散装红土镍矿取样、制样、检验方法

散装红土镍矿取样、制样、检验方法INDUSTRYSTANDARDSOFSAMPLING，SAMPLEPREPARATIONANDINSPECTIONMETHODOFLATERITENICKELORE一、目的PURPOSE为规范散装红土镍矿检验业务工作，确保检验工作的公正和准确。THEPURPOSEISTOREGULATETHEACCURACYOFTHEINSPECTIONOFLATERITICNICKELORE二、适用范围SCOPEOFAPPLICATION适用于亚洲和泛太平洋地区的氧化镍矿（俗称红土镍矿）检验工作。ITISAPPLICABLETOTHEINSPECTIONOFLATERITICNICKELOREINASIANPACIFICAREA该工作规范介绍了针对上述镍矿的品质化验的引用标准，装、卸货的取样、制样方法，保证针对该产品的检验在品质和取制样的操作上更有代表性。THESPECIFICATIONSINTRODUCETHEQUOTEDSTANDARDFORCHEMICALANALYSISOFTHELATERITICNICKELOREASWELLASMETHODSOFSAMPLINGTHENUMBEROFINCREMENTSISDETERMINEDUPONTHEABOVEREGULATIONSIFTHECONSIGNMENTCONSISTSOFMORETHAN2CARGOS,EACHTRUCKSHALLBESAMPLEDWHENTRUCKSARELOADEDWITHDIFFERENTQUANTITY,THEDISTRIBUTIONOFINCREMENTSSHALLBEBASEDONTHEQUANTITYC份样量的确定（见表1）DETERMINETHEMASSOFINCREMENTASSPECIFIEDINTABLE1表1份样量的确定TABLE1DETERMINETHEMASSOFINCREMENT公称最大粒度（MM）NOMINALTOPSIZE份样量（KG）INCREMENTMASS公称最大粒度（MM）NOMINALTOPSIZE份样量（KG）INCREMENTMASS224以下21001501522431541502002031550820025025501001025030030D取样工具SAMPLINGIMPLEMENTS/TOOLS取样工具包括铁锹、取样铲（见图1、表2）、钢锤、取样容器（料桶或塑料袋和编织袋等）、标签、唛头笔和照相机。SAMPLINGDEVICESINCLUDESHOVEL,SAMPLINGSCOOPASSPECIFIEDINFIGURE1,TABLE2,STEELHAMMER,SAMPLINGCONTAINERBARREL,PLASTICBAGS,WOVENBAGS,ETC,LABELS,SHIPPINGMARKPENANDCAMERA（图1）FIGURE1表2取样铲规格TABLE2SPECIFICATIONSOFSAMPLINGSCOOP取样铲尺寸MMDIMENSIONSOFINCREMENTSCOOP铲号SCOOPNUMBER最大公称粒度（MM）NOMINALTOPSIZE容积（ML）VOLUMEABCDE1501503500045019045038017012512521000380160380320150100100110003001303002601207070370020010020017080505016001507515013065404073011063110955030315380905090804020224270804580703515161807040706030101012060356050255670503050402032635402540301511163020302512E如果卸货港取样受条件限制时，允许在卸货过程中按上述的规定单独抽取水分样，然后在码头转堆至堆场过程中按上述规定抽取品质样。IFSAMPLINGCONDITIONSARELIMITEDINTHEDISCHARGEPORT,MOISTURESAMPLESCANBETAKENSEPARATELYDURINGDISCHARGEWHILEQUALITYSAMPLESCANBETAKENDURINGTHETRANSFERRINGOFCARGOFROMTHEQUAYTOTHESTOCKYARD4、通知委托人，要求委托人提供必要的配合。INFORMTHECLIENTANDASKTHEMFORNECESSARYCOOPERATION5、检验人员根据取样方案，明确取样时间、地点，准备好清洁、合适的取样工具、样品存放容器如带防水膜的编织袋、密封样品桶、封识等以及安全帽和反光背心等防护用品。到达取样地点后，根据货物的实际情况，亲自或组织现场取样工人按取样方案要求进行取样。ACCORDINGTOTHESAMPLINGSCHEME,THEINSPECTORSSHALLDEFINETHESAMPLINGTIMEANDPLACE,PREPARECLEANANDSUITABLESAMPLINGEQUIPMENTINCLUDINGSAMPLESTORAGEIMPLEMENTSSUCHASWATERPROOFWOVENBAGS,AIRPROOFCONTAINERS,SEALS,ETC,HARDHATS,REFLECTIVEVESTANDOTHERSAFETYEQUIPMENTPPEPERSONALPROTECTIONEQUIPMENT6、取样基本要求GENERALREQUIREMENTSFORSAMPLINGA取样原则上应在货物装卸、加工、堆垛或衡量的移动过程中进行，不具备在传送带上取样的，应在新露出的矿石表面上随机定点取样。INPRINCIPLE,SAMPLINGSHALLBEPERFORMEDDURINGTHEPROCESSOFLOADING/UNLOADING,STACKINGORWEIGHINGWITHOUTCONDITIONOFSAMPLINGFROMTHECONVEYORBELT,SAMPLINGSHALLBEPERFORMEDRANDOMLYATREGULARPOINTONTHEFRESHEXPOSEDSURFACEOFTHECARGOB第一个份样可在第一间隔内随机确定不可在第一间隔的起点开始，以后按计算的间隔取，在操作过程中不得随意变动取样间隔。注取样时应同时取出冲刷样品。THEFIRSTINCREMENTCANBETAKENRANDOMLYDURINGTHEFIRSTINTERVALNOTATTHEBEGINNINGOFTHEFIRSTINTERVAL,ANDTHEREAFTERINCREMENTSSHOULDBETAKENASPERTHECALCULATEDINTERVALWHICHSHOULDNOTBEADJUSTEDDURINGTHEOPERATIONREMARKWHILESAMPLING,WASHINGSAMPLESSHALLBETAKENSIMULTANEOUSLYC取样工具的开口度至少为最大公称粒度的3倍，但不得小于100MM，每个份样用合适的取样工具一次性取出，如果一次取出有困难，亦可在同一处分几次取出样品。对于粒度较大的（如粒度大于150MM）可以采用取样框代替取样铲来确定应取的份样。THEOPENINGOFTHESAMPLINGDEVICESHALLBEATLEAST3TIMESOFTHENOMINALTOPSIZE,WHICHCANNOTBELESSTHAN100MMEACHINCREMENTSHALLBETAKENONCEBYSUITABLESAMPLINGIMPLEMENTIFTHEINSPECTORHADDIFFICULTYINTAKINGONEINCREMENT,TAKINGSEVERALATTHESAMEPOINTISALSOALLOWEDFORTHELARGERPARTICLESIZECARGOIFTHESIZEISOVER150MM,SAMPLINGFRAMECANBEUSEDTOSUBSTITUTESAMPLINGSCOOPTODETERMINEINCREMENTSD取样过程中应保证每个份样量基本一致，偏差不得大于标准所规定的的质量变动系数。DURINGSAMPLING,MAKESURETHATEACHINCREMENTSHALLBECONSISTENTWITHVARIATIONSNOTLARGERTHANTHEQUALITYVARIATIONFACTORSPECIFIEDINTHESTANDARDE取样过程中应注意观察取样批的粒度分布情况，应能保证所取份样的粒度比例符合取样间隔或取样部位的粒度比例，所得大样的粒度分布应与整批矿产品的粒度分布基本吻合。DURINGSAMPLINGPROCEDURE,PAYATTENTIONTOTHESIZEDISTRIBUTIONOFSAMPLINGLOT,ANDMAKESURETHATTHESIZEPROPORTIONOFINCREMENTSBEINGTAKENISINACCORDANCEWITHTHESAMPLINGINTERVALORSAMPLINGPOINTTHEREFORE,THESIZEDISTRIBUTIONOFBULKSAMPLEMATCHESTHATOFTHEWHOLECONSIGNMENTF不同品质规格或粒度规格的货物分舱装运时，应根据具体情况分舱独立取样，各舱结果加权平均后，作为交货批的结果。WHENCARGOWITHDIFFERENTSPECIFICATIONSINTERMSOFQUALITYAND/ORSIZEISLOADEDSEPARATELYINEACHCARGOHOLD,SAMPLINGSHALLBESEPARATELYPERFORMEDPERHOLDTHERESULTSOFEACHHOLDSHALLBECALCULATEDBYWEIGHEDMEANASTHECOMPOSITERESULTFORWHOLECONSIGNMENTG如已达到预定的份样数，而作业仍在进行，应按原定间隔继续取样，直到整批货物作业完毕。IFINCREMENTNUMBERISENOUGHBEFORECOMPLETIONOFOPERATION,SAMPLINGSHALLBECONTINUEDASPERTHEORIGINALINTERVALUNTILTHEENDOFOPERATIONH取样过程中，必须保证样品不受任何污染。DURINGSAMPLINGPROCEDURE,MAKESURETHATSAMPLESSHALLNOTBECONTAMINATED7、现场取样时必须查核商品标记、批次、数量、重量等，样品容器上应进行唯一性标识，必要时及时施加封识，并采取适当的防护措施，防止样品改变特性或丢失。WHENSAMPLINGONSITE,MAKESURETOCHECKTHECARGOSMARK,LOT,NUMBER,QUANTITY,ETCTHECONTAINEROFSAMPLESHALLBEUNIFORMLYMARKEDANDSEALEDIFNECESSARY,ANDTAKESUITABLESAFETYMEASUREINCASEOFIDENTITYCHANGEORLOSS8、取样人员应做好取样记录包括天气情况，取样过程中若发现货物外观异常或有外来杂物和污染等异常情况，须及时处理，必要时拍照取证，并及时向其上级汇报。SAMPLINGPERSONNELSHALLMAKEAREPORTINCLUDINGWEATHERCONDITIONSDURINGSAMPLINGIFANYIRREGULARITYOCCURS,LIKEUNUSUALLOOKINGMATERIAL,IMPURITIESAND/ORCONTAMINATION,ACTIONINATIMELYMANNER,TAKEPHOTOSANDREPORTTOTHEPRINCIPAL9、委托人要求偏离预定的取样方案时，检验人员应及时向其上级汇报，并做好详细记录。IFTHECLIENTREQUESTSTHEIMPLEMENTATIONOFADIFFERENTSAMPLINGSCHEME,THEINSPECTORSSHALLREPORTTOTHEPRINCIPALINTIMEANDTAKEDETAILEDNOTES二）、样品的制备SAMPLEPREPARATION1、制样工具SAMPLEPREPARATIONDEVICESA颚式破碎机（大、中、小号）JAWCRUSHERL,M,SB）对辊破碎机ROLLCRUSHERC）圆盘粉碎机或密封式震荡研磨机DISKPULVERIZERORAIRPROOFSHAKINGGRINDERD）份样铲及挡板INCREMENTSCOOPANDBAFFLEE）二分器RIFFLEF）盛样容器SAMPLESTORAGECONTAINERG）钢板STEELPLATEH）干燥箱（能调节温度，使箱内任一点的温度在设定温度在5之间）DRYINGOVENWITHADJUSTABLETEMPERATURECONTROLTHATWORKSWITHIN5OFTHESETTINGI）不锈钢金属十字分样架STAINLESSSTEELCROSSDIVIDINGFRAMEJ）分样筛224MM、10MM、1MM、180M筛SIEVES224MM、10MM、1MM、180M2、样品的制备包括干燥必要时、破碎、混合和缩分等一系列操作，应根据商品特性和所测项目按有关制样标准的要求进行，以使样品符合测试要求。SAMPLEPREPARATIONINCLUDESASERIESOFOPERATIONSUCHASDRYINGIFNECESSARY,CRUSHING,MIXING,DIVIDING,ETCITSHALLBEPERFORMEDACCORDINGTOTHENATUREOFTHECARGOANDPERTHESTANDARDOFTHESUBJECTTESTS,SOASTOCOMPLYWITHTHEREQUIREMENTSOFTHETESTS3、样品制备过程中应防止损失、污染或其他可能改变其特性的情况发生。DURINGSAMPLEPREPARATION,PREVENTLOSS,CONTAMINATIONORANYOTHERSITUATIONSWHICHMAYCHANGETHEIDENTITYOFTHESAMPLE4、水分样应用清洁、密封或防水容器储存，当批量很大、作业时间较长或遇阴雨、高温天气时，应将取样批合理划分为几个部分，每一部分应尽快制备成副样测定水分，防止由于样品水分变化而产生偏差。THEMOISTURESAMPLESHALLBESTOREDINCLEAN,AIRPROOF/WATERPROOFCONTAINERIFTHEREARETOOMANYLOTS,LONGPERIODSOFRAINORPERIODSOFVERYHOTWEATHER,THESAMPLINGLOTSHALLBEDIVIDEDINTOSUBSAMPLESFORWHICHTHEMOISTURESHOULDBETESTEDASSOONASPOSSIBLE,INCASETHEAFOREMENTIONEDFACTORSARECAUSINGSIGNIFICANTCHANGESTOTHEMOISTURECONTENT5、水分样的制备MOISTURESAMPLEPREPARATION在制水分样时，每2500吨做一个水分样，将每单元每批所取样品从盛样容器中倒出，按照标准的缩分方法（网格法）快速取出检测水分样品（15分钟之内完成，取水分样时充分考虑粒度比例，在碰到大块货物的时候，应按所占份样铲的容积砸取相应的比例，剩余部分只能作为品质样而不能作为粒度筛分），并取出5KG作为检测水分的保留样品（保留样品需注意密封完好）。每单元水分试验样的个数及水分试验样的最小质量见表3、表4。WHENPREPARINGMOISTURESAMPLES,ONEMOISTURESAMPLEISPREPAREDFOREACH2500MTLOTTAKETHESAMPLESOFEACHLOTOUTOFTHESTORINGCONTAINER,ANDUSINGINCREMENTDIVISIONMETHOD,EXTRACTTHEMOISTURESAMPLEASQUICKLYASPOSSIBLEWITHIN15MINUTESCONSIDERATIONNEEDSTOBEGIVENTOTHEPARTICLESIZEWHILETAKINGMOISTURESAMPLESWHENMETWITHOVERSIZECARGO,THISSHOULDBEBROKENUPONCEOVERSIZEHASBEENMANUALLYREDUCEDITCANNOTLATERBEUSEDFORSIZINGPURPOSESTAKE5KGASTHERETAINEDTESTEDMOISTURESAMPLERETAINEDSAMPLESHALLBEINANAIRPROOFCONTAINERTHENUMBERANDMINIMUMMASSOFPARTSFORMOISTUREDETERMINATIONISSPECIFIEDINTABLE3ANDTABLE4表3水分试验样的个数TABLE3NUMBEROFPARTSFORMOISTUREDETERMINATION试样制备MOISTURESAMPLEPREP每个交货批的副样个数NUMBEROFSUBSAMPLEOFEACHLOT被测试验样个数NUMBEROFTESTS从大样中制备FROMTHEBULKSAMPLE从副样中制备最少ATLEASTFROMTHESUBSAMPLE最少ATLEAST从份样中制备FROMTHEINCREMENT最少ATLEAST表4水分试验样的最小质量TABLE4MINIMUMMASSOFPARTSFORMOISTUREDETERMINATION试验样的最大公称粒度（MM）NOMINALTOPSIZEOFMOISTURESAMPLEMM试验样的最小质量（KG）MINIMUMMASSOFMOISTURESAMPLEKG3151022451001注粒度大于315MM时应破碎到315MM以下REMARKWHENTHESIZEISOVER315MM,ITSHALLBECRUSHEDBELOW315MM6、品质样的制备QUALITYSAMPLEPREPARATIONA由于镍矿的水分较大，粘度较大，不利于粒度筛分和品质样的制备，因此对于较粘和水分大的货物应当将其进行预干燥自然风干或使用风干机，使样品较易破碎，在风干的过程中要防止样品被污染。在交货批检验项目有粒度要求时，应当先进行粒度分析，然后将所有样品包括粒度分析后的样品全部进行破碎。破碎后的样品充分混合后，置于清洁的钢板上进行缩分，每一个取样单元作为一个大样（参照下列流程图）。SINCENICKELOREHASHIGHMOISTURECONTENTANDCANALSOBESTICKYWHICHISNOTGOODFOREITHERSIZINGANDQUALITYSAMPLEPREPARATIONITCANBEPREDRIEDINTHEAIRORBYAIRDRYER,WHICHSHOULDMAKEITEASIERTOHANDLEDURINGTHEDRYINGPROCESS,PREVENTTHESAMPLEFROMBEINGCONTAMINATEDIFTHECLIENTREQUIRESSIZEDETERMINATIONFORTHECONSIGNMENT,THESIZEDETERMINATIONSHALLBEPERFORMEDFIRST,ANDTHENALLTHESAMPLESINCLUDINGTHOSEAFTERSIZINGSHALLBECRUSHEDTHECRUSHEDSAMPLESHALLBEMIXEDTHOROUGHLYANDPUTONTOACLEANSTEELPLATEANDDIVIDED,WITHEACHSAMPLINGLOTASABULKSAMPLEASSPECIFIEDINBELOWFLOWSHEET制样流程图SAMPLEPREPARATIONFLOWSHEETB）样品破碎的具体方法DETAILEDMETHODOFCRUSHINGSAMPLE样品的破碎应使用机械设备，手工破碎只限于破碎个别大块样品至第一阶段破碎机的最大给料粒度。THECRUSHINGOFTHESAMPLESHALLBEPERFORMEDBYMECHANICALMEANSMANUALCRUSHINGISONLYTOBEUSEDTOCRUSHSPECIFICLARGEPIECESOFCARGOINORDERTOALLOWFURTHERCRUSHINGBYMECHANICALMANS破碎前需用本批镍矿同一来源的冲刷样品对破碎机进行清洗，然后再用毛刷等工具清扫干净，破碎后残留在破碎机内部的样品，必须全部取出，防止污染下一个样品。BEFORECRUSHING,THECRUSHERSHALLBECLEANEDBYTHESAMEORIGINWASHINGSAMPLEOFTHISNICKELORE,ANDTHENSWEPTWITHBRUSHAFTERCRUSHING,THEREMAINEDSAMPLESHALLBECOMPLETELYREMOVEDSOASNOTTOCONTAMINATETHENEXTONEC）样品的缩分方法SAMPLEDIVISIONMETHOD网格法将样品充分混合后置于已用样品刷好的钢板上，铺成长方形平堆，然后将平堆划成等分的网格，缩分大样时不得少于20格；缩分副样时不得少于12格；缩分份样时不得少于4格。用挡板及样品铲插至底部，从每个格取等量的一铲，集合为缩分样品，当大样数量多时，可将大样分成几个等分，分次按上述操作进行（见图2）。样品最大粒度，样层厚度和份样铲尺寸如表5、图3。INCREMENTDIVISIONMIXTHESAMPLETHOROUGHLYANDPUTITONTOTHESTEELPLATEINTHESHAPEOFARECTANGLEDIVIDETHESURFACEINTOEQUALSEGMENTS,NOTLESSTHAN20SEGMENTSWHILEDIVIDINGTHEBULKSAMPLEANDNOTLESSTHAN12SEGMENTSWHENDIVIDINGTHESUBSAMPLENOTLESSTHAN4SEGMENTSWHILEDIVIDINGTHEINDIVIDUALINCREMENTSUSEBAFFLEANDINCREMENTSCOOPTOINSERTTHEENDANDDRAWANEQUALSCOOPFROMEACHSEGMENTTOMAKEADIVIDEDSAMPLEIFTOOMUCHQUANTITYOFBULKSAMPLE,CANDIVIDETHEBULKSAMPLEINTOSEVERALPARTSANDACTSEVERALTIMESASPERTHEABOVEASSPECIFIEDINFIGURE2MAXIMUMSIZEOFSAMPLE,THICKNESSOFSAMPLEANDDIMENSIONSOFINCREMENTSCOOPARESPECIFIEDINTABLE5ANDFIGURE3表5样品最大粒度、样品层厚度和份样铲尺寸TABLE5MAXIMUMSIZEOFSAMPLE,THICKNESSOFSAMPLEANDDIMENSIONSOFINCREMENTSCOOP份样铲尺寸（MM）DIMENSIONSOFINCREMENTSCOOP样品最大粒度（MM）MAXIMUMSIZEOFSAMPLE样品层厚度（MM）THICKNESSOFSAMPLEABCD份样铲材料厚度（MM）THICKNESSOFMATERIALSFORINCREMENTSCOOP224354580458070210253560356050152030503050401315254025403005110153015302505（图3FIGURE3）圆锥四分法将样品置于已用样品刷好的钢板上，堆成圆锥形，每铲由圆锥顶尖落下，使其均匀地沿锥尖散落，注意勿使圆锥中心错位，如此反复至少移堆三次，使其充分混匀，然后将锥尖压平，用十字板自上插下，分成四等份，任取两个对角的等份，重复操作数次，缩分至不少于最少留样量。CONINGANDQUARTERINGMETHODPUTTHESAMPLEONTOTHESTEELPLATEINTHEFORMOFACONEEACHSCOOPSHALLBEINSERTEDFROMTHETOPOFCONICALTOMAKEITSPREADALONGTHETOPEVENLY,ANDPAYATTENTIONNOTTOMISPLACETHECENTEROFCONEDOITATLEAST3TIMESANDMIXEDTHOROUGHLYTHENFLATTENTHETOPANDUSETHECROSSPLATEFROMTOPTOBOTTOMTODIVIDEINTO4EQUALSEGMENTS,RANDOMLYTAKEOUT2OPPOSITESEGMENTSANDDOITREPEATEDLYFORSEVERALTIMESANDFINALLYDIVIDEDINTONOTLESSTHANTHEMINIMUMRETAINEDQUANTITY由于大颗粒样品堆成圆锥时容易产生偏析，造成缩分偏差，样品粒度大于10MM不宜使用圆锥四分法，最好使用二分器。SINCEALARGEPARTICLESIZECANEASILYCAUSEDIVISIONDEVIATION,MATERIALOVER10MMISNOTSUITABLEFORCONINGANDQUARTERINGMETHODINTHISINSTANCEARIFFLEDIVIDERSHOULDBEUSED二分器缩分法二分器系非机械式样品缩分器，通常用手工给料，样品通过二分器被分成二等份，一份保留，另一份弃去。格槽宽度至少为样品最大粒度的25倍，二分器的一半槽数一般为8个以上，所用的二分器须参照GB20074和GB20075的规定。RIFFLEDIVISIONMETHODARIFFLEISAKINDOFNONMECHANICALSAMPLEDIVIDER,WHICHISUSUALLYFEDMANUALLYTHESAMPLEISDIVIDEDINTO2EQUALPARTSBYRIFFLE,WITHONERETAINEDANDONEREJECTEDTHEWIDTHOFEACHCELLISATLEAST25TIMESOFTHESAMPLESTOPSIZE,ANDTHENUMBEROFHALFCELLOFTHERIFFLEISMORETHAN8THERIFFLEUSEDSHALLREFERTOGB20074SCATTERTHESAMPLEEVENLYALONGALLTHECELLSOFTHERIFFLEWHILEDIVIDINGCONTROLTHESPEEDOFFEEDINGTOASSURENOCONGESTIONOFCELLIFANYCONGESTION,SHALLCLEANUPBEFORECONTINUEC通过二分器的样品收集于两个接收容器中。SAMPLETHROUGHRIFFLEWILLBECOLLECTEDINTO2RECEIVINGCONTAINERSD随机选择一个接收器内的样品为保留样品，如需进一步缩分，保留样品可以再次或多次通过二分器，此时要从二分器两侧的接收器内交替收集保留样品，接收器应与主体密合，以减少粉尘和水分的损失。RANDOMLYSELECTTHESAMPLEINONERECEIVINGCONTAINERASRETAINED,ANDIFFURTHERDIVISIONISNEEDED,THERETAINEDSAMPLECANBEPUTTHROUGHTHERIFFLEONTWOORMOREOC