JP3528048B2 - Determination of pozzolan in cement - Google Patents
Determination of pozzolan in cementInfo
- Publication number
- JP3528048B2 JP3528048B2 JP2000288175A JP2000288175A JP3528048B2 JP 3528048 B2 JP3528048 B2 JP 3528048B2 JP 2000288175 A JP2000288175 A JP 2000288175A JP 2000288175 A JP2000288175 A JP 2000288175A JP 3528048 B2 JP3528048 B2 JP 3528048B2
- Authority
- JP
- Japan
- Prior art keywords
- pozzolan
- cement
- amount
- aqueous solution
- cement composition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 239000004568 cement Substances 0.000 title claims description 114
- 239000000203 mixture Substances 0.000 claims description 60
- 239000007864 aqueous solution Substances 0.000 claims description 42
- 238000000034 method Methods 0.000 claims description 38
- 230000002378 acidificating effect Effects 0.000 claims description 33
- 239000000047 product Substances 0.000 description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- 238000002156 mixing Methods 0.000 description 12
- 238000004090 dissolution Methods 0.000 description 9
- 239000011398 Portland cement Substances 0.000 description 7
- 239000002253 acid Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 239000002893 slag Substances 0.000 description 6
- 239000010881 fly ash Substances 0.000 description 5
- 238000003908 quality control method Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000002956 ash Substances 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- 239000003245 coal Substances 0.000 description 3
- 238000002309 gasification Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 238000003745 diagnosis Methods 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012916 structural analysis Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229910021487 silica fume Inorganic materials 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004056 waste incineration Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、セメント組成物中
のポゾラン定量方法、及びセメント硬化体中の未反応ポ
ゾラン定量方法に関する。TECHNICAL FIELD The present invention relates to a method for quantifying pozzolan in a cement composition and a method for quantifying unreacted pozzolan in a hardened cement product.
【０００２】[0002]
【従来の技術】近年の環境問題への関心の高まりと共
に、石炭火力発電に伴って発生するフライアッシュや石
炭ガス化スラグ、更には、都市ゴミ焼却灰溶融スラグな
どのシリカ質ポゾランをセメント混和材や細骨材の代替
品として利用しようとする気運が高まってきた。また、
一方では、特開平１１−１３９８６０号公報に記載され
ている様に、シリカ質ポゾランが持つ「反応が徐々に進
行する」という性質を生かした材料開発もなされてい
る。2. Description of the Related Art With the recent increasing interest in environmental problems, fly ash and coal gasification slag generated by coal-fired power generation, and siliceous pozzolan such as municipal waste incineration ash molten slag are used as cement admixtures. There is a growing desire to use it as a substitute for fine aggregate. Also,
On the other hand, as described in Japanese Patent Application Laid-Open No. 11-139860, material development has been carried out by taking advantage of the property that the siliceous pozzolan "reacts gradually".
【０００３】しかしながら、これらのセメント組成物
は、現行ＪＩＳのフライアッシュポルトランドセメント
中のフライアッシュ混和率の上限である３０％と比べて
シリカ質ポゾランの混合率が多いことから、製造後の品
質管理に問題のあることが明らかとなってきた。即ち、
セメント組成物中に含まれるシリカ質ポゾランの定量方
法としては、通常は、塩酸水溶液にセメント組成物を溶
解させて、溶解残分量からはポゾランの含有率を求める
方法が採用されているが、この様な方法では、ポゾラン
混合率の高いセメント組成物の場合には、セメント成分
が溶解した後もｐＨが低く維持されるために、ポゾラン
が溶解して酸溶解残分量が相対的に低下し、ポゾラン含
有率を正確に求めることができず、セメント製造時や受
け入れ時の品質管理方法としては適さないという問題が
新たに生じてきた。However, since these cement compositions have a large mixing ratio of siliceous pozzolan in comparison with 30% which is the upper limit of the fly ash mixing ratio in the current JIS fly ash Portland cement, the quality control after production is high. Has become apparent. That is,
As a method for quantifying the siliceous pozzolan contained in the cement composition, usually, a method of dissolving the cement composition in an aqueous hydrochloric acid solution and determining the content rate of pozzolan from the residual amount of dissolution is adopted. In such a method, in the case of a cement composition having a high pozzolan mixing ratio, since the pH is maintained low even after the cement components are dissolved, the pozzolan is dissolved and the acid dissolution residual amount is relatively reduced, There is a new problem that the pozzolan content cannot be accurately determined and is not suitable as a quality control method during cement production or acceptance.
【０００４】[0004]
【発明が解決しようとする課題】本発明の主な目的は、
シリカ質ポゾラン混合比の高いセメント組成物であって
も、簡単な操作でポゾラン含有率を正確に定量できる方
法を提供することである。The main object of the present invention is to:
It is an object of the present invention to provide a method capable of accurately quantifying the pozzolan content by a simple operation even with a cement composition having a high siliceous pozzolan mixing ratio.
【０００５】[0005]
【課題を解決するための手段】本発明者は、上記した目
的を達成すべく鋭意研究を重ねてきた。その結果、シリ
カ質ポゾランを含有するセメント組成物を酸性水溶液に
溶解する際に、水溶液のｐＨを特定の範囲に維持するこ
とによって、セメント組成物中のポゾラン混合比に無関
係にポゾラン量を正確に定量することが可能となり、更
に、この方法は、セメント硬化物中の未反応ポゾランの
定量方法としても有効であることを見出し、ここに本発
明を完成するに至った。The inventor of the present invention has conducted extensive studies in order to achieve the above object. As a result, when a cement composition containing siliceous pozzolan is dissolved in an acidic aqueous solution, by maintaining the pH of the aqueous solution in a specific range, the pozzolan amount can be accurately measured regardless of the pozzolan mixing ratio in the cement composition. It has become possible to quantify, and further, this method has been found to be effective as a method for quantifying unreacted pozzolan in a hardened cement product, and the present invention has been completed here.
【０００６】即ち、本発明は、以下のポゾランの定量方
法を提供するものである。
１． セメント及びシリカ質ポゾランからなるセメント
組成物をｐＨ１．３〜２．７の範囲の酸性水溶液に溶解
し、不溶残分量からポゾラン量を求めることを特徴とす
るセメント組成物中のポゾランの定量方法。That is, the present invention provides the following method for quantifying pozzolan. 1. A method for quantifying pozzolan in a cement composition, which comprises dissolving a cement composition comprising cement and siliceous pozzolan in an acidic aqueous solution having a pH range of 1.3 to 2.7, and determining the amount of pozzolan from the amount of insoluble residue.
【０００７】２． セメント、シリカ質ポゾラン及び骨
材を含有するセメント組成物をｐＨ１．３〜２．７の範
囲の酸性水溶液に溶解し、不溶残分量と骨材の不溶残分
見積量に基づいて、ポゾラン量を求めることを特徴とす
るセメント組成物中のポゾランの定量方法。
３． セメント及びシリカ質ポゾランからなるセメント
組成物から形成されたセメント硬化体を、ｐＨ１．３〜
２．７の範囲の酸性水溶液に溶解し、不溶残分量から未
反応ポゾラン量を求めることを特徴とするセメント硬化
体中の未反応ポゾランの定量方法。
４． セメント、シリカ質ポゾラン及び骨材を含有する
セメント組成物から形成されたセメント硬化体を、ｐＨ
１．３〜２．７の範囲の酸性水溶液に溶解し、不溶残分
量と骨材の不溶残分見積量に基づいて、未反応ポゾラン
量を求めることを特徴とするセメント硬化体中の未反応
ポゾランの定量方法。
５． 酸性水溶液のｐＨが１．７〜２．３の範囲である
上記項１〜４のいずれかに記載の方法。
６． セメント組成物又はセメント硬化物を酸性水溶液
に溶解する際に、ｐＨの変動幅を０．２以内に維持する
ことを特徴とする上記項１〜５のいずれかに記載の方
法。2. A cement composition containing cement, siliceous pozzolan and aggregate is dissolved in an acidic aqueous solution having a pH range of 1.3 to 2.7, and the amount of pozzolan is determined based on the amount of insoluble residue and the estimated amount of insoluble residue of aggregate. A method for quantifying pozzolan in a cement composition, which is characterized by being obtained. 3. A cement hardened body formed from a cement composition composed of cement and siliceous pozzolan has a pH of 1.3 to
A method for quantifying unreacted pozzolan in a hardened cement product, which comprises dissolving in an acidic aqueous solution in the range of 2.7 and determining the amount of unreacted pozzolan from the amount of insoluble residue. 4. A cement hardened body formed from a cement composition containing cement, a siliceous pozzolan and an aggregate is treated with pH.
Unreacted in hardened cement, characterized by being dissolved in an acidic aqueous solution in the range of 1.3 to 2.7, and determining the amount of unreacted pozzolan based on the amount of insoluble residue and the estimated amount of insoluble residue of aggregate. A method for quantifying pozzolan. 5. Item 5. The method according to any one of Items 1 to 4, wherein the pH of the acidic aqueous solution is in the range of 1.7 to 2.3. 6. Item 6. The method according to any one of Items 1 to 5, wherein the pH fluctuation range is maintained within 0.2 when the cement composition or the cement hardened product is dissolved in an acidic aqueous solution.
【０００８】[0008]
【発明の実施の形態】本発明のポゾランの定量方法で
は、セメント及びシリカ質ポゾランを含有するセメント
組成物をｐＨ１．３〜２．７の範囲内に維持した酸性水
溶液に溶解し、不溶残分量からポゾラン量を算出する。BEST MODE FOR CARRYING OUT THE INVENTION In the method for quantifying pozzolan of the present invention, a cement composition containing cement and siliceous pozzolan is dissolved in an acidic aqueous solution maintained within a pH range of 1.3 to 2.7, and the amount of insoluble residue is determined. The amount of pozzolan is calculated from
【０００９】従来のセメント組成物中のポゾランの定量
方法では、一般的に、（１＋１００）塩酸水溶液を用
い、これにセメント組成物を溶解して不溶残分量からポ
ゾラン含有量を求めていた。しかしながら、この方法で
は、ポルトランドセメントの含有率が多いセメント組成
物については、ポルトランドセメント部分がシリカ質ポ
ゾランと比べて酸に溶解し易いために、ポルトランドセ
メント部分の溶解が優先して溶解後のｐＨが上昇し、シ
リカ質ポゾランの溶解が進行し難いのに対して、シリカ
質ポゾランの含有率が高いセメント組成物については、
ポルトランドセメント部分の溶解後も溶液のｐＨが低く
維持されるためにシリカ質ポゾランの溶解が進行し、不
溶残分量からはポゾランの含有量を正確に求めることが
できない。In the conventional method for quantifying pozzolan in a cement composition, an aqueous solution of (1 + 100) hydrochloric acid was generally used, and the cement composition was dissolved in the aqueous solution to determine the pozzolan content from the amount of insoluble residue. However, in this method, for a cement composition having a high content ratio of Portland cement, since the Portland cement portion is more easily dissolved in an acid than the siliceous pozzolan, the dissolution of the Portland cement portion is prioritized and the pH after dissolution is preferentially dissolved. Increase, the dissolution of the siliceous pozzolan is difficult to proceed, while for the cement composition having a high siliceous pozzolan content,
Since the pH of the solution is kept low even after the dissolution of the Portland cement portion, the dissolution of the siliceous pozzolan proceeds, and the pozzolan content cannot be accurately determined from the insoluble residue amount.
【００１０】本発明者の研究によれば、ｐＨを１．３〜
２．７の範囲に維持した酸性水溶液に、シリカ質ポゾラ
ンを含有するセメント組成物を溶解する場合には、セメ
ント組成物中のセメント部分についてはほぼ完全に溶解
するのに対して、シリカ質ポゾランについては実質的に
溶解することなく、不溶残分となることが明らかとなっ
た。このために、ｐＨ１．３〜２．７の範囲内の酸性水
溶液にシリカ質ポゾランを含有するセメント組成物を溶
解させ、不溶残分量をポゾラン量と見なすことによっ
て、セメント組成物中のポゾラン混合比とは無関係に、
正確にポゾラン量を求めることができる。According to the research conducted by the present inventor, the pH value is 1.3 to
When the siliceous pozzolan-containing cement composition is dissolved in the acidic aqueous solution maintained in the range of 2.7, the cement portion in the cement composition is almost completely dissolved, whereas the siliceous pozzolan is dissolved. It was revealed that the above compound did not substantially dissolve and became an insoluble residue. Therefore, the cement composition containing siliceous pozzolan is dissolved in an acidic aqueous solution having a pH range of 1.3 to 2.7, and the insoluble residue amount is regarded as the pozzolan amount, whereby the pozzolan mixing ratio in the cement composition is increased. Irrespective of
The amount of pozzolan can be accurately determined.
【００１１】本発明の方法では、セメント組成物を溶解
させる酸性水溶液のｐＨは、１．３〜２．７の範囲内に
維持することが必要であり、１．７〜２．３の範囲内に
維持することが好ましい。酸性水溶液のｐＨは上記した
範囲内であればよいが、セメント組成物を酸性水溶液に
溶解する際に、ｐＨの変動ができるだけ小さいことが望
ましく、特に、ｐＨの変動幅を０．２以内に維持するこ
とが好ましく、ｐＨの変動幅を０．１以内に維持するこ
とがより好ましい。酸性水溶液のｐＨを所定の範囲に調
整するには、塩酸、硝酸、硫酸等のフッ酸以外の酸を用
いれば良く、特に、塩酸を用いることが好ましい。In the method of the present invention, the pH of the acidic aqueous solution in which the cement composition is dissolved needs to be maintained within the range of 1.3 to 2.7, and within the range of 1.7 to 2.3. It is preferable to maintain at. The pH of the acidic aqueous solution may be within the above range, but it is desirable that the fluctuation of the pH is as small as possible when the cement composition is dissolved in the acidic aqueous solution, and in particular, the fluctuation range of the pH is maintained within 0.2. It is preferable to maintain the fluctuation range of pH within 0.1. In order to adjust the pH of the acidic aqueous solution within a predetermined range, an acid other than hydrofluoric acid such as hydrochloric acid, nitric acid or sulfuric acid may be used, and hydrochloric acid is particularly preferably used.
【００１２】本発明の方法では、セメント組成物の溶解
に伴って水溶液のｐＨが上昇するので、酸性水溶液のｐ
Ｈを所定の範囲内に維持するためには、適当な間隔で酸
性水溶液のｐＨを測定し、ｐＨ値が所定の範囲内になる
ように酸又は酸の水溶液を添加すればよい。例えば、ｐ
Ｈ電極を酸性水溶液中に浸漬し、ｐＨ値を連続的に検出
してコンピューターにデータを送り、ｐＨ値の変動に基
づいて、滴定装置により酸又は酸水溶液を自動的に添加
することにより、ｐＨ値を自動的に一定範囲内に維持す
ることができる。In the method of the present invention, since the pH of the aqueous solution rises as the cement composition is dissolved, the p
In order to maintain H within a predetermined range, the pH of the acidic aqueous solution may be measured at appropriate intervals, and an acid or an aqueous solution of acid may be added so that the pH value falls within the predetermined range. For example, p
By immersing the H electrode in an acidic aqueous solution, continuously detecting the pH value and sending the data to a computer, and by automatically adding an acid or an acid aqueous solution by a titrator based on the fluctuation of the pH value, The value can be automatically kept within a certain range.
【００１３】酸性水溶液の液温は、０〜５０℃程度、好
ましくは１０〜３０℃程度の範囲内とすれば良く、通常
は、室温で用いればよい。酸性水溶液中へのセメント組
成物の溶解時間は特に限定的ではなく、試料の量に応じ
て、試料中のセメント部分の溶解が完全に進行するまで
溶解させれば良く、通常は、２０分から５時間程度の溶
解時間とすればよい。The temperature of the acidic aqueous solution may be in the range of about 0 to 50 ° C., preferably about 10 to 30 ° C., and usually it may be used at room temperature. The dissolution time of the cement composition in the acidic aqueous solution is not particularly limited, and it may be dissolved until the cement portion in the sample is completely dissolved depending on the amount of the sample, and usually 20 minutes to 5 minutes. The dissolution time may be about time.
【００１４】本発明の測定対象とするセメント組成物で
は、セメントの種類については特に限定はなく、例え
ば、ポルトランドセメント等を対象とすることができ
る。また、ポゾランとしてはシリカ質ポゾランが測定対
象となり、ＳｉＯ2含有率が４０重量％以上、好ましく
は５０重量％以上のポゾランが適当である。この様なシ
リカ質ポゾランの具体例としては、フライアッシュ、石
炭ガス化スラグ、焼却灰溶融スラグ、シリカフューム、
もみがら灰、天然ポゾラン等を挙げることができる。In the cement composition to be measured according to the present invention, the type of cement is not particularly limited, and for example, Portland cement or the like can be targeted. As the pozzolan, a siliceous pozzolan is to be measured, and a pozzolan having a SiO 2 content of 40% by weight or more, preferably 50% by weight or more is suitable. Specific examples of such siliceous pozzolan include fly ash, coal gasification slag, incinerated ash molten slag, silica fume,
Examples include chaff ash and natural pozzolan.
【００１５】酸性水溶液中に形成された不溶残分量を秤
量する方法については、特に限定的ではないが、通常、
吸引ろ過装置を用いて、ろ紙（５種Ｃ）で吸引ろ過し、
温水で１０回程度洗浄した後、ろ紙と共に残留物をるつ
ぼに入れて乾燥させ、その後、徐々に加熱してろ紙を灰
化させ、９５０℃±５０℃程度に調節した電気炉中で１
時間程度強熱した後、デシケーター中で放冷し、秤量す
ることによって、不溶残分量を求めることができる。The method for weighing the amount of the insoluble residue formed in the acidic aqueous solution is not particularly limited, but it is usually
Using a suction filtration device, suction filter with filter paper (5 types C),
After washing about 10 times with warm water, put the residue in a crucible together with the filter paper to dry it, and then gradually heat it to incinerate the filter paper and put it in an electric furnace adjusted to about 950 ° C ± 50 ° C.
After igniting for about an hour, it is allowed to cool in a desiccator and weighed to determine the amount of insoluble residue.
【００１６】この様にした求めた不溶残分量を、試料と
したセメント組成物中のポゾラン量と見なすことによっ
て、セメント組成物中のポゾランの含有率を求めること
ができる。The content of pozzolan in the cement composition can be determined by considering the thus obtained amount of insoluble residue as the amount of pozzolan in the sample cement composition.
【００１７】また、セメント組成物中に骨材が含まれる
場合には、上記酸性水溶液にセメント組成物を溶解した
不溶残分中に骨材に基づく不溶残分が含まれる場合があ
る。この様な場合には、測定試料を溶解するものと同様
のｐＨ値の酸性水溶液中に骨材を溶解した場合に不溶分
として残存する骨材の割合を予め求めておき、セメント
組成物中の骨材の配合割合に基づいて骨材に基づく不溶
残分量を見積もり、測定対象とするセメント組成物の不
溶残分量から骨材の不溶残分の見積量を除いた量をポゾ
ラン量とすることによって、骨材を含有するセメント組
成物中のポゾランの含有率を求めることができる。When the cement composition contains an aggregate, an insoluble residue based on the aggregate may be contained in the insoluble residue obtained by dissolving the cement composition in the acidic aqueous solution. In such a case, when the aggregate is dissolved in an acidic aqueous solution having the same pH value as that for dissolving the measurement sample, the proportion of the aggregate remaining as an insoluble matter is obtained in advance, and By estimating the amount of insoluble residue based on the aggregate based on the blending ratio of the aggregate, and taking the amount of pozzolan as the amount of the insoluble residue of the cement composition to be measured minus the estimated amount of the insoluble residue of the aggregate The content of pozzolan in the cement composition containing aggregate can be determined.
【００１８】本発明のポゾランの定量方法によれば、ポ
ゾラン含有率の高いセメント組成物であっても、ポゾラ
ン含有率を正確に測定することができる。従って、セメ
ント組成物の製造工程において、製品を定期的にサンプ
リングして、本発明方法によってポゾラン含有率を求め
ることにより、ポゾラン含有率の高いセメント組成物に
ついても、製品の品質管理を適切に行うことができる。
更に、本発明の方法は、セメント製品の出荷時、セメン
ト製品の購入時等においても、品質管理のためのポゾラ
ン定量方法として非常に有効である。According to the method for quantifying pozzolan of the present invention, the pozzolan content can be accurately measured even in a cement composition having a high pozzolan content. Therefore, in the manufacturing process of the cement composition, the product is regularly sampled and the pozzolan content is determined by the method of the present invention, so that the quality control of the product is appropriately performed even for the cement composition having a high pozzolan content. be able to.
Furthermore, the method of the present invention is very effective as a pozzolan quantification method for quality control even at the time of shipping cement products, when purchasing cement products, and the like.
【００１９】また、本発明のポゾラン定量方法は、セメ
ント及びシリカ質ポゾランからなるセメント組成物から
形成されたセメント硬化体に含まれる未反応ポゾランの
定量方法としても利用することができる。例えば、セメ
ント硬化体の一部をボーリングによるコア採取、ハツリ
等の方法でサンプリングし、これを適当な大きさに粉砕
した後、ｐＨ１．３〜２．７、好ましくはｐＨ１．７〜
２．３の範囲に維持した酸性水溶液中に溶解することに
よって、不溶残分量からセメント硬化体中の未反応ポゾ
ラン量を求めることができる。The method for quantifying pozzolan of the present invention can also be used as a method for quantifying unreacted pozzolan contained in a cement hardened product formed from a cement composition comprising cement and siliceous pozzolan. For example, a part of the hardened cement product is sampled by a method such as core collection by boring or chipping, crushed to an appropriate size, and then pH 1.3 to 2.7, preferably pH 1.7 to
By dissolving in an acidic aqueous solution maintained in the range of 2.3, the amount of unreacted pozzolan in the hardened cement product can be determined from the amount of insoluble residue.
【００２０】セメント硬化体では、通常、セメントの水
和反応生成物、セメントとポゾランの反応生成物、及び
ポゾランの未反応物が含まれる。これらの内で、セメン
トの水和反応生成物とセメントとポゾランの反応生成物
については、ｐＨ１．３〜２．７の酸性水溶液にほぼ完
全に溶解するが、未反応ポゾランについては、この酸性
水溶液には実質的に溶解することなく不溶残分となって
残る。従って、セメント及びシリカ質ポゾランからなる
セメント組成物から形成されたセメント硬化体について
は、ｐＨ１．３〜２．７の酸性水溶液における不溶残分
量を未反応ポゾラン量と見なすことができる。The hardened cement product usually contains a hydration reaction product of cement, a reaction product of cement and pozzolan, and an unreacted product of pozzolan. Among these, the hydration reaction product of cement and the reaction product of cement and pozzolan are almost completely dissolved in an acidic aqueous solution of pH 1.3 to 2.7, but unreacted pozzolan is dissolved in this acidic aqueous solution. Remains substantially insoluble as an insoluble residue. Therefore, with respect to the hardened cement product formed from the cement composition composed of cement and siliceous pozzolan, the amount of the insoluble residue in the acidic aqueous solution of pH 1.3 to 2.7 can be regarded as the amount of unreacted pozzolan.
【００２１】尚、セメント硬化体では、セメント等の成
分は水和物となっているが、セメント硬化体を１０００
℃で１時間程度加熱すれば、水和した水分をほぼ完全に
除去することができる。従って、セメント硬化体の一部
をサンプリングし、１０００℃で１時間程度加熱して加
熱残分量を求めることによって、サンプリングしたセメ
ント硬化体の内で、原料としたセメント組成物の割合を
求めることができる。従って、使用したセメント組成物
の配合表からセメント組成物中のポゾランの配合割合を
知れば、原料として用いたポゾランの内で未反応ポゾラ
ンの割合を求めることができる。In the hardened cement, the components such as cement are hydrates, but the hardened cement is 1000
By heating at ℃ for about 1 hour, the hydrated water can be almost completely removed. Therefore, by sampling a part of the hardened cement product and heating it at 1000 ° C. for about 1 hour to determine the residual heating amount, the ratio of the cement composition used as the raw material in the hardened cement product can be determined. it can. Therefore, if the compounding ratio of pozzolan in the cement composition is known from the compounding table of the used cement composition, the ratio of unreacted pozzolan in the pozzolans used as the raw material can be obtained.
【００２２】また、セメントとシリカ質ポゾランの他
に、骨材を含むセメント組成物から形成されたセメント
硬化体については、前述したセメント組成物中に骨材が
含まれる場合と同様に、骨材の種類に応じて、使用する
酸性水溶液のｐＨ値における不溶残分となる割合を予め
求めておき、配合表中の骨材の配合割合に基づいて骨材
の不溶残分量を見積もり、測定試料とするセメント硬化
体の不溶残分量から骨材の不溶残分の見積量を除いた量
を未反応ポゾラン量とすることによって、セメント硬化
体中の未反応ポゾラン量を求めることができる。In addition to the cement and the siliceous pozzolan, a hardened cement formed from a cement composition containing an aggregate is the same as when the aggregate is contained in the cement composition described above. Depending on the type, the ratio of the insoluble residue in the pH value of the acidic aqueous solution to be used is obtained in advance, and the insoluble residue amount of the aggregate is estimated based on the mixing ratio of the aggregate in the composition table, and the measurement sample The amount of the unreacted pozzolan in the hardened cement product can be determined by determining the amount of the unreacted pozzolan obtained by subtracting the estimated amount of the insoluble residue of the aggregate from the insoluble residue amount of the hardened cement product.
【００２３】以上の方法によってセメント硬化体中の未
反応ポゾラン量を求めることが可能となる。この様にし
て求めたセメント硬化体中の未反応ポゾラン量は、例え
ば、セメント構造物の構造解析、劣化診断等に有効に利
用することができる。By the above method, the amount of unreacted pozzolan in the hardened cement product can be determined. The amount of unreacted pozzolan in the hardened cement product thus obtained can be effectively used, for example, in the structural analysis of the cement structure, deterioration diagnosis, and the like.
【００２４】[0024]
【発明の効果】本発明のポゾランの定量方法によれば、
シリカ質ポゾラン混合比の高いセメント組成物であって
も、簡単な操作で正確にポゾラン含有率を求めることが
でき、セメント製品の品質管理を適切に行うことができ
る。According to the method for quantifying pozzolan of the present invention,
Even with a cement composition having a high siliceous pozzolan mixing ratio, the pozzolan content can be accurately determined by a simple operation, and the quality control of the cement product can be appropriately performed.
【００２５】また、本発明方法によれば、セメント硬化
体中の未反応ポゾラン量を測定することが可能となるの
で、この結果をセメント構造物の構造解析、劣化診断等
に有効に利用できる。Further, according to the method of the present invention, it is possible to measure the amount of unreacted pozzolan in the hardened cement product, and this result can be effectively used for the structural analysis, deterioration diagnosis and the like of the cement structure.
【００２６】[0026]
【実施例】以下、実施例を挙げて本発明を更に詳細に説
明する。EXAMPLES The present invention will be described in more detail with reference to examples.
【００２７】実施例１
シリカ質ポゾランとしてフライアッシュ、石炭ガス化ス
ラグ又は焼却灰溶融スラグを用い、これらのシリカ質ポ
ゾランを普通ポルトランドセメントと混合してセメント
組成物を調製した。EXAMPLE 1 Fly ash, coal gasification slag or incinerated ash molten slag was used as the siliceous pozzolan, and these siliceous pozzolans were mixed with ordinary Portland cement to prepare a cement composition.
【００２８】これらの各セメント組成物１ｇに対して水
２００ｍｌを加えて撹拌し、水溶液のｐＨを測定しなが
ら、塩酸を滴下し、水溶液のｐＨが一定値となるように
２０分間保持した。その後、この水溶液をろ過し、９５
０℃で６０分間加熱して、残分を秤量した。200 ml of water was added to 1 g of each of the cement compositions, and the mixture was stirred. While measuring the pH of the aqueous solution, hydrochloric acid was added dropwise, and the pH of the aqueous solution was maintained at a constant value for 20 minutes. Then, the aqueous solution is filtered to
The residue was weighed by heating at 0 ° C. for 60 minutes.
【００２９】また、比較試験として、ＪＩＳ Ｋ ８１
８０（塩酸（試薬））に規定される塩酸（１＋１００）
２５０ｍｌにセメント組成物１ｇを溶解し、２０分間撹
拌した場合について、上記した方法と同様にして加熱残
分量を求めた。As a comparative test, JIS K 81
Hydrochloric acid (1 + 100) specified in 80 (hydrochloric acid (reagent))
When 1 g of the cement composition was dissolved in 250 ml and the mixture was stirred for 20 minutes, the residual heating amount was determined by the same method as described above.
【００３０】上記した試験結果の評価方法としては、セ
メント組成物中のポゾラン混合割合（ａ）と上記試験に
よる加熱残分量（ｂ）とから、下記式によって定量誤差
を算出し、三種類の混合割合（３０、５０、７０重量
％）の全てにおいて定量誤差が±５％以内を◎、定量誤
差が±１０％以内を○とし、定量誤差が±１０％を上回
るものを含む場合を△とした。As a method of evaluating the above test results, a quantitative error is calculated by the following formula from the pozzolan mixing ratio (a) in the cement composition and the heating residual amount (b) in the above test, and three types of mixing are calculated. In all of the proportions (30, 50, 70% by weight), the quantitative error within ± 5% is ◎, the quantitative error within ± 10% is ○, and the case where the quantitative error exceeds ± 10% is Δ. .
【００３１】定量誤差（％）＝１００（ｂ−ａ）／ａ
試験に用いたセメント組成物の配合割合、酸性水溶液の
種類及び試験結果を下記表１に示す。Quantitative error (%) = 100 (ba) / a The mixing ratio of the cement composition used in the test, the kind of the acidic aqueous solution and the test result are shown in Table 1 below.
【００３２】[0032]
【表１】 [Table 1]
───────────────────────────────────────────────────── フロントページの続き (72)発明者 秋山 達志 大阪府大阪市大正区南恩加島７丁目１番 55号 住友大阪セメント株式会社 セメ ント・コンクリート研究所内 (56)参考文献 特開 平11−209163（ＪＰ，Ａ) コンクリート工学年次論文報告集, 1999年，第21巻第２号，第121−126ペー ジ (58)調査した分野(Int.Cl.7，ＤＢ名) G01N 33/38 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Tatsushi Akiyama 7-55, Minami Enkajima, Taisho-ku, Osaka City, Osaka Prefecture Sumitomo Osaka Cement Co., Ltd. Cement and Concrete Research Laboratory (56) Reference JP 11- 209163 (JP, A) Annual Report on Concrete Engineering, 1999, Vol. 21, No. 2, pp. 121-126 (58) Fields investigated (Int.Cl. 7 , DB name) G01N 33/38
Claims (6)
メント組成物をｐＨ１．３〜２．７の範囲の酸性水溶液
に溶解し、不溶残分量からポゾラン量を求めることを特
徴とするセメント組成物中のポゾランの定量方法。1. A cement composition comprising cement and siliceous pozzolan, which is dissolved in an acidic aqueous solution having a pH range of 1.3 to 2.7, and the amount of pozzolan is determined from the amount of insoluble residue. A method for quantifying pozzolan.
有するセメント組成物をｐＨ１．３〜２．７の範囲の酸
性水溶液に溶解し、不溶残分量と骨材の不溶残分見積量
に基づいて、ポゾラン量を求めることを特徴とするセメ
ント組成物中のポゾランの定量方法。2. A cement composition containing cement, siliceous pozzolan and aggregate is dissolved in an acidic aqueous solution having a pH range of 1.3 to 2.7, and the amount of insoluble residue and the estimated amount of insoluble residue of aggregate are used. A method for quantifying pozzolan in a cement composition, comprising: determining the amount of pozzolan.
メント組成物から形成されたセメント硬化体を、ｐＨ
１．３〜２．７の範囲の酸性水溶液に溶解し、不溶残分
量から未反応ポゾラン量を求めることを特徴とするセメ
ント硬化体中の未反応ポゾランの定量方法。3. A hardened cement product formed from a cement composition comprising cement and siliceous pozzolan,
A method for quantifying unreacted pozzolan in a hardened cement product, which comprises dissolving in an acidic aqueous solution in the range of 1.3 to 2.7 and determining the amount of unreacted pozzolan from the amount of insoluble residue.
有するセメント組成物から形成されたセメント硬化体
を、ｐＨ１．３〜２．７の範囲の酸性水溶液に溶解し、
不溶残分量と骨材の不溶残分見積量に基づいて、未反応
ポゾラン量を求めることを特徴とするセメント硬化体中
の未反応ポゾランの定量方法。4. A cement hardened body formed from a cement composition containing cement, siliceous pozzolan and an aggregate is dissolved in an acidic aqueous solution having a pH range of 1.3 to 2.7,
A method for quantifying unreacted pozzolan in a hardened cement, which comprises determining the amount of unreacted pozzolan based on the amount of insoluble residue and the estimated amount of insoluble residue of aggregate.
である請求項１〜４のいずれかに記載の方法。5. The method according to claim 1, wherein the pH of the acidic aqueous solution is in the range of 1.7 to 2.3.
水溶液に溶解する際に、ｐＨの変動幅を０．２以内に維
持することを特徴とする請求項１〜５のいずれかに記載
の方法。6. The method according to claim 1, wherein when the cement composition or the hardened cement product is dissolved in an acidic aqueous solution, the fluctuation range of pH is maintained within 0.2. .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000288175A JP3528048B2 (en) | 2000-09-22 | 2000-09-22 | Determination of pozzolan in cement |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000288175A JP3528048B2 (en) | 2000-09-22 | 2000-09-22 | Determination of pozzolan in cement |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2002098686A JP2002098686A (en) | 2002-04-05 |
| JP3528048B2 true JP3528048B2 (en) | 2004-05-17 |
Family
ID=18771805
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000288175A Expired - Lifetime JP3528048B2 (en) | 2000-09-22 | 2000-09-22 | Determination of pozzolan in cement |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3528048B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304832C (en) * | 2004-07-16 | 2007-03-14 | 重庆市建筑科学研究院 | Method for detecting content of fly ash in newly stirred concrete |
| CN100520350C (en) * | 2005-12-26 | 2009-07-29 | 重庆市节能技术服务中心 | Method for detecting content of river sand and fly ash in concrete mixture |
| JP6850989B2 (en) * | 2017-07-28 | 2021-03-31 | 三菱マテリアル株式会社 | Method for quantifying silica fume contained in silica fume-containing cement composition and method for producing silica fume-containing cement composition |
-
2000
- 2000-09-22 JP JP2000288175A patent/JP3528048B2/en not_active Expired - Lifetime
Non-Patent Citations (1)
| Title |
|---|
| コンクリート工学年次論文報告集，１９９９年，第２１巻第２号，第１２１−１２６ページ |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2002098686A (en) | 2002-04-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Bertron et al. | Attack of cement pastes exposed to organic acids in manure | |
| Lloyd et al. | Acid resistance of inorganic polymer binders. 1. Corrosion rate | |
| Zhang et al. | Hydration of high-volume fly ash cement pastes | |
| Glasser et al. | Solubility reactions of cement components with NaCl solutions: I. Ca (OH) 2 and CSH | |
| Macphee et al. | Solubility and aging of calcium silicate hydrates in alkaline solutions at 25 C | |
| Siler et al. | Isothermal and solution calorimetry to assess the effect of superplasticizers and mineral admixtures on cement hydration | |
| JP5414170B2 (en) | Coal ash evaluation method | |
| Zornoza et al. | Chloride-induced corrosion of steel embedded in mortars containing fly ash and spent cracking catalyst | |
| US20160061806A1 (en) | Assessment method | |
| JP2011133344A (en) | Evaluation method of expression property of strength of coal ash and improvement method of expression property of strength | |
| Li et al. | Quantitative analysis of fly ash in hardened cement paste | |
| JP3528048B2 (en) | Determination of pozzolan in cement | |
| JP2017142140A (en) | Fly ash activity index prediction method, and method for producing fly ash mixed cement | |
| KR20090037763A (en) | Concrete composition determination method | |
| JP4183367B2 (en) | Coal ash evaluation method | |
| Boualleg | The Study of Slag Cement's Microstructural Properties. | |
| Hime | Chemical methods of analysis of concrete | |
| JP4610396B2 (en) | Method for quantifying slag | |
| Ghanizadeh et al. | A New Method to Measure Available Alkalis of Cementitious Blends | |
| EP4686711A1 (en) | Cement-free acid-resistant alkaline binder | |
| CS247068B2 (en) | Method for determination of solid substances activity | |
| Vishavkarma et al. | Assessment of Hydration Stages in the Property Development of Portland Blended Cement Systems Containing Limestone Powders | |
| Potgieter et al. | Investigation into methods of chloride analysis of South African cement and cement-related materials with low chloride concentrations | |
| CN101315335B (en) | Quick test method for metakaolin activity used for inorganic polymer gelled material | |
| JP2001281235A (en) | Sorting method of coal ash and civil engineering materials |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| TRDD | Decision of grant or rejection written | ||
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20040128 |
|
| A61 | First payment of annual fees (during grant procedure) |
Free format text: JAPANESE INTERMEDIATE CODE: A61 Effective date: 20040209 |
|
| R150 | Certificate of patent or registration of utility model |
Free format text: JAPANESE INTERMEDIATE CODE: R150 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20080305 Year of fee payment: 4 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090305 Year of fee payment: 5 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090305 Year of fee payment: 5 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100305 Year of fee payment: 6 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100305 Year of fee payment: 6 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110305 Year of fee payment: 7 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110305 Year of fee payment: 7 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120305 Year of fee payment: 8 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120305 Year of fee payment: 8 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20130305 Year of fee payment: 9 |