Standard Test Method for Analysis of Toluene by Capillary Column Gas Chromatography1 | （毛细柱）气相谱法检测甲苯 |
4. Summary of Test Method 4.1 A portion of the sample is injected into a gas chromatograph using a microlitre syringe at the specified conditions of the test method. The toluene and other components are separated as they are transported through the column by an inert carrier gas. The components in the effluent are measured by a flame ionization detector (FID). The area of the impurity peaks and toluene are electronically integrated. The peak areas are corrected with effective carbon number (ECN)4 response factors and normalized to 100.0000 %. | 4. 检验方法综述 |
5. Significance and Use 5.1 This test method is suitable for determining the concentrations of known impurities in refined toluene and for use as an integral quality control tool where toluene is produced or used in manufacturing. 5.2 Toluene purity is reported, but a chromatographic analysis cannot determine absolute purity if unknown or undetected components are present in the sample. | 5. 意义和应用 5.1本试验方法适用于测定精制甲苯中已知杂质的浓度，作为生产或生产甲苯的整体质量控制工具。 5.2甲苯纯度报告，但如果样品中存在未知或未检测到的成分，谱分析不能确定绝对纯度。 |
6. Interferences 6.1 If present, nonaromatic hydrocarbons of 13 carbons or greater, alcohols, ethers, and other similar organic compounds can interfere with this test method by co-eluting with the aromatic hydrocarbons. 6.2 Compounds not detected by a FID are not determined by this test method. 6.3 Nonvolatile material is not determined. | 6. 干扰因素 6.1如果存在13个碳或以上的非芳香烃，醇类、醚类和其他类似的有机化合物可以通过与芳香烃共洗脱来干扰本试验方法。 6.2 不能通过FID检测的组分无法用本检测方法检测 6.3 非挥发性物质不能用本方法检测 |
7. Apparatus 7.1 Gas Chromatograph (GC)—any GC built for capillary column chromatography. The system shall have sufficient sensitivity, linearity, and range to obtain a minimum peak height response for 0.0010 wt % impurity of twice the height of the signal background noise, while not exceeding the full scale of either the detector or the electronic integration for the major component. It shall have a split injection system that will not discriminate over the boiling range of the samples analyzed. The system should be capable of operating at conditions given in Table 1. | 7. 仪器设备 7.1 气相谱仪 系统应该具有足够的灵敏度线性和检测范围，最小能检测杂质为0.0010%（该限度的杂质至少满足峰高是噪音的2倍）。主峰的峰高在仪器的检测范围内。任何沸点范围的化合物都可以使用仪器的分流进样系统。 系统按照表一进行设定 |
TABLE 1 Typical Instrumental Parameters | 表一 仪器参数 | |||||||||
Detector: Detector temperature, °C Column: Tubing Stationary phase Film thickness, μm Column temperature, °C Carrier Gas Linear velocity at 70°C, Inlet: Injection port temperature, °C Split ratio Split flow, mL/min Sample size, μL | Flame ionization 150°C 50 m by 0.25 mm Fused silica TCEP 0.40 70 Helium cm/s 25 Split 150°C 40 55 1.0 | 检测器 检测器温度°C 谱柱 管 固定相 膜厚度μm 柱温°C 载气 70℃线速率 进样 进样口温度°C 分流比 分流流速mL/min 样品量μL | FID 150°C 50 m by 0.25 mm 熔融石英管 TCEP 0.40 70 Helium cm/s 25 Split 150°C 40 55 1.0 | |||||||
7.2 Recorder—electronic integration is recommended. 7.3 Capillary Column—fused silica capillary column with 1,2,3-tris-2-cyano-ethoxypropane (TCEP) phase is recommended. Polyethylene glycol (PEG) columns have been successfully used. Other columns may be used after it has been established that such a column is capable of separating all major impurities under operating conditions appropriate for the column. 7.4 Microsyringe—capable of delivering 1 μL of sample. | 7.2 记录仪 7.3 毛细管柱：TCEP固定相的石英柱或者PEG谱柱。如果可以确认其他谱柱在适当条件下能够分离主要杂质，也可以应用。 7.4 微量进样器：能够进1uL的样品。 | |||||||||
8. Reagents 8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. It is intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society,5 where such specifications are available, unless otherwise indicated. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 8.2 Carrier Gas—Helium, 99.99 mole % minimum, is recommended. 8.3 FID Detector Gases: 8.3.1 Hydrogen—99.99 mole % minimum. 8.3.2 Air—less than 10 ppm each of total hydrocarbons and water. | 8. 试剂 8.1 试剂纯度：试剂级别的化学品可以用于检测。除另有说明外，所有试剂均应符合ACS5的规范。如果使用其他等级的试剂，需要保证其纯度不会影响检测的准确度。 8.2 载气：高纯度氦气（99.99%） 8.3 FID检测器气体 8.3.1 氢气：99.99%以上 8.3.2 空气：总烃和水不超过10ppm | |||||||||
9. Hazards 9.1 Consult current OSHA regulations, suppliers’ Material Safety Data Sheets, and local regulations for all materials used in this test method. | 9.风险 9.1请参阅现行的OSHA法规、供应商的材料安全数据表以及涵盖本测试方法中使用的所有材料的当地法规。 | |||||||||
10. Sample Handling 10.1 Collect the samples in accordance with Practice D3437. 10.2 To preserve sample integrity (consistency) and prevent the loss of volatile components, which may be in some samples, do not uncover samples any longer than necessary. | 10. 样品处理 10.1按照D3437惯例采集样品。 10.2 为了保证样品检测完整有效，避免损失组分，检测时间应该足够长，保证所有组分均被检测。 | |||||||||
11. Preparation of Apparatus 11.1 Follow the manufacturer’s instructions for mounting and conditioning the column in the chromatograph. 11.2 Adjust the instrument to the conditions as described in Table 1 to give the proper separations. Allow sufficient time for the instrument to reach equilibrium as indicated by a stable baseline. See Practices E355 and E1510 for additional information on gas chromatography practices and terminology. | 11. 仪器准备 11.1 依据生产说明书装配仪器，配置谱条件。 11.2 按照表一进行仪器参数设定，预热平衡仪器至基线平稳。更多信息参见E355 和E1510 关于谱方法和术语的记录。 | |||||||||
12. Procedure 12.1 Inject an appropriate amount of specimen, typically 1.0 μL, into the chromatograph. A low purity toluene sample chromatogram, which shows the relative retention time of components typically found in commercial toluene, is illustrated in Fig. 1. NOTE 1—Since TCEP is a nonbonded phase, significant retention time shifts can occur with column condition. 12.2 Measure the area of all peaks. The nonaromatics fraction includes all peaks eluting before benzene. Sum together all nonaromatic peaks and report as a total area. | 12 规程 12.1 注入适当量的样品，通常为1.0uL。图一之中是一个低纯度的甲苯样品图片，标示了（市售）甲苯相应的组分的保留时间。 Note1：TCEP是一种非键合固定相，因此保留时间会因为谱条件改变而漂移。 12.2 测量所有的峰面积，所有的非芳香烃组分在苯前被洗脱，将其合并为一个峰报告结果。 | |||||||||
13. Calculation 13.1 Using the ECN weight response factors listed in Table70 2, calculate the concentration of each component as follows: where: Ci = concentration results for component(s) i, weight %, Ai = peak area of component(s) i, and Ri = ECN response factor for component(s) i. 13.2 Calculate the volume percent concentration of each component using the density in Table 2 as follow: where: Vi = calculated vol% concentration of component i Ci = calculated wt% concentration of component(s) i, from 13.1, and Di = density of component i | 13.计算 smdao13.1 利用表2中的ECN权重银子，计算所有组分的含量： 其中： Ci = 组分的含量 %, 212资源Ai = 组分峰面积 Ri = 组分的ECN权重因子 13.2 使用表二计算每个组分的体积百分含量 其中 Vi = 计算组分的体积百分含量vol% Ci = 自13.1计算得到的组分的质量百分含量wt% Di = 组分密度 | |||||||||
Table 2表2 ECN 权重参数和密度 | ||||||||||
组分 | ECN权重参数 | 密度（20℃） | ||||||||
Non aromatics: Benzene Toluene Ethylbenzene p-Xylene m-Xylene o-Xylene Cumene 1,4-Dioxane | 非芳香烃组分 苯 甲苯 乙苯 对二甲苯 间二甲苯 邻二甲苯 异丙基苯 1,4-二氧六环 | 1.0000 0.9100 0.9200 0.9275 0.9275 0.9275 0.9275 0.9333 3.0800 | 0.7255 0.8780 0.8658 0.8658 0.8597 0.8630 0.8786 0.8605 1.0329 | |||||||
14. Report 14.1 Report the following information: 14.1.1 Report impurity concentrations less than 0.0005 % as <0.0005 %. 14.1.2 Report greater than 0.0005 % each of the nonaromatics, benzene, ethylbenzene, xylenes, and cumene to the nearest 0.0001 %. 14.1.3 Report toluene purity to the nearest 0.01 %. | 14.报告 14.1 报告下列信息 14.1.1 报告杂质含量低于0.0005%为＜0.0005% 14.1.2 报告高于0.0005%的杂质（非芳香烃组分、苯、乙苯、二甲苯、异丙基苯）精确到0.0001%。 14.1.3 报告甲苯纯度精确到0.01% | |||||||||
15. Precision and Bias 15.1 Precision—The following criteria should be used to judge the acceptability of results obtained by this test method (95 % confidence level). The precision criteria were derived from six laboratories performing three analyses on three standards over a two-day period. The results of the precision study were calculated using Practice E691. 15.1.1 Intermediate Precision (formerly called Repeatability)—Duplicated results obtained on the same sample in the same laboratory by the same operator on the same instrument should not be considered suspect unless they differ by more than the intermediate precision value shown in Table 3. 15.1.2 Reproducibility—Duplicated results obtained on the same sample by different laboratories, with different operators, different instruments, and at different times should not differ by more than the reproducibility value listed in Table 3. 15.1.3 Bias—Systematic deviation of the method average value or the measured value from an accepted reference value. Since the absolute purity of the toluene solvent could not be determined, an absolute statement of bias could not be determined from this study. An estimate of bias was made by preparing three gravimetric standards with three different concentrations of impurities. The standards were then analyzed as unknowns in the interlaboratory study (see Table 4). | 15. 精密度和偏差 15.1 精密度：以下标准是用于评估检验方法得到的结果的可接受度（95%置信区间）。精确标准来自六个实验室，在两天内对三个标准进行了三次分析。用E691方法计算了精度研究的结果。 15.1.1 中间精密度(可重复性)： 在同一实验室同一家实验室的相同样本上获得的重复结果。同样的仪器中间精密度结果应满足表3规定。 15.1.2 再现性：不同的实验室、不同的操作人员、不同的仪器、不同的时间在同一样本上获得的重复结果，满足表三的相应规定。 15.1.3 偏差：方法的系统偏差平均值或测量值是一个重要的参考值。 由于甲苯溶剂的绝对纯度不能确定，因此不能从这项研究中确定绝对偏差。通过制备三种不同浓度杂质的重量标准对偏差进行了估计。然后在实验室间的研究中将这些标准作为未知数进行分析(见表4)。 | |||||||||
表3 中间精密度&再现性 | 表4 预计偏差 | |||||||||
实际含量（重量%） | 中间精密度 | 再现性 | 诺基亚cdma实际含量（重量%） | 平均值 | 偏差 | |||||
Non aromatics | Non aromatics | |||||||||
STD #1 | 降温母粒 1.6314 | 0.0078 | 0.2024 | STD #1 | 机票查询接口1.6314 | 1.6404 | -0.0090 | |||
STD #2 | 0.9718 | 0.0039 | 0.1243 | STD #2 | 0.9718 | 0.9854 | -0.0136 | |||
STD #3 | 0.0207 | 0.0022 | 0.0081 | STD #3 | 0.0207 | 0.0254 | -0.0047 | |||
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