scholarly journals Green Chemistry: A Simple Manual Apparatus for Potentiometric and Conductometric Micro-Titration of Small Samples for the Educational Laboratory

2021 ◽  
Vol 16 (1) ◽  
pp. 13-20

A simple manual micro-titration method is proposed for the potentiometric and conductometric titration of 200 to 800 µL of liquid samples. The sample to be titrated is dispensed into the titration chamber; the bottom section of a plastic test tube that is glued to the center of a small stirring magnet. After inserting the sensing probe and the tip of the titrant delivery tip into the titration chamber, the chamber-stirring magnet assembly is spun at low speed using a conventional magnetic stirrer. Titrant is delivered (with 0.2 µL resolution) from the submerged tip of a 100-µL capacity micro-pipette by rotating the plunger with the locking ring unlocked. The apparatus has been used for potentiometric titration and conductometric titration of acids and bases usually encountered in educational laboratories. Compared with macro-scale titrations, the obtained accuracy was between +2.2% and -3.9% relative error and the precision ranged between 1.6% and 2.9% relative standard deviation. The proposed procedure cuts the reagent consumption to 1% or less compared with conventional macro-scale titrations.

2019 ◽  
Vol 70 (10) ◽  
pp. 3555-3560
Author(s):  
Costinela Valerica Georgescu ◽  
Cristian Catalin Gavat ◽  
Doina Carina Voinescu

Ascorbic acid is a water-soluble vitamin provided with strong antioxidant action, that fulfills an important immune protective role of the body against infections and prevents various cancers appearance. The main goal of this study was to exactly quantify pure ascorbic acid in tablets of two pharmaceuticals. Proposed objective consisted in improvement and application of a iodometric titration method in ascorbic acid quantitative analysis. Ascorbic acid content per tablet in both studied pharmaceuticals was 173.84 mg, very close to official stated amount of active substance (180 mg). Allowed percentage deviation from declared content of pure ascorbic acid was only 3.42 %, below maximum value of � 5 % imposed by Romanian Pharmacopoeia 10-th Edition, according to European and International standards. Statistical analysis confirmed experimental obtained results and revealed low Standard Error value SE = 0.214476, which has fallen within normal limits. Confidence Level value (95.0 %) = 0.551328 and Standard Deviation SD = 0.525357. were within normal range of values. Relative Standard Deviation (Coefficient of variation or homogeneity) RSD = 26.268% was found below maximum range of accepted values (30-35%). P value = 7.44. 10-6 was located within normal limits, P [ 0.001, so the experimental obtained results has shown highest statistical significance. Thus, studied titration method can be successfully used in quantitative analysis of ascorbic acid from different samples.


1984 ◽  
Vol 67 (5) ◽  
pp. 893-895
Author(s):  
Ivan Sekerka ◽  
Josef F Lechner

Abstract The alkalinity and acidity of water are parameters of great importance for studies of aquatic ecosystems. This paper describes the determination of total alkalinity by using acid-base titration with trichloroacetic acid solution as titrant. Total acidity is determined by titration with ammonium hydroxide solution. Both titrations are monitored conductometrically. Performance is evaluated and compared with performance of the potentiometric titration. Automated conductometric titration is simple, fast (30 s/titration), sensitive (detection limit 0.1 ppm CaC03), and accurate. Relative error of the determination increased from about 1% at high levels to about 10% at 1 ppm CaC03. The relative standard deviation of alkalinity measurements ranged from to 5%; for acidity, these values ranged from 1.5 to 17%. Relative standard deviation reached 33% at lower detection limits. Samples containing noncarbonate contributory components of alkalinity (borate, silicate, phosphate, organic acids) can be reproducibly analyzed.


2019 ◽  
Vol 70 (10) ◽  
pp. 3555-3560

Ascorbic acid is a water-soluble vitamin provided with strong antioxidant action, that fulfills an important immune protective role of the body against infections and prevents various cancers appearance. The main goal of this study was to exactly quantify pure ascorbic acid in tablets of two pharmaceuticals. Proposed objective consisted in improvement and application of a iodometric titration method in ascorbic acid quantitative analysis. Ascorbic acid content per tablet in both studied pharmaceuticals was 173.84 mg, very close to official stated amount of active substance (180 mg). Allowed percentage deviation from declared content of pure ascorbic acid was only 3.42 %, below maximum value of ± 5 % imposed by Romanian Pharmacopoeia 10-th Edition, according to European and International standards. Statistical analysis confirmed experimental obtained results and revealed low Standard Error value SE = 0.214476, which has fallen within normal limits. Confidence Level value (95.0 %) = 0.551328 and Standard Deviation SD = 0.525357. were within normal range of values. Relative Standard Deviation (Coefficient of variation or homogeneity) RSD = 26.268% was found below maximum range of accepted values (30-35%). P value = 7.44. 10-6 was located within normal limits, P < 0.001, so the experimental obtained results has shown highest statistical significance. Thus, studied titration method can be successfully used in quantitative analysis of ascorbic acid from different samples. Keywords: ascorbic acid, antioxidant action, quantitative analysis, iodometric titration, statistic study


Author(s):  
P.F. Collins ◽  
W.W. Lawrence ◽  
J.F. Williams

AbstractA procedure for the automated determination of ammonia in tobacco has been developed. Ammonia is extracted from the ground tobacco sample with water and is determined with a Technicon Auto Analyser system which employs separation of the ammonia through volatilization followed by colourimetry using the phenate-hypochlorite reaction. The procedure has been applied to a variety of tobaccos containing from 0.02 to 0.5 % ammonia with an overall relative standard deviation of 2 %. The accuracy of the procedure as judged by recovery tests and by comparison to a manual distillation method is considered adequate


2020 ◽  
Author(s):  
Saneyuki Ohno ◽  
Tim Bernges ◽  
Johannes Buchheim ◽  
Marc Duchardt ◽  
Anna-Katharina Hatz ◽  
...  

<p>Owing to highly conductive solid ionic conductors, all-solid-state batteries attract significant attention as promising next-generation energy storage devices. A lot of research is invested in the search and optimization of solid electrolytes with higher ionic conductivity. However, a systematic study of an <i>interlaboratory reproducibility</i> of measured ionic conductivities and activation energies is missing, making the comparison of absolute values in literature challenging. In this study, we perform an uncertainty evaluation via a Round Robin approach using different Li-argyrodites exhibiting orders of magnitude different ionic conductivities as reference materials. Identical samples are distributed to different research laboratories and the conductivities and activation barriers are measured by impedance spectroscopy. The results show large ranges of up to 4.5 mScm<sup>-1</sup> in the measured total ionic conductivity (1.3 – 5.8 mScm<sup>-1</sup> for the highest conducting sample, relative standard deviation 35 – 50% across all samples) and up to 128 meV for the activation barriers (198 – 326 meV, relative standard deviation 5 – 15%, across all samples), presenting the necessity of a more rigorous methodology including further collaborations within the community and multiplicate measurements.</p>


2016 ◽  
Vol 12 (4) ◽  
pp. 330-334 ◽  
Author(s):  
Shlear H. Hasan ◽  
Nabeel S. Othman ◽  
Kafia M. Surchi

1998 ◽  
Vol 81 (4) ◽  
pp. 763-774 ◽  
Author(s):  
Joanna M Lynch ◽  
David M Barbano ◽  
J Richard Fleming

Abstract The classic method for determination of milk casein is based on precipitation of casein at pH 4.6. Precipitated milk casein is removed by filtration and the nitrogen content of either the precipitate (direct casein method) or filtrate (noncasein nitrogen; NCN) is determined by Kjeldahl analysis. For the indirect casein method, milk total nitrogen (TN; Method 991.20) is also determined and casein is calculated as TN minus NCN. Ten laboratories tested 9 pairs of blind duplicate raw milk materials with a casein range of 2.42- 3.05℅ by both the direct and indirect casein methods. Statistical performance expressed in protein equivalents (nitrogen ⨯ 6.38) with invalid and outlier data removed was as follows: NCN method (wt%), mean = 0.762, sr = 0.010, SR = 0.016, repeatability relative standard deviation (RSDr) = 1.287℅, reproducibility relative standard deviation (RSDR) = 2.146%; indirect casein method (wt℅), mean = 2.585, repeatability = 0.015, reproducibility = 0.022, RSDr = 0.560℅, RSDR = 0.841; direct casein method (wt℅), mean = 2.575, sr = 0.015, sR = 0.025, RSDr = 0.597℅, RSDR = 0.988℅. Method performance was acceptable and comparable to similar Kjeldahl methods for determining nitrogen content of milk (Methods 991.20, 991.21,991.22, 991.23). The direct casein, indirect casein, and noncasein nitrogen methods have been adopted by AOAC INTERNATIONAL.


1988 ◽  
Vol 10 (2) ◽  
pp. 95-100
Author(s):  
John D. Stong

A laboratory computer controlled potentiometric titrator interfaced to a diode array spectrophotometer is described. The titrator consists of widely used, commercially available components; therefore, major attention is given to modes of interconnection and software implementation in data format and system control. Replicate potentiometric titrations of glycines gave a relative standard deviation in titre of 1.035% and a relative standard deviation in pH of 0.745%. Replicate spectrophotometric titrations of bromophenol blue were analysed at three wavelengths to yield pKa= 3.898 ± 0.075 (1.9% rsd).Methods of data presentation and manipulation are presented.


2017 ◽  
Vol 2017 ◽  
pp. 1-7
Author(s):  
Paula Karina S. Uchoa ◽  
Leandro Bezerra de Lima ◽  
Antonia T. A. Pimenta ◽  
Maria da Conceição F. de Oliveira ◽  
Jair Mafezoli ◽  
...  

A high-performance liquid chromatography method was developed and validated for the quantification of the cytotoxic compounds produced by a marine strain ofAspergillus niger. The fungus was grown in malt peptone dextrose (MPD), potato dextrose yeast (PDY), and mannitol peptone yeast (MnPY) media during 7, 14, 21, and 28 days, and the natural products were identified by standard compounds. The validation parameters obtained were selectivity, linearity (coefficient of correlation > 0.99), precision (relative standard deviation below 5%), and accuracy (recovery > 96).


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