MDD112B-N-040-N2L-130PA0按照 智能壓力變送器 待測物質(zhì)的性質(zhì)不同,測定法分為下列3種。各種類項(xiàng)下未注明時,均系指第一法。
第一法 測定不易粉碎的固體藥品(如脂肪、脂肪酸、石蠟、羊毛脂等)。
MDD112B-N-040-N2L-130PA0取供試品,留意用盡可能低的溫度熔融后,吸入兩端啟齒的毛細(xì)管(同第一法,但管端不熔封)中,使高達(dá)約10mm。在10℃或10℃以下的冷處靜置24小時,或置冰上放冷不少于2小時,凝固后用橡皮圈將毛細(xì)管緊縛在溫度計(同第一法)上,使毛細(xì)管的內(nèi)容物適在溫度計汞球中部。照第一法將毛細(xì)管連同溫度計浸入傳溫液中,供試品的上端應(yīng)適在傳溫液液面下約10mm處;當(dāng)心加熱,俟溫度上升至較規(guī)則的熔點(diǎn)低限尚低約5℃時,調(diào)理升溫速率使每分鐘上升不超越0.5℃,至供試品在毛細(xì)管中開端上升時,檢讀溫度計上顯現(xiàn)的溫度,即得。
第二法 測定易粉碎的固體藥品。
MDD112B-N-040-N2L-130PA0取供試品適量,研成細(xì)粉,除另有規(guī)則外,應(yīng)依照各藥品項(xiàng)下枯燥失重的條件停止枯燥。智能壓力變送器藥品為不檢查枯燥失重、熔點(diǎn)范圍低限在135℃以上、受熱不合成的供試品,可采用105℃枯燥;熔點(diǎn)在135℃以下或受熱合成的供試品,可在五氧化二磷枯燥器中枯燥過夜或用其他適合的枯燥辦法枯燥,如恒溫減壓枯燥。
MDD112B-N-040-N2L-130PA0分取供試品適量,置熔點(diǎn)測定用毛細(xì)管(簡稱毛細(xì)管,由中性硬質(zhì)玻璃管制成,長9cm以上,內(nèi)徑0.9~1.1mm,壁厚0.10~0.15mm,一端熔封;當(dāng)所用溫度計浸入傳溫液在6cm以上時,管長應(yīng)恰當(dāng)增加,使顯露液面3cm以上)中,輕擊管壁或借滋長短適合的干凈玻璃管,垂直放在外表皿或其他適合的硬質(zhì)物體上,將毛細(xì)管自上口放入使自在落下,重復(fù)數(shù)次,使粉末嚴(yán)密集結(jié)在毛細(xì)管的熔封端。裝入供試品的高度為3mm。另將溫度計(分浸型,具有0.5℃刻度,經(jīng)熔點(diǎn)測定用對照品校正)放入盛裝傳溫液(熔點(diǎn)在80℃以下者,用水;熔點(diǎn)在80℃以上者,用硅油或液狀石蠟)的容器中,使溫度計汞球部的底端與容器的底部間隔2.5cm以上(用內(nèi)加熱的容器,溫度計汞球與加熱器上外表間隔2.5cm以上);參加傳溫液以使傳溫液受熱后的液面適在溫度計的分浸線處。將傳溫液加熱,俟溫度上升至較規(guī)則的熔點(diǎn)低限約低10℃時,將裝有供試品的毛細(xì)管浸入傳溫液,貼附在溫度計上(可用橡皮圈或毛細(xì)管夾固定),位置須使毛細(xì)管的內(nèi)容物局部適在溫度計汞球中部;繼續(xù)加熱,調(diào)理升溫速率為每分鐘上升1.0~1.5℃,智能壓力變送器加熱時須不時攪拌使傳溫液溫度堅持平均,記載供試品在初熔至全熔時的溫度,反復(fù)測定3次,取其均勻值,即得?!俺跞邸毕抵腹┰嚻吩诿?xì)管內(nèi)開端部分液化呈現(xiàn)明顯液滴MDD112B-N-040-N2L-130PA0時的溫度。 “全熔”系指供試品全部液化時的溫度。測定熔融同時合成的供試品時,辦法如上述,但調(diào)理升溫速率使每分鐘上升2.5~3.0℃;供試品開端部分液化時(或開端產(chǎn)生氣泡時)的溫度作為初熔溫度;供試品固相消逝全部液化時的溫度作為全熔溫度。遇有固相消逝不明顯時,應(yīng)以供試品合成物開端收縮上升時的溫度作為全熔溫度。某些藥品無法分辨其初熔、全熔時,能夠其發(fā)作突變時的溫度作為熔點(diǎn)。
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