目的 对国标中用直接比色法测定马口铁罐内壁涂层中重金属（以Pb计）的测试方法提出改进建议。方法 对常见的金属涂层样品采用直接比色法试验,针对试验得出的阳性样品,进一步采用电感耦合等离子体发射光谱法（ICP-OES）进行金属元素筛查,同时开展加标复配试验与玻璃板涂层直接比色法验证试验。结果 采用直接比色法对48款金属涂层样品进行重金属筛查,结果显示,仅带涂层的马口铁罐样品的重金属（以Pb计）检测结果呈阳性。经ICP-OES定量测定,除铁、锡元素外,样品中其余重金属元素总质量浓度均低于1.0 mg/L。加标复配试验结果表明,高浓度铁溶液本身呈棕红色,与硫化钠反应后,溶液颜色仍保持棕红色;锡标准溶液与硫化钠反应呈黄绿色,仅对显色结果观察略有影响。玻璃板涂层模拟试验结果均为阴性,表明铁、锡元素来源于金属罐的金属基体,而非来自涂层。结论 国标方法直接测定马口铁罐内涂层重金属（以Pb计）实验结果存在干扰,应结合实际情景重新进行制样,以此得出可靠的实验结果。
Abstract
The work aims to propose an improvement suggestion for the testing method specified in the national standard for determining heavy metals (calculated as Pb) in coatings of tinplate cans with direct colorimetry method. For common metal-coated samples, a direct colorimetric test was conducted. For the positive samples obtained from the test, in addition to using inductively coupled plasma atomic emission spectroscopy (ICP-OES) for metal element screening, a spiked compound test and a direct colorimetric verification test with glass plate coating were also carried out. Forty-eight metal-coated samples were screened for heavy metals with the direct colorimetric method. The results showed that only the inner coating samples of tinplate cans tested positive for heavy metals (calculated as Pb). Quantitative determination by ICP-OES indicated that, with the exception of iron and tin, the total mass concentration of other heavy metal elements in the samples was all below 1.0 mg·L-1. The standard addition test indicated that high-concentration iron solution remained brownish red after reacting with sodium sulfide, while tin standard solution turned yellowish-green, with only a slight impact on color observation. All glass plate coating simulation test results were negative, confirming that iron and tin originated from the metal base of the can, not the coating. The national standard method of directly determining heavy metals (calculated as Pb) in the coating of tin cans has interference. Samples should be redesigned based on the actual situation to obtain reliable results.
关键词
重金属（以Pb计） /
电感耦合等离子体发射光谱法 /
马口铁罐 /
直接比色法
Key words
heavy metals (calculated as Pb) /
ICP-OES /
tin can /
direct colorimetric method
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