A reagent-free SIA module for monitoring of sugar, color and dissolved CO2 content in soft drinks.

This work presents a new sequential injection analysis (SIA) method and a module for simultaneous and real-time monitoring of three key parameters for the beverage industry, i.e., the sugar content (measured in Brix), color and dissolved CO(2). Detection of the light reflection at the liquid interface (the schlieren effect) of sucrose and water was utilized for sucrose content measurement. A near infrared LED (890+/-40 nm) was chosen as the light source to ensure that all the ingredients and dyes in soft drinks will not interfere by contributing light absorption. A linear calibration was obtained for sucrose over a wide concentration range (3.1-46.5 Brix). The same module can be used to monitor the color of the soft drink as well as the dissolved CO(2) during production. For measuring the color, the sample is segmented between air plugs to avoid dispersion. An RGB-LED was chosen as the light source in order to make this module applicable to a wide range of colored samples. The module also has a section where dissolved CO(2) is measured via vaporization of the gas from the liquid phase. Dissolved CO(2), in a flowing acceptor stream of water resulting in the change of the acceptor conductivity, is detected using an in-house capacitively coupled contactless conductivity detector (C(4)D). The module includes a vaporization unit that is also used to degas the carbonated drink, prior the measurements of sucrose and color within the same system. The method requires no chemicals and is therefore completely friendly to the environment.

Pervaporation-flow injection with chemiluminescence detection for determination of iodide in multivitamin tablets.

This paper describes the use of a pervaporation (PV) technique in a flow injection (FI) system for selective improvement in iodide analysis. Iodide in the sample zone is oxidized to iodine, which permeates through a hydrophobic membrane. Detection of the diffused iodine is achieved using the chemiluminescent (CL) emission at 425nm that results from the reaction between iodine and luminol. The method was applied for the analysis of some pharmaceutical products, such as nuclear emergency tablets and multivitamin tablets. Ascorbic acid present in multivitamin samples interfered seriously with the analysis, and off-line sample treatment using anion exchange resin was employed to successfully remove ascorbic acid before the analysis. Ascorbic acid was flushed from the column using 0.4M sodium nitrate followed by elution of iodide with 2M sodium nitrate. The detection limit (3S.D.) of the system was 0.5mgl(-1), with reproducibility of 5.2% R.S.D. at 5mgl(-1). Sample throughput was determined as 30injectionsh(-1). There was good agreement between iodide concentrations from extracted samples determined using four different methods, i.e., PV-FI, gas diffusion-flow injection, potentiometry and ICP-MS. A comparison of the analytical features of the developed pervaporation system with these of the previously reported chemiluminescence gas diffusion-flow injection previously reported is also described.

Determination of iodide by detection of iodine using gas-diffusion flow injection and chemiluminescence.

This work describes development of a flow injection (FI) system for determination of iodide, based on the chemiluminescence (CL) reaction between iodine and luminol. Iodide in the sample zone is oxidized to iodine. Employment of a gas-diffusion (GD) unit allows for selective detection of the generated CL (425nm). Preliminary results showed for concentrations of less than 2mgL(-1), that signals were irreproducible and that the calibration was not linear. In order to solve these problems, a method of 'membrane conditioning' was investigated, in which iodide stream was continuously merged with oxidant to generate I(2) that conditioned the GD membrane and tubing. This minimized surface interaction between the active surface and the I(2) generated from the samples, thus improving both precision and sensitivity. By employing membrane conditioning, it has been possible to reliably detect concentrations down to 0.1mgL(-1). At the optimized condition, an excellent linear calibration (r(2) = 0.999) was obtained from 0.1 to 1.0mgL(-1). The method was successfully applied to determine iodide in some pharmaceutical products such as potassium iodide tablets and a liquid patent medicine. However, for vitamin tablets, ascorbic acid was found to interfere seriously by causing a negative signal.

Simple and selective method for determination of iodide in pharmaceutical products by flow injection analysis using the iodine-starch reaction.

This work exploited the well-known iodine-starch reaction for development of a simple flow-injection (FI) method for determination of iodide in pharmaceutical samples. Iodide in an injected zone was oxidized to iodine. A gas diffusion unit enables selective permeation of iodine through a hydrophobic membrane. Detection was made very selective for elemental iodine by employing formation of the I(3)(-)-starch complex. The detection limit (3 S/ N) of the system was 1 mg I L(-1). For a liquid patent medicine used for asthma treatment we suggested modification of the system. Direct injection of this sample, which contains a particularly high concentration level of iodide (ca. 9000 mg I L(-1)), can be achieved by coupling a dialysis unit to the FI system. This has increased the working range to 6000-10,000 mg I L(-1) without employing complicated nanoliter injection.

Continuous and stopped flow injection for catalytic determination of total iodine in urine.

This paper describes the use of flow injection (FI) techniques for the determination of iodine in urine, based on the catalytic effect of iodide in the redox reaction between Ce(IV) and As(III). The proposed procedures minimize errors in the conventional batch method arising from the reading of absorbance at a fixed time after addition of Ce(IV) reagent. Two FI systems, for the continuous and stopped modes of operation were assembled. In the continuous-FI system, a thermostated bath was used to increase the sensitivity. However this is not necessary for the stopped-FI system. The two systems are comparable in terms of sensitivity, sample throughput and detection limit. The continuous-FI and the stopped-FI exhibited detection limits (3 sigma) of 2.3 and 3 micrograms I l-1 respectively. Both systems have equal sample throughputs of 35 samples h-1. Calibration plots for both techniques are linear. The FI procedures provide very short analysis times compared to the batch procedure. Using the linear regression test, there is no significant difference between the results from the four methods, i.e., continuous-FI, stopped-FI, conventional method and ICP-MS. The proposed methods are readily applicable for automation and can be an alternative to the conventional procedure for the survey of the iodine deficiency disorder. A condition for sample digestion is also proposed to reduce the amount of chloric acid required for complete digestion. Kinetic information of the reaction can also be obtained from the stopped flow mode.