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粗纤维测定仪厂家使用说明书

CXC-06型粗纤维测定仪使用说明书武汉格莱莫检测设备有限公司CXC-06型粗纤维测定仪操作手册CXC-06型粗纤维测定仪是武汉格莱莫检测设备有公司研发、生产的,采用化学与物理相结合完成粗纤维测定分析的成套仪器,适用于粮食、饲料及其他农副产品对粗纤维含量的测定。

由于仪器仍依酸碱洗涤法进行设计,集酸碱处理及冲洗于一体,采用了全封闭的结构形式,用电热直接加温的方法,同时可以做6个样品,操作时样品不需转移,能将物质中的粗纤维分解出来,同时又可根据所需温度单个任意调节,从而达到了准确、快速的目的。

在操作过程中,又有定时控制,无有害物质外溢,因而在整个测试过程中既保证了测试数据的可靠性和准确性,又有益于周围环境的净化,方便了操作人员。

测试结果都符合GB/T5515、GB/T6434的规定。

因此本仪器是各粮食、饲料等行业及科研单位用于测定粗纤维含量的理想设备,是大专院校用作实验的理想仪器。

一、工作原理用固定的酸和碱,在特定的条件下消煮样品,再用乙醚、乙醇,除去醚溶物,经高温灼烧和扣除矿物质的量,剩余量称粗纤维,它不是一个确切的化学实体,只是在公认强制规定的条件下,测出的概略成分,其中以纤维为主,还有少量的半纤维素和木质素。

二、技术指标:1、测定范围:各种食品、饲料及其他农副产品中的粗纤维含量2、测定精度:≤0.2%3、重现性:平行实验结果符合GB/T5515、GB/T6434规定4、测定时间:在仪器上约90min/批5、同时测试样品数:6个/批6、电源:220V50Hz7、额定功率:3.3KVA三、使用说明:1、化验室具备条件:(1)粗纤维测定仪及用具(2)分析天平:感量0.0001g(3)电热干燥箱:(1500W、50-150℃)1台(4)备有变色硅胶干燥瓶2只(5)马福炉1台(6)实验室用粉碎机(7)分样筛:孔径0.45mm2(40目)2、试剂:(1)硫酸:分析纯(2)氢氧化钠:分析纯(3)95%乙醇:分析纯(4)乙醚:A、R级(5)正辛醇:分析纯(消泡剂)(6)石芯试纸(酸、碱)各一份3、操作前的准备:(1)试剂准备:●硫酸溶液(0.128mol/L):取浓硫酸(分析纯)约75ml,用蒸馏水稀释到1000ml,用已知浓度的NaOH液标定后,调整其浓度到1.28±0.005mol/L的硫酸原液,用前用蒸馏水稀释10倍即可。

●碱溶液(0.312mol/L):取饱和NaOH溶液(680g/L)190ml,用不含CO2蒸馏水稀释成500ml加塞振荡均匀,用已知浓度的酸标准液标定后调整其浓度到3.12±0.005mol/L的碱原液,用前用蒸馏水稀释10倍即可。

(2)样品制备:●取有代表性的样品,捡去杂质,按四分法取25g左右。

●将样品放置在60-65℃烘箱内干燥,冷却后粉碎或研磨,全部通过0.84mm2(20目)筛子,其中大于0.42mm2(40目)的不得小于50%,小于0.25mm2(60目)的不得大于10%。

●样品中的脂肪含量超过10%则需要脱脂,(可用测定残渣分析、操作过程按GB/T2906-82进行)。

●将坩埚用开水洗干净,洗至坩埚内不留任何杂质,置于干燥箱内烘1小时左右(温度在105℃)移入干燥器内冷却至室温,编号,再置于干燥器内备用。

4、操作步骤:(1)在已编号的坩埚内准确的称取干净的平均试样或烘干无水的脱脂样品1-3g(谷物2-3g)准确至0.0001g。

(2)接通电源、水源、开启主机电源开关(自来水尽量开足保证冷凝)。

(3)打开酸、碱、蒸馏水预热瓶上盖,分别加入已制备的酸、碱溶液及蒸馏水,加至预热瓶的90%,盖上冷凝球。

(4)开启酸、碱、蒸馏水预热电源开关,调节预热电压旋钮,将其调到顺时针最大(这时左边电压表显示电压为220V左右),等酸、碱、蒸馏水沸腾时,将预热电压调小至酸、碱、蒸馏水微沸。

(5)将装有试样的坩埚移入仪器抽滤位置中,压下手柄并锁紧,将下阀全部关闭。

(6)把酸瓶橡胶管上白色小管插入1号消煮管中,打开加酸瓶橡胶管上夹子在消煮管中加入已沸的酸液200ml(约到消煮管中间刻度线),然后依次在2、3、4、5、6号管中分别加入同样的酸液后夹住加酸橡胶管,再在每个消煮管内加3-4滴正辛醇。

关闭酸预热开关,将推拉手柄提起一点后拉手柄,使加热管盒碰到向前靠近坩埚,然后打开消煮的加热开关。

将挡热板挂在加热盒前面,将消煮管调压旋钮调至最大,此时右边电压表显示220V左右,待消煮管内酸液再次微沸后再将电压调至150-170V左右,使酸液保持微沸状态,向上打开消煮定时开关,保持酸微沸30分钟。

30分钟消煮时间到,则蜂鸣器报警同时自动切断消煮器加热电源。

(7)将消煮加热开关关闭,将挡热板在加热盒前面取下,再将推拉手柄推到底使加热盒离开坩埚后停止加热,将消煮调压旋钮逆时针旋到底,打开1-6号抽滤开关(分别打开,单独进行抽滤),先打开红球抽滤开关,再打开抽滤泵开关将酸液抽掉。

抽滤完毕后,先关闭抽滤泵开关,再关闭抽滤开关。

把蒸馏水瓶橡胶管上白色小管插入1号消煮管中,打开蒸馏水瓶橡胶管上夹子,消煮管中加入蒸馏水后再抽干,连续2-3次。

依此方法把6个消煮管都清洗完毕,然后夹住加蒸馏水橡胶管。

再抽滤过程中如发现坩埚堵塞时,可关闭抽滤泵,先开启反冲红球开关,再打开反冲泵开关用气流反吹,直至出现气泡后关闭反冲泵,关闭反冲红球开关,打开抽滤泵继续抽滤。

洗涤完毕后关闭所有抽滤开关及泵开关。

(8)把碱瓶橡胶管上白色小管插入1号消煮管中,打开加减瓶橡胶管上夹子在1-6号消煮管中分别加入微沸的碱溶液200ml后夹住加碱橡胶管,再在每个消煮管中加入3-4滴正辛醇后重复第6条后半部分和第7条的操作,进行碱消煮、抽滤、洗涤。

(9)以上工作完成后,用吸管分别在消煮管上口加入25ml左右95%乙醇,浸泡十几分钟后抽滤掉。

(10)左手压下手柄拉出锁钩子缓缓上升,使其复位,带好手套,取出存有试样的坩埚,待乙醚和乙醇全部挥发完,再移入干燥箱内在130℃温度下,烘2小时,取出置于干燥器冷却至室温称重(A1)。

(11)将称重后的坩埚,置于500℃马福炉内灼烧30min,待炉温降至200℃以下,从马福炉内取出置于干燥器内冷却至室温后称重(A2)。

(12)测定结果计算:粗纤维%=(A1-A2)÷S1×100式中:CF-----粗纤维百分含量(%)A1------坩埚+粗纤维+残渣及灰分质量(g)A2------坩埚+残渣及灰分质量(g)S1-------试样质量(g)四、注意事项:1、仪器由于经常与酸、碱及水接触,且仪器通有220V交流电,故实验室插座一定要有良好的接地。

2、每次用完仪器后,应用滤纸将抽滤座内的水吸干。

3、当坩埚在500℃的马福炉内灼烧1小时后,不要立即将坩埚取出,否则由于温差太大极易造成坩埚炸裂或影响坩埚使用寿命。

4、在清洗坩埚时,应将坩埚放入30-50%左右浓度的盐酸溶液中浸泡几个小时,然后取出用水清洗后烘干,以备下一次使用。

5、本仪器保修1年。

在一年内如因用户使用不当而造成仪器损坏,本公司保证给与修理,但需视情况酌情收费。

英文版CXC-06Crude Fiber Tester is developed and manufactured by Gramo Testing Equipment Co.,Ltd.in Wuhan.It is a complete set of instruments for crude fibre determination and analysis by combining chemistry with physics.It is suitable for the determination of crude fibre content in grain,feed and other agricultural and sideline products.Because the instrument is still designed by acid-alkali washing method,which integrates acid-alkali treatment and washing,adopts a fully enclosed structure, and can be heated directly by electric heating.At the same time,it can make six samples without transferring.It can decompose the crude fibers in the material and adjust them individually and arbitrarily according to the required temperature,thus achieving the purpose of accuracy and rapidity.In the process of operation,there is regular control and no harmful substance spillover,so the reliability and accuracy of the test data are guaranteed in the whole test process,and it is beneficial to the purification of the surrounding environment, and it is convenient for operators.The test results are in accordance with the requirements of GB/T5515and GB/T6434.Therefore,this instrument is the ideal equipment for measuring the content of crude fibre in grain,feed and other industries and scientific research institutes.It is also an ideal instrument for experiment in Colleges and universities.I.Working PrincipleIt is not an exact chemical entity.It is only a general component determined under the generally accepted mandatory conditions,in which fibers are the main component,and a small amount of hemicellulose and lignin are also found. II.Technical Indicators:1.Scope of determination:crude fibre content in various foodstuffs,feedstuffs and other agricultural and sideline products2.Measurement accuracy:<0.2%3.Reproducibility:Parallel experimental results conform to GB/T5515and GB/T64344.Measuring time:about90minutes per batch on the instrument5.Number of simultaneous test samples:6batches6.Power supply:220V50Hz7.Rated power:3.3KVA3.Instructions for use:boratory qualifications:(1)Crude Fiber Tester and Appliances(2)Analytical balance:Sensitivity0.0001g(3)Electrothermal drying box:(1500W,50-150C)1set(4)2discolored silica gel drying bottles(5)1Mafu stove(6)Laboratory crusher(7)Sample screening:pore size0.45mm2(40meshes)2.Reagents:(1)Sulfuric acid:analytical purity(2)Sodium hydroxide:analytical purity(3)95%ethanol:analytical purity(4)Ether:A,R(5)n-octanol:analytical purity(defoamer)(6)One stone core test paper(acid and alkali)3.Preparations before operation:(1)Reagent preparation:Sulfuric acid solution(0.128mol/L):take concentrated sulfuric acid (analytical purity)about75ml,dilute it to1000ml with distilled water, calibrate it with NaOH solution of known concentration,adjust its concentration to1.28+0.005mol/L sulfuric acid solution,dilute it10times with distilled water before use.Alkali solution(0.312mol/L):190ml of saturated NaOH solution(680g/L)was diluted into500ml of distilled water without CO2and oscillated evenly.After calibration with known concentration of acid standard solution,the concentration of alkali solution was adjusted to3.12(+0.005mol/L)and diluted 10times with distilled water before use.(2)Sample preparation:Take representative samples,pick up impurities,take about25g according to the quartile method.The samples were dried in an oven at60-65C,crushed or ground after cooling. All the samples passed through0.84mm2(20mesh)sieves.The sieves larger than 0.42mm2(40mesh)should not be less than50%,and those less than0.25mm2 (60mesh)should not be more than10%.If the fat content in the sample is more than10%,degreasing is necessary.(The residue can be determined and analyzed according to GB/T2906-82).The crucible is washed with boiling water and no impurities are left in the crucible.The crucible is dried in a drying box for about1hour(at105C)and cooled to room temperature.The crucible is numbered and stored in the dryer for reserve.4.Operation steps:(1)In the numbered crucible,1-3g(grain2-3g)of clean average sample or dry degreased sample is accurately weighed to0.0001g.(2)Turn on the power supply,water source and switch on the mainframe power supply(tap water should be fully turned on to ensure condensation).(3)Open the cap of the preheating bottle of acid,alkali and distilled water, add the prepared acid,alkali solution and distilled water to90%of the preheating bottle,and cover the condensation ball.(4)Turn on the switch of acid,alkali and distilled water preheating power supply,adjust the knob of preheating voltage,and adjust it to the maximum clockwise(when the left voltmeter shows a voltage of about220V).When the acid,alkali and distilled water boil,the preheating voltage will be reduced to the slight boiling of acid,alkali and distilled water.(5)Transfer the crucible with the sample into the filter position of the instrument,press down the handle and lock,and close all the lower valves.(6)Insert the white tubule on the rubber tube of the acid bottle into the No. 1cooking pipe,open the clamp on the rubber tube of the acid bottle and add 200ml of boiled acid liquid(about the middle scale line of the cooking pipe), then add the same acid liquid into the No.2,3,4,5and6tubes respectively, then clamp the acid rubber tube and add3-4drops of n-octanol to each cooking pipe.Turn off the acid preheating switch,lift the push-pull handle a little and pull the handle back,so that the heating tube box touches the crucible forward,and then turn on the cooking heating switch.Hang the heat shield in front of the heating box and adjust the pressure regulating knob of the cooking tube to the maximum.At this time,the right voltmeter shows about220V.After the acid in the cooking tube is boiled again,the voltage is adjusted to150-170V to keep the acid in a slight boiling state.Open the time switch of the cooking upward and keep the acid in a slight boiling state for30minutes.When the cooking time reaches30minutes,the buzzer alarms and automatically cuts offthe heating power of the digester. (7)Turn off the cooking heating switch。

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