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【商检行业标准(SN)】 出口粮谷及油籽中烯菌酮残留量检验方法

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  • SN0584-1996
  • 现行

基本信息

  • 标准号:

    SN 0584-1996

  • 标准名称:

    出口粮谷及油籽中烯菌酮残留量检验方法

  • 标准类别:

    商检行业标准(SN)

  • 标准状态:

    现行
  • 发布日期:

    1996-11-15
  • 实施日期:

    1997-05-01
  • 出版语种:

    简体中文
  • 下载格式:

    .rar.pdf
  • 下载大小:

    416.11 KB

标准分类号

  • 中标分类号:

    农业、林业>>农业、林业综合>>B04基础标准与通用方法

关联标准

出版信息

  • 页数:

    15页
  • 标准价格:

    12.0 元
  • 出版日期:

    1997-05-01

其他信息

  • 起草人:

    荣会、王明太、牟峻、李庆才
  • 起草单位:

    中华人民共和国吉林进出口商品检验局
  • 归口单位:

    中华人民共和国国家进出口商品检验局
  • 提出单位:

    中华人民共和国国家进出口商品检验局
  • 发布部门:

    中华人民共和国国家进出口商品检验局
  • 主管部门:

    中华人民共和国国家进出口商品检验局
  • 相关标签:

    出口 粮谷 及油籽 残留量 检验 方法
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标准简介:

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本标准规定了出口粮谷及油籽中烯菌酮残留量检验的抽样、制样和气相色谱测定方法。本标准适用于出口糙米、玉米、大豆、花生仁中烯菌酮残留量的检验。 SN 0584-1996 出口粮谷及油籽中烯菌酮残留量检验方法 SN0584-1996

标准内容标准内容

部分标准内容:

中华人民共和国进出口商品检验行业标准SN 05841996
出口粮谷及油籽中烯菌酮残留量检验方法
Mcthod for the determination of vinclozolinresiducs in cereals and oil sceds for export1996-11-15发布
中华人民共和国国家进出口商品检验局1997-05-01实施
50584-1996
本标准长地落(B/:.1--19浓标痛化T作导划第1单元:标准的起卓与在述划则、第1部分:乐准缩写热基木划定及,0001二995出口商品中农药.典药残也量及牛物每索检验方法际准销写的欣本规定的要发过行编书的.其广迎守方法是参考国内外代关文梵,经研究、改逊利验运后而制定的。云标准同时制定一推样和制栏方法:测定低限是板据占际上对谷皮剂格中带菌的我首量的最高限盘和测定方法的教度而制定的。本标准附录A为提示的阴录:
本标准由中大氏和国家并凹口品资验局据出计归。本标准起艺单位,工华人民共和玉吉林逊出商异检验局。本标准主要起草人:茉会、王明不,会域,李庆本标准系首次发市的行止际准。[
1范围
中华人民共和国进出口商品检验行业标准出口粮谷及油籽中烯菌酮残留型检验方法
Methad for the determinatinn af vinclozolirresidues in cereals and oil xeeds for exportSN058-1995
本标准规定了出;跟芥及油籽中希菌酮残留册验的抽样,司样和气柑色谐测定方讼,本标碰适月山二糙米,玉米、大豆、花生仁烯菌酮战留些的检,2抽荐和制拌
2.1检验批
双个超过211为一检验托,2011袋装随米约400装袋装玉米成大豆约3200装装装花生仁约34nm施。工米或大豆有时为敢装品同验验批节两品高且有可特正,如包装、惊证,产求,规格和等级等,2.7抽样
2-2.1袋装货品
接式1>计算拍择装激
本中,
全北发效:
油扩数。
注:值取些效,小款求分司前进位为禁微22.2供货品(下米戒人
货堆高度不性过2五,接货堆区设点。以为一个取栏区,再风设中及日角臣边1处个点。等地划一个表丰区,增设3个点。2.3抽样工具
2.3.1金两单普片样器:金长55m(包薪于柄),直径1.5--2.0cm.沟指长度声超过装角线长度的2.3.?金厚双取择器安分m2m(均拦两种,内、管同部位分以下,1个:,每个153m宽2.~2.51m。以等内径为2.5~5.m取挡保头长:m2.3.3段作铲或取样与。
2. 3. 2 等伴长。
2.3.5样器,简或2,空封。
2.3.6分拦成适用端动,
2.4猫法
2.2.1按猴拍样
中华人民共和国回察进出口商品检验周19961115批滑19970501实施
SNC584-1996
2.4.1.1阅包抽料,以增案内各部位随机拍取2.2.1规定的应推样带数的10%(每批一般不少于3装!存袋口链线全能拆并,平置1分样有或其他洁净的铺格物上,及手暴提我底两角,提起约成4倾价例拖约1四,使我内货物全部倒出。合右袋内利袋间完质忌还匀,确识情说正常店,用取价铲随机七各部位拍改性品,井即将车品例人盛样器内:每推取推品的数应整本较。2.4.1.2我内油:恢么.2.1规定的应抽半袋数除削包推样期数).在堆保因周的上,11.下各层以业线形走向随机拍收:蒸我精米,卡来,人点,花牛亡,月下方法进行取样,到箱米,日余需总取革2.,1州口切下,从每教“角农斜对用方向插人装内.然后将香槛旋转卧上,抽出取空能·三就将作品倒人落样器内。对玉义或大豆.用1长的企历双登管最替(2.3.2),关闭德,从每袋为依彩对仰方间捕入袋内,落启旋转内管以开启爬二,得样右流满内管后,再旋转为盘以关闭种口,抽出取样,立冲轿样品倒人盛提器内,
对花生二,游应拖各袋拆装口箱线3一外.用取样勺从开:处抽取详品,立印整好装口.并将所联样品到人些样器内。
再袋抽取样品范数量变与2.4.1.1基本数,每批所拆收的详品总量应不少于=kg,2.4.2散积独挡,按2.2.2规定的收样点添点油取样元.将胶栏器2.3.2)赠口关闭,以须斜4角势拒人货排至相应深度,旋转圾库器内管以开片抽口,待样品流期内尺,再能转内告以关闭措。推当取栏器,文即将样品倒人盛样器内。从各点所抽成样品的数量严基本一致。每批所抽取的样品总量应不少于4k。2.4.3大缩分
装装作站:合并从削包式袋内抽样所限全部样品,例分样布上,月公样板胺四分法靠分样品至不少于2驾·倒入盛样器内,加后标明标记,并及时送交实验室。数积样品:海拍取的伞部单品阅二分样上·以按上述袋装详品方法逆行,2.5试样制备
2.5.1制年上具
2.5.1.1磨环机。
2.5. 1.2粉碎机。
7.5.1.3筛子206筛、2.0mm孔筛。2.5. 1. 4 分样板。
2.5.1.5盛样册:其塞广口瓶。
2.5.2制样方法
2-5.2.1米、卡米或人可试样司条,将单品按四分法缩分至1kg.用腾摔(2.5.1.1)全前磨碎并道讨26日好,门.均分成两处为试样,分装人洁净的盛样盟内,密时.标明标证,25.2.2花主1.试样=备:存样品接日分祛缩分至%(006,用样品必醉机(2.5.1.2)粉碎,使全邮通对2.0mr圆乳带,混了,均分放两份作为试分装干汽疗护盛样器内,案闭标明标记.2.6证报举存
将试样于5以下光保存,
注,用及过科中必险成效生图物的3测定方法
3.1人法提要
试样中戒留的筛菌酮柔用石油髓提取.提取滤经乙畸反取后,用硅胶层析柱净化,再以就乙款行尘化,用配有电子俘获检器均气相色谱仪测定,外标法定量。3.2试剂和材料
除导有规定外所用试剂均分析纸,3.2.1石油醒:重蒸簡。
3.2.2乙晴:重点愉。
3. 2. 3丙酮。
SN05841996
氯乙酬素液:20%(V/V>.取20mL.氯乙酰氯浴于R0mL石快健中,混匀后,避光低温保存,3.2.5无水硫酸钠:650C灼烧4h,格即后忙于密封客器中备用。3.2.6硅改晨护用.100--200目,用菊在120C活化3h冷却后忙F封容器中舒对3.2.7
的标准品纯度
3.2.的奶菌耐标准溶液:准确称取适盘烯菌酮标睡品.用少量百油醛溶解,并以石由性型表度为心.angml.的标准储备液。根据需要再以不满释成当的标准「作游液3.3仅幕和设备
3.3.1气拒色满仅,配有用子伴状检测器。3.3.2撮蔗器
3. 3. 3航转蒸发器,
恒提水溶竭。
3.3.5望声波发坐群。
3.3.6孤璃净比性.25cm×!.5mtc1.自下而上依次填装2cm高元水蔬酸钠,15g硅胶.2am高无水硫酸钠。使用前用5个mL石油预淋,3.3.7微量注射举:1℃l.。
3.4测定步强
3.4.1报取
称取试样约20g(精确至).=g).置予250ral.具塞形瓶中,加入30ml石醛.振满提取5c.mim,将摄取疫过滤丁2ml.分凌满斗中,并用50mI.而洞醒分两次洗换残查,过滤,会并德液十:逆分液斗书:
3.4.2净化
明入m之脑于主述并波漏斗中.报摇1r·静置1irt,收菜下房子瞻相,上房有油相再分别用2×50rml.乙脂报取。合升之丁款形瓶中,于低于40水资中用膜转蒸发器添编全近十,用1:m1.石油酷处二次超声波浓荡浮解残查:井将溶解液恢入玻璃化中.用150mL油淋港弃大流出液,再入1CCm.内酮-石汇(一混合波洗脱,收洗脱液于梨形瓶,于低于(水浴巾乱能转然发依缩至十。
3.4.3衍兰化
质20mT石过期产波解变查人0.5m醛氯穿变,如,室温~避光放30m荧置期问过行断绞轻搭。区应结束正.于板于40水浴中能转蒸发器浓缩至千,加入3心L飞袖醒以溶解残适,十低4心术浴中月旋转蒸发器浓至干。准确如人.石油以落凝残盗,游液供气拍色讲通定。
3.4.4标准物衔衍生化
准确移取10.道当液度的部菌削标阵1.作奔液十日理试中,用效气次一,控3.4.3探作进行行生化片,决气担色详测定
3.4.5德定
3.4.5.色落杀件
)色谱柱:填定柱!m×3.2ma(id).点充物为10%(m/m5E-3c十ChrcmoorhwAw-DMCS80-100日;
5)色谱扑温度,85
c】进样口温度:260℃;
d)抢激器温度:2T:
SN0584-1996
e)裁气,气,纯99.99%,40l/mim;f)进样量,1 μI.
3.4.5.2色潜测定
根据波中被测农药含情说选完萨度相近的标准工作滤,标准工作液和待测样液中药的润应宜均应在仅器检测的线性范围内,对衍生化的示难工作液与样疫应等体积参插进栏测定,在上还色谱条件一,烯画阐氧乙酰化物的保留时间约为5.6min。探准品色谱图见对录A中室A1。3.4.6空自试验
除不如试单外,均按上述测定步题进行。3.5给采计其和表述
用色谱数磐处理机或按式(2)计算试中筛菌制留全显:x
式中,X--或样中烯期酮残留含量.rng/kgA.e.P
一—样满中烯商酮氧乙酰化衔生物的色谱峰高.m:标准工作液中烯医酮氢酰化衍生物的色潜峰高·mm:标准工作液中烯菌制的浓度.ug/mL;样筛量终定容体积,ml.
最终样液所代麦的试样盘吗。
注,计响结果需将空户直扣险,4测定低限、回收率
4.1测定低限wwW.bzxz.Net
本方法的测定低限为0.02(1g/k%4.2回收率
4.2.1米中矫菌能的回收率实:
烯菌酮添度在0.020mg/kg时,可收率为e.2%希苗切浓度在0.5mg/kg时,回收率为2.-%浠菌酮添划涨度在0.200g/kg时回收率8S.C%。4.2.2正米中菌期的回收率实验整菌纳添加变在0.020mgg时可收率火$2.7%烯菌添加浓在U.u50mg/kg时回收率为56.3%;烯菌耐添加添变止0.2rm/kg时,同收率为3.5系。益.2.3天豆一烯剂酮的同收本交数错:书函添添度在0.020g/kg时,回收率为89.2;带深丽添如浓度在n心mg/kg时+回收率87.1医酮添加法度在U.mg/kg时回收率为84.兴。4.2.4花生仁中希画酮的向收率实验数据:炜菌泰加添度在0.020mkg时,回收率为89.2:烯菌添浓度在skg时回收;
烯菌酬添加浓度0.2;g/kg时日收率为82.(2
SN3584796
(示附示)
标准品气相色增图
A1烯菌削标洋品之航化行生物一作色潜困SN 0584—1996
Forcword
Ttis stinda:d was drafred it. acetrdance with the requirenents ot GB/T 1. 1 1993\Dircetives to:the work o: standa:diaa:on Lni: l:ldraiing and presentation of srandardsPrr l,eneral :ulea fo:rafting stendard:\yad SN/T Oul—Isus\Gisacrel rules fcr drafting thu atendurd ms-hod: for the de-1err'im f nexlirilr, ve'etinary al-ug fes'ues mml lio'uxins in rwmaditirs fny exugrt\. the,rethnd nf determiration af this standa:d was drsfted by relerriax -o relevan: donestic aud freign lit-erature thruugh research.mudilicatior atd veriticainn. In iddtior.me:huds o: samplre znd sampleFreparatiun are alse ypcrified ir rhig standard.The liil of d-+tirimd'stay i el-li-rel ins thik ':uletl o thr lss f th turtrut intetriiu.]maxinllm Jirits Eor vir.cloanlir. resicues ir. cereale and aii seeds and rine sensiivity af tle mettn?Annex A nt this stardarc is ar. igfarmative znnex.Thig srandard was proposed by arc ig under the charge oi the State Adninisartion ol lnport andExport Eouirodity lrs[uetin o: the Peuple's Republu uf China.This 3'alul:l was diadirl hy Jilir: Jmprl Fnl Fxjrt Crnmmodity Gusprricn Bure.i af heFeople's Republic ot Chinz.
The na:n drafrers nf this standard are Kong Hui, Wang Mingtal,Mu Jun,Li ChingcaiThis stanoard is grufcssional stutudard promulgurei for the first timc.Nnre:''tia Eng ish wetsin tonng nthn frnm the Chinrap tr x',is sn'rly fit guentarProfcssionatStandard of thePeopile'sRepublic of Chinafor Import and Export Commodity Inspection5841996
Method for the determination of vinclozulinresidues in cereals and oil secds for cxport1Seupc
Jhis alandard spaciies the Tretlind of anpling aaraple prcperetian and dcrerminetia of vineloznlin reaidurs by gas chrurautogrepty in eereals arul wil seeds for uxiurt.This stutdarl is appi.illr o ih+ iletrrinit- :[ vierllir. rexilurh on'eni in anprliehed rire.maize,soyahesa and pearu for exmrt.2Sumpling wnd sample preparallon2-1Inspcctian lot
Eugh insprrlikin 2.2.1 Cargn in ba5
Caleuate the umser of bage to be taken by formulat!)a=VN
Nzotal numbur of bugy it. n lur;a—mumher uf ligx k: Ip :kruNote, value a is with de.imal-rcund ol: tise decime! pell,wlicb ia edded ss un.tv to tlht integral part of .!2.2.2 Cargn in hulktraaizx ar 5oyahean ?The height cl the cargo pile should not exceed 2 m. Sel up areas arr spots for zamping o the pilesurface. 5o m'is cora!cered ax en srea,in which 5 apata shall be fixec,one ir the centre ari tou: sfcur corrcrstj u from the murginufthe crru.Fur att udeitiwnel srco.thrcrmore sempiing spoes shalbr [ixed.
2.3Sanpling tao.s
Approved by the State Administratlon ofImpartand KxpurtCommadityInspeclian afEhe Peuple's Kepublic uf China un Nuv. 15.199EImplewented from May1.1997
S05841996
2. 3. 1 M+t:illi. ars:al+t, l.eug hturlml:ny humll-j. a m. dianeter: 1. s2. u cmi faove length.nrygcr than hele tte diaper.al icngth ot the bag.2- 3.2 Metallie douale-casiag aamplar,l.ength 1 m,2 m :hoth includin tundle with suru: slu.s urd:fferrat seetinns uad respeetively a: tht saru heigln- fu- hu. it uer -nd 2. 3- 5Seple trnainer:Cau ur lg+whie f i l riler.2. 3. 6 C.mhtor n.ha: ruitable mareral)shcer:For san.ple dividingtcuarterirg)2. 4Saraplirg Procedure
2. 4.1 For cargo in bars
2.4. 1. 1 Suupliug by ernpiyiug rml, T':uw 10 peruent nf ile ntinmbn: f bag5 specificd in 2. 2. 1(nu-iens tha: baas)at any part af ae pile at random, L'nsearr. and open the bagiad lay i on a cleen c.oth:heet(or uther clear sheet),Grasp lighi (wo aornerx cf :he hag horton ard raise uy to an urgl- of 4b'.tug backwarc. Ir ca : m unci. all ennient of the beg is emptied uur, Cheuk whetur ile yaalily u: giuul.is unifen witbin and urtween ilit laz- Afir: cmdirui:g ihr grls a- ir rnrxal rrrcition,ecoop upihr kinple Erom different Farls of the out-poured cantent at rar.com,aad gromptly place : a samplecantainer,The quautity of the zample dtawn from each hag shou'd be barinally -n- samc.2.4.1.2Sampling iram inside tae bag%,Druw thu uaplusfruru ttu nanilut t,f bags ,rrifial in 2.2Itby dcducting the nuraber uf bugw tleawn in 2. 4. I. >n In'lrwa,Alrrg lhr nne wave af rine pile.drawih+ sanples finn t'se haps ni the upper,nidd.c aad .nwe pzr-s around thc pile at zandom. Fur unpoi-ished rice.maize zuyavear: or peanul procser: as fellows:For unpelighed rice -insert the aetllie seup.cr(2. 3, t), w:th ile groovu [aeing dowuwurd.-li: gt.relly intu ench beg.ttun :aru the aampler 13),r:r: w am il+ imp'er nl p-ump.y paut the s+mple in a rrtainel.
For maize or syabtan.instr: the ineti:Jle deuble-casaig samper(2. 3, 2.lengtk 1 ni(the sl:tssaauld he cleaed whle insertung -ndisgonally :nte caeh baz. Tum the inacr casiaa to oucr the slols suthat the sumplu may fill up - inrpr n:le. agai- irr ilit irtr 1ssing I: :lkise llir slels and draw natthe sanzler. Fromptly pour thc sample inta a sample containe:.Fer peanut-pariially unseam(3 5 sri:cheajrke ba mcuth,seoop ojt the ganple from cack beg(with a udi:n: ihe bng openink. Promptly closr -he b.g by stnming,and [eur tht stmrle intu u sam)ple turt:.irrr.
Th :m.ilri nf sarple draon frnn. zach hag shauld be basizally the 5ame as i- 2, 4. 1. 1. The tata.weigh: oi tae saple u: each Jet saould be not less than 4 kg-2.4 ?Sampl:ng from the rergo in buikInser1 the. (leuule casing Nun:ple-t2. 3. 2)xu:rhn +rly inti 1br ailr :1 li+ spk1x x[rifiel in 2. 2. 2Ll app:cpria:e depth at 1s(the slrs should be closed waile inscrticg in>. Tum the jucer casing tuopen the slots so that the aample may f:ll up inner tuha. Agair.1urn the inner caaing To close the sliataRnd draw our the gampler. Promptly pour the sumple inro a sarmpl: err.taincr. The amoun: of sumj:ldrnwn frur all the spulx sha'l hr lasinaliy ile samt.Tne toral weight af the :ep:erentaive samp.c af eaca Int xhould be not less than kg.2. 4.3Reducion ot gross sanpleSN 054—1996
Fnr cargo in Dage:Pour all the zamples(from beth 2. 4, 2. 1 and 2, 4. 1. 2)on a clean sheet. ReduceTo nor lesas rhar: 2 kg by quartering with a plete. Plce in u sumple ivtuiter,seul.label and erad io th.Iesoratary intimr.
Far inrgri in br:lk :Pru all he drawrs saupie anto a clean eheer and procerd as Ear rargo in bagstiescribed above.
2.5 Preparatiun of test sample2. 5. 1Tolg
2- 5- 1. 1 Grinder.
2. 5. t.2Pulv-icer.
2. 5. T. 3 Sievz:20-resh sicve.2, mm :ound-hole seive.2 5. 1.4 Plate Ior yuerering.2.5.1.5Sanple cenrainer,Wide mouth bortlewiuh ground stupper,2- 5- 2Prued:ire
2. 5. 2. 1 Frr unpalisnad rice.nmaize nr sayabean; Reduce hy quarterir.g tp ca 1 kg. Grind with agrinder (2. 5. 1. 1)ta let all pass th:ougt. u 20-mesh sieve. Mix thoroughly and divide in1o 1wo equa)por-:ons.plzce in clean zample containers as the tesr aample.seal and lahel.2. 5. 2. 2 For pcBnur Reduee by quartcring te ca 5u gipulveriz with pulverizerl2, 5. 1. 2to et alpess thruugh a 2, inot round E:ck- sirvr, M x iharonglly ianri :livile in:in two riual portions as 1he teg[Niinples. Pli+ in rlean cnatainers.seal and Label.2.6 Storage of test sample
The legl aemplea ahou.d he arored belnw -: Cand kep:avway iram lighe.Nste: lt the uurse if ecupu.g ai sauple paepajatiun.piauton u at te 1gken lo eroid conauineton o? anyfaictuts whn h lay taue- Lale cl:urge e[ resille uelleel.3Meihcd af deterinatinn
3.1 Princjple
Th:r vinu-lixsl n resirlues in ile 1es1 eample are axtracted with petroleum ethe:. The extract is pa-citinned wich acctonitrile ar.c clcaned ay by passing thruugh a silica gel column. The pesticice is thetdsrivuged iih chleroacstui rhleride. Ierenunarinn 1g de by eaes of a gag chronarorreph cquipged w:th clcrton eapture detector,us:ng exiernal starcard inethud.3. 2Ragunt+ ari ma -rl.
T.nierx nhe:wise spec:fied,the reagzns sh.iuld he analytically pure.3.2. 1Pe-ruleum ethe::Red:stillel,3.2.2 Acetorilrale.Keiiariled.3. 7. 3Acetore.
3- 2. 4Ch.orwttyl .llhilr :licm:2n?(v?.nir.r! 2 eaf. nf :-h:etr.e+h-il+lisn. ve ia St
ml., of peralr jm rllrt and ir.ax iharugh.y.snre cl.larnaceryl rhlrride: salminn in a freezer.co r:ot xFose ta light.
3. 2. 5Ankyc rolls andium sulfareIga1lc at Hs3 C tor 4 a,and scep l a tghtly ciogcd centaine.3. 2. 6 Silicl gul ;Fur chroruulogrnphiu usu.rt2p) incet .brforu usu-arl al 12uc: [ur 3 hiikl keelin + tighily +l.--l :ou :inp.3.2, 7Vinelnarlin staadard,Fu:ityeyu%.3.2.8Viacluzolia standard zolution: Accurately weign an adeyuzle amount of vinclotolin stsndard,S 05841996
dlisenive in a sraali volutue uf prtrubeum ether. Didute with petruluuam ethet co form a standard stock solution of 0, loo mg/mL, in cancentraticn. Then dilute the etandard scrck nlutiau with petroleum erherto the rquircd concentration ag the standard working solutson.3.34pparatus und cquipmcnt
3. 3, 1 Gas chramatagraph et:uipEed wi:h elecirrm capiurr retetior.3.3-2 Shaker.
3.3.3 Ratary evapararor.
3. 3. 4 'urisur: tempereture wuter beth.3. 3- 5 Til:raanni: gereratoe.3.3.6 (lass cleanup.column:25 cm X 1.5 cm(id),add in epuence 2 em(heigh:)sf anhyrlrous soliumsulfate.J5 g ni silica gel.2 cm(height Jof arhydrous zodium zullate. Rinse the celumn rith 50 mL afpetru.euin ether 5eforr use.3. 3. 7 Miern-sysinge:l pel..3.4IP'racedure
3.4.1Extraction
Wecigh ca 2u g(aacurate rs c. - gJo: rhe les: sample into a 25C m. conical Elask with stoppe:-add5n mE uf priruieun ther.uxeruct for 30 min on u shakcr. Filter the Exirset into a 25C ml. separator.Rinse the residue twice with 30 mi.t.n 1nial,)isf petrolu -ibpr,fi'ter unel uoinbitu tb:e washings in thgseparator
3 4.2 Cleanup
Adll 5( nl uf aceturuirile inu the sapt.rutur.saake for 1 mir.,set aaide for 1o mir. Collecr :heJnwer acetonitrile laya:. The petroleum eihrr phn+ in +wiri.ctrd witt: 2 × Sul mL ut ececun:trilc. Combine the acetonitrile phases in = pear shaged bnstle and evaporete i: :early in tirynrxs in :t witrr-lwillbelove 43 C with the rotary evaporator, I'ben disso,ve the residue by sl-rasonic wave three times withI5 mL af pctroicum cther in total.Transfer cach me rhe solunan :nro ihe glass cleanug-solumn.\herwash Ie riurrn winl lo me, Ppir,leu-n :he: urld diseard the efflueat. Eluze with 1cs ml. of ecetone-petrcleum e:he: (5+9s)mixed salatinn .rllee: rbe eluale in a Frar--hii biile ur:tl v iurult tu lrynezs ic a water-bath belcw40 t:witha rotaryevaporator,3.4.3Lxrivatization
[vissrlve 1he rexidne hy iliruskinin: wive wiil. 2(i nt uf putroleum ether,chc add (o. 5 ml. ofchloroaretyl elaride solutian,strpper wica a cap,the an.n- sn in lurl .uxiale ai rugrn temperuture for32 mia kept uway Irom light with occasional saaking Afte: :he rcactinn is nver,evapnrale il ir drynessin e watcr brth bela 4uC wita a rtery vaporeior. add 5o ml of petroleum ether tr dissnlve the-nsilutnil tljuratu egain tu dryness in u wuter beth belew 4u C with rorary evaporatar.Add ex-ae.y Io, t: nl. of pesinlenm rilrr io dishrdve lle rrxielnr,slit solutiur: is rtudy for Gc dererminatinn.3. 4.4['n:ivatizatio of the erander?Accuzaiely Pipe:lo.O mL of vinclozolin aiandard working solution of suitable concei:tralinr in:rilubu ich sro2percvaporare to dryncga by blrwirg wi-h a gtrcam nf nitroge:Proceed as in zectioni d, Far lerivalicalirm.lhe derivrilixpil nlanrlurl wrking uslmi,r in uged fur Gc determinetion.3 4. 5Detem.inazion
3. 4. 5. 1 Gc operauirg conditior.a)Chrsmetngraphic enlumrrf-laag.3 m× 3.2 mm(id;.packed wi:h :o%(m/ari5E-30 pr. Chro-urbwAWDMCS(a-1o0mcsh);
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