Dissolving gypsum.

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Dissolving gypsum.

Postby PeeBee » Sat Jan 21, 2017 17:32

I've been messing about with gypsum additions to emulate the beer I grew up with - Marston's Pedigree. With some success too, but I'm running into problems that could be putting me off trying further experiments.

At the moment I'm getting about 230ppm sulphate into my water in the form of gypsum, and another 70ppm as Epsom salts. This has a marked effect on the flavour (malt flavours, I don't really notice the reputed effects on hop bitterness). The flavour is instantly recognisable as Pedigree. I'm about at maximum for dissolving gypsum (only about 0.5g/L), it's quite a process, involving putting the gypsum in a litre of water (about 25g), using a stick blender on it for about 1 minute, settling for 2-3 minutes, returning the clear (-ish) portion back to the 60L of brewing water, recharging the flask with another litre, and repeating several times (5-6?) until the gypsum is mainly dissolved.

The problems are:

1: It's time consuming! Taking at least an hour (about 60L for sparging, but another 20 for mashing).

2: I'm getting about 230ppm sulphate dissolved, but Burton water is reputed to have 600-800ppm. About 1/4 can be attributed to Epsom Salt but that's easy to dissolve.

3: While the effect on the flavour is definitely going the right way, those effects are not as strong as the real thing (hardly surprising, I'm not getting so much gypsum dissolved).

4: THE BIG ONE! The flavour enhancement is temporary. From tapping the barrel (at this point only about two weeks from starting brew) there is only three weeks before the flavour effect evaporates. It then becomes an "average" beer. As my smallest brew length is 40L this means there is still an entire keg unbroached.

The beer is served with minimal carbonation (equivalent to 1-2psi), from hand pump and at about 14-5degrees. I am very aware that serving chilled and at high carbonation will kill such subtle effects.

SO... Has anyone got a tried and tested method for dissolving large quantities of gypsum? Some 1-2g/L? I understand that gypsum dissolves best at 40degrees (NOT boiling) and will try that next (I've been trying at 15-20degrees). Has anyone effectively dealt with similar problems with gypsum, especially the "only temporary" one?

Cheers :thumb:
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Re: Dissolving gypsum.

Postby Dennis King » Sat Jan 21, 2017 18:17

I only use small amounts that are split 50/50 in the mash and boil. The mash salts I add to the grain. With the boil I put some first runnings in a jug add the salts and stir like made for several mins. before adding to the boil.
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Re: Dissolving gypsum.

Postby Aleman » Sat Jan 21, 2017 20:19

Just because profiles are quoted with that level of sulphate in doesn't mean the brewers used it!!, Indeed I've seen books that suggest the maximum level that brewers used would have been about 350mg/l ;)

In cold(20C),distilled, water gypsum will dissolve at a maximum of 2750mg/l, warming it doesn't help as it is less soluble in hot water . . . even 40C is going to have a detrimental effect.

I'll be quite frank, I treat the full volume of the water, the night before, and have no issues getting 350-400mg/l sulphate from gypsum . . . but, here is the rub, I have practically nothing in the water, if you have medium to high levels of calcium, or are using calcium chloride, as well, then you are going to have the devils own job to get it to dissolve, and trying to get it to happen in a small volume of liquor is making it even harder.

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Re: Dissolving gypsum.

Postby PeeBee » Sun Jan 22, 2017 02:48

Aleman wrote:Just because profiles are quoted with that level of sulphate in doesn't mean the brewers used it!!, Indeed I've seen books that suggest the maximum level that brewers used would have been about 350mg/l ;) ...


I've been using about 300ppm because it was a recommended profile (Bru'n Water) which also stated it was more practical than trying to emulate the 6-800ppm in Burton water. But I want to move on for the afore-mentioned reasons. 300ppm just holds out the temptation to try for higher levels.

Aleman wrote:...In cold(20C),distilled, water gypsum will dissolve at a maximum of 2750mg/l, warming it doesn't help as it is less soluble in hot water . . . even 40C is going to have a detrimental effect. ...


My "targets" are still below the maximum (1-2g/l, you say 2.7 is the max.) so that sounds hopeful. I'd picked up (from Bru'n Water again) that gypsum attains its greatest solubility at 40C, you would say less? Searching Google wasn't producing any sound evidence but I got a few "solubility" graphs suggesting best solubility is around 25-40C but didn't look like I was in for a breakthrough.

Aleman wrote:...I'll be quite frank, I treat the full volume of the water, the night before, and have no issues getting 350-400mg/l sulphate from gypsum . . . but, here is the rub, I have practically nothing in the water, if you have medium to high levels of calcium, or are using calcium chloride, as well, then you are going to have the devils own job to get it to dissolve, and trying to get it to happen in a small volume of liquor is making it even harder.


Now that's very interesting, so before I attempt to dissolve the gypsum, DON'T attempt to dissolve all the other junk (Epsom salt, calcium chloride, sodium bicarbonate, etc.). Googling this only compounded a rising headache. I know my technique of hand-blending in a litre wont dissolve the gypsum, but I was hoping getting it finely suspended in a small volume before tipping into the bigger one would help. My water is off Denbigh Moor (Llyn Brenin) and contains next to nothing.

Thanks
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Re: Dissolving gypsum.

Postby PeeBee » Sun Jan 22, 2017 02:58

Dennis King wrote:I only use small amounts that are split 50/50 in the mash and boil. The mash salts I add to the grain. With the boil I put some first runnings in a jug add the salts and stir like made for several mins. before adding to the boil.

Along time ago (eek) I did used to practice adding the gypsum to the mash ingredients. But as I've grown into a incurable control freak, such a technique always leaves one thinking "just how much did dissolve"?
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Re: Dissolving gypsum.

Postby HTH1975 » Sun Jan 22, 2017 03:15

The way I've seen brewing salts used in a commercial setting is to mix them in with the grains when you mash in. That's the same thing that Murphys told me to do when I got my water report from them with their recommendations for brewing salt additions.

I don't treat my sparge water other than half a campden tablet, as all the salts are in the mash from the start.

2016: 330L brewed (72 gallons, over 8 firkins)
2017: 105L brewed (need to update this figure)
Drinking: Landlord clone
Conditioning: ciders from 2016, hedgerow barrolo, 1914 Courage RIS (10%).
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Re: Dissolving gypsum.

Postby Eric » Sun Jan 22, 2017 13:26

HTH1975 wrote:The way I've seen brewing salts used in a commercial setting is to mix them in with the grains when you mash in. That's the same thing that Murphys told me to do when I got my water report from them with their recommendations for brewing salt additions.

I don't treat my sparge water other than half a campden tablet, as all the salts are in the mash from the start.


That can be all well and good in many situations, but the OP reports he has virtually nothing in his water. That could result in all calcium salts being rinsed from the mash before many of the sugars. This, in turn, might lead to a rise in pH allowing extraction of some of the unwanteds that calcium in sparge water might otherwise deposit in the mash.

My water mostly has 95ppm calcium and until recently have generally added salts only to the mash and kettle. Of late I have been experimenting adding small amounts of salts to the grain bed during fly sparging which seem to slow rise in pH of runnings and increase extraction rate. This is work in progress and I currently couldn't dispute any findings to the contrary, but my beers would seem to have improved.
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Re: Dissolving gypsum.

Postby HTH1975 » Sun Jan 22, 2017 16:00

Maybe AMS would work better for you if soluability is a problem and you're concerned about having no salts left in the mash at the sparge stage... http://www.murphyandson.co.uk/Datasheets/AMS.pdf

2016: 330L brewed (72 gallons, over 8 firkins)
2017: 105L brewed (need to update this figure)
Drinking: Landlord clone
Conditioning: ciders from 2016, hedgerow barrolo, 1914 Courage RIS (10%).
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Re: Dissolving gypsum.

Postby PeeBee » Sun Jan 22, 2017 17:31

Before this thread runs off in a direction I wasn't planning...

I do not have a particular problem with pH at any stage, which I guess is down to adequate water treatment. I started this thread solely to figure out a good way of adding large amounts of gypsum so it can more directly influence the flavour of the beer; because gypsum will "taste" and modify the taste (and aroma, as in the famous Burton "snatch"). And perhaps figure out how to make those changes to flavour a lot less transient (at the moment I only get the desired flavour enhancements for about three weeks).

What I've gleaned so far is to attempt dissolving the gypsum first, before any attempt to dissolve the easier stuff (especially <other> calcium salts), and warm the water only very slightly before attempting to dissolve gypsum (between 25C and 40C, say 30C?).

(EDIT: 22/01 19:10 inserted "<other>" for clarity, in reaction to following post).

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Re: Dissolving gypsum.

Postby Eric » Sun Jan 22, 2017 19:42

Gypsum is a calcium salt, calcium sulphate dihydrate, CaSO4. 2H2O.
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Re: Dissolving gypsum.

Postby Kev888 » Sun Jan 22, 2017 20:45

Maybe my water is conducive, but it only takes a bit of stirring (manually, with a big spoon) to dissolve quite a lot of gypsum in the full volume of (tepid) mash water. Its a little stubborn certainly, but nothing hugely taxing. I usually add the gypsum before other salts mainly because it takes longer to dissolve; perhaps this order is a happy accident.

Personal preferences vary; I just like to dissolve my salts in clean liquor in order to visually check that they have dissolved properly, and its also easier to stir/mix to uniformity before the grain is introduced. But its not the only method.

Eric's point about not neglecting the sparge liquor (If I understood correctly) makes sense to me too, if the water is lacking. We know that pH is important in the sparge (as well as the mash) so salts diminishing too far during that stage would be detrimental. I'm also coming to the conclusion that decent calcium levels in all mash/sparge/boil stages is no bad thing.

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Re: Dissolving gypsum.

Postby EvansTheSteam » Sun Jan 22, 2017 21:57

Damn it, this forum doesn't change!
Nit picking to the Nth degree about Gypsum and Epsom...I despair.
Come on chaps, brewing is an art, not a science!

I await the flak
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Re: Dissolving gypsum.

Postby HTH1975 » Sun Jan 22, 2017 22:05

I'd say it's a balance of art AND science. You can take the arty approach and you'll eventually find your way by trial and error. Alternatively, you can fully understand the science behind things and use that to your advantage.

2016: 330L brewed (72 gallons, over 8 firkins)
2017: 105L brewed (need to update this figure)
Drinking: Landlord clone
Conditioning: ciders from 2016, hedgerow barrolo, 1914 Courage RIS (10%).
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Re: Dissolving gypsum.

Postby Eric » Sun Jan 22, 2017 22:18

PeeBee wrote:I've been messing about with gypsum additions to emulate the beer I grew up with - Marston's Pedigree. With some success too, but I'm running into problems that could be putting me off trying further experiments.

At the moment I'm getting about 230ppm sulphate into my water in the form of gypsum, and another 70ppm as Epsom salts. This has a marked effect on the flavour (malt flavours, I don't really notice the reputed effects on hop bitterness). The flavour is instantly recognisable as Pedigree. I'm about at maximum for dissolving gypsum (only about 0.5g/L), it's quite a process, involving putting the gypsum in a litre of water (about 25g), using a stick blender on it for about 1 minute, settling for 2-3 minutes, returning the clear (-ish) portion back to the 60L of brewing water, recharging the flask with another litre, and repeating several times (5-6?) until the gypsum is mainly dissolved.

The problems are:

1: It's time consuming! Taking at least an hour (about 60L for sparging, but another 20 for mashing).

2: I'm getting about 230ppm sulphate dissolved, but Burton water is reputed to have 600-800ppm. About 1/4 can be attributed to Epsom Salt but that's easy to dissolve.

3: While the effect on the flavour is definitely going the right way, those effects are not as strong as the real thing (hardly surprising, I'm not getting so much gypsum dissolved).

4: THE BIG ONE! The flavour enhancement is temporary. From tapping the barrel (at this point only about two weeks from starting brew) there is only three weeks before the flavour effect evaporates. It then becomes an "average" beer. As my smallest brew length is 40L this means there is still an entire keg unbroached.

The beer is served with minimal carbonation (equivalent to 1-2psi), from hand pump and at about 14-5degrees. I am very aware that serving chilled and at high carbonation will kill such subtle effects.

SO... Has anyone got a tried and tested method for dissolving large quantities of gypsum? Some 1-2g/L? I understand that gypsum dissolves best at 40degrees (NOT boiling) and will try that next (I've been trying at 15-20degrees). Has anyone effectively dealt with similar problems with gypsum, especially the "only temporary" one?

Cheers :thumb:



Suggest you click here and select the data sheet for Calcium Sulphate (gypsum).
On the second page there is a section headed "Application" which deals with quantities in excess of 75g/hl which is equivalent to 0.75g per litre as you intend.
You will see they also refer to pH, the influence of calcium in brewing should only be ignored at your peril.

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Re: Dissolving gypsum.

Postby PeeBee » Mon Jan 23, 2017 02:25

EvansTheSteam wrote:Damn it, this forum doesn't change!
Nit picking to the Nth degree about Gypsum and Epsom...I despair.
Come on chaps, brewing is an art, not a science! ...

Not "nit picking". And not trying to do science things with gypsum. I'm using gypsum as an ingredient, but it doesn't want to play at my games so I'm seeing if there is any "science" to help me. At the Burton water levels of gypsum it contributes a very distinct flavour, but during my youth (when I used to live not far from where you say you do) I didn't hold my glass up and say "its the gypsum doing that" but after 45 years of brewing I finally can say that now (if I really wanted to :geek: ).
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Re: Dissolving gypsum.

Postby EvansTheSteam » Mon Jan 23, 2017 04:24

PeeBee wrote:I used to live not far from where you say you do


Yes, I'm a terrible liar aren't I!

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Re: Dissolving gypsum.

Postby mabrungard » Sat Jan 28, 2017 20:12

The 600 to 800 ppm sulfate reputed for Burton water is from local groundwater results. However, the local hydrology and aquifers led to significant dilution of those concentrations at the breweries. Sulfate-rich water permeates up through the local marl into the shallow sand and gravel aquifer. That shallow aquifer is directly connected to River Trent, whose waters are much less mineralized. When there is little groundwater withdrawal from the shallow aquifer, that water might have been as high as reputed. The preponderance of breweries in Burton meant that there was a lot of withdrawal at one time. Many of those breweries drilled wells directly into the deep aquifer below the marl to get more mineralized water, but they did have to dilute it with the shallow water to make it suitable for brewing.

600 to 800 ppm sulfate is not a goal you should seek in brewing, but I do suggest that you try adding an appropriate slug of gypsum to a glass of your beer to replicate that level. See if you like it. Most have found that it's not ideal.

Colin Kaminski (co-author of the Water book) told me that he brewed some pale ales at his brewery in Napa California with 600 ppm sulfate. He said he liked the beers, but most of his customers did not.

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Re: Dissolving gypsum.

Postby Eric » Sun Jan 29, 2017 12:31

mabrungard wrote:
600 to 800 ppm sulfate is not a goal you should seek in brewing, but I do suggest that you try adding an appropriate slug of gypsum to a glass of your beer to replicate that level. See if you like it. Most have found that it's not ideal.

Colin Kaminski (co-author of the Water book) told me that he brewed some pale ales at his brewery in Napa California with 600 ppm sulfate. He said he liked the beers, but most of his customers did not.


Adding gypsum to beer wouldn't be representitive as much, perhaps most calcium from gypsum additions would be deposited at all stages of brewing.

Beer made with 600 to 800ppm sulphate from gypsum might not make the beer you are expecting, but you, like Colin Kaminski, would know first hand how such beers might taste. Several years since I brewed with close to 500ppm sulphate and produced an overly dry beer that took longer than I'd hoped to loose its rougher edges, but I'm pleased I did as it was a worthy experiment.
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Re: Dissolving gypsum.

Postby PeeBee » Sun Jan 29, 2017 14:21

mabrungard wrote:... 600 to 800 ppm sulfate is not a goal you should seek in brewing, but I do suggest that you try adding an appropriate slug of gypsum to a glass of your beer to replicate that level. See if you like it. Most have found that it's not ideal. ...

Okay, if I'm possibly going about it wrong bumping up the sulphite levels (but I'll try the "slug of gypsum to a glass" technique, thanks for that), any idea why the desired flavour enhancement evaporates after three weeks or so? The resultant aged beer, while still good, lacks that something that once made it "exceptional". (This is not a "one off", it keeps happening which is tragic having just figured out how to arrive at my goal).

There is the possibility that it would happen to "the real stuff" if kept that long, I have to remember I'm trying retain an emulation of something that was never intended to be aged. But I hear stories of Burton IPAs made to very high strengths and exported on voyages lasting months, yet still being described as having the "Burton snatch".


(EDIT: Tried the "slug of gypsum to a glass" technique - 0.25g in half pint - but can't say I could notice a lot of difference. It certainly didn't reverse the loss of specific "enhancement". Did it taste "drier"? Possibly if stretching the imagination. Can't understand anyone disliking it as
not any noticeable difference to me.).

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Re: Dissolving gypsum.

Postby PeeBee » Sun Jan 29, 2017 14:41

Eric wrote:... Several years since I brewed with close to 500ppm sulphate and produced an overly dry beer that took longer than I'd hoped to loose its rougher edges, but I'm pleased I did as it was a worthy experiment.

That's not tying up with what I'm currently doing, but holds out some hope for what I want to do...

My recipe is 100% malt (2% roast for colour) mashed at 64C to get a dry finish (adding sugar is another way but I don't want to do that). And keeping it longer is exactly what I don't want to do! Not that I ever detect "rougher edges", but I'm currently only using 300ppm sulphite.

EDIT: I've given that recipe a name too... Gwehelyth. (Figure it out!).
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Re: Dissolving gypsum.

Postby HTH1975 » Sun Jan 29, 2017 17:19

PeeBee wrote:
Eric wrote:... Several years since I brewed with close to 500ppm sulphate and produced an overly dry beer that took longer than I'd hoped to loose its rougher edges, but I'm pleased I did as it was a worthy experiment.

That's not tying up with what I'm currently doing, but holds out some hope for what I want to do...

My recipe is 100% malt (2% roast for colour) mashed at 64C to get a dry finish (adding sugar is another way but I don't want to do that). And keeping it longer is exactly what I don't want to do! Not that I ever detect "rougher edges", but I'm currently only using 300ppm sulphite.

EDIT: I've given that recipe a name too... Gwehelyth. (Figure it out!).


Have you considered AMS? - seems that your issue is getting enough sulphates dissolved. AMS seems the natural choice.

2016: 330L brewed (72 gallons, over 8 firkins)
2017: 105L brewed (need to update this figure)
Drinking: Landlord clone
Conditioning: ciders from 2016, hedgerow barrolo, 1914 Courage RIS (10%).
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Re: Dissolving gypsum.

Postby Eric » Sun Jan 29, 2017 19:12

HTH1975 wrote:
Have you considered AMS? - seems that your issue is getting enough sulphates dissolved. AMS seems the natural choice.


AMS is a mix of hydrochloric acid and sulphuric acid. It will increase sulphate but also chloride provided there is sufficient alkalinity present, else it will simply strip the nickel off the heating element. Sulphuric acid would be the obvious choice, but only if the OP's water is alkaline and needs treating.

Have I missed a water analysis? Can anyone advise the mineral content of this water?
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Re: Dissolving gypsum.

Postby GrowlingDog » Sun Jan 29, 2017 23:13

Eric wrote:Have I missed a water analysis? Can anyone advise the mineral content of this water?


There's a sensible suggestion. Before messing about adding this that or the other to your water, it would be a really good idea to know what is in it to start with.
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Re: Dissolving gypsum.

Postby PeeBee » Sun Jan 29, 2017 23:43

Eric wrote:... Have I missed a water analysis? Can anyone advise the mineral content of this water?

You want the water analysis? It's not going to say much ('cos there ain't much to say):
http://www.dwrcymru.com/pdf-data/WaterQuality_2014%20%20%20%20%20%20B06_20131231.pdf
I'm not about to chuck any "AMS" in it. But I do use phosphoric acid when I'm feeling like unnecessarily faffing about (0.41mL was the calculated amount that went into 60L for sparging my last brew). If anyone needs to know how to measure out quantities like that ...
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Re: Dissolving gypsum.

Postby HTH1975 » Mon Jan 30, 2017 00:34

PeeBee wrote:
Eric wrote:... Have I missed a water analysis? Can anyone advise the mineral content of this water?

You want the water analysis? It's not going to say much ('cos there ain't much to say):
http://www.dwrcymru.com/pdf-data/WaterQuality_2014%20%20%20%20%20%20B06_20131231.pdf
I'm not about to chuck any "AMS" in it. But I do use phosphoric acid when I'm feeling like unnecessarily faffing about (0.41mL was the calculated amount that went into 60L for sparging my last brew). If anyone needs to know how to measure out quantities like that ...


Nice water for making lager.

2016: 330L brewed (72 gallons, over 8 firkins)
2017: 105L brewed (need to update this figure)
Drinking: Landlord clone
Conditioning: ciders from 2016, hedgerow barrolo, 1914 Courage RIS (10%).
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