羊毛物理分析测试.doc

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1、Analysis and Physical Testing Methods of Wool forContinuous Chlorination Processes对连续氯化处理的羊毛进行的物理实验分析方法- CONDITIONS OF ISSUE 刊物条款All information, recommendations and suggestions appearing in this document are based on tests and data believed to be reliable. However, no guarantee, either expressed or

2、 implied, is made by CMT-Hicorp as to the results obtained nor can CMT-Hicorp accept any liability arising directly or indirectly from the use of information contained herein.本文件中出现的所有信息和建议都是经过实验和可信数据得出的,值得信赖. 不过, 赛特环球不对结果做任何保证,也不会承担因信息的使用所产生的直接或间接责任, 也不会信任此处所含的建议.Further, the information contained

3、herein should not be contrued as being complete, since additional information may be necessary or desirable when particular or exceptional circumstances exist. Nothing contained herein shall be contrued as conferring rights under, or recommending the infringement of, any patent.此处的信息解释并不完整, 因为有时会发生异

4、常情况,这时会缺少相关信息. 任何从赛特环球得到的建议仅作参考,并不能作为处理问题的教程. 此处所作解释未经授权, 也未违反相关专利.NOTE Where figures are given as examples, experience values or recommendations, it is important that they are considered with due regard to the test method used, as and where applicable, to obtain them. Direct comparisons should not

5、be made unless results are obtained using the same test method.给出的例子, 经验数值以及建议,都是经过实验得出的, 如果适用, 请采纳之. 例如, 测试含油量时与机器紧密相关, 相关执行方法和解决方法值得借鉴. 不要直接比较, 除非使用同样的试验方法并得到同样的测试结果. THE USE OF PROPRIETARY NAMESThe fact that chemicals and other products with proprietary names may be mentioned in this publication

6、does not imply that substitutes of equal value or better value are not obtainable. 本刊物中含有专有名称的化学制品及其他产品, 并不意味着不可使用相同价值或更高价值的替代物CONTENTS目录 1. pH Determination of Wool using Test Method IWTO-2 使用IWTO-2测试方法对羊毛pH值进行测定2.Determination of Oil and Fat Content of Wool 对羊毛油脂含量进行测定 2.1The WIRA Rapid Oil Extrta

7、ction Test WIRA快速抽油测试2.2 Soxhlet Extraction Using Test Method IWTO-10 使用IWTO-10方法进行的索氏抽取3.Determination of Regain of Treated Wool using TestMethod IWTO-34 使用IWTO-34方法对处理过的羊毛进行回潮率测定4. Determination of Sliver Weight 毛条重量测定5.Determination of Degree of Felting of Treated Wool Tops using the Kroy Felting

8、 Tester 使用Kroy制毯装置对处理过的羊毛进行毯制等级测定1. pH Determination of Wool using Test Method IWTO-2使用IWTO-2测试方法对羊毛pH值进行测定The pH value of wool can be determined by measuring the pH of a water extract of a sample of wool.可以通过对从羊毛样品中抽取的液体进行pH值测定, 此值即为羊毛的pH值.Reagents 助剂Distilled water 蒸馏水Buffer solutions 缓冲液Apparatus

9、 器具150 ml Glass-stoppered flask 150毫升玻璃磨口烧瓶Mechanical shaker 机械摇动器pH meter 酸碱计150 ml Beakers 150毫升烧杯Analyticalbalance 分析天平Method 方法(a) Three samples ( 2 g each ) of the wool tops are cut into 1 cm lengths. 将三份羊毛样品(每份2克)切成1厘米. (b) Put each into a stoppered glass flask with 100 ml distilled water and

10、mechanically shake for 1 hour. 放入盛有100毫升蒸馏水的烧瓶中, 机械摇动一小时. (c) Measure the pH value of the aq ueous extract using a pH meter fitted with a suitable electrode system and determine the mean value. 使用酸碱计(装有电极系统)测定水提物的pH值, 确定平均值. (d) The pH probe should be standardised on a daily basis using freshly-made

11、 buffer solutions. pH值探针必须每天用新鲜的缓冲液冲洗, 使其标准. 2.Determination of Oil and Fat Content of Wool 羊毛中油脂含量的测定2.1 The WIRA Rapid Oil Extraction Test WIRA快速抽油测定法This rapid method enables a result to be obtained in 10 min. to 15 min. and is intended primarily for control of processing.这种方法可以在10-15分钟内得出结果, 主要使

12、用于加工控制.Reagents 助剂Dichloromethane ( methylene chloride ) 二氯甲烷Apparatus 器具Cotton wool 棉绒Analytical balance 可分析天平Extraction apparatus, consisting of : 提取装置由以下组成:(a) a metal tube with a capillary end, 一根末端细窄的金属管(b) a metal plunger and weight-piece (1 kg), 一个金属活塞和承重片(一千克)(c) an electrically heated, temp

13、erature-controlled hot-plate, 一个电热的,温度可调的加热盘(d) an aluminium foil tray, 一个铝箔托盘(e) two aluminium tray supporting rings.两个铝托盘, 有弹簧支撑.The assembled apparatus is illustrated in Fig. 1. 示意图如下 Fig. 1Method 方法(a) Weigh a clean tray (W1) and assemble onto hot plate with ring weight. 对托盘称重(W1), 用弹簧将其安装到加热盘上.

14、(b) Place a small plug of cotton wool in the tip of the metal tube. 用一小块棉绒塞住金属管嘴. (c) Push 2 g of wool into tube and fit to tester. 将2克的羊毛推入管子, 放入测试机. (d) Assemble push rod, collar and weight and push into tube. 安装好推杆, 轴环以及称重, 推入管子. (e) Add 10 ml dichloromethane into tube, collecting the extract on

15、the heated aluminium tray. 往管子内加入10毫升的二氯甲烷, 将提取液收集到加热的铝托盘上. (f) When dichloromethane ceases to flow, press weigh piece and plunger to remove further extract from the wool. 当二氯甲烷停止流动, 按压承重片和活塞, 清除羊毛上的多余抽液.(g) Allow the solvent to evaporate, remove the tray, cool for 1 min and weigh (W2). 让溶剂蒸发, 移开托盘,

16、 冷却1分钟,然后称重(W2)(h) Dismantle tube etc., remove wool from tube with a wire hook. 拆除管子等, 用钩子将羊毛从管中取出. Calculation 计算 ( W2 - W1 ) x 100 = oil & fat content ( % ) Wt of wool sample(羊毛重) 油脂含量Check on dichloromethane 检查二氯甲烷Weigh an aluminium tray before and after drying out a tray full of dichloromethane

17、with no wool. The weight of the tray should not have changed. 在烘干盛有二氯甲烷但未放羊毛的的托盘之前和之后, 对铝盘称重. 铝盘重量不能改变. 2.2Soxhlet Extraction Using Test Method IWTO-10 索氏抽取法Reagents 试剂Dichloromethane ( methylene chloride ) 二氯甲烷Apparatus 器具Soxhlet extractor : 索氏提取器Assembled with ground glass joints and protected aga

18、inst the entry of moisture by means of a tube containing a drying substance. The extractor of the Soxhlet shall have a capacity of about 200 ml to 300 ml and the flask 250 ml.该器具装有毛玻璃, 管子里有烘干装置, 以防湿气进入. 索氏提取器容量应当在200-300毫升之间, 烧杯250毫升. Dessicator 干燥器Drying oven 干燥炉100 ml conical flasks 100毫升锥形烧杯Funne

19、l 漏斗Distillation unit 蒸馏装置Fat-free filter papers 无脂过滤纸Analytical balance 分析天平Method 方法(a) Weigh two test samples of 20 + 0.05 g. 称取两份测试样品, 每份20 + 0.05 g克. (b) Place a circle of filter paper slightly greater in diameter than that of the Soxhlet barrel so as to cover completely the exit of the siphon

20、tube. 用过滤纸卷一个圈, 直径稍微大于索氏筒的, 这样可以完全盖住虹吸管的出口(c) Pack a small portion of sample tightly at the bottom of the barrel, then introduce the rest in such a way that the wool is below the level of the bend of the siphon. 在筒的底部用用一小部分样品紧紧塞住, 采用同种方法将剩余的放在低于虹吸管弯曲的位置. (d) Assemble the extraction apparatus and pla

21、ce it on the preheated water bath. 装上提取器, 将其置于预先加热的水槽上面. (e) Pour in through the condenser sufficient dichloromethane to cause a first siphoning. 通过冷却器注入大量二氯甲烷, 产生第一次虹吸作用. (f)Adjust the heating so that 20 - 24 siphonings occur within the extraction time of four hours. 调整温度, 使它在四小时的抽取时间内进行20-24次虹吸作用.

22、 (g) Filter the contents of the extraction flask through filter paper into a tared, preheated 100 ml conical flask. 通过滤纸往一配衡的预先加热的100毫升锥形烧瓶里滴入抽取瓶里的液体. (h) Wash the extraction flask and filter with dichloromethane until they are free from fatty matter. 清洗抽取瓶, 滴入二氯甲烷直到无油脂. (i) When the distillation of

23、 dichloromethane is completed, detach the flask and heat on the water bath for a further 5 minutes. 当二氯甲烷完全蒸馏, 将烧瓶与热水槽分开5分钟. (j) Heat the conical flask for 30 minutes in a drying oven. 在干燥炉里将锥形烧瓶加热30分钟. (k) Remove the vapour from the flask and heat for a further 5 minutes. 去除烧瓶里的蒸汽, 继续加热5分钟. (l) Put

24、 in a desiccator and weigh afterwards, thus obtaining the weight of the dichloromethane soluble extract (e). 接着放入干燥器和量重器里, 得到二氯甲烷溶解抽取物的重量(e). Calculation 计算The total oil & fat content can be expressed either :油脂含量表示如下:(a) as a percentage of the conditioned weight of the de-greased sample 样品油脂公量百分比:e

25、 x 100 = total oil & fat content ( % ) 20 - e 油脂含量(%)or (b) as a percentage of the dry weight of the de-greased sample或者, 样品油脂干量百分比e x 100 = total oil & fat content ( % ) w 油脂含量百分比(%)e is the weight of the dichloromethane soluble extract. e 表示二氯甲烷溶解抽取物的重量w is the dry weight of the extracted test sam

26、ple. w 表示抽取测试过的样品的干量 Normally, equation (b) is used in the processing plant. 通常, (b)方程式应用于炼油厂里. The relationship between the Soxhlet result and the WIRA rapid result is that theSoxhlet will always produce a result about 2 to 3 times higher than that of the rapid result. Although Soxhlet testing requ

27、ires more time, it is clearly much more accurate.索氏法得到的结果是WIRA法得到结果的2-3倍. , 虽然索氏法费时较多, 但其结果相对准确. Warning: Tests using dichloromethane should be carried out with adequate ventilation, preferably in a fume-extraction cupboard or under an extraction hood. The solvent should not be allowed to come into

28、contact with skin or eyes. Use goggles and rubber gloves where possible and avoid inhaling fumes of the solvent. 警告: 当执行使用二氯甲烷的试验时, 应保证通风良好, 最好使用臭气抽取柜或者在排气罩下进行. 助剂不要接触皮肤或进入眼睛. 必要时使用护目镜或橡胶手套, 避免吸入助剂臭气. 3.Determination of Regain of Treated Wool using Test Method IWTO-34 使用IWTO-34对加工过的羊毛进行回潮率测定The WIRA

29、 rapid drying unit is used to determine the moisture regain of treated wool. WIRA快速烘干装置用来测定羊毛的回潮率. Apparatus 器具WIRA rapid drying unit WIRA快速烘干装置Analytical balance 分析天平Method 方法(a) Weigh can with lid (W1). 称重带盖的罐子(W1)(b) Weigh can and lid with approximately 200 g of wool sample (W2). 称重带盖的罐子和大约200克的羊

30、毛样品(W2)(c) Dry at 105C + 3C for 10 - 15 minutes. 在温度105C + 3C下烘干10-15分钟. (d) Weigh can with sample together with lid. 称重带盖的罐子和羊毛样品(e) Dry for another 5 minutes and re-weigh. 继续烘干5分钟, 接着在称重. (f) Repeat (d) & (e) until 2 weighing readings are the same within + 0.05 g. (W3) 重复步骤d) 和 (e)直到两次称重一致(浮动+ 0.0

31、5 g.)(W3)Calculation 计算待添加的隐藏文字内容3 ( WO ) - ( WD ) x 100 = Moisture Regain ( % ) ( WD ) 回潮率( WO ) Original weight of wool = ( W2 ) - ( W1 ) 原始羊毛重量( WD ) Final dry weight of wool = ( W3 ) - ( W1 ) 烘干后的重量 4.Determination of Sliver Weight 毛条重量测定Sliver weight should be determined to establish the rate o

32、f production duringcontinuous top-treatment. 在连续毛条处理过程中, 须测定毛条重量来决定生产效率. Apparatus 器具Measuring ruler 量尺Analytical balance 分析天平Method 方法(a) Obtain at least 5 x one metre lengths of top by random sampling. 随意采样5根毛条, 每条1米. (b) Weigh the samples individually. 分别称重样品. (c) Work out the average sliver weig

33、ht in grammes per metre.计算毛条的平均重量 (克/米)5.Determination of Degree of Felting of Treated Wool Tops using the Kroy Felting Tester 使用Kroy制毯机对毛条进行制毯等级测定This test is applied to the sliver to assess, in a semi-quantitative manner, the effectiveness of the shrink-resist treatment. The test can be useful for

34、 in-plant control purposes, although it should not be used for confirmation of a successful treatment. 本实验采用半定量方式来测定防缩处理的效果. 虽然本实验不能用于确认处理的完美性, 但对于厂房控制非常有用. Chemicals 化学助剂Use a solution of ECE Reference Detergent of 0.5g/l. 使用ECE参考清洁剂溶液, 浓度0.5克/升. Distilled water is not essential, but hard water (ov

35、er 100 ppm CaCO3) should be avoided. 可以不用蒸馏水, 但不得使用硬水(碳酸钙含量超过100ppm)Equipment 设备Kroy Felting Tester Kroy制毯测试机Preparation of test specimen 试样的准备(a) Place the top sliver on a flat surface and cut a length of 650mm 20mm. 把毛条置于凭证的表面, 截一段650mm 20mm. (b) Adjust the weight of sliver to 12g 2g by adding to

36、or removing a strip of wool. 添加或去除一段毛条, 将其重量调整为12g 2g. (c) Secure one end of the sample with a tie-band approximately 10mm from the end. 使用约10毫米的带子从一端固定样品的末端. (d) Secure the tied end in a clamp or under a heavy weight and carefully split the sample lengthwise into three ends of equal thickness. 将连接端

37、固定在夹子上, 小心的纵向劈开样品, 使三个条等厚. (e) Plait the three strands into one sample by folding the outer strands over the centre one in turn. 像编辫子那样将三股编为一股, (f) Secure the second end of the specimen with a tie-band as before, to give a final plaited length of metre. 用绳子固定样品的另一端, 编后的长度为0.5米. (g) Make sample into

38、a band by tying both ends securely together. 将样品首尾紧紧连接. (h) Cut away any excess wool or tie-band from the knot.从结头上剪掉多余的羊毛或绳子. Operation of Kroy Felting Tester Kroy制毯机的操作(a) Add detergent solution to trough. 往水槽里添加清洁剂(b) Set test temperature to 40C and test duration to 30 minutes. 将温度调至40C, 试验时间30分钟

39、. (c) Set the speed at 50% of maximum. 将速度设为最高速的的二分之一. (d) Place the sample(s) in the machine and switch on heating. 将样品置入机器内, 按下加热按钮 (e) After reaching test temperature switch on run and close transparent cover. 待达到试验温度时, 按下开始按钮, 关闭透明盖. (f) Rinse sample(s) in cold water after run and grade as follo

40、ws. 操作完成后用冷水淋洗样品, 等级如下:Grading of The Tested Sample(s) 测试羊毛样品的分级The degree of felting of the fibre in the sample is assessed according to the scale shown below. 根据下列对比评定纤维制毯的等级:GRADE 等级DESCRIPTION 描述 1Felted, no visible features. 粘接, 无明显痕迹2Felted, impossible to pull apart, somefeatures apparent. 粘接, 不易分离, 有一些痕迹3Borderline, pulled apart with great difficulty. 边线, 极难分开 4Borderline, pulled apart with somedifficulty. 边线, 很难分开 5Pulled apart with ease, some entanglement. 可以轻易分开, 有些缠结 6Easy to pull apart, slight resistance. 容易分开, 抵抗力微弱7Superwash, no resistance. 连续防缩, 无耐抗性

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