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Plating layer of Ni and Pd in the spectrophotometric

Sample solution was tested. 2ml sample solution from each of the experimental method by rough measurement, and then take the right amount based on measurements of sample solution, precious metals by experimental methods for 6 parallel determinations. The results shown in Table ①. The conversion was informed that the plating layer above the content of the sample M were 15.9%, 24.3% and 19% in Hong Kong. ⑧ method accuracy and detection limits: Apply the sample plating solution,[link widoczny dla zalogowanych], the addition of a certain amount of Ni standard solution, the method of sample determination by the determination of the recovery obtained, the results shown in Table ②. Press 2 times the standard deviation of the blank and slope of working curve is defined as the ratio of detection limit, the method detection limit of nickel measured 0.1756pg/ml. Table ① Ni plating layer of the determination of the sample {. 1g/25m1) MeasurementofNiinelectroplatedlayers3.2IM Determination: ① complex absorption spectra and first derivative spectra: in the wavelength range 350.0 ~ 700.0nm with the United States BeckmanDU 7HS spectrophotometer scan of a Pd complex was The absorption spectrum (Figure ①), obtained by the conversion of the first derivative spectra (Figure ②) Figure ① that the complex absorption maximum at 4O7.5nm. ② we can see from the chart, the first derivative of complex peaks and troughs fall 425.0nm and 388.5nm,[link widoczny dla zalogowanych], respectively, at. Therefore, select the 425.0nm and 388.5nm this as a first derivative of the measurement wavelength (peak a peak method). ② the influence of pH on complex formation: Experiments show that when the sulfuric acid solution used in the dosage of 1:3 1 ~ 7ml, the measured absorbance of the largest and most stable. Therefore, this paper select Add 2.0ml of sulfuric acid solution. ③ reagent dosage and protection of choice: Experiments show that the amount of potassium iodide solution in 0.8 ~ 2.5ml, ascorbic acid content between the 1.0-3.0ml, the measured absorbance of the largest and most stable . Therefore, this paper plus ascorbic acid solution of potassium iodide solution, 2.5ml and 2.0ml. ④ rate of complex formation and stability of time: at room temperature and acidic potassium iodide solution Pd rapid response, immediate color. The one in the United States BeckmanDU 7HS spectrophotometer automatically scan, the results showed that the absorbance at 90mln essentially unchanged. m Figure ② Pd in the first derivative spectra of ions ThefirstderivativespectrLanofPd ⑤: According to the actual situation of the sample plating, coating attached to cu, can be soaked in chromic acid lotion to remove, in addition to the solution containing Ni2, cl a, NO3 ions in the first class the highest level possible under the determination of Pd had no effect on them although the complex Ni2 absorbance have a certain influence, but by seeking to eliminate the first derivative of its impact. ⑥ Work Curve: in 7 were transferred into 25ml volumetric flask in different amounts of Pd standard solution,[link widoczny dla zalogowanych], the contents of which were 0,[link widoczny dla zalogowanych],20,40,60,80,1 ∞ pd2 and 120gg. The following steps by determination of the experimental method. To measure the value of precious metals the first derivative dA / n Pd content of the corresponding working curve derived mapping. The fitted equations for dA / n = 2.15CPd +1.214, c ~ of the unit / 25II】 l, the correlation coefficient 7 = 0.9998. ⑦ determination of plating samples: from each of the above sample solution 2ml, rough measurement by experimental methods, and then take the right amount based on measurements of sample solution, according to experimental methods for 6 parallel determinations. The results shown in Table ③. The conversion was informed that the plating layer above the Pd content of the sample were 84.1%,[link widoczny dla zalogowanych], 75.7% and 80.2%. ⑧ accuracy of the method: Apply the sample plating solution, the addition of a certain amount of Pd standard solution, the method of sample determination by the determination of the recovery obtained, the results shown in Table ④. Table ③ Pd plating layer of the determination of the sample results (Xu _/25) MeasurementofPdinelectroplatedlayers Table ④ accurate results (/ 25) ExperimentalaccuracyandrecoveryratioofPd References 1 amidine Guozhen and so on. Uv-visible spectrophotometry (the book). Beijing: Atomic Energy Publishing Du. 1.277 ~ 289:322 ~ 3342 King enshrined in a camp such as nickel stone roller PTFE coated chemical re-filling station in the sickle and the determination of hypophosphite attack. Analytical Chemistry, 1997,25 (12): 14 (~ 63 Wang enshrined in irrigation, such as electroplating Spectrophotometric determination of palladium in Zhangzhou Normal College, a dragonfly, 10 (2): 8385

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