Ash determination

B. Langfoid, L. Latimei, and K. Ash, Determination of Carbon Utilising a HECO TR—12 Mnalycyer, Teledyne Wab Chang Corp., Albany, Oieg., 1977. Ref 38, p. 260. 

Ash content (DIN 52 005). Unwanted presence of inorganic impurities due to incorrect filtration of neutralization residues and rust contaminants is undesirable because may contribute to premature ageing. Ash determination provides some interesting information. In general, most resins have ash content lower than 0.1%. 

TABLE III. Composition of the Fractions and Their Reaction Products, Mass %. N.D. Means Not Determined (in the Case of the Residue from Fraction C Insufficient Sample Was Available for an Ash Determination). Note That the Method for Backing Out Naphthalene from the Bottoms Involves Normalizing the Composition to C + H + O = 100%. 

Since acid-forming amino acids are present primarily in proteins, a number of papers have reported the effect of feeding various levels of protein to human subjects. Sherman and Gettler (23) postulated that food ash determined the acidity or alkalinity of the urine. 

Food-control laboratories seeking to be accredited for the purposes of the Directive should include, as a minimum, the following techniques in generic protocols HPLC, GC, atomic absorption and/or ICP (and microscopy). A further protocol on sample preparation procedures (including digestion and solvent dissolution procedures) should also be developed. Other protocols for generic methods which are acceptable to UKAS may also be developed. Proximate analyses should be addressed as a series of specific methods including moisture, fat, protein and ash determinations. 

Procedure. Prepare a filter tube by placing in a cool muffle furnace, increase the temperature to 500°C, and maintain it for 30 min. Remove and allow to cool in a desiccator. To avoid damaging the sinter, do not allow the temperature to reach 515°C. Weigh 0.5 g of the sample, as received, but ground to 1 mm, into the crucible. At the same time, weigh a separate portion for DM and ash determination. Wash the sample in the filter tube with 3 x 25 ml portions of petroleum spirit. Suck as dry as possible under gentle vacuum and complete the removal within 10 min at 60°C in an oven specified for use with flammable solvents. 

Ash Determination. This is one of the tests for the detn of purity of substances consisting primarily of one or more organic compds... 

Table VII shows the analytical wavelengths chosen, the concentration ranges calculated to the whole coal, average relative standard deviations, and detection limits in ash determined by the spectrographic method.

To assess the validity of this procedure, a series of coal ashes analyzed by the British Coal Utilization Research Association (BCURA) were again analyzed with the two types of ash prepared in our laboratories. Calibrations for these analyses were prepared from U. S. Geological Survey and National Bureau of Standards rock standards, IB, Gl, Wl, and Nos. 78, 79, 88. The values determined for the BCURA coal ashes agreed excellently with results obtained at BCURA by Dixon et al. (3). Standard deviations were calculated for the duplicate coal ash determinations Si 0.07%, Ti—0.01%, Al—0.06%, Fe—0.05%, Mg—0.02%, Ca—0.03%, K—0.01%, P—0.01%, and V—1.3 ppm. These deviations are comparable with Class A wet silicate analyses and indicate a high degree of precision. 

The data from the mercury in ash determinations are presented in Table V. Four types of ash samples were analyzed and reported bottom, initial mechanical, final mechanical (multicones), and electrostatic ash. Because of the inability to empty an initial mechanical, a final mechanical, and an electrostatic ash hopper simultaneously prior to the start of a test, normally only three ash samples were collected during any one test. 

The results of the mass balance are summarized in Table VI. The ratio of the mercury found in the gas stream to the amount of mercury released from the coal but not recovered in the ash is given in the third column. The average of this ratio is 1.19, with a standard deviation of 0.24. Within one standard deviation unit there is not a significant difference between the measured ratio and the expected ratio of 1.0. Therefore, based on 14 ratios at one plant, there is not a statistically significant difference between the total mercury found in the stack gas and the amount expected in the stack gas from the coal and ash determinations. Dual tests 13 and 14 showed close ratios of 0.88 and 0.95. 

Hie coal was ground in the laboratory and sized to pass 200 mesh. Ash determinations on tne ground coal sample were made, and an average value of 5.2% was used to correct for the ash content of the extracted coals. 

These small fragments are almost impossible to see in the polymer, even under a microscope. However, evidence of the fracturing is seen by examining the ash via mercury intrusion. An example is shown in Table IV, where Davison Grade 952 Cr/silica was allowed to polymerize ethylene to various yields. The polymer was then burned away, and the porosity of the catalyst ash determined by mercury intrusion. 

Starting with the idea that there are large differences in hardness between the building materials used in the two types of milling, we tried to obtain a correction factor via ash determinations. This was... 

The ash determined in the above manner furnishes One of the best criteria for deciding what quality of flour has been used in making the bread. If mineral substances or even so-called baking powder were added to the flour, the ash would show an increase in this case, tests 14 and 15 are applied. 

Salts (Ash).—Determined as with diffusion juice on 2-3 grams of substance, to which sulphuric acid is added directly. 

Total moisture of coal Ultimate analysis of coal Ultimate analysis of coke Chlorine in coal and coke Phosphorus in coal and coke Arsenic in coal and coke Analysis of coal ash and coke ash Determination of moisture-holding capacity of hard coal General introduction and methods for reporting results Determination of total moisture of coke Proximate analysis, determination of moisture content of the general analysis test sample... 

Analyses reported on a dry basis are calculated on the basis that there is no moisture associated with the sample. The moisture value (ASTM D-3173 ISO 331 ISO 589 ISO 1015 ISO 1018 ISO 11722) is used for converting as determined data to the dry basis. Analytical data that are reported on a dry, ash-free basis are calculated on the assumption that there is no moisture or mineral matter associated with the sample. The values obtained for moisture determination (ASTM D-3173 ISO 589) and ash determination (ASTM D-3174) are used for the conversion. Finally, data calculated on an equilibrium moisture basis are calculated to the moisture level determined (ASTM D-1412) as the equilibrium (capacity) moisture. 

Feedstock material and processed solids were analyzed for glucan, xylan, arabinan, and acetyl groups by quantitative acid hydrolysis according to standard methods (25). The acid-insoluble residue was considered as Klason lignin, after correction for the acid-insoluble ash (determined by igniting the contents at 575°C for 5 h). 

The sample does not contain more than 0.1% sulfated ash, determined on 1.0 g. 

Residue on Ignition (Sulfated Ash) Determine as directed in Method I under Residue on Ignition, Appendix IIC, igniting a 3-g sample. 

IIIC. The weight of nitrogen determined, multiplied by 6.25, gives the weight of protein. Use the second sample of residue for the ash determination [see Ash (Total), below]. The weight of the residue, corrected for the blank, protein, and ash, is equal to the weight of the total fiber (see Calculations, below). 

Acid-Insoluble Ash Determine as directed in the general method, Appendix EC. 

The residue called insoluble matter might be conveniently used for the ash determination. 

Estimate the molar flow rate (kmol/min) of each element in the coal (other than those in the ash). Determine the feed rate (kmol/min) ot Oi required for complete combustion of the coal. 

Elemental Analysis. Carbon, hydrogen, nitrogen, oxygen, sulfur, phosphorous, and ash determinations were made on freeze-dried samples of raw foam, and humic and fulvic acids isolated from Como Creek and Suwannee River foam and water samples by Huffman Laboratories (Golden, CO). Trace-metal analysis was performed on freeze-dried Como Creek foam by Huffman Laboratories (Golden, CO). 

Extensive analytical efforts to fully characterize the oil shales are underway at Exxon Research and Engineering Company s Baytown Laboratories. No significant losses of any metals of concern are observed during high temperature ashing. An alternate means of rapid ash determination uses a Parr combustion bomb. The ash can be dissolved by alkaline fusion in a Claisse fluxer or by acid dissolution in a Parr bomb. The solutions thus prepared are analyzed by atomic absorption or by inductively coupled plasma emission spectrometry for major (Al, Ca, Fe, K, Mg, Na, Si, Ti) and trace elements (As, B, Ba, Be, Cd, Co, Cr, Cu, Li, Mn, Mo, Ni, P, Sr, U, V, Zn). Kerogen enriched shales need to be ashed before the dissolution, otherwise low recoveries are obtained. Overall accuracy and precision of metals determination is within... 

The Parr oxygen combustion bombs were used for a rapid ash determination and for sample preparation for IC. About 0.5 g of shale or shale oil was mixed with 0.5 g of white oil in a stainless steel cup. Five mL of water was placed in the bottom of the bomb which was then assembled and pressurized to 30 atmospheres of oxygen. After combustion, the bomb was allowed to cool for ten minutes and then opened slowly. The inside walls of the bomb were washed with water, and all the washings were combined, filtered if necessary, and diluted to 50 mL. The residue in the cup was dried at 110°C for 15 minutes and reweighed for ash determination. 

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