STANDARD OPERATING PROCEDURES
Contents
1. Boa Agroforest Centre Oo Code METH11V01 Diagnostics Lab Date July 30 2014 Author Robin Chacha STANDARD OPERATING PROCEDURES METHOD FOR ANALYSING SOIL SAMPLES FOR MINERAL COMPOSITION USING XRD Contact Details Telephone 254 20 7224000 4235 4279 4163 Email icraf speclab cgiar org Laboratory Manager Soilspec_ Lab Manager cgiar org Website www http worldagroforestry org research land health Address Details World Agroforestry Centre Mailing P O Box 30677 00100 Nairobi Kenya Physical address United Nations Avenue Off Limuru Road Gigiri Nairobi Kenya aaa STANDARD OPERATING PROCEDURE Date July 30 2014 or Qoae Code METH 11V01 Agroforestry Title Method for analyzing soil samples for mineral Author Robin Chacha composition using XRD METHOD DOCUMENT CONTROL LOG Name and position Signature Author s Beatrice Oware Laboratory Technician signature for completeness and correctness of document Verifiers Robin Chacha Senior Laboratory signature for completeness and Technician correctness of document signature for completeness and correctness of document Authorizer Mercy Nyambura Laboratory Manager signature for completeness and correctness of document Distribution of valid copies of this document G143D X Ray Diffraction Lab Revise before date Historical data dates2. applications in geology material science environmental science chemistry forensic science and the pharmaceutical industry among others In Agriculture it has application in qualitative and quantitative analysis of actual minerals in top soils and sub soils in classification of soils in terms of weather able and nutrient rich minerals to measure soil fertility potential and use of mineralogical data in pedo transfer functions to directly predict soil functional properties PRINCIPLE Powder diffraction is routinely used as a fingerprint identification technique of various solid materials in the laboratory It is a high tech rapid cheap and non destructive technique for qualitative and quantitative analysis of crystalline compounds about 95 of all solid materials in the soil are crystalline When X rays interact with a crystalline substance or powder a diffraction pattern called a diffractogram is produced and can be quantified Information obtained from this patterns include phase composition of a sample types and nature of crystalline phases minerals present crystal structure amount of amorphous OM content micro strain size and orientation of crystallites XRD has become an indispensable method for materials investigation characterization and quality control The angle and intensity of the diffracted beam recorded by a detector forms a diffraction pattern which provides information about a sample The diffraction pattern for ever
3. ANDARD OPERATING PROCEDURE Date July 30 2014 soipiantspecrat Code METH 11V01 Diagnostics Lab Title Method for analyzing soil samples for mineral Author Robin Chacha composition using XRD Agroforest Centre id ANNEX 2 Reference Interval Corundum mount Checking performance and verification of Al203 commercial the instrument With peaks occupying standard same position no shifting Run Monthly Quartz Mineral Checking peak position intensity and SiO2 Commercial shape standard Run Monthly 12 Mineral composition using XRD SOP
4. Centre STANDARD OPERATING PROCEDURE Date July 30 2014 Qa Code METH 11V01 Diagnostics Lab Author Robin Chacha Title Method for analyzing soil samples for mineral composition using XRD SAFETY AND ENVIRONMENT Refer to HS 01 XRD Safety manual Regulation of the manufacture and use of analytical X ray instruments is adopted from the United States system When used properly X ray instruments pose few risks to careful users Care should be taken when using any analytical X ray instrument Never put any part of your body in the expected path of the main beam Strictly only trained personnel should be allowed to operate the XRD spectrometer and should have studied the operator s manual thoroughly Manufacturer s overall radiation safety instructions should be adhered to Eating drink or smokes are prohibited in laboratory For other safety information refer to Laboratory Safety manual REQUIREMENTS Equipment a AD2 PHASER Diffractometer with appropriate software b McCone micronizing mill c Weighing balance d Centrifuge e Oven f Vortex mixer Material a Corundum and quartz standard reference material b Standard 55mm sample discs made from PMMA a COklmkloolant Innovatek cooler fluid b Soft brush c PH indicator strips non bleeding d Weighing paper 4 x4 e Mortar and pestle 5 Mineral composition using XRD SOP Agroforest Centre STANDARD OPERATING PROCEDUR
5. E Date July 30 2014 Soil Plant Spectral Code METH 11V01 Diagnostics Lab Title Method for analyzing soil samples for mineral composition using XRD Author Robin Chacha f Test Sieve 250 um mesh g Spatulas Squeeze bottles i Non fluffy lab tissues j Hygrothermometer Chemical a Hexane99 b Ethanol 99 c Deionized water PROCEDURE Sample preparation Refer to METH 11 a Milling Samples are milled using a McCrone Grinding Mill with agate grinding elements in a jar The unique grinding action of the mill rapidly reduces particles to sub micrometer sizes and mixes for homogenization required for quantitative and qualitative analytical methods Approx 10 um Make sure to retrieve as much sample as possible after milling Centrifuge to remove ethanol decant dry and crush sample Sample mounting randomly oriented mounts a Load the randomly prepared samples into the well of a low background sample holder and tap gently on the bench to help fill and pack to avoid sample displacement which causes peak shifts b Using a sharp razor tap the sample surface slowly in all directions to distort orientation a few times and then continue to level while gently removing the loose 6 Mineral composition using XRD SOP aaa STANDARD OPERATING PROCEDURE Date July 30 2014 or Qoa Code METH 11V01 Agroforestry Title Method for analyzing soil samples for mine
6. able data Here should be a scheduled maintenance service including setup calibration repair record keeping to verify that equipment is functioning properly Every equipment should be dedicated to a specific laboratory room and its instrument manuals from the manufacturer should be kept in the room Data Recording and Record Keeping The generation of all environmental data should be completely and consistently documented so the results can be assessed by an independent party If data are maintained electronically data should be backed up on a regular basis and stored in a separate location from the original data if possible All data recording should be checked by the laboratory supervisor for correctness and completeness and each entry should be checked for accuracy of transcription Diffractogram evaluation 1 The intensity of the quartz peak should be more than 10000 counts at a d spacing3 34 4 26 1 82 other minerals appearing at the exact position of the d spacing e g calcite at d spacing of 3 03 2 Narrow peak represent non clay minerals silicates carbonates oxides while the broader peaks represent clay mineral Phase identification Refer to QC 03 1 Use a quartz pattern as a quality control peak to check if it has a peak at the right position at d spacing of 3 34 4 25 1 80 2 Check if one is able to search matches the other minerals phases by matching the database and the pattern standards to identify 9 Mineral
7. bration Standards Use mounted corundum to check verification of the instrument working conditions at least once a month Use of quartz standards to check to check the intensity of the quarts peak in the sample Maximum counts high peak 9000 but with Soil Plant Spectral Diagnostic lab method we get more than 3000 counts for the quartz peak and this is a good confirmation of our sample preparation procedure Personnel Personnel working at the sample reception laboratory performing sample processing and preparations should meet background and training specifications outlined qualifications and should follow the guidance provided concerning safety and protective outerwear 8 Mineral composition using XRD SOP STANDARD OPERATING PROCEDURE Date July 30 2014 ain Qoa Code METH 11V01 Agroforestry Title Method for analyzing soil samples for mineral composition using XRD Author Robin Chacha Workflow A workflow chart showing work procedure is displayed as guidance in order used to reduce the potential for contamination Laboratory manuals and notebooks also should remain in designated rooms The laboratory uses electronic data reporting to avoid this potential source of contamination Standard bench sheets are used in the various processes and ensures that all necessary data is recorded in a consistent manner Equipment The equipment used to perform sample preparations should function properly to generate reli
8. composition using XRD SOP STANDARD OPERATING PROCEDURE Date July 30 2014 eis hatte Centre Osa Code METH 11V01 Diagnostics Lab Author Robin Chacha Title Method for analyzing soil samples for mineral composition using XRD 3 Checking on the reproducibility of the patterns when scanned again No shifting of peaks at their position same peak with height and intensity REFERENCES PHASER user s manual Doc M88 EXX141 D2PHASER from unpacking to first measurement Doc M88 EXX155 VI D2 PHASER service manual Doc M88 EXX143 VI ATTACHMENTS Knime software File maker software 10 Mineral composition using XRD SOP Eaa Oa World Diagnostics Lab Centre STANDARD OPERATING PROCEDURE Date July 30 2014 Code METH 11V01 Title Method for analyzing soil samples for mineral composition using XRD Author Robin Chacha ANNEX1 Work Flow X Ray Diffraction Laboratory Workflow Objective functions properties This Laboratory uses X Ray diffraction to determine the soil mineralogy For characterizing soil mineralogy as a key determinant of nearly all soil Sonics Mix sample with water then use Dispersion Fraction sonic probe machine to break the particles Sedimentation F amp Siphoning Leave suspension for 12hrs in a glass cylinder for it to settle then transfer to plastic containers Prepare the filtration s
9. et up then filter the suspension for 12hrs then do the first measurement analysis Put the desiccators on ethene glyco and place in oven for 12 hrs at 60 70 C Then take the second measurement analysis Hot Plate Place desiccators on hot plate for 20mins then take the final measurement Overlay Check the overlay spectra for Spectra the three readings LEGEND Preparation Action point Decision point Tape notes Stored data DOOD Process route cez Put the mould on a desiccators EOE Quality Clay fraction whole rock approach Decant Ethanol Hexane Addition Oven Dry at 80 C for 1 4 hrs 20min for clay fraction and 30min for all rock approach Sample Deposition Measurement Control Peak Identify the minerals Identification present using EVA software 11 Mineral composition using XRD SOP From Sample Processing Factory Add 9g of ethanol to 3g soil sample then mill for 12 min Transfer sample to cetrifuge tube and place them on centrifuge at 4000rpm for 10mins for soil to settle at the bottom Add 0 5ml of hexane to the sample and mix well using voltex mixer To Archives Excess sample is archived in capped glass vials Put sample in sample holders till compact using a razor blade ST
10. ity above background or as integrated intensity the area under the peak When sample material is analyzed by XRD a range of diffracted peaks will occur and a diffractogram is obtained The angle of each peak is used to identify the mineral 7 Mineral composition using XRD SOP Agroforest Centre STANDARD OPERATING PROCEDURE Date July 30 2014 Qa Code METH 11V01 y Diagnostics Lab Author Robin Chacha Title Method for analyzing soil samples for mineral composition using XRD phase while the intensity of the peak will indicate relative amount present The result of an XRD measurement is a Diffractogram showing a Phases present peak positions b Phase concentrations peak heights c Amorphous content background hump d Crystallite size strain peak widths A search of the ICDD standard database of x ray diffraction patterns enables quick phase identification for a large variety of crystalline samples QUALITY CONTROL Sample preparation During sample loading or packing of the sample on the disc holders the key point to consider is the preferred orientation and its effect on the diffractogram The density of the packing has to be moderate to allow X ray beam to go through the particles to achieve maximum good particle statistics Sample particles must be randomly oriented and have a flat smooth and homogeneous surface to achieve a good resolution grains less than 10um is needed Cali
11. of previous issues Date retrieval to be filled in once the document has become obsolete and is archived Changes in this version compared to previous version Describe what has changed in the text of this version compared to the previous version 2 Mineral composition using XRD SOP T Qur Code METH 11V01 Agroforestry Title Method for analyzing soil samples for mineral Author Robin Chacha STANDARD OPERATING PROCEDURE Date July 30 2014 composition using XRD SCOPE AND APPLICATION The determination of the types and relative amounts of the minerals present in soil soil mineralogy is determined routinely because of its strong influence on soil behavior its use in soil classification and its relevance to soil genetic processes ICRAF Soil Plant Spectral Diagnostic Laboratory uses X ray diffraction technique for qualitative and quantitative assessment of minerals in soils X ray diffraction is the most powerful technique used for analysis of minerals and offers mineral phase s identification and quantification The standard operation describes the Whole rock approach where the sample is prepared into a random powder which helps in analysis of total amounts and identification of non clay minerals present The analysis provides information about the minerals present in a sample and also the abundance It can be applied to all types of soil samples X ray diffraction has a wide range of
12. ral Author Robin Chacha composition using XRD excess sample powder by scrapping off from the edges of the well of the sample holder c It is very important to have the correct sample level to the well surface since any error in the height of the sample will cause peak displacement d After measurement the disc can be off loaded and washed with tap water and then re used Sample measurement a Switch on the instrument and let it warm for thirty minutes Refer to EQUIP 06 b Pull down the spherical handle of the stage and place onto sample holder into the sample position of the stage Goniometer c Lift the sample back into the sample measurement position by pulling up the spherical handle of the stage and slide down the instrument door Press down door handle with force in order to close it correctly d Activate the High Voltage e Set measurement parameters for a typical Lynx eye Refer to EQUIP 06 f Select start button to initiate acquisition Data acquisition The intensity of diffracted X rays is continuously recorded as the sample and detector rotate through their respective angles A peak in intensity occurs when the mineral contains lattice planes with d spacings appropriate to diffract X rays at that value of 8 Results are presented as peak positions at 20 and X ray counts intensity in the form of a table or an x y plot shown above Intensity is either reported as peak height intensity that intens
13. y phase is as unique as a fingerprint Phases 3 Mineral composition using XRD SOP STANDARD OPERATING PROCEDURE Date July 30 2014 a Osa Code METH 11V01 Agroforest Centre composition using XRD Title Method for analyzing soil samples for mineral Author Robin Chacha with the same chemical composition can have drastically different diffraction patterns Use of the position and relative intensity of a series of peaks is used to match experimental data to the reference patterns in the database such as the Powder Diffraction File PDF The PDF contains over 200 000 diffraction patterns of crystalline phases Modern computers have automated search match programs that determine what phases are present in a sample by quickly comparing the d spacing of the unknown to those of known materials in the International Centre for Diffraction Data ICDD Powder Diffraction File PDF ABBREVIATIONS AND DEFINITIONS XRD X Ray diffraction RELATED DOCUMENT Laboratory manuals quality service safety training Policy documents EQUP 06 XRD EQUP 09 Balances EQUP 11 Centrifuges EQUP 12 Ovens EQUP 17 McCrone Micronizing Mill EQUP 23 All software QC 03 Quality assessment Laboratory Safety Manual XRD Logbook RELATED FORMS XRD sample list WF 10 Soil mineralogy analysis using Bruker D2 PHASER Diffractometer System workflow 4 Mineral composition using XRD SOP Agroforest
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