scholarly journals Optimasi dan Validasi Metode KCKT untuk Identifikasi dan Penetapan Kadar Metabolit Nitrofuran dalam Bakso Udang

2021 ◽  
Vol 8 (2) ◽  
pp. 117
Author(s):  
Rachma Ayuningtyas ◽  
Riesta Primaharinastiti ◽  
Mochammad Yuwono
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Relative Standard

Pendahuluan: Dikarenakan sifat dari Furazolidon, furaltadon, dan nitrofurantoin yang karsinogenik, perlu dilakukan pengawasan terhadap cemaran metabolit nitrofuran dalam produk berbahan dasar udang. Nitrofuran dimetabolisme secara cepat dalam jaringan tubuh hewan. Tujuan: Penelitian ini bertujuan melakukan validasi metode KCKT untuk penetapan kadar metabolit nitrofuran dalam bakso udang. Metode: Metabolit furazolidone, furaltadone dan nitrofurantoin yaitu 3-amino-2-oxazolidinone (AOZ), 3-amino-5-methylmorpholino-2-oxazolidinone (AMOZ), dan 1-aminohydantoin (AHD) diderivatisasi menggunakan 2-nitrobenzaldehida, diekstraksi dalam etil asetat dan dicuci dengan n-heksana, kemudian disuntikkan ke dalam system KCKT dengan detektor UV-PDA. Pemisahan dilakukan dengan kolom C-18 46 x 250 mm, 5 mm. Sebagai fase gerak adalah ammonium asetat 20 mM : asetonitril (70:30), dengan laju alir 0.5 mL/menit, suhu kolom 40oC, dan volume injeksi 100 µL. Hasil: Metode yang digunakan dapat memisahkan semua metabolit dari senyawa pengotor dengan waktu analisis 40 menit, dan menghasilkan linieritas yang baik dalam rentang konsentrasi 51,90 – 103,79 ng/mL (AOZ); 56,63 - 101,39 ng/mL (AMOZ); dan 49,92 - 89,86 ng/mL (AHD). Akurasi metode dipresentasikan sebagai rekoveri dengan hasil sebesar 78,50 - 102,29% untuk AOZ; 77,02 - 99,87% untuk AMOZ; and 85,54 - 99,77% untuk AHD. Presisi metode dinyatakan dalam simpangan baku relatif (relative standard deviation, RSD) dengan hasil masing-masing adalah 6,10 - 19,90%; 3,68 - 17,75%; and 2,75 - 12,58% untuk AOZ, AMOZ, dan AHD. LOD dan LOQ sebesar 3,09 ng/mL dan 10,29 ng/mL (AOZ); 6,84 ng/mL dan 22,82 ng/mL (AMOZ); serta 4,61 ng/mL dan 15,36 ng/mL (AHD). Kesimpulan: Metode uji dapat digunakan untuk skrining awal untuk mendeteksi dan penetapan kadar cemaran metabolit nitrofuran pada bakso udang.

An Automated Procedure for the Determination of Ammonia in Tobacco

1972 ◽  
Vol 6 (4) ◽  
Author(s):  
P.F. Collins ◽  
W.W. Lawrence ◽  
J.F. Williams
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Distillation Method ◽  
Relative Standard ◽  
Tobacco Sample ◽  
Automated Determination

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

How Certain Are the Reported Ionic Conductivities of Thiophosphate-Based Solid Electrolytes? an Interlaboratory Study

2020 ◽  
Author(s):  
Saneyuki Ohno ◽  
Tim Bernges ◽  
Johannes Buchheim ◽  
Marc Duchardt ◽  
Anna-Katharina Hatz ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Ionic Conductivity ◽  
Relative Standard Deviation ◽  
Solid Electrolytes ◽  
Ionic Conductivities ◽  
Ionic Conductors ◽  
Energy Storage Devices ◽  
Activation Barriers ◽  
Storage Devices ◽  
Relative Standard

<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>

scholarly journals Indirect and Direct Determination of the Casein Content of Milk by Kjeldahl Nitrogen Analysis: Collaborative Study

1998 ◽  
Vol 81 (4) ◽  
pp. 763-774 ◽  
Author(s):  
Joanna M Lynch ◽  
David M Barbano ◽  
J Richard Fleming
Keyword(s):  
Standard Deviation ◽  
Nitrogen Content ◽  
Relative Standard Deviation ◽  
Collaborative Study ◽  
Direct Determination ◽  
Raw Milk ◽  
Method Performance ◽  
Relative Standard ◽  
Milk Casein

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.

scholarly journals A computer-controlled potentiometric/spectrophotometric titrator

1988 ◽  
Vol 10 (2) ◽  
pp. 95-100
Author(s):  
John D. Stong
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Bromophenol Blue ◽  
System Control ◽  
Data Format ◽  
Relative Standard ◽  
Spectrophotometric Titrations ◽  
Computer Controlled ◽  
Major Attention ◽  
Diode Array Spectrophotometer

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.

Determination of Nitrate in Water by HPLC

2013 ◽  
Vol 448-453 ◽  
pp. 406-408
Author(s):  
Jing Liu ◽  
Xiao Na Ji ◽  
Qing Kai Ren ◽  
Sheng Shu Ai ◽  
Li Jun Wan ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Recovery Rate ◽  
High Performance ◽  
Separation Efficiency ◽  
Fast Analysis ◽  
Relative Standard

We established a method fordetermination of nitrate in water by High Performance Liquid Chromatography(HPLC). The sample was analysed by HPLC-ADA and was quantitated by externalstandard method after being simply processed. This methd has the advantages ofhigh separation efficiency and fast analysis. The experiment result showed thatthe linearly dependent coefficient was0.994, the recovery rate was between 98.7%～105.7%,the relative standard deviation（RSD）wasless than 2.1 %, and the lowest detectable limit is 0.01ng (S/N=1.6).

scholarly journals Determination of 1,3-Dichloropropanol in Soy Sauce and Related Products by Headspace Gas Chromatography with Mass Spectrometric Detection: Interlaboratory Study

2005 ◽  
Vol 88 (5) ◽  
pp. 1404-1412 ◽  
Author(s):  
Sarah Hasnip ◽  
Colin Crews ◽  
Nicholas Potter ◽  
Paul Brereton ◽  
Henri Diserens ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Internal Standard ◽  
Mass Spectrometric ◽  
Soy Sauce ◽  
Headspace Gas Chromatography ◽  
Relative Standard ◽  
Headspace Gas

Abstract An interlaboratory study was performed to evaluate the effectiveness of a headspace gas chromatography (GC) method for the determination of 1,3-dichloro-propan-2-ol (1,3-DCP) in soy sauce and related products at levels above 5 ng/g. The test portion is mixed with an internal standard (d5-1,3-DCP) and ammonium sulfate in a sealed headspace vial. After achieving equilibrium, the headspace is sampled either by gas-tight syringe or solid-phase microextraction (SPME) and analyzed by GC with mass spectrometric detection. 1,3-DCP is detected in the selected-ion mode (monitoring m/z 79 and 81 for 1,3-DCP and m/z 82 for the deuterated internal standard) and quantified by measurement against standards. Test materials comprising soy, dark soy, mushroom soy, and teriyaki sauces, both spiked and naturally contaminated, were sent to 9 laboratories in Europe, Japan, and the United States; of these, 5 used SPME and 4 used syringe headspace analysis. Test portions were spiked at 5.0, 10.0, 20.0, 100.0, and 500.0 ng/g. The average recovery for spiked blank samples was 108% (ranging from 96–130%). Based on results for spiked samples (blind pairs at 5, 10, 20, 100, and 500 ng/g) as well as a naturally contaminated sample (split-level pair at 27 and 29 ng/g), the relative standard deviation for repeatability (RSDr) ranged from 2.9–23.2%. The relative standard deviation for reproducibility (RSDR) ranged from 20.9–35.3%, and HorRat values of between 1.0 and 1.6 were obtained.

scholarly journals A Novel Process for Manufacturing High-Friction Rings with a Closely Defined Coefficient of Static Friction (Relative Standard Deviation 3.5%) for Application in Ship Engine Components

Materials ◽  
2022 ◽  
Vol 15 (2) ◽  
pp. 448
Author(s):  
Wojciech S. Gora ◽  
Jesper V. Carstensen ◽  
Krystian L. Wlodarczyk ◽  
Mads B. Laursen ◽  
Erica B. Hansen ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Friction Coefficient ◽  
Relative Standard Deviation ◽  
Static Friction ◽  
Laser Surface ◽  
Laser Surface Texturing ◽  
Textured Surface ◽  
Fibre Lasers ◽  
Static Friction Coefficient ◽  
Relative Standard

In recent years, there has been an increased uptake for surface functionalization through the means of laser surface processing. The constant evolution of low-cost, easily automatable, and highly repeatable nanosecond fibre lasers has significantly aided this. In this paper, we present a laser surface-texturing technique to manufacture a surface with a tailored high static friction coefficient for application within driveshafts of large marine engines. The requirement in this application is not only a high friction coefficient, but a friction coefficient kept within a narrow range. This is obtained by using nanosecond-pulsed fibre lasers to generate a hexagonal pattern of craters on the surface. To provide a suitable friction coefficient, after laser processing the surface was hardened using a chromium-based hardening process, so that the textured surface would embed into its counterpart when the normal force was applied in the engine application. Using the combination of the laser texturing and surface hardening, it is possible to tailor the surface properties to achieve a static friction coefficient of ≥0.7 with ~3–4% relative standard deviation. The laser-textured and hardened parts were installed in driveshafts for ship testing. After successfully performing in 1500 h of operation, it is planned to adopt the solution into production.

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