《工业分析 Industrial Analysis》课件-项目四：肥料分析

项目四：肥料分析任务一：固体样品采样方法固体样品采样工具与采样方法课程：工业分析中文Scenario4:FertilizerAnalysisTask1:SamplingmethodforsolidsamplesSamplingtoolsandmethodsforsolidsamplesCourse:IndustrialAnalysisEglish

一、固体样品采样工具固体存在形态粉末状颗粒状表面坚硬的固体固体一般均匀性较差，存在形态不同，使用的采样工具也有差异，同时注意取样有代表性中文

一、SamplingtoolsforsolidsamplesTheformofsolidexistencethestateofsomethingwhichlikepowdergraininessAsolidwithahardsurfaceSolidsgenerallyhavepooruniformity,andthesamplingtoolsusedduringsamplingmayvaryduetotheirdifferentshapes.Atthesametime,itisimportanttoensurethatthecollectedsamplesarerepresentativeEglish可采集粉末状、小颗粒状、块状固体样品，一般从物料堆表面采集样品取样铲中文Thesamplingshovelcancollectpowder,smallparticle,andblocksolidsamples,usuallycollectedfromthesurfaceofthematerialpileSamplingshovelEglish取样探子适用于粉末、小颗粒、小晶体等固体化工产品采样，可深入样品内部采集样品。采样探子分为末端开口的采样探子、末端封闭的采样探子、窗口关闭式采样探子和布袋式采样探子。末端封闭式布袋式可封闭式中文SamplingprobeThesamplingprobeissuitableforsamplingsolidchemicalproductssuchaspowders,smallparticles,andsmallcrystals,andcancollectsamplesdeepinsidethesample.Samplingprobesaredividedintoendopeningsamplingprobes,endclosedsamplingprobes,windowclosedsamplingprobes,andbagsamplingprobes.endclosedsamplingprobebagsamplingprobewindowclosedsamplingprobeEglish取样钻：由金属圆筒和旋转钻头组成，适用于较坚硬的固体采样中文Samplingdrill:composedofametalcylinderandarotatingdrillbit,suitableforsamplinghardersolidsEglish3、确定采取样品的方法一般采样程序为：1、确定采取的样品数2、确定采取的样品量

二、采样方法中文3.DeterminethemethodoftakingsamplesThegeneralsamplingprocedureis:1.Determinethenumberofsamplestobetaken2.Determinethesamplesizetobetaken

二、SamplingmethodEglish1、采样单元数的确定（1）单元物料

采样单元数n的确定(N为总件数）:

单元数＞500时，按n=3×单元数＜500时，按照规定件数取样中文1.Determinationofthenumberofsamplingunits（1）UnitmaterialDeterminationofthenumberofsamplingunitsn(Nisthetotalnumberofpieces):Whenthenumberofunits>500,

Whenthenumberofunitsislessthan500,takesamplesaccordingtothespecifiednumberofpiecesEglish总体物料单元选取的最少单元总体物料单元选取的最少单元1~10全部单元182~2161811~4911217~2541950~6412255~2962065~8113297~3432182~10114344~39422102~12515395~45023126~15116451~50024152~18117采样单元数的规定中文OverallmaterialunitOverallmaterialunitMinimumunitsselectedMinimumunitsselectedTotalunitsRegulationsonthenumberofsamplingunitsEglish当物料量少于2.5t，采样量为7个单元（或点）当物料量为2.5~80t时，采样量单元为当物料量大于80t，采样为40个单元（2）散装物料中文Whenthematerialquantityislessthan2.5t,thesamplingquantityis7units(orpoints)Whenthematerialquantityis2.5-80t,thesamplingunitisWhenthematerialquantityisgreaterthan80t,thenumberofsamplingunitsis40（2）bulkmaterialsEglish对采得的样品如需要制样处理时，必须满足加工处理的需要2、样品量的确定满足以下要求满足三次重复检测用量当需要留存备考样品时，满足备考样品量中文Ifsamplepreparationandprocessingarerequiredforthecollectedsamples,theymustmeettheprocessingrequirements2、DeterminationofsamplesizeMeetthefollowingrequirements:SatisfytheusageofthreerepeatedtestsWhenitisnecessarytoretainpreparationsamples,theamountofpreparationsamplesmustbemetEglishT-采样的质量间隔Q-样品批量，tn-采样的单元数3、采样方法的确定（1）从物料流中采样用合适采样器随机或按一定时间间隔采样，如按时间间隔采样，采样的质量间隔T为：中文T-qualityintervalforsamplingQ-thetotalamountofabatchofsamples,tn-numberofsampledunits3、Determinationofsamplingmethod（1）SamplingfrommaterialflowWhensamplinginthematerialflow,useasuitablesamplertorandomlyoratacertaintimeintervalforsampling.Ifsamplingisdoneatatimeinterval,thequalityintervalTforsamplingis:Eglish布点时首末两个点距车角至少1米，其他点平均布置取样点布置在运输工具的对角线上，可以用三点法、五点法布置采样点。三点法五点法（2）从运输工具中采样中文Whenarrangingpoints,thefirstandlasttwopointsshouldbeatleast1meterawayfromthecornerofthecar,andtheotherpointsshouldbeevenlyarrangedonthediagonalThesamplingpointsarearrangedonthediagonalofthetransportationvehicle,andcanbearrangedusingthethree-pointmethodorthefivepointmethod.three-pointmethodfivepointmethod（2）SamplingfromtransportationvehiclesEglish（3）从物料堆中采样根据物料堆的形状和子样的数目，将取样点分布在堆的顶部、腰部、底部（底部距地面0.5m）采样时先除去0.2m的表层再采样中文（3）SamplingfrommaterialpileAccordingtotheshapeofthematerialpileandthenumberofsubsamples,distributethesamplingpointsatthetop,waist,andbottomofthepile(0.5

mfromthegroundatthebottom)Remove0.2

mofsurfacelayerbeforesamplingEglish项目四：肥料分析任务二：磷肥分析肥料种类及磷肥制样方法课程：工业分析中文Scenario4:FertilizerAnalysisTask2:PhosphatefertilizeranalysisFertilizertypesandphosphorusfertilizersamplingmethodsCourse:IndustrialAnalysisEglish一、肥料种类及取样方法

植物生长，几乎需要所有的化学元素，但最主要的是N、P、K三要素。肥料的作用？肥料是促进植物生长，提高农作物产量的重要物质之一。

N、P、K由何而来呢？植物生长的三要素？肥料中文一、Fertilizertypesandsamplingmethods

Plantgrowthrequiresalmostallchemicalelements,butthemostimportantonesareN,P,andK.Whatisthefunctionoffertilizer?Fertilizerisoneoftheimportantsubstancesthatpromoteplantgrowthandincreasecropyield.

N、P、KWherediditcomefrom?Whatarethethreeelementsofplantgrowth?fertilizerEglish磷肥的作用促进籽粒饱满；促使棉花、瓜类、茄果类蔬菜及果树的开花结果，提高结果率；增加甜菜、甘蔗、西瓜等的糖分；油菜籽的含油量。近年来世界磷肥工业逐渐复苏，生产能力增长较快，中国、美国及印度成为世界三大磷肥生产国。中文TheroleofphosphatefertilizerPhosphatefertilizercanpromoteplumpgrains;Promotethefloweringandfruitingofcotton,melons,eggplantvegetables,andfruittrees,andimprovethefruitingrate;Increasethesugarcontentofsugarbeets,sugarcane,watermelons,etc;Increasetheoilcontentofrapeseed.Inrecentyears,theworld'sphosphatefertilizerindustryhasgraduallyrecoveredandproductioncapacityhasgrownrapidly.China,theUnitedStates,andIndiahavebecometheworld'sthreelargestphosphatefertilizerproducingcountries.Eglish

以矿物、空气、海水等为原料，经化学和机械加工方法制造，能供给农作物营养及提高土壤肥力的化学物质。肥料包括自然肥料和化学肥料。中文

Chemicalfertilizersarechemicalsmadefromminerals,air,seawater,andotherrawmaterialsthroughchemicalandmechanicalprocessingmethods,whichcanprovidenutrientstocropsandimprovesoilfertility.Fertilizersincludenaturalfertilizersandchemicalfertilizers.ClassificationofchemicalfertilizersDividedbynutritionalelementsnitrogenfertilizerphosphatefertilizerpotashfertilizerCompoundfertilizerTraceelementfertilizerEglish

有效成分含量，磷肥以有效五氧化二磷的质量分数表示。氮肥以氮元素的质量分数表示。钾肥以氧化钾的质量分数表示。微量元素以该元素的质量分数表示。

化学肥料的分析项目包括水分含量，有效成分含量和杂质含量等分析。化学性质酸性肥料:硫酸铵中性肥料:尿素碱性肥料:碳酸氢铵中文Theeffectiveingredientcontentisexpressedasthemassfractionofeffectivephosphoruspentoxideinphosphorusfertilizer.Nitrogenfertilizerisexpressedasthemassfractionofnitrogenelement.Potassiumfertilizerisexpressedasthemassfractionofpotassiumoxide.Traceelementsarerepresentedbytheirmassfraction.Theanalysisitemsofchemicalfertilizersincludemoisturecontent,activeingredientcontent,andimpuritycontent.化学性质Acidfertilizer:ammoniumsulfateNeutralfertilizer:ureaAlkalinefertilizer:ammoniumbicarbonate

ClassifiedbychemicalpropertiesEglish

取样时，将取样探子由袋口的一角沿对角线插入袋内的1/3～3/4处，旋转180°后抽出，刮出钻槽中物料作为一个子样。取样探子

对于袋装化肥，通常规定50件以内抽取5件；51～100件，每增10件，加取1件；101～500件，每增50件，加取2件；501～1000件以内，每增100件，加取2件；1001～5000件以内，每增100件，加取1件。将子样均匀地分布该批物料中，然后用采样工具进行采集。二、肥料的取样中文Whensampling,insertthesamplingprobediagonallyfromonecornerofthebagopeninginto1/3to3/4ofthebag,rotate180°,andthenextractit.Scrapeoutthematerialinthedrillinggrooveasasubsample.samplingprobe

Forbaggedfertilizers,itisusuallyrequiredtoextract5pieceswithin50pieces;51-100pieces,foreveryadditional10pieces,anadditionalpiecewillbetaken;101-500pieces,foreveryadditional50pieces,anadditional2pieceswillbetaken;Within501-1000pieces,foreveryadditional100pieces,anadditional2pieceswillbetaken;Within1001-5000pieces,foreveryadditional100pieces,anadditionalpiecewillbetaken.Distributethesubsamplesevenlyamongthebatchofmaterials,andthencollectthemusingsamplingtools.二、SamplingoffertilizersEglish

在分析之前，应将所采的一瓶样品粉碎至规定粒度(一般要求不超过1~2mm)，混合均匀，用四分法缩分至100g左右，置于洁净、干燥瓶中，作质量分析之用。

将每批所选取的样品合并在一起充分混匀，然后用四分法缩分至不少于500g，分装在两个清洁、干燥并具有磨口塞的广口瓶或带盖聚乙烯瓶中，贴上标签。注明生产厂家、产品名称、批号、采样日期和采样人姓名。一瓶供试样制备，一瓶密封保存2个月以备。中文

Beforeanalysis,thecollectedsamplesshouldbecrushedtothespecifiedparticlesize(generallynotexceeding1-2mm),mixedevenly,andreducedtoabout100gusingthequarteringmethod.Theyshouldbeplacedinacleananddrybottleforqualityanalysis.

Combinetheselectedsamplesfromeachbatchandmixthoroughly.Then,usethequarteringmethodtoreducethemtonolessthan500g.Dividethemintotwoclean,drywidemouthedbottlesorcappedpolyethylenebottleswithgroundstoppers,andlabelthem.Indicatethemanufacturer,productname,batchnumber,samplingdate,andnameofthesampler.Onebottleisforsamplepreparation,andonebottleissealedandstoredfor2monthsforpreparation.Eglish三、磷肥制样方法1、磷肥分类分类

自然磷肥：磷矿石、骨粉及骨灰等化学磷肥：以自然矿石为原料，经化学加工处理的含磷肥料中文三、Samplepreparationmethodforphosphatefertilizer1、ClassificationofphosphatefertilizersClassificationNaturalphosphatefertilizer:phosphaterock,bonemeal,andboneash,etcChemicalphosphorusfertilizer:afertilizercontainingphosphorusobtainedthroughchemicalprocessingusingnaturaloresasrawmaterialsEglish

酸法磷肥(速效磷肥)：用无机酸加工处理磷矿石所制造的，如过磷酸钙，重过磷酸钙，因其中含有易溶于水的磷化物，植物易吸收，故又称为“速效磷肥”。

热法磷肥(迟效磷肥)：磷矿石和其他配料(如白云石、滑石等)或不加配料，经高温煅烧分解所制造的磷肥。如钙镁磷肥、钢渣磷肥等。因其所含磷化物难溶于水，施用后经长时间后可被土壤中有机弱酸缓慢溶解而被植物吸收，故又称为“迟效磷肥”。化学磷肥根据加工方法不同可以分为：中文Acidbasedphosphatefertilizer:Fertilizermadebyprocessingphosphaterockwithinorganicacids,suchascalciumsuperphosphateandheavysuperphosphate,isalsoknownas"quickactingphosphatefertilizer"becauseitcontainswater-solublephosphidesthatareeasilyabsorbedbyplants.Thermalphosphatefertilizer:phosphaterockandotheringredients(suchasdolomite,talc,etc.)orphosphatefertilizerproducedbyhigh-temperaturecalcinationanddecompositionwithoutingredients.Suchascalciummagnesiumphosphatefertilizer,steelslagphosphatefertilizer,etc.Duetoitsinsolublephosphidesinwater,itcanbeslowlydissolvedbyorganicweakacidsinthesoilandabsorbedbyplantsafterlong-termapplication,henceitisalsoknownas"delayedactingphosphatefertilizer".Chemicalphosphorusfertilizercanbedividedinto:Eglish

磷肥的组成较为复杂，往往一种磷肥中同时含有几种不同性质的含磷化合物。磷肥的主要成分是磷酸的钙盐，有的还含有游离的磷酸。磷肥组成不一样，溶解性不一样，制样方法也是有差异的。中文

Thecompositionofphosphorusfertilizerisrelativelycomplex,oftencontainingseveralphosphoruscontainingcompoundswithdifferentpropertiesinonetypeofphosphorusfertilizer.Themaincomponentofphosphatefertilizeristhecalciumsaltofphosphate,someofwhichalsocontainfreephosphate.

Thecompositionofphosphorusfertilizervaries,andthesolubilityandsamplepreparationmethodsalsovary.Eglish

检验中是指被柠檬酸铵溶液或2%柠檬酸溶液溶解的含磷化合物。中文WatersolublephosphoruscompoundsPhosphoricacid,calciumdihydrogenphosphate(alsoknownasmonocalciumphosphate)[Ca(H2PO4)2]Calciumsuperphosphateandheavysuperphosphatemainlycontainwater-solublephosphoruscompounds,sotheyarealsocalledwater-solublephosphorusfertilizers.CitricacidsolublephosphoruscompoundsThephosphoruscompoundsthatcanbedissolvedbyacidicsubstancessecretedbyplantrootsandabsorbedandutilizedbyplantsarecalledlemonsolublephosphoruscompounds.Suchascrystallinecalciumhydrogenphosphate,alsoknownasdicalciumphosphate(CaHPO4

·2H2O)ortetracalciumphosphate(Ca4P2O9

or4CaO·P2O5).Citricacidsolublephosphoruscompoundsrefertophosphoruscontainingcompoundsdissolvedinammoniumcitratesolutionor2%citricacidsolutionduringtesting.Eglish全磷：磷肥中所有含磷化合物中含磷量的总和。

不论是全磷还是有效磷仅是制备试液的方法不同，其测定方法相同。有效磷：水溶性磷化物和柠檬酸溶性磷化合物中的磷。中文Totalphosphorus:Thetotalphosphoruscontentofallphosphoruscontainingcompoundsinphosphorusfertilizer.Whetheritistotalphosphorusoreffectivephosphorus,themethodofpreparingthetestsolutionisdifferent,andthedeterminationmethodisthesame.Effectivephosphorus:phosphorusinwater-solublephosphidesandcitricacidsolublephosphoruscompounds.InsolublephosphoruscompoundsPhosphoruscontainingcompoundsthatareinsolubleinorganicweakacids,suchastricalciumphosphate[Ca3(PO4)2],ironphosphate,aluminumphosphate,etc.,arecalledinsolublephosphoruscompoundsEglish

称取过磷酸钙约1.5g或重过磷酸钙约0.8g（含P2O5约200-300毫克）于小乳钵中，加水约25mL，小心研磨5-10分钟，静置待澄清。以慢速滤纸倾泻过滤于已经预先注有1：1硝酸5mL的250mL容量瓶中。向乳钵内的残渣中，再加水约25mL，继续研磨、澄清、过滤，共三次。最后一次，将残渣全部转移于滤纸上。充分洗涤至容量瓶内溶液的体积约230mL左右。稀释至刻度，混合均匀，供测定水溶性磷。例如：（1）水溶性磷的提取2、磷肥制样方法中文

Weighabout1.5gofcalciumsuperphosphateorabout0.8gofheavycalciumsuperphosphate(containingabout200-300milligramsofP2O5)inasmallbowl,addabout25mLofwater,carefullygrindfor5-10minutes,andletitstandforclarification.Pourandfilterslowlywithfilterpaperintoa250mLvolumetricflaskprefilledwith5mLof1:1nitricacid.Addabout25mLofwatertotheresidueinthebowl,continuegrinding,clarifying,andfilteringthreetimes.Forthelasttime,transferalltheresidueontothefilterpaper.Washthoroughlyuntilthevolumeofthesolutioninthevolumetricflaskisabout230mL.Dilutetothemark,mixevenly,andusethissolutionformeasuringwater-solublephosphorus.example：（1）Extractionofwater-solublephosphorus2、SamplepreparationmethodforphosphatefertilizerEglish（2）柠檬酸溶性磷的提取中文（2）ExtractionofCitricAcidSolublePhosphorusUsinganammoniasolutionofammoniumcitrateora2%citricacidsolutionasanextractant,thephosphorusfertilizerresidueafterextractingwater-solublephosphorusisextracted.Theammoniasolutionofammoniumcitrate,alsoknownasPetermannreagent,iscomposedof173gofunweatheredmonohydratecitricacidand51gofammoniain1LofsolutionEglish在测定全磷时，通常直接用盐酸和硝酸混合酸溶，盐酸是溶解难溶性磷化合物，硝酸主要是防止磷被还原成PH3而挥发损失。（3）难溶性磷的提取中文Whenmeasuringtotalphosphorus,amixtureofhydrochloricacidandnitricacidisusuallyusedtodissolvephosphorusfertilizerdirectly.Hydrochloricaciddissolvesinsolublephosphoruscompounds,whilenitricacidmainlypreventsphosphorusfrombeingreducedtoPH3andcausingvolatilizationloss.（3）ExtractionofinsolublephosphorusinsolublephosphorusisgenerallydissolvedinstrongacidssuchashydrochloricacidEglish项目四：肥料分析任务四：钾肥分析钾肥分析课程：工业分析中文Scenario4:FertilizerAnalysisTask4:PotassiumfertilizeranalysisPotassiumfertilizeranalysisCourse:IndustrialAnalysisEglish一、钾肥种类中文一、TypesofpotassiumfertilizersPotassiumfertilizerisdividedintotwocategories:naturalpotassiumfertilizerandchemicalpotassiumfertilizer.Thesumofwater-solubleandweaklyacidsolublepotassiumsaltsinpotassiumfertilizeriscalledeffectivepotassium.Thesumofavailablepotassiumandinsolublepotassiumsaltsiscalledtotalpotassium.ThepotassiumcontentofpotassiumfertilizerisexpressedasK2O.Whenmeasuringeffectivepotassium,asamplesolutionisusuallypreparedbydissolvingitinhotwater;Ifthesamplecontainsweaklyacidsolublepotassiumsalt,dissolvetheavailablepotassiuminhotwaterwithasmallamountofhydrochloricacidadded.Whenmeasuringthetotalpotassiumcontent,thesamplesolutionisgenerallypreparedbystrongaciddissolutionoralkalimeltingmethod.Eglish二、钾肥分析方法

钾肥中有效钾的测定方法有四苯硼酸钾重量法、四苯硼酸钠容量法和火焰光度法。四苯硼酸钾重量法和四苯硼酸钠容量法简便、准确、快速，适用于含氧化钾量较高的钾肥测定。当试样中含氧化钾小于2%时，采用火焰光度法测定。中文二、Analysismethodsforpotassiumfertilizer

Themethodsfordeterminingeffectivepotassiuminpotassiumfertilizersincludepotassiumtetraphenylborategravimetricmethod,sodiumtetraphenylboratevolumetricmethod,andflamephotometry.

Thepotassiumtetraphenylborategravimetricmethodandthesodiumtetraphenylboratevolumetricmethodaresimple,accurate,andfast,suitableforthedeterminationofpotassiumfertilizerswithhighpotassiumoxidecontent.Whenthecontentofpotassiumoxideinthesampleislessthan2%,flamephotometryisusedformeasurement.Eglish（1）方法原理：在碱性条件下加热消除试样溶液中铵离子的干扰，加入乙二胺四乙酸二钠(EDTA)螯合其他微量阳离子，以消除干扰分析结果的阳离子。在微碱性介质中，四苯硼酸钠与钾反应生成四苯硼酸钾沉淀，过滤、干燥沉淀并称量。1、四苯硼酸钾重量法中文(1)Methodprinciple:Heatunderalkalineconditionstoeliminatetheinterferenceofammoniumionsinthesamplesolution,andadddisodiumethylenediaminetetraacetate(EDTA)tochelateothertracecationstoeliminatetheinterferenceofcationsintheanalysisresults.Inaslightlyalkalinemedium,sodiumtetraphenylboratereactswithpotassiumtoformpotassiumtetraphenylborateprecipitate,whichisfiltered,dried,andweighed.1、potassiumtetraphenylborategravimetricmethodwhiteEglish（2）结果计算氧化钾(K2O)的含量w1以质量分数%表示，按下式计算：中文（2）resultcalculation

Thecontentofpotassiumoxide(K2O)w1isexpressedasamassfraction%,andiscalculatedusingthefollowingformula:Eglish（3）实验步骤

移取一定量溶液，加入EDTA溶液及酚酞指示液，在搅拌下逐滴加入氢氧化钠溶液至红色出现并过量1mL。加热微沸15min(此时溶液应保持红色)。在搅拌下逐滴加入四苯硼钠溶液，在流水中迅速冷却至室温并放置15min。先过滤上层清液，再用洗涤液转移沉淀至过滤器中，用洗涤液洗涤沉淀，干燥称量。中文（3）Procedure

Takeacertainamountofsamplesolution,addEDTAsolutionandphenolphthaleinindicatorsolution,andaddsodiumhydroxidesolutiondropwisewhilestirringuntilredappearsand1mLofexcesssodiumhydroxidesolutionisadded.Heatandslightlyboilfor15minutes(atthistime,thesolutionshouldremainred).Addsodiumtetraphenylboratesolutiondropwisewhilestirring,rapidlycooltoroomtemperatureinflowingwater,andletitstandfor15minutes.Firstfiltertheupperclearliquid,thentransfertheprecipitatetothefilterwithwashingsolution.Washtheprecipitatewithwashingsolution,dryit,andweighit.Eglish（1）方法原理在碱性条件下加热消除试样溶液中铵离子的干扰，加入乙二胺四乙酸二钠(EDTA)消除其他阳离子的干扰，在微碱性介质中，以过量的四苯硼酸钠与钾反应生成四苯硼酸钾沉淀，过滤，滤液中过量的四苯硼酸钠以达旦黄作指示剂，用季铵盐返滴至溶液由黄变成明显的粉红色2、四苯硼酸钠容量法中文(1)MethodprincipleHeatunderalkalineconditionstoeliminatetheinterferenceofammoniumionsinthesamplesolution,andadddiso