“…It is usually necessary to use a glass rod to push the filter to the cylinder bottom. After the filter is placed in the 0.04M TCM, add 1 ml sulfamic acid for nitrite interference elimination (9). Mix gently, wait 5 min; add 1 ml HCHO solution, mix gently, wait 5 min; and finally add 1 ml PRA, again mixing gently.…”
0.2mM were stable and sufficiently concentrated to give quantitative results. The thiocyanate concentration was found to be important in driving the reaction to completion and affected the rate of complex formation. Low absorbances observed at concentrations less than about 0.2M might, in part, result from the decomposition of I(SCN)zto form the non-absorbing ISCN (IO).Hydrogen ion concentrations were about 1M in all cases.Lower concentrations caused a slight decrease in stability and higher concentrations (above 2-3M) led to the decomposition of thiocyanic acid (9).Absorbance measurements on thirty separately prepared solutions are shown in Table I. Precision of replicate measurements is good and the overall accuracy has a range of about f3%. A linear least squares fit to the data gives a slope of 41100 f 200 1. mol-' cm-l and a y-intercept of Possible interferences from extraneous ions were examined. Table I1 summarizes these observations. In each case, two solutions of identical iodide concentrations were compared with an extraneous ion added to one. These were carried through the procedure in parallel.Clearly, chloride presents no serious interference at the levels examined and bromide lowers the absorbance only a few percent. The fact that the chloride interference does not change with chloride concentration suggests that the 2% difference in absorbance may be a measurement error rather than an interference. Sulfate, a frequent interference in iodide analyses, causes a small decrease in absorbance.The transition metal ions interfered to varying extents. Since thiocyanate complexes form with these cations, interferences are to be expected.-0.003.
“…It is usually necessary to use a glass rod to push the filter to the cylinder bottom. After the filter is placed in the 0.04M TCM, add 1 ml sulfamic acid for nitrite interference elimination (9). Mix gently, wait 5 min; add 1 ml HCHO solution, mix gently, wait 5 min; and finally add 1 ml PRA, again mixing gently.…”
0.2mM were stable and sufficiently concentrated to give quantitative results. The thiocyanate concentration was found to be important in driving the reaction to completion and affected the rate of complex formation. Low absorbances observed at concentrations less than about 0.2M might, in part, result from the decomposition of I(SCN)zto form the non-absorbing ISCN (IO).Hydrogen ion concentrations were about 1M in all cases.Lower concentrations caused a slight decrease in stability and higher concentrations (above 2-3M) led to the decomposition of thiocyanic acid (9).Absorbance measurements on thirty separately prepared solutions are shown in Table I. Precision of replicate measurements is good and the overall accuracy has a range of about f3%. A linear least squares fit to the data gives a slope of 41100 f 200 1. mol-' cm-l and a y-intercept of Possible interferences from extraneous ions were examined. Table I1 summarizes these observations. In each case, two solutions of identical iodide concentrations were compared with an extraneous ion added to one. These were carried through the procedure in parallel.Clearly, chloride presents no serious interference at the levels examined and bromide lowers the absorbance only a few percent. The fact that the chloride interference does not change with chloride concentration suggests that the 2% difference in absorbance may be a measurement error rather than an interference. Sulfate, a frequent interference in iodide analyses, causes a small decrease in absorbance.The transition metal ions interfered to varying extents. Since thiocyanate complexes form with these cations, interferences are to be expected.-0.003.
“…al. 5 On two different days bubblers were used to measure SO2 in Denver. Parallel sampling was done with either no filter or a prefilter placed in front of the bubbler.…”
“…The proposed μFBA method uses the same p-rosanilineformaldehyde-sulfite reaction seen in previous papers, [11][12][13][14] and known for more than 50 years. 26 Sulfite reacts with formaldehyde and p-rosaniline (acidified with hydrochloric acid) to form a highly conjugated alkyl amino sulfonic acid, which presents an intense purple coloration and maximum absorption at 560 nm. 11,27 The μFBA uses an integrated detection system, which employs a high intensity green LED with a maximum wavelength of 565 nm as its radiation source, a phototransistor as its detector, and a very simple electronic circuit described in detail elsewhere.…”
An automated microsystem for sulfite determination in beverages was developed. It presents higher sampling throughput, lower chemical consumption and less waste generation than previous flow methods, while using the same p-rosaniline-formaldehyde-sulfite reaction. The sampling rate, limit of detection (LOD), and relative standard deviation (RSD) were estimated at 130 h −1 , 80.0 μg L-1 , and < 1.3% (n = 5), respectively. Recoveries ranged from 96.8 to 102.6%.
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