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          溶解熱法測定水泥水化熱的實驗步驟介紹

          時間:2022-01-18 09:37 點擊:

            水泥遇水后發生一系列物理化學反應時放出的熱量稱為水化熱,以J/g表示。水泥的水化熱和放熱速度直接關系到混凝土工程的質量。在大體積混凝土結構中甚至能產生幾十度的溫差,巨大的溫度應力會導致混凝土開裂,加大了混凝土被腐蝕的速率。水化熱測試對水泥的生產、使用及理論研究都非常重要。水泥水化熱測試分為直接法(代用法)、間接法(基準法)兩種。

            溶解熱法測定水泥水化熱:

            溶解熱法也稱為基準法,溶解熱法在國際上具有較大的通用性和可比性,尤其適用于測定水泥長齡期水化熱。

            實驗原理:

            依據蓋斯定律,化學反應的熱效應只與體系的初態和終態有關而與反應的途徑無關。它是在熱量計周圍溫度一定的條件下,用未水化的水泥和水化一定齡期的水泥分別在一定濃度的標準酸溶液中溶解,測得溶解熱之差,作為該水泥在該齡期內所放出的水化熱。

            儀器設備:

            ①熱量計、保溫水槽、內筒、廣口保溫瓶、貝克曼差示溫度計、攪拌裝置、曲頸玻璃漏斗、直頸裝酸漏斗

           ?、谔炱?/span>

            ③高溫爐

           ?、芎銣厥?/span>

           ?、菟嗨嚇悠?/span>

            試劑:

            ①氧化鋅:標定熱量計熱容量

           ?、贖F溶液

            ③(2±0.02)mol/L的硝酸溶液

            實驗步驟:

           ?、贅硕崃坑嫙崛萘緾

            貝氏溫度計或量熱溫度計、保溫瓶及塑料內襯、攪拌棒等應編號配套使用。使用貝氏溫度計試驗前應用量熱溫度計檢查貝氏溫度計零點。如果使用量熱溫度計,可直接測定。

            在標定熱量計熱容量的前24 h應將保溫瓶放入內筒中,酸液攪拌棒放入保溫瓶內,再將內筒放入恒溫水槽內。使恒溫水槽內的水溫調整并保持到(20士0.1)℃。

            稱取(13.5士0.5)℃的(2.00士0.02)mo1/L硝酸溶液約410 g,量取8 ml 40%氫氟酸加人量杯內,再加入少量剩余的硝酸溶液,用直頸加酸漏斗加到保溫瓶內,插入貝氏溫度計或量熱溫度計,中途不應拔出避免溫度散失。

            用攪拌棒攪拌20 min后,在溫度計上讀出溫度,此后每隔5min讀數一次,連續15 min,每5 min上升的溫度差值相等時(或三次溫度差值在0.002℃內為止。記錄最后一次酸液溫度,此溫度值即為初測讀數。

            將稱量好的(7士0.001)g氧化鋅徐徐加入保溫瓶酸液中,加料過程須在2 min內完成。

            從讀出初測讀數起分別測讀20min、40 min、60min、80 min、90 min、120min時溫度計的讀數。

            熱量計在各時間內的熱容量按下式計算,計算結果保留至0.1。

            式中:

            C—熱量計熱容量,單位為焦耳每攝氏度((J/℃);

            G0——氧化鋅重量,單位為克(g);

            T—氧化鋅加人熱量計時的室溫,單位為攝氏度(℃);

            Ta——θa加貝氏溫度計0℃時相應的攝氏溫度(如使用量熱溫度計時,ta的數值等于θa的讀數)單位為攝氏度(℃);

            R0—經校正的溫度上升值,單位為攝氏度(℃);

            1072.0—氧化鋅在30℃時溶解熱,單位為焦耳每克(J/g);

            0.4—溶解熱負溫比熱容,單位為焦耳每克攝氏度[J/(g·℃)];

            0.5—氧化鋅比熱容,單位為焦耳每克攝氏度[J/(g·℃)〕。

            R0值按下式計算,計算結果保留至0.001℃:

            式中:

            θ—初測期結束時(即開始加氧化鋅時)的溫度計讀數,單位為攝氏度(℃);

            Θa—溶解期第一次測讀的貝氏溫度計或量熱溫度計的讀數,單位為攝氏度(℃);

            Θb—溶解期結束時測讀的貝氏溫度計或量熱溫度計的讀數,單位為攝氏度(℃);

            熱量計熱容量應平行標定兩次,以兩次標定值的平均值作為標定結果。如果兩次標定值相差大于5.0J/℃時,應重新標定。

            在下列情況下,熱容量應重新標定:

            a)重新調整貝氏溫度計時;

            b)當溫度計、保溫瓶、攪拌棒更換或重新涂覆耐酸涂料時;

            c)當新配制的酸液與標定熱量計熱容量的酸液濃度變化大于士0.02 mol/L時;

            d)對試驗結果有疑問時。

           ?、谖此嗳芙鉄岬臏y定

            A.進行準備工作和初測期試驗,并記錄初測溫度θ0’;

            B.讀出初測溫度后,立即將一份水泥試樣在2min內加入酸液中,然后按各品種水泥測讀溫度的時間,準時讀記貝氏溫度計讀數θa和θb。第二份試樣重復第一份的操作。

            C.余下二份試樣置于(900-950)℃下灼燒90min,灼燒后立即將盛有試樣的坩堝置于干燥器內冷卻至室溫,并快速稱量。灼燒質量G1以二份試樣灼燒后的質量平均值確定,如二份試樣的灼燒質量相差大于0.003 g時,應重新補做。

            D.未水化水泥的溶解熱按下式計算,計算結果保留至0.1。

            式中:

            q1—未水化水泥試樣的溶解熱,單位為焦耳每克((J/g);

            C—對應測讀時間的熱量計熱容量,單位為焦耳每攝氏度(J/℃);

            G1—未水化水泥試樣灼燒后的質量,單位為克(g);

            T’—未水化水泥試樣裝人熱量計時的室溫,單位為攝氏度(℃);

            ta’—未水化水泥試樣溶解期第一次測讀數θa’加貝氏溫度計0℃時相應的攝氏溫度;

            R1—經校正的溫度上升值,單位為攝氏度(℃);

            0.8—未水化水泥試樣的比熱容,單位為焦耳每克攝氏度[J/(g.℃)]。

            R1值按下式計算,計算結果保留至0.001℃:

            E.未水化水泥試樣的溶解熱以兩次測定值的平均值作為測定結果,如兩次測定值相差大于10.0J/g時,應進行第三次試驗,其結果與前試驗中一次結果相差小于10.0 J/g時,取其平均值作為測定結果,否則應重做試驗。

           ?、鄄糠炙嗳芙鉄岬臏y定

            A.在測定未水化水泥試樣溶解熱的同時,制備部分水化水泥試樣。測定兩個齡期水化熱時,稱100 g水泥加40 mL蒸餾水,充分攪拌3 min后,取近似相等的漿體二份或多份,分別裝入符合要求的試樣瓶中,置于(20士1)℃的水中養護至規定齡期。

            B.進行準備工作和初測期試驗,并記錄初測溫度θ0‘’。

            C.從養護水中取出一份達到試驗齡期的試樣瓶,取出水化水泥試樣,搗碎研磨至全部通過0.60 mm方孔篩,混合均勻放人磨口稱量瓶中,并稱出4.200 g士0.050 g(精確至0.001lg)試樣四份,然后存放在濕度大于50%的密閉容器中,稱好的樣品應在20min內進行試驗。兩份供作溶解熱測定,另兩份進行灼燒。從開始搗碎至放入稱量瓶中的全部時間應不大于10min。

            D.讀出初測期結束時的溫度后,立即將稱量好的一份試樣在2min內加酸液中,然后按規定不同水泥品種的測讀時間,準時讀記貝氏溫度計或量熱溫度計讀數。第二份試樣重復第一份的操作。

            E.余下二份試樣進行灼燒。

            F.經水化某一齡期后水泥的溶解熱按下式計算,計算結果保留至0.1 J/g:

            式中:

            q2—經水化某一齡期后水化水泥試樣的溶解熱,單位為焦耳每克(J/g);

            C—對應測讀時間的熱量計熱容量,單位為焦耳每攝氏度((J/℃);

            G2—某一齡期水化水泥試樣灼燒后的質量,單位為克(g);

            T’’—水化水泥試樣裝入熱量計時的室溫,單位為攝氏度(℃);

            ta’’—水化水泥試樣溶解期第一次測讀數加貝氏溫度計0℃時相應的攝氏溫度,單位為攝氏度(℃);

            Ta’—未水化水泥試樣溶解期第一次測讀數加貝氏溫度計0℃時相應的攝氏溫度,單位為攝氏度(℃);

            R2—經校正的溫度上升值,單位為攝氏度(℃);

            1.7—水化水泥試樣的比熱容,單位為焦耳每克攝氏度[J/(g℃)];

            1.3—溫度校正比熱容,單位為焦耳每克攝氏度〔J/(g℃)〕。

            E.部分水化水泥試樣的溶解熱測定結果按規定進行。

            ④水泥水化熱結果計算

            水泥在某一水化齡期前放出的水化熱按下式計算,計算結果保留至1:

            式中:

            q—水泥試樣在某一水化齡期放出的水化熱,單位為焦耳每克(J/g);

            q1—未水化水泥試樣的溶解熱,單位為焦耳每克(J/g);

            q2—水化水泥試樣在某一水化齡期的溶解熱,單位為焦耳每(J/g);

            ta’—未水化水泥試樣溶解期第一次測讀數加貝氏溫度計0℃時相應的攝氏溫度,單位為攝氏度(℃);

            0.4—溶解熱的負溫比熱容,單位為焦耳每克攝氏度[J/(g·℃)]。

            注意事項

           ?、貱O2與水泥作用的影響:本試驗造成誤差的最大因素在于水化的水泥樣品處理過程中吸收了CO2,使部分水化的水泥試樣溶解熱降低,導致水化熱結果偏高。

           ?、跓Я康挠绊?/span>

           ?、蹆x器熱容量的影響

           ?、軠y讀溫度數的誤差

           ?、菟嚇佑昧?/span>

           ?、奘覝氐挠绊?/span>

            ⑦水灰比的影響


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