Determination of the Content of Fluorine and Chlorine in Inorganic Insulation Materials by Ion Chromatography

2018 ◽  
Vol 768 ◽  
pp. 41-45
Author(s):  
Shi Hua Liu ◽  
Qing Dan Yuan ◽  
Peng Chen ◽  
Xuan Li ◽  
Di Shao

A fast and accurate method for simultaneous determination of the content of fluorine and chlorine in inorganic thermal insulation materials by ion chromatography was developed. The samples were cut into pieces of weight less than 40mg, washed with water as the extractant, heated for 30 min and then centrifuged, filtered through a 0.22 μm microporous membrane, and the cation was removed using a SEP-H column. The solution was rinsed with 20/30 mM KOH as the mobile phase, separated by anion exchange column and then detected using a conductivity detector. The mass concentration of fluorine and chlorine in the range of 0.1-10mg/L was linearly related to their peak area, the detection limit of fluorine was 0.030mg/Land the detection limit of chlorine was 0.016mg/L. The relative standard deviations (n=6) of the three typical inorganic insulating materials (glass wool, rock wool and mineral wool) were less than 2.0% and the rate of recovery of fluoride and chloride ion was between 97% and 101%.The method had good accuracy and recovery rate. The absolute error of the measured value between ion chromatography and the national standard was less than 0.20%.The results showed that the method was suitable for the determination of the content of fluorine and chlorine in inorganic thermal insulation materials

Author(s):  
E. Esteve-Juan ◽  
R. Puchades ◽  
A. Maquieira

A method for acetate determination using IC separation and FI post-column spectrophotometric detection based on the La(OH)3-I2 reaction has been developed. The chromatographic conditions (eluants, flow-rates, sensitivity, and so on) and FI variables (length of coils, injection volume, pH, ... ) were optimized. Linearity was observed over the concentration range 0 to 1 gl-1 with HAc as standard (r = 0.9916) and a detection limit of 0.1 g AcH/l. The IC-FI method afforded a low relative standard deviation (3.6%) and was free from interferences. The IC-FI procedure was applied to the determination of acetate in mustard sauce and the results obtained agree with those provided by the reference method. Additionally, the developed method permits the simultaneous chromatographic analysis of other anions such as chloride, nitrate, phosphate, sulphate, and so on.


2014 ◽  
Vol 1033-1034 ◽  
pp. 558-562 ◽  
Author(s):  
Wei Qu ◽  
Cheng Ying Zhou ◽  
Shuang Liu

A method was proposed for the determination of copper, iron, nickel, lead, cadmium and chromium in electroplating wastewater by ICP-AES. Working conditions and selection of spectral lines were optimized. The mixed and single standard for 6 elements were analyzed, spectrum with high sensitivity, low spectral interference, high ratio of signal with background, low detection limit were selected. The detection limit was 0.002, 0.003, 0002, 0.008, 0.002, 0.007mg/L. The effects of inhalation rate and the spectral intensity in nitric acid, hydrochloric acid, perchloric acid and sulfuric acid solution were tested. Nitrate acid with low viscosity, low surface tension and high atomization efficiency was selected. The accuracy and precision were tested, the relative error was less than 5.2%, relative standard deviation was less than 2.4%.It was accord with national standard. It proved that the determination of copper, iron, nickel, lead, cadmium and chromium in electroplating wastewater by ICP-AES was feasible.


1989 ◽  
Vol 54 (3) ◽  
pp. 616-621 ◽  
Author(s):  
Záviš Holzbecher

It has been found that phosphoric acid decreases the first excitation maximum of Ce(III) at 256 nm, increases the second excitation maximum at 297 nm and shifts the fluorescence maximum from 350 to 346 nm. Under optimum conditions, with λexc = 297 nm and λem = 346 nm, Ce(III) can be determined fluorimetrically with a detection limit of 1.2 ng ml-1 in 12M-H3PO4 medium. No interference was observed from a 20-200 fold excess of HCl, H2SO4, Na, K, NH4+, Al and the rare earth elements. HNO3 interferes and Ce(IV) and Fe(III) interfere strongly. It follows from the stereofluorograms of Ce and Tb that the spectra of the two elements are practically independent. The detection limit for Tb(III) in 0.02-2.5M-H2SO4 medium for λexc = 222 nm and λem = 494 nm is 33 ng ml-1. No interference was observed from a 5-20 fold excess of Al3+ and the other rare earth elements. The determination is slightly less sensitive in H3PO4 or HCl medium. The relative standard deviation of the measurement for 10 ng ml-1 Ce(III) or 50 ng ml-1 Tb(III) is about 3%.


Author(s):  
Elena Yusenko ◽  
Evgeniya Polyntseva ◽  
Anna Lyzhova ◽  
Olga Kalyakina

Abstract Oxalate concentration differs in various daily consumed food products. The role of oxalic acid in the human body is very significant, as its compounds are responsible for the stability of biological membranes. However, insoluble calcium and magnesium oxalates can be accumulated in the body in the form of kidney stones. Oxalate concentration has been measured by high performance liquid, gas after derivatization and ion chromatography (IC). The most effective method for the simultaneous determination of oxalate and inorganic anions is ion chromatography with conductometric detection. Here, we report the results of the measurement of oxalic acid in bleak and green tea samples. Separation was performed by IC on an anion-exchange column Shodex IC SI-90 with surface-layer sorbent and conductimetric detection. The main analytical features of the method were: limit of detection of oxalic acid 0.03 mg/l, linear range 0.1-20 mg/l, correlation 0.9998, relative standard deviation 1%. The method did not need specific sample treatment and was successfully applied to the analysis of black and green tea samples. Oxalic acid was determined in the ranges 16.7-84 mg/l for green tea and 63-116 mg/l for black tea. Green tea contained lower oxalate ions concentration than black tea. The IC method has a lower detection limit for oxalate ions than HPLS and GC, ten and two times less, respectively


2018 ◽  
Vol 33 (2) ◽  
pp. 47
Author(s):  
Orlando Fatibello-Filho ◽  
Heberth Juliano Vieira

A spectrophotometric flow injection method for the determination of paracetamol in pharmaceutical formulations is proposed. The procedure was based on the oxidation of paracetamol by sodium hypochloride and the determination of the excess of this oxidant using o-tolidine dichloride as chromogenic reagent at 430 nm. The analytical curve was linear in the paracetamol concentration range from 8.50 x 10-6 to 2.51 x 10-4 mol L-1 with a detection limit of 5.0 x 10-6 mol L-1. The relative standard deviation was smaller than 1.2% for 1.20 x 10-4 mol L-1 paracetamol solution (n = 10). The results obtained for paracetamol in pharmaceutical formulations using the proposed flow injection method and those obtained using a USP Pharmacopoeia method are in agreement at the 95% confidence level.


2001 ◽  
Vol 84 (1) ◽  
pp. 59-64 ◽  
Author(s):  
Inês P A Morais ◽  
António O S S Rangel ◽  
M Renata S Souto

Abstract A turbidimetric flow-injection system was developed for the determination of sulfate in natural and residual water samples, with no previous treatment, using spectrophotometric detection. The precipitating agent, 7.0% (w/v) barium chloride solution prepared in 0.10% (w/v) polyvinyl alcohol, was added by using the merging-zones approach. A 100 mg/L sulfate solution in 0.07M nitric acid was mixed with the sample before it entered the injection loop to improve the detection limit, provide in-line pH adjustment, and prevent the interference of some anionic species. The relative standard deviations of the results were between 1.4 and 3.0% and were in agreement with results obtained by the reference method. Samples within a linear concentration range of 10–120 mg SO42−/L can be analyzed at a rate of 40/h. The detection limit is 5 mg SO42−/L.


2011 ◽  
Vol 2011 ◽  
pp. 1-5
Author(s):  
Ayushi D. ◽  
Arijit Sengupta ◽  
Sangita D. Kumar ◽  
A. G. Kumbhar ◽  
G. Venkateswaran

A simple, rapid and accurate method for the determination of monoethanolamine (MEA) in PHWR steam-water circuits has been developed. MEA is added in the feed water to provide protection against corrosion while hydrazine is added to scavenge dissolved oxygen. The quantitative determination of MEA in presence of hydrazine was accomplished using derivatization ion chromatography with conductometric detection in nonsuppressed mode. A Metrosep cation 1-2 analytical column and a Metrosep cartridge were used for cation separation. A mixture of 4 mM tartaric acid, 20% acetone and 0.05 mM HNO3was used as eluent. Acetone in the mobile phase leads to the formation of different derivatives with MEA and hydrazine. The interferences due Na+and NH4 +were eliminated by adopting a simple pretreatment procedure employing OnGuard-H cartridge. The limit of detection limit of MEA was 0.1 μg mL−1and the relative standard deviation was 2% for the overall method. The recovery of MEA added was in the range 95%–102%. The method was applied to the determination of MEA in steam generator water samples.


2016 ◽  
Vol 680 ◽  
pp. 52-55
Author(s):  
Hong Yan Guan ◽  
Jian Jun Ding ◽  
Zhong Bao Guo ◽  
Ming Yu Wang ◽  
Yi Fei Mei

The determination of chloride ions in concrete materials accurately is far and away crucial, since chloride ions can cause corrosion of steel and concrete cover off. The conventional potential method and silver nitrate titration method usually show features of simple operation and short duration, nevertheless, they are not suitable for accurate analysis for concrete attributing to their low accuracy and detection limit. In this paper, an ion chromatography method was presented to determine chlorine in concrete materials. Concrete samples were pre-processed and then extracted with distilled water. The extraction solutions were purified on a 0.22 μm filter membrane, an On Guard SPE-RP column and a SPE-H column sequentially for eliminating undissolved substance, organisms and metal ions before ion chromatographic analysis. The chromatographic separation was performed on a Dionex ICS-1000 Chromatographic using 25.0 mmol/L KOH solutions as mobile phase at 1.0 mL/min. Results show that the detection limit of the method was 0.004 mg/L. The linear relationship of the external Cl- standard solutions was 0.9994, and the sample analytical RSD was 0.44%.


2018 ◽  
Vol 5 (4) ◽  
pp. 172128 ◽  
Author(s):  
Ming Ding ◽  
Kailiang Wang

A practical method for the determination of cyanide in bamboo shoots has been developed using microdiffusion preparation integrated with ion chromatography–pulsed amperometric detection (IC-PAD). Cyanide was released from bamboo shoots after Conway cell microdiffusion, and then analysed by IC-PAD. In comparison with the previously reported methods, derivatization and ion-pairing agent addition were not required in this proposed microdiffusion combined with IC-PAD method. The microdiffusion parameters were optimized including hydrolysis systems, temperature, time, and so on. Under the optimum conditions, the linear range of the calibration curve for cyanide was 0.2–200.0 µg kg −1 with satisfactory correlation coefficients of 0.9996 and the limit of detection was 0.2 µg kg −1 ( S/N  = 3). The spiked recovery range was from 92.8 to 98.6%. The intra-day and inter-day relative standard deviations of cyanide were 2.7–14.9% and 3.0–18.3%, respectively. This method was proved to be convenient in operation with high sensitivity, precision and accuracy, and was successfully applied in the determination of cyanide in bamboo shoot samples.


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