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1、A national laboratory of the U.S. Department of Energy Office of Energy Efficiency rinse the solids off of the spatula into the bottle. Add 100-400 ml deionized water to each bottle, ensuring that the total weight of each bottle and cap with sample is equal to all other centrifuge bottles. Each bott
2、le should be no more than full. Cap tightly and shake each bottle vigorously for at least 30 seconds. 10.1.6 Repeat step 10.1.3. Decant the liquor without disturbing the pellet. Residual liquid may be removed with a pipette. Dispose of the wash water appropriately. 10.1.7 Repeat steps 10.1.5 and 10.
3、1.6 until glucose remaining in wash is less than 0.05 g/L, as determined by YSI or equivalent method. 10.1.8 Record the weight of the bottle, cap, and washed sample. Perform LAP “Determination of Total Solids in Biomass”, convection oven method, on a portion of the homogenized solids. Store remainin
4、g solids in refrigerator or freezer, or dry, as appropriate. 310.2 Filtration method. 10.2.1 Record the weight of a Buchner funnel with filter paper to the nearest 0.01 g on an analytical balance. Tare the balance. Add 100-150 g of homogenized slurry sample. Record the weight of the sample to the ne
5、arest 0.01 g. Analyze samples in duplicate. 10.2.2 Filter the sample using vacuum filtration. Filtration should last no longer than five minutes. Extensive filtering time can concentrate the liquor and should be avoided. If filtration is difficult, the centrifugation technique described in 10.1 shou
6、ld be used instead. Slurries with very little liquor may require a pneumatic or hydraulic hand press to press liquor out of the whole slurry. 10.2.3 Save and refrigerate the liquor for later analysis. 10.2.4 While sample is still under vacuum, add approximately 200 ml deionized water. Stir the sampl
7、e, taking care to not disturb the filter paper. Filter the sample. 10.2.5 Repeat step 10.2.3 until glucose remaining in wash is less than 0.05 g/L, as determined by YSI or equivalent method. 10.2.6 Record the weight of the funnel, filter paper, and washed sample. Perform LAP “Determination of Total
8、Solids in Biomass” on a portion of the homogenized solids. Store remaining solids in refrigerator or freezer, or dry, as appropriate. 10.3 If FISD is required, perform LAP “Determination of Total Solids in Biomass”, convection oven method, on a portion of the whole slurry. 11. Calculations 11.1 Calc
9、ulate the amount of fraction insoluble solids in the slurry, utilizing LAP “Determination of Total Solids in Biomass”, convection oven method, to obtain the oven dry weight (ODW) of the washed solids and the ODW of the slurry, if necessary. ODWwashed solids%FISS(Fraction Insouble Solids Slurry)= x 1
10、00Weight bottle,cap,& slurry -Weight bottle&cap ODWwashed solids%FISD(Fraction Insouble Solids Dry)= x 100ODWslurry 11.2 To report or calculate the relative percent difference (RPD) between two samples, use the following calculation (X1 X 2) RPD = 100 X mean Where:X1 and X2 = measured values Xmean =
11、 the mean of X1 and X2 11.3 To report or calculate the root mean square deviation (RMS deviation) or the standard deviation (st dev) of the samples, use the following calculations. First find the root mean square (RMS), of the sample using4 n 2 x 1 RMS = xm = mean = n Then find the root mean square
12、deviation, or standard deviation, using n )2(xi xm 1RMSdeviation = = stdev = n Where: xm=the root mean square of all x values in the set n=number of samples in set xi=a measured value from the set 12. Report Format 12.1 Report percent insoluble solids to two decimal places. RPD and RMS deviation may
13、 also be reported. 13. Precision and Bias 13.1 Determined by data quality objectives and laboratory specific Quality Assurance Plan. 14. Quality Control 14.1 Reported Significant Figures or Decimal Places: Determined by data quality objectives and laboratory specific Quality Assurance Plan. 14.2 Rep
14、licates: Duplicate analyses, at minimum. 14.3 Blank: None. 14.4 Relative percent difference criteria: Determined by data quality objectives and laboratory specific Quality Assurance Plan. 14.5 Calibration verification standard: None. 14.6 Sample size: 50-200 g 14.7 Sample storage: Store slurry and l
15、iquor samples in the refrigerator in sealed containers so the volatile component concentration remains consistent. Wet solids should be stored in sealed containers in the refrigerator or freezer. Solid samples with less than 10% moisture by weight may be stored in sealed containers at room temperatu
16、re. 14.8 Standard storage: None. 14.9 Standard preparation: None. 14.10Definition of a batch: Any number of samples which are analyzed and recorded together. The maximum size of a batch will be limited by equipment constraints. 14.11Control charts: None. 5 15. Appendices 15.1 None. 16. References 16.1 NREL LAP “Determination of Total Solids in Biomass”. 16.2 NREL Ethanol Project CA
