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A routine method for the determination of copper is described. After dissolving the sample and adding a KI/KCNS solution, the released iodine is back-titrated with thiosulfate. The endpoint indication is potentiometric.

It has been known for years that consuming too much nitrates from foodstuffs can result in cyanosis, particularly for small children and susceptible adults. According to the WHO standard, the hazard level lies at a mass concentration c(NO3-) ≥ 50 mg/L. However, more recent studies have shown that when nitrate concentrations in the human body are too high, they can (via nitrite) result in the formation of carcinogenic and even more hazardous nitrosamines.Known photometric methods for the determination of the nitrate anion are time-consuming and prone to a wide range of interferences. With nitrate analysis continually increasing in importance, the demand for a selective, rapid, and relatively accurate method has also increased. Such a method is described in this Application Bulletin. The Appendix contains a cselection of application examples where nitrate concentrations have been determined in water samples, soil extracts, fertilizers, vegetables, and beverages.

Potentiometric titration is an accurate method for determining chloride content. For detailed instructions and troubleshooting tips, download our Application Bulletin.

Formaldehyde can be determined reductively at the DME. Depending on the sample composition it may be possible to determine the formaldehyde directly in the sample. If interferences occur then sample preparation may be necessary, e.g. absorption, extraction, or distillation.Two methods are described. In the first method formaldehyde is reduced directly in alkaline solution. Higher concentrations of alkaline or alkaline earth metals interfere. In such cases the second method can be applied. Formaldehyde is derivatized with hydrazine forming the hydrazone, which can be measured polarographically in acidic solution.

The Application Bulletin describes the determination of suppressor in acid copper baths by smartDT. The determination of suppressor with dilution titration (DT) involves numerous additions with standard solution or sample to reach the evaluation ratio. Usually fixed, equidistant addition volumes are used. With smartDT, variable addition volumes are used that are dynamically calculated by the software. At the beginning, the volumes are bigger. Towards the evaluation ratio, the addition volume becomes smaller to guarantee a good accuracy of the result. The operator defines the first and the smallest addition volume to be used. All volumes in between are calculated by the software considering the progress of the determination. The time saving with smartDT compared to a classic DT with fixed addition volumes can be up to 40%. smartDT is suitable for nonlinear regression and quadratic regression as well as linear interpolation. It can be used for determination of suppressor in acid copper baths as well as in tin and tin-lead baths and works with 1, 2, and 3 mm Pt working electrodes. A 800 Dosino is required for the automatic addition of suppressor standard or sample. The method can also be used in fully automated systems.

Copper is arguably one of the most technologically relevant metals, especially for the semiconductor industry. The deposition process used in this industry is known as the dual-damascene process and it involves the electrodeposition of copper from an acidic cupric compound, in the presence of additives.This Application Note illustrates the use of the Autolab rotating ring disc electrode (RRDE) for the study of electrodeposition of copper and the detection of the Cu+ intermediate.

Determination of free acid in copper refining solutions.

Determination of copper, principally in copper mining and refining solutions. The method may also be used fordetermination of purity of copper metal. Optimal results are obtained when aliquots containing copper in the rangeapproximately 3 - 6 mmol Cu are titrated.

Determination of Fe3+ and Cu2+ in copper refining solutions by thermometric titration. It was found that the conventional approach of masking Fe3+ to permit the iodometric determination of Cu2+ is not possible in some copper refining solutions.

Determination of nitrate in a copper plating bath after conversion of nitrate to ammonium. Direct potentiometric measurement using the NH3-ISE.

Monitoring organic additives in copper plating baths is crucial. The 2060 CVS Process Analyzer optimizes copper electroplating by providing precise bath control.

Special brighteners are used in electroplating baths in order to provide the refined surfaces with greater brightness. The concentration of brighteners must be kept constant at all times in order to ensure uniform end product quality. This Application Note describes how brighteners are determined in parallel with IC and CVS. The corresponding CVS application can be found under AN-V-183.

Acid copper baths are mainly used for the copper deposition on semiconductor wafers. Small amounts of chloride increase the speed of deposition and reduce anode polarization. However, higher concentrations are undesired, as this will decrease the quality of the copper deposition. Therefore, it is quite important to monitor the amount of chloride to have an effective, yet high-quality copper deposition process.In this Application Note, a fully automated solution based on titration is presented. In comparison to ion chromatography, titration offers the benefit that no dilution of the sample is necessary, and the hardware is comparatively low-priced. Furthermore, the fully automated solution allows users to minimize handling errors, to reduce workloads, and to guarantee outstanding reproducibility.

Copper can be determined using photometric titration with EDTA at a wavelength of 520 nm.

Determination of suppressor «Copper GleamTM 2001 Carrier» in acid copper baths by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of brightener «Copper GleamTM 2001 Additive» in acid copper baths by modified linear approximation technique (MLAT) using cyclic voltammetric stripping (CVS).

Determination of suppressor «Cupracid BL-CT» in acid copper baths by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of brightener «Cupracid BL» in acid copper baths by linear approximation technique (LAT) using cyclicvoltammetric stripping (CVS).

Determination of suppressor «Cupraspeed» in acid copper baths by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of brightener «Cupraspeed» in acid copper baths by modified linear approximation technique (MLAT)using cyclic voltammetric stripping (CVS).

The concentration of Sb(total) in an acid Cu bath is determined by anodic stripping voltammetry using hydrochloric acid as electrolyte. Due to the excess of Cu the deposition potential has to be chosen only 50 mV more negative than the Sb signal

Determination of suppressor «MACuSpecTM PPR 100 Wetter» in acid copper baths by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of brightener «MACuSpecTM PPR 100 Brightener» in acid copper baths by modified linear approximation technique (MLAT) using cyclic voltammetric stripping (CVS).

Determination of suppressor «MultiBondTM 100 Part A20» in an acid copper bath by dilution titration (DT) using cyclicvoltammetric stripping (CVS).

Determination of suppressor «InPulse H6» in acid copper baths by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of brightener «InPulse H6» in acid copper baths by modified linear approximation technique (MLAT) using cyclic pulse voltammetric stripping (CPVS).

Determination of suppressor «Thru-Cup EVF-B» in acid copper baths by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of brightener «Thru-Cup EVF-1A» in acid copper baths by modified linear approximation technique (MLAT) using cyclic voltammetric stripping (CVS).

Determination of leveler «Thru-Cup EVF-R» in acid copper baths by response curve technique (RC) using cyclic voltammetric stripping (CVS).

The concentration of Cu in a cyanidic Cu bath is determined by polarography.

Determination of suppressor «Top Lucina α-M» in acid copper baths by dilution titration (DT) using cyclic voltammetric stripping (CVS).

Determination of brightener «Top Lucina α-2» in acid copper baths by modified linear approximation technique (MLAT) using cyclic voltammetric stripping (CVS).

Determination of leveler «Top Lucina α-3» in acid copper baths by response curve technique (RC) using cyclic voltammetric stripping (CVS).

The determination of suppressor with dilution titration (DT) involves numerous additions with standard solution or sample to reach the evaluation ratio. Usually fixed, equidistant addition volumes are used. With smartDT, variable addition volumes are used that are automatically calculated by the software. At the beginning, the volumes are bigger. Towards the evaluation ratio, the addition volume becomes smaller to guarantee a good accuracy of the result. The operator defines the first and the smallest addition volume to be used. All volumes in between are calculated by the software considering the progress of the determination. Using smartDT with intelligent addition volumes, the determination of suppressor can be significantly accelerated with the same or even better accuracy than with the classic DT. The time saving per determination is between 20 and 40%.

brightRC enables reliable CVS (or CPVS) brightener quantification without repeated standard additions, especially for additive systems with nonlinear signal behavior. By using external response curve (RC) calibration and flexible regression, it avoids systematic errors inherent to linear standard addition methods and significantly reduces analysis time. This makes brightRC ideal for high throughput routine control in stable copper plating baths.

For the past three decades, Cyclic Voltammetric Stripping (CVS) has been the standard practice for analyzing organic additives in electroplating copper baths in the circuit board and wafer plating industries. The variations in the compositions of such baths have created a need for more optimized method development routines. New advancements in the hardware and software protocols for CVS have simplified the overall process of method optimization to a great extent. In this study, the process of method optimization is discussed in conjunction with these protocols.

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