VDA-275-中英文完整版本.docx

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1、Determination of Formaldehyde from Vehicle Interior with Modified Flask Method VDA 275改良烧瓶法测定汽车车内空气中的甲醛Moulded composites and fleeces for vehicles 汽车用模制复合材料和绒毛Determination of formaldehyde release 甲醛释放量的测定Test procedure called modified flask method 测试程序成为改良烧瓶法1. Purpose and application 目的和应用The pres

2、ent test method describes a necessary procedure to the method of the formaldehyde release fromthe vehicle interior. 试验方法描述了从车辆内部释放甲醛的方法的必要步骤The procedure is applied to the check of the equability of the production of form parts. 本程序适用于形状件生产的均匀性检验It can be applied restrictedly for the material develo

3、pment and to the receiving control 它可限制应用于材料开发和接收控制.2. Reference to other testing methods 参考其他测试方法VDA 276- Measuring procedure of formaldehyde, ammonia and phenols release form the vehicle interiorwith the use of 1 m2 chamber. VDA 276-使用 1 平方米的试验箱测量车辆内部甲醛、氨和酚的释放量3. Name 名称Name of the procedure of th

4、e formaldehyde release method. VDA 275.甲醛释放方法的程序名称 VDA 2754. Principle 原则In the test, samples of certain masses and dimension are fastened in a closed 1 litred Polyethylene flaskwith distilled water and are stored in steady temperature for a defined time. The bottles are then cooledand the dissolved

5、 formaldehyde in the distilled water is determined. The result is expressed in weight(mg/kg). 在试验中，一定质量和尺寸的样品用蒸馏水固定在一个密闭的 1 公升聚乙烯烧瓶中，并在规定的时间内保持稳定的温度。然后冷却瓶子，测定蒸馏水中溶解的甲醛。结果以重量（mg/kg）表示5. Reagents 试剂For the analysis, reagents of analytic grade and distilled or demineralized water must be used. Theforma

6、ldehyde content is determined photometry after the Acetylaceton method. Nevertheless, otherprocedures should be allowed if they correspond in specifications to the reference procedure for theanalysis 分析时，必须使用分析级试剂和蒸馏水或除盐水。用乙酰丙酮法测定甲醛含量。然而，如果其他程序与分析的参考程序的规范一致，则应允许使用这些程序5.1 Acetylaceton p.a. 乙酰丙酮5.2 Am

7、monium acetate p.a. 醋酸铵Remark: Commercially pre-prepared solutions can be used when the identical result is achieved.备注：当达到相同的结果时，可以使用商业预处理溶液6. Test equipment 试验设备6.1 Balance with range 1 mg 量程1 mg 的天平6.2 Well ventilated warm chamber which is able to hold a temperature from 1032C.通风良好的暖室，能够保持 1032的温

8、度6.3 Circulating air warm chamber which is able to hold a temperature from 602C循环空气暖室，能够保持 602的温度6.4 Spectrophotometer 分光光度计6.5 Test apparatus 试验装置-1 litred Polyethylene flask with a lid (see appendix picture 1) 1 公升带盖聚乙烯瓶(见附件图 1)-Hooks from high-grade steel with poetries, used in the lid of the tes

9、t bottle 高级钢制钩，用于测试瓶盖6.6 Lab. Device 实验室设备-Precision burette 50ml, calibrated at 20C50ml 精密滴定管，20校准-2 Measuring cylinder, 1000ml, calibrated at 20C 2 个 1000ml 量筒，20校准-6 Measuring cylinder, 100ml, calibrated at 20C6 个 100ml 量筒，20校准-Pipette, 5ml, calibrated at 20C 50ml 移液管，20校准-Pipette, 10ml, calibrat

10、ed at 20C 10ml 移液管，20校准-Pipette, 15ml, calibrated at 20C 15ml 移液管，20校准-Pipette, 20ml, calibrated at 20C 20ml 移液管，20校准-Pipette, 25ml, calibrated at 20C 25ml 移液管，20校准-Pipette, 50ml, calibrated at 20C 50ml 移液管，20校准-Pipette, 100ml, calibrated at 20C 100ml 移液管，20校准-Conical flask, 250ml250ml 锥形瓶-Bottle, 5

11、0ml with stop 50ml 瓶子，带塞子-Watch glass with diameter of 120mm 120mm 表面皿-Desiccator 干燥器-Cuvette with suitable thickness for the spectrophotometer 分光光度计用合适厚度的比色杯-Stop watch 秒表7. Specimen 样品7.1.1 Specimen: The test bodies should be taken from suitable and representative places of the vehicleinterior par

12、ts 试样：试验体应取自车辆内部合适且具有代表性的地方7.1.2 The size of the test bodies in each case should be 40 mms x 100 mms x thickness. At least 6test bodies are taken, of it 5 parts for the test and 1 for the moisture content test 每种情况下，试验体的尺寸应为 40 mms x 100 mms x 厚度。至少取 6 个试验体，其中 5 个用于试验，1 个用于含水量试验8. Realization of the

13、 check 实现检查8.1 Number of the check: These are professional method to be carried out 检查次数:这些都是要执行的专业方法8.2 Determination of the moisture content 水分含量的测定The moisture content is determined with DIN EN 322 含水量按 DIN EN 322 测定8.3 Regulation of the formaldehyde release 甲醛释放的调节The test bodies become precise-

14、weighed out before the beginning of the analysis on the analysis scales on 0.01 g. In each of the Polyethylene flask become 50 ml distilled water is pipetted. 在 0.01 g的分析天平上开始分析之前，对试验体进行精确称重。在每个聚乙烯烧瓶中，用移液管移取 50 ml 蒸馏水For the connection, the test bodies will provide 10 mms of the upper edge concentri

15、c with 1 to 2 mmsof drilling for the purpose of connection in the hanging hook. 对于连接，试验体将提供 10 mm 的上边缘同心，并提供 1 至 2 mm 的钻孔，以连接吊钩After fixing of the test bodies in the hook (see appendix: picture 1) the vessel is closed and is kept more than 3 hours in the warm chamber (6.3) with a steady temperature

16、at 60C. 将试验体固定在吊钩中（见附录：图 1）后，容器关闭，并在 60的恒温箱（6.3）中保持 3 小时以上At the end of the test time the vessels from the warm chamber are taken. After 60 minute stabilizing time at ambient temperature the test bodies from the test bottle are removed. 试验结束时，从温室取出容器。在环境温度下稳定 60 分钟后，从试验瓶中取出试验体8.4 The control test 对照

17、试验The attempt is carried out without test body in parallel. 试验是在没有平行试验体的情况下进行的8.5 Regulation of the formaldehyde concentration in the absorbent solution 吸收液中甲醛浓度的调节 The formaldehyde content of the absorbent solution is detected by photometry after the Acetylaceton method. 用乙酰丙酮法测定吸收液中甲醛的含量8.5.1 The

18、principle 原则The chemical reaction (see appendix on the so-called Hantzschen: picture 2) with which dissolved formaldehyde reacts in solution react with Ammonia and Acetylaceton to form Diacetyldihydrolutidin (DDL). The absorption maximum of DDL is 412 nm. The reaction is specific for formaldehyde. 溶

19、解的甲醛在溶液中与氨和乙酰丙酮反应生成二乙酰二水解素（DDL）的化学反应（见所谓的 Hantzschen:图 2 附录）。DDL 的最大吸收波长为 412nm。这种反应是甲醛特有的。8.5.2 Reagent 试剂8.5.2.1 Acetylaceton solution 乙酰丙酮溶液4ml of Acetylaceton are dispensed in a 1000 ml to measuring cylinder and is made up to 1000 ml with distilled water. The solution air-tighted and can be used

20、 for 4 weeks if kept away from light. 在 1000ml 的量筒中加入 4ml 乙酰丙酮，用蒸馏水配制成 1000ml。溶液密闭，避光使用 4 周8.5.2.2 Ammonium acetate solution 醋酸铵溶液200 g of ammonium acetate is dispensed in a 1000ml measuring cylinder and make up to 1000ml with distilled water. 在 1000 毫升量筒中加入 200 克醋酸铵，用蒸馏水补充至 1000 毫升8.5.3 Reaction 反应

21、10ml of the absorbent solution (8.3) are taken with a pipette and are moved in a 50ml bottle with 10 ml Acetylaceton solution (8.5.2.1) and 10 ml ammonium acetate-solution (8.5.2.2). The bottle is closed, shaken and warmed up for 15 minutes in a waterbath at 40C. The greenish-yellow solution is then

22、 cooled at ambient temperature, protected from the sunlight (about one hour). The optical density of this solution is determined with a wavelength of 412 nm by distilled water with a Spectrophotometer (6.4). A control is determined in parallel with distilled water and is taken into consideration wit

23、h the calculation of the bottles value (9.2). 用移液管吸取 10ml 吸收液（8.3），并将其移入 50ml 瓶中，加入 10ml 乙酰丙酮溶液（8.5.2.1）和 10ml 醋酸铵溶液（8.5.2.2）。将瓶子关上，摇动，在 40的水浴中加热 15 分钟。然后在室温下冷却绿黄色溶液，防止阳光照射（大约 1 小时）。用蒸馏水和分光光度计（6.4）在 412nm波长下测定该溶液的光密度。控制与蒸馏水平行确定，并在计算瓶值时考虑（9.2）。Remark: After every test, the PE flasks are cleaned in a

24、lab washer. Should this not be sufficient, it is advisable that the flasks are kept at 70C openly in a circulating air warm chamber for approximately 16 h. 备注：每次测试后，聚乙烯烧瓶在实验室洗衣机中清洗。如果这还不够，建议将烧瓶公开地保持在 70的循环空气暖室中约 16 小时。8.5.4 Calibration curve 校准曲线The calibration curve (see appendix: pictures 3 and 4)

25、 is constructed by means of a formaldehyde standard solution whose concentration was determined by titration with iodine. The calibration curvemust be checked at least once per week. 校准曲线（见附录：图 3 和图 4）由甲醛标准溶液构成，其浓度通过碘滴定测定。校准曲线必须每周至少检查一次。8.5.4.1 Formaldehyde-standard solutions reagent solutions 甲醛标准溶

26、液试剂溶液Iodine 典 c(I2 )=0.05 mol/升Sodium thiosulfate 硫代硫酸钠 c(Na2S2O3 )=0.1 mol/l Sodium hydroxide 氢氧化钠 c(NaOH) = 1mol/l Sulfuric acid 硫酸 c(H2SO4 )= 1 mol/lIndicator solution 1% m/m 指示剂溶液 1% m/mThe Titer of the solutions must be checked before use. 使用前必须检查溶液的滴定度About 1 g of formaldehyde solution (concen

27、tration of 35 to 40%) are solved in a 1000 ml measuring cylinder with distilled water and are filled in up to mark. The exact formaldehyde concentration is determined as follows: 约 1g 甲醛溶液（浓度为 35%至 40%）用蒸馏水溶解在 1000ml 量筒中，并填充至标记处。准确的甲醛浓度测定如下20ml of the formaldehyde-standard solution are mixed with 25

28、ml iodine solution and 10ml mixed sodium hydroxide solution. After 15 minute stabilizing time under light, 15ml sulfuric acid is added to the mixture. The excess iodine reacts with the thiosulfate solution. At the end of the titration some drops of indicator solution are added. The control is carrie

29、d out with 20ml to distilled water in parallel.将 20 毫升甲醛标准溶液与 25 毫升碘溶液和 10 毫升氢氧化钠混合溶液混合。在光照下稳定 15 分钟后，向混合物中加入 15ml 硫酸。过量的碘与硫代硫酸盐溶液发生反应。滴定结束时加入几滴指示剂溶液。用 20 毫升蒸馏水平行控制。The formaldehyde content is calculated with the following formula: c (HCHO) =(Vo-V)x15 c(Na2S2O3) x 1000/20 Where: c (HCHO): Formaldehy

30、de concentration in mg/l甲醛含量的计算公式为：c（HCHO）=（Vo-V）x15c（Na2S2O3）x 1000/20 其中：c（HCHO）：甲醛浓度，mg/lVo: Volumes of the thiosulfate solution for the control in ml V: Volumes in thiosulfate solution in ml .Vo:对照品硫代硫酸盐溶液的体积，单位为毫升 V：硫代硫酸盐溶液的体积，单位为毫升c(Na2S2O3): Concentration of the thiosulfate solution in mol/l

31、硫代硫酸盐溶液浓度，单位为 mol/l Remark: 1ml 0.1 mol/l thiosulfate solution corresponds to 1 ml 0.05 mol/l of iodine solution and 1.5 mg of formaldehyde 备注：1 毫升 0.1 摩尔/升硫代硫酸盐溶液相当于 1 毫升 0.05 摩尔/升碘溶液和 1.5 毫克甲醛8.5.4.2 Formaldehyde calibration solution (with thickness of the cuvette: 1 cm) From the formaldehyde stan

32、dard solution, determined in 8.5.4.1, becomes a volume which contains 15 mg of formaldehyde from a microburette in a 1000ml measuring cylinder and filled with distilled water up to mark filled in. 1 ml of this solution contains 15 g formaldehyde. 甲醛校准液（比色杯厚度：1cm）从8.5.4.1 测定的甲醛标准溶液中，变为 1000ml 量筒中的微导管

33、中含有 15mg 甲醛的体积，并充满蒸馏水，直至标记填充。1 毫升该溶液含有 15 微克甲醛8.5.4.3 Calibration curve 校准曲线0, 5, 10, 20, 50 or 100 ml are filled in by the formaldehyde calibration solution (8.5.4.2) in a 100ml measuring cylinder and with distilled water up to mark. 10ml of solution are photometrically analyzed with the same proce

34、dure, as that of 8.5.3. 用甲醛校准液（8.5.4.2）在 100ml 量筒中加入 0、5、10、 20、50 或 100ml，蒸馏水至刻度。用与 8.5.3 相同的程序对 10ml 溶液进行光度分析。The optical densities are applied against the formaldehyde concentration (between 0 and 15 g/ml) on standard curve. The upward gradient is determined graphically or is calculated. 根据标准曲线上的

35、甲醛浓度（介于 0 和 15 微克/毫升之间）施加光密度。向上梯度以图形方式确定或计算8.5.4.4 Formaldehyde calibration solution (with thickness of the cuvette: 5 cm) From the formaldehyde-standard solution, determines under 8.5.4.1, becomes a volume which contains 3 mg of formaldehyde with a microburette in a 1000ml measuring cylinder and ma

36、ke up to mark with distilled water. 1ml of this solution contains 3 g of formaldehyde. 甲醛校准液（比色杯厚度：5cm）与甲醛标准溶液的距离，按 8.5.4.1 测定，用 1000ml 量筒中的微量管制成含有 3mg 甲醛的体积，并用蒸馏水配制标记。1毫升该溶液含有 3 微克甲醛。8.5.4.5 Calibration curve 校正曲线0, 5, 10, 20, 50 or 100 are filled in by the formaldehyde calibration solution (8.5.4.

37、4) ml in a 100ml measuring cylinder and with distilled water up to mark. 0、5、10、20、50 或 100 用甲醛校准液（8.5.4.4） ml 在 100ml 量筒内，用蒸馏水灌满至刻度10ml of solution is photometrically analyzed with the same procedure, as that of 用相同的方法对 10ml溶液进行光度分析8.5.3. The optical densities are applied against the formaldehyde c

38、oncentrations (between 0 and 3g/ml) on standard curve. The upward gradient is determined graphically or is calculated. 根据标准曲线上的甲醛浓度（介于 0 和 3 微克/毫升之间）施加光密度。向上梯度以图形方式确定或计算9. Calculation of the results 计算结果9.1 Moist content 含水量The moist content H (in masses % m/m) of the form part arises from the follo

39、wing formula 含水量 H(质量百分比 m/m)由下式可得:m1 - m0H =m0x 100Besides, is:另外m1: the masses of the test bodies before the drying in gramm1 是烘干前试样的质量，单位为克m0: the masses of the test bodies after the drying in gramm0 是烘干后试样的质量，单位为克9.2 Formaldehyde release with flask method 用烧瓶法释放甲醛The whole amount of dissolved fo

40、rmaldehyde becomes from the upward gradient factor of the photo-metrical regulation and the whole volume of the absorbent liquid (here: 10ml) investigates. ThisFormaldehyde is calculated with the weight corrected on dry weight of the test body in mg /kg. Calculation of the formaldehyde delivery in m

41、g / kg: 溶解甲醛的总量是由光度调节的向上梯度因子和吸收液的总体积（这里是 10ml）决定的。该甲醛的计算方法是根据试验体的干重校正后的重量（mg/kg）。甲醛释放量的计算（mg/kg）：(As - AB) x f x V x (100 + H) x F = mg HCHO/kg m x 1000As: the optical density of the analyzed solution 分析溶液的光密度AB: the optical density of the analysis with distilled water f: the upward gradientfactor o

42、f the calibration function (in g/ml) 蒸馏水分析的光密度f：校准函数的向上梯度因子（g/ml）m: the masses of the test body in g 试样的质量H: the moisture content of the test material in percent V: the volume ofthe absorbent solution (50 ml) 试验材料的含水量百分比V：吸收溶液的体积（50毫升）atro: absolutely dry test material 绝对干燥试验材料F: Factor to the calcu

43、lation of the result of analysis in kg mg / kg; F=10 计算分析结果的系数，单位为kg【mg/kg】；F=1010. Test report 试验报告In the test report the following information should be given with reference to this test method, ifnecessary: 在试验报告中，如有必要，应提供与本试验方法有关的下列信息：- Origin of the test material 试验材料的来源- Place, position and st

44、ate of the material at the time of the sampling, in particular the humidity 取样时材料的位置、位置和状态，特别是湿度-date and production of the material 材料的日期和生产-date of the sampling 抽样日期-date of the test performed 试验日期-moisture content (%) at the time of the check (according to 8.2) 检查时的含水量百分比（根据 8.2）-formaldehyde release after the flask method (mg of formaldehyde / kg dry test material) 烧瓶法后甲醛释放量（mg 甲醛/kg 干试验材料）-description of other details 1) 其他细节说明 1）1)Report on all occurrences which are not according to this test regulation 报告所有不符合本试验规则的情况(withdrawal of the test bodies, conditioning etc.) 退出试验机构、调节等