This presentation addresses an automated quantitative analysis designed for determination of chloroanilines (CA) in personal cleansing (PC) liquid products containing trichlorocarbonilide (TCC). These materials may be present as impurities in the germicides as used, or they may be formed from the germicides during processing. This is a fully automated analysis which covers everything from sample preparation to determination of CA at the parts per million level. The CA is diazotizated by addition of sodium nitrite. After a prescribed reaction time, the excess nitrous acid is destroyed with ammonium sulfamate. The diazotizated CA is derivatized with naphthylethylene diamine and the level determined by difference in the UV-VIS absorption at approximately on peak (555 nm) and background (660 nm). Linearity, accuracy, and precision ensure the validity of the robotics method. The method has a linearity working range from 0 to 100 ppm (correlation coefficient, R = 0.9995). The method gives acceptable recoveries: R = 102% for liquid soap. Relative standard deviation is 1.14%. These results demonstrate that the system can determine the concentration of CA in PC products. This automated CA analysis frees up analysts from routine laboratory work for more technically difficult projects. The robot is capable of managing 36 samples per day, which is more than three times higher capacity than the manual procedure. © 2000 John Wiley & Sons, Inc. Lab Robotics and Automation 12:282–285, 2000

A flow injection system with online sample preparation is proposed for the determination of phosphite in liquid fertilizers by spectrophotometry. After loop-based injection, phosphite is oxidized by an acidic permanganate solution (1.0 10⁻² mol L⁻¹ KMnO₄ + 1.0 mol L⁻¹ H₂SO₄) in a heated reactor (50 °C). The phosphate generated is then determined by the molybdenum blue method. Influence of flow rates, temperature, and concentration and order of addition of reagents, sample volume, and reactor configuration for the blue complex formation on recorded signals were investigated. The flow system was applied to phosphite determination in commercial samples of liquid fertilizers. The proposed system handles about 80 samples per hour [0.05–0.40% (w/v) H₃PO₃; R = 0,9998), consuming about 80 μL sample, 1 mg KMnO₄, 25 mg (NH₄)₆Mo₇O₂₄, and 10 mg ascorbic acid per determination. Results are precise [relative standard deviation ≤ 3.5% for 0.1% (w/v) H₃PO₃, n = 12] and in agreement with those obtained by gravimetry at 95% confidence level. © 2000 John Wiley & Sons, Inc. Lab Robotics and Automation 12:286–290, 2000

Monitoring of urinary glucose level is of great interest in health control. As a fast and accurate means to achieve this purpose, a potentiometric glucose biosensor based on SnO₂ film was developed. The optimum manufacturing conditions and the functional characteristics of the biosensor were established. The n-type Sb-doped SnO₂ semiconductor film properties were characterized using electrochemical impedance spectroscopy. Measurements on urine samples yielded results that are in good agreement with those obtained with the Nylander method and more accurate than those obtained with a test paper. Taking into account that urine samples do not need pretreatment and that by the renewal of the enzyme membrane the stability period of the biosensor may be prolonged over 8 days, it may be used in continuous flux, too. © 2000 John Wiley & Sons, Inc. Lab Robotics and Automation 12:291–295, 2000

A robotic system was implemented to automate the polymer ash procedure performed in the Plastics Technical Center's Materials Evaluation Laboratory. The system automates ASTM Test Method D 5630: “Standard Test Method for Ash Content in Thermoplastics (Procedure B)” and Phillips Ryton poly(phenylene sulfide) (PPS) laboratory procedures “Determination of Ash of PPS Compounds” and “Ash Content of Polyphenylene Sulfide.” These procedures determine the ash content of the respective resins using a rapid, muffle furnace ashing technique. The robot system automates all aspects of the procedure, including taring the crucibles, inserting the samples into and retrieving the samples from the muffle furnace, weighing the crucibles, recording the weights, cooling the crucibles, calculating and reporting the results, and storing the data. Data generated on polyolefin (polyethylene and polypropylene) and Ryton poly(phenylene sulfide) samples show that the system generates data that are reproducible and equivalent to those obtained by manual application of the ASTM and Phillips procedures. The robot system has been successfully used to determine ash values ranging as low as 0.02 wt% for polyolefin resins and as high as 40+ wt% for PPS compounds. A comparison of results from the automated procedure to those obtained by the manual application of the procedure demonstrated that the robot provided equivalent values, with estimates of the precision that were at least as good as the manual procedure. Since its installation, the system has been used extensively, increasing the laboratory's testing capacity and providing labor savings of more than 0.5 human-years annually. © 2000 John Wiley & Sons, Inc. Lab Robotics and Automation 12:296–304, 2000

This article reports the use of solid phase spectrophotometry associated with flow injection technique for simultaneous determination of zinc and nickel with 1-(2-thiazolylazo)-2-naphthol (TAN) immobilized on a C₁₈ bonded silica support in the concentration range from 0.30 to 1.0 μg mL ⁻¹ of both ions. The multicomponent analysis was implemented using the absorbance signals in different intervals of time in a flow injection analysis peak for each sample solution inserted into the analytical path. A partial least squares (PLS) algorithm for model construction was developed in QuickBasic 4.5 as a subrotine in order to assemble it in a data acquisition program, permitting the concentration estimation in real time. The proposed method was successfully applied to nickel and zinc determination in synthetic mixtures with analytical throughput of 43 samples per hour. The results obtained with the proposed method were compared with Inductively Coupled Plasma Atomic E Mission Spectrometry (ICP-AES) data, and the results agreed with 95% confidence level. © 2000 John Wiley & Sons, Inc. Lab Robotics and Automation 12:305–311, 2000

A fully automated spectrophotometric analyzer for continuous, unattended determination of inorganic nitrogen (nitrite, nitrate, and ammonia) was developed. The analysis involves online UV photo-induced conversion of nitrate to nitrite and chemical oxidation of ammonia to nitrite. In both cases, nitrite was then subsequently determined by spectrophotometry using the sulfanilamide and N-1-naphthyl-ethylenediamine color reagents. Experimental conditions investigated to optimize the determination of nitrate and ammonia are presented. The linear ranges of the methods for nitrate and ammonia are 0.01–14 ppm and 0.01–5 ppm, respectively. The proposed method is simple, low cost, and sensitive. The analyzer was operated automatically and unattended for a period of 30 days. © 2000 John Wiley & Sons, Inc. Lab Robotics and Automation 12:312–316, 2000

Managing vast amounts of information associated with DNA array technology presents a challenge. This article describes a synergistic analysis management (SAM) system, which integrates microarray and laboratory data along with analysis steps to present a synergistic view to the researcher. We describe tools for data management in array fabrication, automated image analysis, and array data mining. All the described modules allow for seamless flow of information and are connected through a database. SAM will enhance microarray projects at pharmaceutical and academic institutions, which face the problems of high throughput microarray data management. © 2000 John Wiley & Sons, Inc. Lab Robotics and Automation 12:317–327, 2000