scholarly journals Improving Inter-Laboratory Reproducibility in Measurement of Biochemical Methane Potential (BMP)

Water ◽  
2020 ◽  
Vol 12 (6) ◽  
pp. 1752 ◽  
Author(s):  
Sasha D. Hafner ◽  
Hélène Fruteau de Laclos ◽  
Konrad Koch ◽  
Christof Holliger
Keyword(s):  
Standard Deviation ◽  
Data Processing ◽  
Relative Standard Deviation ◽  
Measurement Methods ◽  
Test Duration ◽  
Organic Substrates ◽  
Biochemical Methane Potential ◽  
Validation Criteria ◽  
Relative Standard ◽  
Methane Potential

Biochemical methane potential (BMP) tests used to determine the ultimate methane yield of organic substrates are not sufficiently standardized to ensure reproducibility among laboratories. In this contribution, a standardized BMP protocol was tested in a large inter-laboratory project, and results were used to quantify sources of variability and to refine validation criteria designed to improve BMP reproducibility. Three sets of BMP tests were carried out by more than thirty laboratories from fourteen countries, using multiple measurement methods, resulting in more than 400 BMP values. Four complex but homogenous substrates were tested, and additionally, microcrystalline cellulose was used as a positive control. Inter-laboratory variability in reported BMP values was moderate. Relative standard deviation among laboratories (RSDR) was 7.5 to 24%, but relative range (RR) was 31 to 130%. Systematic biases were associated with both laboratories and tests within laboratories. Substrate volatile solids (VS) measurement and inoculum origin did not make major contributions to variability, but errors in data processing or data entry were important. There was evidence of negative biases in manual manometric and manual volumetric measurement methods. Still, much of the observed variation in BMP values was not clearly related to any of these factors and is probably the result of particular practices that vary among laboratories or even technicians. Based on analysis of calculated BMP values, a set of recommendations was developed, considering measurement, data processing, validation, and reporting. Recommended validation criteria are: (i) test duration at least 1% net 3 d, (ii) relative standard deviation for cellulose BMP not higher than 6%, and (iii) mean cellulose BMP between 340 and 395 NmLCH4 gVS−1. Evidence from this large dataset shows that following the recommendations—in particular, application of validation criteria—can substantially improve reproducibility, with RSDR < 8% and RR < 25% for all substrates. The cellulose BMP criterion was particularly important. Results show that is possible to measure very similar BMP values with different measurement methods, but to meet the recommended validation criteria, some laboratories must make changes to their BMP methods. To help improve the practice of BMP measurement, a new website with detailed, up-to-date guidance on BMP measurement and data processing was established.

scholarly journals How Different Are Manometric, Gravimetric, and Automated Volumetric BMP Results?

Water ◽  
2020 ◽  
Vol 12 (6) ◽  
pp. 1839 ◽  
Author(s):  
Corrado Amodeo ◽  
Sasha D. Hafner ◽  
Rúben Teixeira Franco ◽  
Hassen Benbelkacem ◽  
Paul Moretti ◽  
...  
Keyword(s):  
Automated System ◽  
Biochemical Methane Potential ◽  
Ch4 Production ◽  
Automated Method ◽  
Validation Criteria ◽  
Relative Standard ◽  
Mode 2 ◽  
Methane Potential ◽  
Manual Methods ◽  
The Mean

The objectives of this study were to: (1) quantify differences in biochemical methane potential (BMP) measured using three measurement methods, including two popular methods (a commercial automated system (AMPTS II) and manual manometric) and one newer method (gravimetric), and (2) assess the importance of the mixing position in the measurement sequence. Powdered microcrystalline cellulose was used as the substrate in simultaneous tests. All methods gave similar results (<8% difference in the mean BMP) and were reasonably accurate (recovery of 80–86% of the theoretical maximum BMP). Manometric BMP values were consistently lower than gravimetric by 4–5%. Precision was lower for the automated method (relative standard deviation (RSD) of about 7%) than for the manual methods (RSD about 1–3%). Mixing after biogas measurement resulted in 3% higher BMP for both manual methods than mixing before, due to the lower measured CH4 production from blanks. This effect may be linked to a fraction of CH4 that remains dissolved or even as attached bubbles, and suggests that mixing before measurement is preferable. The automated volumetric and gravimetric methods (mode 2) gave very similar mean BMP values (1% different). However, kinetic analysis showed that methane production was faster with the automated volumetric method. This could come from an error in the estimation of the CH4 production rate for the automated method, or an increase in the degradation rate due to better mixing. Both automatic volumetric and manual gravimetric measurements met current validation criteria for mean cellulose BMP, but the RSD from the automated system exceeded the limit.

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 Biochemical Methane Potential of Cork Boiling Wastewater at Different Inoculum to Substrate Ratios

2021 ◽  
Vol 11 (7) ◽  
pp. 3064
Author(s):  
Roberta Mota-Panizio ◽  
Manuel Jesús Hermoso-Orzáez ◽  
Luis Carmo-Calado ◽  
Gonçalo Lourinho ◽  
Paulo Sérgio Duque de Brito
Keyword(s):  
Anaerobic Digestion ◽  
Biogas Production ◽  
Treatment Plant ◽  
Organic Substrates ◽  
Biochemical Methane Potential ◽  
Volatile Solids ◽  
Working Volume ◽  
Methane Potential ◽  
Bmp Test ◽  
Cork Industry

The present study evaluates the digestion of cork boiling wastewater (CBW) through a biochemical methane potential (BMP) test. BMP assays were carried out with a working volume of 600 mL at a constant mesophilic temperature (35 °C). The experiment bottles contained CBW and inoculum (digested sludge from a wastewater treatment plant (WWTP)), with a ratio of inoculum/substrate (Ino/CBW) of 1:1 and 2:1 on the basis of volatile solids (VSs); the codigestion with food waste (FW) had a ratio of 2/0.7:0.3 (Ino/CBW:FW) and the codigestion with cow manure (CM) had a ratio of 2/0.5:0.5 (Ino/CBW:CM). Biogas and methane production was proportional to the inoculum substrate ratio (ISR) used. BMP tests have proved to be valuable for inferring the adequacy of anaerobic digestion to treat wastewater from the cork industry. The results indicate that the biomethane potential of CBWs for Ino/CBW ratios 1:1 and 2:1 is very low compared to other organic substrates. For the codigestion tests, the test with the Ino/CBW:CM ratio of 2/0.7:0.3 showed better biomethane yields, being in the expected values. This demonstrated that it is possible to perform the anaerobic digestion (AD) of CBW using a cosubstrate to increase biogas production and biomethane and to improve the quality of the final digestate.

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.

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