ImageVerifierCode 换一换
格式:PDF , 页数:6 ,大小:53.58KB ,
资源ID:746847      下载积分:10000 积分
快捷下载
登录下载
邮箱/手机:
温馨提示:
如需开发票,请勿充值!快捷下载时,用户名和密码都是您填写的邮箱或者手机号,方便查询和重复下载(系统自动生成)。
如填写123,账号就是123,密码也是123。
特别说明:
请自助下载,系统不会自动发送文件的哦; 如果您已付费,想二次下载,请登录后访问:我的下载记录
支付方式: 支付宝扫码支付 微信扫码支付   
注意:如需开发票,请勿充值!
验证码:   换一换

加入VIP,免费下载
 

温馨提示:由于个人手机设置不同,如果发现不能下载,请复制以下地址【http://www.mydoc123.com/d-746847.html】到电脑端继续下载(重复下载不扣费)。

已注册用户请登录:
账号:
密码:
验证码:   换一换
  忘记密码?
三方登录: 微信登录  

下载须知

1: 本站所有资源如无特殊说明,都需要本地电脑安装OFFICE2007和PDF阅读器。
2: 试题试卷类文档,如果标题没有明确说明有答案则都视为没有答案,请知晓。
3: 文件的所有权益归上传用户所有。
4. 未经权益所有人同意不得将文件中的内容挪作商业或盈利用途。
5. 本站仅提供交流平台,并不能对任何下载内容负责。
6. 下载文件中如有侵权或不适当内容,请与我们联系,我们立即纠正。
7. 本站不保证下载资源的准确性、安全性和完整性, 同时也不承担用户因使用这些下载资源对自己和他人造成任何形式的伤害或损失。

版权提示 | 免责声明

本文(FORD FLTM AV 102-01-2000 DETERMINATION OF PERCENT SILICA-PRODUCING VOLATILES IN SILICONE RUBBER ADHESIVES SEALERS WHICH CURE AT ROOM TEMPERATURE (Replaces FLTM AV 002-01)《室温固化型硅橡胶胶.pdf)为本站会员(fatcommittee260)主动上传,麦多课文库仅提供信息存储空间,仅对用户上传内容的表现方式做保护处理,对上载内容本身不做任何修改或编辑。 若此文所含内容侵犯了您的版权或隐私,请立即通知麦多课文库(发送邮件至master@mydoc123.com或直接QQ联系客服),我们立即给予删除!

FORD FLTM AV 102-01-2000 DETERMINATION OF PERCENT SILICA-PRODUCING VOLATILES IN SILICONE RUBBER ADHESIVES SEALERS WHICH CURE AT ROOM TEMPERATURE (Replaces FLTM AV 002-01)《室温固化型硅橡胶胶.pdf

1、 FORD LABORATORY TEST METHOD AV 102-01 Date Action Revisions 2000 08 30 Revised Editorial no technical change A. Cockman 2000 05 22 Editorial no technical change A. Cockman 1989 10 23 Printed copies are uncontrolled Page 1 of 6 Copyright 2000, Ford Global Technologies, Inc. DETERMINATION OF PERCENT

2、SILICA-PRODUCING VOLATILES IN SILICONE RUBBER ADHESIVES/SEALERS WHICH CURE AT ROOM TEMPERATURE Application This test method establishes a procedure to determine the percent silica - producing volatiles present in an RTV sealant. Silica - producing volatiles are contributors to the fouling of oxygen

3、sensor systems used in the control of vehicle emissions. As a contributing source of contamination, the volatile potential of TRV sealants can be accurately monitored by the use of this procedure. Utilizing this method in conjunction with the realistic maximum volatility tolerance level can help min

4、imize the risk of oxygen sensor disfunction from formed - in - place sealants. Scope The procedure consists of four basic steps: 1) the RTV s ealant is cured to its elastomeric form; 2) the volatiles are extracted from the cured sealant; 3) the extract is separated and measured by gas chromatography

5、; and, 4) the GC results are quantified using a siloxane calibration. The volatile silicones from a commercial RTV sealant are primarily cyclodimethyl - siloxane. Other species present having GC retention times similar to those of the cyclics are assumed to be silicone as well. Apparatus and Materia

6、ls Required Gas Chromatograph Varian Model 2720 or equivalent, equipped with a thermal conductivity or flame ionization detector and linear temperature programmer. Column A column capable of separating cyclosiloxanes, e.g. 3.0 m x 3.0 mm stainless steel standard wall packed with 5 % OV - 101 on Chro

7、mosorb W , HP grade, 80/100 mesh. Inlet packing should be Chromosorb W, HP grade 80/100 mesh. The maximum operating temperature for OV - 101 in 350 C. Use of other phase materials with maximum operating temperatures closer to the 290 C procedure temperature may r esult in column bleed and a shift in

8、 the base line. A base line shift will affect integration of the higher cyclics and linears. Recorder-Integrator (1 MV) Hewlett - Packard Model 3390 A or equivalent, for data acquisition. Glass Plates 0.89 mm thick, for curing the wet formed - in - place sealant (see Figure 1). FORD LABORATORY TEST

9、METHOD AV 102-01 Page 2 of 6 Copyright 2000, Ford Global Technologies, Inc. Teflon Slab (see Figure 1) Humidity Chamber A humidity chamber for curing samples, or a controlled laboratory environment with a relative humidity of 40 to 60 %. Wrist-Action Mechanical Shaker VWR Catalog Number 57040 - 027

10、or equivalent. Vials Flint glass, 30 mL, VWR Catalog Number 66011 - 165 or equivalent. Screw cap, size 22 - 400 with polyethylene cone liner, VWR Catalog Number 16217 - 067 or equivalent. Syringe Capable of accurately delivering 20 + 0.1/ - 0.0 microlitre (no plastic elements due to solvents used).

11、Serum Bottles/Hypodermic Vials Due to the volatility of pentane, the standard solution should be sealed to minimize evaporative loss. Use capped serum bottles, Fisher Catalog Number 06406E or 1 mL disposable hypodermic vials with septums. Balance Top load balance with glass draft shield capable of 0

12、.0001 g accuracy. Reagents All must be reagent grade. Silicone Standards Polydimethylcyclosiloxanes can be obtained from base manufacturers (G E, Wacher Silicones, Huls America or Silar). Pentane Dodecane Spectral grade (99 %). Helium For carrier gas. Conditioning and Test Conditions All test values

13、 indicated herein are based on material conditioned in a controlled atmosphere of 23 +/ - 2 C and 50 +/ - 5 % relative humidity for not less than 24 h prior to testing and tested under the same conditions unless otherwise specified. FORD LABORATORY TEST METHOD AV 102-01 Page 3 of 6 Copyright 2000, F

14、ord Global Technologies, Inc. Procedure A. Preparations 1. Cured Sample. Tape two 0.889 + 0.051/ - 0.000 mm thick glass plates to the Teflon slab so they are approximately parallel and about 50 mm apart. Place a quantity of RTV sealant on the Teflon slab between the two plates and near one end. Draw

15、 a third plate across the deposited RTV, spreading it to an even thickness (0.889 mm) between the t aped plates. The spreading plate riding on the parallel plates maintains the necessary sample thickness. Avoid entrapped air and knit lines when preparing the sample. Allow this sample to cure for 24

16、hours at 25 C and 50 % relative humidity (see Figure 1). Cut three (3) strip specimens for each candidate material that produce the desired sample weight (1 g) in one piece. The cured sample thickness should be 0.899 mm. Make the cuts in the following locations on the cured slabs (see Figure 2). 2.

17、Stand ard Solution. Add 0.1 g (weighed to the nearest 0.1 mg) of each pure cyclic (98 %) to 1.0 g of dodecane (99 % - weighed to the nearest 0.1 mg). Add 10 +/ - 0.1 mL of pentane to the container and seal to prevent evaporation. 3. GC Operating Conditions. Use the following settings for this analys

18、is. Variation is allowed provided there is sufficient separation of peaks. Inlet: 290 C Detector: 290 C Column: 50 C to 320 C at 10 C/minute with 20 minutes hold at upper limit He Carrier Gas Flow Rate: 35 mL/ minute. 4. Calibration. Use the operating conditions described in A.3 and inject a one (1)

19、 microlitre sample of the standard solution. Response factors for the individual cyclics are calculated using the following equation: R f D n = Amt. D n in std. soln. x Area dodecane in chromatogm. Area D n in chromatogm. Wt. dodecane in Std. soln. Response factors for cyclic species vary in a relat

20、ively linear manner from D 5 through D 10 , so that response factors for cyclics not in the standard solution can be calculated from the known response factors of the cyclics in the standard solution. All unknowns which appear in the analysis are assumed to be siloxanes. All unknowns are given, as r

21、esponse factors, the average response factor calculated for the cycl osiloxanes from D 4 through D 1 0 . FORD LABORATORY TEST METHOD AV 102-01 Page 4 of 6 Copyright 2000, Ford Global Technologies, Inc. B. Test: 1. Extraction. Pre -weigh each cured sample (0.98 to 1.02 g). Weigh 0.015 to 0.025 g of d

22、odecane to the nearest 0.0001 g and place it in the 30 mL vial. Add about 10 mL of pentane. Place the curved sample into the vial and seal the container immediately to prevent evaporative loss. Shake for 16 hours. Note: The sequence is important due to the volatility of the solvents used. 2. Inject

23、40 microliters when using a thermal conductivity detector, or 1 to 5 mic roliters when using a flame ionization detector, into the column at the recommended test conditions (A.3). 3. After the elution is complete, about 35 minutes, identify the peaks and quantify them by integration using the follow

24、ing equations: % D n = R f D n (Area D n in chromgm) x Wt. of dodecane in sample x 100 Area dodecane in chromgm Wt. RTV in sample Perform the calculation for D 4 - D 10 . % Unkn.= R f D 4 - D 10 (Area unkn. in chrgm) x Wt. dodecane in sample x 100 Area dodecan e in chromgm Wt. RTV in sample R f D 4

25、- D 10 = Average response factors of D 4 - D 10 . Perform the calculation for all unknowns that elute between D 4 - D 10 . % Siloxane Volatiles = Sum of % cyclics D 4 - D 10 and sum of % unknowns eluting from D 4 - D 10 . Notes: Silicone volatiles below D 5 may not be detected at their correct level

26、s due to their loss from the sealant as it cures for 24 hours at 25 C and 50 % relative humidity. Dodecane can mask D 5 forms and the beginning of the first unknown. Any D 3 not lost would be masked by impurities in pentane. Weight precision is extremely important if the results are to be reproducib

27、le. C. Reporting: 1. Three data points shall be reported for each sample as % total volatiles. 2. Final results for siloxan e should be expressed as 0.00 %. Report D 4 through D 10 for total volatiles as cyclics plus unknowns (L 4 through L 10 ). 3. Automated devices for measuring and calculating pe

28、ak areas should be used. No planimeters. 4. All observed and recorded data on whi ch the calculations are based. 5. Date of the test, the conditions of cure and thickness of the sample. FORD LABORATORY TEST METHOD AV 102-01 Page 5 of 6 Copyright 2000, Ford Global Technologies, Inc. D. Precision and

29、Bias: 1. Statements on precision and bias were prepared in accordance with “Evaluating the Measurement Process“, D. J. Wheeler and R. W. Lyday, c.1984. 2. The results were determined from an inter laboratory program with six materials and six laboratories. Testing was conducted on three separate day

30、s within each laboratory. 3. Repeatability refers to within - laboratory variation (op erator) and reproducibility refers to between laboratory variation. 4. Bias, in statistical terminology, is the difference between an average test value and the reference, or true, test property value. Reference v

31、alues do not exist for this test method si nce the value or level of the test property is exclusively defined by the test method. Bias, therefore, cannot be determined. E. Calculations: 1. Total Volatiles - Est replication std. dev. = 0.0338 Est. uncert. for a single meas. (median uncert.) = 0.67 =

32、0.023 95 % upr. bound = 2.00 = 0.068 Repeatability (oper. effect) = 0.0399 Meas. error std. dev. = + = (0.0338) + (0.0399) = 0.052 Est. sample to sample std. dev. = 0.28 Signal to Noise ratio / = 5.38. Thus the number of distinct product categories that can be reliably distinguished is 1.41 x 5.38 =

33、 7.59 2. Percent Cyclics - Est. replication std. dev. = 0.031 Est. uncert. for a single meas. (median uncert.) = 0.67 = 0.02 95% upr. bound = 2.00 = 0.06 Repeatability (oper. effect) = 0.067 Meas. error std d ev. = + = (0.031) + (0.067) = 0.074 Est. sample to sample std. dev. = 0.33 Signal to Noise

34、ratio / = 4.46. Thus the number of distinct product categories that can be reliably distinguished is 1.41 x 4.46 = 6.29 Chemicals, materials, parts, and equipmen t referenced in this document must be used and handled properly. Each party is responsible for determining proper use and handling in its facilities. FORD LABORATORY TEST METHOD AV 102-01 Page 6 of 6 Copyright 2000, Ford Global Technologies, Inc. Figure 1 Apparatus to Make Cured Slabs Figure 2 Locations for Sample Cuts from Cured Slabs

copyright@ 2008-2019 麦多课文库(www.mydoc123.com)网站版权所有
备案/许可证编号:苏ICP备17064731号-1