空气中邻氯苯乙烯的气相色谱快速测定法

目的 建立应急快速检测空气中邻氯苯乙烯气相色谱测定方法.方法 用注射器采集工作场所空气中的邻氯苯乙烯,直接进样,经30 m×0.53 mm×0.25μm FFAP毛细管色潜柱分离,氢火焰离子化检测器检测.结果 本方法 在0～1200 μg/L范围呈线性关系;样品在注射器中可保存5 h;方法 的重现性好,不同浓度的相对标准偏差为1.28%～1.97%;回归方程式为Y=1403 0+7207X,r=0.9999.方法 的最低检出浓度为5.2 mg/m3;空气中与邻氯苯乙烯共存的苯乙烯、对氯苯乙烯、间氯苯乙烯等在本方法 条件下不干扰测定.结论 该方法 各项指标均达到GBZ/T 210.4-2008<职业卫生标准制定指南第四部分:工作场所空气中化学物质检测方法 >的要求,适用于工作场所空气中邻氯苯乙烯的现场监测.

Abstract：

Objective To establish a rapid gas chromatographic method for determination of ochlorostyrene in the air of workplace. Method The air samples were collected by syringes, injected directly to the GC system, and then separated by a FFAP capillary column (30 m×0.53 mm×0.25 μm ), finally determined by a Flame Ionization Detector. Results A good linear correlation was showed within a range of 0～ 1200 μg/L,with regression formula Y= 14 030+7 207X(r=0.999 9 ). The air sample could be stably stored in the syringe for 5 hrs. The relative standard deviation (RSD) of repeated injection of o-chlorostyrene standard solutions at three different concentration by six times was 1.28%～1.97%. The minimun detectable concentration was calculated to be 5.2 mg/m3. Other coexistent volative organic compounds such as styrene, p-chlorostyrene, and m-chlorostyrene didn't interfere with the determination under the experimental conditions of this method.Conclusion This method meets the requirement of "Guide for establishing occupational health standardsPart 4: Determination methods of air chemicals in workplace". It is applicable for determination of oChlorostyrene in the air of workplace.     

工作场所空气中三氯氧磷的离子色谱测定法

目的 建立工作场所空气中三氯氧磷(POCl3)的离子色谱测定方法.方法 工作场所空气中的三氯氧磷用吸收液吸收后成为盐酸,用色谱柱分离、电导检测器检测,保留时间定性、峰高或峰面积定量.结果 三氯氧磷在0.72～5.76 μg/ml范围内呈线性关系,相关系数为0.9999;方法 的检出限为0.12μg/ml.当采样体积为15 L时,工作场所空气中三氯氧磷的最低检出浓度为0.08 mg/m3.不同浓度的三氯氧磷相对标准偏差为3.3%～6.2%,回收率为97.8%～103.8%.样品在室温下至少可保存7d.结论 该方法 各指标符合GBZ/T 210.4-2008<职业卫生标准制定指南第4部分工作场所空气中化学物质测定方法 >的要求,适用于工作场所空气中三氯氧磷的检测.

Abstract：

Objective To establish a ion chromatography method for determination of phosphorus oxychloride in the air of workplace. Method The phosphorus oxychloride in the air of workplace was collected by absorb liquid and turned into hydrochloric acid, then separated in column and detected with conductivity detector, qualified by elution time and quantified by peak height or peak area. Results The linear range of phosphorus oxychloride in air of workplace was 0.72～5.76 μg/ml with its correlation coefficient 0.9999. The detecting limit of the method was 0.12 μg/ml. The smallest detecting concentration of the method was 0.08 mg/m3 for 15 L sampling air. Relative standard deviation was 3.3%～6.2% and the recovery was 97.8%～ 103.8%.The sample could be resaved at room temperature at least for seven days. Conclusion The indicators of the method correspond GBZ/T 210.4-2008. It is a good method to determine phosphorus oxychloride in the air of workplace.     

工作场所空气中二硼烷的等离子体发射光谱测定

目的 建立工作场所空气中二硼烷的样品采集及测定方法.方法 工作场所空气中的二硼烷用氧化剂浸渍活性炭管采集.采用体积分数为3%的H2O2解吸,采用等离子体发射光谱(ICP-AES)方法对溶液中硼进行定量.结果 本方法采样效率为99.6%,二硼烷5.66μg和56.6μg加标水平的解吸效率分别为90.9%和99.5%,批内和批间精密度相对标准偏差均小于8.0%.标准曲线范围0.1～10.0 μg/ml(以硼含量计),该方法空气中的二硼烷的最低检出浓度为0.011 mg/m3(以采集15 L空气样品计),最低检出浓度为0.035 mg/m3(以采集15 L空气样品计).结论 该方法适用于工作场所空气中二硼烷的采集及浓度测定.

Abstract：

Objective A sampling method was established to collect diborane in the air of workplace and an ICP-AES method was developed to determine the Boron in desorbed solution.Method Diborane in the air of workplace was collected by solid sorbent tube filled with oxidant impregnated activated carbon.The adsorbed diborane was desorbed into 3% H2O2 aqueous,and then the desorbed Boron was determined by ICP-AES.Results The sampling efficiency of this method was 99.6% with the desorption efficiency of diborane with 5.660 μg and 56.6 μg spiked were 90.9% and 99.5%,respectively.Both the intra-and inter-precision RSD were less than 8%.The standard curve of this method ranged from 0.1 to 10.0 μg/ml (Boron),and the LOD and LOQ were 0.011 mg/m3 and 0.035 mg/m3 (15L samples) respectively.Conclusion The method established was suitable for diborane sampling and determination in the air of workplace     

工作场所空气中氢化锗的原子荧光测定法

目的 建立工作场所空气中氢化锗原子荧光测定方法.方法 活性炭管采样,硝酸解吸过滤,原子荧光光谱仪检测.结果 浓度在0.85～300.00 μg/L范围内线性关系良好,相关系数r=0.9993;最低检出限和最低检出浓度为0.51 μg/L和0.000 17 mg/m3(以采集48 L空气样品计),加标回收率为90%～106%;用相对标准偏差表示批内精密度为3.3%～5.9%,批间精密度为3.7%～6.3%.结论 该方法线性范围宽,灵敏度高,精密度好,适用于工作场所空气中氢化锗的测定.

Abstract：

Objective An atomic fluorescence (AFS) method was developed to determine germanium hydride in the air of workplace.Method Germanium hydride in the air of workplace was collected by charcoal tube,and desorbed by nitric acid followed filtration with 0.22 μm cellulose filter,the AFS was used to determine Germanium in the desorbed solution.Results The linear was good at the range of 0.85～300 μg/L with the correlation coefficient of 0.9993;the LOD and LOQ were 0.51 μg/L and 0.000 17 mg/m3,respectively.The recovery was ranged from 90% to 106%,the RSD of intra- and inter- precision were 3.3%～5.9% and 3.7%～ 6.3%.Conclusion The linear range,sensitivity and precision of the method were all satisfied for the determination of germanium hydride in the air of workplace.     

工作场所空气中磷酸的离子色谱测定法

目的 建立工作场所空气中磷酸的离子色谱测定法.方法 空气中磷酸经微孔滤膜采集后,用去离子水洗脱,经色谱柱分离,电导检测器检测,用离子色谱法进行分离测定,保留时间定性,峰高或峰面积定量.结果 方法 线性范围为0～20 μg/ml,相对标准偏差(RSD)为1.95%～3.31%,洗脱效率为103.0%～109.6%,最低检出限为0.1 μg/ml(进样量20.0μl),若采集75 L空气进行测定,最低检出浓度为0.01 mg/m3.结论 该方法 采样方便,样品处理简单,灵敏度高,可靠性好,试验过程不需化学试剂,对环境无污染,可用于工作场所空气中磷酸的检测.

Abstract：

Objective To develop a method to determin phosphoric acid in the air of workplace by ion chromatography. Methods Phosphoric acid was collected by millipore filter and washed by deionized water then detected by ion chromatography. Results Linearity range of test was 0～20 μg/ml, relelive standard deviation (RSD) was 1.95%～3.31%, the elution efficiency was 103.0%～ 109.6%, determination limit was 0.1 μg/ml (when sample size was 20.01 ), concentration limit was 0.01 mg/m3(when the collected air was 75 L).Conclusion This method is convenient for air collection, simple, with high sensitivity and good precision, is a good method for determination of phosphoric acid in the air of workplace.     

空气中四种羧酸的同时测定

目的 建立工作场所空气中乙酸、丙酸、丙烯酸及甲基丙烯酸4种羧酸同时测定的毛细管柱气相色谱方法.方法 硅胶管吸附空气中乙酸、丙酸、丙烯酸及甲基丙烯酸,用丙酮解吸后毛细管柱气相色谱(FID)测定.结果 乙酸、丙酸、丙烯酸及甲基丙烯酸浓度分别在3.4～500.0、2.1～500.0、2.9～500.0及1.6～500.0 μg/ml范围内线性关系良好;线性方程分别为:y=-4.3+1.46x(r=0.999);y=0.4+2.37x(r=0.999);y=10.4+1.73x(r=0.999);y=-2.3+3.21x(r=0.999);检出限分别为3.4、2.1、2.9及1.6 μg/ml.若采集15 L空气样品,最低检出浓度分别为0.2、0.1、0.2及0.1 mg/m3;平均解吸效率分别为92.2%～92.8%、94.1%～97.4%、94.8%～95.4%及94.1%～98.3%;相对标准偏差分别为1.1%～4.0%、1.2%～7.8%、0.9%～4.0%及1.6%～4.8%.结论 本方法适用于工作场所空气中4种羧酸浓度的同时测定.

Abstract：

Objective Four kinds of acids (acetic acid,propionic acid,acrylic acid and methylacrylic acid) in the air in a workplace were quantitatively determined by gas chromatography synchronously.Methods Four acids in the air were adsorbed by silica gel tube sampling and solvent desorption using acetone,then analyzed by GC with FFAP capillary column.Results To acetic acid,propionic acid,acrylic acid and methylacrylic acid,the linear regression equations were respectively y=-4.3+1.46x (r=0.999),y=0.4+2.37x(r= 0.999),y=10.4+1.73x(r=0.999) and y=-2.3+3.21x(r=0.999).The detection limits were respectively 3.4μg/mL,2.1 μg/mL,2.9 μg/mL and 1.6 μg/mL.The average desorption efficiencies were respectively 92.2%~92.8%,94.1%～97.4%,94.8%～95.4% and 94.1%～98.3%.The relative standard deviations were 1.1%～4.0%,1.2%～ 7.8%,0.9%～4.0% and 1.6%~4.8%.Conclusion The method is suitable to determine four kinds of acids in the air in a workplace.     

工作场所空气中二苯胺的紫外分光光度测定法

目的 建立工作场所空气中二苯胺的紫外分光光度测定法.方法 用硫酸处理过的玻璃纤维滤膜采集空气中二苯胺,无水乙醇解吸后紫外分光光度法测定.结果 该方法的线性范围为0.19～60 mg/m~3(以采集15 L空气计算),回归方程y=0.13x-0.016,相关系数为0.9999,检出限0.28μg/ml(以吸光度为0.02计算),精密度为1.9%～8.4%,平均采样效率99%,平均洗脱效率为98%,穿透容量大于2.2 mg,样品在室温或冷藏条件均至少可保存10 d.结论 该方法适用于工作场所空气中二苯胺的测定.

Abstract：

Objective To establish a UV spectrophotometry method for determination of diphenylamine in air of workplaces.Methods The air samples were collected by glass fiber filter treated with sulfuric acid,desorbed with alcohol by ultrasonic for 10min,determined by UV spectrophotometry.Results The detection range of the method was 0.19-60 mg/m~3 (the air volume was15L).The regression equation:y=0.13x-0.016.The correlation coefficients was 0.999 9.The detection limit was 0.28μg/ml.The relative standard deviations was 1.9%-8.4%.Sample-collected efficiency was 99%,desorotion efficiency was 98%and the penetration capacitv was more than 2.2 mg.Sample stability was 10 days at least by being stored in a refrigerator at 4℃or by ambient storage.Conclusion This method is applicable to the determination of diphenylamine in air of workplaces.     

水中氰化物的安培检测-离子色谱测定法

目的 建立水中氰化物的安培检测-离子色谱方法.方法 以0.1 mol/L氢氧化钠与10%(V/V)丙酮作淋洗液,用离子色谱进行样品分离,外标法定量,并实验了7种常见阴阳离子、2种电化学活性物质对氰化物测定的影响.结果 线性范围为0.05～100μg/L,回归方程为y=0.020 3x+6.173 7,相关系数为0.999 1,RSD<10%,样品的加标回收率为97.0%～102.1%,检出限为0.05μg/L.结论 该方法快速、准确、安全,可用于水中氰化物测定.

Abstract：

Objective A method was developed for the determination of cyanide in water by ion chromatography with direct amperometric detection.Methods The eluent used was 0.1 mol/L NaOH and 10%(V/V) acetone.The samples were analyzed by using ion chromatography as well as external standard curve.The effects of 7 common ions,2 electrochemical active substances on the determination of cyanide were studied.Results The linear range of the method was 0.05-100 μg/L and the correlation coefficient was 0.999 1.The RSD was<10%.The rates of recovery were 97.0%-102.1%and the detection limit was 0.05μg/L,There was no significance between the determining results of samples with ion chromatography and those with isonicotinic acidpyrazolone colorimetric method.Conclusion The method was rapid,accuracy and security,and it can be used for the detection of trace cyanide in water.     

尿中四氢呋喃的顶空固相微萃取-气相色谱测定法

目的 建立测定尿中四氢呋喃的顶空固相微萃取-气相色谱法.方法 以顶空固相微萃取技术处理尿样,用带氢焰离子化检测器的气相色谱仪测定尿中的四氢呋喃.通过对萃取头类型、萃取时间和温度、解吸温度和时间等影响萃取效率的因素的研究,获得了优化的试验条件.结果 在优化条件下,方法 的线性较好,样品的加标回收率为93.0%～100.8%,相对标准偏差为0.96%～3.85%,检出限可以达到0.5μg/L.结论 该方法 适用于尿中四氢呋喃的测定.

Abstract：

Objective Headspace solid-phase microextraction (HS-SPME) was used pre-concentration procedure for the determination of tetrahydrofuran in urine by gas chromatography with hydrogen flame detector. Methods Several parameters controlling SPME was studied and optimised: SPME fiber, extraction time and extraction temperature, desorption time and desorption temperature. Results Under optimal conditions, the correlation coefficient was 0.9998 and good recoveries (range from 93.0%～100.8%) were achieved,the detection limit was 0.5μg/L. Conclusion The method can be applied to the determination of trace amount of tetrahydrofuran in urine.     

某矿井及选煤厂煤尘作业场所现状调查

Objective through a detection of dust in the coal mines workplace, to understand the status of occupational hazards, and the evaluation of occupational hazards, provide subject to control occupational hazards. Method according to production process and "hazardous substances in workplace air monitoring, sampling norms" and other standards to determine the sampling points and sampling of coal dust.Result underground mining operations in 21 subjects with time-weighted average concentration of dust types pass rate of 28.6%, of which five types of dust hazard grade Ⅱ, six types of dust hazard rating of 0, and the remaining types of grade Ⅰ dust hazard levels. Coal dust test six types of time-weighted average concentration of 83.3% pass rate, only one types of dust hazard grade Ⅰ, all the rest is 0. Calculated by the detection of dust overrun 18 times operating sites, the pass rate of 72.2% results. Conclusion purified water spray and air flow curtain of dust control has played a certain role, but the work of underground working conditions and environmental constraints, most of the dust concentration in workplace occupational exposure limits do not meet the requirements, recommended the strengthening of dust or Dust the daily management and maintenance of equipment, strengthen the ventilation, personal protection officers to strengthen operations.     

工作场所空气中13种卤代烃的溶剂解析气相色谱同时测定法

目的建立溶剂解析毛细管气相色谱法同时测定工作场所空气中13种卤代烃的测定方法。方法采用活性炭吸附管采集空气中的卤代烃,用CS2进行解吸,经FFAP毛细管色谱柱分离,氢火焰离子化检测器(FID)检测。结果方法可同时分离测定空气中的13种卤代烃,相关系数均可达0.999以上,精密度在0.91%～1.55%之间,加标回收率在88.8%～111.9%之间。结论该研究所建立的方法灵敏度高、精密度好,准确,适用于同时检测工作场所空气中的多种卤代烃。     

八通阀气体进样-气相色谱法测定作业场所空气中的芳香烃类化合物

目的:建立作业场所空气中多种芳香烃类化合物的八通阀气体进样-气相色谱法。方法:作业场所空气样品经热解吸后,使用八通阀气体进样,DB-1毛细管色谱柱分离,火焰离子化检测器检测。结果:在选定的实验条件下,各化合物的保留时间重复性和面积重复性的相对标准偏差分别小于0.2%和3.0%(n=6)。结论:本法适合于作业场所空气中多种芳香烃类化合物的测定。     

工作场所空气中甲基环己烷的气相色谱测定方法

目的 建立工作场所空气中甲基环己烷的气相色谱测定方法。方法 《车间空气监测检验方法》研究规范的要求进行实验室实验及现场实验。结果 100mg活性碳对甲基环己烷的穿透容量大于15．05mg，当甲基环巳烷的浓度为21．7－127．0mg/m^3时，采样效率均达99．64％－100．00％；样品在碳管中至少可保存8d，方法的重现性好，不同浓度的相对标准偏差（RSD）为4．4％－8．4％；平均解吸效率为91．8％－96．．6％；方法的最低检测浓度为0．13mg/m^3；空气中与甲基环巳烷共存的苯、甲苯、正巳烷、正庚烷等在本方法条件下不干扰测定。结论 此方法各项指标达到《车间空气监测检验方法》研究规范的要求，适用于工作场所空气中甲基环己烷的现场监测。     

工作场所空气中二氯甲烷的溶剂解吸—气相色谱测定法

目的建立溶剂解吸—气相色谱测定工作场所空气中二氯甲烷的检测方法。方法采用溶剂解吸型活性炭管进行采样,二硫化碳解吸,毛细管柱进行分离,氢焰离子化检测器检测,保留时间定性,峰高或峰面积定量。依据"工作场所空气中毒物检则方法的研究规范"的要求,对方法进行实验室研究验证。结果在样品测定条件下,标准曲线线性范围在25～4000μg/ml之间,相关系数在0.999以上;检出限为1.2μg/ml;相对标准偏差(RSD)在1.87%～4.36%之间;加标回收率在98.5%～99.2%之间;采样效率在91.0%～97.6%之间;穿透容量大于2.0 mg;平均解吸效率为90.3%;样品在室温下至少可保留7 d。结论该方法各项实验室验证指标均符合"《工作场所空气中毒物检测方法的研究规范(原WS/T73-1996)》"的要求,经过在检测与评价工作中应用,证实该方法可以用于工作场所空气中有毒物质二氯甲烷的测定。     

作业场所空气中乙醚的溶剂解吸气相色谱法研究

目的:建立作业场所空气中乙醚的溶剂解吸气相色谱测定方法。方法:用溶剂解吸型活性炭管采样空气中的乙醚,二硫化碳解吸,经DB-FFAP毛细管色谱柱分离,FID检测器测定。结果:乙醚在0μg/ml～3408μg/ml呈良好的线性关系,线性相关系数为0.99998,方法检出限为1.36μg/ml,相对标准偏差0.24%～4.9%,解吸效率为84%～92%,采样效率为100%,加标回收率在97%～99%,穿透容量为2.9 mg,在4℃冰箱中样品至少可稳定10 d。结论:该方法各项指标均能达到《工作场所空气中毒物检测方法研究规范》的要求,现场应用试验也得到了相符性结论。该方法适用于工作场所空气中乙醚的检测。     

空气中苯系物及卤代烷烃化合物的毛细管气相色谱测定法

目的 探讨二硫化碳解吸-毛细管气相色谱法测定工作场所空气中苯系物及卤代烷烃的检测方法.方法 工作场所空气中的苯系物及卤代烷烃经活性炭管采集,二硫化碳解吸后,注入带氢火焰离子化检测器(FID)的气相色谱仪进行分析,以保留时间定性,峰面积定量.结果 苯、甲苯、对二甲苯、间二甲苯、邻二甲苯、乙苯、苯乙烯、四氯化碳、三氯甲烷、1,2-二氯乙烷的线性范围分别为0.019～81.600、0.018～91.200、0.018～88.800、0.018～56.800、0.011～92.000、0.012～63.200、0.018～93.200、0.449～2 298.400、0.252～1 287.000、0.076～390.000 mg/m3,回收率为88.4%～98.1%,RSD为1.0%～6.0%.结论 该方法能够有效分离和准确测定空气中苯系物及卤代烷烃化合物,具有较好的精密度与准确度,适合现场空气中该类化合物的测定.     

工作场所空气中28种挥发性有机物的气相色谱快速测定法

目的建立工作场所空气中28种挥发性有机物的快速测定方法。方法用活性炭采集工作场所空气中挥发性有机物,经二硫化碳解析后用毛细管气相色谱法测定。结果 28种挥发性有机物在一定浓度范围内线性关系良好,相关系数r>0.995,相对标准偏差为0.4%～6.5%,最低检出限远低于职业化学中毒现场剂量水平,目标组分平均解吸效率在77.3%～105.8%。结论方法准确度高,操作简便,灵敏快速,适用于工作场所空气中挥发性有机物的快速测定。     

工作场所空气中4种丙烯酸酯类化合物的气相色谱同时测定法

目的建立工作场所空气中丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸甲酯、丙烯酸丁酯的气相色谱测定方法。方法采用活性炭管采集,二硫化碳解吸,经HP-FFAP毛细管柱分离,氢火焰离子化检测器检测,GC标准曲线法定量。结果4种丙烯酸酯类化合物分离完全,线性、重现性良好,方法检出限为0．16～0．27wg／ml。以1．5L的采样量计算空气中的浓度为0．11～0．18mg／m^3。结论方法准确、灵敏,适用于工作场所空气中多种丙烯酸酯类化合物的测定。