《家紡乳膠產(chǎn)品 天然乳膠含量的測(cè)定（征求意見(jiàn)稿）》編制說(shuō)明

膠制品中的橡樹蛋白能抑菌抗螨，減少使用者氣喘和過(guò)根據(jù)《省市場(chǎng)監(jiān)管局關(guān)于下達(dá)2022年度江蘇省地方標(biāo)準(zhǔn)項(xiàng)目計(jì)劃的通知》（蘇市監(jiān)標(biāo)﹝2022﹞192號(hào)）要求，地方標(biāo)準(zhǔn)《家紡乳膠產(chǎn)品天然乳膠含量的2022年7月至2022年12月，計(jì)劃下達(dá)后，通過(guò)調(diào)研對(duì)樣品成分的定性與定量分別進(jìn)行測(cè)試、研究及確認(rèn)，本文件規(guī)定了采用多種儀器方法對(duì)家紡乳膠產(chǎn)品中的天然乳膠進(jìn)行定性分本文件適用于由天然乳膠或天然乳膠與合成乳膠并用的混合乳膠加入配合本文件的試驗(yàn)原理是：采用裂解氣相色譜-質(zhì)譜聯(lián)用儀對(duì)試樣中是否含有天然乳膠進(jìn)行定性，然后采用X射線熒光光譜儀對(duì)含有天然乳膠的試樣中的硫含表1乳膠枕樣品主要成分信息樣品序號(hào)樣品信息1約90%天然乳膠2約77%天然乳膠、5%合成乳膠3約73%天然乳膠、10%合成乳膠4約67%天然乳膠、15%合成乳膠a)異戊二烯的特征離子峰質(zhì)譜b)異戊二烯二聚體的特征離子峰質(zhì)譜c)丁二烯的特征離子峰質(zhì)譜d)苯乙烯的特征離子峰質(zhì)譜圖1乳膠樣品熱裂解特征離子峰質(zhì)譜 a)分析一b)分析二c)分析三d)分析組圖圖21號(hào)樣品裂解色譜圖a)分析一b)分析二c)分析三d)分析組圖圖32號(hào)樣品裂解色譜圖a)分析一b)分析二L_______L____c)分析三d)分析組圖L_______L____圖43號(hào)樣品裂解色譜圖c)分析三d)分析組圖圖54號(hào)樣品裂解色譜圖信息一致。因此，熱裂解-氣相色譜-質(zhì)譜分析方00m0——索氏提取前試樣質(zhì)量，單位為克（g表2試樣索氏提取后剩余物含量樣品序號(hào)索氏提取前試樣質(zhì)量/g索氏提取后試驗(yàn)質(zhì)量/g剩余物含量/%14.7674.53595.1525.3085.11696.3735.0694.87996.2445.0924.91196.45對(duì)經(jīng)索氏提取后的剩余物進(jìn)行熱重測(cè)試，測(cè)試儀器為：DTA8122型熱重分a)1號(hào)樣品b)2號(hào)樣品c)3號(hào)樣品d)4號(hào)樣品圖11乳膠枕樣品索氏提取后不溶物熱重分析圖經(jīng)索氏提取后的測(cè)試樣品TGA測(cè)試曲線中，第一步失重為天然乳膠分解失則第一、二步合計(jì)為天然乳膠分解失重，剩余物質(zhì)為灰分其含量為b。苯乙烯-丁二烯合成乳膠的DTG特征峰溫出現(xiàn)在428℃附近。聚異戊二烯和苯乙烯-丁二烯乳膠通過(guò)分峰擬合可以計(jì)算出天然乳膠或天然乳膠與合成乳膠二者表3乳膠樣品索氏提取剩余物熱重測(cè)試數(shù)據(jù)樣品序號(hào)索氏提取剩余物含量/a索氏提取剩余物經(jīng)熱重測(cè)試后剩余含量/bA天然197.482.52284.060.94384.040.88484.740.81加工而成，各組分含量（重量比）如下：膠體（天然乳膠份，乳化劑0.2~0.4份，穩(wěn)定劑0.2~0.4份，膠凝劑3~4份，發(fā)泡劑2~3份，硫法成型，過(guò)高的硫含量會(huì)導(dǎo)致橡膠硬化，降低橡膠表4參考樣品配料表配合劑名稱STD01STD02STD03STD04STD05STD06生膠/g300300300300300300硫化促進(jìn)劑TBBS/g2.42.42.42.42.42.4氧化鋅/g7.57.57.57.57.57.5硬脂酸/g硫磺/g3.154.756.337.969.61硫含量/%2.0%2.5%3.0%4.0%將參考樣品置于樣品盒中放入試樣架上，將試樣架置于X射線熒光光譜儀表5參考樣品均勻性測(cè)試結(jié)果(?)序號(hào)一次測(cè)試二次測(cè)試三次測(cè)試120.3820.3620.32220.3520.3820.31320.4220.3720.36420.3620.3820.35520.3320.3920.38620.4320.4120.36720.3220.3820.31820.3920.4320.35920.4120.4220.3720.3320.3720.3520.3520.3720.3920.3120.4120.3620.3720.3120.3320.4120.3520.4320.3920.3320.35表6橡膠參考樣品硫含量均勻性測(cè)試統(tǒng)計(jì)結(jié)果項(xiàng)目S總平均值X（%）20.37（%）0.03Fα值(α=0.05）2.04F分布量標(biāo)準(zhǔn)偏差SH（%）0.0109表7參考樣品硫含量短期穩(wěn)定性測(cè)試結(jié)果(?)2#3#4#5#6#7#20.3520.3120.3820.3520.3120.3620.3320.4120.3220.3720.3720.3720.3520.3220.3620.4220.3820.3820.3520.3520.3520.3820.3520.38第2天20.3720.3320.3320.3920.3920.3920.3920.3520.3620.3620.3120.3120.3720.3320.3420.3320.3620.3520.3520.3520.3320.3320.3520.3720.3920.3320.3320.3520.3520.3820.3620.3820.3920.3220.3720.3720.3920.3920.3720.3920.3520.3520.3520.3720.3720.3220.3220.3520.3320.3820.3420.3420.3220.4220.3420.3920.4020.4220.3220.3820.3820.3820.3620.3820.3520.3520.3520.3520.3520.3120.3520.3520.3820.3220.3420.3220.4120.4120.3320.3820.3620.3620.3920.3920.3920.3320.3920.3520.3320.3720.3720.3420.3620.3620.4320.36表8參考樣品硫含量短期穩(wěn)定性測(cè)試統(tǒng)計(jì)分析結(jié)果項(xiàng)目S時(shí)間節(jié)點(diǎn)數(shù)n5t0.95,6（95%置信水平的t檢驗(yàn)因子）3.182斜率|b1|0.0007T×s(b1)0.0016不確定度0.007穩(wěn)定性結(jié)論|b1|<t×s(b1)穩(wěn)定從表8可以看出，參考樣品中|b1|均遠(yuǎn)小于t?s(b1)，依此判定其短期穩(wěn)定性表9參考樣品硫含量長(zhǎng)期穩(wěn)定性測(cè)試結(jié)果(?)2#3#4#5#6#7#9#20.3920.3620.4520.3520.3620.3220.3520.3220.3720.3720.3320.3820.4320.3620.3920.3520.3520.3120.3420.3920.3620.3520.3820.3420.3420.3420.3620.3420.3220.3520.3220.3620.4120.3620.3620.3620.3620.3520.3520.3220.4420.3520.4420.4320.4120.4320.4120.3920.3520.3520.4320.3920.3820.3520.3620.3720.3720.3720.3220.38第2月20.4120.3820.4020.3320.3320.3320.3920.3220.3620.3120.3220.3720.4220.3420.3920.3520.3520.3520.3520.3520.3120.4320.4320.3420.3420.3720.3720.3320.3120.3720.3820.4520.4120.3520.3220.3220.3220.3120.3120.3120.3720.3620.3720.3920.3620.3120.3520.3320.3620.3620.2920.3820.3720.3720.3720.3720.3720.3720.3720.3920.3420.3920.3320.2820.3120.3320.3920.3120.3220.3220.3320.3620.4320.3120.3120.3120.3120.3120.3120.3820.4120.4320.4120.3920.3020.3520.3520.3520.3520.3520.3820.3120.3720.3620.3620.3620.3220.3620.3320.3720.3620.3320.3620.3920.3720.3120.3120.3320.3320.3320.3320.3720.3320.3120.3320.3320.3620.3620.3620.3220.3620.4120.3320.3620.3620.3720.3720.3720.3420.3420.3520.3620.3820.3920.3720.3720.3420.3220.3220.3620.3320.4320.3920.3320.3620.3220.3220.3220.3720.3520.3720.3620.3720.3520.3520.3820.3520.3920.3220.3320.2920.4320.3620.3120.3720.3720.3920.3820.3520.3520.3120.4220.3220.3620.3920.3320.3320.3420.3120.37表10參考樣品硫含量長(zhǎng)期穩(wěn)定性測(cè)試統(tǒng)計(jì)分析結(jié)果項(xiàng)目S時(shí)間節(jié)點(diǎn)數(shù)n8t0.95,6（95%置信水平的t檢驗(yàn)因子）2.45斜率|b1|0.0005T×s(b1)0.0012不確定度0.009穩(wěn)定性結(jié)論|b1|<t×s(b1)穩(wěn)定表11校準(zhǔn)曲線方程、相關(guān)系數(shù)序號(hào)工作曲線方程線性范圍γ21y=6.6078x－0.18320.99952y=6.6415x－0.16520.99943y=6.7321x－0.19210~4.0%0.99934y=6.5352x－0.22150.99925y=6.6533x－0.21110.99956y=6.5212x－0.11310.9993RSD/%由表11可知：校準(zhǔn)曲線的線性相關(guān)系數(shù)均大于0.999、校準(zhǔn)曲線斜率的式中，常數(shù)n與置信區(qū)間相關(guān)，本項(xiàng)目中取n=3（置信概率為99.73%C采用參考樣品作為質(zhì)控樣對(duì)測(cè)試結(jié)果進(jìn)行監(jiān)測(cè)，選取兩種濃度的參考值與標(biāo)準(zhǔn)偏差2倍之和差確定允許區(qū)間，樣品多次平行測(cè)試結(jié)果的平均值表12方法準(zhǔn)確度與精密度參考樣品編號(hào)標(biāo)準(zhǔn)值/%測(cè)定均值/%RSD/%2#2.502.47分別采用X射線熒光光譜法、能量色散X射線熒光光譜法以及GB/T表13不同測(cè)試方法結(jié)果比對(duì)樣品序號(hào)XRF/%EDX/%離子色譜/%偏差/%12.2523.8232.9942.31綜上所述，本項(xiàng)目建立的X射線熒光光譜元素分析方法準(zhǔn)確度和精密度可同時(shí)解