TWI337256B - Extended life mineral acid detection tape - Google Patents

Extended life mineral acid detection tape Download PDF

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TWI337256B
TWI337256B TW094129406A TW94129406A TWI337256B TW I337256 B TWI337256 B TW I337256B TW 094129406 A TW094129406 A TW 094129406A TW 94129406 A TW94129406 A TW 94129406A TW I337256 B TWI337256 B TW I337256B
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acid
solvent
group
detection zone
coupling agent
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Tamami Yamaguchi
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Zellweger Analytics Ag
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    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
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    • G01N31/221—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for investigating pH value
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    • G01—MEASURING; TESTING
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    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T436/00—Chemistry: analytical and immunological testing
    • Y10T436/17—Nitrogen containing
    • Y10T436/173845—Amine and quaternary ammonium

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Description

九、發明說明： 【發明所屬之技術領域】 本發明係關於一種哥命延長型礦物酸偵測帶且尤其係關 於種當投X使用時在至少〗個月日夺期内具有一致之氣體 敏感性及可接受之背景顏色的礦物酸偵測帶。 【先前技術】 目前，現有礦物酸偵測帶可以若干種化學類型為基礎。 種酸偵測系統利用含有pH指示劑染料之礦物酸偵測帶。 然而，在偵測帶上基於酸之染色是不穩定的且pH指示劑染 料本身具有毒性。同樣在該系統中，酸氣體濃度與色斑強 度之間的關係呈非線性，因而需要複雜之光學監測組件。 此外，少數pH指示染料適用於該等光學監測組件且該等偵 測帶具有約一個月時期之有限有用壽命。 另一種礦物酸監測帶系統依靠酸相t之重氮偶合反應來 提供強烈紅顏色以指示酸氣體的存在。儘管該系統對酸氣 體敏感，但是該系統之有用壽命有限。又，該系統之敏感 f生及帶走景顏色對具有溫度及光敏感性的帶配方中之化學 品（諸如伯胺及偶合試劑）不穩定。隨著時間過去，該礦物酸 氣體偵測帶之背景變黑，且由於帶背景變黑，因此帶之敏 感性降低。例如，該等帶在4-6週使用期内展現出顯著的背 景落差。同樣，在室溫條件下，該帶在3〇天時期内之變黑 導致30-40〇/〇之視覺讀數落差。另外，該偵測系統具有不穩 定的帶敏感性及在30天時期内介於1〇-2〇%之間及在9〇天時 期内介於40-60%之間的敏感性減小量。因此，該等礦物酸 104346.doc 1337256 偵測帶系統在其投入使用後有用壽命限於至多3〇天之時 期。因而，該等帶在使用30天時期後必須加以替換以便提 供對酸氣體的可接受之監測。 又，酸氣體濃度與帶顏色強度之間的反應速率在偵測低 濃度酸氣體時呈非線性。所得反應曲線為S型，其導致該等 礦物酸偵測帶回應慢且偵測範圍狹窄。 【發明内容】 本發明一目的係提供針對現有礦物酸偵測帶之有限使用 壽命之解決方案。利用具有低毒性及減小之溫度及光依賴 性的偶氮偶合試劑，以便藉此提供具有至少3個月有用壽命 之改良礦物酸債測帶來得到此解決方案。 本發明一目的係提供礦物酸偵測帶，其在室溫條件下經 至少90天之延長時期仍具有一致之帶背景穩定性。 本發明另一目的係提供在延長時期内對低酸濃度水平敏 感之礦物酸偵測帶。 本發明又一目的係提供重氮偶合試劑，其經延長時期在 穩定之氣體偵測帶中具有低抗毒性及減小之溫度及光依賴 性。 本發明又一目的係提供在擴大之pH範圍内具有穩定性之 驗化礦物酸偵測帶。 本發明另一目的係使用多元醇使酸檢測帶均勻地浸潰有 重氮偶合試劑’以提供在至少90天内具有濕氣及樣品氣體 捕獲功效的帶。 根據本發明，提供用於偵測礦物酸氣體（諸如鹽酸、氫溴 104346.doc 1337256 酸、氫氟酸、氫碘酸、硝酸、硫酸、磷酸及乙酸）之酸氣體 偵測帶’且當其投入使用時使礦物酸偵測紙的有用壽命延 長至至少三個月之時期。 I皆由使纖維素紙基材通過含有配方溶液之浴液，而用配 方溶液浸透壽命延長型礦物酸偵測帶。配方溶液包括以溶 劑總體積計介於8-9體積％之間的pH緩衝液及以溶劑總重 量计介於約0·07-0 · 1 〇重量％之間的試劑級變色酸，該變色酸 係作為偶合劑添加至組合物中。向配方組合物中添加以溶 劑總重量計0.25-0.38重量％的組成範圍内的硝酸鈉以利於 重氮化反應進行。向組合物中添加以溶劑總重量計介於 0.3-0.5重量％之間的溴化鈉穩定劑，且向組合物中添加以溶 劑總重量計介於〇· 1 5-0.35重量％之間的重氮化偶合劑_試劑 級對胺基苯磺酸。向組合物中添加以溶劑總體積計介於 4-4.5體積％之間的含有〇_1%乙基紅ipH指示劑，且向組合 物中添加以溶劑總體積計介於4_5 5體積％之間的包含多元 酉子之濕潤劑。將各試劑按所示順序溶解於其量介於3 ·3至3 $ 公升之間的作為溶劑之甲醇中。 當適當地混合配方溶液時，接著使紙帶基材穿過含有該 配方溶液的浴液。接著使經塗覆之紙基材穿過—米長之= 箱，該烘箱維持在7G.8()t之溫度範圍内。經塗覆之帶紙以、 介於每分鐘2.2至3.4米之間的速度穿過烘箱。從乾燥供箱退 出之經乾燥礦物酸伯測帶具有淡淡的或輕微的黃顏色。 【實施方式】 本發明係關於用於監測環堉中少成斗缺六士 衣吮Τ之礦物酸存在之壽命延長 I04346.doc 型確物酸偵測帶。用根據本發明之配方溶液浸透纖维素帶 氏基材（確火為自Whatman, Inc.麟得的Chroma-1)以提供具 有至少90天延長壽命之偵測帶。 配方溶液包含0.26 Μ氫氧化鈉加上0.009 Μ硼砂之pH緩 沒Γ /夜，其佔溶劑總體積之8_9體積％。或者，pH緩衝液可為 0‘28 Μ氫氧化鈉加上〇，15 M 3(環己基胺基）_丨_丙烷磺酸（下 文稱作CAPS)，其佔溶劑總體積之8_9體積％。藉由減少pH 緩衝液之量’帶敏感性得以增加而背景變黑作用亦增加。 將緩衝溶液之量增加至超過此範圍，導致配方溶液之敏感 性降低。利用pH緩衝物質及丙氡基化二醇濕潤劑穩定偵測 帶。 將以溶劑總重量計介於〇 〇7_〇.丨重量％之間的試劑級變 色駄偶合劑添加至配方溶液中。藉由增加配方中此偶合劑 之重’帶背景之背景變黑作用加速，歸因於導致偶合劑自 偶合之過量偶合劑。 配方溶液可視情況含有以溶劑總重量計約〇 〇5_0 .丨1重量 /〇的试劑級Ν-奈基乙二胺二鹽酸鹽（下文稱作nEd)。NED係 用於增加對鹽醆氣體之敏感性。背景變黑作用加速更快， 歸因於導致反應機制中發生自偶合之過量偶合劑。可選偶 合劑NED亦可選自由Ν，Ν·:曱基笨胺、亞胺基聯节及龍膽 酸組成之群。配方溶液進一步包括用於重氣化反應之亞硝 酸納°亞确酸納之量以溶劑總重量計介於0.25-0.38重量％ 之間。 又’該配方利用包含溴化鈉之穩定劑。穩定劑之量以溶 l()4346.doc 1337256 劑總重量計介於0 032_0 05重量％之間。 配方洛液進一步包括作為重氮化偶合劑之試劑級對胺基 苯續酸。偶合劑之量以溶劑總重量計介於〇15_0 35重量〇/〇 - 之間。偶合劑亦可選自由間胺基笨磺酸、鄰胺基笨曱酸、 間胺基乙酿笨胺及對硝基笨胺組成之群。配方溶液另外包 括以〉谷劑總體積計介於4_4 5體積％之間的含有〇.丨％乙基紅 之pH指示劑。pH指示劑在pH為約4.5時顯紅色且在pH為6.5 鲁 時顯貫色。藉由增加pH指示劑之量，在開始偵測時線性度 得到提高。希望與酸氣體接觸時顏色由無色/黃色變化至紅 色或藍色。用於配方溶液中的可接受之額外指示劑可選自 由乙基橙、甲基紅及皂黃組成之群。 最後，將以溶劑總體積計介於Π5體積％之間的濕潤劑 (包含一部分乙二醇及一部分丙氧基化丙三醇）添加至配方 浴液中。藉由降低多元醇中丙氧基化丙三醇之量，偵測帶 曝露於目標氣體時其敏感性得到增加。然而，帶背景變黑 • 作用更加迅速地發生。藉由增加此濕潤劑物質之量來降低 敏感性。可利用之其它濕潤劑為聚乙二醇或丙三醇。 將各試劑（包括dHM %谪菸槐A满丨丨、m丄人丄β _
降低。 如U)所示， 與樣品裔.中 >所示，配方溶液中所存在之亞硝酸根離子及芳族胺 氣流中所存在之酸氣體反應以形成中間體重氮鹽。 104346.doc 1337256 此重氮鹽之特徵在於含有重氮離子，其為親電子試劑，意 欲獲得可共享之電子物質以達到平衡。 ⑴
》+NaN〇2
H03S
2HX
N ^X'+Nax+lHaO
如（2)所示，重氮鹽與芳族偶合化合物變色酸偶合以形成 紅-橙色的偶氮錯合物。 (2)
NI^X' OH OH
此等錯合物在浸透之壽命延長型礦物酸偵測帶上為看得 見的色斑。色斑在帶上之強度與樣品流中所存在之毒性氣 體之量有關。
利用此酸偵測帶可偵測礦物酸，包括溴化氫、氣化氫、 氣化氫、換化氫、琐酸、硫酸、填酸及乙酸。 偵測帶包含纖維素紙基材，其在市場上售作Chroma-1。 藉由使紙帶穿過含有配方溶液之浴液，用配方溶液浸透紙 式偵測帶。接著使該帶穿過具有大約一米長度且維持在 70-80°C之間的烘箱。經浸透帶在烘箱中以一定速度前進以 提供在烘箱中介於約45至75秒之間的滯留時間。在退出烘 箱時，該帶具有淡淡的黃顏色且將其纏繞至帶盒上。 如圖1 -5中所示，與根據當前技術之樣品偵測帶D相比較 104346.doc -10- 而a ’用配方溶液之變體浸透紙式偵測帶以提供各種樣品 A-C。在圖1巧中，樣品A為利用含有硼砂及多元醇之pH緩 衝液的標準配方溶液，該多元醇為一部分乙二醇及一部分 丙氧基化丙三醇；樣品B為樣品A之標準配方溶液，其中該 PH緩衝液含有少於1〇%之丙氧基化丙三醇；樣品c為樣品a 之標準配方溶液，其中該pH緩衝液包括3_(環己基胺基 丙烧％ St (CAPS)，且樣品D為代表當前技術的含有對硝基 苯胺之紙式偵測帶，芳族胺發生反應以提供重氮鹽，其接 著與偶合化合物N-萘基伸乙基二鹽酸鹽反應。 特定而言，在圖1及圖2中，用配方溶液處理紙式偵測帶 樣品A-C且提供超過9〇天之穩定背景。特定而言，在圖1中， 背景在室溫條件下於i 00視覺計數内變化，在9〇天内有5〇/〇 落差，且在圖2中，在高溫條件下於100_300視覺計數内變 化 4曰示10 %落差。又，如圖3及圖4中所示，在室溫下（圖 3 )及向溫下（圖4)用配方溶液處理紙式偵測帶樣品A_c且在 至少9 0天内提供1 〇 %以内的敏感性，而習知之酸偵測帶（由 樣品D代表）導致介於約4〇_60%之間的敏感性落差。 另外，如圖5中所示’與現有酸偵測帶樣品〇相比較，用 配方浴液處理紙式谓測帶樣品A及C，對於低酸氣體濃度水 平而言’可提供增加之回應時間。 將以上圖解說明及描述當作本發明之優選實施例，儘管 如此’應瞭解該等描述及說明僅僅是示範性的且在不偏離 本發明精神之情況下可對其進行多種修改及調整。 【圖式簡單說明】 104346.doc

Claims (1)

  1. 十、申請專利範圍： 1 ♦ 一種用於偵測空氣流中礦物酸的浸透有一配方溶液之债 測帶，該配方溶液基本上係由下列成份組成：（a)以溶劑 總體積計濃度介於約8-9體積％之間的pH緩衝物質；（b)以 溶劑總重量計介於0.07-0,1〇重量％之間的第一偶合劑；（c) 與該酸氣體及重氮化偶合劑反應以形成重氮鹽之亞硝酸 鈉，該亞硝酸鈉具有以溶劑總重量計介於約0.25-0.3 8重 量％之間的濃度；（d)以溶劑總重量計介於約0.30-0.50重 量％之間的溴化鈉穩定劑；（e)以溶劑總重量計介於約 〇.1 5-0.35重量％之間的該重氮化偶合劑；（f)以溶劑總體積 叶介於4-4.5體積。/〇之間的pH指示劑；及（g)以溶劑總體積 計介於4-5.5重量％之間的包含多元醇之濕潤劑，該配方溶 液之各成份係溶解於3_3至3.5公升甲醇溶劑中。 2·如請求項1之偵測帶，其中該pH緩衝物質係選自基本上由 0.26 Μ氫氧化鈉及0.009 Μ硼酸鈉或0.028 Μ氫氧化納及 〇·15 Μ 3-(環己基胺基）-1·丙磺酸或0.26 Μ氩氧化納及 〇·〇12 Μ碳酸氫鈉組成之群。 3.如請求項1之偵測帶，其中該第一偶合劑為試劑級變色 酸。 4*如請求項丨之偵測帶，其中該重氮化偶合劑係選自基本上 由試劑級磺胺酸、間胺基苯磺酸、鄰胺基苯甲酸、間胺 基乙酿笨胺及對硝基苯胺組成之群。 5 ·如叫求項1之偵測帶，其中該pH指示劑係選自基本上由乙 基紅、乙基橙、甲基紅及皂黃組成之群。 I04346.doc 1337256 6 ·如請求項1之偵剛帶，盆φ兮、、a袖+ 〃中6亥濕潤劑係選自基本上由-部 分乙二醇加上一部分丙童其 刀内氣基A丙二#或聚乙二醇或丙三 醇組成之群。 如請求項1之偵測帶’其中該配方溶液進-步包括在添加 該漢化鈉穩定劑之後添加至該配方溶液中之第二偶合 劑0 · 8·如請求項7之偵測帶，其中該第二偶合劑係選自基本上由 試劑級N-〇-萘基）乙二胺二鹽酸鹽、N，N-二曱基苯胺、亞 胺基聯节及龍膽酸組成之群。
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