“…From this we derive a limit of detection (c L ) of 0.1 µM (background corrected signal). c L was calculated according to Long and Winefordner (1983) and is equal to 3 times the background signal standard deviation divided by the sensitivity. With respect to smog chamber experiments our detection limit for a sampling volume of 500 l is 0.52 nmol m −3 , which is about 2000 times lower than the one reported by Docherty et al (2005).…”
Abstract.A new off-line instrument to quantify peroxides in aerosol particles using iodometry in long path absorption spectroscopy has been developed and is called peroxide long path absorption photometer (Peroxide-LOPAP). The new analytical setup features important technical innovations compared to hitherto published iodometric peroxide measurements. Firstly, the extraction, chemical conversion and measurement of the aerosol samples are performed in a closed oxygen-free (∼ 1 ppb) environment. Secondly, a 50-cm optical detection cell is used for an increased photometric sensitivity. The limit of detection was 0.1 µM peroxide in solution or 0.25 nmol m −3 with respect to an aerosol sample volume of 1 m 3 . The test reaction was done at a constant elevated temperature of 40 • C and the reaction time was 60 min.Calibration experiments showed that the test reaction with all reactive peroxides, i.e. hydrogen peroxide (H 2 O 2 ), peracids and peroxides with vicinal carbonyl groups (e.g. lauroyl peroxide) goes to completion and their sensitivity (slope of calibration curve) varies by only ±5 %. However, very inert peroxides have a lower sensitivity. For example, tert-butyl hydroperoxide shows only 37 % sensitivity compared to H 2 O 2 after 1 h. A kinetic study revealed that even after 5 h only 85 % of this inert compound had reacted.The time trends of the peroxide content in secondary organic aerosol (SOA) from the ozonolysis and photooxidation of α-pinene in smog chamber experiments were measured. The highest mass fraction of peroxides with 34 % (assuming a molecular weight of 300 g mol −1 ) was found in freshly generated SOA from α-pinene ozonolysis. Mass fractions decreased with increasing NO levels in the photooxidation experiments. A decrease of the peroxide content was also observed with aging of the aerosol, indicating a decomposition of peroxides in the particles.
“…From this we derive a limit of detection (c L ) of 0.1 µM (background corrected signal). c L was calculated according to Long and Winefordner (1983) and is equal to 3 times the background signal standard deviation divided by the sensitivity. With respect to smog chamber experiments our detection limit for a sampling volume of 500 l is 0.52 nmol m −3 , which is about 2000 times lower than the one reported by Docherty et al (2005).…”
Abstract.A new off-line instrument to quantify peroxides in aerosol particles using iodometry in long path absorption spectroscopy has been developed and is called peroxide long path absorption photometer (Peroxide-LOPAP). The new analytical setup features important technical innovations compared to hitherto published iodometric peroxide measurements. Firstly, the extraction, chemical conversion and measurement of the aerosol samples are performed in a closed oxygen-free (∼ 1 ppb) environment. Secondly, a 50-cm optical detection cell is used for an increased photometric sensitivity. The limit of detection was 0.1 µM peroxide in solution or 0.25 nmol m −3 with respect to an aerosol sample volume of 1 m 3 . The test reaction was done at a constant elevated temperature of 40 • C and the reaction time was 60 min.Calibration experiments showed that the test reaction with all reactive peroxides, i.e. hydrogen peroxide (H 2 O 2 ), peracids and peroxides with vicinal carbonyl groups (e.g. lauroyl peroxide) goes to completion and their sensitivity (slope of calibration curve) varies by only ±5 %. However, very inert peroxides have a lower sensitivity. For example, tert-butyl hydroperoxide shows only 37 % sensitivity compared to H 2 O 2 after 1 h. A kinetic study revealed that even after 5 h only 85 % of this inert compound had reacted.The time trends of the peroxide content in secondary organic aerosol (SOA) from the ozonolysis and photooxidation of α-pinene in smog chamber experiments were measured. The highest mass fraction of peroxides with 34 % (assuming a molecular weight of 300 g mol −1 ) was found in freshly generated SOA from α-pinene ozonolysis. Mass fractions decreased with increasing NO levels in the photooxidation experiments. A decrease of the peroxide content was also observed with aging of the aerosol, indicating a decomposition of peroxides in the particles.
“…The LOD is usually defined as the analyte concentration that produces an analytical signal equivalent to three times the standard deviation observed for 16 measurements of a blank solution. (48) Another definition for the LOD of ICP-OES is related to the SBR of the analyte line at a given concentration, c, and the relative standard deviation (RSD) of the background, RSD B as shown in Equation (9) (49) :…”
Inductively coupled plasma/optical emission spectrometry (ICP/OES) is a powerful tool for the determination of metals in a variety of different sample matrices. With this technique, liquid samples are injected into a radiofrequency (RF)-induced argon plasma using one of a variety of nebulizers or sample introduction techniques.The sample mist reaching the plasma is quickly dried, vaporized, and energized through collisional excitation at high temperature. The atomic emission emanating from the plasma is viewed in either a radial or axial configuration, collected with a lens or mirror, and imaged onto the entrance slit of a wavelength selection device. Single element measurements can be performed costeffectively with a simple monochromator/photomultiplier tube (PMT) combination, and simultaneous multielement determinations are performed for up to 70 elements with the combination of a polychromator and an array detector. The analytical performance of such systems is competitive with most other inorganic analysis techniques, especially with regards to sample throughput and sensitivity.
“…The limit of quantification [38,39] and the limit of detection, as defined by IUPAC [40] were found to be 1.02 ng mL -1 and 0.35 ng mL -1 , respectively. Ten replicate determinations of a standard geological sample containing 0.01 µg g -1 of gold(III) using the general procedure gave a relative standard deviation of 1.09%.…”
A excellent sensitive and selective method for spectrophotometric determination of trace gold has been developed, the method is based on the color reaction of gold(III) with new reagent 5-(2-hydroxy-5-nitrophenylazo)rhodanine (HNAR). Under optimal conditions, HNAR reacts with gold(III) to form a 1:5 orange complex, which has an maximum absorption peak at 480 nm. Maximum enhancement of the absorbance of the complex was obtained in the presence of the mixed surfactant of Triton X-100 and CTMAB; the reaction completed rapidly and the absorbance is stable for 5 h at least at 20 degrees C; 0-48 microg L(-1) Au(III) obeyed Beer's law. The apparent molar absorptivity of the complex, Sandell's sensitivity, the limit of quantification, the limit of detection and relative standard deviation were found to be 2.0x10(6) L mol(-1) cm(-1), 0.000,098,483 micro g cm(-2), 1.02 ng mL(-1), 0.35 ng mL(-1) and 1.09%, respectively. The effect of co-existing ions was studied seriously; most metal ions can be tolerated in considerable amounts. Its sensitivity and selectivity are remarkably superior to other reagents in the literature. The proposed method was used successfully to determine trace gold in geological samples. Moreover, the synthesis, characteristics and analytical reaction of HNAR with gold are also described in detail.
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