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Cbd oil extraction lab technique

preparations. sample Full-thickness and hSOC

bladeacc
12.06.2018

Content:

  • preparations. sample Full-thickness and hSOC
  • There was a problem providing the content you requested
  • best available cellular system (19), and the full-thickness human skin organ Full-thickness hSOC and sample preparations. Biopsies of. These hSOC SZ95 sebocytes under in vitro conditions that mimicked “acne- assays, .. signaling pathways (Fig- Full-thickness hSOC and sample preparations. The air and CO2 reactivity of the coke samples were measured In the experiment, testing samples with 5 g weight and 1– mm width were placed in the . During the preparation, when the quantity of DBT added was kept . In this experiment, CaONHSOC and CaOHSOC coke samples.

    preparations. sample Full-thickness and hSOC

    Table 1 3 summarizes the moistures for each run. No Oregon Program run. Sam- pling ended immediately. Tube repaired and train leak checked. Data recorded at 5 minute intervals rather than on a percent of fuel burned basis. Second filter tore during run, probably during pretest leak check. Second filter installed backwards in sample train.

    A second meter box was used for the duration of the test. Meter gamma was corrected by proportion- ing the bio calibrations based on percent of the respec- tive gas volumes. All dilution tunnel samplers shutdown for 70 minutes while repairs ware made.

    Sam- pling restarted simultaneously. Stack samplers continued operat: Operator failed to record meter temperature. Meter tem- perature estimated to be for the test. Operator failed to record meter temperature for first 13 readings of 35 reading test. Average recorded readings used for calculations.

    Lost power after 5 minutes of sampling. Power restored and testing resumed after 5 minutes downtime. After testing was completed the elbow between the con- denser and XAD module was broken as the operator was removing the sample train from the stack. Lost power to samplers and stove scale. Test ended after 70 minutes of burn. Stove charged, doors were closed then testing started. Readings continued adding the final weight, prior to the power lcss, to the scale reading.

    Stove doors were opened for S minutes after 6 minutes of burn. Stove doors were opened zor 6 mirutes after 90 minutes of burn. Stove doors were opened for 1 minute after minutes of burn. Stove doors open for first 10 minutes of test. Stove doors opened for 5 minutes after 65 minutes of burn. Stove docrs opened for 5 minutes after minutes of burn. Stove doors opened for 3 minutes after min- utes of burn. Stove doors opened for 1 minute after minutes of burn.

    Fire died after minutes. Less than 3 punds of wood burned. However, when woodstoves are used, products of both complete and Incomplete combustion of wood are emitted. Three sampling methods are currently being use i to collect samples to characterize woodstove emissions: The first two methods both collect a sample directly from the stdck, while the third method requires dilution of the entire stack flow first, with subsequent collection of a sample from these diluted gases.

    For Oregon Method 7, the following com2onents are analyzed: For the ASTM dilution tunnel, filters and probe wash are analyzed. The task leaders served complementary roles in areas of project coordination overseeing sample preparations gas chromatography TOO and gravimetric GRAY analysis, GCIMS, quality control, and data analysis and validation.

    The task leaders also enacted quality assurance procedures described in the Quality Assurarna Project Plan with supervision by and coordination with both the Project Director and Quality Assurance Q. The samples were provided by Engineering Science and consisted of the following: For QA purposes selected burns employed dual H1 6s In the stack which resulted In as many as seven sample sets for analysis.

    The sample collection period was during the months of September, Octobc. The analysis of samples followed procedures published by the state of Oregon as shown In Figurt Analysis of the M 5 samples followed published AEE.. Level 1 procedures with the following exceptions: Oregon Method 7 sample fraction and analytical matrix.

    ASTM sample fractions and analytical matrix. Probe washes were desiccated at roan tomperature and weighed. The filters were desiccated at room temperature and weighed. The dried probe residues and filters were combined and Soxhiet extracted with methylene chloride.

    The condensate, condensate Impinger rinse, impinger water, and impinger rinse were combined and extracted by the Level 1 partition procedure. Quantitative calibration of the T 0 procedure for the purpose of mass determination was accomplished by the use of mixtures of known concentration of the normal hydrocarbons decane, dodecane, and tetradecane.

    The peak area due. This method is applicable to organic liquids, solid sample extracts, aqueous extracts, and extracts from the Modified Method 5 sampling train sorbent module. The analysis was performed after the sample material was concentrated in order to have sufficient GRAY material to weigh in an accurate manner. Chromato rapnic conditions were selected to optimize both peak resolution and analysis time.

    No samples were analyzed until tune criteria were met. Target compounds were Identified using characteristic ions and retention t1. The analysis was performed In the full scan mode. The target compounds were put into the calibration solution at five concentration levels and each sol ution was analyzed to estabi Ish a response factor database. Quantitation of compounds was performed by the method of relative response factors.

    The number of area units per nanogram was then multiplied by an appropriate factor I. Note that the number is representative of the Quantifiable Limit, not the Limit of Detection. A determination of the quantifiable limit for the overall method would require a determination of compound recoveries over the range of interest and Incorporation of this recovery factor into the determination. Daily analysis included a demonstration of DFTPP tune, daily calibration check, a quality control sample, and analytical sampi es.

    Finnigan MAT Column: The spectra and results of the library search were Inspected and manual Interpretation was cuperlirposed upon the automated computerized Interpretation. The data are reported as scan number, compound s Identified at that elution time 1 and three parameters reported from the NBS library search algorithm which aid In estimating the quality of the identification.

    However, 1 a compound was not Identified In the library search, the results are reported as ma: That Is, if components coelute, these parameters can be quite low because the spectrum does not represent a pure component. However, the Identification can still be entirely valid. As Illustrated this method matrix Is comprised oc five major components: The samples were weighed and checked every 2 hours until constant weight was establ Ishod.

    The chloroform extraction was repeated twice more with addition of the bottom CHC1 3 layers to the tared beaker. Extraction was repeated three times on the BR and BM fractions using diethyl other in place of chloroform. The ether layers were transferred to the same beaker used for chloroform. The combined solvent extract was evaporated to dryness and desiccated 24 hours.

    The probe rinse PR in MaC1 2 was evaporated at roan tomperature In a tared beaker, desiccated, and weighed to the nearest 0. The data were carefully logged into sample notebooks on a daily basis by the analysts to minimize the collection of invalid data.

    Daily control checks consisted of examination of reproduc1t iltty of duplicate Irijoctions, sample blanks, and quality control samples that were analyzed during the daily analysis cycle.

    The analysts recorded any unusual instances In the daily cycles such us power loss or fluctuations, tanporary leaks or adjustments, or operator error.

    Probl ns were documented as detected and appropriate corrective action taken to maximize the validity of the database. The analysts on each task double checked all data entries to ensure accurate transcriptions and calculations. The data were then reviewed by each respective Task Leader and corrections made If necessary. I porylIflO dlbenze a,h anthraC efll ndeno 1.

    Proficiency tests were administered to the analyst using prepared standards containing known amounts of stearic acid, elcosane, and triphenylmethane In a total voUine of mL of methylene chloride.

    The results for the GRAY tests are as follows: It should be noted that the same analyst performed all GRAY analyses. These reagent solvent blanks consisted of the same volume of solvent used In analyzing the samples.

    Any unusually hi reagent blanks were noted and the blanks reanalyzed. Linear regression analysis of the calibration curve resulted in a correlation coefficient of 0. C 7 and C 19 peaks were not Included in the regression analysis.

    One calibration standard in the middle of the linear working range was used as the daily QC standard. Duplicate injections of the QC standard were performed daily prior to sample analysis.

    If the new standard failed to meet the criteria, the 1nstrt nent was recalibrated. Duplicate Injections were performed for all samples analyzed. The T values were calculated by subtracting the appropriate field blanks from the total values. Daily analysis was initiated by a check of DFTPP to verify that the Instrumental tune as acceptable prior to the analysis of samples. Tuning data are Included as Appendix J.

    The Instrument was calibrated by analysis of five calibration samples at a concentration of 5, 10, These points were Incorporated Into a database and the mean, standard deviation, and per cent coefficient of variation calculated. ICO QC standard analysis. The linear plots are Included as Appendix K. Calibration checks were performed daily prior to sample analysis.

    A check sample containing naphthaleno, phenanthrene, fluoranthene, pyrene, and chrysene was analyzed daily. DuplIcate analyses were performed for four samples. These samples were injection duplicates, not process duplicates, since an entire sample e. A peak Is observed at approximately scans In the sample chromatograms. F phenol 15, 6, Several modifications to the analytical procedures were made based on EPA approval.

    No other significant procedural problems were noted. Upon thorough examination of the original and revised Draft WoodstoveS Report several modifications were made in the previously reported data. The first set of three audit samples were submitted and analyzed simultaneously with the first set of woodsteve burns. The second set of three audit samples were submitted at a later date and analyzed along with the last sot of voodsteve burns. The final set of three audit samples showed an average recovery target compounds of 89 percent for both low and high spiked concentrations.

    The minimum requirement for total mass of sample t. This procedure Is depicted in the attached figure. This modification was a result of analyzing three Radian Audit Samples and screening several eoodstove extracts at the original i. The Audit Samples t ere submitted to the laboratory to evaluate the method performance.

    These were prepared and analyzed upfront prior to actual samDle analyses. Preliminary GRAY and TCO Total Chromatographable Organics analyses tiero unable to detect the spiked concentrations within the linear working range of the standard curves, 1n iIcat1ng the need for further concentration of the samples. November 19, TO: Triplicate values for one of the calibration points one analysis cn each of three successive dais will be used to assess analytical precision; rn an, standard deviation, and percent coefficient of variation will be calculated.

    A linear regression will be performed for each of the points of the or 4 glnal calibration curve and the value of the correlation coefficient will be reported. If you have any questions please call J.

    Modification to woodstove QAPP. As per the standard operating procedure for TCO analysis, a multi-point calibration curve was performed that covered the range from 0. A five point calibration curve was used. A linear regression calculation was performed using the five GC responses obtained for the five concentrations on the curve. The results are given below: Therefore, when the intercept wds subtracted from blank values to determine TCO amounts, negative values were obtained.

    The TCO linear regression line was plotted to determine if any of he points were significantly skewed. The highest concentration point were significantly skewed. The highest concentration point analyzed deviated noticeably from the regression line and was causing the intercept of this line t3 be large.

    Since few samples had TCO values In this range, th. The v Iues are given below: Modification to TCO analysis. December 13, TO: The changes are as follows: It was noticed that labels with the Radian number and sample ID were placed on the petri dish bottom. This resulted In the dish weights approximately mg higher. The second and third weights were averaged and then subtracted from the first weight to get the 1. The label weight was then subtracted fran the GRAY value to get the correct filter weight.

    Radian found several tare weights that had been miscalculated. This value is then multiplied by the total number of ml In the sample to obtain a value of micrograms per total sample. In order to perform a calculation Involving the number of ml. Otherwise, the multiplication should be by a factor of 10, The result Is that the digits as reported In the data tables are correct but the units are Incorrect: Susan Fernandes Project Director: Are SOPS available for sample custody?

    All samples logged In manually and through SAM? All samples labelled appropriately log-In date, disposal date, client, etc. All completely analyzed samples marked with an stored separately In the refrigerator eXD to indicate with holding time requirements? Are all TCO samples stored In freezer. Are all dry GRAY samples stored are stored in a in a dessicator? Are standards stored separately in the refrigerator? Is the refrigerator checked monthly for expired sample dates?

    QuantitatIve calibration using stock solution of decane, dodecane, and tetradecane? CalibratIon curve linear with standard. CalibratIons recorded In a permanent record?

    AnalytIcal balance calibrated to tO. Frequency of calibration well documented? Balance calibrations recorded in a permanent record? Is all apparatus that contacts a COncer trated or evaporated residue sample glass, teflon, aluminum, or steel? Frequency of calibration well documanted? Are calibration data kept in a permanent record? Is a daily bakeout done and a QC sample analyzed to test for Contamination? If contamination Is fou 8 d, is the column baked out at C for 20 Lilnutes and Is a blank check repeated?

    Is a QC sample run daily to check C 7 -C 17 window? Is a reagent sample run for each new reagent batch? Is the needle flush2d with Place a flush vial solvent Oichloromethane between between samples but Injections? Is the GC Inlet septum changed daily? Is analyst proficiency demomstrated prior to testing following SOP guidelines? Opens from the top. Is the dessicating cabinet have a Sealing around It.

    Is the evaporation of samples carried out in an area clean of airborne dust and organic vapors? Are 2 reagent blanks analyzed each day samples are run? If a sample needs to be re- analyzed but insufficient sample remains, Is the initial resilt reported with a qualifying statement? Are the following QC samples analyzed: Is the GC column and sample inlet system evaluated using the appropriate standards?

    Is the MS performance evaluated using the following: Are QC results kept in a permanent record? Uave standards been analyzed periodically to verify that each analytical method Is In control? Do QC records Indicate corrective action taken on data that has been rejected? Are questionable results considered acceptable by authorized persons chemist, engineer, etc. Are all QC data accessible for all analytical results?

    Are preventive maintenance for each Instrument, activities service calls documented in standard forms? Are permanent service records Task Leader, for all instruments available and maintained logbooks?

    Project Director and 4. Do s the laboratory supervisor Task Leader. Is a storeroom available for Inventory of spare parts?

    Are the following general on- hand laboratory supplies maintained? Are the following GC supplies Inventoried: Are the following MS maintenance procedures performed: Are all samples accompanied by sample tracking form and appropriate signatures? Do sample worksheets contain all pertinent information, including methods of dilution or concentrati cm?

    Do all instruments have documented troubleshooting procedures? The specific ancillary methods used varied with the test location. The anissions sampling on the Timber-eze stove began within 5 minutes after the stove was loaded with the fuel charge. This was a deviation from the Oregon procedure and was corrected for all subsequent burns.

    All other test burns were conducted with the emissions sampling starting one minute or less before the stove test charge was placed in the firebox. For the ASTh method acetone and methanol are specified.

    Those recoveries were made according to the procedures. In addition, a methylene chloride rinse of the 0M7 front and back halves was made and recovered separately. The MMS train was recovered using methylene chloride. Those fractions were recovered sepa- rately. Following sample recovery, all samples were sealed and safely stored until transportcJ to the laboratory for analysis. Samples were delivered to the lab within 1 week of their collection.

    Tare weights were given to Radian for determination of final weights. Application of the code simplified tracking samples throughout the collection, handling, enalysis and reporting processes. The sample numbering syste. A copy of the laboratory report is provide i in Appendix D. Analytical Methodo are described there.

    The analyzer has a 0 to 5 percent CO range and a 0 to 20 percent CO 2 range. The 02 analyzer was an MSA stack gas analyzer which uses a ft. That instrument has a r? The gas sample was extracted using a stainless steel probe bent into the gas flow.

    A glass fiber filter was used to i enove particulate material. A gas sample conditioner including two impingers with water in an ice bath, was upstrean of the filter. This latter calibration theck demonstrated performance of the systes. Span d ecks were made using a single gas every 2 to 3 hours during each test and after eacn test. This is discussed further in Section 5. The SO 2 was injected at a rate that resulted in a downstream concentration of less than ppo 0M7 6.

    A critical orifice was used to control the injection rate. The orifice was calibrated using bub- ble meters prior to the test prcgram. The procedure followed for the tracer gas analyzer calibration was sim- ilar to that followed for CO. CO 2 and Span gases were on hand to cal- ibrate the instrument to ppm. Problems with the tracer gas system were identified after the first test but it was not witil an audit was conducted that the problem was determined to be apparent reactions of the SO 2 in the system.

    The SO 2 was used as a guide for proportional sampling but the accuracy of the actual values collected are S us pact. That array would interfere with the and sample syst ns and was not used for this test program. Flue gas temperatures were measured at the center of the stack approx- imately 1 duct diameter downstream of the sampling location.

    The dilution tunnel temperature was measured at a similar point in that duct. Thermocouples were calibrated as per PA Method 2. Wet bulb and dry bulb ter peratures were monitored and recorded every 5 minutes at a location 1 ct dian eter downstream of the stack sample collection pint OH 3. A comparison of stack gas moisture measurements resulting from the three methods is presented in Section 5. The dilution tunnel noisture content was measured using the Gt7 and M samples. Sawdust was collected when the wood was cut to build fuel cribs.

    The shavings were placed in plastic bags and labeled to identify the specific cribs constructed from that particular board. Blocks of wood were also collected at the same time and sealed in plastic bags. The dust and wood blocks were submitted t a subcontract laboratory for heat content and density analysis respectively. The heat contents for each crib were used in the Fc calculations discussed in Section 2.

    The laboratory repnrt is provided in Appendix D. The Radian Corporation prepared a separate plan for the laboratory analysis portion of the program. In addition to adhering as closely as possible to the test procedure described in Section 4, validation criteria were identified for the sampling program.

    A systems audit was conducted by Research Trianc4e Institute Rn at the woodstove test facility during the sampling program. Following submittal of the first draft report RTI conducted a data quality audit.

    The draft audit report gave this sampling program and the resulting data an acceptable rating with qualifications. The qualification was lifted fran the audit rating after ES responded to the draft audit report indicating that the validation criteria specified in the QAPP would be canpared to the actual sampling and stove operating condi- tions.

    The comparison must be made with an understanding of the relative importance of the cr3 terj. A brief discussion of the criteria is included at the end of Appendix E in response to canments made in the auditors report. Tables 7a through 7e present a summary of sampling conditions for each of the samples collected. The parameters considered ncst critical were included in the table and used to characterize the data from each sample run.

    No isokinetic sampling was considered to make the results of the corresponding sample unacceptable u. A total mass catch of less than 30 milligrams was considered significant enough to require qualifying the data if the sample volume was below the criteria volume.

    If either the mass catch was in excess of 30 milligrams or the sample volume was larger than the criteria volume then the results were considered acceptable.

    Several of the sample train validation criteria were satisfactory for all samples collected. These included post test leak rate, condenser outlet temperature, and orsat leak rate. Zero and span drift corrections were made assunu. These data were entered into the woodstove program Appendix C. Several test burns that do not reliably reflect actual anisslons accord- ing to Oregon stove operating procedures must be qualified.

    Sampling stopped after minutes. These data were not entirely deleted fran the results because they can be con- sidered useful for test method evaluation. The dilution tunnel flow criteria were neglected during this test program. Most flows were greatly in excess of the This criteria was not used to qualify or invalidate any samples. Those blanks were for use by the lab in making blank corrections.

    Train blanks were collected to demonstrate the efficiency of sample recov- ery and possible contamination of samples in the stove test facility environment.

    Those blanks were obtained by charging a sample train as if it were a actual sample. The sample train was then leak checked, sealed, allowed to sit over- night and leak checked again. Tables 8 and 9 present the results of analyses of train blanks. Many of the train blank results are higher than normal acceptable levels. Since the water used for charging the MMS trains was from the same container as the water used to charge the 0M7 trains that source of contamination can be eliminated as pDssibility.

    As mentioned in Section 4, the methylane chloride did not appear to be a satisfactory sol- vent for the materia collected during sampling. Ineffect ve sample recovery using MeC1 2 may have left residue in the sample trains which would then result in high train blanks.

    Table 10 presents the results of the duplicate samples in units of grams per hour except for the samples collected in the stack during test burn 1 That burn was not completed and no stack flow rate could be calculated using the Oregon woodatove program.

    Those results were calculated using the F calculations. The large amount of resulting data underwent multiple checks to minimize the number of errors. All data reduction was done twice by two different data handlers. The two sets of data were then compared. Any in- consistencies resulted in a third check of that particular portion of the data to resulve the discrepancy.

    The example calculations were prepared by the field team leader and given to the data processor for input to the computer. Reference Method 3 specifies a range for F 0 of 1. Table 11 presents the average CRIS a 2 02, and O values for each test horn and the corresponding orsat analyses. F 0 was cai. Some of the project participants are concerned with the accuracy of these data since they are the basis for calculating stack gas flow rates and heat outputs which are used to calculate emission rates.

    The CD4S criteria were a 5 percent zero drift and a 2 percent span drift. The effect of these drift allowances on the F 0 can be signifi- cant. The worst case span drift situations allowable under the validation criteria would be for a negative 1. In this case the average 02 and CO 2 values would have been Thus, it appears that the F 0 calculation is highly sensitive to instrument drift.

    The F 0 is an oxygen balance evaluation. The instrument used for this test program uses a zirconium oxide detector which operates at a t nperathre of C. NA Insufficient data were collected to ccinplete these calculations. This could esu1t in a 1: Errors in tne CT 4 measurements uld result in errors in the stack gas flows calculated using the CHO balance which would result in a proportional and direct error in the calc ated MM5 and cti7 stack emission rates.

    Since the dilution tunnel flows were measured using a standard pitot tube, errors in the CEMS would not cause an error in those emission rates. It was finally determined that the SO 2 was apparently reacting with other components of the flue gas including material condensed in the SO 2 sample Line or material collected on the filter.

    Span d ecks were erratic. Increasing the SC 2 concentration entered into the calcula- tion increases the stove heat output, the percent oxygen and overall combustion efficiency while decreasing the wood combustion efficiency, stack gas flow rate, and percent CO 2. Inaccurate SO 2 measurements precluded reliable proportional- sampling in the stack.

    The dry fuel composition was assumed to be 51 percent carbon, 7. PC wag calculated using the heat content determined for each crib used during the test program Appetidix D. The resulting heat input and stack flows were used to calculate the results summarized in tables 3a, 3b and 3c of Section 2.

    Table 1 3 summarizes the moistures for each run. No Oregon Program run. Sam- pling ended immediately. Tube repaired and train leak checked. Data recorded at 5 minute intervals rather than on a percent of fuel burned basis.

    Second filter tore during run, probably during pretest leak check. Second filter installed backwards in sample train. A second meter box was used for the duration of the test. Meter gamma was corrected by proportion- ing the bio calibrations based on percent of the respec- tive gas volumes. All dilution tunnel samplers shutdown for 70 minutes while repairs ware made. Sam- pling restarted simultaneously. Stack samplers continued operat: Operator failed to record meter temperature.

    Meter tem- perature estimated to be for the test. Operator failed to record meter temperature for first 13 readings of 35 reading test. Average recorded readings used for calculations. Lost power after 5 minutes of sampling. Power restored and testing resumed after 5 minutes downtime. After testing was completed the elbow between the con- denser and XAD module was broken as the operator was removing the sample train from the stack. Lost power to samplers and stove scale. Test ended after 70 minutes of burn.

    Stove charged, doors were closed then testing started. Readings continued adding the final weight, prior to the power lcss, to the scale reading. Stove doors were opened for S minutes after 6 minutes of burn.

    Stove doors were opened zor 6 mirutes after 90 minutes of burn. Stove doors were opened for 1 minute after minutes of burn. Stove doors open for first 10 minutes of test. Stove doors opened for 5 minutes after 65 minutes of burn. Stove docrs opened for 5 minutes after minutes of burn. Stove doors opened for 3 minutes after min- utes of burn. Stove doors opened for 1 minute after minutes of burn.

    Fire died after minutes. Less than 3 punds of wood burned. However, when woodstoves are used, products of both complete and Incomplete combustion of wood are emitted. Three sampling methods are currently being use i to collect samples to characterize woodstove emissions: The first two methods both collect a sample directly from the stdck, while the third method requires dilution of the entire stack flow first, with subsequent collection of a sample from these diluted gases.

    For Oregon Method 7, the following com2onents are analyzed: For the ASTM dilution tunnel, filters and probe wash are analyzed. The task leaders served complementary roles in areas of project coordination overseeing sample preparations gas chromatography TOO and gravimetric GRAY analysis, GCIMS, quality control, and data analysis and validation.

    The task leaders also enacted quality assurance procedures described in the Quality Assurarna Project Plan with supervision by and coordination with both the Project Director and Quality Assurance Q. The samples were provided by Engineering Science and consisted of the following: For QA purposes selected burns employed dual H1 6s In the stack which resulted In as many as seven sample sets for analysis.

    The sample collection period was during the months of September, Octobc. The analysis of samples followed procedures published by the state of Oregon as shown In Figurt Analysis of the M 5 samples followed published AEE..

    Level 1 procedures with the following exceptions: Oregon Method 7 sample fraction and analytical matrix. ASTM sample fractions and analytical matrix. Probe washes were desiccated at roan tomperature and weighed. The filters were desiccated at room temperature and weighed. The dried probe residues and filters were combined and Soxhiet extracted with methylene chloride.

    The condensate, condensate Impinger rinse, impinger water, and impinger rinse were combined and extracted by the Level 1 partition procedure. Quantitative calibration of the T 0 procedure for the purpose of mass determination was accomplished by the use of mixtures of known concentration of the normal hydrocarbons decane, dodecane, and tetradecane. The peak area due. This method is applicable to organic liquids, solid sample extracts, aqueous extracts, and extracts from the Modified Method 5 sampling train sorbent module.

    The analysis was performed after the sample material was concentrated in order to have sufficient GRAY material to weigh in an accurate manner. Chromato rapnic conditions were selected to optimize both peak resolution and analysis time. No samples were analyzed until tune criteria were met. Target compounds were Identified using characteristic ions and retention t1. The analysis was performed In the full scan mode. The target compounds were put into the calibration solution at five concentration levels and each sol ution was analyzed to estabi Ish a response factor database.

    Quantitation of compounds was performed by the method of relative response factors. The number of area units per nanogram was then multiplied by an appropriate factor I. Note that the number is representative of the Quantifiable Limit, not the Limit of Detection. A determination of the quantifiable limit for the overall method would require a determination of compound recoveries over the range of interest and Incorporation of this recovery factor into the determination.

    Daily analysis included a demonstration of DFTPP tune, daily calibration check, a quality control sample, and analytical sampi es. Finnigan MAT Column: The spectra and results of the library search were Inspected and manual Interpretation was cuperlirposed upon the automated computerized Interpretation. The data are reported as scan number, compound s Identified at that elution time 1 and three parameters reported from the NBS library search algorithm which aid In estimating the quality of the identification.

    However, 1 a compound was not Identified In the library search, the results are reported as ma: That Is, if components coelute, these parameters can be quite low because the spectrum does not represent a pure component. However, the Identification can still be entirely valid. As Illustrated this method matrix Is comprised oc five major components: The samples were weighed and checked every 2 hours until constant weight was establ Ishod.

    The chloroform extraction was repeated twice more with addition of the bottom CHC1 3 layers to the tared beaker. Extraction was repeated three times on the BR and BM fractions using diethyl other in place of chloroform. The ether layers were transferred to the same beaker used for chloroform. The combined solvent extract was evaporated to dryness and desiccated 24 hours.

    The probe rinse PR in MaC1 2 was evaporated at roan tomperature In a tared beaker, desiccated, and weighed to the nearest 0. The data were carefully logged into sample notebooks on a daily basis by the analysts to minimize the collection of invalid data. Daily control checks consisted of examination of reproduc1t iltty of duplicate Irijoctions, sample blanks, and quality control samples that were analyzed during the daily analysis cycle.

    The analysts recorded any unusual instances In the daily cycles such us power loss or fluctuations, tanporary leaks or adjustments, or operator error. Probl ns were documented as detected and appropriate corrective action taken to maximize the validity of the database. The analysts on each task double checked all data entries to ensure accurate transcriptions and calculations. The data were then reviewed by each respective Task Leader and corrections made If necessary.

    I porylIflO dlbenze a,h anthraC efll ndeno 1. Proficiency tests were administered to the analyst using prepared standards containing known amounts of stearic acid, elcosane, and triphenylmethane In a total voUine of mL of methylene chloride.

    The results for the GRAY tests are as follows: It should be noted that the same analyst performed all GRAY analyses. These reagent solvent blanks consisted of the same volume of solvent used In analyzing the samples.

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    Full List of References and Notes. In STM and XAS experiments, the sample preparation began with repeated sputter / heating cycles of the Ag() Above the slab are 8 effective atomic (Ag) layers thick of vacuum. value of the spin- orbit Hamiltonian HSOC = λ L.S, where λ is the atomic spin-orbit. Sample preparation was. Energy E HSOC = α(ez × k) · σ where α is . the DOS with a Lorentzian (40 meV full width at half maxi- mum) to . a full definition of these terms is found. . HSOC. No NGS standard applicable. Purpose, range of application, terminology . Sample preparation for carbon analyser: Aliquots of the samples must Depth interval: unknown.



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    Full List of References and Notes. In STM and XAS experiments, the sample preparation began with repeated sputter / heating cycles of the Ag() Above the slab are 8 effective atomic (Ag) layers thick of vacuum. value of the spin- orbit Hamiltonian HSOC = λ L.S, where λ is the atomic spin-orbit.

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    a full definition of these terms is found. . HSOC. No NGS standard applicable. Purpose, range of application, terminology . Sample preparation for carbon analyser: Aliquots of the samples must Depth interval: unknown.

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    about two feet thick constructed in about AD and an inner wall about five the archaeological archive at the Museum of London and is also engaged upon a preparation . full list of all the material examined, together with the items . incomplete example of a stoneware mineral water bottle imported.

    artmoney

    full width at half maximum (FWHM), ω for the Lorentzian FWHM, and α for ratio hSOC of the XPS components is determined by the order of degeneracy: hSOC = 2 .. Figure The sample holder used to prepare the samples in the UHV.

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    KPU SURREY HIGH SCHOOL ON-CAMPUS (HSOC) a “2” beside your second choice in case your first choice course is full. . of handling and firing ceramic materials of different sizes, thicknesses, They will work with basic techniques of clay preparation, joining, Below are a few examples (not an.

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