高純氟化銨溶液 編制說明

修訂《高純氟化銨溶液》編制說明（征求意見稿）一、工作簡況(一)任務(wù)來源1、基本信息根據(jù)“國標(biāo)委發(fā)〔2023〕58號《關(guān)于下達(dá)2023年第三批推薦性國家標(biāo)準(zhǔn)計(jì)劃及相關(guān)標(biāo)準(zhǔn)外文版計(jì)劃的通知》”的要求，2024年完成GB/T30901-2014《高純氟化銨溶液》國家標(biāo)準(zhǔn)的修訂工作，計(jì)劃編號為：20231332-T-606。本標(biāo)準(zhǔn)由中巨芯科技股份有限公司、多氟多新材料股份有限公司、浙江凱圣氟化學(xué)有限公司、貴州甕福藍(lán)天氟化工股份有限公司、中巨芯（湖北）科技有限公司、湖北興力電子材料有限公司、湖北宜化氟化工有限公司、福建永晶科技股份有限公司、瑞士萬通中國有限公司、中海油天津化工研究設(shè)計(jì)院有限公司等單位共同起草。全國化學(xué)標(biāo)準(zhǔn)化委員會(huì)無機(jī)化工分技術(shù)委員會(huì)負(fù)責(zé)技術(shù)歸口。2、簡要情況1)產(chǎn)品概況主體成分分子式：NH4F主體成分分子量：37.04產(chǎn)品性質(zhì)氟化銨溶液為無色透明液體。相對密度1.009。溶液呈弱酸性，遇熱分解生成氨和氟化氫。產(chǎn)品用途主要用于電子行業(yè)業(yè)，作為集成電路(IC)和超大規(guī)模集成電路(VLSI)芯片的清洗和腐蝕劑，可與氫氟酸配成緩沖腐蝕液。2)生產(chǎn)方法原料為高純氟化氫和高純氨，經(jīng)中和反應(yīng)制得成品。3)修訂標(biāo)準(zhǔn)的目的和意義高純氟化銨溶液是微電子技術(shù)加工制作過程中不可缺少的關(guān)鍵性化學(xué)品之一，主要用于太陽能光伏電池、液晶顯示器件、集成電路(IC)和超大規(guī)模集成電路(VLSI)芯片的清洗和腐蝕，是上述各行業(yè)制作過程中的關(guān)鍵性基礎(chǔ)化工材料之一。它的純度和潔凈度對集成電路的成品率、電性能及可靠性都有十分重要的影響。它基于微電子技術(shù)發(fā)展而發(fā)展，同時(shí)又制約微電子技術(shù)發(fā)展。近年來，全球電子化學(xué)品市場需求增長速度很快，近兩年保持10%以上的增速。2014年國家標(biāo)準(zhǔn)實(shí)施后，促進(jìn)了高純氟化銨溶液行業(yè)生產(chǎn)技術(shù)的發(fā)展，使我國具備一定生產(chǎn)力和國際市場競爭力。近年來國內(nèi)外市場對高純氟化銨溶液需求量逐年增加，對品質(zhì)的要求也有所提高，當(dāng)下已經(jīng)成為我國產(chǎn)品在國際市場擴(kuò)大占有率的一個(gè)關(guān)鍵時(shí)期。隨著生產(chǎn)技術(shù)水平的不斷提高，該產(chǎn)品的質(zhì)量得到了進(jìn)一步的提升，已經(jīng)具備了向更高端應(yīng)用領(lǐng)域進(jìn)軍的能力。2014年標(biāo)準(zhǔn)實(shí)施已10年，應(yīng)用情況已發(fā)生改變，使該標(biāo)準(zhǔn)規(guī)定的一些技術(shù)內(nèi)容不再適應(yīng)行業(yè)的發(fā)展，急需修訂。通過本標(biāo)準(zhǔn)的修訂，使優(yōu)質(zhì)產(chǎn)品的生產(chǎn)有據(jù)可依，對推廣先進(jìn)生產(chǎn)技術(shù)、規(guī)范產(chǎn)品質(zhì)量、指導(dǎo)企業(yè)生產(chǎn)、滿足用戶的使用具有十分重要的意義。本標(biāo)準(zhǔn)的實(shí)施可以進(jìn)一步促進(jìn)高純氟化銨溶液行業(yè)良性、健康地發(fā)展，推動(dòng)我國優(yōu)質(zhì)產(chǎn)品在國際市場的占有率不斷擴(kuò)大。(二)主要工作過程1、起草階段（2023.10～2024.6）1）起草工作組2由中巨芯科技股份有限公司、多氟多新材料股份有限公司、浙江凱圣氟化學(xué)有限公司、湖北興力電子材料有限公司、中巨芯（湖北）科技有限公司、貴州甕福藍(lán)天氟化工股份有限公司、湖北宜化氟化工有限公司、福建永晶科技股份有限公司、瑞士萬通中國有限公司、中海油天津化工研究設(shè)計(jì)院有限公司等單位組成起草標(biāo)準(zhǔn)工作組。2）分工情況天津院主要負(fù)責(zé)資料收集、編寫文獻(xiàn)小結(jié)、召開標(biāo)準(zhǔn)工作方案會(huì)、數(shù)據(jù)統(tǒng)計(jì)、編寫標(biāo)準(zhǔn)各階段草案、編制說明及相關(guān)附件等工作。其他單位主要負(fù)責(zé)試驗(yàn)方法驗(yàn)證及數(shù)據(jù)累積工作。3）調(diào)查研究過程天津院接到上級部門下達(dá)的修訂GB/T30901-2014《高純氟化銨溶液》國家標(biāo)準(zhǔn)計(jì)劃后，于2023年10月～2024年1月進(jìn)行了調(diào)研及資料準(zhǔn)備工作。首先查閱了國內(nèi)外標(biāo)準(zhǔn)及有關(guān)技術(shù)資料，并向生產(chǎn)、使用單位發(fā)函進(jìn)行調(diào)查，廣泛征求對標(biāo)準(zhǔn)修訂工作的意見，在此基礎(chǔ)上提出了文獻(xiàn)小結(jié)。2024年3月在四川省成都市召開了修訂標(biāo)準(zhǔn)工作方案會(huì)，參加會(huì)議的有包括天津院在內(nèi)的8家企業(yè)，會(huì)上7家生產(chǎn)單位就各自的產(chǎn)能、生產(chǎn)工藝、產(chǎn)品質(zhì)量和用戶使用情況進(jìn)行了介紹。與會(huì)代表就此標(biāo)準(zhǔn)的分類、用途、指標(biāo)項(xiàng)目和指標(biāo)參數(shù)、分析方法及檢驗(yàn)規(guī)則、包裝、貯存、運(yùn)輸?shù)葍?nèi)容進(jìn)行了深入、細(xì)致地討論，提出了工作方案，并對各項(xiàng)工作任務(wù)及工作進(jìn)度做了詳細(xì)地安排。4）驗(yàn)證過程起草工作組成員針對試驗(yàn)驗(yàn)證方案開展了試驗(yàn)驗(yàn)證工作。對比驗(yàn)證數(shù)據(jù)分析及驗(yàn)證評價(jià)（或結(jié)論）見本編制說明第四章。2、標(biāo)準(zhǔn)征求意見階段（2024.7～2022.8）1）廣泛征求意見在起草階段工作基礎(chǔ)上，由負(fù)責(zé)起草單位對工作組討論稿進(jìn)行了進(jìn)一步的討論和修改，于2024年6月提出標(biāo)準(zhǔn)草案征求意見稿及編制說明，其后向無機(jī)化工分技術(shù)委員會(huì)的委員、生產(chǎn)企業(yè)、使用單位及檢驗(yàn)機(jī)構(gòu)等單位發(fā)送了征求意見稿及編制說明，并在天津院官網(wǎng)上（）公開征求意見。二、國家標(biāo)準(zhǔn)編制原則1)GB/T1.1-2020《標(biāo)準(zhǔn)化工作導(dǎo)則第1部分：標(biāo)準(zhǔn)化文件的結(jié)構(gòu)和起草規(guī)則》；2)貫徹國家的有關(guān)方針、政策、法律、法規(guī)；3)有利于合理開發(fā)和利用國家資源，推廣科學(xué)技術(shù)成果；4)積極采用國際標(biāo)準(zhǔn)和國外先進(jìn)標(biāo)準(zhǔn)，促進(jìn)對外經(jīng)濟(jì)技術(shù)合作與對外貿(mào)易的發(fā)展；5)保障安全和人民的身體健康，保護(hù)環(huán)境；6)充分考慮使用要求，維護(hù)消費(fèi)者的利益；7)技術(shù)先進(jìn)、經(jīng)濟(jì)合理、安全可靠、協(xié)調(diào)配套。三、國內(nèi)外標(biāo)準(zhǔn)及對比目前收集到了有關(guān)高純氟化銨溶液的國內(nèi)外標(biāo)準(zhǔn)有：SEMIC20－0213《40%氟化銨規(guī)范和指南》。SEMI標(biāo)準(zhǔn)代表國際先進(jìn)水平，因此本標(biāo)準(zhǔn)參考SEMI標(biāo)準(zhǔn)進(jìn)行修訂。國內(nèi)外標(biāo)準(zhǔn)指標(biāo)對比見附表1。四、標(biāo)準(zhǔn)修訂主要內(nèi)容及確定依據(jù)31.指標(biāo)分級的補(bǔ)充和完善在超凈高純試劑的發(fā)展方面，不同線寬的集成電路必須使用不同規(guī)格的超凈高純試劑進(jìn)行蝕刻和清洗，超凈高純試劑的關(guān)鍵在于控制其所含的金屬離子的多少和試劑中塵埃顆粒的含量。對于線寬較小的集成電路，幾個(gè)金屬離子或灰塵就足以報(bào)廢整個(gè)電路。目前收集到的國際半導(dǎo)體設(shè)備與材料組織（SEMI）制定的國際統(tǒng)一的超凈高純試劑要求見表1所示。表1工藝化學(xué)品SEMI國際標(biāo)準(zhǔn)等級SEMI標(biāo)準(zhǔn)C1（Grade1）C7（Grade2）C8（Grade3）C12（Grade4）（Grade5）金屬雜質(zhì)≤1mg/kg≤10μg/kg≤1μg/kg≤0.1μg/kg≤0.01μg/kg控制粒徑/μm≤1.0≤0.5≤0.5≤0.2—顆粒/個(gè)/mL≤25≤25≤5——適應(yīng)IC線寬范圍/μm>1.20.8～1.20.2～0.60.09～0.2＜0.09SEMIC20－0213標(biāo)準(zhǔn)規(guī)定了三個(gè)級別，分別對應(yīng)表2中的C1、C7和C8。2014年版標(biāo)準(zhǔn)制定時(shí)根據(jù)高純氟化銨溶液的主要用途，只設(shè)置了UP-S、UP-SS二個(gè)等級。具體適用情況如下：UP-S級：主要用于線寬為0.2μm～0.6μm集成電路的清洗與蝕刻；UP-SS級：主要用于線寬為0.09μm～0.2μm集成電路的清洗與蝕刻。UP-S級對應(yīng)的是表2的C8，UP-SS級對應(yīng)表2的C12，其設(shè)置基本滿足高端客戶的需求，但與SEMI標(biāo)準(zhǔn)相比缺少對低端產(chǎn)品的規(guī)格要求。隨著集成電路制作精度的不斷細(xì)化，對濕化學(xué)品品質(zhì)進(jìn)行合理劃分，通過分等分級的方式即可以滿足下游不同級別加工的需求，又可以節(jié)約資源，避免質(zhì)量過剩造成浪費(fèi)。因此本次修訂擬對缺少的等級進(jìn)行補(bǔ)充，參考同類產(chǎn)品《工業(yè)高純氫氟酸》行業(yè)標(biāo)準(zhǔn)中的規(guī)定，分等分級確定如下：a)EL級：主要用于太陽能光伏電池及液晶顯示器件等的制造；b)UP級：主要用于線寬為0.8μm～1.2μm集成電路的清洗與蝕刻；c)UP-S級：主要用于線寬為0.2μm～0.8μm以上集成電路的清洗與蝕刻；d)UP-SS級：主要用于線寬為0.09μm～0.2μm集成電路的清洗與蝕刻；e)UP-SSS級：主要用于線寬小于0.09μm集成電路的清洗與蝕刻。2.增設(shè)項(xiàng)目的修改影響集成電路蝕刻和清洗效果的主要因素為產(chǎn)品所含陰離子、金屬離子和試劑中塵埃顆粒的數(shù)量。根據(jù)SEMI標(biāo)準(zhǔn)中項(xiàng)目的情況，結(jié)合用戶對生產(chǎn)廠家的要求，2014年版標(biāo)準(zhǔn)確定的項(xiàng)目如下：外觀、總酸度（以HF計(jì)）、氟硅酸（H2SiF6）含量、氯化物（以Cl計(jì)）含量、硝酸鹽（以NO3砷（As）、硼（B）、鋇（Ba）、鈣（Ca）、鎘（Cd）、鉻（Cr）、銅（Cu）、鐵（Fe）、鉀（K）、鋰（Li）、鎂（Mg）、錳（Mn）、鈉（Na）、鎳（Ni）、鉛（Pb）、鈦（Ti）、銻（Sb）、錫（Sn）、鋅（Zn）。本次修訂標(biāo)準(zhǔn)參考同類產(chǎn)品《工業(yè)高純氫氟酸》（HG/T4509-2023）標(biāo)準(zhǔn)，根據(jù)目前下游行業(yè)的實(shí)際需求，確定增設(shè)銀（Ag）、金（Au）、鉍（Bi）、鈹（Be）、鈷（Co）、鎵（Ga）、鍺（Ge）、鉬（Mo）、鈮（Nb）、鈀（Pd）、鍶（Sr）、鉭（Ta）、鉈（Tl）、鋯（Zr）14項(xiàng)陽離子項(xiàng)目。3.調(diào)整UP-S級和UP-SS級中4項(xiàng)陰離子含量根據(jù)匯總收集的修標(biāo)意見和下游用戶的反饋，對2014版標(biāo)準(zhǔn)中UP-S和UP-SS兩個(gè)級別產(chǎn)品的44項(xiàng)陰離子含量提出了更高的要求，本次修訂確定進(jìn)行提高，調(diào)整后指標(biāo)要求見表2。4.設(shè)置了UP-S級和UP-SS級新增陽離子項(xiàng)目的指標(biāo)要求2014版標(biāo)準(zhǔn)UP-S級和UP-SS級中新增了14個(gè)陽離子項(xiàng)目，根據(jù)下游行業(yè)的需求設(shè)置了指標(biāo)要求，設(shè)置的指標(biāo)要求見表2。5.調(diào)整顆粒指標(biāo)根據(jù)下游客戶的需求，本次修訂確定對UP-S級顆粒指標(biāo)進(jìn)行調(diào)整，由原來的10個(gè)/mL調(diào)整為5個(gè)/mL。同時(shí)針對EL級增設(shè)了≥1.0μm項(xiàng)目，針對UP-SSS級增設(shè)了≥0.1μm項(xiàng)目。6.設(shè)置了新增的EL級、UP級和UP-SSS級指標(biāo)要求本著與國外先進(jìn)標(biāo)準(zhǔn)接軌的原則，根據(jù)收集到SEMI標(biāo)準(zhǔn)中指標(biāo)要求的情況，結(jié)合目前用戶對產(chǎn)品的要求，新增EL級、UP級和UP-SSS級要求，指標(biāo)值與SEMI標(biāo)準(zhǔn)的C1、C7和Grade5基本保持一致（見表1）。確定設(shè)置的指標(biāo)要求見表2。7.本次修訂標(biāo)準(zhǔn)確定的指標(biāo)要求綜合上述對產(chǎn)品等級、指標(biāo)項(xiàng)目、指標(biāo)值的調(diào)整，本次修訂確定的指標(biāo)要求見表2。表2本次修訂后確定指標(biāo)要求UP-S級UP-SS級UP-SSS級氟化銨（NH4F）w/%40.0±1.0氟硅酸銨[(NH4)2SiF6]w/（mg/kg）≤——51色度/Hazen≤5pH（10g/L溶液，25℃)6.0～7.5氯化物（以Cl計(jì)）/（mg/kg）≤550.20.050.01硝酸鹽（以NO3計(jì)）/（mg/kg）≤330.10.050.01磷酸鹽（以PO4計(jì)）/（mg/kg）≤110.10.050.01硫酸鹽（以SO4計(jì)）/（mg/kg）≤550.20.050.01銀（Ag）/(μg/kg）≤-10.10.02鋁（Al）/(μg/kg）≤10.10.02砷（As）/(μg/kg）≤30010.10.02金（Au）/(μg/kg）≤-10.10.02硼（B）/(μg/kg）≤10.10.02鉍（Bi）/(μg/kg）≤-10.10.02鋇（Ba）/(μg/kg）≤10.10.02鈹（Be）/(μg/kg）≤--10.10.02鈣（Ca）/(μg/kg）≤10.10.02鎘（Cd）/(μg/kg）≤10.10.02鈷（Co）/(μg/kg）≤--10.10.025鉻（Cr）/(μg/kg）≤10.10.02銅（Cu）/(μg/kg）≤10.10.02鐵（Fe）/(μg/kg）≤10.10.02鎵（Ga）/(μg/kg）≤--10.10.02鍺（Ge）/(μg/kg）≤-10.10.02鉀（K）/(μg/kg）≤10.10.02鋰（Li）/(μg/kg）≤10.10.02鎂（Mg）/(μg/kg）≤10.10.02錳（Mn）/(μg/kg）≤10.10.02鉬（Mo）/(μg/kg）≤-10.10.02鈉（Na）/(μg/kg）≤10.10.02鈮（Nb）/(μg/kg）≤-10.10.02鎳（Ni）/(μg/kg）≤10.10.02鈀（Pd）/(μg/kg）≤-10.10.02鉛（Pb）/(μg/kg）≤10.10.02銻（Sb）/(μg/kg）≤10.10.02錫（Sn）/(μg/kg）≤10.10.02鍶（Sr）/(μg/kg）≤-10.10.02鉭（Ta）/(μg/kg）≤-10.10.02鈦（Ti）/(μg/kg）≤10.10.02鉈（Tl）/(μg/kg）≤-10.10.02釩（V）/(μg/kg）≤--10.10.02鋅（Zn）/(μg/kg）≤10.10.02鋯（Zr）/(μg/kg）≤-10.10.02顆粒(≥1.0μm）/（個(gè)/mL）≤————(≥0.5μm）/（個(gè)/mL）≤—5-—(≥0.2μm）/（個(gè)/mL）≤——-—(≥0.1μm）/（個(gè)/mL）≤——--8.氟化銨含量測定方法的改進(jìn)2014年版標(biāo)準(zhǔn)使用甲醛法測定氟化銨含量，實(shí)際檢測的是產(chǎn)品中的銨根含量，計(jì)算時(shí)折算為氟化銨含量。調(diào)研時(shí)發(fā)現(xiàn)目前生產(chǎn)行業(yè)和用戶均使用電位滴定法測定氟化銨含量，該方法是以pH復(fù)合電極作為測量電極，以氫氧化鈉為滴定劑，通過電位突越指示滴定終點(diǎn)。電位滴定法與甲醛法測定機(jī)理完全不同，因此沒有對2種方法進(jìn)行對比。上下游行業(yè)普遍認(rèn)可電位滴定法的原因主要是該方法人為影響因素較小，方法精密度較高，考慮到目前行業(yè)實(shí)際情況，本次修訂確定將氟化銨含量測定方法由甲醛法修改為電位滴定法。6本次修訂標(biāo)準(zhǔn)對電位滴定法2個(gè)主要內(nèi)容進(jìn)行了統(tǒng)一：1）測定步驟中是否加入飽和硝酸鉀溶液，加飽和硝酸鉀溶液的目的是為了掩蔽氟硅酸對游離酸的影響，高純氟化銨溶液中氟硅酸含量一般不會(huì)高于50mg/kg，其對游離酸的影響是非常小的，從表3給出的10個(gè)樣品的對比試驗(yàn)數(shù)也可以看出，是否加入飽和硝酸鉀溶液對游離酸含量測定結(jié)果影響不大，因此本次修訂標(biāo)準(zhǔn)電位滴定法測定步驟中確定不加入飽和硝酸鉀溶液。表3加入硝酸鉀飽和溶液影響游離酸含量的對比試驗(yàn)數(shù)據(jù)（%）樣品編號123456789方法一0.0090.0100.0080.0080.0780.0790.0590.0590.0800.080方法二0.0100.0110.0090.0080.0800.0810.0600.0610.0820.081差值0.0010.0010.0010.0000.0020.0020.0010.0020.0020.0012）分析了不同測定步驟對分析結(jié)果的影響，并對測定步驟進(jìn)行了統(tǒng)一。高純氟化銨溶液pH規(guī)定為6.0～7.5，當(dāng)產(chǎn)品pH接近6時(shí)，產(chǎn)品中包含的游離酸會(huì)對氟化銨含量產(chǎn)生正影響，因此計(jì)算時(shí)應(yīng)該進(jìn)行扣減；當(dāng)產(chǎn)品pH接近7時(shí)，產(chǎn)品中所含的游離酸含量是很低的，對氟化銨含量測定結(jié)果的影響可以忽略不計(jì)。從圖1的實(shí)測情況也可以得到以上相同的分析。a）2個(gè)滴定終點(diǎn)b）1個(gè)滴定終點(diǎn)圖1滴定終點(diǎn)情況示意圖1a）所示是產(chǎn)品pH接近6時(shí)，滴定時(shí)可以測定出游離酸含量（即出現(xiàn)的第1個(gè)電位突躍計(jì)算氟化銨含量時(shí)需要用第2個(gè)電位突躍點(diǎn)消耗的氫氧化鈉標(biāo)準(zhǔn)滴定溶液的體積減掉第1個(gè)電位突躍消耗的體積（即扣除了游離酸含量）。圖1b）所示是產(chǎn)品pH接近7或超過7時(shí)，滴定只出現(xiàn)一個(gè)電位突躍點(diǎn)，則計(jì)算氟化銨含量時(shí)，用該電位突躍點(diǎn)消耗的氫氧化鈉標(biāo)準(zhǔn)滴定溶液的體積進(jìn)行計(jì)算即可。9.修改完善氟硅酸銨含量測定方法1）對分光光度法測定步驟進(jìn)行修改和完善標(biāo)準(zhǔn)執(zhí)行中發(fā)現(xiàn)2014年版標(biāo)準(zhǔn)規(guī)定的硅鉬藍(lán)分光光度法測定氟硅酸銨含量有些地方需要進(jìn)行改進(jìn)，主要表現(xiàn)為工作曲線范圍過寬，最高點(diǎn)的吸光度超過1；試劑氯化鈉溶液加入量過高，硼酸的加入使測定結(jié)果平行性變差，還原劑可使用抗壞血酸進(jìn)行替代；本次修訂標(biāo)準(zhǔn)將氟硅酸銨含量指標(biāo)要求進(jìn)行了下調(diào)，因此需要將氟硅酸銨測定方法中工作曲線范圍、比色皿、測定波長進(jìn)行調(diào)整。為了解決以上問題本次修訂對方法調(diào)整如下：1）工作曲線范圍下調(diào)至0mg/L~0.8mg/L；2）配合工作曲線范圍下調(diào)，將比色皿長度由2cm調(diào)整為5cm；3）測定波長根據(jù)GB/T23842-2009《無機(jī)化工產(chǎn)品中7硅含量測定通用方法還原硅鉬酸鹽分光光度法》的規(guī)定，由795nm調(diào)整為815nm；4）根據(jù)指標(biāo)調(diào)整適當(dāng)調(diào)整稱樣量。調(diào)整前后工作曲線對比情況見表4。表4分光光度法測定氟硅酸銨含量中工作曲線調(diào)整前后對比標(biāo)準(zhǔn)測定波長長度工作曲線范圍及吸光度A22014年版0mg/L1mg/L2mg/L3mg/L4mg/L5mg/L0.0300.3450.6590.9701.2921.6091.0000.1370.4080.6840.9711.2491.5210.9999本次修改815nm0mg/L0.1mg/L0.2mg/L0.4mg/L0.6mg/L0.8mg/L0.0230.0850.1750.3220.4860.6540.99910.1280.2150.2890.4380.5760.7330.9994從對比數(shù)據(jù)可以看出，2014年版標(biāo)準(zhǔn)的工作曲線范圍吸光度確實(shí)超過了1，本次新調(diào)整的工作曲線從吸光度范圍到線性都可以滿足雜質(zhì)分析要求。方法修改前后對比試驗(yàn)數(shù)據(jù)列于表5。表5分光光度法修改前后對比試驗(yàn)數(shù)據(jù)單位單位1對比數(shù)據(jù)/（mg/kg）單位2對比數(shù)據(jù)/（mg/kg）樣品號GB/T30901-2014本次修改方法GB/T30901-2014本次修改方法10.0790.00630.370.2920.110.0320.080.0830.280.0850.170.1840.0930.0777.245.7850.280.0423.052.3522.9370.233.752.7080.750.04612.559.649--0.95--2.02對比結(jié)論d=0.318Sd=0.408t=2.2由t表查得t0.05（7）=2.37t＜t0.05（7）即兩種方法測定結(jié)果之間無顯著性差異d=0.613Sd=0.973t=1.99由t表查得t0.05（9）=2.26t＜t0.05（9）即兩種方法測定結(jié)果之間無顯著性差異從對比試驗(yàn)數(shù)據(jù)和數(shù)據(jù)統(tǒng)計(jì)計(jì)算結(jié)果來看，修改前后的測定結(jié)果不存在顯著性差異，因此本次修訂對原方法的測定步驟進(jìn)行如上調(diào)整。2）增加ICP-MS法測定低含量樣品修訂過程中企業(yè)反映個(gè)別氟硅酸銨含量低于0.05mg/kg的樣品，使用分光光度法測定的結(jié)果精密度較差，建議增加ICP-MS法測定低氟硅酸銨含量的樣品。本次修訂在資料性附錄中推薦了ICP-MS法對低氟硅酸銨含量樣品進(jìn)行測定，相關(guān)實(shí)驗(yàn)數(shù)據(jù)列于表6。表6ICP-MS法測定氟硅酸銨含量相關(guān)驗(yàn)證數(shù)據(jù)8工作曲線線性氟硅酸銨含量八平行試驗(yàn)數(shù)據(jù)/(μg/kg）12345678平均值標(biāo)準(zhǔn)偏差0.150.280.280.380.580.530.440.490.390.15氟硅酸銨加標(biāo)回收試驗(yàn)數(shù)據(jù)本底含量加標(biāo)量加標(biāo)后含量加標(biāo)回收率0.21μg/kg104.2%0.88μg/kg105.4%0.75μg/kg105.4%樣品實(shí)測數(shù)據(jù)/(μg/kg）0.450.860.260.310.210.620.610.39本標(biāo)準(zhǔn)規(guī)定的硅鉬藍(lán)分光光度法與本標(biāo)準(zhǔn)的指標(biāo)要求相互匹配，ICP-MS法只適用于氟硅酸銨含量很低的情況，因此本標(biāo)準(zhǔn)只是將該方法作為推薦的方法置于資料性附錄中，在氟硅酸銨含量小于0.05mg/kg時(shí)，由供需雙方協(xié)商一致后可選擇使用本標(biāo)準(zhǔn)附錄推薦的方法進(jìn)行測定。10.修改完善陰離子含量測定方法隨著產(chǎn)品中陰離子含量的逐步降低，使原標(biāo)準(zhǔn)中工作曲線不再適用，因此根據(jù)各級別產(chǎn)品的實(shí)際情況，采取增加工作曲線范圍或增加產(chǎn)品稱樣量的方式進(jìn)行調(diào)整。本標(biāo)準(zhǔn)參考工業(yè)高純氫氟酸標(biāo)準(zhǔn)（HG/T4509-2023）中陰離子含量試驗(yàn)步驟進(jìn)行完善。新的工作曲線根據(jù)不同陰離子含量配套工作曲線濃度范圍見表7。表7陰離子工作曲線濃度范圍工作曲線編號陰離子含量標(biāo)準(zhǔn)溶液濃度1234110μg/mL50μg/L200μg/L20.2mL40μg/L340.0μL80.0μL4μg/L911.修改完善陽離子含量測定方法隨著產(chǎn)品中陽離子含量的逐步降低，使原標(biāo)準(zhǔn)中工作曲線不再適用，因此根據(jù)各級別產(chǎn)品的實(shí)際情況，采取增加工作曲線范圍或增加產(chǎn)品稱樣量的方式進(jìn)行調(diào)整。本標(biāo)準(zhǔn)參考工業(yè)高純氫氟酸標(biāo)準(zhǔn)（HG/T4509-2023）中陽離子含量試驗(yàn)步驟進(jìn)行修改完善。本標(biāo)準(zhǔn)包含的5個(gè)等級產(chǎn)品陰離子含量最高要求和最低要求相差10000倍，因此需要增加工作曲線并對原來的工作曲線濃度進(jìn)行調(diào)整以適應(yīng)各級別產(chǎn)品中陽離子含量的測定，確定的3條工作曲線范圍數(shù)據(jù)利于表8。表8陽離子工作曲線范圍工作曲線編號產(chǎn)品規(guī)格編號混合標(biāo)準(zhǔn)使用溶液濃度移取陽離子標(biāo)準(zhǔn)使用溶液的體積12341200.0μL20.1μg/mL200.0μL3UP-SS、UP-SSS0.01μg/mL200.0μL12.其他內(nèi)容的修改根據(jù)實(shí)際采樣情況本標(biāo)準(zhǔn)采樣描述修改為：采樣應(yīng)符合GB/T6678和GB/T6680的規(guī)定。在潔凈環(huán)境中使用專用的采樣器進(jìn)行采樣，采樣前先清洗采樣器和采樣瓶。將產(chǎn)品混勻后采樣，分裝于清潔、干燥的塑料瓶中，密封保存。所取樣品不少于2瓶，每瓶不少于500mL。根據(jù)各生產(chǎn)單位提出的修改意見，包裝的修改主要集中在包裝容積和包裝方式兩個(gè)方面。2014年標(biāo)準(zhǔn)在凈含量的規(guī)定為“200kg或根據(jù)用戶要求協(xié)商確定凈含量”，本次修改根據(jù)實(shí)際情況，將包裝凈含量修改為4L、20L、200L、1000L。包裝方式增加內(nèi)襯塑料耐腐蝕材質(zhì)的槽罐。SEMIC20-0213GB/T30901-2014本標(biāo)準(zhǔn)確定指標(biāo)C1.3-95C7.18-95--UP-S級UP-SS級UP-S級UP-SS級UP-SSS級外觀干凈無色無色透明無色透明氟化銨（NH4F）/%39.0～41.040.0±1.040.0±1.0氟硅酸銨[(NH4)2SiF6]/(mg/kg)≤---5——51色度/Hazen≤---5pH（10g/L溶液，25℃)6.0～7.56.0～7.56.0～7.54220.20.05550.20.050.01330.10.05330.10.050.010.05110.10.050.01硫酸鹽(以SO4計(jì)）/(mg/kg)≤2220.20.05550.20.050.01銀（Ag）/(μg/kg)≤------10.10.022002砷（As）/(μg/kg)≤(As和Sb)110.130010.10.02------10.10.02硼（B）/(μg/kg)2002鋇（Ba）/(μg/kg)≤-2鈹（Be）/(μg/kg)≤-------10.10.02鉍（Bi）/(μg/kg)≤------10.10.02鈣（Ca）/(μg/kg)≤2002鎘（Cd）/(μg/kg)≤-2鈷（Co）/(μg/kg)≤-------10.10.022銅（Cu）/(μg/kg)≤22002SEMIC20-0213GB/T30901-2014本標(biāo)準(zhǔn)擬定指標(biāo)C1.3-95C11.2-94C7.18-95UP-S級UP-S級UP-SS級UP-SSS級-------10.10.02------10.10.02鉀（K）/(μg/kg)3002—220022002------10.10.023002------10.10.02300110.15010.10.02鉛（Pb）/(μg/kg)≤3002鈀（Pd）/(μg/kg)≤------10.10.02銻（Sb）/(μg/kg)≤—2錫（Sn）/(μg/kg)≤2002鍶（Sr）/(μg/kg)≤------10.10.02鉭（Ta）/(μg/kg)≤------10.10.023002鉈（Tl）/(μg/kg)≤------10.10.02釩（V）/(μg/kg)—110.1--10.10.02鋅（Zn）/(μg/kg)≤2002鋯（Zr）/(μg/kg)------10.10.02顆粒(≥1.0μm）/(個(gè)/mL)≤-----————(≥0.5μm）/(個(gè)/mL)≤---—5-—(≥0.2μm）/(個(gè)/mL)≤-5-——-—(≥0.1μm）/(個(gè)/mL)≤-----——--項(xiàng)目SEMI標(biāo)準(zhǔn)GB/T30901-2014本標(biāo)準(zhǔn)確定試驗(yàn)方法外觀的測定-氟化銨的測定自動(dòng)電位滴定法氟硅酸銨的測定-硅鉬藍(lán)分光光度法硅鉬藍(lán)分光光度法附錄中增加ICP-MS法色度-鉑鈷比色法鉑鈷比色法pH計(jì)法pH計(jì)法pH計(jì)法氯化物的測定離子色譜法離子色譜法硝酸鹽的測定磷酸鹽的測定硫酸鹽的測定雜質(zhì)金屬離子的測定ICP-MSICP-MSICP-MS顆粒的測定散射光自動(dòng)粒子計(jì)數(shù)器粒子計(jì)數(shù)器粒子計(jì)數(shù)器附表3：質(zhì)量月報(bào) 中巨芯科技股份有限公司/浙江凱圣氟化學(xué)有限公司工業(yè)高純氟化銨質(zhì)量月報(bào)（產(chǎn)品型號：UPSS級）項(xiàng)目2022.12022.22022.32022.42022.52022.62022.72022.82022.92022.102022.112022.12氟化銨（NH4F）w/%39.539.540.540.540.240.339.839.64039.640.239.9氟硅酸銨[(NH4)2SiF6]/(mg/kg)111111111111色度/HazenpH（10g/L溶液，25℃)7.17.2氯化物（以Cl計(jì)）/（mg/kg）0.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.001硝酸鹽（以NO3計(jì)）/（mg/kg）0.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.001磷酸鹽（以PO4計(jì)）/（mg/kg）0.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.001硫酸鹽（以SO4計(jì)）/（mg/kg）0.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.001銀（Ag）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鋁（Al）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005砷（As）/(μg/kg）0.0980.0920.0640.080.0630.0120.0130.0350.0890.0110.0570.022金（Au）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005硼（B）/(μg/kg）0.0060.0140.0080.0120.0130.0120.010.0110.0180.020.0110.015鉍（Bi）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鋇（Ba）/(μg/kg）0.0170.010.0160.0130.0150.0350.0370.0270.0380.0150.040.028鈹（Be）/(μg/kg）0.0210.0270.0110.0120.0090.0120.0240.0140.0110.0290.0080.017鈣（Ca）/(μg/kg）0.0720.0440.0380.0420.0390.060.0610.0510.0780.0370.0550.06鎘（Cd）/(μg/kg）0.0090.0120.0090.0110.010.010.0090.0090.0080.010.0070.009鈷（Co）/(μg/kg）0.010.0070.010.0090.0090.0050.0050.010.0050.0060.0050.008鉻（Cr）/(μg/kg）0.0280.010.010.0270.0240.030.0150.020.0120.010.0140.028銅（Cu）/(μg/kg）0.0090.0130.0130.010.0120.0060.010.0060.0080.0110.010.008鐵（Fe）/(μg/kg）0.0240.0220.0830.0780.0650.0770.0790.0830.0690.0730.0250.027鎵（Ga）/(μg/kg）0.0520.0620.0270.0310.0630.040.020.040.0380.0570.0490.024鍺（Ge）/(μg/kg）0.0240.0250.0320.0250.0230.0290.0260.0250.0270.0210.0230.032鉀（K）/(μg/kg）0.010.0090.0060.010.0070.010.0080.0080.0080.0090.010.01鋰（Li）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鎂（Mg）/(μg/kg）0.0070.0050.0060.010.0070.0060.0080.0050.0090.0070.0090.005錳（Mn）/(μg/kg）0.010.010.0080.0080.0050.0050.0080.010.010.0060.0080.005鉬（Mo）/(μg/kg）0.0080.0080.0070.0050.0070.010.0070.0060.0120.0120.0080.012鈉（Na）/(μg/kg）0.0050.0080.0080.0060.010.0090.0090.010.0070.0070.0090.008鎳（Ni）/(μg/kg）0.0270.0280.0280.0090.0160.0220.0270.0060.0230.030.0090.008鉛（Pb）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005銻（Sb）/(μg/kg）0.0290.0060.0110.0160.0140.0060.0170.0110.0280.0110.0110.017錫（Sn）/(μg/kg）0.0120.0050.010.0090.0110.0110.0110.0050.0120.0120.0080.005鍶（Sr）/(μg/kg）0.0070.010.010.0070.0060.0110.0060.010.0080.0070.0050.005鉭（Ta）/(μg/kg）0.0060.0070.0050.0080.0090.0060.0110.010.0120.0080.0080.005鈦（Ti）/(μg/kg）0.0070.0070.0070.0110.0130.0130.0130.0070.0090.0070.0130.009鉈（Tl）/(μg/kg）0.0090.0110.020.0090.0110.0140.0090.0170.0060.010.010.012釩（V）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鋅（Zn）/(μg/kg）0.0120.0250.0250.0160.0260.0050.0140.0160.0110.010.0110.021顆粒(≥1.0μm）/（個(gè)/mL）(≥0.5μm）/（個(gè)/mL）(≥0.2μm）/（個(gè)/mL） 中巨芯科技股份有限公司/浙江凱圣氟化學(xué)有限公司工業(yè)高純氟化銨質(zhì)量月報(bào)（產(chǎn)品型號：UPSSS級）項(xiàng)目2022.12022.22022.32022.42022.52022.62022.72022.82022.92022.102022.112022.12氟化銨（NH4F）w/%40.139.839.940.340.540.539.740.439.5氟硅酸銨[(NH4)2SiF6]/(mg/kg)111111111111色度/Hazen555555555555pH（10g/L溶液，25℃)氯化物（以Cl計(jì)）/（mg/kg）0.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.001銀（Ag）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鋁（Al）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005砷（As）/(μg/kg）0.010.0170.0180.0170.0140.0110.0150.0120.0150.0160.0160.01金（Au）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005硼（B）/(μg/kg）0.0060.0120.0090.0160.0090.0060.0070.0170.0110.0070.0150.014鉍（Bi）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鋇（Ba）/(μg/kg）0.0070.0110.0150.0170.0080.0050.0080.0060.0140.0150.0130.016鈹（Be）/(μg/kg）0.010.0050.0070.0140.0130.0080.020.0050.010.010.0090.007鈣（Ca）/(μg/kg）0.020.0120.0120.0110.0140.0080.0170.010.0110.0140.0110.011鎘（Cd）/(μg/kg）0.0060.0070.010.010.0080.0050.0090.010.0120.0060.0110.009鈷（Co）/(μg/kg）0.0080.0050.0090.0050.0070.010.0060.0080.0070.0090.0050.005鉻（Cr）/(μg/kg）0.0080.0090.0170.0120.0120.0160.0110.0150.0150.0190.0110.020銅（Cu）/(μg/kg）0.0090.0080.0120.010.0110.0120.0090.0070.0080.0090.0120.011鐵（Fe）/(μg/kg）0.0130.0130.0110.0080.0190.0160.0150.0150.0090.0110.0090.016鎵（Ga）/(μg/kg）0.0070.0150.0160.0140.0090.0190.0190.010.0080.0080.0160.006鍺（Ge）/(μg/kg）0.0110.0110.010.010.0090.0160.0130.0110.0170.0160.0120.008鉀（K）/(μg/kg）0.010.010.0090.0070.0090.010.0080.010.0080.0080.0050.006鋰（Li）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鎂（Mg）/(μg/kg）0.0080.0090.0060.0090.010.010.0090.0060.0070.010.0080.005錳（Mn）/(μg/kg）0.0070.0080.0080.0050.0050.0080.010.0060.0080.0080.0070.01鉬（Mo）/(μg/kg）0.0120.0060.0080.0050.0090.0090.0120.0120.0070.0050.0110.006鈉（Na）/(μg/kg）0.0080.010.010.0070.0090.0090.0090.010.0070.0060.0050.009鎳（Ni）/(μg/kg）0.0160.0170.0110.010.0200.0130.0130.0110.0180.0070.010.014鉛（Pb）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005銻（Sb）/(μg/kg）0.0170.0190.0060.0070.0050.0120.0150.0160.0130.010.0190.016錫（Sn）/(μg/kg）0.0090.0080.0090.0080.0090.0050.0080.010.0080.0090.0120.006鍶（Sr）/(μg/kg）0.0070.010.0060.0080.010.0080.0090.0090.0080.0060.0090.011鉭（Ta）/(μg/kg）0.0110.0080.0090.0120.0120.0130.0130.0060.0060.0050.0070.007鈦（Ti）/(μg/kg）0.0090.0110.0120.010.0090.0120.0120.0130.0130.0060.0120.009鉈（Tl）/(μg/kg）0.020.0140.0070.0050.0120.010.0190.010.0090.0070.0060.008釩（V）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鋅（Zn）/(μg/kg）0.0110.0140.0190.020.0170.0130.0110.0200.030.0200.0120.014顆粒(≥1.0μm）/（個(gè)/mL）0.1000000.1000(≥0.5μm）/（個(gè)/mL）(≥0.2μm）/（個(gè)/mL）5.3(≥0.1μm）/（個(gè)/mL）49.937.436.245.336.249.336.540.240.437.639.244.1 中巨芯科技股份有限公司/浙江凱圣氟化學(xué)有限公司工業(yè)高純氟化銨質(zhì)量月報(bào)（產(chǎn)品型號：UPSS級）項(xiàng)目2023.12023.22023.32023.42023.52023.62023.72023.82023.92023.102023.112023.12氟化銨（NH4F）w/%40.24040.439.640.339.54039.84040.539.640氟硅酸銨[(NH4)2SiF6]/(mg/kg)111111111111色度/HazenpH（10g/L溶液，25℃)氯化物（以Cl計(jì)）/（mg/kg）0.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.001銀（Ag）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鋁（Al）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005砷（As）/(μg/kg）0.0830.0530.0140.0760.0310.0690.0780.0270.0180.0330.0740.035金（Au）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005硼（B）/(μg/kg）0.0190.0130.0110.0190.0140.020.010.0080.0120.0060.0060.015鉍（Bi）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鋇（Ba）/(μg/kg）0.0380.0240.0330.0050.0160.0190.0350.0090.0390.0140.0260.036鈹（Be）/(μg/kg）0.0250.0120.0090.0050.0080.0110.0130.0180.0280.0160.0090.011鈣（Ca）/(μg/kg）0.0670.050.0740.0480.0750.0640.0610.0770.0720.050.0560.047鎘（Cd）/(μg/kg）0.0050.0090.0060.0050.0050.010.0050.0090.0080.0060.0110.007鈷（Co）/(μg/kg）0.010.0080.0080.010.0080.0050.0090.0070.0080.010.0050.006鉻（Cr）/(μg/kg）0.0260.0070.0220.0230.0110.020.0190.010.0140.0110.0060.018銅（Cu）/(μg/kg）0.0110.0070.0070.0080.010.0090.0090.0120.0080.0070.0090.008鐵（Fe）/(μg/kg）0.0210.0380.0320.0670.0420.0420.0790.0260.080.040.0330.052鎵（Ga）/(μg/kg）0.0610.030.0220.0290.0270.0370.0380.0310.0550.0450.0220.063鍺（Ge）/(μg/kg）0.0240.0290.0260.0260.0320.0310.0280.0210.0290.0210.030.027鉀（K）/(μg/kg）0.0050.0090.0050.010.0050.0050.0070.0090.0060.0090.0050.006鋰（Li）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鎂（Mg）/(μg/kg）0.0080.0080.0080.0060.010.010.0060.0060.0060.0060.010.01錳（Mn）/(μg/kg）0.0070.0050.0090.0060.0080.0080.0050.0060.0050.0060.010.009鉬（Mo）/(μg/kg）0.010.010.0060.0080.0070.0070.0090.0110.0120.0060.0090.006鈉（Na）/(μg/kg）0.0050.0080.0070.0090.010.0050.010.0090.010.010.0070.007鎳（Ni）/(μg/kg）0.0140.0090.0070.0110.0120.0270.0270.0080.020.0120.0120.011鉛（Pb）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005銻（Sb）/(μg/kg）0.0060.0280.0250.0190.0160.0060.0260.0190.0090.0260.030.005錫（Sn）/(μg/kg）0.0120.0090.0080.0110.010.0060.0110.0060.010.0070.0120.007鍶（Sr）/(μg/kg）0.0070.0050.0070.0060.0110.0050.0090.0110.010.0090.0080.01鉭（Ta）/(μg/kg）0.0090.0110.0120.0060.0110.0090.0120.0070.0130.010.0080.011鈦（Ti）/(μg/kg）0.0130.010.0070.0060.0080.010.0090.0080.0070.0070.0060.005鉈（Tl）/(μg/kg）0.0150.0050.0050.0080.0130.0140.0070.0150.0090.0080.0130.005釩（V）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鋅（Zn）/(μg/kg）0.0170.0170.0280.0120.0170.0210.0190.0090.0150.0210.0220.027顆粒(≥1.0μm）/（個(gè)/mL）(≥0.5μm）/（個(gè)/mL）(≥0.2μm）/（個(gè)/mL）58.67.6 中巨芯科技股份有限公司/浙江凱圣氟化學(xué)有限公司工業(yè)高純氟化銨質(zhì)量月報(bào)（產(chǎn)品型號：UPSSS級）項(xiàng)目2023.12023.22023.32023.42023.52023.62023.72023.82023.92023.102023.112023.12氟化銨（NH4F）w/%40.14040.240.340.540.439.539.640.440.439.639.5氟硅酸銨[(NH4)2SiF6]/(mg/kg)111111111111色度/Hazen555555555555pH（10g/L溶液，25℃)氯化物（以Cl計(jì)）/（mg/kg）0.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.0010.001銀（Ag）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鋁（Al）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005砷（As）/(μg/kg）0.010.0160.0110.0180.0160.0110.0160.010.0190.0140.0110.017金（Au）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005硼（B）/(μg/kg）0.0190.0150.0060.0120.0080.0180.020.020.0160.0060.0080.013鉍（Bi）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鋇（Ba）/(μg/kg）0.0120.0110.0080.0070.0110.0180.0070.0090.0160.0170.010.007鈹（Be）/(μg/kg）0.0090.0070.030.010.0160.0090.0140.0070.0140.0120.0150.017鈣（Ca）/(μg/kg）0.0080.0120.0170.020.0130.0170.0120.0150.0130.0110.0170.019鎘（Cd）/(μg/kg）0.0120.0070.0060.0060.0120.0060.0060.0070.0050.0080.0070.01鈷（Co）/(μg/kg）0.0070.0080.0080.0070.0050.0050.0080.0080.0060.0070.0070.006鉻（Cr）/(μg/kg）0.0210.0150.0110.0110.0180.010.0160.0070.0070.0090.0120.014銅（Cu）/(μg/kg）0.010.0110.0060.0130.0060.0110.0070.0080.0110.0090.0130.01鐵（Fe）/(μg/kg）0.010.0080.0190.0120.010.0120.0150.0120.010.0170.0110.01鎵（Ga）/(μg/kg）0.0190.0160.0070.0080.0170.010.0070.0160.0060.0110.0070.012鍺（Ge）/(μg/kg）0.0130.0060.0170.010.010.0060.0130.0160.0110.0090.0060.011鉀（K）/(μg/kg）0.0090.0090.0050.0050.0090.0090.0080.0080.0070.0050.0050.007鋰（Li）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鎂（Mg）/(μg/kg）0.0090.0070.0070.0070.0070.0060.010.010.0070.0060.0090.01錳（Mn）/(μg/kg）0.0060.010.010.0070.0050.0070.0070.0090.0090.0060.010.006鉬（Mo）/(μg/kg）0.0080.0080.0080.0070.0050.0110.0090.0090.0120.0110.0090.007鈉（Na）/(μg/kg）0.0060.0090.0060.0070.0050.0080.0090.0060.0090.0050.0080.007鎳（Ni）/(μg/kg）0.0090.0180.0050.0190.020.0170.0140.0150.0190.0190.0150.012鉛（Pb）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005銻（Sb）/(μg/kg）0.0180.0080.0160.0120.0050.0060.0130.0050.0130.0090.0070.009錫（Sn）/(μg/kg）0.0060.0080.0060.0120.0050.010.0120.0050.010.0050.0090.009鍶（Sr）/(μg/kg）0.0070.0050.0080.0090.0050.0050.0080.0060.0110.0080.0050.006鉭（Ta）/(μg/kg）0.0050.0050.010.0070.0060.0130.010.0110.0060.0130.0120.008鈦（Ti）/(μg/kg）0.0120.0060.0090.010.0110.0090.0080.0080.0060.0130.0060.013鉈（Tl）/(μg/kg）0.0070.0130.0150.0110.0130.0160.0140.0140.0190.0180.0070.019釩（V）/(μg/kg）0.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.0050.005鋅（Zn）/(μg/kg）0.0080.0150.0200.0190.0140.020.0060.0140.0130.0160.0190.014顆粒(≥1.0μm）/（個(gè)/mL）000000.10.100000(≥0.5μm）/（個(gè)/mL）(≥0.2μm）/（個(gè)/mL）5.3(≥0.1μm）/（個(gè)/mL）43.548.441.13647.249.938.745.336.236.944.441.6 湖北興力電子材料有限公司工業(yè)高純氟化銨溶液質(zhì)量月報(bào)（產(chǎn)品型號：UP-S級）項(xiàng)目2022.12022.22022.32022.42022.52022.62022.72022.82022.92022.102022.112022.12氟化銨（NH4F）w/%40.4440.5140.3540.2840.6540.5640.4740.3340.4240.2940.1840.22氟硅酸銨[(NH4)2SiF6]/(mg/kg)未檢出未檢出未檢出未檢出未檢出未檢出未檢出未檢出未檢出未檢出未檢出未檢出色度/Hazen112111211112pH（10g/L溶液，25℃)氯化物（以Cl計(jì)）/（mg/kg）000.0010.0020.001000.00100000.0090.0060.0030.0080.0050.0020.0010.0020.0040.0050.0030.006未檢出未檢出未檢出未檢出未檢出未檢出未檢出未檢出未檢出未檢出未檢出未檢出0.0030.0050.0010.0020.0030.0010.0010.0010.0040.0030.0010.001銀（Ag）/(μg/kg）0.0250.0220.0190.0270.0230.0250.0170.0130.0210.0090.0160.023鋁（Al）/(μg/kg）0.3380.1260.0300.0360.2190.0580.0620.2110.1360.1550.261砷（As）/(μg/kg）0.0220.0270.0250.0200.0190.0160.0280.0240.0220.0160.0670.036金（Au）/(μg/kg）0.0160.0190.0220.0090.0150.0130.0180.0260.0160.0210.0140.011硼（B）/(μg/kg）0.5230.4350.1880.0320.1060.2110.1860.0680.0820.0910.136鉍（Bi）/(μg/kg）0.0060.0050.0050.0060.0050.0040.0070.0050.0060.0050.0060.008鋇（Ba）/(μg/kg）0.0070.0090.0060.0080.0050.0060.0090.0060.0080.0050.0070.005鈹（Be）/(μg/kg）0.0660.0960.0820.0530.0630.0710.0590.0850.0490.0380.0560.061鈣（Ca）/(μg/kg）0.2350.0810.3110.2790.1690.2630.1530.0660.0930.1270.1880.203鎘（Cd）/(μg/kg）0.0410.0480.0260.0190.0170.0250.0220.0350.0180.0240.0260.015鈷（Co）/(μg/kg）0.1630.1580.1490.1360.1270.1320.1080.1150.1190.1260.105鉻（Cr）/(μg/kg）0.3460.2630.2910.2190.1770.1920.1630.0920.0850.0560.1070.113銅（Cu）/(μg/kg）0.3380.1000.1450.1250.0940.1360.1190.1050.0910.1030.128鐵（Fe）/(μg/kg）0.5610.4360.2890.3140.2990.1750.1560.1670.1800.1540.1460.133鎵（Ga）/(μg/kg）0.1330.0850.0280.0410.0550.0510.0380.0640.0700.0290.015鍺（Ge）/(μg/kg）0.2220.0960.0830.0600.0710.0590.0750.0620.0850.0550.0520.063鉀（K）/(μg/kg）0.2160.0360.0710.0520.0460.0490.0410.0630.0270.0350.0380.041鋰（Li）/(μg/kg）0.0250.0150.0050.0160.0090.0190.0200.0170.0100.0070.0110.008鎂（Mg）/(μg/kg）0.0190.0110.0070.0050.0090.0100.0130.0160.0080.0060.0020.012錳（Mn）/(μg/kg）0.0220.0160.0650.0250.0090.0110.0060.0080.0130.0050.0070.015鉬（Mo）/(μg/kg）0.0440.0610.0390.0270.0330.0310.0400.0360.0300.0380.0450.036鈉（Na）/(μg/kg）0.0120.0220.0110.0450.0250.0180.0270.0220.0160.0190.0090.005鎳（Ni）/(μg/kg）0.0920.2110.1010.1090.0770.0830.0920.0990.0810.0710.0690.052鉛（Pb）/(μg/kg）0.0120.0160.0190.0220.0150.0610.0260.0170.0130.0180.0280.019銻（Sb）/(μg/kg）0.0160.0190.0080.0100.0170.0330.0250.0130.0070.0180.0210.011錫（Sn）/(μg/kg）0.0400.0560.0420.0380.0290.0180.0230.0280.0260.0330.017鍶（Sr）/(μg/kg）0.0190.0150.0090.0130.0170.0080.0280.0210.0110.0160.0150.014鉭（Ta）/(μg/kg）0.0020.0010.0050.0030.0010.0060.0090.0070.0040.0020.0020.003鈦（Ti）/(μg/kg）0.1800.1810.1610.5470.2100.2310.1900.2060.1880.1930.2010.198鉈（Tl）/(μg/kg）0.0090.0110.0080.0050.0070.0130.0190.0090.0060.0140.0030.008釩（V）/(μg/kg）0.0130.0040.0160.0060.0090.0110.0070.0070.0050.0080.0150.009鋅（Zn）/(μg/kg）0.0210.0480.0320.0300.0220.0350.0510.0660.0800.0230.0300.025顆粒(≥1.0μm）/（個(gè)/mL）————————————(≥0.5μm）/（個(gè)/mL）(≥0.2μm）/（個(gè)/mL）————————————湖北興力電子材料有限公司工業(yè)高純氟化銨溶液質(zhì)量月報(bào)（產(chǎn)品型號：UP-S級）項(xiàng)目2023.12023.22023.32023.42023.52023.62023.72023.82023.92023.102023.112023.12氟化銨（NH4F）w/%40.5140.6540.5640.4740.3340.4240.2940.1840.5140.3540.2840.55氟硅酸銨