Spectrophotometric method for determination of sulfide with iron(III) and nitrilotriacetic acid by flow injection.

A manual colorimetric method for determination of sulfide has been adapted to flow injection, systematically optimized, and more fully characterized. Its intended application is for measurement of sodium sulfide reagent strength in pulp process streams, and sulfide contamination in effluent from Kraft pulp mills. In the flow-injection method developed, a sample solution containing sulfide is reacted with a mixture of iron(III) and nitrilotriacetic acid under ammoniacal conditions. The absorbance of the intensely-colored green product of this reaction is measured at 636 nm. Excess sulfite is present as a color stabilizer. A linear dynamic range of 20-100 ppm sulfide is readily achieved; the relative standard deviation is less than 1.2% (n = 10) throughout this range, and 0.37% (n = 10) midrange at 60 ppm. The usable dynamic range is 8-250 ppm sulfide. Long-term stability of the method is ensured by periodically performing an automatic cleaning cycle using a hydrochloric acid wash solution. This prevents tube discoloration and removes any precipitates which are formed under strongly alkaline conditions. The sample throuhput rate is at least 30/hr, given alternate acid wash cycles.

Versatile IEEE-488 data acquisition and control routines for a diode array spectrophotometer.

The UV-visible diode array spectrophotometer is a work-horse instrument for many laboratories. This article provides simple data acquisition and control routines in Microsoft QuickBasic for a HP-8452A diode array spectrophotometer interfaced to an IBM PC/XT/AT, or compatible, microcomputer. These allow capture of full spectra and measure absorbance at one or several wavelengths at preset time intervals. The variance in absorbance at each wavelength is available as an option.

Spectrophotometric determination of palladium with sulfochlorophenolazorhodanine by flow injection.

Sulfochlorophenolazorhodanine (as its sodium salt) has been used in the automated development of a sensitive flow-injection procedure for the spectrophotometric determination of palladium. The resulting method has high sample throughput, good precision, and low consumption of both sample and reagents. The optimum pH for the reaction is 5.0 and the response is constant at pH between 4.7 and 5.3. The sensitivity (calibration slope) of the procedure is 4.4 x 10(3) l./mole. The linear dynamic range is 0.045-30.0 mug/ml. The sample throughput is at least 120/hr. An automated procedure for optimization of analytical variables is described and a two-variable response surface for the system is given. Interference studies on 19 metal ions show that the method has good selectivity.

Computer-controlled apparatus for automated development of continuous flow methods.

An automated apparatus to assist in the development of analytical continuous flow methods is described. The system is capable of controlling and monitoring a variety of pumps, valves, and detectors through an IBM PC-AT compatible computer. System components consist of two types of peristaltic pumps (including a multiple pump unit), syringe pumps, electrically and pneumatically actuated valves, and an assortment of spectrophotometric and electrochemical detectors. Details of the interface circuitry are given where appropriate. To demonstrate the utility of the system, an automatically generated response surface is presented for the flow injection determination of iron(II) by its reaction with 1,10-phenanthroline.