Electroless nickel plating bath containing glycine and sodium citrate as chelating agent by means of deposition rate, bath life and phosphorous content in the deposited films was studied and simultaneous analysis of ions in plating bath by isotachophoresis was tried. Bath composition was; NiSO4⋅6H2O 30g/L, NaH2PO2⋅H2O 30g/L, NH2CH2COOH 40g/L, Na3C6H5O7⋅2H2O 20g/L, Pb(NO3)2 2mg/L. Plating area was 400cm2; bath volume was 4L; and bath temperature 88±2°C. The supply solution was NiSO4⋅6 H2O 450g/L, NaH2PO2⋅H2O 500g/L, Pb(NO3)2 60mg/L. The deposition rate from this bath was 0.2-0.3μm/min, 2-3 times faster than the general malic acid bath. Bath life was more than 50 hours in continuous plating and about 6 turns could be obtained. Though phosphorous content in the deposited films depended on bath pH and the amount of sodiun hypophosphite, phosphorous content could be kept to 5-13wt% or 12wt% constant by adjustng the concentrations of nickel sulfate and sodium hypophosphite in the supply solution. Bath composition was so changed with plating that analysis of ions in the plating solution by isotachophoresis using 0.01mol HCl leading solution and 0.01mol sodium caproate terminal solution was tried. As a result of it, concentrations of hypophosphite, phosphite, phosphate ions and also of citric acid ion could be analysed simultaneously and with high precision.