固相萃取-高效液相色谱法测定水中微囊藻毒素质量控制指标研究

采用固相萃取－液相色谱法，通过统计全国多家实验室的测定数据，对水中微囊藻毒素测试的平行样测定相对偏差、空白加标回收率、实际样品加标回收率、空白加标回收率平行样相对偏差以及样品加标回收率平行样相对偏差5个质控指标进行了研究，并给出了质控指标评价标准，提出在概率P和γ均为0.90时，其平行样测定允许最大相对偏差应控制在7.3%；空白加标质量浓度为0.005~20 μg/L时，回收率的控制范围为61%~125%；样品测定浓度为未检出、加标质量浓度在0.2~3.6 μg/L时，实际样品加标回收率控制范围为66%~108%；空白加标、样品加标回收率平行样最大相对偏差应分别控制在3.9%和8.9%。在概率P和γ均为0.95时，其平行样测定允许最大相对偏差应控制在8.3%；空白加标质量浓度为0.005~20 μg/L时，回收率的控制范围为49%~137%；样品测定浓度为未检出、加标质量浓度在0.2~3.6 μg/L时，实际样品加标回收率控制范围为60%~114%；空白加标、样品加标回收率平行样最大相对偏差应分别控制在5.2% 和14.8%。     

超高效液相色谱-串联质谱法分析土壤及沉积物中氨基甲酸酯农药

利用超高效液相色谱-串联质谱,建立土壤和沉积物中痕量氨基甲酸酯农药的分析方法。该方法用体积比1:1的二氯甲烷/甲醇对土壤和沉积物样品进行加速溶剂萃取,GCB/PSA固相萃取小柱对萃取液进行净化,内标法定量,用超高效液相色谱-串联质谱法分析土壤和沉积物中20种氨基甲酸酯农药。20种氨基甲酸酯农药在0.02~1.0 μg/mL范围内线性良好(r≥0.99),检测限为0.20~0.60 ng/g。沉积物加标样品(20ng/g)和土壤加标样品(20ng/g)的回收率分别为33.2%~101.9%、38.8%~120.5%,相对标准偏差为6.1%~28.0%、2.3%~16.0%。沉积物加标样品(2.0 ng/g)回收率为43.0%~100.0%,相对标准偏差为2.1%~11.3%。     

甲醇提取-吹扫捕集-气质联用法快速测定土壤中8种苯系物

采用甲醇提取-吹扫捕集的前处理方法并结合气相色谱-质谱仪来测定土壤样品中的8种苯系物。实验结果表明,8种苯系物在前处理过程中被有效提取出来并被准确定性和定量,对于低浓度样品也具有良好的实验效果。此方法的检出限为0.3～0.8μg/kg,测定下限为1.2～3.2μg/kg。加标低、中、高3种不同质量比的标准物质,经实验分析土壤中8种苯系物相对标准偏差(RSD)为2.1%～6.8%,加标回收率为91.0%～105%,与相关行业标准相比具有一定的优势。     

快速溶剂萃取-气相色谱/串联质谱法测定农作物中的有机氯农药

建立快速溶剂萃取,固相萃取柱净化,气相色谱/串联四极杆质谱检测分析农作物中23种有机氯农药残留的方法。以油菜为样品,加标浓度为5、10、25、50μg/kg时,平均回收率在72%~101%之间,相对标准偏差3%~14%(n=5)。8种农作物(莴笋、黄瓜、蒜苗、辣椒、油菜、茄子、玉米和水稻)加标浓度为25μg/kg时的平均回收率在71%~113%之间,相对标准偏差3%~16%(n=5)。方法检出限0.75~1.76μg/kg之间。     

环境中寄生虫(卵)的检测方法及回收率

环境中常见的寄生虫(卵)有蛔虫、肝吸虫、血吸虫、贾第鞭毛虫和隐孢子虫等,针对其特点已形成以虫卵密度、免疫和血清特性等为基础的检测方法,比较分析不同寄生虫不同检测方法的准确度、精确度、回收率差异及优缺性,为实际工作提供技术依据。     

串联四极杆质谱(GC-QqQ-MS/MS)测定土壤中的有机氯农药和多氯联苯

建立了用加速溶剂萃取仪(ASE)萃取、凝胶渗透色谱(GPC)净化、气相色谱/串联四极杆质谱多反应监测、同时测定土壤中17种有机氯农药和19种多氯联苯的方法.加标浓度在3.3μg/kg时的平均回收率在79.6%～93.2%之间,相对标准偏差在2.9%～13.0%之间,定量限在0.01～0.51μg/kg之间.在检测土壤样品中的有机氯农药和多氯联苯残留方面,Gc-QqQ-MS/MS相对于气相色谱/电子捕获检测器(GC-ECD)和GC-MS的选择离子检测(SIM)模式具有非常明显的优势,尤其是在低浓度水平的定性和定量方面.     

超声波萃取-高效液相色谱-串联质谱同时测沉积物中10种PPCPs化合物

基于EPA1694方法,应用超声波萃取-高效液相色谱-串联质谱技术,建立了沉积物中对乙酰氨基酚、林可霉素、甲氧苄啶、咖啡因、阿奇霉素、磺胺甲唑、泰乐菌素、地尔硫卓、卡马西平及氟西汀等10种药物和个人护理品(PPCPs)的分析检测方法。样品经超声萃取、离心和SAX阴离子交换柱净化,以高效液相色谱-串联质谱仪多反应监测(MRM)模式进行离子定性、定量分析。10种药物加标回收率实验结果表明:添加低浓度样品20 ng/g,回收率为61.1%~128.5%,相对标准偏差(RSD)为1.7%~17.5%(n=5);添加高浓度样品400 ng/g,回收率为66.4%~126.7%,RSD为2.3%~18.0%(n=5),最低检测限为0.12~4.46 ng/g。该方法具有检测限低和回收率高的特点,并经实际样品验证发现,该方法适用于检测沉积物中10种PPCPs化合物。     

黄河甘宁蒙段表层沉积物中总磷3种提取方法的比较

通过微波消解法、标准测试方法(SMT)和碱熔法分别测定了水系沉积物成分分析标准物质GBW07307a(GSD-7a)中的总磷(TP)含量,并分别采用3种方法对采集于黄河流域甘宁蒙段表层沉积物样品进行TP含量和样品加标回收率的测定。结果表明:测定标准物质的相对误差绝对值:微波消解法碱熔法SMT法;变异系数:微波消解法碱熔法SMT法。同时,微波消解法提取的表层沉积物TP含量的范围为634.3~909.2μg/g;SMT法TP含量的范围为627.1~889.5μg/g;碱熔法TP含量的范围为559.1~784.8μg/g。微波消解法的测定结果相对偏高,SMT法的测定结果相对偏低。样品加标回收率平均值:微波消解法SMT法碱熔法;变异系数:微波消解法碱熔法SMT法。综合测定标准物质中TP含量以及样品加标回收率实验结果的准确度和精密度,对于黄河甘宁蒙段表层沉积物,使用SMT法提取TP较优于微波消解法和碱熔法。     

溶解性有机碳对微库仑法测定水中可吸附有机卤素的影响

微库仑法测水样中可吸附有机卤素(AOX)受多种因素影响,其中溶解性有机碳(DOC)的影响非常显著。DOC对微库仑法2种前处理方法(双柱法和振荡法)的影响差异很大。双柱法受DOC影响较小,当DOC浓度小于1 000 mg/L时,AOX加标回收率范围为94.0%~104%。振荡法受DOC影响较明显,随着DOC浓度的升高,AOX回收率持续下降,当DOC浓度达到1 000 mg/L时,AOX加标回收率下降至72.1%,但DOC浓度小于100 mg/L时,AOX加标回收满足方法要求。进一步研究发现,DOC对振荡法的影响主要由于竞争吸附降低了活性炭对AOX的吸附容量,而非吸附速率,虽然增大活性炭用量可在一定程度上减小DOC对AOX测定的影响,但对样品进行稀释是减少DOC影响的最简单高效的办法。同时,DOC对不同类型的有机卤代物影响不同,有机溴受DOC影响程度小于有机氯。     

过氯乙烯滤膜采样-酸消解-钼蓝光度法测定磷酸雾

建立了过氯乙烯滤膜采样 -酸消解 -钼蓝分光光度法测定磷化车间磷酸雾的监测方法。实验室模拟采样的捕集效率为 95 7%～ 99 1 %。单个实验室对含 5μg和 1 5μg样品进行多次测定 ,其相对标准差小于 5% ,样品加标回收率为 98 2 %～ 1 0 0 5% ,方法检测限为 0 0 0 7mg/m3。对标样测定 ,结果均在给定值范围内。用该法与等离子发射光谱法(ICP)对 5个样品进行比对测定 ,结果均令人满意。     

Mercury, Methylmercury, and Selenium Concentrations in Eggs of Common Loons (Gavia immer) from Canada

Concentrations of Hg and Se were determined for a total of 125Common Loon (Gavia immer) eggs collected from lakes in Alberta, Saskatchewan, Ontario, Quebec, New Brunswick and NovaScotia, Canada between 1972 and 1997. Resulting data were compared to Hg and/or Se concentrations known or suspected tocause reproductive impairment in birds. Organic (methyl) Hg analyses were also performed on a subset of 24 loon eggs. Thirty-nine of 125 eggs had total Hg levels exceeding those (0.6 g g^-1 ww, or 2.5 g g^-1 dw)previously reported to be associated with reproductive impairment in common loons (Barr, 1986), and 9 of 125 eggshad Hg concentrations higher than the level associated withreproductive impairment in birds generally 1 g g^-1 ww; (Thompson, 1996). Selenium concentrations in loon egg samples were less than levels known to cause reproductiveimpairment in birds. A weak but significant positive correlation was observed between egg-Hg and -Se concentrations(r = 0.511, p < 0.05). On average, methylmercury accounted for about 87% of total Hg in 24 eggs analysed for both total and organic Hg. In this subset of eggs, the relationship between organic (methyl) Hg and Se was significant (r = 0.538, p = 0.007) while that found between inorganic Hg and Se in the same eggs was not significant (r = 0.353, p = 0.091). This relationship was unexpected and was contrary to relationships established for organic and inorganic Hg vs. Se in adult loon liver and kidney tissue (Scheuhammer et al., 1998b).     

Heavy Metals in the Eggs and Muscle of Horseshoe Crabs (Limulus Polyphemus) from Delaware Bay

Lead, mercury, cadmium, chromium and manganese concentrations were measured in the eggs of horseshoe crabs (Limulus polyphemus) from 1993, 1994 and 1995; and from chelicera muscle in 1995 from Delaware Bay. Metal concentrations in the eggs represent levels derived from females. In eggs, mercury levels were below 100 ppb or were non-dectable; cadmium levels were generally low in 1993 and 1995 but were relatively higher in 1994; lead levels in eggs decreased from 558 ppb in 1993 to 87 ppm in 1995; selenium increased from 1993 to 1995; chromium decreased from 1993 to 1995; and manganese generally decreased. Leg muscles had significantly lower levels of all metals than eggs, except for mercury.     

催化光度法测定鸡蛋中的碘

研究了在 80～ 1 0 0℃条件下制备样品 ,利用催化光度法间接测得鸡蛋中碘的含量。在 0～ 0 .0 2 1 mg/ L内符合比耳定律 ,摩尔吸光系数达 2 .0 3× 1 0 5L.mol- 1 .cm- 1。可用于其它食品中微量碘的测定。     

长江上游合江江段鱼类早期资源与向家坝水库生态调度效果初步研究

合江江段是长江上游干流保持河流生境、适宜喜流水性鱼类栖息的重要江段。为了掌握合江江段鱼类早期资源动态,分析向家坝水库生态调度的效果,于2020年向家坝水库生态调度前后,开展了鱼类早期资源逐日监测。研究期间,共采集到鱼类早期资源5目10科38种(属),其中仔鱼29种(属)、鱼卵19种(属),包括特有鱼类6种。广适应性和喜流水性种类分别有18种和15种,其中,仔鱼分别为17种和11种,鱼卵分别为6种和9种。仔鱼平均密度为(89.06±78.55)ind./1000 m³,广适应性鱼类太湖新银鱼(Neosalanx taihuensis)和吻虎鱼属(Rhinogobius spp.)占绝对优势。鱼卵平均密度为(19.89±20.5)ind./1000 m³,喜流水性种类吻(Rhinogobio typus)、铜鱼(Coreius heterodon)等占优势地位。调度期间,共采集到仔鱼9种、鱼卵7种(其中6种为漂流性卵,含2种特有种),仔鱼和鱼卵密度的增加与调度过程基本同步。研究结果表明,合江江段是喜流水性鱼类(包括多种特有鱼类)重要的产卵和育幼江段,向家坝水库生态调度促进了产漂流性卵鱼类(包括多种特有鱼类)的繁殖。     

Organochlorine Contaminants in Herring Gull Eggs from the Great Lakes, 1974-1995: Change Point Regression Analysis and Short-Term Regression

The temporal trends (1974-1995) of 11 organochlorine contaminants in herring gull eggs from 13 colonies throughout the Great Lakes were statistically analyzed using two regression methods on logarithmically transformed data. Change point analysis was used to determine if there had been significant year to year fluctuations in contaminant levels and/or changes in long-term trends. Short-term regressions were conducted on 6 major compounds for two time periods (early 1990s and early 1980s) to compare the rates of decline. Overall, change point analyses indicated that for most of the comparisons (75%) there had been significant year to year fluctuations in contaminant levels. They also indicated that for most of the comparisons (67%) the rate of decline after the change point was as fast as or faster than before the change point, this pattern was most common for dieldrin and heptachlor epoxide at certain locations. In 19% of the comparisons the rates of decline had slowed or stabilized, this was most common for PCB and pentachlorobenzene. In 14% of the comparisons there were no significant temporal trends, this was most common for photomirex and mirex. Results for short-term regression showed that out of 78 comparisons for each time period, 5 (6%) were declining significantly in the early 1990s and 11 (14%) were declining significantly in the early 1980s. Both types of regression indicated that, for most of the herring gull egg contaminant database, recent logarithmic rates of decline were similar to those seen previously in the sampling period. For PCB 1254:1260, a group of compounds of particular toxicological importance, change point analyses indicated that the logarithmic rates of decline in herring gull eggs from western Lake Ontario were slower from 1987-1995 than they were from 1974-1986. At both Lake Superior colonies and the Niagara River colony PCB 1254:1260 concentrations ceased to decline in the mid-1980s. At the colony in Green Bay, Lake Michigan, PCB 1254:1260 levels have shown no significant temporal trend since 1976. At the remaining 8 colonies, PCB 1254:1260 levels continue a logarithmic decline in recent years at the same rate as or faster than previously.     

Mercury in Tree Swallow Food, Eggs, Bodies, and Feathers at Acadia National Park, Maine, and an EPA Superfund Site, Ayer, Massachusetts

We monitored nest boxes during 1997–1999 at Acadia National Park, Mt. Desert Island, ME and at an old-field site in Orono, ME to determine mercury (Hg) uptake in tree swallow (Tachycineta bicolor) eggs, tissues, and food boluses. Also, in 1998–1999 we monitored nest boxes at Grove Pond and Plow Shop Pond at a U.S. Environmental Protection Agency Superfund site in Ayer, MA. We recorded breeding success at all locations. On average among locations, total mercury (THg) biomagnified 2 to 4-fold from food to eggs and 9 to 18-fold from food to feathers. These are minimum values because the proportion of transferable methyl mercury (MeHg) of the THg in insects varies (i.e., 35%–95% of THg) in food boluses. THg was highest in food boluses at Aunt Betty Pond at Acadia, whereas THg in eggs was highest at the Superfund site. A few eggs from nests at each of these locations exceeded the threshold (i.e., 800–1,000 ng/g, wet wt.) of embryotoxicity established for Hg. Hatching success was 88.9% to 100% among locations, but five eggs failed to hatch from 4 of the 11 clutches in which an egg exceeded this threshold. MeHg in feathers was highest in tree swallows at Aunt Betty Pond and the concentration of THg in bodies was related to the concentration in feathers. Transfer of an average of 80%–92% of the Hg in bodies to feathers may have enhanced nestling survival. Residues of Hg in tissues of tree swallows in the Northeast seem higher than those of the Midwest.     

锅炉烟尘测试中锅炉负荷率的计算方法探讨

GB5468 -91规定 ,锅炉烟尘测试时 ,必须对锅炉的运行负荷进行测试 ,而实际监测过程中 ,许多锅炉房不具备测试的计量条件 ,为了解决这一问题 ,文章提出利用烟气量和空气过剩系数计算锅炉负荷率。在实际监测工作中 ,该方法方便、易于操作 ,所得结果和标准规定方法所得结果有很好的一致性     

城市空气质量周报效用分析

介绍了世界上一些发达国家的空气污染预报的做法和采取的措施,阐述了我国开展空气质量预报的方针和方法,指出了周报是预报的基础工作。叙述了我国空气质量周报的污染参数的选取、污染指数的分级及其浓度限值和污染指数计算及确定,分析并总结了开展城市空气质量周报所发挥的效用是提高公众的环保意识,加大了治理污染的力度,转变了环境监测的职能,促进了环境监测事业的发展     

水中总硬度测量不确定度的评定

采用EDTA滴定法测定水质总硬度的测量不确定度评定。充分考虑测量重复性、标准溶液的配制、滴定等过程对测量的影响,计算水中总硬度的测量相对合成标准不确定度为1·81×10-3。     

Environmental Assessment of the Impact of Ozone to the Neuston of the Sea-Surface Microlayer of the Gulf of Mexico

Substantial amounts of NOx (146 000 t/y) and total hydrocarbons (294 000 t/y) are released to the marine atmosphere by the large number of oil and gas operations over Federal waters of the Gulf of Mexico (GOM). Under appropriate meteorological conditions these emissions react to form ozone (0–54 g/m3 over-water) which can affect the marine environment. Using a dry deposition model, this work examines the amount of ozone derived from oil and gas offshore operations and deposited in the sea surface of the Gulf of Mexico, and assesses its impact on the neuston of the sea-surface microlayer. Surface integrated estimates of ozone deposited from oil and gas operations over the sea surface ranges from 400 kg to 1800 kg which results in sea surface concentrations of 15 g/m3. This estimate and the actual toxic ozone levels suggest no acute, toxic impacts to the neuston. However, indirect effects may occur through changes to the pelagic foodwebs and organic carbon pathways. Another potential pathway for ozone impacting the environment is through the production of bromate. Based on the concentrations and time scales (11–139 days) only sublethal effects appear to occur, but uncertainties associated with this assessment need to be further studied. From an ecological perspective, the environmental impacts and risks of NOx and VOC discharges from offshore platforms need to be assessed for neuston and other components of the marine ecosystem.