硫酸銅電解浴中のにかわの定量
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Glue has been widely used as an addition reagent for the acid copper plating baths. The situation of the glue in the plating baths are devided into decomposed glue and remained glue, and the results of their rational analysis were represented by three values of (1) total glue, (2) remained glue and (3) decomposed glue. The three methods of determination are different only in the preliminary treatment of the sample and the sample solutions with appropriate pretreatment are subjected to Kjeldahl digestion and Nessler photometry for determination of total nitrogen amounting to about 10% in glue. The recommended procedures are as follows pretreatment: (1) Total glue. Two milliliters of sulfuric acid, 35 mg of mercuric oxide and 0.5 m<I>l</I> of 30% hydrogen peroxide are added to the sample solution. It is evaporated to fumes and transferred to a 50 m<I>l</I> distillation flask with a small amount of water. (2) Remained glue. The sample solution in a 100 m<I>l</I> Erlenmeyer flask is neutralized with 50% (w/v) sodium hydroxide and then 2 m<I>l</I> in excess. It is kept on a boiling water bath for 90 min. with aeration to remove the decomposition product. After cooling and neutrarization with sulfuric acid, the procedure (1) for total glue is carried through. (3) Decomposed glue. The sample solution is directly placed into the distillation flask.<BR>Distillation and color development: Connect the distillation flask with a steam distillation apparatus. Place a receiver containing 1.0 m<I>l</I> of water. The height of the end of the delivery tube is adjusted to dip into the surface of the water. Add 20 m<I>l</I> of 30% (w/v) sodium hydroxide solution to the flask from funnel and carry out the steam distillation. Remove the receiver when the distillate amounts to 9.5 m<I>l</I>. Add 0.2 m<I>l</I> of Nessler reagent and make up to 10 m<I>l</I> with water. Allow to stand for 15 min. and measure the absorbance at 420 nm against a reagent blank.<BR>The sensitivity is 59 μg glue/cm<SUP>2</SUP> for an absorbance of 0.1. The ingredients in common plating baths including H<SUB>2</SUB>SO<SUB>4</SUB>, Cu, Ni, Bi, As, Sb, Sn and Zn do not interfere.
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- 硫酸銅電解浴中のにかわの定量