately three orders of magnitude faster then the reactive collisions rate. A comparison with the recent results obtained by Simons is also made.     

Non-destructive method for the analysis of gold(I) cyanide plating baths Complexometric determination of nickel and indium

A method is described for rapid determination of nickel and indium in gold(I) cyanide baths containing large amounts of citric acid and/or sodium citrate, without previous destruction of organic matter. Gold is removed by extraction with ethyl acetate. In one aliquot of the solution indium is masked with thioglycollic acid and nickel is precipitated with sodium diethyldithiocarbamate, extracted into chloroform, stripped into water and determined complexometrically. In a second aliquot indium and nickel are precipitated together with the same reagent and stripped into water, then nickel is masked with 1,10-phenanthroline, and indium is determined by direct titration with EDTA.     

Neutron activation determination of rheumium in rocks and ores after preliminary extraction with pyridine

A simple neutron-activation method for the determination of rhenium based on a preliminary extractive separation of the latter from molybdenum and tungsten is described. The sample is decomposed with sodium peroxide, a small amount of water is added and the resulting pulp is extracted with pyridine. The extract is evaporated to dryness, the residue is dissolved in water and the solution is passed through a column packed with Dowex 50WX8 in H⁺ form to eliminate the metal impurities. The HReO₄ passed, after neutralization with ammonia, is evaporated to dryness in penals, which then are irradiated with thermal neutrons.     

Spectrophotometric and gravimetric determination of sulfur in sebacate-base lubricants

Sulfur is determined in sebacate-base lubricants spectrophotometrically and gravimetrically. In the spectrophotometric method, a 0.2–0.3-g sample is treated with mixed acids, magnesium chloride is added, and the solution is evaporated to dryness. The sulfate is reduced to hydrogen sulfide by treatment with a mixture of hydriodic. hypophosphorous, and hydrochloric acids, and the hydrogen sulfide is distilled into ammonia solution. Lead citrate reagent is added and the brownish yellow color of lead sulfide sol is measured. An improved technique and apparatus for the distillation is described. In the gravimetric method, a 5-g sample is treated with mixed acids, antimony and tin are volatilized by treatment with hydrobromic acid, and sulfur is precipitated as barium sulfate. The recommended range of the spectrophotometric method is 0.005–0.15%,and that of the gravimetric method is 0.01–1% sulfur.     

Thermal performance evaluation of a solar air heater with and without thermal energy storage

This communication presents the experimental study and performance analysis of a solar air heater with and without phase change material (PCM) viz. paraffin wax and hytherm oil. There are three different arrangements viz. without PCM, with PCM and with hytherm oil to study the comparative performance of this experimental system. Inlet, outlet temperatures and radiation with respect to time have been recorded and found that the output temperature in case with thermal energy storage (TES) is higher than that of without TES, besides, the outlet temperature with paraffin wax is slightly greater than that of with hytherm oil. Also there is no energy gain in the evening in case of without TES but in case of with TES there is a heat gain for around 4 h in the evening which gives the backup for hot air for around four more hours which is the main advantage of this systems with TES. Based on the data, the efficiency of the system has been calculated and it is noted that the efficiency in the case of heat storage is higher than that of without TES, besides the efficiency in the case of the paraffin wax is slightly higher than that of the hytherm oil case.     

Confirmation of phenylbutazone residues in bovine kidney by liquid chromatography/mass spectrometry

A confirmatory method is described for phenylbutazone (PB) residues in bovine kidney tissue. Ground kidney tissue is diluted with water, and the mixture is made basic with 25% ammonium hydroxide in water; the lipids are extracted with ethyl and petroleum ethers. The ether layer is discarded, and the tissue is acidified with 6N HCl. PB residues are extracted with tetrahydrofuranhexane (1 + 4). The extract is passed through a silica solid-phase extraction column, and the eluate is evaporated to dryness. The residue is dissolved in acidified acetonitrile-water-acetic acid (50 + 49.4 + 0.6). A single quadrupole mass spectrometer coupled to a liquid chromatograph with an electrospray interface is used to confirm the identity of the PB residues in the kidney extract. Negative-ion detection with selected-ion monitoring of 4 ions is used. Sets of control and fortified-control kidney tissues (at 50, 100, and 200 ppb PB) and several kidney tissue field samples were analyzed for method validation. The method was tested further during the course of a survey to determine the incidence of PB residues in bovine kidney samples obtained from slaughterhouses across the country. In addition, the method was tested for use with an ion-trap mass spectrometer coupled to a liquid chromatograph, which allowed confirmation of PB at lower levels (5-10 ppb) in kidney tissue.     

Studies on Thermal Stability and Fluid Property of PVC Filled with Hydrotalcite

IntroductionIt is well known that PVC is a kind of valuableplastic and used in many fields.But PVC isunstable against heat and light,and at the heat-molding step,the thermal decomposition of it maytake place.Finally,the decomposition will reducethe mechanical strength and lose otherproperties ofPVC.In order to overcome those disadvantages,athermal stabilizer is added in the PVC material toreduce the thermal decomposition,and organiccompounds of metals such as Sn,Pb,Ca,Ba,Znand Cd are u…     

Complexometric determination of aluminium in iron ore,sinter, concentrates and agglomerates

A method for the complexometric determination of aluminium in iron ore, sinter, concentrates and agglomerates encountered in international trade is described. The sample is fused in a zirconium crucible with a mixed flux of sodium carbonate and sodium peroxide. The fused mass is completely soluble in hydrochloric acid. The R₂O₃ oxides are then precipitated with ammonia and redissolved in hydrochloric acid. Elements such as iron, titanium and zirconium are separated from aluminium by solvent extraction with cupferron and chloroform. After removal of traces of organic matter from the aqueous phase, the solution is treated with an excess of EDTA, which is then back-titrated with zinc solution (Xylenol Orange as indicator). Addition of ammonium fluoride then releases EDTA equivalent to the aluminium and this is titrated with zinc solution. The method is rapid. The precision and accuracy are excellent, and the results comparable with those obtained by the referee method.     

Facilitated and reverse transport of electrolytes through an asymmetric membrane

It is well known that the asymmetry of a membrane structure is closely related to its functions. Transport of ions is also affected by the asymmetry of the membrane structure. In this paper, ion transport through an asymmetric membrane is discussed theoretically. Equations are derived for the partition coefficient and the fixed charge density of a membrane with different surfaces. It is concluded that facilitated transport as well as reverse transport takes place both in membranes which are asymmetric with respect to the partition coefficient and in membranes with asymmetric charge distribution. In addition, the following two kinds of asymmetric membranes were prepared: one is a cellulose acetate—collodion membrane, which is asymmetric with respect to the partition coefficient, and the other is an NaOH-treated collodion—collodion membrane, which is asymmetric with respect to the membrane charge density. Ion transport through these membranes was investigated in order to verify the validity of the theory; the experimental results are in agreement with the theory.     

Potentiometric determination of boron in graphite microspheres for nuclear engineering

The well-known acidimetric determination of boron via the boric acid-mannitol complex is applied to the analysis of boron-loaded graphite microspheres used in nuclear engineering. After the sample is accurately ground, it is fused with an oxidizing alkaline flux. The melt is dissolved with warm water, the solution is acidified to completely remove carbon dioxide and the boric acid is titrated potentiometrically with carbonate-free sodium hydroxide after its complexing with mannitol.The determination of at least 0.2% boron in graphite is carried out with an average error of less than 1%.     

The polarographic determination of copper and zinc in plants and soils

A method is described whereby the extraction and polarisation of copper and zinc with maximum, sensitivity is possible. Interference from cobalt is prevented by extracting with dithizonc in the presence of dimethylglyoxime.The supporting electrolyte used is dccimolar potassium hydrogen phthalate which permits satisfactory waves for both copper and zinc (with greater sensitivity for copper, than is the case with the ammonia-ammonium chloride electrolyte).     

Determination of streptomycin residues in food by solid-phase extraction and liquid chromatography with post-column derivatization and fluorometric detection

A reliable and sensitive procedure is presented for the analysis of streptomycin (STP) in food of animal origin, like meat, milk and honey. The method is based on a separation by ion-pair liquid chromatography with β-naphthoquinone-4-sulfonate (NQS) postderivatization and fluorescence detection. The clean-up of the extract is done by solid-phase extraction, firstly with a cation-exchange cartridge and secondly with an octadecyl cartridge. The selectivity is very good and not many interfering peaks are observed for various food matrices. The streptomycin recovery of the total procedure is superior to 80%. The procedure is quantitatively characterized and repeatability, linearity, detection and quantification limits are very satisfactory. A special focus is given to STP residues in honeys and a survey on 64 commercial honeys is presented. For honey analysis, the HPLC method is compared with an immunoassay test (ELISA), and the possibility of using this test for screening with and without solid-phase extraction clean-up is also discussed.     

Determination of sulphur functions with N-iodosuccinimide

Titrimetric determination of thioureas, thiols, xanthates and dithiocarbamates with N-iodosuccinimide (NIS) is described. The method for xanthate can be applied to carbon disulphide (converted into xanthate with potassium ethoxide). Acidic and non-aqueous solutions of the oxidizing agent are stable. The procedures are rapid and accurate to 0.1% with a precision of 0.2%. Hydrogen sulphide and thiocarbonyl compounds interfere. The behaviour of N-bromosuccinimide and NIS with thiols in aqueous medium is compared. It is shown that iodine is the oxidizing species in both cases. The limitations of iodine as a reagent for thiol determination are discussed. Cysteine, which cannot be determined with iodine, can be determined with NIS. The role of methanol in non-aqueous determination of thiols is discussed. Methanol accelerates the oxidation, which is otherwise slow in acetonitrile medium.     

Potentiometric argentimetric method for the successive titration of sulphide and dissolved sulphur in polysulphide solutions

Sulphide sulphur and dissolved sulphur in a polysulphide solution can be successively determined with satisfactory accuracy and reproducibility by potentiometric argentimetry in which a sulphide-selective indicator electrode is used. Before the titration, polysulphide ions need to be converted by an excess of potassium cyanide into thiocyanate and sulphide ions. The excess of cyanide ions is masked with formaldehyde and sulphuric acid, then the solution is made alkaline with ammonia and titrated with silver nitrate till the first end-point is reached (sulphide sulphur). After the acidification of the solution with sulphuric acid, the titration is continued till the second end-point is attained (dissolved sulphur).     

Combined supercritical-fluid chromatography/mass spectrometry in the analysis of diuron in plasma using on-line phase-system switching

On-line sample pretreatment by means of the phase-system switching approach is an interesting technique for the analysis of aqueous samples, e.g., plasma, by means of supercritical-fluid chromatography. In order to analyse plasma samples the following analytical procedure is used. The plasma sample is injected on to a short precolumn, which is washed with water and subsequently dried with nitrogen. Next, the solutes are desorbed with the supercritical mobile phase, analysed with packed-column supercritical-fluid chromatography and detected with either a UV detector or a mass spectrometer, equipped with a moving-belt interface. The herbicide diuron is selected as a test compound to study the feasibility of this approach. Using a selective detector the procedure is sufficiently sensitive to detect diuron in plasma, but not appropriate to detect the diuron metabolites in a post-mortem plasma sample. These have been identified with liquid chromatography/mass spectrometry. The detection limit of diuron in plasma using the procedure described is about 30 ng/mL.     

Use of hydroxylamine hydrochloride in the titrimetric determination of manganese in pyrolusite

A procedure is described for the determination of total manganese in pyrolusite. The sample is decomposed with hydroxylamine hydrochloride solution. The residue left after filtration is fused with sodium carbonate and extracted again with hydroxylamine hydrochloride solution. A suitable aliquot is titrated with EDTA at pH 10, with Eriochrome Black T as indicator, after masking of interfering elements.     

Rapid analysis of fertilizers by the direct-reading thermometric method

The authors have developed rapid methods for the determination of the main components of fertilizers, namely phosphate, potassium and nitrogen fixed in various forms. In the absence of magnesium ions phosphate is precipitated with magnesia mixture; in the presence of magnesium ions ammonium phosphomolybdate is precipitated and the excess of molybdate is reacted with hydrogen peroxide. Potassium is determined by precipitation with silico-fluoride. For nitrogen fixed as ammonium salts the ammonium ions are condensed in a basic solution with formalin to hexamethylenetetramine; for nitrogen fixed as carbamide the latter is decomposed with sodium nitrite; for nitrogen fixed as nitrate the latter is reduced with titanium(III). In each case the temperature change of the test solution is measured. Practically all essential components of fertilizers may be determined by direct-reading thermometry; with this method and special apparatus the time of analysis is reduced to at most about 15 min for any determination.     

Development and validation of a gas chromatography/mass spectrometry procedure for confirmation of para-toluenesulfonamide in edible fish fillet tissue

Chloramine-T is a disinfectant being developed as a treatment for bacterial gill disease in cultured fish. As part of the drug approval process, a method is required for the confirmation of chloramine-T residues in edible fish tissue. The marker residue that will be used to determine the depletion of chloramine-T residues from the edible tissue of treated fish is para-toluenesulfonamide (p-TSA), a metabolite of chloramine-T. The development and validation of a procedure for the confirmation of p-TSA is described. Homogenized fish tissue is dried by mixing with anhydrous sodium sulfate, and the mixture is extracted with methylene chloride. The extract is passed through a silica gel solid-phase extraction column, from which p-TSA is subsequently eluted with acetonitrile. The acetonitrile extract is evaporated, and the oily residue is dissolved in hexane. The hexane solution is shaken with fresh acetonitrile. The acetonitrile solution is evaporated and the residue is redissolved in dilute potassium hydroxide solution. The aqueous solution is extracted with methylene chloride to further remove more of the fat co-extractive. The aqueous solution is reacted with pentafluorobenzyl bromide in presence of tetrabutylammonium hydrogensulfate. The resulting di-(pentafluorobenzyl) derivative of p-TSA is analyzed by gas chromatography/mass spectrometry. This method permits the confirmation of p-TSA in edible fish tissue at 20 ppb.