Standard Operation Procedure (SOP) Analytical methods in anaerobic digestion batch reactions

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1 Standard Operation Procedure (SOP) Analytical methods in anaerobic digestion batch reactions : 3 Pages: 7 Author: Lucien Biolley Date: Approved: Valid from: Changed: File: SOP_AnaerobicDigestion_Analysis_151119

2 1 Application area The analytical methods described in this SOP are divided in the two groups of application. Hence the measurements for mass balance studies and the measurements for process control. - Mass balance parameter: TS, ots, TOC - Process control parameter: ph, alkalinity, determination of volatile fatty acids, analysis of gas volume and quality 2 Mass balance parameter 2.1 TS - total solids (TSS-total suspended solids) Recommendations: To get a feel for the accuracy perform always at least double determination and a blank. Label and record the weight of the aluminum dish (Weight A). Hint: You need to be able to identify the label after 2 hours at 550, so make it strong! Shake, stir, or mix the contents in the sample container in order to obtain a more uniform (preferably homogeneous) aliquot for analysis. Consider the dilution of your sample. Approximately 10 ml / g of sample are filled into the aluminum dish, now the filled dish is weighed again (Weight B) Dry for 24 to 48 hours at 105 C. Put the aluminum dish for 15 Minutes in the desiccator and determine the weight (Weight C). Is your sample really dry? Think about it and repeat the last to steps until you obtain constant weight. Calculate the TS from the difference before and after the drying of the sample. (%) = 100 Figure 1: Oven with sample in aluminium dish Seite 2 von 7

3 2.2 ots - organic total solids (VS-volatile solids) The ots is used to characterize input and output of the anaerobic digestion batch reactors. The results will allow to creating a mass balance as well as the calculation from simple gas production into the BMP (gas production per mass of organic dry matter). The ots determination is a follow up procedure to the TS. This means the sample of the TS determination is reused in this method. The weight of the aluminum dish is used again from the TS measurement (Weight A). Burn the sample in a muffle furnace for 2 to 4 hours at 550 C. Put the aluminum dish for 15 Minutes in the desiccator and determine the weight (Weight D). Is your sample really dry? Think about it and repeat the last to steps until you obtain constant weight. Calculate the ots from the difference of weight before and after the burning. (%) = 100 Figure 2: Oven for ots determination Seite 3 von 7

4 2.3 TOC Total organic carbon Like the ots the TOC is used to characterize input and output of the anaerobic digestion batch reactors. The results are used to create a simple C - balance. Recommendations: To get a feel for the accuracy perform always double determination and a blank also for TOC. And again consider the dilution of your sample. The precise procedure for the TOC from Dr. Lange is provided with the manuals included with each box of the tests. To make sure being within the measurement range a dilution is needed. One possible approach to get appropriate dilutions, is to estimate the absolute ots value of a sample (apply measurements) and to consider all of it as the maximum amount of TOC. Figure 3: Dr. Lange TOC measurement set up Seite 4 von 7

5 3 Process control parameter 3.1 ph The fermentation process only takes place under certain conditions. For example the optimum range for methane forming microorganisms is approximately ph Thus we are interested to keep the ph within this range. To measure the ph you should have some reactors with a special application, which allows you to reach the liquid phase of the bottles without opening it. Take a syringe and put it on the adapter of the reactor with special application. Suck some liquid from the reactor into the syringe. Since the reactor is under pressure the liquid will flow automatically once the valve is opened (app. 0.5 ml is enough). Determine the ph value by measuring with a variety of ph-papers. Repetition frequency: To be on track of what is going on inside the reactor the ph should be measured every second day. Figure 4: Different ph-measurement indicator papers Seite 5 von 7

6 3.2 Volatile fatty acids / Alkalinity Volatile fatty acids are composed of the organic components during the fermentation process, especially during the first reaction steps of the decomposition. As long as the rest of the fermentation is not yet in full progress the reaction can acidify itself. Therefore monitoring the amount of these acids is crucial. Alkalinity on the other hand counteracts the acids mentioned above and helps the fermentation process to stabilise. To assess a fermenter state these two measures are much more expedient. Take a sample of app ml from the well mixed reactor Fill the sample in a 10 ml plastic tube Centrifuge the sample for 10 min at 6500 rpm (! level out the centrifuge!) Take the supernatant and fill it into a fresh 10 ml plastic tube Centrifuge the samples again for 30 min at 6500 rpm Collect the supernatant and filtrate it into a beaker with known tare weight Determine the sample mass Dilute it with 10ml of distilled water Titrate with H 2 SO mol/l to less than ph 4 Use the method according to Kapp to calculate the concentration (see Appendix) Repetition frequency: For a sufficient monitoring of the fermenter this Titration has to be repeated at least once a week. A single measurement is sufficient concerning the availability of the medium. Figure 5: Titration device, left: sampling unit, middle: feed unit, right: process control computer Alternative measures: Volatile fatty acids are also detectable by IC (Ion chromatography). In some cases the titration result has to be doubted due to the method and the calculation behind it. Therefore the IC might function as a measure of validation. Seite 6 von 7

7 3.3 Analysis of gas quality Biogas does not consist of only one gas. In particular it is a mixture of CO2 and CH4, which is varying during the fermentation process. To get an insight on the gas production and to quantify the potential it is important to analyze the gas quality. 1. Fill all the gas of one series (e.g. cellulose) of your manual batch reactors into the restek gas bag (see figure 5, left) 2. Make sure the pump (see figure 5, right) is running 3. Open the valve at the restek gas bag and let the pump suck the sample gas through the gas sensors 4. Observe the signal displayed on the computer but wait until the signal has reached the limit (app. 2 min). Repetition frequency: This analysis is repeated every time the produced gas is released due to the reaching of a threshold overpressure. Figure 6: Bluesens gas Sensors for Methane and Carbondioxide measurements Seite 7 von 7

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