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ISUZU ENGINEERING STANDARD MATERIALS ISC-F00-001A铃木工程标准材料Method of measuring concentration of Volatile OrganicCompounds (VOC) emitted from car parts汽车零部件VOC(挥发性有机化合物)浓度测试方法Established on : July 30, 2004 制订:2004.7.30Revised on : July 21, 2005 修订:2005.7.21Reaffirmed on: January 1, 2012重申:2012.1.11. SCOPE 范围 This standard specifies the method of measuring the concentration of volatile organic compounds (VOC) emitted from the materials of car parts in order to facilitate researches for reducing in-occupant-room VOC including 7 compounds; formaldehyde, acetaldehyde, toluene, xylene, ethylbenzene, styrene and tetradecan, among the substances which are listed in the guideline on the interior air contaminants made by the Ministry of Health, Labor and Welfare. 该标准详细说明了从汽车零部件材料中挥发的挥发性有机化合物浓度测试方法,目的是方便对降低“内部-居住者-空间”VOC包括7种:甲醛、乙醛、甲苯、二甲苯、乙苯、苯乙烯、十四烷的调查,包含于“健康,劳动,保障政府部门”制订的内部空气污染物方针列出的物质。2. REFERENCE STANDARD 参考标准 “Determination of the of volatile organic compounds and aldehydes for building products Small chamber method (JIS A 1901)”. “建筑产品挥发性有机化合物和醛发散的决定小房间方法(JIS A 1901)3. VOC COLLECTION APPARATUSES AND SAMPLE PREPARATION VOC收集装置和样品准备3.1 VOC Collection Apparatuses VOC收集装置 - Tedlar Bags (10) having a sleeve with a cock (made by GL Science or equivalents) XX袋(10)其上有带有龙头的袖子(由GL Science制造或等效的替代品)- Clips or Teflon tape (ASF-110 made by Chukou Kagaku or equivalents) to seal Tedlar Bags 夹子或特氟纶带子(ASF-110由Chukou Kagaku制造或等效的替代品)来密封聚氟乙烯薄膜袋子- Pure nitrogen (purity : 99.9% or higher) in pressure vessel 纯氮(纯度:99.9%或更高)置于压力容器内- A Suction Box, 10 (made by Oumi Odor Air Service or equivalents) 一个抽气泵,10L(由Oumi Odor Air Service制造或等效的替代品)- Activated carbon (Activated carbon for column chromatography made by Wako Junyaku Kogyo or equivalents or equivalents) 活性碳(柱状套色版活性炭由Wako Junyaku Kogyo制造或等效的替代品)- Teflon tube (With a length enough to connect apparatuses, such as from the Tedlar Bag to VOC collection tubes, to sampling pump, etc.) 特氟纶管(有足够的长度来连接装置,例如从聚氟乙烯薄膜袋子到VOC收集管,到采样泵,等等)- Silicone tube (Used between Teflon tube and Tedlar Bag, TENAX tube or DNPH cartridge to connect them) 硅树脂管(用于特氟纶管和聚氟乙烯薄膜袋子、TENAX管、DNPH 滤筒之间连接)- An air bath regulated at 65C 一个空气浴缸通常在65C - TENAX TA-packed glass tubes, 6mm (outside dia.) x 159mm (length), or equivalent for collecting toluene (hereinafter abbreviated as TENAX tube) TENAX TA-packed 管,6mm(外径) 159mm(长度),或用来采集甲苯的等效的替代品(以下简述为TENAX 管)- A DNPH-Silica cartridge (GL-pack mini AERO made by GL science, Sep-Pak and DNPH-Silica made by Japan Waters or equivalents) for collecting aldehydes (hereinafter abbreviated as DNPH cartridge) 一个DNPH-硅石滤筒(GL-pack mini AERO由GL science制造,Sep-Pak and DNPH-Silica由Japan Waters制造或等效的替代品)来收集醛(以下简述为DNPH滤筒)- A pump for gas collection and a gas flow meter : A unit capable of collecting gas at a rate of 100 1000 m/min. (SP-208-1000 Dual, made by G.L. Science, or equivalents) 一个气体采集泵和一个气流表:一个采集气体单位能效在100 1000 m/min. (SP-208-1000 Dual由 G.L. Science制造或等效的替代品)- Vacuum pump (Iwai Air pump APN-085V-1 made by Iwai Co. Ltd. Or equivalents) 真空泵(Iwai Air pump APN-085V-1由Iwai Co. Ltd.制造或等效的替代品)3.2 Sample Preparation 样品准备 Samples of completed car parts for VOC measurement shall be, as a rule, left in the shipping package at room temperature until tests which should be performed 14 days after the manufacture of the car parts,为VOC测量准备的已完成的汽车零件样品,按要求需要在室温下留在海运集装箱直至试验,试验需要在汽车零件制造14天后进行, however, may be tested 10 to 20days after the manufacture, provided the period from the manufacture to the test and the storage condition during the period are reported. 然而,也可能在制造10至20天后进行试验,这就需要提供从制造到试验的周期时间以及这一周期内的储存条件。Samples shall be cut, as a rule, into 10x10cm test pieces but parts having a width less than 10cm shall be cut to 10cm lengthwise and those having overall sizes less than 10cm are tested as entireties. Composite materials including laminations shall be sampled as inseparable entireties. Parts allowing disassembly such as bolted assemblies, shall be disassembled and cut into the above mentioned lengths and sizes but those which should not be disassembled such as electric and electronic parts shall be tested as entireties. The measurements on size and area of each test piece shall be reported. 按要求,样品需要切成1010cm的试片,当零件宽度小于10cm需要切成10cm纵向切片,零件整个尺寸都小于10cm的以整体进行试验。复合材料包含多层时需要作为不可分离的整体做样。零件可以分解,例如螺栓装配件,需要分解并切成上述长度和大小,但是有些不能分解的如电线及电气原件需要作为整体试验。对于每一试片的尺寸和区域的测量均需列入报告。4. VOC EMISSION AMOUNT ANALYSIS VOC 释放总量分析4.1 Preparation of Bags for Analysis 分析用袋子的准备1) Obtain Tedlar Bags (hereinafter referred to as bags) equal in number to the number of specimens plus two (1) . 取比样品数量多两个数量的聚氟乙烯薄膜袋子(以下简称袋子)(1) Bags are used one for each of the specimens and the plus two bags are used one for blank test and one for a nitrogen-gas container. Without suction box, the number of necessary bags are equal to the number of specimens plus one for blank test. 每个样品使用一个袋子,额外的两个一个用作空白试验另一个装氮气。除了吸气箱,所必需的袋子数量与样品数相等,只增加一个空白试验用的。 2) Attach a silicone tube, 2 3 cm in length, to the end of the Teflon sleeve of each bag with a Teflon cock. If bags without Teflon cock are used, plug the Teflon tube. If bags with one end open are used, seal the opening using plastic clips. 将一个硅树脂管长度方向上2-3cm与带有龙头的特氟龙袖子末端相连。如果袋子不与特氟龙龙头配套使用,就堵上特氟龙管子。如果用一端开口的袋子用特氟龙带子密封开口。3) Connect one end (inlet) of serially connected two activated carbon cartridges to a nitrogen supply line valve and the other end (outlet) to an opening of a 3-way cock, the remaining two openings of the cock being connected to a vacuum pump and a bag. See Fig. 1将连续相连的两个活性炭滤筒一端(进口)连接到一个氮气供应线阀上,另一端(出口)连接到三通龙头的一个开口上,三通龙头另外两个开口连接到一个真空泵和一个袋子上,见图1.4) Operate the 3-way cock to fill the bag with nitrogen and then suck the nitrogen from the bag using the vacuum pump (2) 操作三通龙头用氮气充满袋子,再用真空泵从袋子中吸取氮气(2) while flattening the rumpled bag to allow the gas to be fully sucked up. 将弄皱的袋子整平来让气体被完全吸净5) Repeat the step 4) above 3 to 5 times for complete purge. All of the bags for VOC specimens and for blank test shall be plugged quickly immediately after nitrogen gas is sucked up. 重复上述步骤4)3到5次来彻底抽净。一旦氮气被抽光,所有为VOC试样及空白试验准备的袋子必须快速堵住。6) Fill a bag used as a nitrogen-gas container (nitrogen bag) with nitrogen after the step 5) is finished.在步骤5)完成后用氮气充满用作氮气容器的袋子(氮气袋)4.2 Putting Test Pieces into Bags and Sealing Bags, and Connecting Tubes on Suction Box Notes for sealing bags containing test pieces : 将试样放入袋内,密封袋子,连接管子和吸气箱。密封装有试样的袋子注意:- Use throwaway polyethylene gloves (Saniment or equivalent products) to handle test pieces. Do not touch test pieces with the naked hand. 使用用后及仍的聚乙烯手套(Saniment或等效的替代产品)来拿取试样,请勿用裸手触碰试样。- Unless otherwise specified, a test piece should be placed in a bag with the surface having the largest area kept apart from the bag surface. However, a test piece with an adhesive surface, such as pressure-adhesive tape, should be placed in a bag with the backup paper peeled off and the adhesive surface closely applied to the bag. 除非另有指定,一个试样应该使试样的最大表面远离袋子表面放置到袋内。然而,一个带粘性表面的试样,例如压力-粘性带,应该按照反面远离粘面靠近袋子放置在袋内。1) Place a test piece in a bag, seal and deaerate the bag using a vacuum pump. 放置一个试样到袋内,密封并用真空泵排去袋内气体。 How to seal a bag after a test piece is placed in it (Example): 一试样放入袋中后怎样密封袋子(示例):Cut off a corner of the bag (3) , place a test piece in the bag, immediately fold back the cut edge of the bag corner inwardly and seal using Teflon tape (4) as shown in Fig. 2 below. 切除袋子一角,将一试样放入袋内,迅速向内翻折袋角的切除边缘并用特氟龙带子密封,如下图2所示。(3) Bags having an opening at a corner may be used. 袋角有开口可能是用过的袋子(4) For sealing the bag, plastic clips may be used in stead of Teflon tape 密封袋子,塑料夹子可以替代特氟龙带子2) Connect the outlet end of an activated carbon cartridge (one of the cartridges used in 4.1) to the nitrogen introduction tube leading through the suction box wall to the bag in the suction box. Nitrogen flow through the cartridge shall be in the same direction as described in 4.1. See Fig. 3. 将一个活性炭滤筒(4.1中所使用的其中一个)的出口端连接到氮气传输管,穿过吸气箱壁至吸气箱内的袋子,氮气流经滤筒方向应与4.1中描述一致。见图3.3) Connect the nitrogen bag to the inlet of the cartridge. 将氮气袋连接至滤筒的进口4) Connect the sampling pump to the outlet of the suction box. 连接收集泵至吸气箱出口5) Place a bag containing a test piece, prepared in the step 1, and connect it to the nitrogen introduction tube so that nitrogen gas can be introduced into the bag. See Fig. 3. 拿一个按照步骤1准备的盛有试样的袋子,将其连接至氮气传输管,于是氮气能够输入袋中。见图36) Before fitting the lid on the suction box, run the sampling pump to stabilize its operation with the flow rate set at 500m/min.在盖上吸气箱盖子之前,先运行收集泵使其稳定工作流动速率在500m/min.7) Connect the sampling pump to the outlet of the suction box, suck up 50.2 of air from the box (it takes approx.10 min) to introduce nitrogen gas in the same volume as the sucked-up air into the bag containing a test piece. Stop the pump, allowing it to be at rest for 2 min, take out the bag from the box and close the cock of the bag, if not provided with a cock, plug the Teflon tube opening. All bags including a blank bag shall undergo this procedure. 将收集泵与吸气箱出口相连,从箱中吸出50.2空气(大约耗时10分钟)导入与吸出空气等体积的氮气到盛有试样的袋中。停止泵的运行,让其静止2分钟,从箱中取出袋子并关闭带上的龙头,如袋上不带有龙头,就堵住特氟龙管的开口。所有袋子中包括一个空白袋,不进行该程序。Nitrogen gas (5) may be introduced into the bags each containing a test piece using an integrating flow meter instead of the suction box provided that impurities in nitrogen gas is sure to be eliminated by a activated carbon cartridge. 氮气(5升)可能导入袋中,每个袋中都盛有试样,使用集流仪器替代吸气箱,提供的氮气中杂质确保被活性炭滤筒清除。4.3 Preparation for Sampling 采样准备1) Connect the Teflon tube of a bag to the sampling pump. 将一个袋上的特氟龙管连接到收集泵2) Start the sampling pump operating (5) and adjust it to the specified flow rate. 开启收集泵工作使其稳定在指定的流动速率 (5) Sampling pump shall be brought into operation 30 min in advance. 收集泵需要提前运行30分钟3-a) Preparation for VOC (other than aldehydes) measurement : Regenerate TENAX tubes by baking them in advance at 250C for at least 6 hours (new tubes) or at least 2 hours (reused tubes). VOC(除了醛)测试准备:通过提前在250C烘焙至少6小时(新管)或至少2小时(再生管)来更新TENAX管。3-b) Preparation for aldehydes measurement : Take out DNPH-Silica cartridges in a necessary number from a refrigerator and leave them at room temperature at least 10 min before starting sampling operation so that they can become as warm as the room temperature. Immediately before measurement, take off a cartridge from the bag and cover the cartridge thoroughly with aluminum foil for shading except on the inlet and outlet ends.醛测试准备:从冷藏室内取出必须数量的DNPH-Silica滤筒,开启收集动作前将它们放置在室温下至少10分钟,这样它们可以变得与室温一样。在即将测试前,拿一个滤筒远离袋子,用铝箔彻底的覆盖滤筒,除了进口和出口端。4.4 VOC Emission and Collection (See Fig. 4.) VOC散发与采集(见图4)1) Place a bag containing a test piece or a blank-test bag, filled with 5 of nitrogen, in an oven heated preliminary to 65C, extend the Teflon tube of the bag through the hole in the top of the oven and make it secured there using a clip. 将已充满5升氮气,装有试样的袋子或空白袋子放置在预热到65C的烤箱内,延伸袋上的特氟龙管穿过烤箱顶部的洞口,并用夹子将其固定。2) Leave the bag in the oven kept at 65C for 2 hours to allow VOC to emit. 将袋子留在烤箱内保持65C 2小时来让VOC释放。3) Remove the plug from the Teflon tube secured on the top of the oven, connect the tube to one end of the TENAX tubes joined together in a row (6) and connect the other end to the sampling pump. Collect 1 of in-bag gas at a gas flow rate of 100 250m/min and another 1 of in-bag gas again at the same gas flow rate with new TENAX tubes in a row. 移除固定在烤箱顶端的特氟龙管堵头,将管子一端与TENAX管在一列上连接为一体,并将另一端与收集泵相连。在100 250m/min流动速率下收集1升袋内气体,再用新TENAX管在一列上收集1升袋内气体。 (6) To avoid VOC breakthrough, two TENAX tubes are connected in a row and the analysis results are reported as the total of the both tubes; however, a single tube may be used if the tube has proved to achieve a collection rate of 95% or higher. 为防止VOC透出,两个TENAX管连接成一列,分析结果记录为所有管子的总数,然而在已证明可以达到采集率95%或以上时也可用一个管子。4) Connect a DNPH cartridge to the Teflon tube leading from the bag and suck up all of the remaining gas (approx. 3) at a gas flow rate of 100 800m/min. Amount of the collected VOC can be calculated from the total amount of collected gas measured using the flow mater. 将DNPH滤筒连接至从袋子引出的特氟龙管,以100 800m/min流动速率吸净残留气体(大约3L)。VOC收集总量可以通过流量计测出的气体收集总量计算得出。5) On completion of sampling, pull off the inlet-side and outlet-side joints of the TENAX tube (or DNPH cartridge), cap the TENAX tubes (or DNPH cartridge). Analysis shall be made on the TENAX tube within 3 days after collection. DNPH cartridge shall be kept in a special bag and stored at 10C or lower until the analysis to be performed within 3 days. 采样完成,拉出TENAX管(或DNPH滤筒)的进口端和出口端接头。盖上TENAX管(或DNPH滤筒)。分析应该在收集后3天内进行。DNPH滤筒应存放在特制袋内,储存在10C或更低的温度下,直至分析在这3天内完成。5. COLLECTED GAS ANALYSIS AND REPORT 已收集气体分析与报告5.1 Quantitative Analysis of Aromatic Hydrocarbons Including Toluene 芳香烃中甲苯定量分析From the aromatic hydrocarbons collected in TENEX tubes, toluene, xylene, styrene, ethylbenzene and tetradecan shall be isolated and subjected to quantitative analysis respectively using a gas chromatograph mass spectrometer (GC-MS) having a heating device for desorption. Analysis shall be performed in accordance with Determination of the emission of volatile organic compounds and aldehydes for building products small chamber method (JIS A 1901), ISO 16017-1 and ISO/DIS16000-6. 从TENEX采集的芳香烃,甲苯,二甲苯,苯乙烯,乙苯以及十四烷应隔离分类,使用带有加热分离装置的“气体套色聚集分光计(GC-MS)”分别进行定量分析。分析将按照“建筑产品挥发性有机化合物和醛发散的决定小房间方法(JIS A 1901)”,ISO 16017-1以及ISO/DIS16000-6。Note) Amount of xylene may be represented as the total of the isomers, the amounts of individual isomers are not required. 注意)二甲苯含量可以代表异构体的总量,特殊异构体数量不是必须的。5.2 Quantitative Analysis of Aldehydes 醛的定量分析 Aldehydes collected in the DNPH cartridge are in the form of aldehydeDNPH compounds. The compounds shall be extracted by acetonitrile and the volume of the compounds in the acetonitrile solution shall be exactly diluted to 5ml and then formaldehyde and acetoaldehyde are isolated and subjected to quantitative analysis respectively using the high performance liquid chromatography. Analysis shall be performed in accordance with Determination of the emission of volatile organic compounds and aldehydes for building products small chamber method (JIS A 1901) and ISO/DIS16000-3.滤筒中收集的醛是醛-DNPH化合物形式的。这种化合物可以用氰化甲烷萃取,这种化合物在氰化甲烷溶剂中的量可以精确稀释到5ml,然后甲醛和乙醛被隔离分类,分别使用高性能液体套色板进行定量分析。分析将按照“建筑产品挥发性有机化合物和醛发散的决定小房间方法(JIS A 1901)” 以及ISO/DIS16000-3。5.3 Analysis Report分析报告The concentration of a volatile organic compound shall be calculated according to the following formula : 挥发性有机化合物浓度应按照以下公式计算:When two different results are obtained from two specimens (n = 2) in the collection using TENAX tubes, the higher value shall be reported as the amount emitted from a test piece, 100cm 2 in size (g / a 100-cm 2 test piece).The results of VOC collection from test pieces less than 100cm 2 or entire assemblies shall be reported as the amount emitted from a test piece (g / a test piece). 用TENAX管采集得,两个不同结果从两个样品(n=2)获得,较高值应作为试样的释放量报告,试样大小100 cm 2(g / a 100-cm 2 试样)。从小于100cm 2或整个试样采集的VOC结果应按试样(g / a 试样)释放量报告。For the parts disassembled into pieces as described in Sec. 3.2, the analysis shall be performed on each of the pieces

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